CN102585519A - Modified wax dispersing agent and preparation method of latex agglutination powdered ink - Google Patents
Modified wax dispersing agent and preparation method of latex agglutination powdered ink Download PDFInfo
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- CN102585519A CN102585519A CN2011104542180A CN201110454218A CN102585519A CN 102585519 A CN102585519 A CN 102585519A CN 2011104542180 A CN2011104542180 A CN 2011104542180A CN 201110454218 A CN201110454218 A CN 201110454218A CN 102585519 A CN102585519 A CN 102585519A
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Abstract
The invention provides a modified wax dispersing agent, which is prepared by preparing initial wax particles by using a phase inversion emulsification method and sequentially encapsulating the wax particles through polymer resin. The preparation method comprises the following steps of: carrying out a phase inversion emulsification method on wax, one or a plurality of emulsifiers and water at a temperature higher than the wax melting point so as to obtain initial wax particles, sequentially adding an alcohol solvent, monomers and an initiator into the system and carrying out dispersion polymerization reaction for encapsulating the wax particles, and afterwards, cooling to the environmental temperature so as to obtain the modified wax dispersing agent. The encapsulated wax particle has a core-shell structure that the core is wax and the external layer is resin; the particle diameter of the encapsulated wax particle is 0.1-2.0 microns; by wrapping the external wax layer with the resin layer, the compatibility of the wax and binder resin can be improved effectively; and the wax can be dispersed uniformly in ink powder, has a good compatibility with the resin and has a uniform particle size distribution. The latex agglutination powdered ink further provided by the invention and prepared from the wax dispersing agent has good photographic fixing performance and has no phenomenon of photosensitive drum film formation and developer roller pollution.
Description
[technical field]
The present invention relates to stamping machine or copier technology field, relate to emulsion aggegation ink powder and use the wax dispersion preparation method, and relate to the emulsion aggegation ink powder that comprises the wax that has wherein strengthened the system consistency, belong to field of functional materials.
[background technology]
Wax is widely used in the industrial circles such as foodstuffs industry, pharmaceuticals, makeup at present.Employed wax amount accounts for the total amount consumed less than 1% of wax in stamping machine or duplicating machine.But, for the laser printer ink powder,, wax is added in the ink powder configuration material can assist ink powder to get loose from fixing roller for satisfying low oil or not having in the fusion roller design of oil, therefore, wax is one of integral constituent material of ink powder particle.Especially recently, when advancing energy-conservationization of stamping machine or manifolder, wax is considered to be used to make the most important material of necessary low-temperature fixing ink powder.
The interpolation of wax not only can play a significant role as parting agent when hot photographic fixing, and wax can reduce the rub resistance etc. that ink powder to the pollution of developer roll, effectively strengthens the glossiness of print image and improves image.The increase of wax addition can effectively improve the elevated temperature excursions temperature, but the wax amount of ink powder is too much, will run counter to desire to the release improvement of heat fixing roll, and making to the control scraper of developer or the film forming on the photoreceptor to become problem.On the other hand, when wax and resin glue consistency were bad, the wax particle that exposes at toner surface will increase, and can cause comparatively fast taking place film forming equally.
The ink powder developer has carried out broad research to ink powder with the particle diameter and the control method of wax in ink powder.Earlier tiny wax particle dispersion is added to organic phase, organic phase is added to preparation ink powder dispersion liquid in the water phase surfactant mixture.This method can effectively reduce the formation of no wax and surface wax ink powder particle, but this method has very high selectivity to the kind of wax.Another kind method is, is added to preparation ink powder dispersion liquid in the water phase surfactant mixture after wax directly is dissolved in organic solvent, afterwards organic solution evaporated, and uses the pollution that causes to reduce the later stage ink powder.This method can reduce the effective size of grain of wax particle in the ink powder, but the adding of organic solvent has increased the difficulty of later stage toner particle diameter control, and resin and wax particle can not be realized active adsorption and then influence the later stage fixing performance.
[summary of the invention]
Technical problem to be solved by this invention is the defective that overcomes above-mentioned prior art, provide a kind of can be homodisperse in ink powder, with resin compatible preferably, the wax particle dispersion and the preparation method of even particle size distribution.
