CN102736458B - Method for preparing black and colorful powdered ink by gathering-fusing method - Google Patents
Method for preparing black and colorful powdered ink by gathering-fusing method Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000006185 dispersion Substances 0.000 claims abstract description 69
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 239000000049 pigment Substances 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 27
- 229920005989 resin Polymers 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 25
- 239000000839 emulsion Substances 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 21
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000498 ball milling Methods 0.000 claims abstract description 6
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
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- 238000007720 emulsion polymerization reaction Methods 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
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- 238000005406 washing Methods 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 45
- 239000003795 chemical substances by application Substances 0.000 claims description 43
- 239000000843 powder Substances 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 19
- 238000007500 overflow downdraw method Methods 0.000 claims description 16
- 239000000047 product Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000007648 laser printing Methods 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
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- 239000003921 oil Substances 0.000 claims description 5
- 230000000630 rising effect Effects 0.000 claims description 5
- 150000005846 sugar alcohols Polymers 0.000 claims description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 239000007859 condensation product Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000001056 green pigment Substances 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical class CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
- 239000001110 calcium chloride Substances 0.000 claims description 2
- 235000011148 calcium chloride Nutrition 0.000 claims description 2
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 claims description 2
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 2
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical class CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 2
- 125000004494 ethyl ester group Chemical group 0.000 claims description 2
- 235000011187 glycerol Nutrition 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
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- 229920000151 polyglycol Polymers 0.000 claims description 2
- 239000010695 polyglycol Substances 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 claims description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- MFGZXPGKKJMZIY-UHFFFAOYSA-N ethyl 5-amino-1-(4-sulfamoylphenyl)pyrazole-4-carboxylate Chemical compound NC1=C(C(=O)OCC)C=NN1C1=CC=C(S(N)(=O)=O)C=C1 MFGZXPGKKJMZIY-UHFFFAOYSA-N 0.000 claims 1
- 230000009477 glass transition Effects 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 8
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- 239000002609 medium Substances 0.000 description 3
- 239000002671 adjuvant Substances 0.000 description 2
- 239000006229 carbon black Substances 0.000 description 2
- 235000019241 carbon black Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
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- 238000005265 energy consumption Methods 0.000 description 2
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- 241001504664 Crossocheilus latius Species 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- -1 can obtain Huang Substances 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- YRIUSKIDOIARQF-UHFFFAOYSA-N dodecyl benzenesulfonate Chemical compound CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 YRIUSKIDOIARQF-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229940071161 dodecylbenzenesulfonate Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
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- 239000012530 fluid Substances 0.000 description 1
- 230000008570 general process Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- SSILHZFTFWOUJR-UHFFFAOYSA-M hexadecane-1-sulfonate Chemical compound CCCCCCCCCCCCCCCCS([O-])(=O)=O SSILHZFTFWOUJR-UHFFFAOYSA-M 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
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- 238000010298 pulverizing process Methods 0.000 description 1
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- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical class OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a method for preparing black and colorful powdered ink by a gathering-fusing method. The method comprises the steps of: 1) mutually dissolving a polyatomic alcohol solvent with deionized water to obtain a mixed solvent; 2) respectively, preparing a resin emulsion through emulsion polymerization reaction, preparing a wax dispersing liquid through high temperature emulsification and preparing a pigment dispersing liquid and a charge adjustor dispersing liquid through ball milling dispersion by taking the mixed solvent as a medium; 3) mixing the resin emulsion, the wax dispersing liquid, the pigment dispersing liquid and the charge adjustor dispersing liquid according to proportion at room temperature, and agitating uniformly; adjusting pH of the system to 1-2 and heating to 40-600 DEG C, and forcibly agitating for 1-3 hours to obtain clusters of 10-15 microns; 4) raising the temperature to 100-1200 DEG C, forcibly agitating for 3-5 hours, and fusing the clusters gradually to form solid particles; and 5) cooling, filtering, washing and airing to obtain the powdered link. The method provided by the invention is simple in process, convenient and safe, and high in production efficiency.
