* GB785083 (A)

Description: GB785083 (A) ? 1957-10-23

Carbon paper

Description of GB785083 (A)

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BE546536 (A) FR1130895 (A) LU33807 (A) BE546536 (A) FR1130895 (A) LU33807 (A) less Translate this text into Tooltip

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The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes.

13 J 7, ' 1 _ - PATENT SPECIFICATION 785,083 Date of Application and filing Complete Specification: August 29, 1955. No 24703/55 Application made in United States of America on March 28, 1955. Complete Specification Published: October 23, 1957. Index at acceptance:-Classes 109 ( 4), H; and 140, A( 1 A: 2 G: 2 N 2: SF: 5 X: 1;B 2). International Classification:-B 411. COMPLETE SPECIFICATION Carbon Paper We, THE GOODYEAR TIRE & RUBBER COMPANY, a corporation organized under the laws of the State of Ohio, United States of America, with offices at 1144 East Market Street, Akron, Ohio, United States of America, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to

be performed, to be particularly described in and by the following statement:- This invention relates to an improved carbon paper and a process of producing it. The carbon paper is designed particularly for use on typewriters, duplicators and other machines for reproducing copies of all sorts of written documents, invoices, etc The carbon paper may be supplied to the machines as individual sheets, or may be supplied in book form for producing any desired number of copies. A further use for the carbon paper is as a ribbon for a typewriter or other duplicating machine This ribbon may be of any desired width. One difficulty heretofore experienced in using carbon papers is that a thin paper is required to produce a clearly defined impression, but thin papers are apt to be died out or otherwise damaged by the type hitting them, particularly when the type hits with the force necessary to produce a large number of copies It is the object of this invention to produce a very thin carbon paper sufficiently strong to withstand repeated impressions made with sufficient force to pro, duce a large number of copies The paper has additional advantages as will be more fully explained in what follows. The carbon paper of this invention is strengthened by laminating rubber hydrochloride to it The ordinary unstretched rubber hydrochloride film on the market is at least about 0008 inch thick This is so thick that on lamination to even the thinnest carbon paper it does not give good impressions Likewise it does not have the desired tensile strength When rubber hydrochloride film is heated and then stretched to at least double its original dimensions it is not only made thinner, but its tensile strength is im 50 proved The film may be stretched to as much as six times its original arear while still retaining sufficient elasticity to withstand the blows from the type of a typewriter or the like, and this may be very satisfactorily 55 employed for lamination to the tissue paper from which carbon paper is manufactured. The film may be stretched in one direction, or it may be stretched -both laterally and longitudinally Such film is known in the 60 trade as "oriented". In the manufacture of carbon paper, the oriented film is laminated to one side of a thin, strong tissue paper by any suitable adhesive The carbon transfer composition 65 is applied to the other side of the sheet. The carbon transfer composition may be applied to the sheet before lamination, but in most lamination processes it will be desirable to laminate the oriented film to the tis 70 sue before applying the carbon transfer composition to it.

In laminating very thin webs of rubber hydrochloride film to a tissue it is difficult to prevent the occurence of wrinkles or un 75 laminated areas According to the preferred process of this invention the film is oriented on the same roll which accomplishes the lamination of the film to the tissue paper. Since the film is oriented under tension and 80 it is held flat against the surface of the roll between the time it is oriented and the time it is laminated to the paper, no wrinkling occurs and the film is flat and smooth as it is laminated to the paper 85 The carbon composition used on the paper is not a part of the invention The following composition has been found satisfactory, but many other compositions may be used. Carnauba wax 9 parts by weight 90 1 1i 785,083 Montan wax 6 -Violet dye 7 Mineral oil 63, Lamp black 15 Although the invention is described more particularly in connection with the preparation of a blue-black carbon paper, it is to be understood that papers bearing coloring compositions other than those containing carbon black may be utilized Such papers are known as red carbon paper, etc. The invention will be described more particularly in connection with the accompanying drawings, in whichFig 1 is an enlarged cross section through the carbon paper; and Fig 2 is a flow sheet, shown quite diagrammatically, which illustrates a process of producing the carbon paper. Figure 1 is purely illustrative The carbon composition A may be black or any color, and have any carrier base The tissue paper B may be of any thickness up to, for example, 35 pounds per ream Papers of 15 pounds per ream and less in weight which are not strong enough to be used alone, are satisfactory, because the oriented film contributes very appreciable tensile and impact strength to the laminated sheet Although as will be illustrated in connection with the drawings, the adhesive C may be a wax, other adhesives such as latex adhesives, etc. may be used. The oriented film will ordinarily not be over about O 004 inch thick It may, for example, be not more than 0002 inch thick. There are various methods of producing the laminated sheet Although it is possible that the oriented film may be laminated to the tissue to which the carbon transfer composition has first been applied, the simpler procedure is that illustrated in Fig 2 The tissue B from the roll 1 is coated with a composition C from the bath 2 by the applicator roll 3 This adhesive may, for example, be composed of 5 to 10 per cent of butyl rubber in a microcrystalline paraffin wax. Suitable waxes of this type are SoconyVacuum 2300 or Sovawax 100 ("Sovowax is a registered trade mark) Both of these waxes are microcrystalline paraffins Latextype adhesives which may be used