For achieving the above object; The present invention at first provides a kind of modified waxes dispersion liquid; It is to prepare initial wax particle through phase conversion emulsifying; And then form through the encapsulated wax particle preparation of fluoropolymer resin, it is that nuclear, polymkeric substance are the nucleocapsid structure particle of shell that said encapsulated wax particle adopts dispersion copolymerization method to form with wax, the particle diameter of described encapsulated wax particle is at the 0.1-2.0 micron.
Above-mentioned modified waxes dispersion liquid preparation method provided by the invention may further comprise the steps:
1) in reaction flask, add wax, heating up dissolves it fully;
2) treat that wax dissolves fully after, add emulsifying agent, high-speed stirring makes its dissolving, dispersion, oil phase disperses fully;
3) add the certain temperature deionized water, disperse preparation water/oily dispersion liquid;
4) in system, add the certain temperature deionized water again, disperse preparation oil/aqueous dispersions;
5) reduce temperature to normal temperature;
6) alcoholic solvent is added in the initial wax dispersion ultra-sonic dispersion;
7), under the common agitation condition, the homogeneous mixture solotion of monomer, initiator is slowly dropped to above-mentioned system 70 ℃ of temperature;
8) it is subsequent use to reduce to room temperature after isothermal reaction for some time.
The present invention also provides a kind of emulsion aggegation ink powder preparation method; It is with the modified waxes dispersion liquid of above-mentioned preparation and contains binder resin emulsion, one or more tinting materials, CCA dispersion liquid and one or more additive emulsion aggegations formation agglutinator; Wherein: modified waxes is 5-30%Wt, contains adhesive resin 60-90%Wt, and the tinting material add-on is the 1-30%Wt of ink powder; The CCA addition is ink powder 0.1-7%Wt, and additive is 0.1-5%Wt; Cohesion or the above-mentioned agglutinator of fusion reclaim the after scouring drying then, and promptly obtaining median size is the emulsion aggegation toner particles of 5-15 micron.
Wax dispersion of the present invention is with the outer resin-coated layer of wax particle; It is that wax, skin are the nucleocapsid structure of resin that this encapsulated wax particle has kernel; Since resin layer can select for use with ink powder with resin glue consistency material preferably; Thereby can effectively improve the consistency and the adsorptivity of wax particle and resin glue, realize the homodisperse of wax particle in the ink powder particle.
Wax dispersion preparation technology of the present invention is simple, prepared wax dispersion with the consistency of resin glue and in the ink powder particle uniform distribution property all be improved.On the one hand, owing to adopt the phase reversion emulsion process to prepare wax dispersion, resulting wax dispersion particle diameter is less, is beneficial to the uniform distribution of later stage aggegation process in the ink powder particle, has reduced the appearance of no wax and surface wax ink powder particle; On the other hand, as seed, effectively improved the sympathy with resin glue at the outer resin-coated layer of wax with initial wax particle through dispersion copolymerization method.Getting wax dispersion with unmodified conventional emulsification method compares; The resulting modified waxes dispersion liquid of this method has small particle size, narrow diameter distribution concurrently, than the characteristics of high-compatibility; Be preferred for the preparation of chemical method ink powder particle, more preferably be used for emulsion agglutination ink powder preparation technology.
The fixing toner performance that contains above-mentioned modified waxes dispersion liquid of the present invention's preparation is good, no photosensitive drums film forming, developer roll contamination phenomenon.
[description of drawings]
Fig. 1 is the process flow sheet of modified waxes dispersion liquid preparation of the present invention.
[embodiment]
For realizing the object of the invention,, the present invention is done further detailed description below in conjunction with embodiment.Should be appreciated that specific embodiment described herein, only be used to explain the present invention, and be not used in qualification the present invention.
The present invention at first provides a kind of modified waxes dispersion liquid, and it is to prepare initial wax particle through phase conversion emulsifying, and then forms through the encapsulated wax particle preparation of fluoropolymer resin.
It is that nuclear, polymkeric substance are the nucleocapsid structure particle of shell that wherein said encapsulated wax particle adopts dispersion copolymerization method to form with wax, and the particle diameter of described encapsulated wax particle is at the 0.1-2.0 micron.
