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1. do 2 Trisodium phosphate so do lution 5 NaOH _ do_ es Ethyl Alcoh d0___ Motor Oil do__ 5 BOQ ss oe oe AA EA do AAA rasa essen do 9x9 Thickness Gauge _ do 125 are practical to give the product within the scope of my claims Specifically I find that chlorinated paraffin should contain not less than 45 chlorine nor more than 60 that the charge stock shall preferably be in 6 should be not less than 15 C or more than 55 C and that the percent binder in the finished composition should be within the limits of 18 5 and 25 to produce tile to conform to Federal Specification SS T 307 al though there are possible an almost infinite number of combinations of charge stock degree of chlorination melting point of chlorinated paraffin ratio of vinyl resin 10 15 20 25 30 35 45 10 5 6 0 to 15 0 13 5 to chlorinated paraffin of binder to filler etc The properties of the vinyl polymer to be used may be determined principally by the following tests within the limitations shown a Mold tranparency test Method of Test 16 attached Method of Test 17 1 attached An additional example of the number of variations which may be practiced within the scope of my inven tion is as follows EXAMPLE IL TILE VINYL TYPE 1 Paraffinic hydrocarbon of approximately CopH4 aver age composition was continuously chlorinated to a2. United States Patent Office 3 005 791 Patented Oct 24 1961 1 3 005 791 FLOORING MATERIALS John W Church Newburgh N Y assignor by memme assignments to The Ruberoid Co South Bound Brook N J a corporation ef New Jersey Filed Sept 18 1957 Ser No 684 706 9 Claims Cl 260 27 This invention relates to compositions suitable for floor coverings and is herein described as embodied in what may be called 1 A grease resistant asphalt tile although the tile contains no asphalt as covered by Federal Specification SS T 307 2 A vinyl tile conforming to the Type I description under L T 751 In the drawing FIG 1 is a diagrammatic sketch of apparatus for carrying out the chlorination of paraffin and FIG 2 is a top plan view of a mold test transparency gauge In flooring compositions great resistance is a highly desirable characteristic Asphalt tile as it is now made to conform to Federal Specfication SS T 3065 is not made so as to be grease resistant A limited amount of so called asphalt tile is made to conform to the require ments of grease resistant tile Federal Specification SS T 307 However special synthetic resins considerably more costly than those used in the SS T 3065 type are required and the cost of the resultant product is so high as to limit its use There are other forms of flooring compounds which are grease resistant such as the vinyl tiles under Federal Specifications L T 75
3. Great Britain Oct 27 1948 of the copolymer l 713 905 Great Britain Aug 18 1954 ne UNITED STATES PATENT OFFICE CERTIFICATION OF CORRECTION Patent No 3 005 791 October 24 1961 John W Church It is hereby certified that error appears in the above numbered pat ent requiring correction and that the said Letters Patent should read as corrected below Column 2 line 68 for produce read product column 4 line 9 for hydraulic read hydrochloric line 32 for CasH62 read CosHga line 57 for Vinvy read Vinyl column 7 line 55 for and or read and or column 9 line 36 after paper insert on an Signed and sealed this 10th day of April 1962 SEAL Attest ERNEST W SWIDER DAVID L LADD Attesting Officer Commissioner of Patents
4. This high solvent power plasticizer D O P acts as a coupler between the low solvent power 40 chlori nated parafin and vinyl resin when it is there to at least three parts DOP to one part chlorinated paraffin When these portions are exceeded and particularly when the currently commercial chlorinated paraffin is used along as the entire plasticizer component the above mentioned undesirable phenomena occurred In FIG 1 there is diagrammatically illustrated appara tus for carrying out the paraffin chlorination In FIG 1 numeral 1 designates a reservoir of paraffinic hydrocar bon and or partially chlorinated hydrocarbon Numer al la designates a gas liquid separation zone of said reservoir Numeral 2 designates a circulating pump Numeral 3 designates a chlorine supply Numeral 4 designates a heat exchanger Numeral 5 designates a a condenser Numeral 6 designates the spent gas efflux In the drawing there is shown two similar units 10 19a The spent gas efflux 6 of unit 10 is connected to pump 2 of the second unit The second unit 10a acts as a scrubber to remove chlorine from the spent gas effluent from the first unit 10 Additional scrubbing units may be placed in series if desired When chlorina tion has been completed in unit 19 the product is removed and the vessel 1 recharged with hydrocarbon Raw chlo rine may be introduced into unit 16a and then unit 10 becomes a scrubbing unit Molding test Transparency The area o
