CN106033175A - Color toner and preparation method thereof - Google Patents
Color toner and preparation method thereof Download PDFInfo
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- CN106033175A CN106033175A CN201510117133.1A CN201510117133A CN106033175A CN 106033175 A CN106033175 A CN 106033175A CN 201510117133 A CN201510117133 A CN 201510117133A CN 106033175 A CN106033175 A CN 106033175A
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Abstract
The present invention provides a color toner and a preparation method thereof. The preparation method comprises: respectively preparing reaction components such as a polymer emulsion, a wax dispersing liquid, and a coloring agent dispersing liquid; adding the three reaction components into deionized water, dispersing, adjusting the pH value of the mixture to below 4, increasing the temperature of the system, and adjusting the pH value to a neutral state when the particle size of the particles in the mixture achieves 7-9 [mu]m to obtain toner powder primary particles; increasing the temperature of the system, adding a polymerization reaction monomer and an initiator, carrying out a polymerization reaction, carrying out thermal insulation on the reaction system at a temperature of 90-110 DEG C when the particle size of the particles in the reaction system achieves 9-11 [mu]m, stopping the thermal insulation when the circularity of the particles in the reaction system is 0.90-0.98, cooling the reaction system, separating, and drying to obtain toner particles; and adding an external additive to the toner particles, and carrying out stirring mixing to obtain the color toner. The color toner produced by using the production method of the present invention has good fixing property and good durability during printing and copying.
Description
Technical field
The present invention relates to electrophotographic image forming technical field, be specifically related to a kind of colored carbon powder and preparation method thereof.
Background technology
Xerography is formation electrostatic latent image on photoreceptor or electrostatic recording medium, then with colored carbon
Powder sticks to make it develop on described electrostatic latent image, followed by hot-pressing roller under the action of heat and pressure,
It is transferred to carbon powder image on paper form fixing image.The performance of colored carbon powder and quality are by direct shadow
Ring image quality.
Colored carbon powder is generally by fluoropolymer resin, coloring agent (pigment or dyestuff), wax, external additive (electricity
Lotus controlling agent etc.) etc. become be grouped into.The colored carbon powder being conventionally used to electrostatic development generally uses melted pulverizing
Prepared by method, the method be by resin, coloring agent, additive through melting mixing, extrude, cool down, broken
The operations such as broken, superfine grinding, classification, addition external additive, are finally made colored carbon powder.But, this
Kind preparation method also exists toner and cannot colored carbon powder shape dispersed in resin, preparation not advise
Then, particle diameter is relatively big and the defect such as wider distribution, thus it is poor (easy to there is fixation performance when causing printing, duplicate
Roll banding), resolution is low, shade deviation, the useless more high defect of powder rate, the method technique is the most multiple simultaneously
Miscellaneous, the most relatively costly.
There is many defects in the colored carbon powder owing to using the physical methods such as melted pulverizing to prepare, follow-up gradually
Development has the technology using chemical method to prepare colored carbon powder, gathers including suspension polymerization and emulsion
Legal.
Suspension polymerization refers to that monomer is suspended in medium with the form of droplet and carries out radical polymerization, should
Method can efficiently control the size of colored carbon powder granule, so that the mobile performance of carbon dust, charge
Can be improved significantly.But, utilize carbon dust broad particle distribution prepared by the method, so that carbon dust turns
Print efficiency reduces and resolution is not good enough, and the carbon powder particle obtained is too round, thus the recovery of carbon dust with
Cleaning relative difficulty.
Emulsion polymerization relative suspension polymerization is more easy to obtain the colored carbon powder that particle size distribution is less.Existing
Emulsion polymerization prints performance when preparing colored carbon powder partially in order to improve the anti-of colored carbon powder, it usually needs carry
The consumption of high wax, is now easily caused wax and moves to the surface of carbon powder particles, not only pollute carrier and development
Sleeve, also can make colored carbon powder fixation performance when printing poor；Additionally, wax also can form wax on photoreceptor
Film and cause durability to reduce.
Summary of the invention
The present invention solves above-mentioned technical problem, it is provided that a kind of colored carbon powder and preparation method thereof, profit
The colored carbon powder fixation performance and the endurance quality when printing and duplicate that prepare by this preparation method are good.
A first aspect of the present invention, it is provided that the preparation method of a kind of colored carbon powder, comprises the following steps:
1) reactive component is prepared respectively:
Preparing macromolecule emulsion, described macromolecule emulsion is cinepazid polymer emulsion or polyester resin emulsion；
Wax and surfactant are added in deionized water and makes wax dispersion；
Coloring agent and surfactant are added in deionized water and makes colorant dispersion；
2) at room temperature by prepared macromolecule emulsion, wax dispersion and colorant dispersion add go from
In sub-water and disperse, the pH value of regulation mixture to less than 4 and raises system temperature, to be mixed
In thing, the particle diameter of particle reaches the pH value of regulation mixture extremely neutrality during 7-9 μm, obtains carbon dust primary grain
Son；
3) raise the temperature of carbon dust primary particle place system, and add polymerization reaction monomer and initiator enters
Row polyreaction, when the particle diameter of particle reaches 9-11 μm in question response system, makes reaction system exist
90-110 DEG C of insulation, in question response system, the circularity of particle stops insulation when being 0.90-0.98, then to instead
Answer system to carry out cooling down, separate, be dried, obtain carbon powder particle；
4) in the above-mentioned carbon powder particle made, add external additive, be mixed and made into colored carbon powder.
In the present invention, the print performances such as the durability of colored carbon powder, fixing ability can be considered
Being controlled each mass parameter of described macromolecule emulsion, mass parameter such as can include vitrification temperature
Degree (Tg), molecular weight ranges, molecular weight distribution etc..Show after deliberation: if the Tg of macromolecule emulsion is less than
40 DEG C, the durability of carbon dust will be deteriorated, if can promote carbon dust when the Tg of macromolecule emulsion is higher than 75 DEG C
Fixing temperature raises, thus causes the low inferior problem of fixing ability；Therefore, can control under comprehensive consideration
The vitrification point of described macromolecule emulsion is 40-75 DEG C, and this vitrification point can use differential scanning
Calorimeter (DSC) records.
Further, it is also possible to the weight average molecular weight controlling described macromolecule emulsion is 4000-1000000, molecule
Amount is distributed as 2-30, so that the colored carbon powder of preparation has more excellent print performance, and this macromolecule
The weight average molecular weight of emulsion and molecular weight distribution use gel permeation chromatography (GPC) to record.Further, originally
Invent the solid content to prepared macromolecule emulsion to limit without strict, in embodiments of the invention,
The solid content of macromolecule emulsion is preferably less than 50%.