instead of the wax are Union Paste M-575 ("Union" is a Registered Trade Mark) or M-560. These may be used cold, but the waxes are applied at a temperature above their respective melting points. The coated tissue passes over a doctor blade on leaving the adhesion bath, and then after passing under the roller 5, passes over the roll 6 which is preferably rubber coated Here the oriented film is-laminated to it. The unstretched rubber hydrochloride film is supplied from the stock roll 10 It is ordinarily a film not over 001 inch thick. For example, it may be 0008 inch thick. This passes over the governor roll 11 to the laminating roll 12 This laminating roll is heated, for example, to 210 'F (plus or 70 minus 10 degrees) It is advantageously chrome plated It may be heated by steam, electricity, or other means. The surface speed of the laminating roll 12 is at least twice the surface speed of the 75 governor roll 11 As the film approaches the laminating roll, the heat from the roll softens it, and it is stretched just prior to contacting this roll Then, in the stretched condition, it is wrapped flat against the roll 80 so that there is no opportunity for it to shrink or wrinkle or become otherwise distorted = While lying flat against the laminating roll it makes flat pressure contact with the tissue, as the tissue and the film pass be 85 tween the two rolls 6 and 12 The adhesive coating on the paper is softened by the heat of the laminating roll, and a smooth uniform bond is formed between the contacting surfaces of the oriented film and the tissue 90 paper. The amount the film is stretched depends upon the difference in surface speeds of the rolls 11 and 12 The roll 12 may, for example, have a surface speed four to six or 95 more times that of the roll 11 Assuming, for example, that the unstretched film on the roll 10 is 0008 inch thick and that the roll 12 has a speed four times that of the roll 11, the oriented film will be stretched 100 to a thickness of 0002 inch. The laminated sheet after passing under the guide roll 15 is coated with the carbon transfer composition A from the tank 16. -The applicator roll 17 applies the carbon 105 transfer composition to the opposite side of the tissue from that to which the film has been laminated The carbon transfer composition may, for example, be the wax composition previously described This is ap 110 plied hot The sheet passes over a doctor blade after the composition is applied It is necessary to cool the carbon paper before winding it up, both in order to cool the coated composition and to be sure that the orent 115 ed film is cool and not tacky Therefore, the carbon paper passes under

the cold roll 18 before going to the wind-up 20 This cold roll may, for example, be cooled to 'F 120 The finished sheet does not smudge When rolled, the carbon composition contacts the film surface, but the film surface is so smooth and non-adhering that there is no transfer of the carbon to it 125 Ordinary carbon paper tends to absorb moisture on its uncoated side This tends to make the paper curl By coating the uncoated side with the oriented film, both sides become moisture proof and there is no 130 -2 785,083 further tendency of the paper to absorb moisture, so it always lies flat. An outstanding advantage of the laminated sheet is that it is thinner than most carbon papers and, therefore, gives a clearcut impression The oriented film has both a high tensile and impact strength with considerable resilience and elasticity Thus the improved carbon paper of this invention has prolonged life. The examples are illustrative Modifications may be made without departing from the invention which is defined in the claims which follow.

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* GB785084 (A)

Description: GB785084 (A) ? 1957-10-23

Polyazo dyestuffs

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The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in

particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes.

PATENT SPECIFICATION PATENT SPECIFICATION Inventor: HANS BAUMANN l, ' f 7859084 Date of Application and filing Complete Specification: Aug 31, 1955. No 24957/55. o If': Complete Specification Published: Oct 23, 1957. Index at acceptance:-Class 2 ( 4), P 2 G 2 C 31 P 2 H( 5: 6; 11; 12: 15: 21), P 4 (D: F), P 6, P 8 (A 1 A: B 3: C 3: DI: E), International Classification:-CO 9 b COMPLETE SPECIFICATION Polyazo Dyestuffs -We, BADISCHE ANILIN & SODA-FABRIK AKTIENGESELLSCHAFT, a Joint Stock Company organised under the laws of Germany, of Ludwigshafen Rhein, Germany, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: This invention relates to new polyazo dyestuffs More particularly, the invention relates to a new class of polyazo dyestuffs derived from a 44 diamino-diphenylmethane-3 31dicarboxylic acid and to a process of manufacturing these dyestuffs. It is an object of this invention to provide new polyazo dyestuffs, in particular polyazo dyestuffs for colouring leather and complex metal compounds, in particular complex cupric compounds, of said new polyazo dyestuffs. Another object is to provide polyazo dyestuffs derived from a 4 41-diamino-diphenylmethane-3 '3-dicarboxylic acid and containing at least four azo groups and at least two sulphonic acid groups. A still further object is to provide a method for preparing these dyestuffs. The polyazo dyestuffs according to this invention have the general formula MOOC, o 4 Al _NH 2 F C t { >Sw P dark brown to black shades having a very good fastness. The polyazo dyestuffs of this invention may be prepared by tetrazotizing a 4 41-diaminodiphenylmethane-3 31-dicarboxylic acid of the formula -z 400 C" wherein Z is a hydrogen atom or a phenyl or methyl group, and then coupling the resultant tetrazo compound with two molecules of aromatic compounds capable of being coupled and which still contain at least one azo group each and at least two sulphonic acid groups together. According to one embodiment of the invention, the new polyazo dyestuffs may be obtained by coupling one molecule of the tetrazotised

4 41-diamino diphenylmethane3.3 '-dicarboxylic acid with two molecules of an aromatic azo compound which contains an aromatic radical with at least two couplingdirection hydroxy and/or amino groups and at least one sulphonic acid group. An example of such aromatic azo compounds is the mono azo dyestuff prepared by reacting diazotized p-nitro-aniline with 1amino-8-hydroxy-naphthalene 3 6-disulphonic acid, the said dyestuff having the formula H O I'I W ( A y K 42 < " O wherein Z is a hydrogen atom or a methyl or a phenyl group, and Ar, and Ar 2 are identical o O 3 S \ so 3 C or different aromatic radicals, each of these aromatic radicals containing at least one further or the disazo dyestuff of the formula azo group and containing together at least two sulphonic acid groups The outstanding merit of these new polyazo dyestuffs is-the fact that they are, in particular o, in the form of their complex compounds with <"m-N r 7 r copper, cobalt or chromium salts, excellentq S | pHs% dyestuffs for leather, and yield thereby deep, SO lPrice 3 s 6 d l i i i i i o 7 ttfrazotized benzidine with one molecule of 1amino-8-hydroxy naphthalene-3 6-sulphonic acid and' one -molecule of 2-hydroxy naphthalene-3 6-sulphonic acid. According to another embodiment of the invention, one molecule of the tetrazotized 4.41-diamino diphenylmethane 3 3 t-dicarb oxylic acid is coupled first with an aromatic compound (I) which is free from azo groups but contains at least two couplig dire _ ng hydroxy andid/o 6 r amino groups, and one molecule of the disazo dyestuff thus obtained is then -converted by a further coupling reaction with two molecules of an aromatic compound (II) into a polyazo dyestuff, the radicals of the aromatic compounds -used for the two coupling reactions containing together at least two-sulphoni' acid groups. If, for the first coupling reaction, aromatic compouinds which fire free from amino groups are used, the second coupling reaction may be performed with two molecules of any aromatic diazo compound If, however, the aromatic compounds used in the first coupling reaction contain amino groups, the resulting disazoamino dyestuff can be tetrazotised and coupled with any aromatic compound capable of being coupled with a diazo or tetrazo compound Suitable 4:41-diamino-diphenylmethane-3 31dicarboxylic acids may be prepared by condensing two molecules of anthranilic acid with one molecule of formaldehyde, or benzaldehyde respectively, in acid medium as described by Heller and Fisselmanr (Liebigs Annalen der Chemie vol 324 ( 1902), p 118) It is also possible to prepare the 4 41-diaminodiphenylmethane-3 31-dicarboxylic acids in situ and to tetrazotize the raw and unpurified reaction mixture without isolating the 4 41-diaminodiphenylmethane-3 31-dicarboxylic acids. :Compounds which may be coupled with the ltetrazotized 4 41

