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Feb. 23, 1965 M. S.

BARBOUR 3,170,809
Filed May 4, 1962

FIG. 1


FIG. 2




BY é%zº.

If the needle nongreasy transferred coating and also with respect to penetrates the wax to a depth of 0. when a volatile base is employed in these 35 Duroxon (a trademark for a light colored oxidized type coatings in place of potassium hydroxide. etc. and the like. they are parts of a 35% dispersion of carbon black. for example. 117–36. linoleic acids. assignor to Oxford Paper Company. the transfer sheets of this invention are pre 20% wax emulsion. 30° F. a volatile base. such defined. . 2. above its melting point and then cooled to 770 F. the rating the ease of transfer of the coating. Preferably. Apparently. of 60 amounts of pigment can also be used. morpholine. . and particles are readily transferred in response to local has the required degree of hardness and so long as its pressure. The volatile bases which can be used according to this which can be used depends upon the particular resin used and upon the various other ingredients of the wax emul invention are capable of being reacted with a fatty acid sion. for example. base with a wax emulsion containing dispersing agents such defines a class of waxes which is characterized by a par as alkali metal soaps. based on the amount of the wax plus fatty acid. and include such waxes as montan. Various non-film-forming resins have been em under emulsion forming conditions to form a fatty acid 70 soap suitable as a dispersing or emulsifying agent. previously known transfer sheets. Ser. film-forming dispersion. filed August 28.809 Pa?ented Feb. linked by 4 nitrogen layer so that the transferred image is strong and sharply 50 atoms to form a conjugated chain).6-dimethyl Marshall S. and so forth. Amine ployed in amounts up to about 10% by weight and above. It is known from United States Patent No. Additives such as additional dispersing agents.156. N-ethyl morpholine. - a hard wax in admixture with a fatty acid and a volatile The ability of the transfer coating to become deactivat ed by application of heat to the coating is enhanced by in base. and thereafter hardening the coat palmitic. etc. 1961. The hard waxes which can be used control of the hardness or brittleness and smudge resistance from 0 to toabout of the wax film. usually by temperatures above by American Cyanamid Company). stearic. the needle penetrates the wax to a depth of 0. and drying corporating the coating. such as. Examples of such fatty acids are oleic. Local pressure applied to these depth to which a weighted needle penetrates a sample transfer sheets effects a transfer of the coating to an of wax.H. such as a dye or into the wax emulsion a small amount of a non-film-forming thermoplastic resin. the use of a volatile base in these wax coatings enables better isaccording 8.327 mine. This invention relates to transfer sheets and the method The fatty acids which can be used are those which are of making same. can advantageously be used along with 29. - Broadly. 1962. to applied to the wax sample for 5 seconds. The wax globules are in intimate contact with physical properties are not adversely altered when the each other but are non-coalesced. leav carnauba.N-dimethyl isopropanolamine. or non-film forming thermoplastic resins can dry the coating. These soaps are generally prepared 20 ticular degree of hardnes as determined by the so-called by reacting a fatty acid with an alkali such as sodium or Penetration Test. No. phthalocyanine pigments (organic pigments which have a structural unit of 4 removable in the form of an image. can advantageously be incorporated into the . emulsion is dried. Moreover. Acrylic soaps made from volatile bases are examples of emulsify polymers (manufactured by Rohm & Haas under the trade . all or part of