4706 4710.output

* GB785113 (A)

Description: GB785113 (A) ? 1957-10-23

Improvements in and relating to the treatment of leather diaphragms and thelike

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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 Inventor:-AMBROSE JOHN CRUISE. Date of filing Complete Specification Dec 20, 1954 Application Date: Sept 22, 1953 N'o 26109/ 53 ' Complete Specification Published: Oct 23, 1957. Index at Acceptance:-Classes 2 ( 6), P 8 A, P 8 D( 2 B 2: 8 A), P 8 P( 2 X: 3 6 X), P 9 A, P 9 D( 1 B 1: 3), P 9 P( 2 X: 3: 6 X); and 76, C 2 B. International Classification:-C 14 c. COMPLETE SPECIFICATION. Improvements in and relating to the Treatment of Leather Diaphragms and the like. We, UNITED GAS INDUSTRIES LIMITED, of 51 Lincoln's Inn Fields, London, W C 2, a British Joint-Stock Corporation, do hereby declare the invention, for which we pray that a patent may be granted to us, and the manner by which it is to be performed, to be particularly described in and by the following statement:- This invention relates to leather diaphragrms and like leather articles such as are used, for example, in gas meters, gas water heaters, control devices of various types, pumps, valves and in other mechanisms or apparatus where the diaphragm or the like is required to

perform an operation in dependence upon the flexibility which it possesses as a result of the random orientation of the fibres and fibrils of its structure. In all such applications of the diaphragm or the like, it is highly desirable that the initial flexibility of the leather shall be maintained, to secure uniformity and accuracy in the performance of the function for which it is used over an extended period. The flexibility may vary, however, by reason -of the effect of external influences such as moisture, vapours or gases, or through changes set up by loss of oil dressing or by absorption of gaseous constituents or even by reason of repeated flexure mechanically imposed upon the diaphragm or the like during the performance of-its function. The variation in flexibility will be in some instances an increase, while, in other instances, it will be a reduction, but in all cases the variation is undesirable. The invention has among its objects to impart to the leather diaphragms and the like in question a degree of stability, more f E particularly in respect of flexibility, greater than that which they naturally possess, to ensure a higher degree of uniformity and accuracy of the mechanism in which is used such a diaphragm or the like, and to lengthen the useful life of such a diaphragm or the like in the performance of its function. According to the invention the leather intended for the diaphragms or the like is treated by impregnation with at least one monomeric ethylenically unsaturated compound which, applied in an emulsion or dispersion, polymerises upon the fibres and fibrils of the structure of the leather. The monomeric compounds that may be used for the purpose of the invention include unsaturated polyesters that will polymerise upon and in the leather treated, to which they may be applied in an aqueous or oil emulsion or dispersion, or mixtures of compounds which, under like conditions, will produce copolymers upon and in the leather. Some of the copolymer-forming compounds that may be used include acrylonitrile, ethyl meth-acrylate and other suitable compounds that will polymerise upon a substance immersed in the emulsion or dispersion in which they are contained These compounds are polymerisable at room temperatures without additional heat and without pressure, but the use of heat in a varying degree and pressures varying from atmospheric pressure is not excluded from the application of the invention The selection of a particular compound may be determined according to the degree of stability of the leather required. The leather may be submitted to the treatment with the monomeric

polymerisable compound as a distinct step or such treat785 -13 785,113 55. : 7, 1 1'I 1, e 1 1 785,113 ment may be incorporated with the oil or other dressings of the leather. As an example of a specific application of the invention, semi-chrome leather intended a for the diaphragms of a gas meter, and of a thickness approximating to 0 5 of a millimetre, is soaked in an aqueous dispersion of ethyl meth-acrylate of a concentration of about 30 per cent monomer and 70 per cent water for a period ranging from 10 to 30 minutes at room temperature in the range of 550 to 650 F The leather is then air-dried at a temperature under 1000 F The methacrylate polymerises into a flexible coating over the fibres and fibrils of the structure of the leather, and, being flexible, allows the fibres and fibrils to move freely while restraining any tendency on their part to contraction. After drying, the leather is dried and dressed in the usual manner The effect of the polymerised meth-acrylate on the leather may be controlled by the concentration of the dispersion in which the leather is soaked. It is not essential that the leather shall be soaked in the emulsion or dispersion For example, the leather may be brushed on one or both sides over the whole surface or so as to leave an annulus untreated adjacent the periphery or at the centre, or both Again, the brushing may be replaced by spraying. The treatment may take place in the tannery after the fat liquoring, the emulsion or dispersion being drummed into the leather or skins or sprayed thereon, in each case before the drying in the tannery.

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* GB785114 (A)

Description: GB785114 (A) ? 1957-10-23

Improvements in luminescent materials




PATENT SPECIFICATION Inventor: PETER WHITTEN RANBY ' Date of filing Complete Specification Nov 5, 1954. Application Date Dec 1, 1953. Complete Specification Published Oct 23, 1957. Index at Acceptance:-Class 39 (i), 54 (C: F: G: H:-J: P: Q) International Classification: -C 09 k. COMPLETE SPECGFICATION Improvements in Luminescent Materials We, THORN ELECTRICAL INDUSTRIES LIMITED, a British company, of 105-109, Judd Street, London, W C 1, do hereby declare the inevntion, 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:The present invention relates to luminescent materials for use for example in fluores, cent discharge lamps and in the formation of cathode ray tube screens and X-ray screens Luminescent materials comprising calcium pyrophosphate activated by tin have been proposed in British Patent Specification No. 578,272 The heating conditions disclosed in that specification are such that the tin compound in the matrix must be in the stannic state These luminescent materials can be excited by cathode rays but not by the 2537 or 3650 A U radiations. Other luminescent materials proposed in our Patent Specification No 746,272 comprise the pyrophosphates of the bivalent metal calcium and of one or more of the bivalent metals magnesium strontium, barium or zinc, activated with tin or with both tin and manganese, the proportion of tin being not less than 005 %' by weight of the luminescent materials, the composition being such that the molecular ratio of metal oxide (excluding the tin activator) to phosphorous pentoxide lies between the limits 2:0 9 and 2:1 4 inclusive, 'and the amount of calcium constituting not more than 98 molecular per cent of the total bivalent metal (excluding the tin activator or'the tin and