5. chlo rine content of 52 5 had a melting point of 15 C a specific gravity of 1 257 and a color of one 1 on the Barrett scale The average temperature of chlorination was 100 C since it was not necessary to go to quite as high a tem perature in this case as in the original case because of b Relative viscosity __ __ the lower viscosity The finished product was immedi ately degassed and chilled to room temperature In this case the following tile formula was used Chlorinated Paraffin 2_ 11 840 Vinyl Copolymer 2_ 7 900 Polymerized rosin_ 875 Stabilizer 2 22 2222 ee eens 260 Ground limestone 46 125 7R Asbestos Fibre_ AA 30 000 Pigment cocoa 3 000 100 000 1Such as epoxy resin barium cadmium laureate barium ricinoleate and others This tile gave the following test results when tested in accordance with Federal Specification SS T 307 and with Federal Specification L T 751 Tile Floor Vinyl Plastic L T 751 Requirements Ys Sample Specimen 7 0 to 15 0 14 2 35 0 5 Average Shall not crack or break Not less than 6 eS Nos more than 015 lin Not greater than 030 Not greater 1 0 Not poe than 120 Do Do Not mere than 120 Do rai n Do A CEA OA ae Do 8 992 to 9 008 01125 120 to 130 0 005
6. grease resistant properties will be found wanting It should be understood that paraffinic materials in and of themselves are not miscible nor compatible with vinyl polymers and copolymers in the ranges described herein Only by careful chlorination of the paraffinic hydrocarbon to at least 45 may the paraffin be ren dered soluble in and permanently miscible with the vinyl polymer Furthermore if the chlorination is car ried out in such a way that either a Portions of the paraffin are chlorinated to a low degree even though the average chlorine content may be at the proper level the chlorinated produce will take on the characteristics of the least chlorinated fraction and therefore cause impermanent miscibility with the resultant loss in grease resistant properties or still further b If the chlorination is not controlled so that prod 3 005 791 3 ucts of the proper composition are obtained resulting in decomposition then also will the product be lacking in merit A typical method for making the chlorinated paraffin noted above as P 45 is as follows A chlorination apparatus such as shown in the at tached drawing is charged with a melted or liquid hydro carbon at a temperature of 80 C Dry gaseous chlo rine is closely associated with the entire mass of hydro carbon by violent agitation of the hydrocarbon and the chlorine together The exothermic heat of reaction is removed by suitable cooling method
7. successful in controlling the foam The temperature was allowed to rise to an average point of about 110 C and was never allowed to exceed 125 C by control of the exothermic heat generated The reaction was continued for 30 hours at the end of which time analysis revealed that the chlorine content was 58 the ASTM ring and ball softening point was 42 C and the specific gravity was 1 38 The material was immediately cooled to room temperature and was 10 15 20 25 30 35 40 45 50 55 60 65 70 75 4 found to have a color of about 2 on the Barrett scale When the same material was made and any local over heating was permitted or the temperature was allowed to rise substantially above 125 C the material was dark and in some cases almost ink black This color is one indication of decomposition and has a marked effect upon the properties of the product If stored at an elevated temperature over a long period of time or if hydraulic acid gas is not properly stripped decomposi tion with an attendant darkening in color takes place However if it is desired to store the product at a higher temperature it may be stabilized by the use of the usual heat stabilizers commonly used in stabilizing polyvinyl chloride with or without the accompaniment of alka line earth metals or alkaline earth carbonates Whether or not the material is stored at elevated temperatures is purely a matter of indi
8. 000 100 000 1 Such as epoxy resin barium cadmium laureate barium ricinoleate and others The ingredients are placed together in an intensive internal mixer such as a Banbury mixer or a Baker amp Perkins mixer and fluxed together by an intensive knead 10 15 20 30 40 45 50 55 60 65 79 2 ing action to form homogeneous masses of mixed mate tials The masses are suitably sheeted out in manners well known to the art such as being further incorporated on a two roll mill at which time marbleizing stock may or many not be added and reducing to desired thickness by passing through a train of calender rolls while being maintained at an elevated temperature suitable to produce ductility and the required adhesion to the calender rolls The finished sheet is partially cooled and now may be cut into sheets or tiles of any required size or rolled up into rolls This is the typical and rather well known so called Asphalt Tile process In most cases the original calendered sheet is cut up immediately into tiles and any border as well as rejected tiles are returned for reprocessing along with the new batch The system is completely thermoplastic and the product resoftens to workability as soon as its tempera ture is elevated to the desired point In order that the finished composition may pass the grease resistant prop erties of SS T 307 as well as the other requirements the Selection of the
