* GB785028 (A)

Description: GB785028 (A) ? 1957-10-23

Plant growth regulant compositions

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PA NT $PIECWIFCATION Date of Application and filing Complete Specification April 23, 1954. R-R No 11827154. Application made in France on April 24, 1953. ____ gt D Complete Specification Published Oct 23, 1957. Index at Acceptance:-Classes 81 ( 1), El C(l A: 3 A 1: 4 A 2: 4 A 3: 5 D: 6); and 111, B 3 (C 2: F 1: F 2). International Classification: -A 611 CO 5 d, f. COMPLETE SPECIFICATION Plant Growth Regulant Compositions We, AMERICAN CHEMICAL PAINT COMPANY, a corporation organised and existing under the laws of the State of Delaware, United States of America, of Broolkside Avenue, Ambler, Pennsylvania, 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 plant growth regulant compositions which include an auxine and a component for enhancing the activity thereof. It is known that the auxines promote the formation of roots and they are therefore used to improve the propagation of plants by cutting Under other circumstances, they contribute to the setting of the fruits or favour their growing bigger without prematurely falling down

However, they disturb the normal activity and may cause the death of the vegetables treated if the species under consideration are sensitive and the auxines are capable of remaining for a long time in the vegetable organism without being detroyed by the ferments; they are thus of value in the selective or total destruction of weeds. Many processes have been proposed for increasing the activity of auxines They may be divided into three groups: (a) A mixture of several auxines or a mixture of auxines and bodies similar to auxines in their chemical structure are employed The mixture will often exert a greater synergistic action than a single auxine. (b) The solvents or vehicles that convey the auxines to the tissue of the vegetable are selected so as to increase the speed of penetration of the active substance. (c) Non-auxinic substances such as nitrated phenols which are capable by themselves of destroying plants, are added in order that their effect be added to that of the auxines. According to this invention there are provided plant growth regulant compositions comprising, in a liquid solvent medium, an auxine and, as oligo-element additive, at most mg/litre of a compound of boron cobalt, zinc or molybdenum and/or at most 500 mg/ litre of a compound of rhubidium The action of auxines is exerted only on tissues that are already active, that is to say capable of respiration, nutritive exchanges and often of cellular proliferation and, more generally speaking, it is all the greater as the tissues are more active at the time of the action of the auxines. The substances contemplated by this invention as additives are in the group of oligoelements Very small amounts of the latter increase the vitality of the vegetative points and stimulate some or all of the physiological functions of the vegetables. The compositions of the invention are normally applied by spraying on the vegetable growth They are of particular value in the destruction of grass. The following examples will serve to illustrate the invention but are not to be regarded as limiting it in any way:Ex AMPLE I An aqueous solution of a zinc salt such as chloride or nitrate ( 1 to 100 mg/l) is mixed with an equal volume of an aqueous solution of the sodium salt of naphthalene-acetic acid (an auxin) ( 50 mg/l). Instead of employing an aqueous solution of the auxin emulsions may be prepared consisting of the solution of zinc salt and a solution of an auxin in oil Suitable auxines are the methyl and ethyl esters of naphthaleneacetic acid or of naphthoxyacetic or propionic acid, or the ethyl ester or butyl ethylene glycol ester, or any other ester of 2 4-dichlorophenoxyacetic acid or 2 4-5 trichlorophenoxyacetic or propionic acid The concentration of auxine in the emulsion may be

reduced by to 'S by the addition of the zinc salt solution The compositions exert a grass-destroying action. EXAMPLE II Molybdenum salt solutions may be employed instead of the zinc salt solutions of Example I, in concentrations of 1 to 10 mg/l. The molybdenum may be present either in Irrico 3 s 6 dtl-,7 _ ;_ ^, _ j 785,028 the cation of the salt (for instance in the form of molybdenum nitrate), or in the anion of the salt (for instance in the form of ammonium molybdate) In the latter form, it may also be used as an organic compound, as ester in alcohol, and thus have the appearance of a liposoluble substance It is then possible to mix it directly in an oil solution with a liposoluble auxine from the group of esters recited in Example I the weight ratio of auxin to molybdenum being from 1:5 to 1:20 The mixture will then emulsify as if it were auxine alone and makes it possible to use that emulsion of auxine for its various applications with the same efficiency but in smaller quantities, e.g from one half to two thirds the quantity. EXAMPLE III Boron compounds may also be used and make it possible to reduce by 3 to 4 the amount of auxine necessary for a similar effect without the boron, more particularly in selective grass-destruction Borax, sodium borate and free boric acid are the least expensive and the most simple water-soluble forms that may be used But one may also employ in order to facilitate the penetration through the waxy cuticles of the plants, an organic borate such as: ethyl borate, propyl borate, butyl borate, or amyl borate which are then completely soluble in the oils used as vehicles of the liposoluble auxines such as the esters of the 24-D, and 2 4-5 T compounds The ratio of boron to auxine may vary widely: an amount of boron equal to i/20 of the weight of auxine produces a very useful activity; boron 20 times by weight of the auxine produces a greater action but is not proportionate to the increase of the amount of boron It results therefrom that according to the agronomic conditions and the respective costs of the products, it may be advantageous to use, with respect to the auxine which it is desired to reinforce, small or high relative proportions of boron. EXAMPLE r V Rubidium compounds may also be employed in the compositions of this invention In the production of such compositions a solution of a soluble salt of rubidium in a concentration of 1 to 500 mg/I is mixed with a solution of an auxin as described in Example I Due to this addition an economy in the amount of auxine to be used to obtain the same result, which may reach a reduction by 4 to 4 of the weight of auxin is achieved. EXAMPLE V

An important reinforcement of the grassdestroying action of the soluble salts of the 2.4 dichlorophenoxyacetic acid is obtained by adding to the liquid to be sprayed amounts of 60 zinc nitrate and a boron compound each between 20 and 200 mg per litre.