Above-mentioned wax dispersion passes through the outer resin-coated layer of wax particle; The formation kernel is that wax, skin are the nucleocapsid structure of resin; Since resin layer can select for use with ink powder with resin glue consistency material preferably; Thereby can effectively improve the consistency and the adsorptivity of wax particle and resin glue, can obtain the less encapsulated wax particle of particle diameter, thereby realize the homodisperse of wax particle in the ink powder particle.
Referring to Fig. 1, the concrete preparation of above-mentioned wax dispersion may further comprise the steps:
1) in reaction flask, add wax, heating up dissolves it fully;
2) treat that wax dissolves fully after, add emulsifying agent, high-speed stirring makes its dissolving, dispersion, oil phase disperses fully;
3) deionized water of adding certain temperature disperses preparation water/oily dispersion liquid;
4) in system, add the deionized water of a large amount of certain temperatures again, disperse preparation oil/aqueous dispersions;
5) reduce temperature to normal temperature;
6) alcoholic solvent is added in the initial wax dispersion ultra-sonic dispersion;
7), under the common agitation condition, the homogeneous mixture solotion of monomer, initiator is slowly dropped to above-mentioned system 70 ℃ of temperature;
8) it is subsequent use to reduce to room temperature after isothermal reaction for some time.
The preparation method of above-mentioned wax dispersion is dissolved the back fully at wax and is adopted the phase reversion emulsion process, can make resulting wax dispersion particle diameter less, helps the uniform distribution of later stage aggegation process in the ink powder particle, has reduced the appearance of no wax and surface wax ink powder particle.Simultaneously; As seed, at the outer resin-coated layer of wax, effectively improved sympathy with initial wax particle with resin glue through dispersion copolymerization method in the subsequent step; Resulting wax dispersion has small particle size, narrow diameter distribution concurrently, has higher consistency with resin.
Above-mentioned steps 1) in, the kind of wax can be selected according to product needed, and its kind can comprise natural waxs such as rice bran wax, POLISHING WAX-103, gama wax, montanin wax; Oil such as petroleum wax, Microcrystalline Wax is a wax; Polyene wax, Fischer-synthetic waxs such as Top's method synthetic wax; Multifunctional ester cpds such as tetramethylolmethane four cetylates, pentaerythritol tetramyristate, Dipentaerythritol six myristinates, pentaerythritol tetrastearate, the present invention can be that a kind of or two or more combinations in the above-mentioned wax are used.
Above-mentioned steps 1) Heating temperature will be higher than the melting temperature of wax in, to melt this wax.Typically, required Heating temperature is than at least 5 ℃ of the fusing point height of wax or higher, and preferably than the high 10-40 of fusing point ℃ of wax, higher Heating temperature causes less Wax particles to produce usually in the wax dispersion goods.
Above-mentioned steps 2) emulsifying agent is made up of one or more tensio-active agents in.The tensio-active agent of any kind can use, and comprises anionic, cationic and non-ionics, can be independent a kind of use, also can be that two or more mixing is used.
AS comprises sodium laurylsulfonate, X 2073, dodecyl naphthalene sodium sulfate.Cats product comprises the dialkyl benzene alkyl ammomium chloride, lauryl trimethyl ammonium chloride, alkyl benzyl ammonio methacrylate, alkyl benzyl dimethyl brometo de amonio, Trimethyllaurylammonium bromide, methacryloxypropyl methyl trimethoxy ammonium chloride etc.Non-ionics comprises Z 150PH, polyoxyethylene glycol, ROHM; Methylcellulose gum, TKK 021 propyl cellulose, polyoxyethylene cetyl ethers; The polyoxyethylene lauryl ether, polyoxyethylene Octyl Ether polyoxyethylene stearyl ether, polyoxyethylene nonylplenyl ether etc.
Above-mentioned steps 2) the emulsifying agent consumption should rationally be controlled in, is prerequisite to reach guarantee system stability.Said emulsifying agent consumption should be the 1%-20% of wax consumption, preferred 2%-15%.
Above-mentioned steps 3) the deionized water temperature should be not less than the melting temperature of wax in, than at least 5 ℃ of the fusing point height of wax or higher, preferably than the high 10-40 of fusing point ℃ of wax.
