CN104062861A - Preparation method for color carbon powder for electrostatic charge developing - Google Patents
Preparation method for color carbon powder for electrostatic charge developing Download PDFInfo
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- CN104062861A CN104062861A CN201410246455.1A CN201410246455A CN104062861A CN 104062861 A CN104062861 A CN 104062861A CN 201410246455 A CN201410246455 A CN 201410246455A CN 104062861 A CN104062861 A CN 104062861A
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Abstract
The invention relates to a preparation method for color carbon powder for electrostatic charge developing, which solves the problem that for an adopted chemical method for preparing the color carbon powder, the agglutination process cannot control easily, the process difficulty is great, and the quality of obtained color carbon powder is unstable. According to the technical scheme, the steps are as follows: dissolving and dispersing a coloring agent, resin and wax in an organic solvent to obtain an organic phase, and shearing and emulsifying the organic phase in water containing a surfactant; then, distilling to remove the organic solvent in the system to obtain particle dispersion liquid with narrow particle diameter distribution, adding an agglutinant into the particle dispersion liquid for agglutinating to obtain color carbon powder matrix; and finally, carrying out the technical processes such as filtering-washing, drying and mixing to obtain the color carbon powder. According to the preparation method, the process difficulty is low, the condensing process can be controlled easily; the particle diameter distribution of the obtained color carbon powder is narrow, the number of small particles is small, the quality is stable and reliable, and the material adaptation is good.
Description
Technical field
The present invention relates to a kind of preparation method for the duplicating machine of electrofax mode and the development of static charge of printer use colored carbon powder.
Background technology
Colored carbon powder is the required important consumptive material of development of static charge color laser printer, colored digital duplicating machine, mainly resin (comprising styrene-acrylic resin and vibrin etc.), colorant (pigment and dyestuff), adjuvant (charge adjusting agent, mould release etc.), consists of.According to the difference of the color of carbon dust colorant used, carbon dust is divided into colored carbon powder and black carbon powder.The traditional preparation method of carbon dust is " comminuting method " (Physical),, operations such as required resin, colorant, adjuvant process melting mixing, low temperature mechanical disintegration, air-flow crushing, classifications, obtains the carbon dust that granularity is about 10 μ m.Yet, the shortcomings such as this preparation method exists the defects such as the high and colorant of energy consumption is difficult for the carbon powder particle size of dispersed in resin, preparation and shape homogeneity is poor, particle diameter is larger, and easy roll banding when causing printing, duplicating, resolution are low, shade deviation, useless powder rate are higher.Take company that Fuji-Xerox (Fuji Xerox) etc. is representative has developed " emulsion polymerization/co-coagulation method " (chemical method) and has prepared colored carbon powder, first prepare respectively resin emulsion, dispersible pigment dispersion, wax dispersion, so resin emulsion, dispersible pigment dispersion and wax dispersion are blended under the existence of agglutinant and make three kinds of particles aggregate prepare colored carbon powder.Because resin emulsion, dispersible pigment dispersion and three kinds of particles of wax dispersion physical property, chemical property and surface nature between separately has larger difference, therefore there is larger limitation to resin, pigment, wax, selecting of surfactant in the method, and realize simultaneously three kinds of even aggegation processes of particle are difficult to control, technology difficulty colored carbon powder quality large, that obtain is unstable.
Summary of the invention
The object of the invention is in order to solve the problems of the technologies described above, the physical property existing while overcoming three kinds of particles aggregate, chemical property and superficiality qualitative difference, provide that a kind of technology difficulty is low, aggegation process is easily controlled, the particle diameter narrow distribution of the colored carbon powder obtaining, small-particle is few, steady quality is reliable, the preparation method to the good development of static charge use colored carbon powder of adaptability to raw material.
Technical scheme comprises the following steps:
1) colorant grinding distribution in containing the organic solvent of spreading agent, add wherein resin and wax heating for dissolving, obtain the organic phase that contains colorant, resin, wax;
2) in the aqueous solution that contains surfactant, add step 1) in the organic phase that obtains carry out high speed shear emulsion dispersion, obtain emulsion fluid;
3) emulsion fluid is removed to organic solvent through distillation and obtain particle dispersion;
4) in this particle dispersion, add agglutinant to carry out aggegation, obtain colored carbon powder parent, then filter washing, dry, mix additive and obtain colored carbon powder.
