CN101630129B - Azo series charge regulator dispersoid and preparation method thereof and carbon powder - Google Patents
Azo series charge regulator dispersoid and preparation method thereof and carbon powder Download PDFInfo
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- CN101630129B CN101630129B CN200910063444A CN200910063444A CN101630129B CN 101630129 B CN101630129 B CN 101630129B CN 200910063444 A CN200910063444 A CN 200910063444A CN 200910063444 A CN200910063444 A CN 200910063444A CN 101630129 B CN101630129 B CN 101630129B
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- charge
- dispersoid
- adjusting agent
- azo series
- charge regulator
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Abstract
The invention relates to azo series charge regulator dispersoid and carbon powder prepared by adopting the dispersoid, solving the problems that the charge of carbon powder is unstable and the charge regulator is not distributed evenly in the polymerized carbon powder when preparing black carbon powder by the method of emulsion polymerization, ensuring that the prepared black carbon powder has good charge performance and is not affected by continuous use for a long time, temperature and humidity, and carbon powder of high definition graphics can be obtained stably in a long time.
Description
Technical field
The electrophoto-graphic toner that the present invention relates to a kind of azo series charge regulator dispersoid and adopt this dispersion to prepare.
Background technology
Electrophoto-graphic toner is called carbon dust again, and its manufacturing approach mainly contains two kinds of physics method and chemical methods, and the physics method is traditional comminuting method, and chemical method mainly contains two kinds of suspension polymerization, emulsion polymerizations.The polymerization carbon dust of chemical method is the method production through polymerization, its particle diameter little (6-8 μ m), be evenly distributed, carbon powder particle shape subglobular, resolution is very high when printing, glossiness is fine, useless powder rate is also much lower and energy consumption is low, CO
2Discharge capacity only be equivalent to 60% of conventional physical method carbon dust.Therefore the color powder of chemical method has higher print quality, more abundant colors and advantages such as image more true to nature, so in order to improve the perfection of print quality and color representation, the working method of present color powder enters into the chemical method epoch by traditional physics method.
The suspension polymerization is with oil droplet outstanding turbid being distributed in the water system under mechanical raking, therefore forms the distribution of broad easily, owing in water system, form oil droplet, so what obtain basically all is spheroidal particle, though favourable to transfer printing property, cleaning is a problem.Emulsion polymerization is with particles aggregate, is melting carbon dustization in the water system medium, so particle diameter can control very for a short time, and size distribution can be controlled very narrow, and shape of particle also can arbitrarily be controlled.Emulsion polymerization is state-of-the-art in the world at present technology method.However; Also there are some problems in emulsion polymerization; Be difficult to control like the charged characteristic of the carbon dust made, ageing stability, environmental stability etc.; Though the The Nomenclature Composition and Structure of Complexes through telomerized polymer, regulate surface additive kind and consumption can carry out improvement to a certain extent to charged characteristic and stability, still be difficult to the effect that reaches satisfied, and the technical difficulty of adjusting is very big.
Summary of the invention
The objective of the invention is in order to solve the problems of the technologies described above; Dispersion of a kind of azo series charge regulator and preparation method thereof is provided; And the carbon dust that adopts this dispersion preparation; Solved unstable, the charge adjusting agent problem pockety in the polymerization carbon dust of carbon dust charging property in emulsion polymerization
Technical scheme provided by the invention is: a kind of azo series charge regulator dispersoid; Said dispersion is made up of azo series charge regulator, spreading agent, dispersing aid and water; The mean diameter of dispersion is 80～180nm; Above-mentioned azo series charge regulator is the complex compound of azo-compound and chromium, iron, and its general formula is following:
In the formula: R
1-R
4Can be the same or different; The alkoxy of the alkyl of expression hydrogen atom, carbon number 1-18 or alkenyl, carbon number 1-18, can have substituent sulfamoyl, mesyl, hydroxyl, carboxyl, carboxylic ester group, acetylamino, benzamido, halogen atom, nitro or can have substituent aryl, R
5, R
6Expression hydrogen atom, low alkyl group, lower alkoxy, nitro, halogen atom or
Azo series charge regulator dispersoid of the present invention specifically can be enumerated out DL-N30B, DL-N32A, the DL-N33 that produces like Long-Ting of Hubei Chemical Co, and its structural formula respectively as follows.
Said spreading agent is sorbitan mono-laurate (Span-20), anhydrous sorbitol monopalmitate (Span-40), sorbitan monostearate (Span-60), sorbitan monooleate (Span-80), APES, at least a in dodecyl polyethenoxy ether sodium sulfate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, neopelex, polyvinyl alcohol (PVA), polyglycol, polyvinyl pyrrolidone, modified polypropene acid sodium-salt or the AEO.