Above-mentioned steps 3) the deionized water add-on should not be higher than the consumption of wax in, and then prepares initial W/O dispersion system.The deionized water add-on can be the 5%-70%Wt of the consumption of wax, preferred 10%-60%Wt.
Above-mentioned steps 4) deionized water temperature and above-mentioned steps 3 in) in the hot water temperature near or suitable.
Above-mentioned steps 4) the deionized water add-on should be far above the consumption of wax in, be preferably wax consumption 1-5 doubly.
Above-mentioned steps 5) cooling method can adopt the method for any appropriate to realize in, for example lowers the temperature naturally, or needs and fixed speed cooling with 5 ℃ of PMs or certificate.
Above-mentioned steps 6) alcoholic solvent is generally methyl alcohol, ethanol, propyl alcohol etc. in, and system alcohol water proportioning can be controlled preferred 20/1-1/1 according to the system needs.Usually, can also add an amount of stablizer according to the system needs, like described suitable tensio-active agents of preamble such as Vinylpyrrolidone polymer PVP, polyoxyethylene glycol PEG.
Above-mentioned steps 7) initiator can comprise water-soluble and oil-soluble initiator in.As water soluble starter, can enumerate persulfate initiators such as ammonium persulphate, Potassium Persulphate; 2,2 '-azo two (2-methyl-N-(2-hydroxyethyl) propionic acid amide), 2, the two azo series initiators such as (2-methyl-N-(1, two (methylol) 2-hydroxyethyls of 1-) propionic acid amides) of 2 '-azo etc.As oil-soluble initiator, can enumerate Lucidol, peroxo-and peroxo-class initiator and oil soluble azo initiators such as Diisopropyl azodicarboxylate, ABVN such as the tertiary butyl, lauroyl peroxide.
The amount of above-mentioned initiator is generally the 0.1-20%Wt of shell monomers weight, preferred 0.5-10%Wt.Polymerization temperature is preferably greater than 40 ℃, more preferably 70-100 ℃.In addition, preferred 1-25 of reaction times hour, more preferably 2-15 hour.At last, polymerization process optionally adopts nitrogen atmosphere protection monomer radical.
Above-mentioned steps 7) shell monomers is made up of one or more polymerizable monomers in, like mono-vinyl monomer, cross-linkable monomer etc.This shell monomers becomes the resin shell of wax particle through polymerization.As vinyl monomer, can select aromatic ethenyl monomers such as vinylbenzene, vinyl toluene, Vinyl toluene for use; Monoolefine monomer such as ethene, propylene; Vinylformic acid and verivate series monomers thereof such as methyl acrylate, ethyl propenoate, Bing Xisuandingzhi, cyclohexyl acrylate, TEB 3K, Jia Jibingxisuanyizhi, Rocryl 400, SY-Monomer G.Can select Vinylstyrene, isoprene, 1,3-butadiene etc. for use as cross-linkable monomer.
Wax dispersion of the present invention most preferably is used as the additive of emulsion aggegation ink powder.Therefore the present invention further comprises wax dispersion is applied to form emulsion aggegation ink powder; The basic process steps of said emulsion aggegation ink powder comprises: with the modified waxes dispersion liquid of above-mentioned preparation method preparation with contain binder resin emulsion, one or more tinting materials, CCA dispersion liquid and one or more additive emulsion aggegations and form agglutinator; Cohesion or this agglutinator of fusion reclaim after the dry acquisition of washing median size is the emulsion aggegation toner particles of 5-15 micron subsequently.
Among the preparation method of above-mentioned emulsion aggegation ink powder:
The addition of modified waxes is the 5-30%Wt of ink powder.
Binder resin emulsion can be through the emulsion polymerisation process preparation, and exemplary monomer can comprise vinylbenzene, esters of acrylic acid such as methyl acrylic ester, Bing Xisuandingzhi etc.; Vinylformic acid, methylacrylic acid, divinyl; Isoprene, vinyl cyanide, any in the Vinylstyrene etc. or several kinds.Known chain-transfer agent comprises for example lauryl mercaptan or carbon tetrabromide etc.The addition of adhesive resin is the 60-90%Wt of ink powder.