9. 1 and certain linoxin or linoleum types as well as certain types of vinyl compositions lami nated to felt or other cellulosic backings AI of such other products however have disadvantages in one form or another such as a High cost b Failure to pass the curling requirements of both SS T 3065 and SS T 307 I have discovered that an economical composition made conforming to all the desirable characteristics of sS T 307 may be produced by combining a certain type of chlorinated paraffin with a certain type of vinyl poly mer or copolymer to form an organic binder which has such high wetting power and at the same time such ex cellent grease resistance that it may be combined with relatively large amounts of low priced fillers such as ground limestone asbestos fibre and pigments for color so as to give a highly serviceable curlproof grease resis tant flooring material This product may be formed in large sheets or may be marketed in the form of tiles of any convenient size It may also be produced in a variety of thicknesses A typical composition of such a product is as follows EXAMPLE 1 GREASE RESISTANT ASPHALT TILE P 45 chlorinated parafin_ 14 890 Vinyl copolymer detona 4 850 Polymerized rosin _ _ 875 Stabilizer whos oo Sk oe eee 260 Ground limestone 56 825 TR asbestos fbre_ 2 19 300 Pigment _ 2 3
10. 7 Vinyl Polymer 2 consisted of ten parts of vinyl ace tate and 90 parts of vinyl chloride which were dissolved in normal hexane under pressure in the presence of 3 lauroyl peroxide and polymerized under agitation at a the range of CigHz3 to CegHge that the melting point 75 pressure of 100 pounds per square inch at a temperature 3 005 791 7 of 50 C with stringent agitation in accordance with U S Patent No 2 064 565 The resultant polymer had a composition of approximately 90 chloride and 10 acetate and gave the following test results 4 59 cm 3 07 2 solution a Mold transparency test b Relative viscosity Conclusions The use of chlorinated paraffin in vinyl compositions is not new However its use in the proportions cited herein is distinctly new and novel The recommenda tions of the commercial manufacturers of chlorinated paraffin all warn against its use in a greater quantity than 25 of the plasticizer content The conventional prod uct of commerce is 40 chlorinated paraffin and when this product is used in any of the portions cited above it does not make a homogeneous permanently miscible combination the chlorinated paraffin either failing to completely flux the vinyl resin in the first part or exuding or sweating out of it upon cooling Its use in vinyl com positions is recommended with strong solvent power plasticizers such as the di octyl alcohol ester of phthalic acid
11. about 54 and 58 chlorine and having a melting point of around 42 C and 2 about 1 part of a copolymer of about 87 vinyl chloride and 13 vinyl acetate 3 A grease resistant floor tile as defined in claim 1 in which the organic binder consists essentially of 1 about 60 of a chlorinated paraffin of around 52 5 chlorine and having a melting point of around 15 C and 2 about 40 of a copolymer of about 90 vinyl chloride and 10 vinyl acetate 4 A grease resistant floor tile as defined in claim 1 in which the inorganic fillers are mainly calcium carbonate admixed with asbestos 5 A grease resistant floor tile as defined in claim 1 made of the following ingredients in approximately the following proportions Chlorinated paraffin __________ 14 890 Vinyl copolymer _ 4 850 Polymerized rosin _ __________ 875 Stabilizer 52560005 scone es 260 Ground limestone _ _ 56 825 Asbestos fiber _ 19 300 Pigment AAA nl es 3 000 100 000 6 A grease resistant floor tile as defined in claim 1 containing the following ingredients in approximately the following proportions Chlorinated paraffin coc 11 840 Vinyl copolymer _____ N 7 900 Polymerized rosin _ _ 875 Stabilizer Zu ne n aa 260 Ground limestone _ 46 125 Asbestos fiber X 30 000 Pigtient PAE ea 3 000 E 100 000 7 A grease proof composition adapted for use in making grease re