Description
Technical field
The present invention relates to laser printing/xerox with the preparation method of ink powder, the present invention relates to the method that a kind of logical overbunching – fusion method prepares the color laser printing ink powder particularly.
Background of invention
Along with the development of office automation with popularize, the application of laser printing and Xeroxing is increasingly extensive, and is correspondingly huge as the ink powder demand of printing/duplicate main consumptive material, become the main growth point of the industry output value and profit.
Ink powder (or be called toner, Toner) be the particulate aggregate that comprises compositions such as pigment, charge adjusting agent (℃ ℃ A), lubricant based on resin.At present, the ink powder preparation method can be divided into traditional fusion comminuting method, chemical polymerization and Ju Ji – fusion method three major types type.
Traditional fusion comminuting method is that to place mixing roll to mediate on the resin melt temperature by a certain percentage resin, colorant and other composition mixing, the gained fused mass through extrude, cool off, pulverizing, classification, adding adjuvant obtain finished product.This technical matters is easy, production efficiency is high, (problem can be too not outstanding in black and white is printed for these problems but the homogeneity of ingredients of ink powder particle is relatively poor, shape irregularity, size-grade distribution are wide etc., but the quality for colour print will produce great adverse effect), energy consumption height, noise and the dust harzard of production run are big besides.
Chemical polymerization is that " growth " powder rather than " grinding " obtain powder [as USP5648193A, 4983488,6582873,65666028,6740463,6528222, EP0162577,0225476,0302939,0631196], its process generally is that the oil phase that includes monomer, initiating agent, pigment and adjuvant is mixed with water, add spreading agent and handle through mulser, obtain the water base suspending liquid of micro-droplet of oil, the polymerization of heating trigger monomer, oil droplet is solidified into particle, collects drying and obtains ink powder.Compare with traditional fusion comminuting method, properties of product of chemical polymerization good (the regular spherical in shape or elliposoidal of powder shape, narrow particle size distribution, composition are even) etc., be suitable for preparing high-quality particularly color toner, the production run energy consumption is low, the feature of environmental protection good (be medium with water in the preparation process, do not use high temperature and high-tenacity to pulverize).But there are limitations such as technology controlling and process complexity, conditional request strictness, production efficiency be low in this straight polymerization powder process method.
Gathering-fusion method [as: USP5290654,5308734,5403693,6582873,7560505B2] be a kind of change and progress on the chemical method basis, it is the advanced ink powder technology of preparing that combines traditional method and chemical polymerization advantage, its general process is: the aqueous emulsion for preparing the nano-resin ball by emulsion polymerization, the aqueous-based dispersions for preparing materials such as pigment, wax, charge adjusting agent by ball milling respectively, various dispersion liquids are stable with surfactant (spreading agent); In proportion various dispersion liquids are mixed, the environmental baseline of regulation system (adding salt or acid, alkali etc.) produces the flocculation phenomenon, and ultrafine dust is assembled the loose cluster of formation micron order, and the loose cluster growth conditions of control makes its size unlikely excessive; Heating impels loose cluster fusion to form fine and close, and the spheroidization that uses high pressure vessel to carry out particle under higher temperature is handled; Particle obtains product through collection, washing and drying.Ju Ji – fusion method has been inherited the characteristics of the best in quality and process environmental protection of chemical polymerization, also has the simple advantage of traditional method technology concurrently.
The basic step of Ju Ji – fusion method is the aqueous-based dispersions of the various raw materials of preparation, and the successful dispersions in aqueous medium such as the resin of organism attribute, pigment, wax, charge adjusting agent depend on the selection of effective surface activating agent (spreading agent).Spreading agent mainly uses ion-type (negative ion/kation), as institute's dodecyl benzene sulfonate, cetyl sulfonate, dodecyl polyethoxy carboxylate, cetyl trialkyl amine salt, N-dodecyl pyridiniujm etc., regulate its effectiveness because ionic dispersant can change by ionic strength or pH value, the particulate in the initiation dispersed system produces assembles trend.