Various known tinting materials can hard-corely comprise carbon black, nigrosine, pigment of all kinds and mixture etc.The tinting material add-on can be the 1-30%Wt of ink powder.
Flocculation agent can comprise polyvalent metal muriate or inorganic polymer flocculation agent such as sulphate, Poly aluminum Chloride (PAC) such as metallic aluminium, MAGNESIUM METAL 99.Poly aluminum Chloride (PAC) (PAC) is preferred because of strong adsorption bridging effect.The addition of flocculation agent is ink powder 0-5%Wt.
Any suitable charge control agent can be chosen arbitrarily, and the CCA of electronegative type generally uses azo metal complex or salicylic acid complex etc., and positively charged type CCA generally uses quaternary ammonium salt, nigrosine, triphenylmethane compound etc.The addition of charge control agent is ink powder 0.1-7%Wt.
The microparticle that additive adds for purpose for the static behaviour of further adjustment ink powder, flowability, storage stability etc.The additive granules particle diameter is generally less than the ink powder particle.For example, inorganic particle is generally MOXs such as silicon-dioxide, titanium oxide, zinc oxide.Wherein, preferred through the silica dioxide granule of hydrophobization processing.The addition of additive does not have special qualification, is generally ink powder 0.1-5%Wt.
Below in conjunction with embodiment further detailed description is done in the preparation of wax dispersion of the present invention and emulsion aggegation ink powder.Need to prove that hereinafter, " part " and " % " then refers to " weight part " and " %Wt " respectively if no special instructions.
Among the following embodiment, the modified waxes particle dispersion of nucleocapsid structure is suitably diluted, use the civilian BI-90Plus nanometer in Brooker sea/submicron laser particle size analyzer that its particle diameter is measured.
Among the following embodiment, the emulsion aggegation of employing uses resin emulsion A to be styrene-propene butyl acrylate copolymer resin emulsion.This emulsion adopts ammonium persulphate as initiator, and positive Dodecyl Mercaptan prepares through emulsion polymerisation process as chain-transfer agent.Vinylbenzene and Butyl Acrylate Monomer weight proportion are 75: 25.This emulsion solid content is 30%, and second-order transition temperature is 55 ℃.
Among the following embodiment, the emulsion aggegation of employing uses carbon black dispersion liquid to be the ionic dispersion liquid, and content of carbon black is 15%.The CCA dispersion liquid is an ionic, and CCA content is 2%.
Embodiment 1:
(1) preparation of wax dispersion:
In four-hole bottle, add 100 parts in wax, be warming up to 95 ℃, its complete dissolving wax is dissolved fully, add emulsifying agent DOW 2A110 part.After treating that oil phase dissolves fully, add 60 parts of water (95 ℃), disperse 60min; In system, add 160 parts in 95 ℃ of water, reduce temperature normal temperature behind the insulation 30min naturally.
220 parts of ethanol are added to above-mentioned system, are transferred to common agitation condition behind the ultra-sonic dispersion 30min, be warming up to 70 ℃, and logical nitrogen protection.
125 parts of Bing Xisuandingzhis that are dissolved with 5 parts of AIBN are slowly dropped in the above-mentioned system, stablize under the dispersed with stirring condition, reacting after 8 hours cooling, to obtain median size be 0.6 micron modified waxes particle.
(2) preparation of emulsion aggegation ink powder:
With 100 parts of resin emulsions, 20 parts of dispersible pigment dispersions, 15 parts of wax dispersions, 40 parts of quaternary ammonium salt CCA dispersion liquids mix in deionized water, let agglomeration generate.
Add 15 parts of 1% Poly aluminum Chloride (PAC) salpeter solutions, be warming up to 75 ℃ after dropwising, guarantee that agglomeration continues to increase.Treat that particle growth to volume average particle size is approximately 8 microns, add the silicon dioxide granule that 1 part of hydrophobization is handled, be heated to 85 ℃, agglutination particle combines together.
After the cooling of above-mentioned ink powder particle, clean, dry with alkali lye, pure water, promptly obtain the ink powder particle of 8 microns of median sizes.