manganese activators) in the material. According to the present invention an artificial luminescent material comprises calcium pyrophosphate, with or without manganese pyrophosphate, and of the alpha and/or beta form as hereinafter defined by its X-ray diffraction lines, activated by tin in a lower valency state than stannic tin, or by tin in the said lower valency state and the manganese, lPrice 3 s 6 d l the proportion of tin being not less than 0.05 /' by weight of the luminiescent material, the composition being such that the molecular -ratio of metal oxide (excluding the tin acti 50 vator) to phosphorous pentoxide lies between the limits 2:0 9 and 2:1 4 inclusive, and the manganese when present constituting up to about one half of: the metal content (excluding the tin activator) of the luminescent material 55 Preferably the proportion of 'tin is not more -than 10 % by weight '-of the luminescent material Up to, but not including, 2 molecular per cent of the calcium may be replaced by one or more of -the metals strontium, 60 barium, zinc or magnesium. Materials in accordance with the present invention can be excited to fluorescence by ultra-violet light of short wavelength, such as the 2537 A U radiation, 65 Also -according to the present invention, a method of preparing an artificial luminescent material includes the step of heating at a temperature of above 700 C and below the melting point of the luminescent material an 70 intimate mixture comprising a matrix of calcium pyrophosphate, or of calcium pyrophosphate and magnanese pyrophosphate, or compounds yielding such a-matrix on heating, and a tin compound in an amount from 0 05 to 75 %', by weight of the intimate mixture, the composition of the intimate mixture being such that the molecular ratio of metal oxide (excluding the tin activator) to phosphorous pentoxide lies between the limits 2:0 9 and 80 2:1 4 inclusive, the heating conditions being such that the tin in the material is in a lower valency state than stannic tin, and the calcium pyrophosphate is in the alpha and/or beta form as hereinafter 'defined, and the man 85 ganese compound or compounds, when present in the intimate mixture, constituting up to about one half of the metal content (excluding the tin activator) of the matrix. It is sometimes of advantage to first prepare 90 the calcium pyrophosphate matrix and then to incorporate the activating tin compound 785,114 No 33407/53. r? W, -4,z G rice : 2 785,114 therein by heating unde:iinzoxiidising or _ The manganese may be added to the inti 45 weakly-reducing conditions mate mixture in the form of one or more of its Materials prepared by the method in accor compounds, foir example the carbonate or dance with the present invention comprise cal phosphate It is at present believed that at cium pyrophosphate'of the alpha and/or-beta

least some of the manganese incorporated in form as hereinafter defined the material replaces at least some of the bi 50 Theoretically the pyrophosphates 'f bi valent -netal present in the matrix. valent metals contain mnetal 9 ode and phos Suitable mixtures of compounds yielding phorous pentoxide in the ratio of 2:1 respec the calcium pyrophosphate matrix on heating tively However a certain limited latitude in comprise, for example, one or more calcium this ratio is permitted and the present inven compounds such as the carbonate, hydroxide 55 tion is concerned only with luminescent etc, together with the required amount of materials in which the molecular iatfo lies am-nbiuim -hosphate, or precipitated calcium within the limits specified above as being pyrophosphate together with calcium carbonaccording to the present invention It has been ate to make up the required proportion of calfound that slight changes in the 7 said moilecul' cium, or together with ammonium phosphate 60 ratio within the limits spec fie may prqdfce to niake up the required proportion of phosmarked changes in the colour of the phate, as required -fluorescence -produced by the -luminescent: The materials of the present invention are material obtained directly in the form of powders and The tinmay be-added to the intimate mix it is-not -necessary to melt or even sinter the 65 ture in the orn of one or more of its stannous material to obtain luminescence They are -compounds such as the oxide, chloride and -therefore more suitable for use in, for example, phosphate, and it is then important that the -a fluorescent lamp than are materials which heating of the intimate mixture should be -have been melted or even sintered The carried out under non-oxidising conditions to fluorescence exhibited by the materials-when 70 prevent the tin compound or compounds from activated with tin alone and excited by 2537 undergoing oxidation to the stannic valency A U radiation is generally blue in colour. -state Thus, the mixture may be heated in a -When _ manganese is incorporated the -plugged tube 6 r-a 'covered crucible or in a fluorescence exhibited is of longer wavelength non-oxidising atmosphere of, for example, than with tin alone The colour of the 75 steam or nitrogen or mixtures thereof, or mix luminescence is also dependent, at least to tures of hydrpgen with steamf or nitrogen or some extent, on the crystal form of the calcium -both The intimate mixture may be heated in pyrophosphate -matrix, and this in -turn steam without causing the-formation of oxy depends upon the temperature of heating. or hydroxyphosphates becaise the intimate The X-ray diffraction lines for the form 80 -mixture does not contain a sufficiently high of calcium pyrophosphate which we have -proportion-of basic metal oxide for such for called the alpha-form are as follows, where d :mation to