Described step 1) colorant grinding distribution described in to footpath grain is 50-200nm.
Described step 1), in, heating for dissolving temperature is 40-80 ℃.
Described step 2), in, the particle diameter of controlling tiny oil droplet in emulsion fluid is 400-800nm.
Described step 3), in, in particle dispersion, the particle diameter of particle is 300-700nm.
The present invention by successively dissolving colorant, resin and wax and disperse to obtain organic phase in organic solvent, again this organic phase is carried out in containing the water of surfactant to high speed shear emulsification, then distill the particle dispersion that the organic solvent of removing in system obtains particle diameter narrow distribution, to adding agglutinant to carry out aggegation in this particle dispersion, obtain colored carbon powder parent again, finally by filtration wash, be dried, the technological process such as mixing obtains colored carbon powder.Because colorant, resin and wax form a particle dispersion jointly after dispersion, emulsification and distillation, therefore follow-up aggegation process is the aggegation to a particle dispersion, between particle, not there is not the difference of the aspects such as physicochemical property, thereby aggegation process just becomes and easily controls, technique is simple and stable more, the particle diameter narrow distribution of gained carbon dust, small-particle is few, aggegation process does not have special requirement to the selection of resin, colorant, wax, surfactant, adopts the inventive method good to the adaptability of raw material.
Colorant used in the present invention is not particularly limited, and can be any of inorganic pigment or organic pigment, organic dyestuff, can be its combination yet.The cyan colorant that can enumerate has pigment blue 15: 3, pigment blue 15: 4 etc.; Yellow colorants has pigment Yellow 12, pigment yellow 17, pigment yellow 74, pigment yellow 93, pigment yellow 94, pigment yellow 155, solvent yellow 16 2, pigment yellow 180, pigment yellow 185 etc.; Pinkish red colorant has pigment red 31, pigment red 122, paratonere 150, paratonere 184, paratonere 185, paratonere 57:1, paratonere 238, paratonere 256, paratonere 269 etc.; Black colorant has carbon black, magnetic iron ore, aniline etc.
The wax that the inventive method is used is not particularly limited, and can be the higher fatty acid amides such as natural series wax, oleamide, stearic amide such as the hydrocarbon waxes such as low molecular weight polyethylene wax, low-molecular-weight polypropylene wax, low-molecular-weight copolyalkenamer wax, paraffin, microcrystalline wax, behenic acid 20 diester, stearic acid octadecyl ester, pentaerythrite four behenates, Brazil wax, beeswax etc.
The resin that the inventive method is used is not particularly limited, and can be styrene-acrylic resin, vibrin etc.; The preparation method of resin is not particularly limited, and can be polycondensation reaction, bulk polymerization, suspension polymerization, emulsion polymerization, solution polymerization, melt polymerization or interfacial polycondensation etc.
The organic solvent that the inventive method is used has butane, pentane, hexane, sherwood oil, methylene chloride, methenyl choloride, tetrachloromethane, cyclohexane, benzene,toluene,xylene, methyl alcohol, ethanol, ether, ethyl methyl ether, methyl formate, ethyl formate, propyl formate, butyl formate, methyl acetate, ethyl acetate, propyl acetate, butyl acetate, methyl propionate, ethyl propionate, methyl butyrate etc.
Spreading agent used in the present invention is organic dispersing agent, can be that one or more organic dispersing agents are combined use.Organic dispersing agent comprises the polymkeric substance that contains the groups such as amido, ammonium, carboxyl in long-chain alkyl alcohol, chain alkyl acid, chain alkyl amine, chain alkyl acid amides, structure.