Embodiment 2:
(1) preparation of wax dispersion:
In four-hole bottle, add 150 parts in wax, be warming up to 95 ℃, its complete dissolving wax is dissolved fully, add emulsifying agent DOW 2A115 part.After treating that oil phase dissolves fully, add 60 parts of water (95 ℃), disperse 60min; In system, add 200 parts in 95 ℃ of water, reduce temperature behind the insulation 30min naturally to normal temperature.
4400 parts of ethanol are added to above-mentioned system, are transferred to common agitation condition behind the ultra-sonic dispersion 30min, be warming up to 70 ℃, and logical nitrogen protection.
150 parts of Bing Xisuandingzhis that are dissolved with 2 parts of AIBN are slowly dropped in the above-mentioned system, stablize under the dispersed with stirring condition, reacting after 8 hours cooling, to obtain median size be 0.3 micron modified waxes particle.
(2) preparation of emulsion aggegation ink powder:
The preparation method obtains 6 microns ink powder particles of median size with embodiment 1.
Embodiment 3:
(1) preparation of wax dispersion:
In four-hole bottle, add 100 parts in wax, be warming up to 95 ℃, its complete dissolving wax is dissolved fully, add emulsifying agent DOW 2A13 part.After treating that oil phase dissolves fully, add 60 parts of water (95 ℃), disperse 60min; In system, add 160 parts in 95 ℃ of water, reduce temperature behind the insulation 30min naturally to normal temperature.
220 parts of ethanol are added to above-mentioned system, are transferred to common agitation condition behind the ultra-sonic dispersion 30min, be warming up to 70 ℃, and logical nitrogen protection.
125 parts of Bing Xisuandingzhis that are dissolved with 0.63 part of AIBN are slowly dropped in the above-mentioned system, stablize under the dispersed with stirring condition, reacting after 8 hours cooling, to obtain median size be 2 microns modified waxes particles.
(2) preparation of emulsion aggegation ink powder:
The preparation method obtains 15 microns ink powder particles of median size with embodiment 1.
Embodiment 4:
(1) preparation of wax dispersion:
In four-hole bottle, add 80 parts in wax, be warming up to 95 ℃, its complete dissolving wax is dissolved fully, add emulsifying agent DOW 2A110 part.After treating that oil phase dissolves fully, add 60 parts of water (95 ℃), disperse 60min; In system, add 400 parts in 95 ℃ of water, reduce temperature behind the insulation 30min naturally to normal temperature.
220 parts of ethanol are added to above-mentioned system, are transferred to common agitation condition behind the ultra-sonic dispersion 30min, be warming up to 70 ℃, and logical nitrogen protection.
125 parts of Bing Xisuandingzhis that are dissolved with 12.5 parts of AIBN are slowly dropped in the above-mentioned system, stablize under the dispersed with stirring condition, reacting after 8 hours cooling, to obtain median size be 0.6 micron modified waxes particle.
(2) preparation of emulsion aggegation ink powder:
The preparation method obtains 8 microns ink powder particles of median size with embodiment 1.
Embodiment 5:
(1) preparation of wax dispersion:
In four-hole bottle, add 100 parts in wax, be warming up to 95 ℃, its complete dissolving wax is dissolved fully, add emulsifying agent DOW 2A110 part.After treating that oil phase dissolves fully, add 60 parts of water (95 ℃), disperse 60min; In system, add 160 parts in 95 ℃ of water, reduce temperature behind the insulation 30min naturally to normal temperature.
220 parts of ethanol are added to above-mentioned system, are transferred to common agitation condition behind the ultra-sonic dispersion 30min, be warming up to 70 ℃, and logical nitrogen protection.
125 parts of TEB 3Ks that are dissolved with 5 parts of AIBN are slowly dropped in the above-mentioned system, stablize under the dispersed with stirring condition, reacting after 8 hours cooling, to obtain median size be 0.6 micron modified waxes particle.
(2) preparation of emulsion aggegation ink powder:
The preparation method obtains 8 microns ink powder particles of median size with embodiment 1.