diamino-diphenylmethane 3.31-dicarboxylic acids are compounds of the benzene and naphthalene series which contain two coupling-directing hydroxy and/or amino groups such as resorcinol, 1 3-diaminobenzene, I.8-dihydroxynaphthalene mono and disulphonic acids, 6-dihydroxynaphthalene-3sulphonic acid, 3-amino phenol, 3-hydroxydiphenyl amine or 1-amino-8-hydroxynaphthalene and their sulphonic acids. As diazo components which may be coupled onto the disazo dyestuff, formed by the first coupling reaction, where an aromatic compound which is free from amino groups has been used for this first coupling reaction; there may be used the diazotization products of aniline and its homologues and of their nitro or halogenated derivatives, such as nitroanilines and toluidines, 2.5-dichloroaniline, sulphanilic and metanilic acids, 4-chloroaniline-3-sulphonic acid, aniline2.5-disulphonic acid, 4-aminoazobenzene-3 4 'disulphonic acid, or of naphthylamines or their mono or disulphonic acid derivatives, such as 65 1-aminonaphthalene-4-sulphonic acid or 2aminonaphthalene-4 8-disulphonic add The selection of this'compound is made in such a manner that the polyazo dyestuff formed-contains at least-two sulphonic acid groups The 70 term " suilphonic acid " includes the free sulphonic acids as wellt as the salts of these acids, inparticular their alkali metal and ammonium salts. -If a diamino or hydroxyamino compound, 75 preferably of the benzene or naphthalene series, has been used for the first coupling reaction with the tetrazotized 4 41-diaminodiphenylmethane-3 31-dicarboxylic acid, this coupling product may be diazotized or tetrazotized again 80 and then coupled with an aromatic compound capable of being coupled preferably of the benzene or naphthalene series, such as 'a naphthol, a napthylamine or a sulphonic acid of these compounds, an amino naphthol or a 85 sulphonic acid thereof, a 1 3-dihydroxy or a 1.3-diamino -benzene, a 1 3-hy'droxyamino benzene= or the N-alkyl or N-aryl derivatives of these -compounds Care must be taken while performing this reaction-that the polyazo dye 90 stuffs contain at least two sulphonic acid groups The new polyazo dyestuffs may be converted into their complex copper, cobalt or chromium dyestuffs in the conventional manner, for in 95 stance, by reacting them with cupric, cobalt or chromium salts in aqueous solution or suspension, if necessary by adding basic compounds such as ammonia or amines. The new polyazo dyestuffs and their metal 100 complex compounds are excellently suitable for dyeing tanned leather irrespective of the manner in which the leather has been tanned. On account of their good dyeing capacity, they can be used in particular for the production of 105 suede leather Since they usually have a good solubility even in acid baths, the leathers may also be

dyed with these dyestuffs from concentrated baths without bronzing the dyed leather 110 The following Examples are given to illustrate the invention The parts given are by weight unless otherwise specified. EXAMPLE 1. 28.6 parts of 4 4 l-diamino-diphenylmethane-3 31-dicarboxylic acid are dissolved in 250 parts of water and 50 parts of hydrochloric acid (density 1 '16), and tetrazotized with 13 8 parts of sodium nitrite at a temperature between about O Q and 2 C The tetrazo compound forned is combined at about O C With a solution of 22 0 parts of resorcinol dissolved in: 200 parts of 10 % aqueous sodium hydroxide solution After the coupling reaction has been completed, the "intermediate disazo dyestuff" formed is precipitated by 'the addition of hydrochloric acid, filtered and dissolved 785,084 785,0 '84 in 600 paits of water while adding excess solution A tetrakis azo dyestuff having the sodium carbonate The diazo compound of 35 formula parts of metanilic acid is then added to said C O X -th ct c Nth K N OP _ is formed This dyestuff dyes leather in reddish brown shades with a good fastness On suede leather, buff-fast, deep reddish brown shades are obtained. EXAMPLE 2. The "intermediate disazo dyestuff" of Example 1 is coupled with the diazo compound of 51 parts of aniline-2 4 or 2 5-disulphonic acid The obtained tetrakis azo dyestuff is heated several hours in aqueous solution with parts of crystalline cobalt-I-chloride and 32 parts of sodium acetate A cobalt complex compound is thereby formed which dyes chrome tanned leather yellowish brown shades with a good fastness The corresponding copper complex compound yields on leathers, tanned by various methods, medium brown shades, the chromium complex compounds reddish brown shades EXAMPLE 3. A solution of 15 0 parts of anthranilic acid in 125 parts of water and 25 parts of 36 5 % hydrochloric acid is mixed at 70 C with 58 parts of a 3 % aqueous formaldehyde solution. The mixture is stirred at 70 ' C for several hours until the condensation is completed, cooled to O C and tetrazotized with 7 5 parts of sodium nitrite The obtained tetrazo compound is coupled with a solution of 11 0 parts of resorcinol in 200 parts of a 5 % aqueous sodium hydroxide solution To the solution of the "intermediate disazo dyestuff" formed, a solution of 16 parts sodium bicarbonate in 300 parts of water is added Then the diazo compound of 36 parts of 4-amino-azobenzene-3 4 'disuiphonic acid is added The hexakis azo dyestuff resultant of the formula M-O 3 s is salted out, filtered off by suction, and dissolved in water which contains a small amount of ammonia A solution of 25 0 parts of -crystalline copper sulphate in excess aqueous ammonia is added and the polyazo dyestuff converted

