CN101798477B - Thermal transfer ink jet ink nano capsule and preparation method thereof - Google Patents
Thermal transfer ink jet ink nano capsule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a thermal transfer ink jet ink nano capsule and a preparation method thereof. Scattered dye is dissolved in styrene monomer, crylic acid monomer and functional monomer to be mixed into an organic phase; emulsifier is dissolved into distilled water to form aqueous phase; the organic phase is added into the aqueous phase for pre-emulsification to obtain pre-emulsion; emulsifier is dissolved into distilled water, pH value is adjusted to 5-6, and deoxidation is carried out to rise temperature; when temperature rises to 65-70 DEG C, 6-60% of pre-emulsion A is added; when temperature rises to 72-75 DEG C, part of initiator is added to react at the temperature of 75-85 DEG C to form the seed of miniemulsion; residual pre-emulsion A and initiator are dropwise added; temperature rises for curing; and the nano capsule can be obtained by tertiary filtration. The jet ink of the invention realizes nano capsulation, has favourable storage stability and use stability and smooth printing and does not block the sprayer; temperature in the transfer printing process can be controlled by controlling ink density in the control and modulation process of capsulation wall formed by combining different monomers to realize once total transfer or multiple transfers.
Description
Technical field
The invention belongs to fine chemistry industry and light industry field, be specifically related to a kind of thermal transfer ink jet ink nano capsule and technology of preparing.
Background technology
The method of tradition printing technology is to design the stamp pattern earlier, and the artificial colour separation retouches original text plate-making; Generally prepare 8-12 cover dyes in different colors mill base according to color separation; Stamp on roller printing machine, circular screen printer or screen printing machine then, decatize or high temperature curing fixation, reduction clearing; Washing, oven dry at last.There is complex procedures in this technology, is prone to make mistakes, long flow path, cost are high, pollute shortcomings such as big, and the stamp precision is not high, color rendition is poor, can not small serial production, more can not be to the mechanically resistant material stamp.Along with the mode of life transformation of social development, people's pursuing individuality and the enhancing of environmental consciousness; Vigorously advocate in society under the background of energy-saving and emission-reduction; The heat sublimation transfer printing is arisen at the historic moment; And the brand-new printing technology of, less energy-consumption meticulous, personalized with its height, zero release caused the revolution of whole industry, and it will certainly replace traditional printing technology, but the costliness of the particularly hot transfer ink water price of heat sublimation material lattice is restricting the development of China's heat sublimation transfer techniques always.Therefore, carry out the research and development of hot transfer printing ink particularly important.The technology of preparing of a kind of thermal transfer ink jet ink nano capsule that the present invention relates to has reduced the dyestuff loss in the dyeing process with the dispersed dye Nano capsuleization, has kept color reducibility and the storage and the stability in use of the excellence of dyestuff.Simultaneously, the ink that the present invention relates to is a water-based system, greatly reduces its pollution to environment in preparation and use.
Domestic research for hot transfer printing ink; Chinese patent grant number CN 1111192C discloses a kind of thermal transfer print ink for colour printer; But it adopts the blending means of a kind of like this physics of high-speed stirring, and lower and this invention of efficient does not relate to the explanation of size and these aspects of dispersion stabilization; Chinese patent publication number CN 1443808A discloses the preparation method of microcapsule disperse dye, but its capsule grain diameter is distributed as 2～14 μ m, be difficult to satisfy the desktop printer shower nozzle to the ink particle diameter preferably less than the requirement of 300nm; Chinese patent publication number CN 1978552A discloses a kind of preparation method of nano-coloring material aqueous dispersions, and this invention only relates to color ink jet printed, does not relate to hot transfer printing; Chinese patent publication number CN 101245204A discloses a kind of preparation method of thermal sublimation digit printing ink-jet writing ink; Wherein comprise dispersed dye, dispersion agent, tensio-active agent, wetting agent, skimmer and organic solvent; The organic solvent amount big (60～90%) that this invention is used can cause bigger pollution to environment in preparation and use.