Yet, the aqueous systems that utilization comprises above-mentioned spreading agent prepares dispersion liquid (its particle diameter requires at 100 – 300nm) by emulsification or ball milling, the use of spreading agent is generally controlled in a few percent mass concentration scope, the dispersion fluid viscosity was big when dispersant concentration was big, foamability is serious, will bring great trouble and difficulty to technological process.Such situation brings some outstanding problems for present Ju Ji – fusion method: for example the solid content of dispersion liquid is not high, finally makes the preparation efficiency (batch output) lower (total solid content 10 – 15wt.% in the mixed liquor) of ink powder; All need to surpass 1000 ℃ temperature for another example in the spheroidization process of wax emulsion preparation and particle, this means that these processes must the working pressure container, and obviously there is the problem of convenience and security in such operating conditions.
Summary of the invention
In order to overcome the shortcoming of prior art, the invention provides the method that a kind of Ju Ji – fusion method prepares black, color toner, its technology is simple, and is convenient and safe, the production efficiency height.
The present invention solves the technical scheme that its technical matters takes: comprise the following steps: 1) polyalcohols solvent and deionized water are dissolved each other in the ratio of 1:1 – 4w/w, obtain the mixed type solvent, the content of polyvalent alcohol is 20-50wt.%; 2) be medium with above-mentioned mixed solvent, prepare resin emulsion by emulsion polymerization respectively, the solid content of resin emulsion is 15-30wt.%, prepare wax dispersion by high temperature emulsification, the solid content of wax dispersion is 20 – 40wt.%, disperse preparation dispersible pigment dispersion and charge adjusting agent dispersion liquid by ball milling, the solid content of dispersible pigment dispersion and charge adjusting agent dispersion liquid is all 20-40wt.%; 3) at room temperature, resin emulsion, wax dispersion, dispersible pigment dispersion and charge adjusting agent dispersion liquid are mixed in proportion, stir, described ratio is the 75-85wt.% that resin emulsion accounts for gross mass, wax dispersion 5-15wt.%, dispersible pigment dispersion accounts for 5-10wt.%, and the charge adjusting agent dispersion liquid accounts for 1-5wt.%; The pH value of regulation system is to 1-2 and be heated to 600 ℃ of 40 –, is the powerful 1 – 3h of stirring under the 1000 – 2000rpm at rotating speed, obtains the cluster of 10 –, 15 μ m; 4) rising temperature to 100 – is 1200 ℃, is the powerful 3 – 5h of stirring under the 1000 – 2000rpm at rotating speed, and cluster is fused into solid particle gradually; 5) be cooled to 30 ℃ of 20 –, filter, wash, dry with 1000 –, 3000 order sand core funnels, obtain ink powder, powder is subsphaeroidal, size is about 10 μ m.
1), technology is simple, convenient and safe, the production efficiency height the present invention has following advantage:.2), can provide have enough electric charge load capacity, the ink powder of satisfactory thermal parameters combination (can soften rapidly when being heated photographic fixing and flow, energy is rapidly solidified when breaking away from the high-temperature region) and appropriate particle size.