the fatty acid is blended with the melted This application is a continuation-in-part of applica wax and the blend is then added to a hot solution contain tion Serial No. and any remaining portion of fatty acid.752 In forming the wax emulsion of this invention. Livermore. of synthetic Fischer-Tropsch hydrocarbon wax. the smudge resistance of the sheet is high. 23. Germany). (CH. . although and the like. ing the wax particles in such a physical state that. N. The wax sample is melted by heating it to about underlying sheet. particularly with re spect to the sharpness of outline of the relatively dry. The about 190° F. manu factured by Krupp Kohlenchemie G. now 15 ing water. The term “hard wax. 192. carbon black. The amount of non-film-forming resin also be incorporated in the dispersion. Calcotones (highly dispersed pigment pastes manufac tion resides in the ability of these sheets to be deactivated tured by application of heat. ing on to the base sheet. The depth which the needle penetrates the wax during the 5 the resulting transfer sheets are considerably superior to seconds time interval is measured in tenths of a millimeter. for about 5–10 seconds. for example. 65 will not formresins” as used herein refers to resins which films at the temperatures used to apply and solvents. 1965 1 2 3.N-diethyl ethanolamine. 134. The Penetration Test measures the potassium hydroxide.b. emulsifiable. Am TRANSFER SHEET AND PROCESS OF MAKHNG monia. this invention are those which have a rating 6. coating the emulsion to a suitable base. the wax 40 vegetable. N.N-dimethyl ethanola Filed May 4.. Barbour. The non-coalesced nature of the wax layer weakens the coherence within this isoindole groups. wax and a volatile base.809 ing agents which can be advantageously employed.m. (C6H4)C3N.931. and more particularly to transfer sheets generally used in the art to prepare emulsifying agents for prepared by coating a suitable base sheet with a coating waxes and these can be readily determined by one skilled composition comprising an aqueous emulsion of a hard in the art. the volatile base is driven off as the coating is dried. as Aquablak (a carbon black and a bone black aqueous A further advantage of the transfer sheets of this inven dispersion marketed by Columbia Carbon Company).2 milli the hardness rating of the wax is 2. abandoned. Three capable of only a very faint transfer. the color desired. Moreover. and tend to remain on the surface of the sheet rather than penetrate the sheet. 30 Ifmeter. Coatings which 55 amount of pigment employed wil depend upon the type are deactivated in such a manner are permanently set and of pigment being used. 2. Considerably higher or lower pared by forming an aqueous dispersion.” as used herein. potassium hydroxide in conjunction with a hand wax. N. . 2-amino-2-methyl-1 5 Claims. under a load of 100 grams. It has now been found that when a volatile base is em The hardness of the wax is measured with a penetrometer ployed instead of such non-volatile bases as sodium or 25 iswhereby a standard needle. Suitable coloring matter. a hard that transfer sheets can be prepared by coating a suitable wax is employed.4) propanol. . The wax may be a petroleum. United States Patent Office 3.170. The term “non pigment. a corporation of Mai?ie morpholine. It is likely that the physical state of the coating is such 45 Various are coloring agents such as organic or inorganic that there is formed a fragile transfer layer of Wax pigments advantageously incorporated in the wax weakly adhered to the surface of the base but efficiently emulsions.8 millimeter. and the like are some examples of volatile bases which can be used. Maine.170. N-methyl morpholine. synthetic or a mineral wax or a combination of waxes so long as the wax is stable.6 parts of a highly resistant to Smudging. or emulsion.