into its copper complex compound by heating This complex compound dyes leather manufactured by various tanning processes fast neutral brown shades. If instead of 4-amino-azobenzene-3 4 'disulphonic acid there is used an equivalent amount of an amino azo dyestuff obtained by coupling diazotized 2-naphthylamine-5 7disulphonic acid with 1-naphthylamine in conventional manner, a polyazo-dyestuff of the formula lX O o 9 is formed The copper complex compound of this dyestuff prepared by the usual methods yields fast reddish brown shades on leather. EXAMPLE 4 65 28.6 parts of 4 4 '-diamino-diphenylmethane3.3 '-dicarboxylic acid are tetrazotized as in Example 1 and coupled with 63 O parts of 1-amino-8-hydroxy naphthalene-3 6-disulphonic acid in the presence of excess sodium carbonate 70 The "intermediate disazo dyestuff" formed is isolated by acidifying and salting out and dissolved in 1000 parts of water containing -8 parts of a 50 % aqueous sodium hydroxide solution This solution is tetrazotized by the 75 addition of 7 5 parts of sodium nitrite and 70 parts of 36 5 i% hydrochloric acid at a temperature of about 5 C The reaction mixture is stirred for three hours and the excess of nitrite removed by the addition of urea Then an 80 aqueous solution of 22 parts of 1 3-diaminobenzene is added By adding gradually a solution of 56 parts of crystalline sodium acetate in - 4 785,084 parts of water, the coupling reaction is sodium carbonate, and then precipitated by the 5 completed The tetrazo dyestuff formed is addition of sodium chloride The resultant filtered off by suction, dissolved in 200 parts of tetrazo dyestuff of the formula hot water which contains 20 parts of anhydrous K co OH -K 3 v '' dyes chrome tanned leather deep brown shades Ex AMPLE 5. with a good fastness. If the 1-amino-8-hydroxynaphthalene-3 6 The "intermediate disazo dyestuff" of disulphonic acid is replaced by 1-amino-8 Example 4 is tetrazotized as described in hydroxynaphthalene-4 6-disulphonic acid, a Example 4, and then coupled with 22 parts of 20 tetrazo dyestuff is formed which under resorcinol while an excess of sodium carbonate analogous conditions dyes the leather some is added The resultant tetrakis azo dyestuff of what more reddish brown shades the formula o H o , o-X% SK A, So co Wu A p o, -x__/O -_ _/, S c o st' 5 o V -3 s% is filtered off by suction acid as described in Example 3, with 5 8 parts The dyestuff is dissolved in 2000 parts of of a 30 % aqueous formaldehyde solution The water To this solution 52:5 parts of crystalline condensation product is tetrazotized and copper sulphate and 60 parts of crystalline coupled with 31 9 parts of 1-amino-8-hydroxy 40 sodium sulphate are added, and then the mix naphthalene-3 6-disulphonic acid in the ture is heated to about 95 C

for one hour presence of sodium carbonate The "interBy salting out, a copper complex compound mediate disazo dyestuff" is filtered off by is isolated which dyes leather deep neutral suction, dissolved and tetrazotized again and brown shades having an excellent fastness coupled in an alkaline medium with 19 parts 45 EXAMPLE 6 of 3-hydroxy-diphenylamine The solution of 15 0 parts of anthranilic acid are condensed the resultant tetrakis azo dyestuff having the in an aqueous solution containing hydrochloric formula SO 3 Na > 11)121 9 is neutralized with formic acid and 27 5 parts black shades having an excellent fastness. of crystalline copper sulphate are added This If during the last coupling reaction one-half solution is: then boiled for a short time The of the 3-hydroxy-diphenylamine is replaced by copper complex dyestuff formed is salted out 5 5 parts of resorcinol, a mixed polyazo dye-:while the solution is still hot and then sucked stuff of the formula 60 off It dyes chrome tanned leather greenish ON "}Oe Aoc OC Co0 r Y r 85,084 ' is formed which gives a copper coriplex compound which dyes leather in fast deep black shades. EXAMPLE 7. 13; 7 0 parts of anthranilic acid are mixed with 100 parts of hydrochloric acid (density 1.085) After the addition of 52 5 parts of benzaldehyde and 5 0 parts of a 40 % sodium bisuiphite solution the mixture is gradually heated while refluxing to a temperature between 100 and 105 C The mixture is stirred for several hours at this temperature until the condensation is completed Into the still hot mixture, 400 parts of hydrochloric acid (density 1 08 '5) are introduced while stirring and the resultant clear solution is diluted by the addition of water to 1000 parts by volume. parts by volume of this solution are then mixed with an aqueous solution of 13 8 parts of sodium nitrite at a temperature of about O C The partly separated yellow tetrazo compound is gradually introduced into a solution which has been obtained by coupling 24.8 parts of diazotized p-nitroaniline with 54.6 parts of 1-amino-8-hydroxynaphthalene3.6-disulphonic acid, this acid solution having been neutralized after the coupling reaction by the addition of sodium hydroxide During the introduction of the tetrazo compound, the coupling mixture is kept permanently alkaline by the addition of sodium carbonate After the coupling reaction has been completed, the. formed dyestuff is salted out from the boiling reaction mixture and sucked off while still hot. The resultant tetrazo dyestuff of the formula NO O C C 00. o NID a 3 U i dyes chrome tanned grain leather and bark good fastness. tanned leather the same dark blue shades with A polyazo dyestuff of the formula giving similar dark blue shades on leather, is obtained

when there is used instead of diazotized p-nitro-aniline the coupling product of one molecule of tetrazotized benzidine and one molecule of 2-hydroxy-naphthalene-3 6disulphonic acid still containing one diazo group.