The ink that the present invention relates to is a water-based system; Greatly reduce its pollution in preparation and use to environment; And the Nano capsule size distribution that forms is 80～300nm, has excellent colour characteristics and dispersion stabilization, has satisfied desktop well and has printed the requirement to particle diameter.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of preparation method of thermal transfer ink jet ink nano capsule is provided.It is smooth to utilize this preparation method to obtain the prepared ink printed of thermal transfer ink jet ink nano capsule, does not stop up shower nozzle, and color reducibility is good, the heat transfer printing of the fabric that is specially adapted to become more meticulous, clothes, pottery etc.
To achieve these goals, the present invention adopts following technical scheme:
A kind of preparation method of thermal transfer ink jet ink nano capsule comprises the steps, following percentage number average refers to mass percent.
(1) preparation pre-emulsion A
The preparation of organic phase: dispersed dye are dissolved in styrene monomer, acrylic monomer and the functional monomer of removing stopper mix the formation organic phase;
The preparation of water: emulsifiers dissolve is formed water in zero(ppm) water;
The preparation of pre-emulsion A: organic phase is slowly added in the container that fills the stirring of water band in room temperature, stir, under ice-water bath, place the preparatory emulsification of ultrasonic clarifixator to obtain pre-emulsion then;
(2) mini-emulsion polymerization prepared in reaction Nano capsule
The preparation of reaction bed material: in zero(ppm) water, it is 5～6 that the agent of adding pH regulator makes the pH value of system with emulsifiers dissolve, and deoxygenation begins to heat up.
The preparation of nano capsule dispersant liquid: when temperature rises to 65～70 ℃, in above-mentioned reaction bed material, add 6～60% pre-emulsion A.When temperature rises to 72～75 ℃, add the part initiator, the amount of part initiator accounts for 5～20% of total initiator total amount, keeps temperature to react 30～40min down for 75～85 ℃, forms the seed of miniemulsion; Equal speed drips remaining pre-emulsion A in 3～3.5h then, simultaneously the equal fast remaining initiator that drips in 3.5～4h; After all dropwising, be warming up to 86～90 ℃ of slakings;
(3),, obtain nano capsule dispersant liquid through 1 μ m, 0.45 μ m, 0.22 μ m three-stage filtration with above-mentioned synthetic product.
In above-mentioned preparation method, said acrylic monomer is one or both mixing in vinylformic acid, methylacrylic acid, methyl acrylate, TEB 3K, ethyl propenoate, Bing Xisuandingzhi, TGM 1 and the Hydroxyethyl acrylate; Said styrene monomer refers to one or both mixing in vinylbenzene and the divinylbenzene; Said functional monomer refers to diacetone-acryloamide(DAA) and adipic dihydrazide.
In above-mentioned preparation method, the quality summation of said styrene monomer, functional monomer and acrylic monomer is 150～500% of dispersed dye, and wherein the mass ratio of styrene monomer and acrylic monomer is 1～5: 1.The diacetone-acryloamide(DAA) consumption is 1～3% of total quality of material, and is preferred 1.5～2%, and the mass ratio of diacetone-acryloamide(DAA) and adipic dihydrazide is 100: 0.5～1.
In above-mentioned preparation method; Emulsifying agent described in said step (1) or the step (2) is preferably nonylphenol class Soxylat A 25-7 (NP-10; NP-30; NP-40), different tridecanol polyoxyethylene ether (TO-9; TO-20, TO-40), the one or more kinds of mixtures of sodium lauryl sulphate, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate (DB45), sulfo-succinic acid disodium ethoxylated alcohol half ester (A102), alkyl diphenyl base oxide stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate (2A1), wherein the consumption of emulsifying agent is 1.5～25% of amount of dye and styrene monomer, function monomer and an acrylic monomer quality summation.
In above-mentioned preparation method, said dispersed dye are preferably anthraquinone type, azo-type, cationic or quinoline type.
In above-mentioned preparation method, said initiator is preferably a kind of in Ammonium Persulfate 98.5, Sodium Persulfate or the Potassium Persulphate, and consumption is 0.1～1.5 of total quality of material; The pH regulator agent is NaHCO
3, sodium acetate one or both mix, consumption is 0.01～0.5% of total quality of material.