Embodiment 6:
(1) preparation of wax dispersion:
In four-hole bottle, add 100 parts in wax, be warming up to 95 ℃, its complete dissolving wax is dissolved fully, add emulsifying agent DOW 2A110 part.After treating that oil phase dissolves fully, add 60 parts of water (95 ℃), disperse 60min; In system, add 160 parts in 95 ℃ of water, reduce temperature behind the insulation 30min naturally to normal temperature.
220 parts of ethanol are added to above-mentioned system, are transferred to common agitation condition behind the ultra-sonic dispersion 30min, be warming up to 70 ℃, and logical nitrogen protection.
100 parts of SY-Monomer Gs that are dissolved with 10 parts of AIBN are slowly dropped in the above-mentioned system, stablize under the dispersed with stirring condition, reacting after 8 hours cooling, to obtain median size be 0.6 micron modified waxes particle.
(2) preparation of emulsion aggegation ink powder:
The preparation method obtains 8 microns ink powder particles of median size with embodiment 1.
Embodiment 7:
(1) preparation of wax dispersion: in four-hole bottle, add 100 parts in wax, be warming up to 95 ℃, its complete dissolving wax is dissolved fully, add 10 parts of emulsifying agent DOW 2A1.After treating that oil phase dissolves fully, add 10 parts of water (95 ℃), disperse 60min; In system, add 300 parts in 95 ℃ of water, reduce temperature behind the insulation 30min naturally to normal temperature.
220 parts of ethanol are added to above-mentioned system, are transferred to common agitation condition behind the ultra-sonic dispersion 30min, be warming up to 70 ℃, and logical nitrogen protection.
180 parts of Rocryl 400s that are dissolved with 15 parts of AIBN are slowly dropped in the above-mentioned system, stablize under the dispersed with stirring condition, reacting after 8 hours cooling, to obtain median size be 0.6 micron modified waxes particle.
(2) preparation of emulsion aggegation ink powder:
The preparation method obtains 8 microns ink powder particles of median size with embodiment 1.
In embodiment 6,7; The adding of function monomer; Hydroxyl and epoxide group are introduced system, and it can interact with the carboxyl of carbon blacksurface or phenolic hydroxyl group or carry out chemical reaction, so be beneficial to disperse and stable ink powder particle in carbon black; Reduce the possibility that later stage temperature-rise period carbon black leaks, and promote the homodisperse of carbon black in the ink powder particle.
The above embodiment has only expressed the preferred embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art under the prerequisite that does not break away from the present invention's design, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with accompanying claims.
Claims (12)
1. a modified waxes dispersion liquid is characterized in that, it is to prepare initial wax particle through phase conversion emulsifying, and then forms through the encapsulated wax particle preparation of fluoropolymer resin.
2. modified waxes dispersion liquid according to claim 1 is characterized in that, it is that nuclear, polymkeric substance are the nucleocapsid structure particle of shell that said encapsulated wax particle adopts dispersion copolymerization method to form with wax.
3. modified waxes dispersion liquid according to claim 2 is characterized in that the particle diameter of described encapsulated wax particle is at the 0.1-2.0 micron.
4. one kind like each described modified waxes dispersion liquid preparation method of claim 1-3, it is characterized in that, may further comprise the steps:
1) in reaction flask, add wax, heating up dissolves it fully;
2) treat that wax dissolves fully after, add emulsifying agent, high-speed stirring makes its dissolving, dispersion, oil phase disperses fully;
3) add the certain temperature deionized water, disperse preparation water/oily dispersion liquid;
4) in system, add a large amount of certain temperature deionized waters again, disperse preparation oil/aqueous dispersions;
5) reduce temperature to normal temperature;
6) alcoholic solvent is added in the initial wax dispersion ultra-sonic dispersion;
7), under the common agitation condition, the homogeneous mixture solotion of monomer, initiator is slowly dropped to above-mentioned system 70 ℃ of temperature;
8) it is subsequent use to reduce to room temperature after isothermal reaction for some time.
5. modified waxes dispersion liquid preparation method according to claim 4; It is characterized in that; Wax in the said wax dispersion is that natural wax, oil are wax, synthetic wax or multifunctional ester cpds, for a kind of or two or more combination in the above-mentioned wax is used.