take place If the tin is added to the is the crystal lattice interplanar spacing in intimate mixture before the heating in the Angstrom Units and I is the intensity on an form of a stannic compound or-compounds the drbitrary scale using the terms very strong; 85 atmosphere during the-heat treatment should strong; medium; weak; very weak (not be such that the compound is reduced to a used): valency state lower-than stannic tin d I dd I :' 7 04 weak 2 74 medium 182 weak 4 85 weak 2 63 medium 1 77 medium :: 4 18 ':'weak 2 58 medium 1 70 weak 3.72 weak 2 43 medium 160 medium I - 3 49 weak ' 240 medium 1157 weak 3 26 strong 2 08 strong 1 29 medium 315 u'' strong 2 03 medium 1 24 weak 3.04 medium, 1 97 strong Similarly, the X-ray diffraction lines for the called the beta-form are as follows: form of calcium pyrophosphate whiih we have': 785,114 d I di I d I 4.72 weak 2 80 medium 2 22 medium 4.43 weak 2 75 medium 1 99 medium 3.34 strong 2 68 weak 1 95 medium 3.22 strong 2 54 medium 1 85 weak 3.09 medium 2 40 weak 1 83 weak 3.01 very strong 2 33 medium 1 77 medium 2.90 medium 2 27 weak 1 31 medium The X-ray diffraction lines have been determined for the calcium pyrophosphate matrix in the absence of tin and manganese, the positions and intensities of the lines being only slightly modified by the incorporation of the tin and manganese The alpha-form of the calciumrn pyrophosphate is formed at the higher temperatures up to the melting point and the beta-form at the lower temperatures; the temperature at which transition from the betato the alpha-form begins to take place is not precisely known but it is believed at present to be in the range of about 1100 to 1200 C. In order to obtain the maximum intensity of fluorescence with materials predominantly of the beta-form it is desirable that they should be prepared at temperatures near to the transition temperature. Methods of preparing luminescent materials in accordance with the invention will now be described, by way of example All the materials used should be of the high degree of purity which is recognised in the art to be necessary. EXAMPLE 1. 14.0 gins calcium hydrogen phosphate (Ca IPO 4) 0.9 gm diammonium hydrogen phosphate ((NH 4),HP Oj 0.7 gm stannous chloride (Sn C 12 2 HO) are intimately mixed together and then heated in a current of steam in a furnace at 1220 C. for -2 hour When cool the material is ground and can be reheated as before for another 2 hour When cool the powder shows a blue flourescence under excitation by 2537 A U. radiation The material is mainly of the alphaform but may contain a proportion 'of the beta-form. EXAMPLE 2. If the method of Example 1 is modified by including 0 6 gm manganese

hydrogen phosphate (Mn HP 04) in the intimnate mixture and the heating is carried out in a furnace at 1120 C the product when cool shows a bright yellow fluorescence under excitation by 2537 A U radiation The material is essentially of the beta-form. EXAMPLE 3. If the method of Example 2 is modified by carrying out the heating at 1220 C instead of 1120 C the product when cool shows a pink fluorescence under excitation by 2537 A.U radiation. EXAMPLE 4. 7.0 gins calcium carbonate (Ca CO 3) 10.0 gins diammonium hydrogen phosphate 65 ((NH,4)HP 04) 0.5 gins stannous chloride (Sn Cl I 2 H O O) 0.4 manganese hydrogen phosphate (Mn HPO 4) are intimately mixed together and then heated 70 in a closed silica crucible at 850 C for hour When cool the product is ground and reheated in -a current of steam in a furnace at 1220 C The final material is a powder which when cool shows a pink fluorescence 75 under excitation by 2537 A U radiation. The materials of Examples 3 and 4 are of the apha-form but may contain a proportion of the beta-form If the proportion of the beta-form becomes appreciable the fluorescence 80 shown is orange due to the simultaneous emission of pink light from the alphaform and yellow light from the beta-form In order to obtain as high a proportion of the alpha-form (pink fluorescence) as possible 85 variations in temperature during the heating should be avoided (e g by maintaining a slow steady current of steam) and care should be taken to exclude impurities which might encourage the formation of the beta-form 90 Patent Specification No 738,490, which was published after the filing date of the present application, discloses and claims an artificial luminescent material consisting of one or more of barium phosphate, strontium phos 95 phate, and calcium phosphate, the material being activated with tin of which at least part is present in the stannous state, the composition of the material being such that the ratio of gram-atoms of metal (excluding the tin 100 activator) to gram-moles of phosphorous pentoxide is between 2 96: and 2 50:1 inclusive, the strontium when present without calcium present constituting less than 2 44 gram-atoms of the metal in the material (excluding the tin 105 activator), and the calcium when present constituting less than 0 2 gram-atoms of the metal in the material (excluding the tin activator) per gram-mole of phosphorous pentoxide. Such an artificial luminescent material may 110 have an amount of tin present in the material between 0 01 and 0 08 gram-atoms per grammole of phosphorous pentoxide.