Said dispersing aid is at least a in ethanol, butanols, isobutyl alcohol, n-amyl alcohol, n-hexyl alcohol, n-octyl alcohol, lauryl alcohol, acetonitrile, ethylene glycol monobutyl ether, ethylene glycol ethyl ether, propylene glycol monomethyl ether, butanone, cyclohexanone, ethyl acetate or the butyl acetate.
Above-mentioned charge regulator dispersoid; Wherein the charge adjusting agent addition is 5～25% of a dispersion overall weight, and is preferred 10～20%, and the addition of spreading agent is 5%～40% of a charge adjusting agent weight; Preferred 20～30%; The dispersing aid addition is 2%～30% of a charge adjusting agent weight, and is preferred 5～20%, and surplus is a water.
Spreading agent mainly is one type and has surface-active material; It can be distributed to material water insoluble or that be slightly soluble in water in the aqueous systems; And dispersing aid mainly is to assist spreading agent to bring into play the effect of spreading agent; Change is by the surface nature of disperse object, thereby spreading agent can better be played a role in dispersion process.Adopt this series charge regulator dispersoid to prepare carbon dust at emulsion polymerization; Can be so that the charged narrowly distributing of the polymerization carbon powder particles of preparation; And evenly; So just can reduce the deficiency of vocal cores electric weight and cause carbon dust to disperse and the bottom ash that forms, thereby can significantly improve the effect of printing, reduce the bottom ash in the print procedure; And being evenly distributed of carried charge also can reduce the amount of the carbon powder particles that in transfer process, can not be transferred significantly, thereby can reduce the useless powder rate in the print procedure.
The preparation method of above-mentioned charge regulator dispersoid may further comprise the steps:
Required azo series charge regulator, spreading agent, dispersing aid and water are evenly mixed, stirred 15～90 minutes, be configured to pre-dispersed liquid with the linear velocity of 10～40 meter per seconds; The pre-dispersed liquid of preparation was ground under 5000～22000 rev/mins 60～240 minutes.
Carbon dust of the present invention is prepared from through emulsion polymerization containing resin, colorant and azo series charge regulator dispersoid of the present invention at least.With the solid weight meter of said carbon dust, preferably prepare the charge adjusting agent (weight content according to charge regulator dispersoid is converted into amount of solid) that adds in the process by carbon dust weight 1～5% weight at carbon dust, carry out this carbon dust of emulsion polymerization preparation then.
The invention advantage: it is a kind of this dispersion of glue that the present invention provides a kind of azo series charge regulator dispersoid; This dispersion has smaller particle size; Can in the making of emulsion polymerization carbon dust, be evenly distributed in the carbon powder particles; Thereby improve the problem that the carbon powder particles carried charge is not enough, the speed that electrifies is slow and carried charge descends rapidly; The carbon dust that obtains carries out electronics and develops and can obtain the image that bottom ash is few, development density is high, gamut range is wide, expressive force is strong, and the consumption rate of carbon dust and useless powder rate are low; Simultaneously, the color of the charge adjusting agent described in the present invention is generally black or brown, does not influence the color representation power of polymerization black carbon powder, thereby is suitable in the preparation of polymerization carbon dust especially black polymerization carbon dust, using.
Embodiment
Charge adjusting agent embodiment 1
Charge adjusting agent DL-N30B powder 200 weight portions, spreading agent sorbitan monostearate 80 weight portions, dispersing aid butanone 60 weight portions and 1660 weight parts waters were carried out mechanical mixture 30 minutes under the linear velocity of 30 meter per seconds; Again potpourri speed with 18000 rev/mins on muller of gained was ground 120 minutes; Then obtain the dispersion (1) of charge adjusting agent of the present invention, recorded the mean grain size D=121nm of particle through Coulter particle diameter tester.
Charge adjusting agent embodiment 2
40 parts in charge adjusting agent DL-N30B powder, spreading agent lauryl sodium sulfate 2 weight portions, dispersing aid cyclohexanol 0.8 weight portion and 1957.5 weight parts waters were carried out mechanical mixture 60 minutes under the linear velocity of 10 meter per seconds; Again potpourri speed with 22000 rev/mins on muller of gained was ground 90 minutes; Then obtain the dispersion (2) of charge adjusting agent of the present invention, recorded the mean grain size D=128nm of particle through Coulter particle diameter tester.
Charge adjusting agent embodiment 3
Charge adjusting agent DL-N32A powder 500 weight portions, spreading agent disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 100 weight portions, dispersing aid butanone 75 weight portions and 1325 weight parts waters were carried out mechanical mixture 30 minutes under the linear velocity of 20 meter per seconds; Again potpourri speed with 18000 rev/mins on muller of gained was ground 120 minutes; Then obtain the dispersion (3) of charge adjusting agent of the present invention, recorded the mean grain size D=130nm of particle through Coulter particle diameter tester.