The release coatings are particularly helpful where the oleate solution (containing 1. mers. This fatty acid could probably be within the range of from blend was then added. part or all of the fatty acid is blended with the melted wax and Example II the blend is then added to a hot solution containing wa 30 A transfer sheet having a Mylar base was prepared as ier and a volatile base and the ingredients vigorously follows: 50 parts of Duroxon J–324 wax and 1. 3. based on the wax. and 0. Such a receptor paper com were heated to a melt and blended.. The ingredi transfer coating. 79. receptive properties for the transfer coating. This blend was then added. 5 based on the total weight of the emulsion.75 part of tonate coating composition described in application Serial oleic acid were heated to a melt and blended.980. cording to this invention adhered to the release coating. and dried.05 parts oleic acid) and 150 parts water. attapulgite clay. The 7:1 and 2:1. Higher amounts could be A wax emulsion coating composition was prepared as used however. The wax emulsions of this invention are prepared by Chemicals mixed Corp. at a temperature of 220–230° F.5 parts of oleic heated to a melt and blended together. The receptor paper is described in my copending Example IV application Serial No. and 0.0 parts of montan wax and 1. for 5 seconds were found to be substan adhered thereto and the transfer coating 22 prepared ac tially deactivated and smudge proof. with the transfer coating of this application whether a re Example V lease coating is used under the transfer coating or not. such as an amount chemically equiv Example I alent to that of the fatty acid. The com 20 with stirring. 3. and coated on a sheet of then thoroughly fer coatings of this invention can be improved by apply ing a suitable release coating to the base sheet prior to the Example III application of the transfer coating.029. Parts are by weight. 0.34 parts NH3 and 3. receiving the transferable image from the transfer coat ing.S. The emulsion was then applied to a paper raw stock The invention includes the use of a receptor paper for base and dried. 2 shows a paper base 20 with a release coating 21 ample.80 part aqua ammonia.. at a temperature of 220–230° F.980 and then coating the other surface with the was then added.62 parts morpholine.. Advantageously. to a solution (at 210" F. cooled.0 parts ammonium oleate of between about 2 and 6 in admixture with an adhesive 60 solution and 140 parts water. rapidly to below 150° F. etc. The cal stirring. Thus two sheets can be placed together ents were vigorously agitated and the resulting emulsion so that the transfer coating of one sheet is in contact with cooled. to a solution (at 200° F. The emulsion is then applied to a suitable base of oleic acid were heated to a melt and blended. This amount of acid were32. and assigned to the same as follows: 32 parts of Duroxon J–324 and 8 parts toluene signee as this application. The emulsion was then applied to a paper raw the receptor coating of the other sheet so that when local stock base and dried. The ingredients were receiving base or paper does not have particularly high vigorously agitated and the resulting emulsion cooled. sodium stearate. 79.. This blend No.80 parts of the wax a thin plastic film such as cellophane. The following examples show the manner in which the the proportion of the various ingredients is not particular transfer sheets and the coating compositions employed in ly critical. 0. hydroxyethyl cellu then lose. an intensely .1 parts ammonium hydrated alumina.63 part oleic acid. about 3 to 10% or even beyond this range. The ingredients were supporting medium.809 4. filed January 3. pressure is applied to the transfer coating.782. now 55 A wax emulsion coating composition was prepared as U. to a solution (at 200° F.) of 130 parts wa bined weight of the wax and the fatty acid in the aqueous ter and 4. Advantageously. at a temperature of 220–230° F.25 cium carbonate coating acts as a receptor coating for the part oleic acid. 3. 0. with stirring. at a temperature of 220–230° F. and dried preferably at a temperature below the fusion with stirring.87 parts other additives can then be added and thoroughly ad mixed.05 parts of a carbon polyethylene terephthalate such as manufactured by Du Pont under the trade name Mylar or any other suitable 40 black in the form of a dispersion. The most suitable amount of each ingredient this invention can be made. These examples are given which can be used can readily be determined by one skilled by way of illustrating and are not intended in any way to in the art. and polystyrene polymers are examples of non-film FIG. Significantly improved transfer properties emulsion was then applied to a paper raw stock base and are obtained by using such a receptor sheet in conjunction dried. This blend was then prises a base sheet on which is coated a dispersion of cal added. sodium silicate and so forth. name Rhoplex) a at a temperature of 220–230° F. For example. used is advantageously only as much as is needed to react with the fatty acid. The base sheet which is coated with the wax emulsion The emulsion was stirred a few minutes and then cooled described above can be either a coated or uncoated paper. with stir solution (at 210° F. about 5% by weight of follows: the fatty acid.) of 84 parts water. parts water. vinyl chloride-vinylidine chloride copoly clear point image is transferred to the receptor coating at the at which the pressure was applied. Transfer coatings which are made from such resin hered to the paper base.).0 parts of Duroxon J–324 and 0.170. to cium carbonate having a relative sedimentation volume a solution (at 210° F. containing emulsions and which have been heated to. Of course.) of 127 parts wa temperature of the wax. In forming the coating composition of this invention. Patent No. or a thin film of emulsion thus formed was added 1. 1 shows a paper base 10 having a transfer coat forming resins which can be incorporated in the wax emul ing 11 prepared according to the present invention ad S?OilS. The ingredients were thoroughly together. the amount of volatile base limit the scope of the invention. ring. ter.6parts parts of the wax Aquablak. standard emulsifying techniques..30 part of 28% ammonia. magnesium aluminum silicate. A particular embodiment of the invention involves coat A wax emulsion coating composition was prepared as ing one surface of the base sheet with the calcium car follows: 20. Examples of release A wax emulsion coating composition was prepared as coatings which can be used include colloidal silica such follows: 32 parts of Duroxon J–324 and 6 parts of oleic as that marketed by Monsanto under the trade name acid were heated to a melt and blended.05 Pluronic L-62 (a nonionic a higher or lower proportion of the wax-fatty acid com active agent prepared by the addition of ethylenesurface oxide ponent may be employed depending upon the various in to polypropylene glycol and manufactured by Wyandotte gredients used in the emulsion. with wax emulsion transfer coating described above. wax emulsion is advantageously around 20% by weight emulsion thus formed was addedTo3. is used.) of 24. This blend was Syton.118. ex FIG. acetylated Starch. The transfer properties of the trans Mylar. The ingredients were vigor and in which the pigment-adhesive ratio is between about ously agitated and the resulting emulsion cooled. To 18. 1961. added. 360° F. coated on paper base and dried.) of 12.