Embodiment
The present invention includes the following step: 1) polyalcohols solvent and deionized water are dissolved each other in the ratio of 1:1 – 4w/w, obtain the mixed type solvent, the content of polyvalent alcohol is 20 – 50wt.%; 2) be medium with above-mentioned mixed solvent, prepare resin emulsion by emulsion polymerization respectively, the solid content of resin emulsion is 15 – 30wt.%, prepare wax dispersion by high temperature emulsification, the solid content of wax dispersion is 20 – 40wt.%, disperse preparation dispersible pigment dispersion and charge adjusting agent dispersion liquid by ball milling, the solid content of dispersible pigment dispersion and charge adjusting agent dispersion liquid is all 20 – 40wt.%; 3) at room temperature, resin emulsion, wax dispersion, dispersible pigment dispersion and charge adjusting agent dispersion liquid are mixed in proportion, stir, described ratio is the 75 – 85wt.% that resin emulsion accounts for gross mass, wax dispersion 5 – 15wt.%, dispersible pigment dispersion accounts for 5 – 10wt.%, and the charge adjusting agent dispersion liquid accounts for 1 – 5wt.%; PH value to 1 – 2 of regulation system also is heated to 600 ℃ of 40 –, is the powerful 1 – 3h of stirring under the 1000 – 2000rpm at rotating speed, obtains the cluster of 10 –, 15 μ m; 4) rising temperature to 100 – is 1200 ℃, is the powerful 3 – 5h of stirring under the 1000-2000rpm at rotating speed, and cluster is fused into solid particle gradually; 5) be cooled to 30 ℃ of 20 –, filter, wash, dry with 1000-3000 order sand core funnel, obtain ink powder, powder is subsphaeroidal, size is about 10 μ m.
Described polyalcohols solvent is ethylene glycol, glycerine, ethylene glycol condensation product and polyglycol (PEG100 – 800) etc.
Described ethylene glycol condensation product comprises diglycol, triethylene-glycol, tetraethylene-glycol.
The preparation of described resin emulsion comprises the following steps: that (1) is dissolved in 0.5 gram potassium persulfate, 0.42 gram sodium bicarbonate and 6.8 gram methacrylic acid-β-carboxylic ethyl esters in the blending agent, be put in the conical flask stand-byly as A liquid, described 140 gram blending agents are the potpourri that 100 gram deionized waters and 40 restrain ethylene glycol; (2) in 1 liter of three mouthfuls of reaction flask, add blending agent, 2 gram neopelexes, 78 gram styrene, 15.4 gram butyl acrylates and 2.5 gram lauryl mercaptans respectively, the A liquid that adds 28 grams again, behind the mixing pH value is adjusted to 9, handled 5 minutes with mulser then, rotating speed is 10000rpm, and described 260 gram blending agents are the potpourri of 180 gram deionized waters and 80 gram ethylene glycol; (3) reaction bulb device for mechanical stirrer, stirring rate are 800rpm, and the oil bath heating after temperature reaches 700 ℃, drips A liquid remaining in the conical flask, dropwises in 2 hours; Drip off the back 800 ℃ of insulations of 70 – 5 hours, stop reaction, be chilled to room temperature and namely get nano level resin emulsion, particle diameter is 80 – 100nm.Get the partial tree fat liquor, add CaCl2 strong solution breakdown of emulsion, through suction filtration, washing, drying, get powdery resin: solid content is less than 20wt.%, Mw=1.3 * 105, Tg=550 ℃, Tf1/2(2.5Kg adds stone roller)=110 ℃.
The preparation of described wax dispersion comprise the following steps: (1) with 80 the gram Tissuemat Es (
MP950 ℃) and 60 gram ethylene glycol add in 500 ml beakers, be heated to 1300 ℃ of 120 –, under 500 – 1000rpm rotating speeds, stirred 1 – 2 hours, to the wax mixing that liquefies fully; (2) add the deionized water that 80 grams contain 1 gram neopelex again, under 1200 ℃, handle twice with mulser, each 5 minutes, rotating speed is 10000rpm, be powerful the stirring 1 hour under the 1000-2000rpm at rotating speed then, be quickly cooled to room temperature afterwards under brute force stirs, get wax dispersion: particle diameter is less than 250nm, and solid content is less than 40wt.%.
The preparation of described dispersible pigment dispersion comprises the following steps:
The preparation of a, black pigment dispersion liquid: in 80 gram blending agents, add 20 gram carbon blacks (N990) and 0.5 gram neopelex, potpourri places satellite-type bowl mill ball grinder to grind 24 hours, can obtain black pigment dispersion liquid (particle diameter ~ 400nm, solid content ~ 20wt.%); Described 80 gram blending agents are the potpourri of 40 gram deionized waters and 40 gram ethylene glycol; Described satellite-type bowl mill ball grinder rotating speed is rotating speed 500rpm, and zirconium pearl diameter is Φ 2 – 3mm.