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* GB785029 (A)

Description: GB785029 (A) ? 1957-10-23

Improvements in and relating to a laminated material having a wood basis

Description of GB785029 (A)

A high quality text as facsimile in your desired language may be available amongst the following family members:

CH309278 (A) FR1106796 (A) CH309278 (A) FR1106796 (A) less Translate this text into Tooltip

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PATENT SPECIFICATION 785,029 Date of Application and filing Complete Specification: June 15, 1954. No 17522/54.

Application made in Switzerland on June 19, 1953. Complete Specification Published: Oct 23, 1957. Index at acceptance:-Class 140, A( 2 G: 2 H: 5 G 10: 11 KI: 12: 13). International Classifica tion:-B 29 d. COMPLETE SPECIFICATION Improvements in and relating to a Laminated Material having a Wood Basis I, MARCEL FRACHEBOUD, of Arcachon, Gironde, France, a citizen of Switzerland, do hereby declare the invention, for which I pray that a patent may be granted to me, and the method by which it is to be performed, to be particularly described in and, by the following statement: - My invention relates to a novel material adapted to be useed more particularly for the manufacture of packages, and 'which is made of a thin layer of wood veneered on both sides by a thin, sheet of paper, the novelty being that said sheet is, of temporarily waterproof paper, preferably of the glassine type. According to a further feature of this new material the wood layer is moistenable through the paper layers. Still a further feature is that said novel material is thin enough to be capable of being creased and folded without damage when moist and of remaining so creased, or folded once dried. In, a prior publication it has already been proposed to manufacture a light and strong flexible laminated plate made of a single sheet of wood veneer covered on each side with one or more layers of paper, pasteboard or other insulating materials such as paper pulp, oy coating the layersl with glue and uniting them under light pressure insufficient to destroy their normal porosity in a drying atmosphere at approximately 100 C An extraordinarily light and flexible dry plate is said to be thus obtained For packaging purposes it has already been proposed to use packing boxes and, the like manufactures by utilising sheets of cut and unrolled wood upon one or both faces of which thin paper of suitable quality is' stuck, said sheets of wood being channelled or corrugated after sticking; said corrugated material made of unrolled wood veneered with paper may also be employed instead of the usual corrugated paper or cardboard for the manufacture lPrice 3 s 6 d l of packages of all kinds However in this prior proposition the product used for the manufacture of packing boxes is said to be not in any way affected by moisture. I have illustrated by way of example, in the accompanying drawings, a preferred embodiment of my invention In the said drawings: Figure 1 is a plan view, and Figure 2 is a sectional view on a larger scale through line II-II of Figure 1. The piece of material illustrated includes a thin rectangular sheet of wood 1 over the two surfaces of which is glued, a transparent sheet of

waterproofed paper 2, of the glassine type, as used in particular by butchers and by florists This paper resists tearing stresses even when thin and is impervious for some time, i e it remains dry when in contact with water or is in a moist atmosphere during a relatively short time but becomes moist after a somewhat 'extended lapse of time This paper is glued under high pressure by means pf an adhesive having for its main component a synthetic resin and which is not liable to become soft under the action of water, once it has set. The material thus produced becomes supple in the presence of water or of moisture, but is not damaged thereby and its components cannot separate; its resistance returns to its original value as soon as the material has been dried; when said material is moist, it can easily be cut, folded and creased and thus formed into packages for the manufacture of which it is chiefly suitable, in particular light cigar-boxes and small containers for the transportation land sale of fruit and vegetables The packages made of the material described hereinabove offer a higher mechanical resistance to deformation and surface wear than any similar article made 'of untreated woods, having the same thickness.

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* GB785030 (A)

Description: GB785030 (A) ? 1957-10-23

Process for the production of sulphinyl ethyl thiophosphates

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PATENT SPECIFICATION Inventors: DENNIS FREDERICK HEATH and DAVID WILLIAM JOHN LANE Date of filing Complete Specification: July 7, 1955. Application Date: July 12, 1954. No 20349/54. Complete Specification Published: Oct 23, 1957. Index at acceptance:-Class 2 ( 3), C 1 l(A 15: B 6: B 24), C 3 Xo International Classification:-C 07 f. COMPLETE SPECIFICATION Process' for the Production of Sulphinyl Ethyl Thiophosphates We, F Is ONS PEST CONTROL LIMITED, formerly Pest Control Limited, a British Company, of Cambridge Road, Felixstowe, Suffolk, formerly of Bourn, Cambridgeshire, 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 the manufacture of sulphinyl compounds of the general formula: (RO)(R'O)P(O)SC O HS(O)R 1 ' where R, R' and R' are each an alkyl group containing not more than four carbon atoms. These compounds are described and claimed in our prior Specification No 742,796. The present invention provides a process for the production of sulphinyl compounds of the formula: (RO)(R'O)P(O)SCH 45 (O)R'1 where R, R' and R are each an alkyl group containing not more than four carbon atoms which consists in reacting a salt of a compound of the general formula: (RO)(RO 10)P(O)SH, where R and R' have the above-defined meaning, with a compound of the general formula: XCQH 4 S(O)R", where R has the abovedefined meaning and X is a halogen atom, for example a chlorine, bromine or iodine atom, preferably in approximately equimolecular proportions, with or without the presence of a solvent and, if desired, isolating the desired product from the reaction mixture. The process of the invention represents a valuable process whereby the desired product may be obtained in good yield Preferably the salt employed is a compound of the general formula: (RO)(R'O)P(O)SM, where M is an alkali metal atom The process of the invention will be further described below with reference to the use of such a salt.