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* GB785085 (A)

Description: GB785085 (A) ? 1957-10-23

Liquid disinfectant for seed

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The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes.

= _: :, ?,'-:; . PATENT SPECIFICATION Inventors: BERNHARD GAUDIAN and GUNTER GOEZE -785,085 Date of Application and filing Complete Specification: Sept 13, 1955. No.-26170/55. Complete Specification Published: Oct 23, 1957 ,rt = Index at acceptance -Class 81 ( 1), E 1 A( 3 A 2: 3 A 4: 3 B 3: 5 C: 7 A: 7 B) ' International Classification:-A 611 'COMIPLETE'E S'PEEIFI'CATION :::: Liquid Disinfectant for Seed We, FAHLBERG-IIST G MA H a Geiman Company,-of Gruner Platz 12, ( 20 b)) Wolfenr biitted, Germany, do

hereby declare the invention, for whichb we pray that a Patent may be granted to us, and the method by Which it is to be performed, to be particularly desdcribedin and bythe following statement: It is kniiown to combat fungus diseases of seed corn with organic mercury compuiinds before sowing For this purpose two disinfecting methods are known), the dry method and the wet methiod Both have disadvantages, In the dry disinfecting method unavoidable poisonous dust arises, which endangeris the health of the workers -With the wet disinfecting method in most cases re-drying of the disinfected seed is necessary, to prevent harm to the germs) in storage of the disinfected grain, It has also been known to use oily, disinfectants With these disinfectants 200 grams per 100 'kg of seed are sufficient to cover them quite uniformly,, However oily disinfectants often cause harm to the germs, It is further known that for the production of liquid seed, disinfectants, organic mercury compounds or non-metal-containing organic fungicides may be dissolved or suspended in high percentage aqueous solutions o)f salts. Examples of such salts are calcium chloride and magnesium chloride For this purpose further aids to solution,, dispersing or emulsifying agents are needed. According to another known method viscous aqueous colloid solutions in combination with organic mercury compound's may be used However these methods have serious disadvantages, because in most cases they involve the use of emulsionsl and, dispersions, that is, the active substances are not dissolved, or are -only partly dissolved, Thus in disinfecting it cannot be guaranteed that, in the case of continuously operating disinfecting apparatus, a uniform distribution over the seed takes place. Over-dosing and under-dosing can easily take lPrice 3 s 6 d 1 place, which render the disiniectig effect dubious A further disadvantage is that an aqueous solution or dispersion wets the seed, or runs more on the seed than is the case for example 50 with organic solvents. It is known that organic mercury compounds in most cases are very difficult to dissolve at normal temperature in organic solvents, so that it is not possible to dissolve-them in fthei 55 quantities needed, for disifecting purposes, for example in, ethyl alcohol For example phenylHg-acetate or ethy-lg-chloride are only soluble in alcohol with difficultyat normal temperature Ethyl g-bromide only dis 60 solves to a slight extent in alcohol on, setting of a disinfectant to, 2 % of mercury. Now it has, been found that by the addition of alkaline earth metal salts,, alkali metal, salts, or amnmonium salts, or organic acids, such as 65 ammonium acetate, potassium thiocyanate, potassium propionate and' the like, in general, organic mercury compounds

surprisingly dissolve in alcohols. Furthermore it has been found that phenyl 70 Hg-acetate for example, which is almost insoluble in water, is not precipitated out of an alcoholic solution on dilution with water, so that in this manner also the seed can be disinfectedc in all wet disinfecting processes, such 75 as dipping disinfection, short disinfection, and sprinkling disinfection. However in the production of the liquid disinfectant it is, not absolutely necessary to add the prepared salts, but these can be caused to 80 arise in the production of the liquid disinfectant by chemical reaction of the components In these cases) also solution occurs,It is also possible to dissolve mixtures; of organic mercury compounds in this way, Mixtures of solvents 85 can also be used 'Furthermore insectoicides, wetting agents and adhesives, or dyestuffs can be added. grams of this liquid disinfectant are sufficient for example to cover 100 kg of 90 2. wheat or barley -or xy, unifoiytnly For Qats 2 grams, of this sblution applied, to 1 kg of 2,50-300 grams are needed, and in the case rye are sufficient to prevent an, infection of ofroot-seedi 500 600 gramsare needed fusarium 25 Offher alcohols which may be used are proEXAMPLES plachl opoyachlbutyl alcohol 1 4 2,1 %Y phen-yl-Hg- ace'tate and, isobutyl alcool

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* GB785086 (A)

Description: GB785086 (A) ? 1957-10-23

Novel unsaturated ketones and a process for the manufacture thereof

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The EPO does not accept any responsibility for the accuracy of data and information originating from other authorities than the EPO; in particular, the EPO does not guarantee that they are complete, up-to-date or fit for specific purposes.