The preparation of b, Huang, product, green pigment dispersion liquid: use pigment yellow-74(Pigment Yellow-74 respectively), paratonere-122(Pigment Red-122) and phthalocyanine blue (β-CuPc) replace carbon black in the preparation of described black pigment dispersion liquid, can obtain Huang, product, green pigment dispersion liquid respectively: particle diameter is less than 200nm, and solid content is less than 20wt.%.
The preparation of described charge adjusting agent dispersion liquid comprises the following steps: that (1) is in 90 gram blending agents, a kind of charge adjusting agent that adds 20 grams, salicyclic acid derivatives zinc complex for example, and 1 the gram neopelex, potpourri places satellite-type bowl mill ball grinder to grind 24 hours, can obtain the charge adjusting agent dispersion liquid: particle diameter is less than 300nm, and solid content is less than 20wt.%; Described 90 gram blending agents are the potpourri of 60 gram deionized waters and 30 gram ethylene glycol; The rotating speed that grinds in the described satellite-type bowl mill ball grinder is 500rpm, and zirconium pearl diameter is Φ 2-3mm.
The preparation of powdered black ink comprises the following steps: under (1) room temperature, resin emulsion, 15 grams, 20wt.% black pigment dispersion liquid, 10 grams, 40wt.% wax dispersion and 3 grams with 150 grams, 20wt.%, in the there-necked flask that the adding of 20wt.% charge adjusting agent dispersion liquid is 250 milliliters, mixing and stirring; (2) regulate pH and be not more than 1, be heated to 50-60 ℃, the powerful stirring 1-3 hour obtains the cluster of 10 –, 15 μ m under the 2000-5000rpm rotating speed; (3) rising temperature to 110 – is 1150 ℃, and continues to stir, and rotating speed is 1000 – 1500rpm, and the time is 3 – 5 hours, and cluster progressively is fused into solid particle, and powder is subsphaeroidal, the about 10 μ m of size; (4) be cooled to 30 ℃ of 20 –, filter, wash, dry with 1000 –, 3000 order sand core funnels; (5) the improved silica powder of adding 20 – 30nm, addition is the 1wt.% of gained grain weight amount, as adding composition outward, obtains being applicable to the powdered black ink of laser printing.
The preparation of Huang, product, cyan ink powder comprises the following steps: to adopt the preparation process of described powdered black ink, replace described black pigment dispersion liquid with Huang, product, green pigment dispersion liquid respectively, can obtain being applicable to Huang, product, the cyan ink powder of color laser printing.
The present invention is specified by above instantiation.It is pointed out that in spirit of the present invention and the scope stated, can make some variations and modification.Therefore, above-mentioned specific embodiment is not for restriction the present invention.
Claims (8)
1. one kind is gathered the method that collection – fusion method prepares black, color toner, it is characterized in that: comprise the following steps: 1) polyalcohols solvent and deionized water are dissolved each other in the ratio of 1:1 – 4w/w, obtain the mixed type solvent, the content of polyvalent alcohol is 20 – 50wt.%; 2) be medium with above-mentioned mixed solvent, prepare resin emulsion by emulsion polymerization respectively, the solid content of resin emulsion is 15 – 30wt.%, prepare wax dispersion by high temperature emulsification, the solid content of wax dispersion is 20 – 40wt.%, disperse preparation dispersible pigment dispersion and charge adjusting agent dispersion liquid by ball milling, the solid content of dispersible pigment dispersion and charge adjusting agent dispersion liquid is all 20 – 40wt.%; 3) at room temperature, resin emulsion, wax dispersion, dispersible pigment dispersion and charge adjusting agent dispersion liquid are mixed in proportion, stir, described ratio is the 75 – 85wt.% that resin emulsion accounts for gross mass, wax dispersion 5 – 15wt.%, dispersible pigment dispersion accounts for 5 – 10wt.%, and the charge adjusting agent dispersion liquid accounts for 1 – 5wt.%; PH value to 1 – 2 of regulation system also is heated to 60 ℃ of 40 –, is that brute force stirred 1 – 3 hours under the 1000 – 2000rpm at rotating speed, obtains the cluster of 10 –, 15 μ m; 4) rising temperature to 100 – is 120 ℃, is that brute force stirred 3 – 5 hours under the 1000 – 2000rpm at rotating speed, and cluster is fused into solid particle gradually; 5) be cooled to 30 ℃ of 20 –, filter, wash, dry with 1000 –, 3000 order sand core funnels, obtain ink powder, powder is subsphaeroidal, size is about 10 μ m.