In one embodiment of this invention, can be by by initiator, surfactant, styrene list
Body, acrylate monomer, chain-transferring agent addition deionized water carries out polyreaction, prepares phenylpropyl alcohol polymerization
Thing emulsion.
Further, when preparing cinepazid polymer emulsion, under oxygen-free environment, by described initiator, table
Face activating agent, styrene monomer, acrylate monomer and chain-transferring agent are (0.1-3) in mass ratio:
(0.2-5): (40-60): (10-30): (0.05-5), adding temperature is to carry out in the deionized water of 70-90 DEG C
Polyreaction, makes described cinepazid polymer emulsion；Particularly, polymeric reaction product is carried out cooling and
Filter.Wherein it is possible to realize oxygen-free environment by being passed through noble gas (such as nitrogen) to reaction system,
And can under agitation carry out this polyreaction, mixing speed can control at 150-200rpm；This
Outward, first can add surfactant in deionized water, then add styrene monomer, acrylate
Add initiator while monomer and chain-transferring agent and carry out polyreaction, and 100 mesh filter screens can be used
Polymeric reaction product is filtered.
Preferably, the vitrification point controlling described cinepazid polymer emulsion is 50-65 DEG C, Weight-average molecular
Amount is 10000-600000, and molecular weight distribution is 4-15.
In another embodiment of the present invention, can stir by polyester resin is added in organic solvent
After being completely dissolved, add deionized water and alkali disperses, remove organic solvent subsequently, prepare described
Polyester resin emulsion.Wherein, the quality between described polyester resin, organic solvent and deionized water is controlled
Than being (1-5): (5-20): (6-30), and the particle diameter controlling described polyester resin emulsion is
50-500nm, pH are 6-8；The organic solvent used can be alcohols, ketone (butanone), amide
Class (DMF), sulfone class (dimethyl sulfoxide), cyclic ethers class (oxolane), acetic acid second
Ester, and the mixture of above solvent.
Preferably, the vitrification point controlling described polyester resin emulsion is 50-70 DEG C, is further
55-65℃；Molecular weight is 5000-1000000, is 10000-500000 further；Molecular weight distribution is
3-30, is 4-15 further.
In one embodiment, described wax and surfactant additions deionized water is made wax dispersion
Liquid, may include that by wax and surfactant be 1:(0.02-0.3 in mass ratio) add deionized water
In, heating makes the temperature of this system disperse higher than after the fusing point of wax, and making particle diameter is 80-500nm
Wax dispersion；Wherein, the fusing point of described wax is 50-130 DEG C；Especially it is possible to selection fusing point is
The wax of 50-110 DEG C；If the fusing point of wax is higher than 130 DEG C, then when being unfavorable for printing, carbon dust is melted enters paper fibre
Dimension, produces impact, and when the fusing point of wax is less than 50 DEG C, carbon dust may be made to be easier to temperature fixing performance
It is bonded on photocon or Metering blade.The particle diameter of above-mentioned wax dispersion uses Malvern laser particle instrument
MS2000 records.
In concrete scheme of the present invention, the wax of use can be the combination of one or more of: paraffin,
The petroleum wax such as microwax, vaseline and derivant；The polyolefin-wax such as Tissuemat E, polypropylene wax and
Derivant；The synthetic waxs such as Fischer-Tropsch wax；The rice natural system such as wax, Brazil wax wax；Ester system can also be used
Wax, department of botany's wax, animal system wax, SOLID ORGANIC silicon wax, lignite wax etc..
Additionally, described scattered mode is the most strictly limited by the present invention, can be such as dispersed with stirring and
/ or homogenous disperse, wherein dispersed with stirring can use the conventional equipments such as high-speed shearing machine to carry out, and homogenizing divides
Dissipating to use the conventional equipments such as high pressure homogenizer to carry out.Specifically, when preparing wax dispersion, permissible
First implement dispersed with stirring 0.5-2h, then carry out homogenous disperse, thus realize dispersed；Further, this
The bright solid content to this wax dispersion limits without strict, in embodiments of the invention, and wax dispersion
Solid content is preferably less than 40%.
In one embodiment, coloring is made described coloring agent and surfactant additions in deionized water
Agent dispersing liquid, may include that by coloring agent and surfactant be 1:(0.02-0.4 in mass ratio) add
Disperseing after deionized water and grind, prepared particle diameter is the colorant dispersion of 80-800nm.Above-mentioned
The particle diameter of colorant dispersion uses Malvern laser particle instrument MS2000 to record.
Additionally, when preparing colorant dispersion, dispersed with stirring can be used, and can control stirring point
The rotating speed dissipated is 2500-3500rpm, and jitter time is 0.5-8h；Further, this coloring agent is divided by the present invention
The solid content dissipating liquid limits without strict, in embodiments of the invention, and the solid content of colorant dispersion
It is preferably less than 50%.
Further, in terms of the solid contents in each reactive component, can be with rate-determining steps 2) described in high
Mass ratio between molecule emulsion, wax dispersion and colorant dispersion is (30-50): (5-15):
(6-20) system temperature, and is raised after dispersed with stirring to 35-50 DEG C.
The present invention is to step 2) in the bronsted lowry acids and bases bronsted lowry that used of pH of regulation mixture have no particular limits.
Acid can be one or more in sulphuric acid, nitric acid, hydrochloric acid；Alkali can be sodium hydroxide, hydroxide
One or more in potassium, ammonia.
Further, step 3) in, raise the temperature of carbon dust primary particle place system to 70-90 DEG C,
And to control the mass ratio between polymerization reaction monomer and initiator be 100:(0.3-0.6), meet high score simultaneously
In sub-emulsion, the mass ratio between solids and polymerization reaction monomer is (1-10): 1.
The inventors discovered that, carry out polyreaction at carbon dust primary particle with polymerization reaction monomer and initiator
During, when particle diameter reaches 9-11 μm in reaction system, make reaction system at 90-110 DEG C
Insulation, detects the circularity of particle simultaneously, circularity is controlled at 0.90-0.98, and this circularity scope has
It is beneficial to recovery and the cleaning of carbon dust.In embodiment of the present invention, can be had based on those skilled in the art
Standby basic general knowledge and skills determine the circularity of particle, it is for instance possible to use Sysmex FIPA
3000 detection circularities.