12. ed hydrocarbon together prior to incorporation with the rest of the flooring composition batch This will depend however upon the time temperature and degree of mixing employed in the mixing of the tile batch and is not a pre requisite unless it be desired that the time of mixing of the ultimate batch be short Although I mention the particular way in which the resin in this particular case was made and its particular characteristics there are other recipes and procedures which may be used within the scope of my limitations to give the desired result for instance instead of the polymerization taking place in water suspension it could be done in the presence of a liquid hydrocarbon such as described in the U S Patents Nos 2 064 565 and 2 075 429 The ratio of chlorinated paraffin to vinyl poly mer selected for this particular case is not rigid and I have determined that ratios between 1 5 to 1 and 4 to 1 16 Sample SS T 307 Requirements Specimen Oue minute penetration mils ooo Ten minute penetration mils Maximum allowed mils Indentation at 115 F mils __ Residual a MAMA AA annaia a a A Shall not crack or breaks Not less than 4 __ Dimensional Stability _ Impa Deflection Flexibility Curl and Alkali Resistance Scratch din Control Inches _ Lard do Wesson cot do tonseed oil Kerosene
13. f transparency of a molded unplasticized vinyl copolymer as calculated from a transparency gauge 15 see FIG 2 is a means of measurement devised to compare the flow or thermoplastic properties of the vinyl copolymer and to obtain an indirect qualitative measure ment of the processing behavior of the vinyl copolymer in a given vinyl asbestos tile formulation Apparatus 1 Carver Hot molding press see attached description 1 Carver Cold molding press see attached description 2 Teflon 014 gauge sheets 6 x 6 2 Aluminum plates 5 6 x 5 6 x 1 2 1 Transparency gauge 1 Stopwatch 1 Torsion balance Procedure 1 Weigh out 10 grams of the vinyl copolymer to be tested and place in a small pile approximately 5 cm in diameter on a 014 gauge 6 x 6 piece of Teflon or equivalent type of coated fabric which is supported by a flat 5 g x 5 6 x 14 aluminum plate 10 15 20 25 30 35 40 45 50 55 60 65 70 75 8 2 Cover the vinyl copolymer with another sheet of Teflon and a 5 g x 5 g x 14 aluminum cover plate 3 The sandwich of the two aluminum plates the two Teflon sheets and the vinyl copolymer comprise the mold assembly 4 A Carver Laboratory Press described as attached hereto is heated electrically to 155 C with the platens in contact with each other so as to assure uniform heat ing of both plates When the temperature has r
14. ingredients used must be carefully made and the processing conditions must also be carefully con trolled This tile 3 08 1 ratio P45 vinyl gave the follow ing test results when tested in accordance with Federal Specification SS T 307 Sample SS T 307 Requiremenis Specimen One minute penetration mils _ _ 9 4 6 0 to 15 0 Ten minute penetration mils 14 7 Maximum allowed mils 14 8 14 8 Indentation at 115 F mils _ 32 0 36 0 O K Shall not crack or break gt 2 Not less than 4 015 Not greater than 030 055 1212 aiana do 125 Not greater than 170 Wesson Oil hydrogen do 130 Do i ated cottonseed oil 2 Kerosene 100 Do 2 TSP 055 Do i 9 000 MD2x8 992 to 9 008 N 9 000 MD Thickness Gauge do 38 125 120 to 130 1 Covering both class 1 and class 2 oil and alkati resistance tests 2 Wesson Oil hydrogenated cottonseed oil used as a substitute for cottonseed oil 3 Machine direction 4 Against machine direction The chlorinated paraffin which is not grease resistant in and of itself is converted into a grease resistant binder by complete and thorough solution in and miscibility with the vinyl copolymer If for any reason the asso ciation is incomplete or the two do not remain in com plete miscibility with each other and if the chlorinated paraffin tends to sweat or exude from the gelled mass obtained then the
15. iod so as to achieve as high mobility and as high distribution of gas as possible The product is preferably cooled immediately as soon as the reaction is finished to as low a temperature as possible and still permit it to be handled The particular chlorinated paraffinic material used in the above formula was produced as follows Crude petroleum wax of approximately the compo sition CapHas was melted brought to a temperature of 80 C and charged into a glass tank equipped with a recirculating pump connected by pipe lines to the glass vessel The pump caused the liquid to move at a high velocity to a pipe line into which dry chlorine gas was introduced Reaction in part was almost instantaneous and the by product hydrochloric acid gas along with a relatively small amount of unreacted chlorine was led over into a second or scrubbing reactor and the gas from it in turn was led to a third so that the exit gas was almost entirely hydrochloric acid gas In order to avoid foaming at certain points during the reaction period a small amount of a volatile paraf finic hydrocarbon having a boiling range of 400 to 500 F was introduced into the system and a reflux condenser was mounted on the exit of each chamber to condense any of this somewhat volatile hydrocarbon carried off by the hydrochloric acid gas The action of the condensing vapor upon the viscosity of the foam layer on top of the mass of chlorinating hydrocarbon was