2. Ju Ji – fusion method according to claim 1 prepares the method for black, color toner, it is characterized in that: described polyalcohols solvent is ethylene glycol, glycerine and ethylene glycol condensation product.
3. Ju Ji – fusion method according to claim 2 prepares the method for black, color toner, and it is characterized in that: described ethylene glycol condensation product is diglycol, triethylene-glycol, tetraethylene-glycol and polyglycol.
4. Ju Ji – fusion method according to claim 1 prepares the method for black, color toner, it is characterized in that: the preparation of described resin emulsion comprises the following steps: that (1) is dissolved in 0.5 gram potassium persulfate, 0.42 gram sodium bicarbonate and 6.8 gram methacrylic acid-β-carboxylic ethyl esters in the blending agent of being made up of 100 gram deionized waters and 40 gram ethylene glycol, is put in the conical flask stand-by as A liquid; (2) in 1 liter of three mouthfuls of reaction flask, add blending agent, 2 gram neopelexes, 78 gram styrene, 15.4 gram butyl acrylates and the 2.5 gram lauryl mercaptans formed by 180 gram deionized waters and 80 gram ethylene glycol respectively, the A liquid that adds 28 grams again, behind the mixing pH value is adjusted to 9, handled 5 minutes with mulser then, rotating speed is 10000rpm; (3) reaction bulb device for mechanical stirrer, stirring rate are 800rpm, and the oil bath heating after temperature reaches 70 ℃, drips A liquid remaining in the conical flask, dropwises in 2 hours; Drip off the back 80 ℃ of insulations of 70 – 5 hours, stop reaction, be chilled to room temperature and namely get nano level resin emulsion, particle diameter is 80 – 100nm.Get the partial tree fat liquor, add CaCl2 strong solution breakdown of emulsion, through suction filtration, washing, drying, get powdery resin: solid content～20wt.%, weight-average molecular weight Mw=1.3 * 105, glass transition temperature Tg=55 ℃, Tf1/2=110 ℃.
5. Ju Ji – fusion method according to claim 1 prepares the method for black, color toner, it is characterized in that: the preparation of described wax dispersion comprises the following steps: that (1) adds 80 gram Tissuemat Es and 60 gram ethylene glycol in 500 ml beakers, be heated to 130 ℃ of 120 –, under 500 – 1000rpm rotating speeds, stirred 1 – 2 hours, to the wax mixing that liquefies fully; (2) add the deionized water that 80 grams contain 1 gram neopelex again, under 120 ℃, handle twice with mulser, each 5 minutes, rotating speed is 10000rpm, be powerful the stirring 1 hour under the 1000 – 2000rpm at rotating speed then, be quickly cooled to room temperature afterwards under brute force stirs, get wax dispersion: particle diameter is less than 250nm, and solid content is less than 40wt.%.
6. Ju Ji – fusion method according to claim 1 prepares the method for black, color toner, it is characterized in that: the preparation of described charge adjusting agent dispersion liquid comprises the following steps: that (1) is in 90 gram blending agents, the charge adjusting agent zinc salicylate complex compound that adds 20 grams, and 1 the gram neopelex, potpourri places satellite-type bowl mill ball grinder to grind 24 hours, can obtain the charge adjusting agent dispersion liquid: particle diameter is less than 300nm, solid content～20wt.%; Described 90 gram blending agents are the potpourri of 60 gram deionized waters and 30 gram ethylene glycol; The rotating speed that grinds in the described satellite-type bowl mill ball grinder is 500rpm, and zirconium pearl diameter is Φ 2 – 3mm.