Solvents useful in the process are, for example, lower aliphatic alcohols and lower lPrice 3 s 6 d l aliphatic ketones Ethyl alcohol has been found to be particularly suitable for use as the solvent in this reaction The thiophosphoric acid reactant may be made in manner known per se by reacting thiophosphoryl chloride PS Cl, with a single alcohol ROH (where R and R' in the general formula are the same) or with two alcohols ROH and ROHI (where R and R' are different), so as to replace two of the chlorine atoms of the PS Cl, by RO and R 10 O-, and then replacing the third chlorine atom by reaction with an alkali metal hydroxide MOH It will be appreciated that the compound thus obtained constitutes an equilibrium of the two tautomeric forms. 0 11 (ROX(R 1 O)PSM and S Il (RO)(RIO)POM (R and R' being either the same or different), which could be more properly expressed by the formula: i+ The 1-halo-2-alkylsulphinyl ethane reactant may be made from the corresponding haloalkylmercapto ethane by oxidation with hydrogen peroxide under mild conditions and at moderate temperatures. The halo-allkylsulphinyl ethane and the thiophosphoric acid reactant react to form a tautomeric mixture of two compounds having the 0 =J S and the p, c 785,030 L lw 6 ', L 0 RO)'O)P S structure respectively, with the former predominating This mixture may, for insecticidal purposes, frequently be used as such, especially as the biologically more active tautomer of the first-mentioned structure is present in higher proportion However, separation of the two tautomers is possible, for example by making use of the considerable difference in their partition ratio between hydrocarbon and water. The thiophosphoric acid reactant may comprise for example OO'-diethyl thiophosphoric acid, OO-dimethyl thiophosphoric acid, Omethyl-01-ethyl thiophosphoric acid, OO-dinormal-propyl thiophosphoric acid and OO'di-iso-propyl thiophosphoric acid The salt of the thiophosphoric acid which is used is most suitably an alkali metal salt, and preferably the sodium salt The 1-halo-2-alkylsulphinyl ethane reactant employed may comprise for example 1-bromo-2-ethylsulphinyl ethane, 1chloro-2-ethylsulphinyl ethane, 1-bromo-2methylsulphinyl ethane, 1-bromo-2-isopropylsulphinyl ethane and 1-bromo-2-normalbutylsulphinyl ethane. In carrying out the reaction according to the present invention it has been found desirable to use a reaction temperature slightly elevated above room temperature, and it is preferred to carry out the reaction at a temperature of the order of 70 -80 C It is to be noted however that temperatures above and below this indicated range may also be used. When using temperatures of the order of 70 -800 C it has been found suitable to use a reaction time of the order of about 2-3 hours.

When using higher temperatures shorter reaction times should preferably be used and when using lower temperatures longer reaction times should preferably be used. The following example is given to illustrate the process of the present invention: EXAMPLE: Preparation of OO 1-diethyl-S-ethylsulphinylethyl thiophosphate: (C H 50)OP(O)SCGH 4 S(O)CGH,. A Preparation of 001-diethyl thiophosphoric acid sodium salt: (C 1 HO)2 P(O)S Na. (Co H,0)PSG 1 was prepared in known manner from PSCI, containing radio-active phosphorus This was run into aqueous sodium hydroxide (about 2 molecules) of sodium hydroxide per molecule of starting material). Water was removed under vacuum, sodium chloride precipitated with absolute alcohol and removed by filtration, the alcohol removed by suction, a little benzene added and the suction continued The salt was thus obtained dry. B Preparation of 1-bromo-2-ethylsulphinyl ethane: Br C O H 4 S(O)C H,. millilitres of 100 volume hydrogen peroxide were added dropwise to 56 grams Br C 2 HSCQH, in 100 millilitres acetone The temperature was maintained at 20 to 30 C. The addition of H O O caused turbidity; consequently it was added at such a rate that the reaction mixture remained just opalescent The reaction took several hours. The product was then evaporated under vacuum, the resulting syrup was taken up in millilitres of water and extracted with 150 millilitres of chloroform The chloroform was removed by high vacuum at a flask temperature not exceeding 40 C. The product was a gum which solidified on cooling It was purified by dissolving in ether and precipitating with petroleum ether (below C fraction) as deliquescent white crystals. C Final Product. To 10 grams sodium salt from A were added 9 6 grams Br CGHSOC 2 H from B in millilitres absolute alcohol, the mixture refluxed 2 hours and the alcohol removed under vacuum Benzene was added and suction again applied to remove the last traces of alcohol, the product taken up in chloroform, washed with water and the chloroform removed by suction. The product contained phosphorus equivalent to 72 % of the phosphorus introduced as _ O (C 2 H 50)Ps S Ta (both estimated as P) A fraction was subjected to partition chromatography, when 80 % of the product was found to be identical with the product of mild oxidation of (C 2 H, O)2 P(O)S Co HSSCH,. The remainder was more oil-soluble and is believed to be (CHO)2