Surfactant used in the present invention can be anionic surfactant, cationic surfactant, non-ionic surfactant.Cationic surfactant has DTAC, DTAB, dodecyl chlorination pyridine, dodecylpyridinium bromide, hexadecyltrimethylammonium chloride, cetyl trimethyl ammonium bromide etc.Anionic surfactant has the slaine of the higher fatty acid such as odium stearate, sodium laurate, sodium dodecylsulphonate, neopelex, lauryl sodium sulfate etc.Non-ionic surfactant has polyoxyethylene ten diether (Poly (oxyethylene) Dodecy Ether), polyoxyethylene margaron (Poly (oxyethylene) Hexadecyl Ether), polyoxyethylene nonylplenyl ether (Poly (oxyethylene) Nonyl-Phenyl Ether), Poly (oxyethylene) polyoxyethylene octadecyl ether (Lauryl Ether), polyoxyethylene ether sorbitan mono-oleic acid ester (Sorbitan Mono-oleate Poly (oxyethylene) Ether), CT-1695 (monodecanoate Sucrose) etc.
Agglutinant can be used the salt of 1 valency or multivalence.Specifically, 1 valency salt can be enumerated sodium salt, sylvite etc., such as sodium chloride, potassium chloride etc.The salt of divalent can be enumerated magnesium chloride, magnesium sulfate, lime chloride, calcium sulphate etc.The salt of 3 valencys can be enumerated aluminium hydroxide, aluminum chloride, aluminium sulphate, sodium phosphate, potassium phosphate etc.
Described additive can be enumerated the micropowders such as hydrophobic monox, titanium dioxide, aluminium oxide, cerium oxide, strontium titanates, resin microsphere, and addition can be with reference to prior art.
In technological process of the present invention, described step 1) in, the preferred grinding distribution of colorant to particle diameter is 50-200nm, and the particle diameter of dispersion is crossed the coloration efficiency reduction that conference causes colorant, and too small meeting causes the meticulous colorant of particle diameter to cause not colouring power not high to the reflection potential of light.
Described step 1) in, heating for dissolving temperature is preferably 40-80 ℃, in this temperature range, wax can be dissolved in the organic solvent that contains resin, colorant preferably, the too low meeting of temperature causes wax not to be dissolved in organic solvent preferably, thereby excess Temperature can affect the performance of some surfactants, emulsification pretreatment process is produced to adverse influence.
Described step 2) in, the particle diameter of controlling tiny oil droplet in emulsion fluid is preferably 400-800nm, in the time of within the scope of this, the particle of removing in the particle dispersion of organic solvent is more consistent aspect composition, aggegation can easily be carried out, when oil droplet size is too small, the particle diameter of particle dispersion may be almost big or small with the particle diameter of colorant particle, there will be single colorant particle, thereby aggegation is exerted an influence; When oil droplet size is excessive, the particle diameter of particle dispersion can be larger, and the particle number needing while causing aggegation to the carbon dust of required particle diameter is less, thereby make aggegation process relatively be difficult to control.
Beneficial effect:
1, the present invention is the resin that forms carbon dust, pigment, wax dissolves dispersion in organic solvent, in water, emulsification finally obtains the particle dispersion night that nano level composition is single again, in this particle dispersion, contain resin simultaneously, pigment, the nano particle of wax, rather than prepare respectively the dispersion liquid of three particles, technological process of the present invention has determined that each particle of this nano particle has identical structure and composition, between each particle, identical structure and composition makes aggegation process be more prone to control, avoided in " emulsion polymerization/co-coagulation method " respectively to resin emulsion, wax dispersion, during three kinds of particles aggregate of dispersible pigment dispersion due to the chemical property of three kinds of particle surfaces, aggegation that the difference of physical property causes is inhomogeneous is the infull problem of aggegation.Preparation technology is simple, reliable, easy operating, the colored carbon powder steady quality of preparation, narrow diameter distribution, and bottom ash, useless powder rate, consumption are lower, have excellent developing performance.
2, the inventive method is wider to the selectivity of raw material, and resin used can be that styrene-acrylic resin can be also vibrin, and the preparation method of resin can be any method in known process for preparing resins; More extensive compared with " emulsion polymerization/co-coagulation method " to the selectivity of pigment, wax, surfactant, applicability is good.