7. Ju Ji – fusion method according to claim 1 prepares the method for black, color toner, it is characterized in that: the preparation of powdered black ink comprises the following steps: under (1) room temperature, the charge adjusting agent dispersion liquid of the wax dispersion of the black pigment dispersion liquid of the resin emulsions of 150 gram 20wt.%, 15 gram 20wt.%, 10 gram 40wt.% and 3 gram 20wt.% added in 250 milliliters the there-necked flask mixing and stirring; (2) regulate pH and be not more than 1, be heated to 60 ℃ of 50 –, powerful stirring 1 – is 3 hours under 2000 – 5000rpm rotating speeds, obtains the cluster of 10 –, 15 μ m; (3) rising temperature to 110 – is 115 ℃, and continues to stir, and rotating speed is 1000 – 1500rpm, and the time is 3 – 5 hours, and cluster progressively is fused into solid particle, and powder is subsphaeroidal, the about 10 μ m of size; (4) be cooled to 30 ℃ of 20 –, filter, wash, dry with 1000 –, 3000 order sand core funnels; (5) the improved silica powder of adding 20 – 30nm, addition are that the 1wt.% conduct of gained grain weight amount is added composition outward, obtain being applicable to the powdered black ink of laser printing.
8. Ju Ji – fusion method according to claim 7 prepares the method for black, color toner, it is characterized in that: the preparation of Huang, product, cyan ink powder comprises the following steps: to replace described black pigment dispersion liquid with Huang, product, green pigment dispersion liquid respectively, can obtain being applicable to Huang, product, the cyan ink powder of color laser printing.
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| CN103345133B (en) * | 2013-06-27 | 2016-03-02 | 金发科技股份有限公司 | A kind of color toner and preparation method thereof |
| CN104330960A (en) * | 2014-10-20 | 2015-02-04 | 中国科学院化学研究所 | Anionic nano wax emulsion as well as preparation method and application thereof |
| CN104360584A (en) * | 2014-11-27 | 2015-02-18 | 邯郸汉光办公自动化耗材有限公司 | Preparation method and application of nano charge control agent dispersion liquid |
| CN105527806A (en) * | 2015-12-21 | 2016-04-27 | 邯郸汉光办公自动化耗材有限公司 | Preparation method of electropositive color toner employing chemical method |
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| US6268102B1 (en) * | 2000-04-17 | 2001-07-31 | Xerox Corporation | Toner coagulant processes |
| JP2004117588A (en) * | 2002-09-24 | 2004-04-15 | Fuji Photo Film Co Ltd | Electrophotographic image receiving sheet and image forming method |
| US6835768B2 (en) * | 2002-08-28 | 2004-12-28 | Xerox Corporation | Wax dispersions and process thereof |
| CN1706889A (en) * | 2004-06-04 | 2005-12-14 | 施乐公司 | Wax emulsion for emulsion aggregation toner |
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|---|---|---|---|---|
| US6268102B1 (en) * | 2000-04-17 | 2001-07-31 | Xerox Corporation | Toner coagulant processes |
| US6835768B2 (en) * | 2002-08-28 | 2004-12-28 | Xerox Corporation | Wax dispersions and process thereof |
| JP2004117588A (en) * | 2002-09-24 | 2004-04-15 | Fuji Photo Film Co Ltd | Electrophotographic image receiving sheet and image forming method |
| CN1706889A (en) * | 2004-06-04 | 2005-12-14 | 施乐公司 | Wax emulsion for emulsion aggregation toner |
| JP2005346083A (en) * | 2004-06-04 | 2005-12-15 | Xerox Corp | Wax emulsion for emulsion aggregation toner |
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