Surfactant used in the present invention is anionic surfactant and/or nonionic table
Face activating agent.Wherein, described anionic surfactant can be selected from alkylaryl sulfonates, alkyl
Sulfate, alkyl ether sulfate, alkyl carboxylate, at least in alkyl alkoxylated carboxylate etc.
Kind, be specifically as follows sodium lauryl sulphate, sodium tetradecyl sulfate, pentadecyl sodium sulfate, 12
Sodium alkyl benzene sulfonate, dodecyl sodium sulfate, methyl stearate sodium sulfonate of ethoxylated, α thiazolinyl sulphur
Acid sodium, SAS, Di-phosphorus pentonide, lauryl alcohol phosphate ester etc., preferably alkylsurfuric acid
Salt, more preferably sodium lauryl sulphate；Nonionic surfactant can be selected from polyoxyethylene cetyl
Base ether, NONIN HS 240, polyoxyethylene oleyl ether, Polyoxyethylene sorbitan Dan Yue
Cinnamic acid ester, polyoxyethylene stearyl ether, NPE, dialkyl phenol polyoxyethylene ether, fat
Alcohol polyethylene glycol oxide ether, polyoxyethylene carboxylate, alkanolamide, polyethenoxy alkanolamide alkyl second
Epoxide compound, alkyl propoxylated compound, alkyl aryl ethoxylates, alkylaryl propoxylate and
At least one in ethylene oxide/propylene oxide copolymer etc., preferably alkylphenol polyoxyethylene, more excellent
Elect the alkylphenol polyoxyethylene containing 8-10 carbon atom as.
The coloring agent that the present invention uses is dyestuff and/or pigment, from resistance to water, light resistance and gas resistance
From the point of view of, preferably pigment.The specifically chosen of pigment is not limited by the present invention, and it can include
But it is not limited to green pigment, such as C.I. alizarol saphirol 2, alizarol saphirol 3, pigment blue 15, pigment blue 15:
1, pigment blue 15: 2, pigment blue 15: 3, pigment blue 15: 4 etc.；Magenta pigment, such as C.I.
Pigment red 30, pigment red 31, pigment red 32, pigment red 37, pigment red 38, pigment red 4 8:1,
Paratonere 53:1, paratonere 57:1, pigment red 112, paratonere 114, pigment red 122, pigment
Red 184 etc.；Yellow uitramarine, such as C.I. pigment yellow 74, pigment yellow 81, pigment yellow 83, pigment yellow
97, pigment yellow 110, pigment yellow 13 8 etc.；Black pigment, such as nigrosine, white carbon black, non magnetic ferrum
Oxysome, copper oxide, activated carbon etc..
The polymerization reaction monomer that the present invention uses can be the combination of one or more of: styrene list
Body, such as styrene, o-methyl styrene, a methyl styrene, p-methylstyrene, to methoxyl group
Styrene, p-ethyl-styrene etc.；Vinyl ester monomers, such as: vinyl acetate, vinyl propionate
Ester, vinyl benzoate, vinyl butyrate etc.；Acrylate monomer, such as: acrylic acid methyl ester., third
Olefin(e) acid ethyl ester, n-butyl acrylate, Isobutyl 2-propenoate, n-propyl, n-octyl,
Dodecylacrylate, acrylic acid-2-ethyl caproite, 2-hydroxyethyl acrylate, acrylic acid are hard
Fatty acyl ester, acrylic acid-2-chloroethene ester etc.；Methacrylate monomer, such as: methyl methacrylate,
Ethyl methacrylate, n propyl methacrylate, n-BMA, isobutyl
Ester, Tert-butyl Methacrylate, n octyl methacrylate, lauryl methacrylate, metering system
Acid-2-hydroxypropyl acrylate, methacrylic acid-2-hydroxy methacrylate, methacrylic acid-2-Octyl Nitrite, metering system
Acid stearoyl ester, phenyl methacrylate, dimethylaminoethyl methacrylate, methacrylic acid two
Ethylamino ethyl ester etc.；Unsaturated carboxylic acid monomer, such as acrylic or methacrylic acid；Containing halogen ethylene
Base monomer, such as vinyl chloride；Nitro class monomer, the copolymer of such as nitrostyrolene etc.；Can also adopt
With acrylonitrile, maleic anhydride, vinyl Ether, methacrylonitrile, acrylamide, methacrylate, maleic acid
Etc. polar acidic based polyalcohol monomer etc..Wherein, preferred polymerization reaction monomer include styrene monomer and
(methyl) acrylate monomer, described styrene monomer with the quality proportioning of (methyl) acrylate monomer is
(40-60): (10-30).
The initiator that the present invention uses is Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate or hydrogen peroxide etc..
By the present invention in that the molecular weight regulating polymer emulsion with chain-transferring agent, chain-transferring agent can be
N-dodecyl mereaptan, tert-dodecyl mercaptan, carbon tetrachloride etc..
Further, in step 4) in, described carbon powder particle is 100 with the mass ratio of external additive:
(0.1-8), it may be assumed that relative to carbon powder particle 100 weight portion, the content of external additive is 0.1-8 weight portion,
It is preferably 100:(0.2-5).If the content of external additive is less than 0.1 weight portion, in carbon dust print procedure
Electrification speed is slow, and mobility is poor, and the charging stability under high temperature is poor；If the content of external additive is big
In 8 weight portions, then part external additive easily separates from carbon dust surface, may adhere in print procedure
To photosensitive surface, easily form film, or cause the band Electricity Functional of developing agent bad at developing trough building up inside
Change.
Additionally, described external additive can be inorganic external additive and/or organic external additive；Wherein,
Described inorganic external additive is in silicon dioxide, titanium dioxide, aluminium oxide, zinc oxide and magnesium oxide
One or more, described organic external additive one or many in polymer pearl and metallic stearate
Kind.In order to improve the bonding cohesion between the mobility of carbon powder particle, suppression carbon powder particle so that it is can
Longer-term storage is stable, even if also can keep stable in the environment of hot and humid for a long time, external additive is excellent
Elect inorganic external additive, more preferably silicon dioxide, titanium dioxide and aluminium oxide as.
A second aspect of the present invention provides a kind of colored carbon powder, and this colored carbon powder is according to any of the above-described described
Preparation method prepare.