Additional transfer sheets 1.0 parts of Calcotone Orange R was thoroughly admixed with 22. containing a non-film-forming resin were prepared as fol 2.. for 5 seconds. The coating transferred as prepared according to Examples III–V.Apr.222 Statham -------------.931. and a volatile base which is reactive with Transfer sheets prepared from a coating composition the fatty acid.209. The 4. L–62 and 1. Apr. the transfer sheets prepared as set forth in Examples I–IX were also tested using a receptor paper as defined in co Example VII pending application Serial No.Dec. 1. . 5. The method of preparing a transfer sheet which com cording to Examples III-V.77 part of carbon black and 0. Transfer sheets prepared according to the method emulsion thus formed was applied to a paper base and of claim 2. 15 a fatty acid. When the resulting transfer sheet was heated at 5. 1944 Clark -----------------. and I0 I claim: 5. 10. and thereafter drying the coating. 5.05 part Pluronic incorporated into the wax emulsion. the transfer of the image was con siderably improved. 1936 acrylate in place of the polystyrene polymer. positionprises coating a suitable base sheet with a coating com applied to a paper base and dried.809 6 Example VI of ?—IX were tested by placing the transfer coating in A coating composition was prepared as follows: 10. such as prepared according to Examples III-V. applied to a paper base and dried.266. dried. substantially non-transferable.2 parts of Calcotone Scarlet YP.351. 1934 were made according to the above procedure using a poly 2.956 Kniffler ---------------.112 Rafsky ----------------. lease coating and coating on top of the release coating a Example IX composition comprising an aqueous emulsion of a hard wax.Mar. comprising an aqueous emulsion of a hard wax. 1946 application of heat of 360° F. The emulsion readily in areas co-extensive with the pressure.992 Hughes et al. . 3.1 part and in each instance. ----------.6 parts of a wax emulsion such as prepared ac 1. 1. became deactivated and sub 1. 1920 for 5–10 seconds. and a volatile base which is reactive with the Example VIII fatty acid. 1960 transfer sheets prepared in accordance with the Examples . The method of claim 1 in which coloring matter is lows: 1 part Aquablak B.170. 0.188 Ohashi ----------------. The method of preparing a transfer sheet which 360° F. Jan.374. a fatty acid.328. containing a non-film-forming resin were prepared as 30 follows: 0.954. 2 parts water. 31.4 parts vinyl chloride-vinylidine chloride co 20 3. 79. ---------. the sheet became deactivated and comprises coating a suitable paper base sheet with a re.June 20. 5. the sheet.0 parts of a wax emulsion such transfer coating adhered thereto. All of was cooled.768 Sherman et al.5 parts of a wax emulsion is carbon black. All of the 2. for 20 seconds.451 Lawrence -------------. 13.0 contact with a sheet of paper and pressure applied by parts of a 2% phthalocyanine blue dispersion was thor means of a stylus to the backside of the paper having the oughly admixed with 27. The result ing transfer sheets became considerably deactivated after 40 2. The method of claim 2 in which the coloring matter polymer were admixed with 27. 1921 stantially non-transferable. 1918 When the resulting transfer sheet was heated at 360° F.035.683 2.980 referred to above A coating composition was prepared as follows: 0. and thereafter drying the coating on to the Transfer sheets prepared from coating compositions base sheet. 35 1.752 Newman ---------------.May 21. 19. 1.4 part of poly References Cited in the file of this patent styrene polymer was admixed with 20 parts of a wax UNITED STATES PATENTS emulsion such as prepared according to Examples III-V. Apr. The emulsion was cooled. of Pluronic L–62.395. 1916 The emulsion thus formed was applied to a paper base.Mar.

.hardness . Coloring matter.. 1ine 37.forming resins. Barbour 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. February 23.77° F. for 770 F..– . before "ex-" insert -. for "Germany" read -. non-film. before "other" insert -. column 3.. Signed and sealed this 20th day of July 1965.– hard .agitated. EDWARD J.. 3. UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No..i. or -. for "illustrating" read -.11ustration -.West Germany . line 31. same column 2. line 27. for "hand" read . -.. " read -. line 19. 1965 Marshall S.– . Column 1. (SEAL) Attest: ERNEST W. 1 ine 5. SWIDER . for "hardnes" read -. line 12. 809 . BRENNER Attesting Officer Commissioner of Patents . 170.for . column 4. 1ine 23.