P(S)OGCH,S(O)CH 5. Physical Properties of the Main Product: Partition ratios: Water/trichloroethylene Water/Benzene = 2.25 + O 05 at 18 C in very dilute solution. = 5.82 + O 10 at 18 C in very dilute solution. Hydrolysis constant: determined in 0 01 Normal Na OH= 3 34 + O 06 (OH-) per minute at 25 4 C. 785,030 For comparison the constants of the oxidation product of (C 2 H 50)2 P(O)SC 2 H 4 SC 2 H 5 are given here: Partition ratios: Water/trichloroethylene = 2 19 + 0 05 at 18 C in very dilute solution. Water/Benzene = 5 83 + O 2 at 18 C in very dilute solution. Hydrolysis constant: determined in 0 01 Normal Na OH= 3 31 + 0 07 (OH-) per minute at 25 4 C. The compounds are plainly identical. The process indicated in the above example may be repeated replacing the reactants employed above by OO'-dimethyl thiophosphoric acid sodium salt and 1-bromo-2-methyl sulphinyl ethane to produce OO-dimethyl-Smethylsulphinyl-ethyl-thiophosphate; or by Omethyl-O 1-ethyl thiophosphoric acid sodium salt and 1-bromo-2-normal-propyl sulphinyl ethane to produce O-methyl-O 1-ethyl-Snormal-propylsulphinyl-ethyl thiophosphate; or by OO-diethyl thiophosphoric acid sodium salt and 1-bromo-2-iso-propyl sulphinyl ethane to produce OOL-diethyl-S-iso-propylsulphinyl-ethylthiophosphate.

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* GB785031 (A)

Description: GB785031 (A) ? 1957-10-23

Improvements in or relating to radio-receiving circuits comprising means forautomatic gain control

Description of GB785031 (A)

PATENT SPECIFICATION 785,03 1 Date of Application and filing Complete Specification: July 12, 1954. No 20384/54. Application made in Netherlands on July 10, 1953. Ha __ Complete Specification Published: Oct 23, 1957. Index at acceptance:-Class 40 ( 5), Q 4 (A 1: D 7: D 9). International Classification:-H 04 h. COMPLETE SPECIFICATION Improvements in or relating to Radio-Receiving Circuits comprising means' for Automatic Gain Control We, PHILIPS ELECTRICAL INDUSTRIES LIMITED, of Spencer House, South Place, Finsbury, London, E C 2, a British Company, 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 radio-receiving circuits comprising means for deriving a regula;ting voltage from the modulated' intermediate-frequency or high-frequency signal voltage, which regulating voltage is applied to the grids of one or more amplifying tubes of the circuit so as to compensate for variations of the input signal amplitude which result from random conditions For such automatic gain control use is generally made of a rectifier, usually a diode, to whose circuit the modulated signal voltage is supplied after amplification, which circuit moreover comprises a source supplying a so-called threshold voltage This threshold voltage results in that the rectifier does not become conductive until the amplitude of the signal voltage supplied to the circuit exceeds a given value, so that the automatic gain control does not become operative until the signal voltage attains this value. The present invention has for its object to provide an improved circuit of this type adapted to secure very effective control so that the regulating voltage increases rapidly in absolute value with an increase in signal voltage from a given value of the signal voltage onwards. It has been suggested to amplify the regulating voltage prior to applying it to the grids of the tubes This consequently necessitates

the use of a direct voltage amplifier which, as is known, entails difficulties Therefore, the direct voltage amplifier is omitted in the receiving circuit according to the invention. A further object of the invention is to provide an improved circuit capable of providing so-called silent tuning in a very simple manner, that is to say that the receiver is inoperalPrice 3 s 6 d l tive until the signal amplitude attains a given value. According to the invention, a radio-receiving circuit comprising means for deriving an automatic gain control voltage from an intermediate-frequency or high-frequency signal voltage, which voltage is applied to the grids of one or more amplifying tubes of the circuit so as to compensate for variations of the input signal amplitude which result from random conditions, said means comprising a rectifier to which the signal voltage is supplied and, in which a delay voltage is operative so that the rectifier does not operate until the amplitude of the signal voltage exceeds a given value is characterized in that the delay voltage is at least for the greater part supplied by a glow discharge tube connrmected in series with a resistor across the high-tension supply terminals. In known circuits, the threshold voltage is, in general, only a few volts, for example volts or less, so that it can be surpassed by the signal voltage without additional amplification of the signal The use of a much higher threshold voltage yields a better control and further advantages referred to hereinafter. When using the invention it will, in general, be necessary to employ an additional amplifying tube for the signal voltage in order to secure such, a signa;l amplitude in the regulating voltage circuit that it exceeds the threshold voltage even in the case of a small input signal. The threshold voltage is preferably 80 V or higher The glow discharge tube may be a neon tube whereof the glow discharge voltage, which is substantially independent of the current passing through the tube, is 85 V This consequently yields a threshold voltage which does not substantially change in the case of supply voltage variations. Where an intermediate-frequency output transformer is used, the high amplification of the modulated signal permits the signal voltage, from which is derived the modula2 785,031 tion voltage to be reproduced, to be taken from so small a portion of said output transformer as to permit in a simple manner direct matching of different loads As will be set out hereinafter, it is possible to use in a simple manner so-called gradient limitation, that is to say limitation of steep output voltage peaks. In order that the invention may be readily carried into effect, an embodiment thereof will now be described, by way of example, with