Embodiment
Carbon dust preparation example 1
In grinding pot, drop into the ethyl acetate of 400 parts, 74,0.56 part of spreading agent DISPERBYK-163 of pigment yellow of 5 parts (German Bi Ke chemistry, BYK-CHEMIE), stir, use ball mill grinding 5 hours, with nano particle size instrument, recording pigment particle size is 120nm; The dispersible pigment dispersion of milled is dropped in stirred pot, in tank, drop into 85 parts of styrene-acrylic resin (Mn=23040, Mw=58000, Tg=62 degree) and 10 parts of Tissuemat E POLYWAX400 (Bake Hughes, BAKERHUGHES), be warming up to 65 degree and stir and to dissolve completely for 50 minutes, obtain the organic phase that contains resin, pigment, wax, solid content is 20%.
In stirred pot, drop into 15 parts of lauryl sodium sulfate, 750 parts of water, being warming up to 65 degree stirs, under 15000rpm rotating speed, with HOMOMIXER, (compose Lai Mikesi, PRIMIX) homogeneous surfaces activating agent aqueous solution, in stirred pot, drop into organic phase, homogeneous 40 minutes, obtains emulsion fluid, and the particle diameter that records tiny oil droplet in emulsion fluid with nano particle size instrument is 512nm; Be warming up to 80 degree, distill out the ethyl acetate in emulsion fluid, be cooled to room temperature and obtain the particle dispersion that contains resin, pigment, wax, the particle diameter that records particle with FPIA-3000 is 420nm, and the solid content of particle dispersion is 12%.
Particle dispersion is moved in reactor, open to stir 100rpm, to progressively adding 50 parts of 10% magnesium chloride brines in particle dispersion.Then under 60rpm stirs, slowly increase the temperature to 80 degree, stir 2～3 hours, make the particle diameter (measuring with FPIA-3000) of particle rise to 6.4 μ m.In solution, add the sodium-chloride water solution that 48 parts of concentration are 10% to stop particle size growth, then being slowly warming up to 98 degree stirrings makes particle gradually to spherical transformation for 3 hours, when the sphericity (measuring with FPIA-3000) of particle reaches 0.97 cooling when above, use hydro-extractor filters, with deionized water washing 6 times, the lower vacuum drying of 55 degree, the particle diameter of this carbon dust is 6.7 μ m, distribution of particles is 1.18, sphericity is 0.982, contains 85% resin, 5% pigment yellow 74 and 10% wax POLYWAX400 in carbon dust.To dried particle, add additive to process and obtain Yellow carbon powder.
Carbon dust preparation example 2
In carbon dust preparation example 1, change pigment yellow 74 into carbon black, other conditions are constant, the particle diameter of the carbon black in the organic phase of grinding with muller is 98nm, and the particle diameter that records tiny oil droplet in emulsion fluid with nano particle size instrument is 547nm, and the particle diameter of removing the particle dispersion that contains resin, pigment, wax after ethyl acetate is 436nm, the particle diameter of gained carbon dust is 7.3 μ m, distribution of particles is 1.25, and sphericity is 0.978, contains 85% resin, 5% carbon black and 10% wax POLYWAX400 in carbon dust.To dried particle, add additive to process and obtain black carbon powder.
Carbon dust preparation example 3
In carbon dust preparation example 1, change pigment yellow 74 into pigment red 122, wax POLYWAX400 changes to behenic acid 20 diester, other conditions are constant, the particle diameter of the pigment red 122 in the organic phase of grinding with muller is 186nm, the particle diameter that records tiny oil droplet in emulsion fluid with nano particle size instrument is 633nm, after removing ethyl acetate, contain resin, pigment, the particle diameter of the particle dispersion of wax is 478nm, the particle diameter of gained carbon dust is 6.5 μ m, distribution of particles is 1.21, sphericity is 0.969, in carbon dust, contain 85% resin, 5% pigment red 122 and 10% wax behenic acid 20 diester.To dried particle, add additive to process and obtain red carbon powder.