The preparation method of the colored carbon powder of the present invention, utilizes the polymerization process implemented step by step, first prepares bag
The carbon dust primary particle of the content of wax and coloring agent, further and makes carbon dust primary particle table by polyreaction
Face forms resin-coating layer, the colored carbon powder that finally gives, it is to avoid wax and coloring agent particle are exposed to carbon
Powder particles surface, thus when solving printing and duplicate, low, the useless powder of easy roll banding, print resolution is many etc. lacks
Fall into；Further, the colored carbon powder made according to the method for the present invention, it is possible to it is same that regulation and control carbon dust particle diameter is distributed
Time, its circularity also in suitable scope (generally 0.90-0.98), overcomes the polymerization of prior art
Method is difficult to regulate and control the particle diameter distribution of carbon dust and the problem of obtained particle " too round ", makes carbon dust beat
It is easily recycled and cleans after print and duplicating.
Utilize colored carbon powder prepared by preparation method of the present invention, the fixation performance and resistance to when printing and duplicate
The most functional.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, implement below in conjunction with the present invention
Example, is clearly and completely described the technical scheme in the embodiment of the present invention, it is clear that described
Embodiment is a part of embodiment of the present invention rather than whole embodiments.Based on the enforcement in the present invention
Example, the every other reality that those of ordinary skill in the art are obtained under not making creative work premise
Execute example, broadly fall into the scope of protection of the invention.
Embodiment 1-1 prepares cinepazid polymer emulsion (a-1)
208g deionized water and 2.2g dodecyl sodium sulfate are joined the reactor with agitating device
In, it is passed through nitrogen to reactor and makes the reaction system in reactor with the air draining in reactor, heating
Temperature is maintained at about 70 DEG C, after the mixing speed of regulation agitating device is about 180rpm, and will be by 80g
Styrene monomer, 30g n-butyl acrylate monomer, 2g methacrylic acid-2-hydroxy methacrylate, 0.11g are just
The mixture that lauryl mercaptan is mixed to get is slowly added in reactor, is simultaneously added dropwise 30ml dissolved with 3.6g mistake
The deionized water of ammonium sulfate carries out polyreaction, and time for adding controls within 6h.
Chromatograph of gel permeation GPC is used to measure molecular weight and the molecular weight of polymer in polymerization reaction system
Distribution, and use differential scan calorimeter DSC to measure vitrification point Tg of polymer, when recording
The weight average molecular weight of polymer is 360000, and number-average molecular weight is 27000, and molecular weight distribution is 13.3,
And when vitrification point Tg is 65 DEG C, reaction system is cooled to room temperature, and uses 100 mesh filter screens
Filter, obtain cinepazid polymer emulsion (a-1).
Embodiment 1-2 prepares cinepazid polymer emulsion (a-2)
185g deionized water and 5g NPE are joined the reactor with agitating device
In, it is passed through nitrogen to reactor and makes the reaction system in reactor with the air draining in reactor, heating
Temperature is maintained at about 80 DEG C, after the mixing speed of regulation agitating device is about 200rpm, and will be by 40g
Styrene monomer, 20g p-methylstyrene monomer, 25g isobutyl methacrylate, 1g metering system
The mixture that acid-2-hydroxypropyl acrylate and 5g tert-dodecyl mercaptan are mixed to get is slowly added in reactor, drips simultaneously
Add 30ml and carry out polyreaction dissolved with the deionized water of 0.1g potassium peroxydisulfate, time for adding control 3h with
In.The weight average molecular weight using chromatograph of gel permeation GPC to record polymer is 145000, and number is divided equally
Son amount is 16800, and molecular weight distribution is 8.6；And use differential scan calorimeter DSC to record vitrification temperature
When degree Tg is 61 DEG C, reaction system is cooled to room temperature, uses 100 mesh filter screens to filter, obtain phenylpropyl alcohol
Polymer emulsion (a-2).
Embodiment 1-3 prepares cinepazid polymer emulsion (a-3)
180g deionized water and 3g Polyoxyethylene cetyl ether are joined the reaction with agitating device
In device, it is passed through nitrogen to reactor and makes the reactant in reactor with the air draining in reactor, heating
It is that temperature is maintained at about 90 DEG C, after the mixing speed of regulation agitating device is about 200rpm, will be by
60g styrene monomer, 28g n-BMA monomer, 2g methacrylic acid-2-hydroxy methacrylate,
The mixture that 2g n-dodecyl mereaptan is mixed to get is slowly added in reactor, is simultaneously added dropwise 30ml dissolved with 3g
The deionized water of sodium peroxydisulfate carries out polyreaction, and time for adding controls within 3h.Employing gel oozes
Chromatograph GPC records the weight average molecular weight of polymer thoroughly is 33200, and number-average molecular weight is 16000, point
Son amount is distributed as 2.2；And use differential scan calorimeter DSC to record vitrification point Tg when being 55 DEG C,
Reaction system is cooled to room temperature, uses 100 mesh filter screens to filter, obtain cinepazid polymer emulsion (a-3).
Embodiment 1-4 prepares polyester resin emulsion (a-4)
Under room temperature, 80g polyester resin NE701 (from Japanese Kao Co., Ltd.) is added 200g first and second
In ketone, after stirring makes it be completely dissolved, add 200g deionized water and 15g concentration is the hydroxide of 3%
Sodium solution, high speed dispersion 10min, butanone is distilled off with Rotary Evaporators decompression subsequently, is cooled to
After room temperature, obtaining polyester resin emulsion (a-4), recording its pH is 7.8.
The particle diameter using Malvern laser particle instrument MS2000 to record this polyester resin emulsion is 280nm,
The molecular weight using chromatograph of gel permeation GPC to record this polyester resin emulsion is 13000, molecular weight divides
Cloth is 20, and uses differential scan calorimeter DSC to record the vitrification point of this polyester resin emulsion
Tg is 56.
Embodiment 2-1 prepares wax dispersion (b-1)
By paraffin that 50g fusing point is about 60 DEG C, 1g anionic and
149g deionized water is stirred pre-dispersed 1h at 85 DEG C, then this pre-dispersed liquid is joined high pressure
Homogenizer carries out homogenous disperse, uses Malvern laser particle instrument MS 2000 to record the particle diameter model of dispersion liquid
Enclose for 80-300nm, stop dispersion, i.e. obtain wax dispersion (b-1).
Embodiment 2-2 prepares wax dispersion (b-2)
Tissuemat E, 15g Polyoxyethylene cetyl ether and 140g that 50g fusing point is about 78 DEG C are gone
Ionized water is stirred pre-dispersed 0.5h at 95 DEG C, then this pre-dispersed liquid is joined high pressure homogenizer
Middle homogenous disperse, the particle size range using Malvern laser particle instrument MS 2000 to record dispersion liquid is
100-350nm, stops dispersion, i.e. obtains wax dispersion (b-2).