IS =,, l,,= " 'O- i' PATENT SPECIFICATION 7859086 Date of Application and filing Complete Specification: Sept 13, 1955. No 26183/55. Application made in United States of America on Sept 13, 1954. Application made in United States of America on Oct 1, 1954. Application made in United States of America on Dec 7, 1954. Complete Specification Published: Oct 23, 1957. Index at acceptance:-Class 2 ( 3), C 1 G( 1 A 1: 1 A 2: 1 E: 2 A 1: 2 A 2:2 A 5: 6 Al: 6 A 2), C 3 A 14 A(LC: 2 D: 6: 8 B). International Classification:-C 07 c. COMPLETE SPECIFICATION Novel' Unsaturated Ketonesl and a Process for the Manufacture thereof C 3 A 8, We, F HOFFMANN-LA ROCH Aktiengesellschaft, a Swiss Co: 124-184, Grenzacherstrasse, Basl land, do hereby declare the ins which we pray that a patent may to us, and the method by which performed, to be particularly de and by the following statement:- The present invention relates ti saturated ketones and a process for facture thereof. The novel unsaturated ketones the invention are substances whi represented by the following gener R 15 2/=CH-CH 2 CFI-CCH, 2 t : ( 1) wherein R' stands for an alkyl taining from 2 to 5 carbon atoms radical and R 2 stands for the me or, together with RW, the pen radical These substances have the of perfumes, having novel nuanc which were unknown hitherto, a used in'the preparation of odorif positions and perfumes or as it in the synthesis of scents and pec According to the process of inventi 6 n, the unsaturated ketoni are manufactured by reacting having the general formula: on C c (II) wherein R 1 and R 2 have the already given, with a hydrogen lPrice 3 s 6 d l & Co, phosphorus halide, condensing the resulting mpany, of substituted primary allyl halide with an le, Switzer-: alkali metal salt of an aceto-acetic-acid ester 35 rention, for and submitting the resulting substituted be granted aceto-acetic acid ester to a ketonic hydrolysis.

it is to be Alcohols which may be used as starting escribed in materials include, -for example, 3-methylpenten-( 1)<o 4-( 3), 3-phenyl buten-( 1)-ol-( 3), 40 o novel un 3,5-dimethyl-hexen-( 1)-ol-( 3) and 1 vinylr the manu cyclohexanol-( 1) For carrying out the first reaction step, it' provided by is preferred to use concentrated aqueous ich may be hydrogen halides-such as concentrated hydro 45 al formula: chloric or hydrobromic acid as sold commercially or phosphorus tribromide During the halogenation an allyl rearrangement takes place whereby the double bond migrates to the 2,3-position and the halogen' attaches 50 3 itself to the C 1 atom The reaction step involving concentrated aqueous hydrogen chloride or bromide is described and claimed radical co in patent specification No 735,828. radical conor a pheyl The second reaction step, in which the 55 or radh l substituted primary allyl halide is reacted thyl radical tamethlylene with an alkali-metal salt of an aceto-aceticotamethylene acid ester, is carried out by known methods, es of scent for example by adding to the halide an alkalind may be metal salt of an aceto-acetic acid ester in the 60 erous com presence of an inert solvent or by adding an :termediates alkali-meta L alcoholate to a mixture of the itrmedt-halide and aceto-acetic acid ester, the alkaliTumles -' the esent metal salt of the aceto-acetic ester then being es aforesaidformed in situ 65 an alcohol In the final reaction step, the substituted an -ac aceto-acetic acid esters are subjected to ketonic hydrolysis by known methods, e g. by treating the substituted aceto-acetic acid. ester with an alkali-metal hydroxide and 70 acidifying the resulting product (with heating if necessary). The invention will now be illustrated by the following examples: EXAMPLE 1 75 significance 600 g of 3-methyl-penten-( 1)-ol-( 3) were halide or a cooled to + 15 C with an ice bath, then Pm Y 1 e 1,800 ml of aqueous 37 % hydrochloric acid fication was accomplished by stirring at were poured into the reaction vessel The 40 o-50 C for 4 hours Concentrated mixture was stirred for 30 minutes The oil, hydrochloric acid was dropped into the recomprising essentially 1 chloro-3-methyl action mixture from a dropping funnel at pentene-( 2), was separated, washed three such a rate that no foaming (due to the 70 times with 500-mil of water and dried over evolution of carbon dioxide) occurred and calcium chloride until the mixture was strongly acid The oil 4,000 ml of benzene 1,040 g of ethyl layer was removed The aqueous layer was aceto-acetate and 378 g of sodium methylate diluted with 2,000 ml of water and extracted were stirred into a 12-litre flak 696 g of with 500 ml of benzene The benzene extract 75 1-chloro-3-methyl-pentene-( 2) were added to and the oil-layer were

combined, washed until the mixture from a dropping funnel within neutral and dried over calcium chloride. 2 hours at 60 C Stirffriig was thend con Upon fractionation there was obtained 5tinued at 60 Cfor 16 hours cyctohexylidene pentanone-( 2) distillingat The mixture was diluted with 4,000 ml 103 C /6 mm n D 25 = 1 4760 80 of water The oil was separated and the ben Instead of 2-cyclohexylidene-ethyl chloride, zene was distilled off in vacuo The thick 1 molecular equivalent of 2-cyclohexylideneresidue -comprising 3-carbethoxy-6-methyl ethyl bromide may be used in this example. octen-( 5)o 6 ne-( 2) was charged into a 5-litre: EXAMPLE 3. flask together with 2,000 ml of ethyl alcohol, 438 g of 3,5-dimethyl-hexen-(l)-ol-( 3) were 85 1,000 ml of water and 500 g of potassium stirred with 1,500 ml of concentrated aqueous hydroxide This mixture was stirred for 2 hydrochloric acid ( 37 % by weight concentrahours, then allowed:to stand for 16 hours, tin of hydrogen chloride) at ca 209 C for the potassium salt of 3-carboxy-6-methyl 30 minuties The -oil layer was separated, octen-( 5)-one-( 2) being thus formed washed twice; each time with 500 ml of 90 Concentrated hydrochloric acid was added water, and dried: over calcium -chloride In to the stirred reaction mixture from a drop this manner there was obtained 1-chloro-3,5ping funnel until the -mixture was strongly dimethyl-hexen-( 2), n D 25 = 1 448. acid The oil layer was removed, and the A 5-litre flask was charged with 3,000 ml. aqueous portion was extracted with 1,000 of benzene, 429 g of ethyl aceto-acetare and 95 ml of benzene The combined oils were 162 g of sodium methylate 428 g of 1washed with water and fractionated to yield chloro-3,5-dimethyl-hexene-( 2) were added at 6-methyl-octen-( 5)-one-( 2) -distilling at 65 60 within 30 minutes, and stirring was conC./10 mm fn D = 1 4412 This -compound had tinued for 6 hours, at 600-70 C The rean odour generally reminiscent-of citrus fruit action mixture was washed with 2,000 ml 100 Instead of ethyl -aceto-acetate, another of water and the benzene was distilled off aceto acetate, fof example methyl aceto at a reduced pressure of 100 mm Hg to yield acetate, may be used _ 3-carbethoxy-6,8-dimethyl nonen-( 5)-one-( 2) EXAMPLE 2 as a straw-coloured oil 445 g of 1-vinyl-cyclohexanol-( 1) was The entire quantity of 3-carbethoxy-6,8 105 stirred -for 1 -hour with-1,500 ml of 37 % dimethyl-nonen-( 5)-one-( 2) was dissolved in aqueous hydrochloric acid The oil was 2,000 ml of ethyl alcohol To the solution separated, washed twice with water, and there were' added 200 g of solid potassium dried over calcium chloride The 2-cycto hydroxide and 200 ml of water The mixture hexyiliden-ethyl chloride obtained had n D-= was stirred for 4 hours at 40 -50 C To 110 1.4994 the resulting solution of the potassium salt of 2-cyclohexylidene-ethyl bromide was

