US2784089A - Light sensitive diazotype compositions containing silica pigment - Google Patents

Light sensitive diazotype compositions containing silica pigment Download PDF

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Publication number
US2784089A
US2784089A US381977A US38197753A US2784089A US 2784089 A US2784089 A US 2784089A US 381977 A US381977 A US 381977A US 38197753 A US38197753 A US 38197753A US 2784089 A US2784089 A US 2784089A
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United States
Prior art keywords
silica
sensitizing
light sensitive
solution
compositions containing
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Expired - Lifetime
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US381977A
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English (en)
Inventor
Joseph E Frederick
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GAF Chemicals Corp
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General Aniline and Film Corp
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Application filed by General Aniline and Film Corp filed Critical General Aniline and Film Corp
Priority to US381977A priority Critical patent/US2784089A/en
Priority to GB1744/54A priority patent/GB762117A/en
Priority to FR1096744D priority patent/FR1096744A/fr
Priority to DEG14392A priority patent/DE950767C/de
Priority to CH333207D priority patent/CH333207A/de
Application granted granted Critical
Publication of US2784089A publication Critical patent/US2784089A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00—Photosensitive materials
    • G03C1/52—Compositions containing diazo compounds as photosensitive substances
    • G03C1/60—Compositions containing diazo compounds as photosensitive substances with macromolecular additives