reference to the accompanying draving which represents diagrammatically a circuit arrangement for radio receivers. The Figure shows the wiring diagram of a I 5 superheterodyne receiver: the reference numeral 1 denotes a band-pass filter tuned to the intermediate-frequency carrier wave, to the primary circuit of which the amplified intermediate frequency signal is applied The secondary circuit is connected between the control grid and the cathode of an intermediatefrequency amplifying pentode 2 The anode circuit thereof comprises an intermediatefrequency band-pass filter comprising circuits 3 and 4 which are also tuned to the intermediate-frequency carrier The direct voltage for automatic gain control is derived from the circuit 3 and the modulation voltage from the circuit 4. The latter is effected by means of a diode which is connected to a tapping on the inductance of the circuit 4 and whose anode is connected, to earth Connected between one end of the circuit 4 and earth is the parallelcombination 6 of a resistor and a capacitor, the latter having such a value as to constitute a small capacitative reactance with respect to the intermediate-frequency oscillations. The low-frequency signals appearing across the parallel combination 6 are supplied by way of a capacitor 17 and a diode 7, which is conducting during normal reception to one of the output terminals 8, the other terminal 8 being earthed In a manner set out hereinafter, the diode 7 serves to suppress the reception if the amplitude of the incoming signal is too small to permit satisfactory reception. The circuit for deriving a regulating voltage comprises a diode 9 with which a resistor is connected in parallel A glow discharge tube 23 is connected between said parallelcombination and earth, a resistor 12 being connected to the positive terminal of the supply The glow discharge tube 23 and the resistor 12 are so selected that a voltage of approximately 80 V is maintained across the tube 23 In the case of a supply voltage of 250 V ithe resistor 12 may be 80 k Ohms The supply of 250 V also feeds the anode of the pentode 2 The intermediate-frequency signal is supplied from the circuit 3 through a capacitor to the anode of the diode 9 This anode is further connected, by way of the seriescombination of nvo resistors 13 and 14 of high value, to the anode of a third diode 15, whereof the cathode is connected to a point whose voltage is slightly negative with respect to earth The voltage for the automatic gain control of the preceding tubes is taken, through 70 a resistor 16, from the anode of the diode 15. A number of capacitors serve to eliminate the intermediate-frequency voltage components from the control voltage The voltage across the tube 23 constitutes a high threshold volt 75 age for the automatic gain control circuit.

The circuit arrangement so far described operates as follows: The incoming signal to the receiver is passed through frequency-changing and amplifying 80 stages so that an output signal at intermediatefrequency appears across the circuit 3 Now it will be appreciated that between the cathode of diode 9 and the anode of diode 15 appears a potential difference which is equal 85 to voltage Vd across tube 23 plus the voltage Vg between the cathode of diode 15 and earth Further, the anode of diode 15 is approximately at the same potential as its cathode, and between the cathode of diode 9 90 and the anode of diode 15 is a potential divider comprising, in series, resistors 10, 13 and 14; thus a delay voltage is produced across diode 9, this delay voltage being provided by the potential drop axross resistor 10 95 The diode 9 will conduct when the peak signal voltage exceeds the delay voltage appearing across the resistor 10 and; the anode of the diode 9 will become less and less positive as the signal level increases The voltage 100 at the anode of diode 15 will, however. remain clamped by this diode at approximately the potential -Vg, until the potential of the anode of diode 9 falls to the same value: for this to occur the peak voltage of 105 the intermediate-frequency signal applied to the diode 9 must exceed (Vd + Vg) volts and the diode 15 is cut off beyond this point. The effect of the automatic gain control is 110 determined by the ratio between the total threshold amplitude and the total voltage in the regulating circuit required to make the receiver fully inoperative Denoting by Vc this required negative bias of the grids of the preceding 115 tubes concerned, the ratio between the output voltage of the rectifier at the instant at which the regulation commences and the output voltage at which the receiver is substantially inoperative is Vd + Vg: Vd l Vg Vc If 120 Vd= 85 V, Vg= 2 V, and Vc= 10 V the ratio is 87:97 which may be deemed satisfactory. By contrast, in known circuit arrangements using automatic gain control with a threshold 125 voltage, this voltage is of the order of say, 6 Volts, the corresponding ratio consequently being 6 + 2: 6 + 2 10 = 8:18, that is to say a much smaller and less advantageous value of the ratio between 130 785,031 supply The resistors 19 and 20 are such that the anode of the diode 7 is negative with respect to the cathode, so that this diode is cut off and the connection between the unearthed output terminal 8 and the circuit 6 is 70 interrupted In this case, consequently, no output signal voltage appears across the terminals 8 Let it be supposed, for example, that the voltage on the anodes of tubes 7, 18 in the absence of a signal is 100 Volts with a supply 75 voltage of 250 Volts The resistors 20 and 19 then may have values of, say, 100 and 180 k Ohms respectively to obtain the setting