pre 3-carboxy-6,8-dimethyl-nonen ( 5) one-( 2) pared similarly by reacting 1-vinyl-cyclo there was then added concentrated aqueous hexanol-( 1) with 48 % aqueous hydrobromic hydrochloric acid ( 37 %) from a dropping acid at ca 20 C funnel:until the: solution was strongly acid115 A 54 itre flask was charged with 390 -g Thirty minutes were required for the addiof -ethyl aceto-acetate, 157 g of sodium tion The solution was then stirred for an methylate and two litres of benzene 414 g additional hour at 50 C. of 2-cyclohexylidene-ethyl chloride were The reaction nmixture was diluted with added at 40 C within 30 -minutes while 2,000 mln -of water and the oil-layer was 120 stirring-vigorously The reaction mixture was removed by means -of a separating funnel. stirred for 3 hours at 60 -70 C then for The aqueous portion was extracted with 500 2 hours -at reflux -temperature After cooling, ml of benzene The combined oils were the-reaction mixture was washed twice-each washed with water until finutral and then time with 2,000 ml of water The -benzene' fractionated In this manner there was ob 125 was distilled in -vacuo The residual light tained 6,8 -dimethyl-nonen-( 5)>one-( 2) disbrown syrup was dissolved in 2,000 ml of tilling at 120 C /35 uinn, N 25 = 1 4432 It ethyl alcohol The-solution was charged into had a pleasant fruity odour reminiscent of a flask together with -200 g -of -potassium fresh apple juice The 2; 4-dinitro-phenyl hydroxide and -50 Q ml; of water The sappni hydrazine derivative melted at 47 C where 130 785,086 wherein R 1 and R 2 have the values given in claim 1, with a hydrogen halide or phosphorus halide, condensing the resulting substituted primary allyl halide with an alkali-metal salt of an aceto-acetic ester and submitting the resulting substituted aceto-acetic acid ester to a ketonic hydrolysis. 6) A process in accordance with claim 5, wherein 3-methyl-penten-( 1)-ol-( 3) is used as the alcohol. 7) A process in accordance with claim 5, wherein 1-vinyl-cyclohexanol-( 1) is used as the alcohol. 8) A process in accordance with claim 5, wherein 3,5-dimethyl-hexen-( 1)-ol-( 3) is used as the alcohol. 9) A process as claimed in claim 5, in which concentrated aqueous hydrochloric or hydrobromic acid is used as halogenating agent. 10) A process for the manufacture of the substances of the formula set forth in claim 1 herein, substantially as described with reference to the examples given. W D WHITAKER, Patent Agent, For F HOFFMANN-LA ROCHE & CO, Aktiengesellschaft. as the semicarbazone derivative melted at 1140 C.

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* GB785087 (A)

Description: GB785087 (A) ? 1957-10-23

Magnetic amplifier modulator

Description of GB785087 (A)

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PATENT SPECIFICATION ; 785,087 Date of Application and filing'Complete Specification: Sept 13, 1955. No 26212/55. Application made in United States of America on Sept, 30, 1954 Complete Specification Published: Oct 23, 1957. Index at Acceptance:-Class 40 ( 4), F 9 J. International Classification:-H 03 f COMPLETE SPECIFICATION Magnetic Amplifier Modulator.

We, BENDIX AVIATION CORPORATION, a corporation of the State of Delaware, United States of America, of Fisher Building, Detroit, Michigan, United States of America, do hereby declare the invention, for which we pray that a patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement: - This invention relates to magnetic amplifiers and more particularly to -a magnetic amplifier modulator: In aviation Instrument Landing Systems, the ILS receiver carried in aircraft has a localizer channel and a:guide-path channel. The electrical output of all receivers used in ILS and omnirange equipment is-a reversible polarity direct current In order to make this information usable in automatic pilot systems, the aforementioned direct current output from the receivers must be converted into proportional carrier frequency voltage 'The present invention provides a magnetic amplifier which is usable in Instrument Landing Systems and other systems and apparatus where amplification and, control-is required According to the invention there is provided a magnetic amplifier having two -magnetic cores, each core having a primary winding connected to an a-c excitation source and a -secondary winding so arranged that the a-c voltages induced in the latter from the former are balanced to produce a substantially zero output voltage in the secondary windings, an output load connected to said secondary windings, and means for applying an input signal directly to said secondary windinligs to vary the flux in said cores so as to produce a differential output in the load The invention will now be described by way o f example with reference to the accompanying drawings, in which: -Fig 1 is a schematic diagram of the modulator. Fig 2 is a perspective view showing the lPrice 3 s 6 d l mechanical arrangement of the windings relative toga pair of cores. Referring to' the drawings and more particularly'to Fig 1, there is shown a modulator having -a balance winding 21, a: two-part 50 excitation winding 22, a two-part bias winding 23, and a control winding, 24. The device has two toroidal cores of high permeability magnetic material Each core has a separate exqitation winding portion and a 55 separate bias winding portion, with a b alance winding and a control-winding being wound around both- of the cores with the individual cores being of the tape wound type. The balance winding 21, wound around both 60 cores I and II, has a balance winding circuit which includes a source of direct current potential 25, which is 'serially connected with a balancing resistor 26 of the variable type, and the balance winding 21, via conductors 41 to 65 43 :The bias winding 23 is serially connected with a source of