6. modified waxes dispersion liquid preparation method according to claim 4 is characterized in that, said preparation process 2) in emulsifying agent form by one or more tensio-active agents, the consumption of said emulsifying agent is the 1%-20% of wax consumption.
7. modified waxes dispersion liquid preparation method according to claim 4 is characterized in that, said preparation process 3), 4) in the Phase inversion emulsification temperature of reaction higher more than 5 ℃ or 5 ℃ than the fusing point of wax.
8. modified waxes dispersion liquid preparation method according to claim 4 is characterized in that, said preparation process 6) in alcoholic solvent adopt methyl alcohol or ethanol, its alcohol/water is than being 20/1-1/1.
9. modified waxes dispersion liquid preparation method according to claim 4 is characterized in that, said preparation process 7) in monomer be that mono-vinyl monomer, cross-linkable monomer or two kinds mix and use, the weight ratio of said monomeric addition and wax is 100: 50-200.
10. modified waxes dispersion liquid preparation method according to claim 9 is characterized in that, said mono-vinyl monomer be use separately aromatic vinyl monomer, and with aromatic vinyl monomer and acrylic ester monomer.
11. modified waxes dispersion liquid preparation method according to claim 4 is characterized in that, said preparation process 7) in initiator be water-soluble or oil-soluble initiator, the addition of said initiator and the weight ratio of resin monomer are 100: 0.5-10.
12. emulsion aggegation ink powder preparation method; It is characterized in that aforesaid right is required the modified waxes dispersion liquid of each preparation of 4-10 form agglutinator with containing binder resin emulsion, one or more tinting materials, CCA dispersion liquid and one or more additive emulsion aggegations, wherein: modified waxes is 5-30%Wt; Contain adhesive resin 60-90%Wt; The tinting material add-on is the 1-30%Wt of ink powder, and the CCA addition is ink powder 0.1-7%Wt, and additive is 0.1-5%Wt; Cohesion or the above-mentioned agglutinator of fusion reclaim the after scouring drying then, and promptly obtaining median size is the emulsion aggegation toner particles of 5-15 micron.
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| CN (1) | CN102585519A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102718911A (en) * | 2012-06-18 | 2012-10-10 | 中国科学院化学研究所 | Wax wrapped type nano resin emulsion and preparation method and application thereof |
| CN103034079A (en) * | 2012-12-27 | 2013-04-10 | 深圳市乐普泰科技股份有限公司 | Suspension polymerization toner with densely charged core-shell structure and preparation method |
| CN104385593A (en) * | 2014-10-15 | 2015-03-04 | 西安交通大学 | Atomization technology-based light-cured rapid prototyping product surface roughness reducing method |
| 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 |
| CN107903946A (en) * | 2017-10-24 | 2018-04-13 | 昆明理工大学 | A kind of preparation method of montanin wax resin distillate |
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| CN101271292A (en) * | 2008-04-30 | 2008-09-24 | 王恒来 | Anti-counterfeit durable colorful ink powder and method for producing the same |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718911A (en) * | 2012-06-18 | 2012-10-10 | 中国科学院化学研究所 | Wax wrapped type nano resin emulsion and preparation method and application thereof |
| CN102718911B (en) * | 2012-06-18 | 2014-01-29 | 中国科学院化学研究所 | Wax wrapped type nano resin emulsion and preparation method and application thereof |
| CN103034079A (en) * | 2012-12-27 | 2013-04-10 | 深圳市乐普泰科技股份有限公司 | Suspension polymerization toner with densely charged core-shell structure and preparation method |
| CN103034079B (en) * | 2012-12-27 | 2015-04-22 | 深圳市乐普泰科技股份有限公司 | Method for producing suspension polymerization toner with densely charged core-shell structure |
| CN104385593A (en) * | 2014-10-15 | 2015-03-04 | 西安交通大学 | Atomization technology-based light-cured rapid prototyping product surface roughness reducing method |
| CN104385593B (en) * | 2014-10-15 | 2016-06-29 | 西安交通大学 | Light-cured rapid prototype component surface roughness based on atomization technique reduces method |
| 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 |
| CN107903946A (en) * | 2017-10-24 | 2018-04-13 | 昆明理工大学 | A kind of preparation method of montanin wax resin distillate |
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Application publication date: 20120718 |