16. ion of apparatus and operation See Service Manual and General Instructions supplied by manufacturer The Carver Laboratory Press is supplied without the heating and cooling accessories These items are ordered separately The press proper has 6 inch square pressing faces between which a pressure of 20 000 lbs can be easily generated by the hydraulic pump handle The press is self contained having its own oil pump reservoir and gauge Hot Plates platens Electric for use with the Carver Laboratory Press These platens are intended for plas tic molding and hot pressing of various kinds They are 6 inches square and are built to operate from a lamp socket They provide any heat desired up to 204 C Each platen is equipped with a thermometer well into which a thermometer can be inserted in order to deter mine the temperatures The platens are supplied with thermoswitch on off switch cord and plug but without thermometer The platens are supplied in either 115 volt A C or D C or 230 volt A C or D C Two i Diametrie degree of transparency Since the chart is spaced in em divisions the direct reading gives a num ber twice that of the radial distance in em or the diametric value 2 Transparency gauge A calibrated chart consisting of ten concentric circles spaced 0 5 centimeter apart and di vided into eight equal sectiens by eight radial lines spaced 45 apart Bach circle is numbered from the center out along each radia
17. isen to 155 C the electricity is turned off the press opened and the mold assembly inserted 5 The press is then closed to contact pressure only and held for one minute 6 Pressure is raised to 2000 1bs sq in on the outer scale which reads the pounds per square inch on the 36 sq in platen 7 Release pressure and transfer to water cooled cold press at 2000 lbs per square inch pressure for two minutes 8 Release cold press pressure and remove vinyl film from mold 9 Measure the Diametric Degree of Transpar ency with the Transparency Gauge by placing the molded film on the gauge and reading the highest visible number or fraction thereof through the film at each of the numbered bisecting lines The Diametric Degree of Transparency is the average transparency obtained from the eight readings of the transparency gauge Tolerance A INDIVIDUAL SHIPMENTS OF VINYL COPOLYMER Two moldings shall be made from each individual ship ment of vinyl copolymer under the above controlled con ditions and eight transparency readings for each mold ing shall be averaged If the average numerical reading of the two moldings show a deviation of greater than 2 from one another other moldings shall be made until two show no greater deviation than 2 The ir relevant data is discarded CARVER LABORATORY PRESS Manufacturer and supplier Fred S Carver Inc One Chatam Road Summit New Jersey U S A Descript
18. ished prod uct Vinyl copolymer The vinyl copolymer used in the above example ana lyzed to show hydrogen chloride acetic acid hydrogen and carbon corresponding to a composition of 13 vinyl acetate and 87 vinyl chloride A 2 solution in cyclohexanone has a relative viscosity of 2 5 and should have a mold transparency spread according to the below method of 7 05 cm to 9 0 cm One method for preparing this type of resin is as follows RECIPE Parts by weight Vinvy chloride monomer___ _ 82 1 Vinyl acetate monomer_ _ ____ 17 9 Water ar 222 2 82 na nie ee ahi 220 0 Lauroyl peroxide_ __ ___ 0 35 Aerosol OT sodium dioctyl sulfosuceinate ___ 041 Methocel methyl cellulose 1500_ _ _ 0 12 Carbon tetrachloride_ _ __ 1 0 Trichlorethylene 2_ 22 22 222 1 0 Lauroyl peroxide is the catalyst for polymerization Aerosol OT sodium dioctyl sulfosuccinate and Metho cel 1500 are emulsifying and suspending agents respec tively Carbon tetrachloride and trichlorethylene are chain stoppers by means of which the molecular weight of the product is controlled Method of procedure Vinyl chloride monomer is first freed from any in hibitor phenol or substituted phenol by washing with 3 005 791 caustic soda It is then dried to free it from any caustic soda or sodium phenolate preferably by distillation The water lauroyl peroxide Aero