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* GB785115 (A)

Description: GB785115 (A) ? 1957-10-23

Apparatus for cleaning tanks in ships

Description of GB785115 (A)

PATENT SPECIFICATION 7859115 Date of Application and filing Complete Specification February 1, 1954. No 2988/54. Application made in Norway on April 25, 1953. DO Complete Specification Published: October 23, 1957. Index at acceptance:-Class 21, C. Interationaid Classification:-C 121. COMPLETE SPECIFICATION Apparatus for Cleaning Tanks in Ships I, AAGE JELMERT, a Norwegian subject, of Bjrn Farmannsgate 4, Oslo, Norway, 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 statment:The present invention relates to apparatus for cleaning tanks in ships, which greatly simplifies the cleaning. The disadvantages of using sea water for cleaning the tanks in ships are commonly known and consist mainly in that the walls of the tanks will corrode as a result of the chemical action of the salts in the sea water. Such corrosion will reduce the commercial value of the ship and the ship may after a lo few years, have to be taken out of service due to damaged tanks When the tanks in a ship have been cleaned by sea water, the washing water polluted with mud or dirt is thrown or discharged

overboard The water, containing oil, mud and other impurities, destroys both animal and plant life along the shores and pollutes the water in harbours For this reason, most or many harbour authorities prohibit the cleaning of the tanks in ships whilst the ships are in harbour and require all ships to clean their tanks while out at sea. It is obvious that such a method in unnecessarily expensive, in that it requires extra time and work before the ship can again be loaded or docked for overhaul. The advantages obtained in washing and cleaning ships' tanks with fresh water have long been known, but the difficulties and expense have been so great that fresh water has not been commonly employed for this purpose It has been proved uneconomic to buy the large quantities of fresh water which are required for a thorough cleaning of the tanks, as the cost of fresh water in many harbours is prohibitive particularly as the expensive fresh water has to be thrown (Price 3 s 6 d) or discharged overboard together with the mud and other impurities, as soon as the ship is at sea Furthermore, some ports are not able to supply the large quantities of fresh water which are required 50 It is an object of the invention to provide apparatus for cleaning tanks in ships, by which method a sufficient quantity of fresh water may be stored and used repeatedly, and by which mud and other impur 55 ities washed off the walls of the tanks are separated from the fresh water and are stored in special containers until it is possible to discharge the mud and dirt at sea. Thus, the tanks may be cleaned in any 60 harbour without violating any regulations, as nothing is illegally thrown or discharged overboard, and the ship is not required to make an unnecessary voyage to sea for the purpose of cleaning the tanks before it may 65 again be loaded or docked. A further advantage of the invention is that the tanks will not be corroded or will be corroded only to a minor extent if the fresh water has the desired properties 70 A further feature of the invention consists in that a detergent may be used together with the fresh water, thus increasing its cleansing properties Instead of fresh water a chemical fluid which is suitable for the 75 purpose may be used. According to the invention apparatus for cleaning a tank in a ship comprises in combination container means for storing fresh water or other suitable non-corrosive fluid 80 at one side or end of the tank, means for pumping the fluid from the storage means to a cleaning apparatus in the tank, means for pumping the fluid with the impurities from the bottom of the tank to a settling 85 container provided at the side or end of the tank remote from the storage means and means for recycling the fluid from an intermediate position in the settling container to the storage means 90 2 785,115 According to the invention

furthermore, the storage container and the settling container may be in open communication and both may be filled, or substantially filled, with cleaning fluid The invention is diagrammatically illustrated by way of example in the accompanying drawing, in which a section through the tanker is shown. Referring to the drawing, two containers 2 and 3 are disposed one on each side of an oil tank 1 The containers 2 and 3 are filled with fresh water or other cleaning fluid, approximately to the level shown in the drawing The containers 2 and 3 are in communication by means of a pipe 16, so that when water is withdrawn from one container, the level of the water in both containers will drop When cleaning the tank 1, the fresh water or other cleaning fluid is pumped by means of a pump 4 through a pipe 5 to the top of the tank 1 where the cleaning fluid is passed through a hose 6 to a cleaning apparatus 7 which is preferably of the Butterworth type. The cleaning fluid is sprayed against the walls 8 of the tank 1 under high pressure, and subsequently flows down the walls to the bottom 9 of the tank together with the oil, rust, sand or other material disengaged from or washed off the walls A powerful pump 10 pumps the cleaning fluid with the impurities through a pipe 11 and through a hatch 12 into the upper part of the container 3 The lighter impurities, such as oil, rise to the surface of the cleaning -fluid, as indicated at 13, while heavier impurities such as rust, sand or the like, form a sediment on the bottom of the container 3, as indicated at 14. The cleaning fluid is thus separated from the impurities in the container 3, and the fluid is returned by means of a pump 15, through the pipe 16 from the container 3 to the container 2, after which the fluid is recirculated A filter 17 may, if required, be provided in the pipe line 16. If the oil 13 at the top of the container 3 is valuable, it may readily be removed for use or for processing; if not, the oil may be 50 discharged overboard at a suitable time and place when the ship is at sea. Near the bottom, the container 3 is provided with a man-hole 18, through which the heavy impurities 14 may be removed as 55 required.