Charge adjusting agent embodiment 4
Charge adjusting agent DL-N33 powder 200 weight portions, spreading agent dodecyl polyethenoxy ether sodium sulfate 10 weight portions, dispersing aid butanols 4 weight portions and 1700 weight parts waters were carried out mechanical mixture 30 minutes under the linear velocity of 40 meter per seconds; Again potpourri speed with 5000 rev/mins on muller of gained was ground 240 minutes; Then obtain the dispersion (4) of charge adjusting agent of the present invention, recorded the mean grain size D=154nm of particle through Coulter particle diameter tester.
Carbon dust embodiment 5
75 parts by weight of styrene emulsion acrylic resins (solids content 35% quality), 15 weight portion carbon black dispersions (solids content 20%), 8 weight account polyethylene wax dispensers (solids content 30% quality) and 200 weight parts waters are mixed; Stirred 5 minutes with 500～1000 rev/mins speed; The pH that regulates mixed system then is 4.0; In mixed system, add 20 weight portion magnesium chloride solutions (solids content 20% quality) then, stir and be warmed up to 58 ℃ after 10 minutes, begin to detect the variation of particle diameter then; When the particle diameter of agglutination particle reaches 7 microns; The sodium chloride solution (solids content 20% quality) that in mixed system, adds 50 weight portions stops the growth of particle, is warmed up to 90 ℃ then always and carries out melting of particle, detects the sphericity of particle with Sysmex FIPA 3000; Cooling when sphericity reaches 0.96, filtration, washing, drying obtain described carbon powder particles (calling " relatively carbon dust " in the following text).
Carbon dust embodiment 6
3 parts of charge regulator dispersoid weight and 200 weight parts waters in 75 parts by weight of styrene emulsion acrylic resins (solids content 35% quality), 15 weight portion carbon black dispersions (solids content 20% quality), 8 weight account polyethylene wax dispensers (solids content 30% quality), the foregoing description 1 are mixed; Stirred 5 minutes with 500～1000 rev/mins speed; The pH that regulates mixed system then is 4.0; In mixed system, add 20 weight portion magnesium chloride solutions (solids content 20% quality) then, stir and be warmed up to 58 ℃ after 10 minutes, begin to detect the variation of particle diameter then; When the particle diameter of agglutination particle reaches 7 microns; The sodium chloride solution (solids content 20% quality) that in mixed system, adds 50 weight portions stops the growth of particle, is warmed up to 90 ℃ then always and carries out melting of particle, detects the sphericity of particle with Sysmex FIPA 3000; Cooling when sphericity reaches 0.96, filtration, washing, drying obtain described carbon powder particles (calling " carbon dust 1 " in the following text).
Carbon dust embodiment 7
Adopt charge regulator dispersoid (2) to replace charge adjusting agent to disperse (1), all the other are with embodiment 6, the carbon powder particles that obtains (calling " carbon dust 2 " in the following text).
Carbon dust embodiment 8
Adopt charge regulator dispersoid (3) to replace charge adjusting agent to disperse (1), all the other are with embodiment 6, the carbon powder particles that obtains (calling " carbon dust 3 " in the following text).
Carbon dust embodiment 9
Adopt charge regulator dispersoid (4) to replace charge adjusting agent to disperse (1), all the other are with embodiment 6, the carbon powder particles that obtains (calling " carbon dust 4 " in the following text).
By 95: 5 weight ratio, the comparison carbon dust of iron powder carrier and embodiment 5 and the carbon dust 1～4 of embodiment 6～9 preparations are mixed then, process comparison developer and developer 1～4 respectively.
The use standard blows afloat the carried charge that method detects this developer; Embodiment 6～9 has been added the developer 1～4 that the carbon dust 1～4 of charge regulator dispersoid (1)～(4) processes and the comparison developer processed the comparison carbon dust that does not add this charge regulator dispersoid compares, and its result is following:
| The performance title | Compare developer | Developer 1 | Developer 2 | Developer 3 | Developer 4 |
| Charged under the general condition (25 ℃, 50%) | -18.1μC/g | -32μC/g | -29μC/g | -31.1μC/g | -35μC/g |
| Low temperature and low humidity (5 ℃, 30%) | -18.0μC/g | -32.2μC/g | -28.7μC/g | -30.6μC/g | -34.4μC/g |
| Hot and humid (60 ℃, 90 %) | -17.2μC/g | -31.3μC/g | -27.8μC/g | -29.9μC/g | -33.5μC/g |
| Development density | 1.28 | 1.42 | 1.49 | 1.50 | 1.46 |
| Bottom ash | 0.030 | 0.001 | 0.003 | 0.006 | 0.002 |
| Useless powder rate | 23％ | 8％ | 5％ | 3％ | 6％ |
| Consumption | 35mg | 21mg | 19mg | 23mg | 20mg |
Result from above table; The charging property that adds the carbon dust for preparing behind the azo series charge regulator dispersoid among the present invention is significantly improved; And effect from printing; The printing effect that adds the carbon dust of this series charge regulator dispersoid also is significantly improved, and bottom ash, useless powder rate and consumption have also all had tangible improvement.