Embodiment 2-3 prepares wax dispersion (b-3)
By the polyethylene that Brazil wax that 30g fusing point is about 84 DEG C, 20g fusing point are about 72 DEG C
Wax, 10g Polyoxyethylene cetyl ether and 140g deionized water are stirred pre-dispersed 2h at 90 DEG C,
Then this pre-dispersed liquid is joined homogenous disperse in high pressure homogenizer, uses Malvern laser particle instrument
It is 120-500nm that MS 2000 records the particle size range of dispersion liquid, stops dispersion, i.e. obtains wax dispersion
(b-3)。
Embodiment 3-1 prepares red colored agent dispersing liquid (c-1)
After 15g NPE is dissolved in 300g deionized water, add 95g pigment red 122 and
20g negative charge controlling agent N-4P (Clariant chemical industry (Chinese) company limited), uses high speed shear dispersion
Machine is under the speed of 3000rpm after dispersed with stirring 8h, then with group, dispersion liquid is strangled (PUHLER) grinds
Machine grinding distribution, uses Malvern laser particle instrument MS 2000 to record the particle diameter distribution of colorant dispersion
Scope stops when 120-600nm grinding, and i.e. obtains red colored agent dispersing liquid (c-1).
Embodiment 3-2 prepares yellow coloring agent dispersing liquid (c-2)
After 35g sodium lauryl sulphate is dissolved in 300g deionized water, add 95g pigment yellow 74 and 25g
Negative charge controlling agent N-23 (Clariant chemical industry (Chinese) company limited), uses high speed shear dispersion machine to exist
Under the speed of 3000rpm after dispersed with stirring 2h, then dispersion liquid group Le (PUHLER) grinder is ground
Mill dispersion, uses Malvern laser particle analyzer MS 2000 to record the particle size distribution range of colorant dispersion
Stop when 100-360nm grinding, i.e. obtain yellow coloring agent dispersing liquid (c-2).
Embodiment 3-3 prepares blue-colored agent dispersing liquid (c-3)
After 2g dodecyl sodium sulfate and 2g Polyoxyethylene cetyl ether are dissolved in 300g deionized water,
Addition 95g pigment blue 15: 3 and 25g negative charge controlling agent N-24 (Clariant chemical industry (Chinese) limited public affairs
Department), use high speed shear dispersion machine after dispersed with stirring 0.5h under the speed of 3000rpm, then will dispersion
(PUHLER) grinder grinding distribution 1h strangles in liquid group, uses Malvern laser particle analyzer MS 2000
Record the particle size distribution range of colorant dispersion to stop when 60-300nm grinding, i.e. obtain blueness
Toner dispersion liquid (c-3).
Embodiment 3-4 prepares black colorant agent dispersing liquid (c-4)
20g dodecyl sodium sulfate and 13g Polyoxyethylene cetyl ether are dissolved in 300g deionized water,
Add 95g carbon black and 25g negative charge controlling agent N-24 (Clariant chemical industry (Chinese) company limited), adopt
After dispersed with stirring 0.5h under high speed shear dispersion machine 3000rpm speed, then dispersion liquid group is strangled
(PUHLER) grinder grinding distribution, uses Malvern laser particle analyzer MS 2000 to record coloring agent
The particle size distribution range of dispersion liquid stops when 60-250nm grinding, and i.e. obtains black colorant agent dispersing liquid
(c-4)。
Embodiment 4-1 prepares red carbon powder (d-1)
At room temperature by the wax dispersion (b-1) of above-mentioned for 120g preparation, the above-mentioned preparation of 120g red colored
Agent dispersing liquid (c-1) and 200g deionized water add in the reactor with agitating device, regulate agitating device
Mixing speed be about 400rpm after, in reactor add the above-mentioned preparation of 256g cinepazid polymer
Emulsion (a-1), after stirring, with the pH value of pH meter detection mixture, with the speed of 15ml/min
Dripping 300g mass content in reactor is the dilution heat of sulfuric acid of 2%, makes mixture in reactor
PH value is 2.0, and then rising temperature of reaction system is to 45 DEG C, and uses Malvern laser particle analyzer MS
The grain diameter of 2000 detection mixture, when particle diameter reaches 8.0 μm left and right, adds in reaction system
50g mass content is the sodium hydroxide solution of 15%, and now the pH of mixture is 7.5, obtains at the beginning of carbon dust
Level particle.
The temperature of continuation rising carbon dust primary particle place system, to about 85 DEG C, is dripped in reactor simultaneously
Add by the ammonium persulfate solution that 50g mass content is 0.4%, 24g styrene, 11g butyl acrylate,
The mixture that 1g methacrylic acid-2-hydroxy methacrylate mixes carries out polyreaction.When in reaction system
When the particle diameter of particle is 9.1 μm, rising system temperature, to 105 DEG C, is incubated and uses Sysmex FIPA
The circularity of particle in 3000 detection reaction systems, in question response system, the circularity of particle is 0.952 left side
Time right, stop insulation, and reaction system is cooled down, filter, wash, be dried, obtain red solid
Body particulate matter.
Calculate by mass percentage, in red solid particulate matter, add 1% hydrophobic silica R812
(from Evnoic Degussa (SEA) Pte., Ltd) and 0.3% silicon dioxide RX50 are (from Evnoic
Degussa (SEA) Pte., Ltd), use Henschel mixer mixing, obtain red carbon powder (d-1)；Use
It is 6.8 μm that Multisizer 3 Kurt grain size analysis calculating instrument measures its volume average particle size.
Embodiment 4-2 prepares Yellow carbon powder (d-2)
At room temperature by the wax dispersion (b-2) of above-mentioned for 114g preparation, the yellow coloring of the above-mentioned preparation of 115g
Agent dispersing liquid (c-2) and 200g deionized water add in the reactor with agitating device, regulate agitating device
Mixing speed be about 400rpm after, in still, continuously add the polymer emulsion of the above-mentioned preparation of 256g
(a-2), after stirring, with the pH value of pH meter detection mixture, with the speed of 15ml/min to still
Middle dropping 300g mass content is the dilution heat of sulfuric acid of 2%, and the pH making mixture is 2.7, then raises
Temperature of reaction system is to 43.6 DEG C, and uses Malvern laser particle analyzer MS 2000 to detect the grain of mixture
Footpath, when particle diameter reaches 8.7 μm left and right, adding 45g mass content in reaction system is the hydrogen of 15%
Sodium hydroxide solution, now the pH of mixture is 7.0, obtains carbon dust primary particle.