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* GB785116 (A)

Description: GB785116 (A) ? 1957-10-23

Improvements in and relating to the production of iron catalysts for organicsynthesis




COMPLETE SPECIFICATION Improvements in and relating to the'Production of Iron Catalysts for Organic Synthesis We, COUNCIL FOR SCIENTIFIC AND IN DUSTRIAL RESEARCH, a corporate body established by Statute, of Charles House, 5-11, Regent Street, London, S.W.1, do hereby declare the invention, for which we pray that 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: For the synthesis of hydrocarbon and oxygen-containing compounds containing more than one carbon atom per molecule from carbon monoxide and hydrogen, catalysts based on iron as the main ingredient are particularly suitable. For use in .a reaction system employing a stationary bed of catalyst granules or in one in which fine particles of catalyst are maintained in a fluidtsed bed by the up-flowing stream of reacting gases, suitable catalysts may be prepared by fusing a mixture of iron oxides and the oxides or salts of activating metals, or by impregnating a sintered form of iron oxide with solutions of salts of activating metals, with or without further sintering of the impregnated material:

Such catalysts possess the merit of cheapness and high resistance to disintegration, but in order to exhibit activity as catalysts for the synthesis they usually require reduction in hydrogen for a relatively prolonged period at a temperature considerably above that normally employed in the synthesis process (namely, at a temperature within the range 350" to 500 G.). While these catalysts possess a satisfactory activity for the synthesis per unit volume of catalyst their activity per unit weight is low and they tend to favour the production of low boiling products- and of excessive amounts of gaseous hydrocarbons. Furthermore, The high density of catalysts prepared in this manner tends to make them unsuitable for use in a liquid-phase reaction system where fine particles of catalyst are maintained in suspension in a liquid medium by the upflowing stream of synthesis gas. These disadvantages of fused and sintered iron catalysts do not apply to cataly.sts prepared by precipitation from solutions of the salts of iron and the activating metals. Catalysts prepared in this manner are of low density and high activity per unit weight; they may be brought into a state of high activity by a short period of treatment in hydrogen at a temperature inthe range of 280 to 350" C. or by treatment in- carbon-monoxide-containing gases under conditions similar to those employed in the synthesis process. Precipitated catalysts are normally prepared from chemically-pure iron and the preparation involves the consumption of large quantities of nitric acid and distilled water. A large and complicated plant is required for their manufacture. Such catalysts are, therefore, much more expensive to prepare than the fused or sintered catalysts. According to the present invention a material reducible to provide a catalyst for the synthesis of compounds containing more than one carbon atom per molecule from carbon monoxide and hydrogen is prepared by heating an intimate mixture of iron oxide with suicient. alkali-metal carbonate or hydroxide to produce alkali metal ferrite, decompo.sing the ferrite by treatment with water (when the iron oxide is liberated in an amorphous and partly hydrated form), washing the decomposed product with - water until substantially free of alkali metal hydroxide, re-impregnating the product with 0.1 to 5.0 per cent of alkali metal salt (such - as the carbonate, and also bringing the product- to a suitable degree of sub-division. We have found that a product so prepared requires a reducing or similar pre-treatment only of the same order as that necessary with precipitated catalysts and yet has high catalytic activity. The product may be reduced or pre treated either when prepared or else immedi mately before use. Under certain circumstances -it may be reduced under the conditions of the synthesis process in which it is to be

used. The process does not require the consumption of expensive chemicals or the use of costly plant Thus in particular since the ferrite is washed to remove substantially all the free alkali metal hydroxide, it is possible to use relatively inexpensive sodium carbonate or hydroxide to produce the ferrite and to incorporate the more expensive potassium com pounds in the final product. Even though the bulk of the alkali metal compound used in the production of the ferrite is recovered as hydroxide and can be disposed of as such or used for the preparation of further ferrite, there is lesste-apital investment- for - sodium compounds - than for potassium-compounds We have also found that impurities in the original iron oxide such as the oxides of aluminium, silicon, molybdenum, tungsten, and acidic radicles such as sulphate and phosphate are converted into water-soluble alkali-metal salts during the formation of the ferrite and are removed during the leaching of the product with water. Thus we are able to use cheap forms of iron oxide so that not only is the process cheap to operate but it employs cheap raw material. The intimate mixture of iron oxide and alkali metal carbonate or hydroxide may be made by finely powdering the materials. The mixture may be heated at a temperature within the range 350 to 1,200 C. (the precise temperature being dependent on the nature of the iron oxide and the alkali-metal compound used) for a sufficient length of time to effect a substantially complete conversion to alkali-metal ferrite. The sub-division of the leached product may be by grinding, sizing, forming, pelleting or the like. The pre-treatment may as usual be by heating with hydrogen or carbon monoxide or mixtures of the two to effect partial or complete reduction of the iron oxide to metailic iron or to effect partial or complete conversion to carbides of iron. Additional promoters may be incorporated by impregnating the washed iron oxide with a readily decomposable salt of the promoting metal. Promoters such as copper or silver or other metals which do not form

water-soluble alkali-metal salts under the conditions employed in the formation of ferrites may be incorporated in the mixture before it is heated. Suitable forms of iron oxide which may be used as raw material for the preparation of catalysts according to this invention include iron ores, iron oxides recovered from the manufacture of -aluminiurir from: bauxite: steel rolling-mill scale, burnt iron pyrites and similar naturallg-occurring or- industrial by- - 'product iron oxides. The invention also includes within its scope synthesis processes in which the catalyst is used and the products of such processes. The -process of preparing the catalyst according to the invention is illustrated by the following example, but is in no way restricted to - the - precise materials and conditions employedin this example. EXAMPLE. @ 1,000 gm. of steel rolling-mill scale, ground to pass a No. 170 B.S. Test Sieve was intimately mixed with 860 gm. of powdered anhydrous potassium carbonate. The mixture was then heated in a muffle furnace at a tem perature of 1,100 C. for 2 hours. Substan tially complete conversion of the iron oxide to the double oxide Fe2O3, K,O was indicated by the loss in weight accompanying the heat treatment, and was established by X-ray diffraction analysis of the resulting product. The sintered cake was roughly broken and extracted for 48 hrs., with distilled water in a continuous extractor of the Soxhlet type. The dried extracted material (1,100 gm.) con tained 94.1 per cent by weight or hydrated iron oxide and 3.9 per cent of potassium salts calculated as K2O@ and X-ray diffraction sanalysis indicated--the- absence of potassium ferrite or crystalline forms of iron oxide. The main constituent of the aqueous extract was potassium hydroxide, but the presence of potassium molybdate and other potassium salts was also-- established. The hydrated iron oxide prepared as de