direct current 25, which source is serially connected with the two portions of the bias winding wound on cores I and II, and 70 a dropping resistor 27, to provide a bias wind ing circuit The two coils of the bias winding 23 are connected in series opposition, as in, dicated by the dots -on the drawings adjacent their respective components, in a conventional 75 dot system, to indicate the start and finish of the windings An excitation winding circuit includes the two portions of the excitation winding 22 positioned; respectively, on cores I and II of the 80 modulator The excitation windings are connected'in series opposition with each other, and in series with a dropping resistor 28, to terminals 29 and 30 for connection to a source of alternating cu'rrent'excitation 31 85 The control winding 24, wound on both cores 1 and II, is connected to output terminals 32 and 33, which are in turn connected, via capacitor 40, to the primary 34 of a {ransformer Tl,'vhich is a coupling transformer 90 IS 2 t 7807 = v 4 $on-r ',; '' A secondary 35 of the transformer T 1 is shown produce a null in the device This is desirable ;"' erlalil' '0 iffcted to a load resistor 36, and because, for a zero signal input, ordinarily l having '-'a ixed tuning capacitor 37, connected there is not a resultant zero outpi Ltsignrl due across said load Input terminals 38 and 39 to manufacturing tolerances>, such "as core are connectable fto' -a signal -v 6 o Ithge F; which pernmieability, 'winding turn -countsy and ' -dis 70 terminals are, while -being in shunt with tributed capacitance capacitor 40, also serially connected with the Therefore, the balance winding:21 provides. control winding -24 ' and -ihe: primary i inding -a means for' nulling the miodultor by m-eansof' 34 of transformer T 1, a very low balancing current ctThe alutie of At a "no signal" condition, 'boih of the resistor 26, which is shown as being; variable, 75 excitation windings on cores I and II have may be a fixed resistor which is'selected'; at the some impedance when the coils are connected signal tested predetermined value of the to a constant current source of excitation of a modulatorto p-roduce the desired low null In predetermined frequency, for example, 400 effect, this low null current unbalances the cycles The control winding 24 is magnetically modulator in a direction opposite to that 80 coupled to both portions of thet excitation cased-by the manufacturing tolerances. winding, since the control winding 24 is wound The resistor 27 adjusts the bias current to around both cores I and II I Hgwever,-there ii ksoiileopredeternined value depending upon the no magnetic coupling between the cores I and defined sensitivity The resistor 28 sets the II per: se The excitationy)vndings on,,cores,I alternating current' excitation to-'some pre 85 and II both induce-voltages:in the control determined value ' winding:24, -but since the voltages are,of equal '

In Fig, 2, the perspective-schematic shows magnitude and of opposite polarity, they, can two discrete cores, with core'I and core II each ' cel outs and:zero voltage appears across the having a bias winding' 23 and an excitation control winding 24: Wdinnding 22, and with th -conitrol and balance 90 The bias windings of 'cores:I aind II are con windings -being-woiund about both cores I and tiected to -the' source 25: of direct current II; While the cores are mechanically distinct potential,:'-f 6 i:magnetizing the cores near and there is no magnetic coupling theresaturation: and thereby preventing hysteresis between, -it is pointed out that the'balance and The directcurrent bias of each coil'sets up a control windings each are'disposed to embrace 95 direct cutrenit flux,'in: its respective core, -with both cores I and II. the:-,flux sources being-equal and opposite -' - While the circuit of Fig; 1 Shows a bias At the "'signal" condition, the signal Es, winding -in ordef that the output frequency which is a direct curfrent voltage, ptovides the will not be doubled by passing through the signal icurreiit in'the control winding 24 ' All 'of coupling -transformer, it -is' to be understood o 100 the direct -current of ithe signal fiows through that the -balance or'null setting winding may -the control winding 24 and the primary 34-of be used in a magnetic amplifier without a bias the trainsformer T 1, since no direct cui'rent'cafi winding for the purposes s&t forth herein The flbw-through the capacitor 40 Capacitor 40 'is balance winding circuit, under this latter condiof large value and, consequently, represents an tion of absence of bias winding; will produce 105 alternating-current short -cieuit so that any the desired null The balance winding circuit alternating current v Oltage 'appearing across may -be used in any magnetic amplifier or cornthe ' control' winding 24 ' will appear un parable saturable reactor circuit to offset the attenuated across the primary winiding 34 of undesirable effects resulting from manufacturT 1 With a giiven polarity, as 'shown by the plus ing tolerances or coil mismatch in general 110 (+. and minus (-) signs on the drawings, the ' Fromfi the'foregoing, it will be seen that the signal current'sets up a' direct -current flux in output will be a 'carrier' frequency whose both-cores I and II This flux produced by the amplitude is proportional to the:amrnplitude of signal current is'in one 'direction;, as shown -by the direct current input signal. the arrowv X, and therefore opposes'the balaicewinding circuitprovides a null 115 flux in one core, as shown by the arrow Y; and setting means which eliminates a mechanical aids the bias fluxl 'in the other-core, as shown adjustment or a precise matching operation of by the arfdw-Z -'" '':' "-' the magnetic amplifier components, and the The core 'in whihi the-fluxes aid becoines device inherently produces a minimum elecmore saturated' and the impedance of that'pari trical

output N the null orno-sigral condition 120 ticular core's wiinding (co il) goes down The determined by the value of the resistor ascercore in vwhich the fluxes/oppose becomes less tained by test'

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