Continue to raise the temperature of carbon dust primary particle place system to about 85 DEG C, drip in still simultaneously by
30g mass content be 0.5% ammonium persulfate solution, 22g styrene, 10g butyl acrylate, 0.5g
The mixture that methacrylic acid-2-hydroxy methacrylate mixes carries out polyreaction.When particle in reaction system
Particle diameter when being 10.5 μm, raise system temperature to 102 DEG C, be incubated and use Sysmex FIPA 3000
The circularity of particle in detection reaction system, in question response system, the circularity of particle is about 0.965
Time, stop insulation, and reaction system is cooled down, filter, wash, be dried, obtain yellow solid
Particulate matter.
Calculate by mass percentage, in yellow solid particulate matter, add 0.8% hydrophobic silica
R202 (from Evnoic Degussa (SEA) Pte., Ltd) and 0.5% silicon dioxide RX50 is (from Evnoic
Degussa (SEA) Pte., Ltd), use Henschel mixer mixing, obtain Yellow carbon powder (d-2)；Use
It is 7.1 μm that Multisizer 3 Kurt grain size analysis calculating instrument measures its volume average particle size.
Embodiment 4-3 prepares blue carbon powder (d-3)
At room temperature by the wax dispersion (b-3) of above-mentioned for 118g preparation, the above-mentioned preparation of 122g blue-colored
Agent dispersing liquid (c-3) and 200g deionized water add in the reactor with agitating device, regulate agitating device
Mixing speed be about 400rpm after, in still, continuously add the polymer emulsion of the above-mentioned preparation of 256g
(a-3), after stirring, with the pH value of pH meter detection mixture, with the speed of 15ml/min to still
Middle dropping 300g mass content is the dilution heat of sulfuric acid of 2%, and the pH making mixture is 3.4, then raises
Temperature of reaction system, to 42 DEG C, uses the particle diameter of Malvern laser particle analyzer MS 2000 test mixing thing,
When particle diameter reaches 8.0 μm left and right, it is added thereto to the sodium hydroxide that 50g mass content is 15% molten
Liquid, now the pH of mixture is 7.5, obtains carbon dust primary particle.
Continue to raise the temperature of carbon dust primary particle place system to about 85 DEG C, drip in still simultaneously by
30g mass content be 0.5% ammonium persulfate solution, 28g styrene, 7g n-BMA,
The mixture that 1g methacrylic acid-2-hydroxy methacrylate mixes carries out polyreaction.When in reaction system
When the particle diameter of particle is 9.6 μm, rising system temperature, to 98 DEG C, is incubated and uses Sysmex FIPA
The circularity of particle in 3000 detection reaction systems, in question response system, the circularity of particle is 0.964 left side
Time right, stop insulation, and reaction system is cooled down, filter, wash, be dried, obtain blue solid
Body particulate matter.
Calculate by mass percentage, in solid blue particles thing, add 1.1% hydrophobic silica
R812 (from Evnoic Degussa (SEA) Pte., Ltd) and 0.4% silicon dioxide RY50 is (from Evnoic
Degussa (SEA) Pte., Ltd), use Henschel mixer mixing, obtain blue carbon powder (d-3)；Use
It is 6.5 μm that Multisizer 3 Kurt grain size analysis calculating instrument measures its volume average particle size.
Embodiment 4-4 prepares black carbon powder (d-4)
Polymer emulsion (a-1) in embodiment 1 changes into the polymer emulsion (a-3) of above-mentioned preparation, and wax disperses
Liquid (b-1) changes the wax dispersion (b-2) of above-mentioned preparation into, and red colored agent dispersing liquid (c-1) changes above-mentioned preparation into
Black colorant agent dispersing liquid (c-4), other conditions are constant, obtain black carbon powder (d-4)；Use
It is 7.0 μm that Multisizer 3 Kurt grain size analysis calculating instrument measures its volume average particle size.
Embodiment 4-5 prepares red carbon powder (d-5)
At room temperature by the wax dispersion (b-1) of above-mentioned for 120g preparation, the above-mentioned preparation of 120g red colored
Agent dispersing liquid (c-1) and 200g deionized water add in the reactor with agitating device, regulate agitating device
Mixing speed be about 400rpm after, in reactor add the above-mentioned preparation of 335g polyester resin breast
Liquid (a-4), after stirring, with the pH value of pH meter detection mixture, with the speed of 15ml/min to
Dripping 300g mass content in reactor is the dilution heat of sulfuric acid of 2%, makes the pH of mixture in reactor
Value is 2.0, and then rising temperature of reaction system is to 40 DEG C, and uses Malvern laser particle analyzer MS
The grain diameter of 2000 detection mixture, when particle diameter reaches 8.0 μm left and right, adds in reaction system
50g mass content is the sodium hydroxide solution of 15%, and now the pH of mixture is 7.5, obtains at the beginning of carbon dust
Level particle.
The temperature of continuation rising carbon dust primary particle place system, to about 85 DEG C, is dripped in reactor simultaneously
Add by the ammonium persulfate solution that 50g mass content is 0.4%, 22g styrene, 12g butyl acrylate,
The mixture that 3g methacrylic acid-2-hydroxy methacrylate mixes carries out polyreaction.When in reaction system
When the particle diameter of particle is 9.9 μm, rising system temperature, to 105 DEG C, is incubated and uses Sysmex FIPA
The circularity of particle in 3000 detection reaction systems, in question response system, the circularity of particle is 0.965 left side
Time right, stop insulation, and reaction system is cooled down, filter, wash, be dried, obtain red solid
Body particulate matter.
Calculate by mass percentage, in red solid particulate matter, add 1% hydrophobic silica R812
(from Evnoic Degussa (SEA) Pte., Ltd) and 0.3% silicon dioxide RX50 are (from Evnoic
Degussa (SEA) Pte., Ltd), use Henschel mixer mixing, obtain red carbon powder；Use
It is 6.8 μm that Multisizer 3 Kurt grain size analysis calculating instrument measures its volume average particle size.
Comparative example 1 prepares comparative example red carbon powder (e-1)
By the wax dispersion (b-1) of above-mentioned for 120g preparation, the red colored agent dispersing liquid of the above-mentioned preparation of 120g
And 200g deionized water adds in reactor with agitating device, the stirring speed of regulation agitating device (c-1)
After degree is for about 400rpm, in still, continuously add the cinepazid polymer emulsion of the above-mentioned preparation of 326g
(a-1), after stirring, with the pH value of pH meter detection mixture, with the speed of 15ml/min to still
Middle dropping 300g mass content is the dilution heat of sulfuric acid of 2%, and the pH making mixture is 2.6, then by body
System is warming up to 42 DEG C, and uses the particle diameter of Malvern laser particle analyzer MS 2000 test mixing thing, works as grain
When footpath reaches 10 μm left and right, in reaction system, add the sodium hydroxide that 50g mass content is 15% molten
Liquid, the pH to 7.5 of regulation mixture, obtain carbon dust primary particle.