In above-mentioned preparation method, the stir speed (S.S.) of the said stirring of step (1) is preferably 1000rpm, mixes churning time and is preferably 20～30min; During said preparatory emulsification, the ultrasonic power of ultrasonic clarifixator is preferably 300～500W, and emulsification times is preferably 15～20min in advance.
In above-mentioned preparation method, being formulated as of step (2) said reaction bed material: in zero(ppm) water, and adding the pH regulator agent, to make the pH value of system be 5～6 with emulsifiers dissolve.And this mixed solution all packed in the four-hole reaction kettle that is connected to stirring, TM, prolong and nitrogen tube, under the stir speed (S.S.) of 200rpm, feed the nitrogen deoxygenation of 15～25min earlier.
Compared with prior art, the present invention has following beneficial effect:
The dispersed dye molecule that the hot transfer ink jet of the present invention uses is many aromatic ring structures or condensed ring structure, and this structure makes itself and water, alcohol and multiple solvent and the consistency extreme difference that is connected material, is prone to layering and assembles.The present invention is because the functional monomer diacetone-acryloamide(DAA) (DAAM) that adopts has hydrogen bond action with dye molecule; Grappling dispersed dye molecule, adipic dihydrazide (ADH) constitutes cross-linking system with DAAM, makes dyestuff be difficult for reuniting; Some tridimensional networks and the spatial stability mechanism of while polymkeric substance; Make dyestuff surface adsorption one deck resin, when dye particles was drawn close, this floor height Molecularly Imprinted Polymer was with mutual tied up in knots; Cause dye particles to lose certain freedom of movement, can keep dye particles metastable suspension in system.
The thermal transfer ink jet ink nano capsule that provides among the present invention can obtain thermal transfer ink jet ink after modulation; Can be applied on the color printer; Utilize computer export target pattern; Output to pattern on the transfer paper with ink printed provided by the invention by stamping machine again, again through heat transfer machine pattern transfer to special medium, like cloth, textile garment, porcelain, metal, crystal etc.Red, yellow, blue, black, pale red, light blue six color ink jet ink can be provided, greatly satisfy personalized demand, solve the supply and demand problem of short run customization, convenient and swift.It is good that the actual proof of using, jetting ink of the present invention also have a color reducibility, and it is inner and combines closely with it that dyestuff can infiltrate medium fully through certain temperature and pressure, not fugitive color; Jetting ink of the present invention has been realized Nano capsuleization simultaneously, therefore has excellent stability in storage and stability in use, prints smoothness and does not stop up shower nozzle; And can be through the control of the formed cyst wall of combining different monomers and the control of modulation process ink inside concentration, the height of controlled temperature in transfer process can be realized once transfer printing or repeatedly transfer printing fully.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that following embodiment will help to understand the present invention, but do not limit content of the present invention.
Embodiment 1 (redness)
Prescription is formed:
Organic phase: 13 gram Red-60 200 dyestuffs (structural formula is seen formula I), 17 gram vinylbenzene, 2 gram diacetone-acryloamide(DAA)s, 3 gram Bing Xisuandingzhis, 3 gram Hydroxyethyl acrylates, 1 gram methylacrylic acid, 0.016 gram adipic dihydrazide;
Water: 1.5 gram NP-30,2.2 gram 2Al, 20 gram zero(ppm) water;
Reaction bed material: 1 gram NP-30,0.9 gram sodium lauryl sulphate, 0.014 gram NaHCO
3, 20 gram zero(ppm) water;
Primary initiator: 0.05 gram SPS, 2 gram zero(ppm) water;
Back initiator: 0.25 gram SPS, 13.07 gram zero(ppm) water.
The preparation method is following:
(1) preparation of pre-emulsion:
The preparation of organic phase: 13 gram Red-60 200s are dissolved in 13 grams have removed the vinylbenzene of stopper, 6 gram diacetone-acryloamide(DAA)s, 3 gram Bing Xisuandingzhis, 3 gram Hydroxyethyl acrylates, 1 gram methylacrylic acid forms organic phase in the 0.036 gram adipic dihydrazide;
The preparation of water: 1.5 gram NP-30 and 2.2 gram 2A1 emulsifiers dissolves are formed water in 20 gram zero(ppm) water;
The preparation of pre-emulsion A: organic phase is slowly added in the container that fills the stirring of water band in room temperature, and stir speed (S.S.) 1000rpm mixes churning time 20～30min.Under ice-water bath, place the emulsification in advance of ultrasonic clarifixator then, its ultrasonic power is 300～500W, obtains pre-emulsion behind emulsification 15～20min in advance.