19. l line for ease of measurement 3 005 791 i 9 i 6 x 6 x 46 Transite boards and two steel wire mesh screens are supplied with the heat platens to separate and insulate them from the main frame of the press The cold press platens with provision for water cooling may be obtained from the supplier RELATIVE VISCOSITY The relative viscosity figure gives a means of compar ing one resin with another It provides a relative indi cation of the average molecular weight of the resin the hardness or the softening temperature All these val ues increase with increasing relative viscosity Apparatus a Ostwald Fenske Pipette Viscometer size 100 Fisher Cat No 13 616 b Fisher Unitized Kinematic Viscosity Bath Fisher Cat No 13 619 1 c Water Bath Clamp Fisher Cat No 15 445 80 d 50 mil Erlenmeyer Flask with glass stopper Fisher Cat No 10 098 e Stop watch f Analytical balance g Torsion balance A 50 ml beaker i Fritter disk filtering funnel Fisher Cat No 10 359 M50 j Mechanical Shaker Will Corp Cat No 23775T k Suction bulb with tube cork assembly for filling pipette 1 Acetone washed filter paper coarse Procedure and calculations Weigh a 1 0 gram sample of the vinyl copolymer resin to the nearest 0 5 milligram on a tared paper analytical balance Transfer the sample to a 50 cc glass stoppered Erlen meyer flask and weigh the flask plus resin on a torsio
20. mputed as follows Solution efflux time Relative viscosity Solvent efflux time Precautions A vacuum line or syringe bulb should be used for 10 15 20 25 30 35 40 45 50 55 60 65 70 75 10 suction and in pipetting cyclohexanone and test solutions Take great care to keep pipettes and solution flasks scru pulously clean and filter all cyclohexanone and resin test solutions through a clean fritter disc filter as viscosity measurements are very sensitive to contaminants and dirty equipment If the regular cleaning procedure is not adequate the pipettes and flasks may be cleaned readily in boiling cyclohexanone Having thus described certain embodiments of the in vention what is claimed is 1 A grease resistant floor tile composed of a be tween about 18 5 and 25 of a solvent soluble or ganic binder consisting essentially of 1 a chlorinated paraffin containing between about 45 and 60 of chio rine and having a melting point of about 15 C to 55 C and 2 a copolymer of about 87 to 90 vinyl chlo ride and 13 to 10 vinyl acetate in the proportions of from about 1 5 to 4 parts by weight of the chlorinated paraffin to t part by weight of the copolymer and b between about 81 5 and 75 of inorganic fillers 2 A grease resistant floor tile as defined in claim 1 in which the organic binder consists essentially of about 3 parts of 1 a chlorinated paraffin containing between
21. n balance Add 15 cc of cyclohexanone slowly and gently swirling to prevent gel formation Add cyclohexanone to bring the total cyclohexanone to 49 grams Place on the mechanical shaker for 6 hours or until the resin is completely dissolved undissolved gel particles can be detected when the flask is held up to a strong light Remove the flask filter the 2 solution through the ace tone washed filter paper Determination of relative viscosity Invert the small capillary tube of the Ostwald pipette into the filtered test solution and by means of the suc tion bulb assembly fill the tube to the calibration mark nearest to the large reservoir bulb of the pipette Place the filled Ostwald pipette in an upright position in a 25 C water bath using care to insure that the capillary tube is vertical the pipette is immersed above the upper cali bration mark and the bath temperature is correct within 0 1 C Allow test solution to stand in pipette for at least 10 minutes to reach equilibrium temperature Suck the sol vent into the small bulb above the capillary Release the suction and measure the time elapsed required for passage of the meniscus between the two calibration marks with a stop watch Repeat the measurement until at least two checks 5 seconds are obtained After each sample is run the pipette should be cleaned by rinsing with acetone blowing with air and drying at 80 C for 10 minutes The relative viscosity is co
22. s Sometimes it is helpful to use ultra violet light as a catalyst for the re action but this is not absolutely necessary Chlorina tion is continued over such time as is necessary and always with violent agitation so that each molecule can be conceived to have been subjected to the same degree of chlorination as the others in the mass Chlorination is continued until a given viscosity softening point specific gravity or chlorine content is reached Either or all of these methods of tests may be employed al though quick tests such as specific gravity or softening point are usually preferred to the longer tests such as percent chlorine in controlling the reaction The re sultant product is now freed from hydrochloric acid gas by blowing with dry air by subjecting to vacuum or by a combination of the two Local overheating is avoided by heat exchange control during the process so as to circumvent decomposition Temperatures used may vary over a wide range Com pletion of reaction is a time temperature function and the higher the temperature which is used the higher the rate of chlorination provided that the temperature does not exceed the point where decomposition begins Gen erally the practical temperature limitations of these ma terials are between 80 C and 125 C As the chlorina tion proceeds the viscosity increases so it is desirable to maintain as high a temperature as possible towards the end of the reaction per