The temperature of continuation rising carbon dust primary particle place system, to about 95 DEG C, is incubated and uses
Sysmex FIPA 3000 detects the circularity of particle in reaction system, the circle of particle in question response system
When degree is about 0.951, stops insulation, and reaction system is cooled down, filter, wash, do
Dry, obtain red solid particulate matter.
Calculate by mass percentage, in red solid particulate matter, add 1% hydrophobic silica R812
(from Evnoic Degussa (SEA) Pte., Ltd) and 0.3% silicon dioxide RX50 are (from Evnoic
Degussa (SEA) Pte., Ltd), use Henschel mixer mixing, obtain comparative example red carbon powder
(e-1)；Employing Multisizer 3 Kurt grain size analysis calculating instrument measures its volume average particle size and is
7.0μm。
Comparative example 2 prepares comparative example Yellow carbon powder (e-2)
Cinepazid polymer emulsion (a-1) in comparative example 1 is changed into the cinepazid polymer emulsion of above-mentioned preparation
(a-2), wax dispersion (b-1) changes the wax dispersion (b-2) of above-mentioned preparation, red colored agent dispersing liquid (c-1) into
Changing the yellow coloring agent dispersing liquid (c-2) of above-mentioned preparation into, other conditions are constant, obtain comparative example yellow carbon
Powder (e-2).
Comparative example 3 prepares comparative example blue carbon powder (e-3)
Cinepazid polymer emulsion (a-1) in comparative example 1 is changed into the cinepazid polymer emulsion of above-mentioned preparation
(a-3), wax dispersion (b-1) changes the wax dispersion (b-3) of above-mentioned preparation, red colored agent dispersing liquid (c-1) into
Changing the blue-colored agent dispersing liquid (c-3) of above-mentioned preparation into, other conditions are constant, obtain comparative example blueness carbon
Powder (e-3).
Comparative example 4 prepares comparative example black carbon powder (e-4)
Cinepazid polymer emulsion (a-1) in comparative example 1 is changed into the cinepazid polymer emulsion of above-mentioned preparation
(a-3), wax dispersion (b-1) changes the wax dispersion (b-2) of above-mentioned preparation, red colored agent dispersing liquid (c-1) into
Changing the black colorant agent dispersing liquid (c-4) of above-mentioned preparation into, other conditions are constant, obtain comparative example black carbon
Powder (e-4).
Comparative example 5 prepares comparative example red carbon powder (e-5)
By the wax dispersion (b-1) of above-mentioned for 120g preparation, the red colored agent dispersing liquid of the above-mentioned preparation of 120g
And 130g deionized water adds in reactor with agitating device, the stirring speed of regulation agitating device (c-1)
After degree is for about 400rpm, in still, continuously add the polyester resin emulsion (a-4) of the above-mentioned preparation of 425g,
After stirring, with the pH value of pH meter detection mixture, drip in still with the speed of 15ml/min
300g mass content is the dilution heat of sulfuric acid of 2%, and the pH making mixture is 2.2, then system is heated up
To 40 DEG C, and use the particle diameter of Malvern laser particle analyzer MS 2000 test mixing thing, when particle diameter reaches
During 10 μm left and right, adding 50g mass content in reaction system is the sodium hydroxide solution of 15%, regulation
The pH of mixture to 7.5, obtains carbon dust primary particle.
The temperature of continuation rising carbon dust primary particle place system, to about 92 DEG C, is incubated and uses
Sysmex FIPA 3000 detects the circularity of particle in reaction system, the circle of particle in question response system
When degree is about 0.962, stops insulation, and reaction system is cooled down, filter, wash, do
Dry, obtain red solid particulate matter.
Calculate by mass percentage, in red solid particulate matter, add 1% hydrophobic silica R812
(from Evnoic Degussa (SEA) Pte., Ltd) and 0.3% silicon dioxide RX50 are (from Evnoic
Degussa (SEA) Pte., Ltd), use Henschel mixer mixing, obtain comparative example red carbon powder
(e-5)；Employing Multisizer 3 Kurt grain size analysis calculating instrument measures its volume average particle size and is
7.0μm。
Application examples 1
Use each colored carbon powder prepared by above-described embodiment and comparative example, with the printer of Hewlett-Packard
Color LaserJet 2600 carries out fixation performance (both pick) for representative and evaluates and durability evaluation.
1, fixation performance evaluation:
The printer that will be equipped with each colored carbon powder is placed on 12h under low temperature and low humidity (10 DEG C/RH10%) environment, so
After carry out assorted 5% coverage rate E letter specimen page and print, continuously print 2500, visual observations fixing section
Divide and whether have carbon dust roll banding, and sampling and testing bottom ash, the results are shown in Table 1.
Table 1 each colored carbon powder fixation performance evaluation result
2, durability evaluation:
The printer that will be equipped with each colored carbon powder is placed on 12h under hot and humid (35 DEG C/RH80%) environment, so
After carry out assorted 5% coverage rate E letter specimen page and print, continuously print 2500, visual observations fixing section
Divide and whether have carbon dust roll banding, and sampling and testing bottom ash, the results are shown in Table 2.
Table 2 each colored carbon powder durability evaluation result
Tables 1 and 2 result shows:
Compared with traditional emulsion polymerisation process (i.e. comparative example 1-4), the present invention is by implementing polymerization step by step
Reaction, the carbon dust primary particle surface comprising wax and coloring agent formed in preparation forms resin bag further
Coating, the colored carbon powder finally given, thus avoid wax and coloring agent particle is exposed to carbon powder particle table
Face, and then solve carbon dust defect such as easy roll banding, poor durability when printing and duplicate.
Additionally, the colored carbon powder circularity made by preparation method of the present invention is suitable, not only printing and
During duplicating, produced useless powder is few, and carbon dust is easily recycled and cleans after printing and duplicating.
Last it is noted that various embodiments above is only in order to illustrate technical scheme, rather than right
It limits；Although the present invention being described in detail with reference to foregoing embodiments, this area common
Skilled artisans appreciate that the technical scheme described in foregoing embodiments still can be repaiied by it
Change, or the most some or all of technical characteristic is carried out equivalent；And these are revised or replace
Change, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.