(2) mini-emulsion polymerization prepared in reaction Nano capsule
The preparation of reaction bed material: 1 gram NP-30 and 0.9 is restrained the sodium lauryl sulphate emulsifiers dissolve in 20 gram zero(ppm) water, and add 0.014 gram NaHCO
3As the pH regulator agent, the pH value that makes system is 5～6.And this mixed solution all packed in the four-hole reaction kettle that is connected to stirring, TM, prolong and nitrogen tube, under the stir speed (S.S.) of 200rpm, feed the nitrogen deoxygenation of 15～25min earlier, begin to heat up.
The preparation of nano capsule dispersant liquid: when temperature rises to 65～70 ℃, in above-mentioned reaction bed material, add the prepared pre-emulsion A of 10% claim 1.When temperature rises to 72～75 ℃, drip the distilled water solution (just causing) of initiator with peristaltic pump, first initiator is 0.05 gram SPS and the aqueous solution of 2 gram dissolved in distilled water, keeps 75～85 ℃ of temperature reaction 30～40min down, the seed of formation miniemulsion; Then in 3h all speed drip the remaining pre-emulsion A of claim preparation, simultaneously in 3.5h all speed drip remaining initiator solution (back initiator), back initiator is 0.25 to restrain the aqueous solution that SPS and 13 restrains dissolved in distilled water.After all dropwising, be warming up to 88 ℃ of slaking 1h.
At last, with above-mentioned synthetic product,, obtain the nano capsule dispersant liquid target product through 1 μ m, 0.45 μ m, 0.22 μ m three-stage filtration.
Embodiment 2 (Huang)
Prescription is formed:
Organic phase: 12 gram DISPERSE YELLOW 54 dyestuffs (structural formula is seen formula II), 15 gram vinylbenzene, 1.5 gram diacetone-acryloamide(DAA)s, 3.5 gram Bing Xisuandingzhis, 3 gram Hydroxyethyl acrylates, 1 gram methylacrylic acid, 0.01 gram adipic dihydrazide;
Water: 1.8 gram TO-20,1.9 gram 2A1,22 gram zero(ppm) water;
Reaction bed material: 0.9 gram TO-20,1.1 gram A102,0.015 gram NaHCO
3, 20.87 gram zero(ppm) water
Primary initiator: 0.055 gram SPS, 2 gram zero(ppm) water;
Back initiator: 0.35 gram SPS, 13 gram zero(ppm) water.
The preparation method is with embodiment 1.
Embodiment 3 (blueness)
Prescription is formed:
Organic phase: 12 gram EX-SF DISPERSE BLUE EX-SF 300 14 dyestuffs (structural formula is seen formula III), 15 gram vinylbenzene, 3 gram divinylbenzenes, 1.8 gram diacetone-acryloamide(DAA)s, 2.5 gram Bing Xisuandingzhis, 2.2 gram Hydroxyethyl acrylates, 1 gram vinylformic acid; 0.01 gram adipic dihydrazide;
Water: 1.4 gram NP-30,2.1 gram DB45,21.48 gram zero(ppm) water;
Reaction bed material: 1 gram NP-30,1 gram DB45,0.01 gram NaHCO
3, 20 gram zero(ppm) water
Primary initiator: 0.15 gram SPS, 2 gram zero(ppm) water;
Back initiator: 0.35 gram SPS, 13 gram zero(ppm) water.
The preparation method is with embodiment 1.