Carbon dust preparation example 4
In carbon dust preparation example 1, change pigment yellow 74 into pigment blue 15: 3, resin changes to vibrin (Mn=15380, Mw=45300, Tg=51 degree), other conditions are constant, with muller, grind the pigment blue 15 in the organic phase obtaining: 3 particle diameter is 134nm, the particle diameter that records tiny oil droplet in emulsion fluid with nano particle size instrument is 668nm, after removing ethyl acetate, contain resin, pigment, the particle diameter of the particle dispersion of wax is 531nm, the particle diameter of gained carbon dust is 6.3 μ m, distribution of particles is 1.27, sphericity is 0.970, in carbon dust, contain 85% resin, 5% pigment blue 15: 3 and 10% wax POLYWAX400.To dried particle, add additive to process and obtain cyan carbon dust.
Carbon dust preparation example 5
In carbon dust preparation example 1, change 5 parts of pigment yellows 74 into 6.5 pigment red 122s, 85 parts of styrene-acrylic resins change to 83.5 parts of resins, 15 parts of lauryl sodium sulfate change 8 parts of DTABs into, 50 parts, the magnesium chloride of agglutinant 10% changes to 34 parts of 10% sodium phosphates, other conditions are constant, the particle diameter of the pigment red 122 in the organic phase of grinding with muller is 152nm, the particle diameter that records tiny oil droplet in emulsion fluid with nano particle size instrument is 561nm, after removing ethyl acetate, contain resin, pigment, the particle diameter of the particle dispersion of wax is 463nm, the particle diameter of gained carbon dust is 6.8 μ m, distribution of particles is 1.13, sphericity is 0.964, in carbon dust, contain 83.5% resin, 6.5% pigment red 122 and 10% wax POLYWAX400.To dried particle, add additive to process and obtain red carbon powder.
Comparative example 1
The preparation of resin emulsion
In reactor, drop into 42 parts of neopelexes and 5000 parts of water, unlatching stirring and dissolving is even.48 parts of ammonium persulfates are dissolved in 500 parts of water.2250 parts of styrene, 600 parts of butyl acrylates, 150 parts of methacrylic acids, 36 parts of lauryl mercaptans are mixed and are moved in the reactor that as above contains water phase surfactant mixture, stir and obtain milky pre-emulsion.Be warming up to 80 degree, in reactor, add ammonium persulfate initiator aqueous solution, stir 8 hours under 80 degree, be cooled to 35 degree, in emulsion, the content of resin is 37.5%, and the nano particle size instrument of take records its particle diameter as 135nm.
The preparation of dispersible pigment dispersion
450 parts of pigment yellows 74 and 47 parts of neopelexes and 2514 parts of water are at room temperature stirred pre-dispersed, then pre-dispersed liquid is joined in high-speed grinder and ground, under 3000rpm through the dispersion of 180 minutes, obtain dispersible pigment dispersion, the content of pigment is 15%, its volume average particle size is 176nm, and this particle diameter is measured by Beckman CoulterLS230.
The preparation of wax dispersion
By 450 parts of Tissuemat E POLYWAX400 (Bake Hughes, BAKER HUGHES) and 46 parts of neopelexes and 2504 parts of water at 90 ℃, to carry out stirring and dissolving even, then this potpourri is joined fast and in homogenizer, carry out high speed homogenization, by the homogeneous of 2h, obtain milky white wax dispersion, the content of wax is 15%, and its volume average particle size is 124nm, and this particle diameter is measured by Beckman Coulter LS230.
The preparation of carbon dust
The preparation process of carbon dust: the colorant dispersion that the wax dispersion that the resin emulsion that is 37.5% 4032 parts of deionized waters, 2432 parts of solid contents successively, 328 parts of solid contents are 15% and 352 parts of solid contents are 15% adds in reactor, open and stir 100rpm, stir.The pH value to 9.8 of the sodium hydroxide solution regulator solution with 4% dropwise adds the magnesium chloride brine that 378 parts of concentration are 10% in solution.Then under 100rpm stirs, slowly increase the temperature to 78 degree, stir 2～3 hours, make the particle diameter (measuring with FPIA-3000) of particle rise to 7.2 μ m.In solution, add the sodium-chloride water solution that 250 parts of concentration are 20% to stop particle size growth, then being slowly warming up to 98 degree stirrings makes particle gradually to spherical transformation for 5 hours, when the sphericity (measuring with FPIA-3000) of particle reaches 0.96 cooling when above, use hydro-extractor filters, with deionized water washing 6 times, the lower vacuum drying of 55 degree, the particle diameter of this carbon dust is 7.0 μ m, sphericity is 0.972, in carbon dust, contain 89.9% contain resin, 4.9% pigment yellow 74 and 5.2% wax.To dried particle, add additive to process and obtain Yellow carbon powder.