scribed was crushed and graded to form granules which passed a No. 7 and remained on a No. 14 B.S. Test Sieve and tested for activity as a synthesis catalyst in a conven tional fixed-bed reactor. The density of the catalyst, the conditions used for the reduction and the conditions- used and results obtained in the synthesis are shown in the Table (catalyst "A"). Results obtained in tests with two other catalysts, "B," prepared by impregnating rolling-mill scale with- 2 per S'ce'n't by weight of- potassium carbonate and heating to 1,000 C., and "C" prepared by precipitation with alkali carbonate from solu tions of ferric nitrate, ferrous chloride and cupric nitrate - and' addition' of potassium carbonate to the washed filter cake, are also shown in the Table. - - - The data given in this table show that the bulk density, ease of reduction and activity for synthesis of Catalyst A, prepared by the procedure of this invention, resemble those of Catalyst C, prepared by precipitation, and are in marked contrast with the properties possessed by the sintered Catalyst B. <img class="EMIRef" id="026473826-00030001" /> Catalyst A -B- C Catalyst bulk density,. g/ml. 0.67 2.00 0.87 Reduction in pure hydrogen Temperature, C. 350 350 300 Time, hours, for complete reduction ~ 12.5 46 40 Synthesis H2.CO ratio of feed gas 2:1 2:1 2:1 Temperature, C. 230 265 230 265 230 265 Pressure, Atm. 20 20 20 20 20 20 Space-velocity of feed gas l./l. catalyst space/h. 634 1040 821 1520 810 1454 l./g. catalyst/h. 0.946 1.552 0.411 0.762 0.931 1.671 Carbon monoxide + hydrogen, converted, per cent 33.5 55.5 32.9 52.7 30.7 50.0

Carbon monoxide + hydrogen, converted, l./g. catalyst/h. 0.305 0.822 0.128 0.381 0.270 0.789 What we claim is, 1. A method of preparing a material reducible to provide" a catalyst - for the synthesis of compounds containing more than one carbon atom per -molecule from carbon monoxide and, hydrogen which comprises heating an intimate mixture of iron, oxide with sufficient alkali-metal carbonate or hydroxide to produce alkali metal ferrite, de composing the ferrite by treatment with water, - washing the decomposed product, with water until substantially free of alkali metal hydroxide, re-impregnating the product with 0.-1 to, 5.0 per cent - of alkali metal salt, and also bringing the product to a suitable degree of subdiylsion. 2. A method according to claim 1, wherein additidnal promoters are incorporated in the mixture before heating. 3.A method according to claim 1 or 2, wherein additional promoters are incor porated by impregnating the washed, decom posed product with a suitable compound of the promoter. 4. zA- method according to any one of claims 1 -to.3- wherein the mixture is heated to a temperature of from 350- to 12000 C 5. A method according to claim 1 of pre paring a material feducible to provide a catalyst for the synthesis of compounds con taining - more than 'one carbon- atom per molecule from carbon monoxide and hydrogen substantially as hereinbefore described in the example. 6. A material reducible to provide a catalyst for the synthesis of compounds containing more than one carbon atom per molecule from carbon monoxide and hydrogen whenever prepared according to the method of any of claims 1.to 5. 7. A method of preparing a catalyst which comprises heating a material according to claim 6 in hydrogen or carbon monoxide or a

mixture thereof. 8. A catalyst for the synthesis of com pounds containing more than one carbon atom per molecule from carbon monoxide and hydrogen whenever prepared according to the method of claim 7. 9. A process for the synthesis of compounds containing more than one carbon atom per molecule from carbon monoxide and hydrogen in which the synthesis is catalysed with a catalyst according to claim 8. 10. Compounds containing more than one carbon atom per molecule whenever produced - by the process claimed in claim 9.

* GB785117 (A)

Description: GB785117 (A) ? 1957-10-23

Improvements in or relating to fibre-drafting elements




COMPLETE SPECIFICATION Improvements in or relating to Fibre-Drafting Elements. We, SILVERTOWN RUBBER COMPANY LIMITED, (formerly The India-Rubber, Gutta Percha & Telegraph Works Company Limited), a British Company, of Herga House, Vincent Square, London, S.W. 1, and