Definitions

  • the present invention relates to light sensitive diazotype materials, and especially to the use of a particular form of finely divided silica dispersed in the sensitizing solutions for said materials in order to enhance the density of the dye images produced in such materials.
  • the manufacture of the usual light sensitive diazotype materials involves the application to a fibrous base, such as paper, of a sensitizing solution containing as its main ingredients a light sensitive diazonium compound and an azo dye coupling component. In the processing of such materials they are exposed to light under a pattern to decompose the light sensitive diazonium compound where the light is transmitted by the pattern. Subsequently, a positive dye image is formed by coupling residual diazonium compound and azo coupler in an alkaline medium, preferably ammonia gas.
  • the bases are generally fibrous in nature and the sensitizing components are applied thereto from an aqueous solution. Consequently, the components of the solutions strike into the base, thereby reducing their availability to the exposure light. In addition, by so striking through, they produce an image of low density and a sensitized material with a low printing speed.
  • Jahoda U. S. P. 2,433,515, observed a somewhat analogous problem in connection with the manufacture of blueprint paper.
  • Jahoda proposed as a solution the precoating of a sized paper with colloidal silica followed by application of the blueprint sensitizing solution. While this procedure is satisfactory for the blueprint industry, it is not for the diazotype industry, and this was admitted by the owner of the Jahoda patent in its publication entitled Reproduction Paper Coating, H. P. Andrews Company, printed by J. E. Weiss & Son, Inc., New York, New York, 1951. This publication, on page 7 in discussing the precoat process of Jahoda states:
  • the precoat processes for direct process paper are based on similar physical principles as the one for blueprint paper. Colloidal silica can also be used for direct process paper, but it has some disadvantages. Much better materials for precoating direct process papers are copolymers of synthetic resins in colloidal water solutions.
  • the colloidal silica itself penetrates the base to a considerable depth, and because of its affinity'forthe sensitizer it carries the same into the base with it.
  • .colloidal silica as available in aqueous dispersions, has
  • the silica is free from, iron, is essentially 99% silicondioxide and has a particle size ranging from .015 to .020 micron.
  • Said silica is manufactured by a high temperature decompositionof a siliceous material ina gaseous medium which insures spontaneous formation of the silica in said medium.
  • Various methods have been worked out. for securing this result.
  • One such method involves the burning of a siliceous material, such as silicon tetrachloride in an atmosphere of hydrogen to effect very rapid formation of the silicon dioxide in a small particle size in a gaseous atmosphere.
  • the same result may be effected while utilizing ethyl silicate as the parent material and air as the gaseous atmosphere.
  • Silica made in this fashion is available from G. L. Cabot, Inc., Boston, Massachusetts, under the trademark Aerosil.
  • Another method involves dissolution of a silicate in a
  • This'method involves adding dilute sodium silicate to.
  • the silica is easily added to the sensitizing composition in the form of a dry powder. It is then dispersed by high speed agitation or the like until the resulting composition is homogeneous. Conversely, the silica may be dispersed separately by slurrying with water or with a small portion of the sensitizing composition to produce a thin, uniformly homogeneous paste which is then added to the slurry of the sensitizing composition with stirring.
  • the quantity of the silica which is added amounts to about .5 to by weight of the sensitizing composition. Best results, however, are obtained when the silica is present in a concentration of 2.5% to 6% by weight of the sensitizing solution.
  • the sensitizing solution is applied to the base material by any convenient means, as for instance, roller application, spraying, brush coating or the like. Care must be taken, however, to insure that the excess is doctored off, either with an air knife, doctor blade or similar means.
  • diazos are those derived from N,N diethyl p phenylenediainine; N benzyl N- ethyl p phenylenediamine; N ethyl p phenylenediamine; N phenyl p phenylenediainine; N,N diethyl- 2 cthoxy p phenylenediamine; N ethyl 2 methylp phenylenediamine; N,N bis( ⁇ 3 hydroxyethyl) pphenylencdianiine; N-e-hydroxyedtyl-N-methyl-p-phenylenediarnine and the like. According to customary procedure these diazos are used in the form of salts stabilized with zinc chloride, tin chloride, cadmium chloride and the like.
  • any of the usual coupling components are satisfactory for my purpose.
  • couplers are 2,3-dihydroxynaphthalene; l,8-dihydroxynaphthalene; resorcinol, octyl resorcinol; p methyl-N-phenylpyrazolone; the amide of oc-resorcylic acid; Z-hydroxynaphthalene-B,6-disulfonic acid; 2,5- xylenol; H acid; acetyl acetanilide; 2,3-dihydroxynaphthalene-G-sulfonic acid and the like.
  • Other couplers are mentioned in the Van der Grinten article supra.
  • the coating solution may also contain the various ad juncts usual in the manufacture of light sensitive diazotype materials. These include metal salts for intensification of the dyestutf image, such as ammonium sulfate, nickel sulfate, zinc chlorideand the like; stabilizing agents such as thiourea, thiosinarnine; naphthalene trisulfonic acid and the like; acids acting to retard precoupling such as acetic acid, boric acid, tartaric acid and the like; hygroscopic agents such as glycol, glycerin and the like; and wetting agents such as saponin, lauryl sulfonate, keryl benzene sulfonate, the oleic acid amide of N-methyl taurine and the like.
  • metal salts for intensification of the dyestutf image such as ammonium sulfate, nickel sulfate, zinc chlorideand the like
  • stabilizing agents such as
  • the base to which the coating solution is applied may be any of those which have been previously suggested for employment in the diazotype field.
  • bases are. high grade all-sulfite paper, rag paper, rayon or cotton cloth, starch filled cloth, partially hydrolyzed cellulose acetate filmbase, regenerated cellulose acetate and the like. 7
  • the pigment contemplated for use herein has many important attributes, some of which are explainable and others of which are inexplicable.
  • the pigment since the pigment is prepared in the gaseous phase, it is easily dispersed due to the high degree. of particle separation and; once properly dispersed remains suspended in the sensitizing solutions without the necessity of agitating orcirculating systems which must'be employed with silica of larger particle, size.
  • the silica does not come into contact with metallic processing equipment, and as a consequence is. almost completely free from contamination with iron, an element which, is extremely detrimental in diazotype materials.
  • a Colloidal silica formed in the liquid phase and employed according to Jahoda and von Glahn and Stanley is highly contaminated with iron.
  • Prints made while utilizing said silica have greatly improved dye density and brightness as compared with prints made according to the process of Jahoda and von Glahn and Stanley. Such prints, moreover, have a desirable matte appearance, possessing excellent pencil tooth in com trasttothe glossy image characteristic of prints obtained who? according to the prior art while using colloidal Silica. Prints produced with the silica described herein, more over, are free from feathering to ink line. Feathering is a common characteristic of prints made while utilizing the colloidal silica of the prior art.
  • sensitizing compositions containing the silica contemplated herein is the possibility of extending diazotype coatings to very desirable bases which heretofore could not be so employed.
  • the inability of the art to use such bases was attributable to a tendency of the bases to repel the coating compositions, for one reason or another, such as supercalendering of the surface, impregnation of the base with hydrophobic materials and the like.
  • the coating of such papers in the past led to little success and in many instances the coating compositions were shed by the surfaces involved to an extent equivalent to the shedding of water by the proverbial ducks back.
  • Bases of the type which I have in mind are, for example, of highly calendered 100% rag paper, particularly when transparentized by use of resinous materials, waterproof tracing paper, tracing cloth ,calendered with hydrophobic lubricants and the like.
  • diazotype materials in which such materials operate as a base, due to the inability of the art to uniformly coat such bases without obtaining a mottled effect, they have been rarely used.
  • the coating compositions containing the silica previously mentioned eliminate the tendency of the bases to repel the coating compositions and to do away with the non-uniform coatings previously obtained.
  • the particular reason why said colloidal silica operates as it does with these particular .surfaces is not known and has not been completely investigated. Conceivably, the phenomenon mentioned is bottomed on a surface abrasion by the silica particles which :renders the surface sufficiently matte in finish so that a smooth coating may be obtained.
  • the silica used herein has :a particle size ranging from .015 to .020 micron, i. e., fit is within the colloidal range.
  • the marked differences in result obtained when using said silica appear to be attributable to some indeterminate physical change which takes place when the silica is laid down with the sensitizing solution. It is my opinion that this physical change involves an agglomeration of the silica particles to a size beyond the colloidal range. explain the diiference in appearance of the prints obtained according to the prior art, on the one hand, and according to my method, on the other hand.
  • Example I A sensitizing solution for black line prints was prepared from the following components:
  • the sensitizing solution was coated on high-grade all sulfite bond paper and dried.
  • the prints made from these coatings had a matte rather than a glossy effect and showed considerable enhancement in density when compared to prints made with the same sensitizing ingredients while employing silica of colloidal or of larger particle size according to prior methods described above.
  • Example II High-grade all sulfite bond paper is coated with a sensitizing solution of the following composition:
  • silica having the characteristics previously stated, is dispersed in the sensitizing solution as in Example I.
  • Example III A high-grade well-sized bond paper is coated with the following sensitizing solution:
  • sensitizing compositions forlight-sensitive diazotype materials comprising an aqueous dispersion of a light sensitized diazonium compound, an-azo dye coupling component and a silica'free from iron'having a particle size ranging from .015 to 0.20 micron, and obtained by rapid high temperature decomposition of a siliceous material in a gaseous medium.
  • compositionas defined in claim 1 wherein the silicais present in-an amount ranging from about .5 to 10% by weight of the sensitizing solution.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)
  • Paper (AREA)
  • Silicon Compounds (AREA)
US381977A 1953-09-23 1953-09-23 Light sensitive diazotype compositions containing silica pigment Expired - Lifetime US2784089A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
US381977A US2784089A (en) 1953-09-23 1953-09-23 Light sensitive diazotype compositions containing silica pigment
GB1744/54A GB762117A (en) 1953-09-23 1954-01-20 Light sensitive diazotype compositions containing silica
FR1096744D FR1096744A (fr) 1953-09-23 1954-01-29 Compositions diazotypes contenant un pigment de silice et sensibles à la lumière, leur procédé d'obtention et leurs modes d'applications
DEG14392A DE950767C (de) 1953-09-23 1954-05-12 Sensibilisierungsgemisch fuer Diazotypiematerialien
CH333207D CH333207A (de) 1953-09-23 1954-05-21 Lichtempfindliche Mischung zur Herstellung von Diazotypiematerialien