Comparative example 2
Change the pigment yellow 74 in the dispersible pigment dispersion preparation in comparative example 1 into pigment red 122, other conditions are constant, the particle diameter of carbon dust of preparation is 6.5 μ m, and sphericity is 0.974, in carbon dust, contain 89.9% contain resin, 4.9% pigment red 122 and 5.2% wax.To dried particle, add additive to process and obtain red carbon powder.
Carbon dust in the embodiment of the present invention and comparative example is tested respectively to (normal temperature 25 degree, often wet 60%), its result is as follows:
Test experiments proves, carbon dust fine grained of the present invention is few, particle diameter narrow distribution, and bottom ash, useless powder rate, consumption are lower, and Recipe is wider to the selectivity of raw material.
Claims (5)
1. a preparation method for colored carbon powder for development of static charge, is characterized in that, comprises the following steps:
1) colorant grinding distribution in containing the organic solvent of spreading agent, add wherein resin and wax heating for dissolving, obtain the organic phase that contains colorant, resin, wax;
2) in the aqueous solution that contains surfactant, add step 1) in the organic phase that obtains carry out high speed shear emulsion dispersion, obtain emulsion fluid;
3) emulsion fluid is removed to organic solvent through distillation and obtain particle dispersion;
4) in this particle dispersion, add agglutinant to carry out aggegation, obtain colored carbon powder parent, then filter washing, dry, mix additive and obtain colored carbon powder.
2. the preparation method of colored carbon powder for development of static charge as claimed in claim 1, is characterized in that described step 1) in, colorant grinding distribution to footpath grain is 50-200nm.
3. the preparation method of colored carbon powder for development of static charge as claimed in claim 1 or 2, is characterized in that described step 1) in, heating for dissolving temperature is 40-80 ℃.
4. the preparation method of colored carbon powder for development of static charge as claimed in claim 1, is characterized in that described step 2) in, the particle diameter of controlling tiny oil droplet in emulsion fluid is 400-800nm.
5. the preparation method of colored carbon powder for development of static charge as claimed in claim 1, is characterized in that described step 3) in, in particle dispersion, the particle diameter of particle is 300-700nm.
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Citations (5)
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| JPH07152202A (en) * | 1993-11-29 | 1995-06-16 | Hitachi Chem Co Ltd | Electrostatic charge developing toner, its production and developer |
| JPH10186714A (en) * | 1996-10-30 | 1998-07-14 | Dainippon Ink & Chem Inc | Manufacture of electrostatic printing toner |
| CN101178551A (en) * | 2006-11-06 | 2008-05-14 | 施乐公司 | Emulsion aggregation polyester toners |
| CN101632043A (en) * | 2007-02-23 | 2010-01-20 | 三星精密化学株式会社 | Method of preparing toner using micro-suspension particles and toner prepared using the method |
| CN101859080A (en) * | 2009-04-13 | 2010-10-13 | 精工爱普生株式会社 | Toner, image forming method and image processing system |
-
2014
- 2014-06-05 CN CN201410246455.1A patent/CN104062861A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07152202A (en) * | 1993-11-29 | 1995-06-16 | Hitachi Chem Co Ltd | Electrostatic charge developing toner, its production and developer |
| JPH10186714A (en) * | 1996-10-30 | 1998-07-14 | Dainippon Ink & Chem Inc | Manufacture of electrostatic printing toner |
| CN101178551A (en) * | 2006-11-06 | 2008-05-14 | 施乐公司 | Emulsion aggregation polyester toners |
| CN101632043A (en) * | 2007-02-23 | 2010-01-20 | 三星精密化学株式会社 | Method of preparing toner using micro-suspension particles and toner prepared using the method |
| CN101859080A (en) * | 2009-04-13 | 2010-10-13 | 精工爱普生株式会社 | Toner, image forming method and image processing system |
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Application publication date: 20140924 |