WILLIAM HENRY MARTIN, a British Subject, of the Company's address -at Silvertown Works, Silvertown, London, E.16, 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: The invention relates to fibre-drafting elements used in connection with the manipulation of fibres of cotton,. rayon, wool, glass, asbestos and the like, such elements com prising spinning roll cots, textile roll covers and draft aprons and other elements used in various operations connected with spinning. A spinning roll cot or textile roll cover is, or may be, mounted on a metal roller or spindle rotating in opposed relation to a fluted metal roller. The textile fibres are passed through the opposed rollers and are drawn therefrom into engagement with a further similar pair of opposed rollers or like means of drafting rotating at a higher speed. A draft apron, which is an endless belt or band, is, in one arrangement mounted on and rotates with a pair of metal rollers in opposed relation to a similar apron mounted in the same way. Between. the aprons. the textile fibres are supported and nipped in their passage towards a pair of drafting rollers rotating at a greater surface speed than the draft aprons. Other arrangements of draft aprons are used. Natural rubber is not suited for fibre drafting elements for use with fibres -. containing natural oils or which are wetted prior to spinning with spinning oils because of the adverse effect of the oils on the rubber and such elements have, in recent years, been manufactured from oil resistant synthetic rubbers such as butadiene/acrylonitrile copolymers as sold under the Registered Trade Marks " Polysar ", "Hycar", "Paracril", "Chemigum", and Perbunan", and polymerized chloroprene (neoprene). - A disadvantage d synthetic rubbers for this purpose is that the textile fibres have an undue tendency to "lapping" round the fibredrafting elements. "Lapping" means that the fibres instead of passing through the fibre-drafting elements, cling to and go round with these elements causing breakage, thinning out or general unevenness of the thread, or the building upon the fibre-drafting elements of bunches of fibre which are eventually carried along with the thread and produce hard and/or soft places and slubs in the finished yarn. There are several causes of lapping. We believe that one of these is connected or related to electrostatic phenomena. Whilst this has not so far as -we are aware, been conclusively proved, we are satisfied that the electrostatic properties o a drafting element are important and that electrostatic attraction may at least aggravate lapping. In

use the rubber becomes charged with static electricity asZ a result of friction with the fibres and on. account of the high resistivity of the rubber the charge may reach a comparatively high value and be very difficult to discharge. Accordingly, the rubber wiU develop a substantial attraction for the fibres which it is difficult to remove. Many proposals have been. made for reducing lapping with synthetic rubber drafting elements. These proposals include the addition of various substances to the synthetic rubber, such as electrolytes which are readily soluble in water (e.g. calcium! nitrate) and which effect the -electrical propertiesof the material The function of such an added soluble electrolyte is dependent upon the presence of water (e.g. absorbed from the atmosphere or applied by dipping the rubber article into water) and the difficulty arises that as the electrolyte is soluble in the water, it is gradually leached out of the rubber and in time loses some of its efficacy. According to the present invention a fibre drafting element composed of a vulcanised butadiene/acrylonitrile - copolymer or polymerised chioroprene synthetic rubber is rendered water absorbent and hence less prone to the accumulation of-electrostatic charges. likely to cause lapping, by the addition tot the rubber of one or more water insoluble hydrophilic - inorganic materials, such as precipitated sili cates and oxides and bentonite clay. The term "hydrophilic" is used herein to mean "water attracting" as distinct from "water retentive ". Thus the hydrophilic materials used in the invention have the pro perty of attracting moisture from the atmo sphere which ensures continuously sufficient electrical conductivity inthe drafting elements to permit dissipation of electrostatic charges; The addition of substances such as diatoma ceous earth which are merely capable of retain ing large quantities of water does not ensure continued conductivity because the water may dry out, in time, Materials which may be used include, for example, precipitated aluninium silicate, pre cipitated calcium silicate, precipitated aluminium oxide, activated alumina, as well as bentonite clay. ~ The materials may be added (e.g. as fillers)

in proportions of 100-150 or more parts by weight of the material to 100 parts of the syn thetic rubber. For exampIe when one of the silicates is used alone it may be added in proportion of 100 parts to 100 parts of rubber and when a mixture of a silicate and bentonite clay is used these may be 30-75 parts of the silicate and 30-75 parts of the clay to each 100 parts of rubber. A water absorption up to a maximum of 40-45% by volume of the composition is desirable. A further difficulty which arises with drafting elements. the synthetic rubber. used in the invention is that although the rubber is oil resistant, nevertheless the natural oils in the fibres and oils added to assist the spinning operation are found to cause local swelling of the elements where they are in substantial con tact with the fibres. Some tackiness of the sur face of the elements may also be caused but this largely can be overcome by choice of suit able plasticisers. An advantage of the addition of the hydrophilic materials according to the invention is that they cause an overall swelling of the -element in which is greater than, and substantially masks, the local swelling caused by the~oils. The following are specific examples of compositions suitable for drafting elements: FIRST COMPOSITION (Particularly suitable for synthetic fibres). Shore durometer (type A) hardness 80-84 Colour grey Sp. Gr. 1.40 Test-cure 30 means. at 310 F. Polysar (Registered Trade Marl) N.P. 350 (butadiene/acrylonitrile rubber) - - - - 34.2% Vulcanised oil - - - - 3.5% Stearic acid - - - - - 0.2% Pale cumarone indene resin ~ - 2.7% Pale cumarone resin liquid - - 3.0% Agerite (Registered Trade Mark) powder - - - - - 0.4%

Resin oil - - - - - - 1.4% Titanium dioxide 98% - 3.6% Graphite - - - - - 1.8% Bentonite clay - - - - - 24.8% White A.R.F. (prepared aluminium silicate) - - - 20.0% Santomerse D (Registered Trade Mark) - - - - - 0.5% - Zinc oxide - -- - - 1.8% Ground sulphur - - - - 1.4% Altax (Registered Trade Mark) accelerator - - - - - 0.7% 100.0% SECOND COMPOSITION (Particularly suitable for natural fibres-e.g. ~wool and cotton). Shore durometer hardness 80-84 Colour grey Sp.- Gr. 1.30 - Test cure 10 mins. at 310 F. Polysar (Registered Trade Mark) N.P. 350 (butadiene/acryloni-, trile rubber) Pale cumarone resin - Resin oil - - - - - - 2.0% Agerite (Registered Trade Mark) powder - - - - - 0.7% Titanium dioxide 98% - - - 3.5% Graphite - - - - - - 2.0% Bentonite- clay - - - - 17.03 % White A.R.F. (prepared aluminium silicate) - - - 12.1% Ground glass 100 mesh - - 22.0% Zinc oxide - - - - - 2.2% Ground sulphur - - - - 0.07% Tuads (Registered Trade Mark) accelerator - - -- - 1.4% - -- 100.00% In the above compositions. the bentonite clay and the aluminium silicate are the water in soluble hydrophilic inorganic materials employed in accordance with the invention. Each of the above compositions is thoroughly and evenly mixed in a mixing mill and processed according to normal procedure. For spinning cots and textile roll covers the composition is extruded, vulcanised and cut to length. For draft aprons a layer of the composition is wrapped on a cylindrical mandrel and a textile reinforcement wound on, after which