referred to. When the voltage at the control grid of the 80 triode 18 goes negative, the current through this triode decreases and the voltage on the anodes of the tubes 7 and 18 increases At a given signal voltage the anode of the diode 7 becomes positive with regard to its cathode, 85 so that the diode passes the signal voltage appearing across the circuit 6 and a low frequency output voltage is set up across the terminals 8. As long as the intermediate-frequency peak 90 voltage across the diode 9 is smaller than or equal to Vd, the junction of resistors 13 and 14 is at a positive potential relative to earth. However, the grid of triode 18 takes current and consequently attains earth potential If the P 5 intermediate-frequency peak voltage across the diode 9 is greater than Vd but less than (Vd +Vg), the automatic gain control is not yet active but the grid of the triode 18 is negative and the circuit operates as described 100 in the preceding paragraph The circuit arrangement for silent tuning is preferably so adjusted that the receiver is made fully operative instead of being fully inoperative upon said variation of the grid voltage of the triode 105 18 This is easily obtained with the use of a normal triode. The circuit arrangement described has the advantage that a small regulating voltage which does not appreciably affect the preced 110 ing tubes will nevertheless suffice to render the receiver operative. The circuit arrangement shown in the Figure permits a part of the voltage set up across the glow-discharge tube to be used as 115 a threshold voltage This is possible by means of a potentiometer. Since the amplification is greatly increased and a high signal voltage occurs across the circuit 4, the tapping point on the coil of 120 said circuit, to which the cathode of the detector 5 is connected, may be near earth. Adequate matching is then secured even 'at low output resistance values of the circuit 6. This resistance may be of the order of several 125 thousands of Ohms In this case effective gradient-limitation, that is to say suppression of sharp voltage peaks, is obtainable without employing any further amplifier stages. In the circuit arrangement shown, the diode 130 the signal voltage at which the threshold is surpassed and the signal voltage at which the receiver is substantially inoperative With the known receiver circuits better results are, of course, obtainable when employing a direct voltage amplifier for the regulating voltage, as is customary in many sets This, however, entails several disadvantages such as, for example, instability and the necessity of using a negative supply voltage of approximately 150 V for amplifying the regulating voltage.

As shown in the Figure, the voltage Vg is preferably adjustable and can readily be derived from the filament voltage supply by rectification. The circuit arrangement so far described permits so-called silent tuning to be achieved in a simple manner To this end a voltage is derived from the regulating circuit, which voltage is applied to the control grid of a triode 18 Said voltage is taken from a point which is driven negative at comparatively small signal amplitudes with an increasing signal In the circuit arrangement shown in the drawing, the common point of the resistors 13 and 14 is used therefor The triode 18 serves to interrupt the signal at small signal amplitudes. It is known per se to design such a circuit arrangement for silent tuning in such a manner that with small signal amplitudes the amplification of one of the amplifying tubes is reduced to a very low value by applying a high negative voltage to the control grid. With larger signal amplitudes, the negative bias of said tube is caused to decrease in absolute value so that signal reception occurs again In the circuit arrangement shown in the Figure, interruption of the signal-reception occurs by the action of a voltage which is low or even positive at low signal amplitudes and is driven more and more negative with higher signal amplitudes This is achieved by connecting the anode of the diode 7 to the anode of the triode 18 so that the anode of the diode 7 is not driven positive relative to its cathode until a sufficient negative regulating voltage appears at the common point of the resistors 13 and 14. The two anodes are moreover connected through a resistor 2 1 to the positive terminal of the supply The cathode of the triode 18 is connected directly to earth, the cathode of the diode 7 being connected to earth through a resistor 19 and through a resistor 20 to the positive terminal. So long as the signal voltage is low, the control grid of the triode 18 is not biassed. The voltage set up at the 'common point of the resistors 13 and 14 may then be positive with respect to earth so that grid current tends to flow in the grid circuit of the tube 18, which current is limited by the resistor 24. Owing to the voltage drop across the resistor 21, the voltage on the anode of the tube 18 is considerably lower than the voltage of the 785,031 7 and the capacitor 22, which is connected between the output leads, serve for the aforesaid gradient-limitation During normal operation a given standing direct current will pass through the diode 7 On the occurrence of a sharp voltage peak the capacitor 22 will be abruptly charged in a positive sense However, the charging current is limited by the standing diode current since the former can naturally

not exceed the standing current. Such a gradient limiter only operates satisfactorily if the resistance of the signal source, that is to say the resistance of the parallel combination 6 is low When using the invention, said resistor may be made a factor 100 smaller than in the conventional receivers where the threshold voltage in the circuit for the regulating voltage is much lower.

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* GB785032 (A)

Description: GB785032 (A) ? 1957-10-23

Self-hardening surface coating compositions

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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 785,032 Date of Application and filing Complete Specification July 14, 1954. No 20575/54. Application made in Germany on March II, 1954. Complete Specification Published Oct 23,1957. Index at Acceptance: -Class 2 ( 6), P 6 A, P 6 C( 7: 8 B: 8 C: 13 B:

13 C: 20 D 3), P 6 (D 1: K 7), P 6 Pl(B: C: D: E 1: F: X), P 6 P( 4 C: 6 X), P 6 ( 52: T 2 A), P 7 A, P 7 C( 7: 8 B: 8 C: 13 B: 13 C: 20 D 3), P 7 D 2 A(l: 2 A: 2 B), P 7 K 8, P 7 P 1 (B: C: D: El: F: X), P 7 P( 4 C: 6 X), P 7 ( 52: T 2 A), P 8 A, P 8 C( 7: 8 B: 8 C: 13 B: 13 C: 20 D 3), P 8 D( 1 A: 1 B: 2 B 2: 2 C), P 8 K 7, P 8 P( 4 C: 6 X), P 8 ( 52: T 2 A), P 9 A, P 9 C( 7: 8 B: 8 C: 13 B: 13 C: 20 D 3), P 9 D(I Al: IBI: 3), P 9 K 7, P 9 P 1 (B: C: D: El: F: X), P 9 P( 4 C: 6 X), P 9 ( 52: T 2 A). International Classification: -C 08 f. COMIPLETE SPECIFICATION Self-Hardening Surface Coating Compositions We, DEUTSCHE GOLD-UND SILBER-SCHEIDEANSTALT VORMALS ROESSLER, of 9, Weissfrauenstrasse, Frankfurt, Main, 1, Germany, a Body corporate organised under the laws of 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 a process of coating copper, zinc or alloys of these metals with a self-hardening surface coating composition. It is known to produce self-hardening surface coating compositions such as adhesives, cements, trowelling masses and lacquers from polymerising substances or mixtures containing the latter, which on hardening form polyethylene compounds, polystyrene compounds, the so-called polyester resins, or resins derived from isocyanates and polyurethanes In this connection it is advantageous to use substances which polymerise rapidly even at room temperature under the action of catalysts. Such catalysts are, for example, redox systems, which contain a teriary amine, -aminosulphone or x-hydroxy-sulphone Mixtures which consist of polymerisable compounds and polymerised compounds are also frequently used as binding agents Such adhesives, cements, trowelling masses and lacquers may also contain the conventional fillers, pigments and plasticisers as well as the binding agent proper. In general, these mixtures of substances have proved exceptionally satisfactory It was only when they were applied to copper and its alloys or zinc and its alloys that occasionally a bond of comparatively low strength was observed, which makes it difficult to use them, for example, for bonding metals. It has now been found that the strength with which such substances or mixtures of substances adhere to copper, zinc and their alloys may be

substantially improved if the mixtures have added thereto small quantities of compounds defined below which form complex compounds with copper or zinc These complex formers are hydroxy-quinolines and enolisable acetone derivatives, for example acetyl acetone or benzoyl acetone. Accordingly the present invention provides a process of coating copper, zinc or alloys of these metals with a self hardening surface coating composition, for example a cement, trowelling mass, adhesive or lacquer, wherein the metal is coated with a mixture of at least one monomeric polymerisable compound having at least one carbon-to-carbon double bond, a polymerisation catalyst and a small amount of hydroxyquinoline or an enolisable acetone derivative, for example acetyl acetone or benzoyl acetone. It has further been found that coatings produced by the process of the invention harden without wrinkling, without external influences and even with exclusion of air to form coatings of exceptional adhesive strength, if they contain, in addition to the monomeric polymerisable compound and, as catalyst at least one tertiary amine or one c-amino-sulphone or one a-hydroxy-sulphone It is also advantageous to use, in addition to the catalysts mentioned above, at least one peroxide compound. As the monomeric polymerisable compound, it is preferable to use an organic compound which contains the terminal group -,CH=CH 2, as for example monomeric styrene A polymerised vinyl compound, for example, polystyrene, may be successfully employed as the wholly or partially polymerised compound The wholly or partially lPrice- 6 d l 785,032 polymerised compound is advantageously mixed with or dissolved in the monomeric compound at the time of use or just prior thereto. Mixtures capable of being used satisfactorily may contain one or more o' p-unsaturated polyester resins In general, it is sufficient if these polyester resins are added in quantities of less than 30 %, preferably 515 % If the proportion added is higher, the adhesive power of the mixture frequently decreases In place of or in addition to the polyester resins, maleic acid anhydride may also be employed with the same success The addition of these substances favourably influences the polymerisation velocity. The adhesive strength of the mixtures may be further improved by the addition of comparatively small quantities of acrylic acid, methacrylic acid, acrylic acid amide, methacrylic acid amide or polymers thereof. The addition of acrylic acid further facilitates the complete intermixing of the monomeric and polymeric compounds Moreover, the separation of the mixture into its components which sometimes occurs when an acrylic acid alkyl ester for example acrylic acid butyl ester,

is present, is prevented by the addition of acrylic or methacrylic acids, their amides or polymers. The said constituents may be added in different ratios, each according to the purpose of use A mixture which contains 60 to 100 parts of the polymer to 100 parts of the monomer is suitable for bonding metals The proportion of polymer is expediently increased for the production of cementing masses. In order to improve the elasticity and softness, the mixtures may also have added thereto so-called internal plasticisers Suitable internal plasticisers include monomeric compounds which produce soft polymers and are compatible with styrene, such as decalol vinyl ether and higher esters of acrylic acid and methacrylic acid Similar effects are produced by addition of the corresponding polymers Furthermore, polyvinyl methyl ether and polyvinyl ethyl ether, for example, are also suitable The mixtures may also contain cross-linking agents, such as divinyl benzenes, and other hardening monomers, for example, methyl methacrylate or p-dichlorostyrene. Among the peroxide compounds acting as catalyst particular reference may be made to benzoyl peroxide, which causes very rapid thorough hardening in combination with tertiary amines, for example, diethanol-p-toluidine The same result is produced if the tertiary amine is completely or partially replaced by 9-aminosulphone or an c'-hydroxysulphone. Further improvements in the hardening may be produced by the addition of comparatively small quantities of catalysation accelerators. Suitable compounds for this purpose are inorganic or organic compounds which contain a labile halogen atom, monohydric or dihydric aliphatic alcohols or small quantities of heavy metal salts 70 The mixtures to be applied may have added thereto other additives which are known per se for coating media, such as pigments, fillers, resins, cellulose compounds, plasticisers and/or oils 75 It has further been found that the reacting substances or mixtures of substances may first be brought together at the place of application or shortly before the time of application. Preferably the components of the mixture 80 which are to react with one another with hardening are drawn from different containers and brought together only at the place of application or shortly before the time of application, thus a liquid polymerising substance 85 which contains the oxidising constituent of a catalytically reacting redox system is supplied from one contaner and a liquid polymerising substance with the reducing constituent of a redox system is supplied from another con 90 tainer. In a preferred embodiment of the process monomeric styrene with an addition of at least one compound forming a labile amine oxide, and