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US381977A US2784089A (en) 1953-09-23 1953-09-23 Light sensitive diazotype compositions containing silica pigment

Publications (1)

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US2784089A true US2784089A (en) 1957-03-05

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US (1) US2784089A (de)
CH (1) CH333207A (de)
DE (1) DE950767C (de)
FR (1) FR1096744A (de)
GB (1) GB762117A (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3155511A (en) * 1960-08-26 1964-11-03 Andrews Paper & Chem Co Inc Precoated diazo reproduction paper
US3624021A (en) * 1960-08-10 1971-11-30 Gaf Corp Powdered glass for use in drafting surfaces and in a diazo-type materials
US3915709A (en) * 1973-04-13 1975-10-28 Gaf Corp Backwetting coating for diazo microfilm

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2399687A (en) * 1942-05-29 1946-05-07 Goodrich Co B F Preparation of finely-divided silicon dioxide
US2433515A (en) * 1945-04-18 1947-12-30 H P Andrews Paper Company Method of making photographic paper
US2566709A (en) * 1947-10-30 1951-09-04 Gen Aniline & Film Corp Diazotype photoprinting materials containing colloidal silica
US2577485A (en) * 1950-09-08 1951-12-04 Du Pont Process of making stable silica sols and resulting composition
US2578605A (en) * 1947-11-01 1951-12-11 Goodrich Co B F Surface-treated silica
US2662013A (en) * 1951-07-18 1953-12-08 Gen Aniline & Film Corp Diazotype photoprinting material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2399687A (en) * 1942-05-29 1946-05-07 Goodrich Co B F Preparation of finely-divided silicon dioxide
US2433515A (en) * 1945-04-18 1947-12-30 H P Andrews Paper Company Method of making photographic paper
US2566709A (en) * 1947-10-30 1951-09-04 Gen Aniline & Film Corp Diazotype photoprinting materials containing colloidal silica
US2578605A (en) * 1947-11-01 1951-12-11 Goodrich Co B F Surface-treated silica
US2577485A (en) * 1950-09-08 1951-12-04 Du Pont Process of making stable silica sols and resulting composition
US2662013A (en) * 1951-07-18 1953-12-08 Gen Aniline & Film Corp Diazotype photoprinting material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3624021A (en) * 1960-08-10 1971-11-30 Gaf Corp Powdered glass for use in drafting surfaces and in a diazo-type materials
US3155511A (en) * 1960-08-26 1964-11-03 Andrews Paper & Chem Co Inc Precoated diazo reproduction paper
US3915709A (en) * 1973-04-13 1975-10-28 Gaf Corp Backwetting coating for diazo microfilm

Also Published As

Publication number Publication date
FR1096744A (fr) 1955-06-23
GB762117A (en) 1956-11-21
DE950767C (de) 1956-10-18
CH333207A (de) 1958-10-15

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