a further layer of composition is applied and the whole is vulcanised. It has been found that even with fibre draft ing elements incorporating hydrophilic materials according to the invention, initial lapping difficulties are sometimes experienced when the elements are first used in a mill. A certain time interval seems to occur before the element absorbs - a sufficiency of water, and during this time interval the textile fibres lap up. With a view to reducing this difficulty there is, in a preferred form of the invention, incorporated in the synthetic rubber mixture, a wetting agent. Examples of suitable wetting agents are the sulphonated lorol types, such as Facemol (Registered Trade Mark) and the alkyl aryl types such as Santomerse D (Registered Trade Mark) embodied in the first of the above examples. The wetting agent decreases surface tension and as a result imparts to the fibre drafting element the property of more rapid water absorption. Such wetting agents are water soluble and may be gradually leached out of the fibre drafting element, but before this can occur the wetting agent is no longer required, since the fibre drafting element has absorbed a sufficiency of water through the presence of the hydrophilic inorganic filler, as already explained. The wetting agent is used solely to accelerate the initial intake of water. What we claim is : - 1. A fibre-drafting element composed of a vulcanised butadiene/acrylonitrile copolymer or polymerized chloroprene synthetic rubber and rendered water absorbent and hence less prone to the accumulation of electrostatic charges likely to cause lapping, by the addition to the rubber of one or more water insoluble hydrophilic inorganic materials, such as precipitated silicates and oxides and - bentonite clay. 2. A fibre-drafting element as claimed in Claim 1 in which the hydrophilic material comprises precipitated aluminium silicate. 3. A fibre-drafting element as claimed in Claim 1 in which the hydrophilic material comprises precipitated calcium silicate. 4. A fibre-drafting element as claimed in Claim 1 in which the hydrophilic material comprises precipitated aluminium oxide. 5. A fibre-drafting element as claimed in Claim 1 in which the hydrophilic material comprises activated alumina. 6. A fibre-drafting element as claimed in any one of rhe preceding

claims in which the hydrophilic material (or the mixture thereof) is added in proportion of 100 or more parts by weight of the material or mixture to 100 parts of the synthetic rubber. 7. A fibre-drafting element as claimed in Claim 6 in which the proportion of hydrophilic material is less than 150 parts to 100 parts of synthetic rubber. 8. A fibre-drafting element as claimed in any one of the preceding claims having a water absorption of 4O-45 % by volume of the com position. 9. A fibre-drafting element as claimed in any one of the preceding claims and including a wetting agent. 10. A fibre-drafting element having a composition substantially according to either of the foregoing examples. PROVISIONAL SPECIFICATION Improvements; in or relating to Fibre-Drafting Elements We, THE INDIA-RUBBER, GUTTA PERCHA & TELEGRAPH WORKS COMPANY LIMITED a British Company, of Herga House, Vincent Square, London, S.W.1, and WILLIAM HENRY MARTIN, a British Subject, of the Company's address at Silvertown Works, Silvertown, London, E.16, do hereby declare this invention to be described in the following statement: The invention relates to fibre-drafting elements used in connection with the manipulation of fibres of cotton, rayon, wool, glass, asbestos and the like, such elements com6 prising spinning roll cots, textile roll covers and draft aprons and other elements used in preparing the fibres for spinning. A spinning roll cot or textile roll cover is mounted on a metal roller or spindle rotating in opposed relation to a fluted metal roller. The textile fibres are passed through the opposed rollers and are drawn therefrom into engagement with a further similar pair of opposed rollers rotating at a higher speed. A draft apron, which is an endless belt or band, is, in one arrangement mounted on and rotates with, a pair of metal rollers in opposed relation to a similar apron mounted in the same way. Between the aprons the textile fibres are supported and nipped in their passage towards a pair of drafting rollers rotating at a greater surface speed than the draft aprons. Other arrangements of draft aprons are used. Natural rubber is not suited for fibre drafting elements for use with fibres containing natural oils or which are wetted prior to spinning with spinning oils because of the adverse effect of the oils on the rubber and such elements have, in recent years, been manufactured from oil resistant synthetic rubbers such as butadienelacrylonitrile

copolymers as sold under the Registered Trade Marks " Polysax". "Hycar", "Paracril", " Chemigum ", and " Perbunan ", and polymerized chioroprene (neoprene). A disadvantage of synthetic rubbers for this purpose isthatthe textile fibres' have an undue tendency to "lapping" round the fibre-drafting elements. " Lapping " means that the fibres instead of passing through the fibre-drafting elements, cling to and go round with these elements causing breakage, thinning out or general unevenness of the thread, or the building up; on the fibre-drafting element of bunches of fibre which are eventually carried along with the thread and produce hard and/ or soft places and slubs in the finished yarn.

4706 4710.output

Law