Claims (3)
1. azo series charge regulator dispersoid; It is characterized in that; Be made up of azo series charge regulator, spreading agent, dispersing aid and water, the mean diameter of dispersion particle is 80～130nm, and said charge adjusting agent addition is 5～25% of a dispersion overall weight; The spreading agent addition is 20%～30% of a charge adjusting agent weight; The dispersing aid addition is 5～20% of a charge adjusting agent weight, and surplus is a water, and wherein said azo series charge regulator is the complex compound of azo-compound and iron, and its general formula is following:
In the formula: R
1-R
4Can be the same or different; Alkoxy, sulfamoyl, mesyl, hydroxyl, carboxyl, carboxylic ester group, acetylamino, benzamido, halogen atom, nitro or the aryl of the alkyl of expression hydrogen atom, carbon number 1-18 or alkenyl, carbon number 1-18, R
5, R
6Expression hydrogen atom, low alkyl group, lower alkoxy, nitro, halogen atom or
2. the described azo series charge regulator dispersoid of claim 1; It is characterized in that; Said spreading agent is sorbitan mono-laurate (Span-20), anhydrous sorbitol monopalmitate (Span-40), sorbitan monostearate (Span-60), sorbitan monooleate (Span-80), APES, at least a in dodecyl polyethenoxy ether sodium sulfate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, neopelex, polyvinyl alcohol (PVA), polyglycol, polyvinyl pyrrolidone, modified polypropene acid sodium-salt or the AEO.
3. method for preparing claim 1 or 2 described azo series charge regulator dispersoids is characterized in that this method may further comprise the steps:
A) azo series charge regulator, spreading agent, dispersing aid and water are evenly mixed, stirred 15-90 minute with the linear velocity of 10～40 meter per seconds, be configured to pre-dispersed liquid, said charge adjusting agent addition is 5～25% of a dispersion overall weight; The spreading agent addition is 20%～30% of a charge adjusting agent weight; The dispersing aid addition is 5～20% of a charge adjusting agent weight, and surplus is a water;
B) pre-dispersed liquid was ground under 5000～22000 rev/mins rotating speed 60～240 minutes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910063444A CN101630129B (en) | 2009-08-05 | 2009-08-05 | Azo series charge regulator dispersoid and preparation method thereof and carbon powder |
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| CN200910063444A CN101630129B (en) | 2009-08-05 | 2009-08-05 | Azo series charge regulator dispersoid and preparation method thereof and carbon powder |
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| CN101630129A CN101630129A (en) | 2010-01-20 |
| CN101630129B true CN101630129B (en) | 2012-09-26 |
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| CN102346390B (en) * | 2011-10-28 | 2013-05-01 | 湖北鼎龙化学股份有限公司 | Charge regulator and preparation method thereof, and carbon powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424628A (en) * | 2001-12-13 | 2003-06-18 | 东方化学工业株式会社 | Charge adjusting resin particle and electrostatic developing toning agent |
| CN1645261A (en) * | 2005-01-20 | 2005-07-27 | 湖北鼎龙化工有限责任公司 | Production of electric charge regulator and carbon powder containing it for electronic camera |
| CN1983044A (en) * | 2001-12-13 | 2007-06-20 | 东方化学工业株式会社 | Charge control agent, charge control resin particles and toner for developing electrostatic images |
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2009
- 2009-08-05 CN CN200910063444A patent/CN101630129B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424628A (en) * | 2001-12-13 | 2003-06-18 | 东方化学工业株式会社 | Charge adjusting resin particle and electrostatic developing toning agent |
| CN1983044A (en) * | 2001-12-13 | 2007-06-20 | 东方化学工业株式会社 | Charge control agent, charge control resin particles and toner for developing electrostatic images |
| CN1645261A (en) * | 2005-01-20 | 2005-07-27 | 湖北鼎龙化工有限责任公司 | Production of electric charge regulator and carbon powder containing it for electronic camera |
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Address after: 430015 Hubei city of Wuhan province Hankou Jianghan Road No. 8 Jinmao Building 19 Patentee after: Hubei Dinglong Cmi Holdings Ltd Address before: 430015 Hubei city of Wuhan province Hankou Jianghan Road No. 8 Jinmao Building 19 Patentee before: Hubei Dinglong Chemical Co., Ltd. |