Embodiment 4 (black)
Prescription is formed:
Organic phase: 11 grams disperse black 1 dyestuff (structural formula is seen formula IV), 16 gram vinylbenzene, 1.6 gram diacetone-acryloamide(DAA)s, 3 gram Bing Xisuandingzhis, 3 gram Hydroxyethyl acrylates, 1 gram vinylformic acid, 0.01 gram adipic dihydrazide;
Water: 1.5 gram NP-30,1.8 gram DB45,23 gram zero(ppm) water;
Reaction bed material: 0.8 gram NP-30,0.9 gram sodium lauryl sulphate, 0.01 gram NaHCO
3, 20 gram zero(ppm) water;
Primary initiator: 0.1 gram APS, 2 gram zero(ppm) water;
Back initiator: 0.4 gram APS, 13.88 gram zero(ppm) water.
The preparation method is with embodiment 1.
Press embodiment 1,2, the dispersed dye nano capsule dispersant liquid of 3,4 prepared red, yellow, blue, black four kinds of colors, its D50 particle diameter (median size), viscosity, package stability is listed in the table below:
Table 1 thermal transfer ink jet ink dispersed dye nano capsule dispersant liquid physicochemical property
Sample average particle diameter viscosity table surface tension stability in storage
(nm) (30℃，CP) (30℃，mN/m)
Embodiment 1 164 9.72 36 is outstanding
Embodiment 2 188 8.64 37 is outstanding
Embodiment 3 88 8.10 32 is outstanding
Embodiment 4 166 7.44 31 is outstanding
Annotate: the stability in storage testing method: sample at room temperature left standstill 3 months, observed flocculation, throw out etc. whether occur, and nothing flocculation and throw out then are evaluated as outstanding after 3 months.
With embodiment 1,2,3,4 prepared nano dye capsules can obtain red, yellow, blue, black, pale red, light blue six look nanocapsule-type thermal transfer ink jet inks through overmodulation.With the pattern of computer design, through the ink-jet printer of hot transfer printing ink is housed, output print is on transfer paper; To be printed on image surface on the heat-transferring printing paper then to object to be printed, and heat about 30 seconds through 180～210 ℃ of temperature through hot transfer printing auxiliary means, the dye substance molecule in the ink just distils, solidifies, infiltrates through and wait to print on the body surface.So just the image color on the paper is transferred on the different materials realistically.Ink according to this preparation is made printing test on EPSON R230, ink-jet is smooth.Through overheated transfer process, the image color that is become is gorgeous again, and is Well-recovered.And through the test of 3 months dispersion stabilizations, still ink-jet is smooth, does not stop up shower nozzle, good stability.
Claims (8)
1. the preparation method of a thermal transfer ink jet ink nano capsule is characterized in that comprising the steps, following percentage number average refers to mass percent:
(1) preparation pre-emulsion A
The preparation of organic phase: dispersed dye are dissolved in styrene monomer, acrylic monomer and the functional monomer of removing stopper mix the formation organic phase;
The preparation of water: emulsifiers dissolve is formed water in zero(ppm) water;
The preparation of pre-emulsion A: organic phase is slowly added in the container that fills the stirring of water band in room temperature, stir, under ice-water bath, place the preparatory emulsification of ultrasonic clarifixator to obtain pre-emulsion then;
(2) mini-emulsion polymerization prepared in reaction Nano capsule
The preparation of reaction bed material: in zero(ppm) water, it is 5～6 that the agent of adding pH regulator makes the pH value of system with emulsifiers dissolve, and deoxygenation begins to heat up:
The preparation of nano capsule dispersant liquid: when temperature rises to 65～70 ℃; In above-mentioned reaction bed material, add 6～60% pre-emulsion A: when temperature rises to 72～75 ℃; Add the part initiator; The amount of part initiator accounts for 5～20% of total initiator total amount, keeps temperature to react 30～40min down for 75～85 ℃, forms the seed of miniemulsion; Equal speed drips remaining pre-emulsion A in 3～3.5h then, simultaneously the equal fast remaining initiator that drips in 3.5～4h; After all dropwising, be warming up to 86～90 ℃ of slakings;
(3),, obtain nano capsule dispersant liquid through 1 μ m, 0.45 μ m, 0.22 μ m three-stage filtration with above-mentioned synthetic product;
Said acrylic monomer is one or both mixing in vinylformic acid, methylacrylic acid, methyl acrylate, TEB 3K, ethyl propenoate, Bing Xisuandingzhi, TGM 1 and the Hydroxyethyl acrylate; Said styrene monomer refers to one or both mixing in vinylbenzene and the divinylbenzene; Said functional monomer refers to diacetone-acryloamide(DAA) and adipic dihydrazide;
The quality summation of said styrene monomer, functional monomer and acrylic monomer is 150～500% of dispersed dye; Wherein the mass ratio of styrene monomer and acrylic monomer is 1～5: 1; The diacetone-acryloamide(DAA) consumption is 1～3% of total quality of material, and the mass ratio of diacetone-acryloamide(DAA) and adipic dihydrazide is 100: 0.5～1.