monomeric styrene with an addition of 95 at least one peroxide compound, are applied simultaneously from two separate containers to the place of application The application of the components may advantageously be effected by means of a spray gun which has 100 two containers for accommodating the substances or mixtures of substances which are to be applied to a surface and delivers them on to the surface through a common spray nozzle or through separate spray nozzles which 105 converge upon the point of application. In a further development of the invention, it has further been found that good results are obtained if the polymerisable components of the mixture on the one hand, and the cata 110 lyst, on the other hand, are only brought together in suitable proportions at the place of application For example, a paste-like mixture of a polymerising substance with a monomeric organic compound having the ter 115 minal group -CH=CH may be used as binding agent By way of example, there may be mentioned a mixture of monomeric styrene with partially polymerised styrene or a mixture of monomeric methyl methylacry 120 late with the polymerised ester It is obvious that the mixture may also contain other substances. If a redox system is used as catalyst, the reducing component of the redox system, for 125 example, a tertiary amine, is added to the pasty mixture The mixture may in certain circumstances also contain small quantities of a polyphenol, for example, hydroquinone, for stabilising purposes 130 785,032 As the catalyst which is to be mixed with the polymerisable components of the mixture only at the place of application, or shortly before the time of application, it is possible with good results to use a compound which, like benzoyl peroxide for example, contains active oxygen The application of the catalyst is facilitated by using it as a solution or suspension, in certain cases in a plasticiser for the binding agent In order to impart the required consistency to this solution or suspension, it is advantageous for the said solution or suspension to have added thereto thickening substances, such as, for example, finely divided silicon dioxide, which has been produced pyrogenically. It has proved to be advantageous, for example when bonding articles together, for the polymerisable components of the mixture on the one hand, and the solution or suspension of the catalyst on the other hand, to be applied from tubes to the place of application. The tube openings may be of such dimensions that a predetermined length of the issuing ribbon of the polymerisable component of the mixture and a predetermined length of the issuing catalyst mixture correspond to the optimum mixing ratio of the two constituents. EXAMPLE 1 Articles of brass were bonded together by the process of the invention

by using the following two component systems:a) 84 parts by weight of polystyrene are dissolved in 100 parts by volume of a mixture of 77 % of styrene, 9 %/ of maleic acid-glycol polyester, 8 % of acrylic acid, 4 % of diethanolp-toluidine and 2 % of acetyl acetone and the total mixture is stabilised with 0 1 % by weight of hydroquinone. b) 5 parts by weight of benzoyl peroxide and 84 parts by weight of polystyrene are dissolved in 100 parts by volume of a mixture of 89 % of styrene, 9 % of maleic acid-glycol polyester and 2 % of acetyl acetone and the total mixture is stabilised with 0 2 % by weight of hydroquinone. One of the surfaces of the brass to be bonded is coated with the component a) and the other with component b) and then the two surfaces are pressed one against the other with moderate pressure The initial adhesion is already so great that the two parts even without applied pressure do not slip off one another: The bonding readily takes place at room temperature; a strength sufficient for these purposes is already obtained after about half an hour. EXAMPLE 2 The bonding process according to the invention was carried out using a cementing mass composed of the following two components:a) 81 parts by volume of styrene, 12 parts by volume of maleic acid-glycol polyester, 4 parts by volume of acrylic acid and 3 parts by volume of diethanol-p-toluidine are mixed and the liquid is stabilised with 0 1 %/ of hydroquione. b) 64 parts by weight of fine polystyrene bead material, 33 parts by weight of quartz powder, 3 parts of hydroxy-quinoline and 3 parts by weight of benzoyl peroxide are mixed. To prepare the mass for application, about 2 parts by volume of the powder b) are stirred into one part by volume of the liquid a) The mass can then easily be worked up in 5 to minutes and solidified a short time afterwards to form an exceptionally strongly adhering mass with good mechanical properties. EXAMPLE 3 A mixture of 85 parts of monostyrene, 84 80 parts of polystyrene, 9 parts of maleic acidglycol polyester, 8 parts of acrylic acid, 4 parts of diethanol-p-toluidine, 4 parts of acetyl acetone and 2 parts of hydroquinone is applied from a tube in the form of a ribbon 85 on to a copper plate Another ribbon consisting of 5 parts of dioctyl phthalate, 6 parts of benzoyl peroxide and 0 3 part of pyrogenically prepared silicon dioxide is laid on the first ribbon from another tube, the said 90 second ribbon being of the same length, but thinner The two masses are quickly mixed with a spatula and spread on the plate A second plate is placed thereon and hardening allowed to take

place at room temperature 95 After 30 minutes, a very firm bonding of the two plates is obtained, the adhesive being completely hardened after 6 hours.

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