23. sistant floor tile consisting essentially of 1 a chlorinated paraffin containing between about 45 and 60 of chlorine and having a melting point of about 15 to 55 C and 2 a copolymer of vinyl chloride and vinyl acetate in the proportions of about 87 to 90 vinyl chloride and 13 to 10 vinyl acetate in the proportions of about 1 5 to 4 parts by weight of the chlorinated paraffin to 1 part by weight of the copolymer 8 A grease proof composition as defined in claim 7 consisting essentially of 1 a chlorinated paraffin con taining between about 54 and 58 of chlorine and 3 005 791 11 12 having a melting point around 42 C and 2 a copoly References Cited in the file of this patent mer of about 87 vinyl chloride and 13 vinyl acetate UNITED STATES PATENTS in the proportions of about 3 parts by weight of the chlorinated paraffin to 1 part by weight of the copolymer 2 421 409 Brookman et al __ June 3 1947 9 A grease proof composition as defined in claim 7 5 2 428 282 Kemmler Sept 30 1947 consisting essentially of 1 a chlorinated paraffin con pe ae mm nn e as taini bout 52 5 of chlori d having a melti 4333 an BUEN rr mm V 2 aiming avou o of cnlorine an aving a memg 2 563 593 Ebola es eee Aus 7 1951 point of around 15 C and 2 a copolymer of about 90 vinyl chloride and 10 vinyl acetate in the propor i FOREIGN PATENTS tions of about 60 of the chlorinated paraffin to 40 10 611 300
24. sol OT Methocel 1500 carbon tetrachloride trichlorethylene and vinyl acetate monomer are previously co incorporated in an agitated charging tank They are then transferred to an agitated glass lined autoclave The air space in the re actor is purged and the vinyl chloride monomer intro duced under pressure from a weigh by difference pressurized weigh tank Agitation is started and the temperature is gradually raised to 55 C by means of a hot water charging jacket on the autoclave Pressure at this point builds up to slightly over 100 p si Reaction is maintained at this pressure until complete as indi cated by the falling pressure When a pressure of 16 p s i is reached the reaction is terminated and the time required is 9 to 10 hours The vessel is vented and the liquid charge dropped into a receiving tank The product is now dewatered and rinsed in a centrifuge and dried at low temperature to produce a fine white powder The form of vinyl polymer is that of a rather finely comminuted powder In order to obtain the particular properties desired in this particular instance a ratio of 3 08 parts of the chlorinated hydrocarbon per part of vinyl polymer was used and at this dilution of the vinyl resin it is extremely important that substantially all of it be dissolved in and be permanently and completely co miscible with the chlorinated paraffin Therefore it is frequently desirable to associate the resin and the chlorinat
25. vidual preference and expediency However either before or at the time of the incorpora tion into the flooring batch chlorinated paraffin as well as the vinyl polymer must be stabilized against decom position The amount of stabilizer to be incorporated depends a great deal upon the composition of the batch itself and it is a well known fact that if alkaline earth metal carbonates such as calcium magnesium or a com bination of the two be used as a large portion of the filler then the amount of other stabilizers required is diminished The above specified properties of the chlorinated paraffin as well as the process for making it may vary within quite wide limits For instance if the chrage stock used had been of an average composition of CosHee the amount of chlorine required to bring it to a melting point of 42 C wouid have been less by about 4 eg about 54 chlorine and as a result the specific gravity of the material would have been some what lower Conversely had the hydrocarbon charged stock been of the order of CysH32 42 C melting point would probably not be achievable within the range of practical chlorination Likewise 42 C melting point is not a specific requirement but either a lower or higher melting point chlorinated product may be used de pendent upon the type and amount of vinyl polymer with which it is to be associated and depending upon the de gree of hardness or softness desired in the fin
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