2. preparation method as claimed in claim 1; It is characterized in that; Emulsifying agent described in said step (1) or the step (2) is the one or more kinds of mixtures of nonylphenol class Soxylat A 25-7, different tridecanol polyoxyethylene ether, sodium lauryl sulphate, dodecyl diphenyl oxide disulfonate, sulfo-succinic acid disodium ethoxylated alcohol half ester, alkyl diphenyl base oxide stilbene-4,4'-bis-(1-azo-3, 4-dihydroxy-benzene)-2,2'-disulfonate, and wherein the consumption of emulsifying agent is 1.5～25% of amount of dye and styrene monomer, function monomer and an acrylic monomer quality summation.
3. preparation method as claimed in claim 1 is characterized in that, said dispersed dye are anthraquinone type, azo-type, cationic or quinoline type.
4. preparation method as claimed in claim 1 is characterized in that, said initiator is a kind of in Ammonium Persulfate 98.5, Sodium Persulfate or the Potassium Persulphate, and consumption is 0.1～1.5% of total quality of material; The pH regulator agent is NaHCO
3, sodium acetate one or both mix, consumption is 0.01～0.5% of total quality of material.
5. preparation method as claimed in claim 1 is characterized in that, the stir speed (S.S.) of the said stirring of step (1) is 1000rpm, mixes churning time 20～30min; During said preparatory emulsification, the ultrasonic power of ultrasonic clarifixator is 300～500W, and emulsification times is 15～20min in advance.
6. preparation method as claimed in claim 1 is characterized in that, being formulated as of step (2) said reaction bed material: with emulsifiers dissolve in zero(ppm) water; And adding the pH regulator agent, to make the pH value of system be 5～6; And this mixed solution all packed in the four-hole reaction kettle that is connected to stirring, TM, prolong and nitrogen tube, under the stir speed (S.S.) of 200rpm, feed the nitrogen deoxygenation of 15～25min earlier; During heat temperature raising to 65～70 ℃, add 6～60% pre-emulsion A.
7. the thermal transfer ink jet ink nano capsule for preparing of the described preparation method of claim 1.
8. the ink for preparing by the preparation method of the said thermal transfer ink jet ink nano capsule of claim 1.
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| CN102585606B (en) * | 2012-03-05 | 2014-02-19 | 中山大学 | Thermal-sublimation water-based intaglio printing ink and preparation method thereof |
| CN102719145B (en) * | 2012-06-29 | 2014-03-26 | 广州大学 | Disperse dye nanocapsule for thermal sublimation digital printing ink-jet ink and preparation method of disperse dye nanocapsule |
| CN103730053A (en) * | 2013-02-26 | 2014-04-16 | 立德高科(北京)数码科技有限责任公司 | Anti-counterfeit mark printed on surface of crystal |
| CN103497589A (en) * | 2013-10-10 | 2014-01-08 | 鲁继烈 | Aqueous disperse dye ink-jet printing ink |
| CN105111361B (en) * | 2015-09-10 | 2018-05-25 | 江南大学 | A kind of preparation method for drawing timber-used Nano-grade latex mill base |
| CN105504990A (en) * | 2016-01-19 | 2016-04-20 | 青岛大学 | Colored polymer microsphere ink for inkjet printing |
| CN105968955A (en) * | 2016-05-24 | 2016-09-28 | 鲁继烈 | Direct spraying ink for dispersed dye spinning |
| CN108299582A (en) * | 2018-02-01 | 2018-07-20 | 大连理工大学 | The nano particle and its preparation method and application of polymer wrapped dye molecule |
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