Claims (11)
1. the preparation method of a colored carbon powder, it is characterised in that comprise the following steps:
1) reactive component is prepared respectively:
Preparing macromolecule emulsion, described macromolecule emulsion is cinepazid polymer emulsion or polyester resin emulsion；
Wax and surfactant are added in deionized water and makes wax dispersion；
Coloring agent and surfactant are added in deionized water and makes colorant dispersion；
2) at room temperature by prepared macromolecule emulsion, wax dispersion and colorant dispersion add go from
In sub-water and disperse, the pH value of regulation mixture to less than 4 and raises system temperature, to be mixed
In thing, the particle diameter of particle reaches the pH value of regulation mixture extremely neutrality during 7-9 μm, obtains carbon dust primary grain
Son；
3) raise the temperature of carbon dust primary particle place system, and add polymerization reaction monomer and initiator enters
Row polyreaction, when the particle diameter of particle reaches 9-11 μm in question response system, makes reaction system exist
90-110 DEG C of insulation, in question response system, the circularity of particle stops insulation when being 0.90-0.98, then to instead
Answer system to carry out cooling down, separate, be dried, obtain carbon powder particle；
4) in the above-mentioned carbon powder particle made, add external additive, be mixed and made into colored carbon powder.
Preparation method the most according to claim 1, it is characterised in that control described macromolecule latex
The weight average molecular weight of liquid is 4000-1000000, and molecular weight distribution is 2-30, and vitrification point is
40-75℃。
Preparation method the most according to claim 1 and 2, it is characterised in that under oxygen-free environment,
By initiator, surfactant, styrene monomer, acrylate monomer and chain-transferring agent it is in mass ratio
(0.1-3): (0.2-5): (40-60): (10-30): (0.05-5), adding temperature is the deionized water of 70-90 DEG C
In carry out polyreaction, prepare described cinepazid polymer emulsion.
Preparation method the most according to claim 1 and 2, it is characterised in that polyester resin is added
In organic solvent, stirring to after being completely dissolved, add deionized water and alkali disperses, removing subsequently has
Machine solvent, prepares described polyester resin emulsion；Wherein, control described polyester resin, organic solvent and go
Mass ratio between ionized water is (1-5): (5-20): (6-30), and controls described polyester resin emulsion
Particle diameter be 50-500nm, pH be 6-8.
Preparation method the most according to claim 1, it is characterised in that described by alive to wax and surface
Property agent add in deionized water and make wax dispersion, including:
It is 1:(0.02-0.3 in mass ratio by wax and surfactant) add in deionized water, heating makes this
The temperature of system is disperseed higher than after the fusing point of wax, makes the wax dispersion that particle diameter is 80-500nm；
Wherein, the fusing point of described wax is 50-130 DEG C.
Preparation method the most according to claim 1, it is characterised in that described by coloring agent with table
Face activating agent adds in deionized water makes colorant dispersion, including:
By coloring agent and surfactant in mass ratio for 1:(0.02-0.4) add deionized water after carry out point
Dissipating and grind, prepared particle diameter is the colorant dispersion of 80-800nm.
Preparation method the most according to claim 1, it is characterised in that with in each reactive component
Solid contents meter, rate-determining steps 2) described in macromolecule emulsion, wax dispersion and colorant dispersion it
Between mass ratio be (30-50): (5-15): (6-20), and after dispersed with stirring raise system temperature extremely
35-50℃。
8. according to the preparation method described in claim 1 or 7, it is characterised in that step 3) in, raise
The temperature of carbon dust primary particle place system to 70-90 DEG C, and control polymerization reaction monomer and initiator it
Between mass ratio be 100:(0.3-0.6), and control solids and polymerization reaction monomer in macromolecule emulsion
Mass ratio is (1-10): 1.
Preparation method the most according to claim 1, it is characterised in that described surfactant is
Anionic surfactant and/or nonionic surfactant, described coloring agent is dyestuff and/or face
Material, described polymerization reaction monomer is selected from styrene monomer, vinyl ester monomers, (methyl) acrylate list
Body, unsaturated carboxylic acid monomer, containing one or more in halogen vinyl monomer and nitro class monomer.
Preparation method the most according to claim 1, it is characterised in that step 4) in, described carbon
Powder particles is 100:(0.1-8 with the mass ratio of external additive), described external additive is inorganic external additive
And/or organic external additive；Wherein, described inorganic external additive selected from silicon dioxide, titanium dioxide,
One or more in aluminium oxide, zinc oxide and magnesium oxide, described organic external additive is selected from polymer pearl
With one or more in metallic stearate.
11. 1 kinds of colored carbon powders, it is characterised in that according to the preparation described in any one of claim 1-10
Method prepares.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107239011A (en) * | 2017-07-15 | 2017-10-10 | 合肥皖水信息科技有限公司 | A kind of preparation method of colored carbon powder |
| CN108319119A (en) * | 2017-12-27 | 2018-07-24 | 广东丽格科技股份有限公司 | A kind of hybrid resin particle, preparation method and its application |
| CN109240051A (en) * | 2018-08-21 | 2019-01-18 | 广东丽格科技股份有限公司 | A kind of ceramics carbon dust and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102369485A (en) * | 2009-04-01 | 2012-03-07 | 日本瑞翁株式会社 | Toner for electrostatic-image development |
| CN102445869A (en) * | 2011-12-28 | 2012-05-09 | 深圳市乐普泰科技有限公司 | Colorful powdered ink used for static development and preparation method thereof |
| CN103631104A (en) * | 2012-08-24 | 2014-03-12 | 珠海莱茵柯电子有限公司 | Color toner and preparation method thereof |
-
2015
- 2015-03-17 CN CN201510117133.1A patent/CN106033175B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102369485A (en) * | 2009-04-01 | 2012-03-07 | 日本瑞翁株式会社 | Toner for electrostatic-image development |
| CN102445869A (en) * | 2011-12-28 | 2012-05-09 | 深圳市乐普泰科技有限公司 | Colorful powdered ink used for static development and preparation method thereof |
| CN103631104A (en) * | 2012-08-24 | 2014-03-12 | 珠海莱茵柯电子有限公司 | Color toner and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107239011A (en) * | 2017-07-15 | 2017-10-10 | 合肥皖水信息科技有限公司 | A kind of preparation method of colored carbon powder |
| CN108319119A (en) * | 2017-12-27 | 2018-07-24 | 广东丽格科技股份有限公司 | A kind of hybrid resin particle, preparation method and its application |
| CN109240051A (en) * | 2018-08-21 | 2019-01-18 | 广东丽格科技股份有限公司 | A kind of ceramics carbon dust and preparation method thereof |
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