CN105017862A - High-performance pigment ink and preparation method thereof - Google Patents
High-performance pigment ink and preparation method thereof Download PDFInfo
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Abstract
The invention discloses high-performance pigment ink and a preparation method thereof, and belongs to the technical fields of fine chemistry industry and high-new materials. The pigment ink at least comprises the following components: a multi-functional polyurethane oligomer, a reaction monomer, a photoinitiator, nanometer pigment, a relevant auxiliary (a diluent and a bactericide) and deionized water. The pigment ink prepared by the method disclosed by the invention is different from conventional ink, and the multi-functional polyurethane oligomer with high water solubility is led, so that the ink has the advantages of good fluency, good decentralized stability, distinct color, high lustrousness and the like; the solidified ink is high in fastness, solidified films are soft in hand feel, and the ink disclosed by the invention can be used for ink jet printing patterns on flexible materials, such as textiles, nonwovens, and paper.
Description
Technical field
The present invention relates to fine chemistry industry and new high-tech material technical field, specifically a kind of high performance pigments ink and preparation method thereof.
Background technology
Compared with dye ink, paint ink has feature that is easy to use, wide application.The keying action of physics or chemistry does not occur between pigment and substrate, but relies on jointing material that pigment is anchored at substrate surface, therefore its laking process is without the need to evaporating washing, has energy-saving and cost-reducing advantage.
Current paint ink be widely used in the flexible materialss such as textiles, non-woven fabrics, paper ink-jet printed in.In application process, generally adopt the mode of thermofixation, photocuring or hardening with radiation.Wherein, photocuring receives the concern of people more and more because of advantages such as its curing speed are fast, cost is low, pollution is few.Relevant enterprise, R&D institution were all studied for the paint ink of photocuring in recent years.There is a large amount of patent report, adopt acrylic ester monomer or performed polymer to prepare paint ink.After emulsion dispersion, then realize the fixation of pigment on substrate by light initiation polymerization.In addition, investigator is also had to carry out modification to this method.Patent CN 103526570A discloses a kind of preparation method of ultraviolet curing ink jet stamp paint ink, use fine emulsion polymerization pigment and light trigger to be coated in emulsion particle and can to significantly improve colour fastness, but still be the jointing material adopting esters of acrylic acid.Patent CN 103436095A discloses a kind of water based ink jet ink of ultraviolet light polymerization, modified polyurethane resin emulsion and acrylic ester emulsion are carried out composite, but there is the problem of consistency between differing materials all the time, and then affect stability and the fluency of ink.
In actual applications, there is the problems such as toughness is low, brute force deficiency, hot sticky cold crisp, wear resistance are poor in the pigment film formed after it is found that acrylate materials solidification.For improving these drawbacks, overcoming the compatibility problem of different properties storeroom simultaneously, needing the curable paint ink that exploitation is new further.
Summary of the invention
The object of the invention is the deficiency overcoming the existence of existing curable paint ink, a kind of high performance paint ink is provided.This ink contains polyurethane multifunction oligomer, can in the technique of not adding emulsifying agent and dispersion agent with reactive monomer copolymerization, thus form highly compatible between each component, paint ink that dispersion stabilization is good.
Technical scheme of the present invention is to provide a kind of high performance pigments ink, and its composition of described paint ink and content are:
(1) the multifunctional polyurethane oligomer of weight percent 5-15%; Described multifunctional polyurethane oligomer has structure shown in formula (I), in formula (I), and R
1=H, OH, CH
3; R
2for vulcabond; R
3for wetting ability dihydroxy compound; R
4for polyester or polyether Glycols, M is volatilizable salt forming agent, and m is 1-3, n is 10-40;
(2) reaction monomers of weight percent 5-15%;
(3) light trigger of weight percent 1-3%w;
(4) nano dye of weight percent 8-20%;
(5) related auxiliaries of weight percent 1-7%;
(6) deionized water of weight percent 40-80%.
In technical solution of the present invention:
Described vulcabond is the one in hexamethylene diisocyanate (HDI), xylylene diisocyanate (XDI), cyclohexanedimethyleterephthalate vulcabond (HXDI), trimethylammonium-1,6-hexamethylene diisocyanate (TMHDI), tetramethyl-m-xylylene diisocyanate (TMXDI), dicyclohexyl methane diisocyanate (HMDI), isoflurane chalcone diisocyanate (IPDI).
The structural formula of described wetting ability dihydroxy compound is (HO)
xq (COOH)
y, (HO)
xq (SO
3h)
y, (NH
2)
xq (COOH)
yor (NH
2)
xq (SO
3h)
y, wherein Q is carbochain containing 1-12 carbon atom or aromatic ring, and x, y are 1-3.Preferred structure is such as formula the wetting ability dihydroxy compound shown in (II).
Described polyester or polyether Glycols are Polyoxypropylene diol (PPG-200, PPG-400, PPG-600, PPG-700, PPG-1000 or PPG-2000), polytetrahydrofuran diol (PTHF-250, PTHF-650, PTHF-1000, PTHF-1400, PTHF-1800 or PTHF-2000), polyoxyethylene glycol (PEG-200, PEG-400, PEG-600, PEG-800, PEG-1000 or PEG-2000), hexylene glycol system polyester glycol (PHA-200, PHA-580, PHA-1000, PHA-1500 or PHA-2000), polycaprolactone glycol (HDO-300, HDO-500, HDO-830, BDO-1000 or BDO-2000), polycarbonate diol (PCDL-500, PCDL-1000 or PCDL-2000) in one.
Described salt forming agent is Trimethylamine 99, triethylamine, diisopropylethylamine, triisopropylamine, tributylamine, N, N-dimethylcyclohexylam,ne, N-methylmorpholine, N, N-dimethylethanolamine, the one in N-methyl-N-(2-hydroxyethyl)-1,3-propylene diamine.
Described reaction monomers is furfuralcohol glycidyl ether, ethylene glycol diglycidylether, glycidyl allyl ether, glycidyl methacrylate, isobornyl acrylate, condensed ethandiol diacrylate, 1, one or more in the Viscoat 295 of 6-hexanediyl ester, ethoxylation, propenoxylated Viscoat 295,1,6-hexylene glycol methoxyl group mono acrylic ester, cyclohexyl acrylate, the just own ester of vinylformic acid, Isooctyl acrylate monomer, vinylformic acid bicyclopentyl 2-ethoxyethyl acetate, vinylformic acid ester in the positive last of the ten Heavenly stems.
Described light trigger is the one in benzoin isopropyl ether, the two methyl ether of benzil, diphenylthanedione, 1-hydroxycyclohexyl phenyl ketone, methyl o-benzoylbenzoate, thiophenyl benzophenone, sulfonic group thia anthraquinone.
Described nano dye is the one that particle diameter is less than in the mineral dye of 300nm, azo pigment, anthraquinone pigment, phthalocyanine pigment, high-visibility pigment.
Described related auxiliaries is catalyzer, thinner, sterilant.Wherein, catalyzer is the one in dibutyl tin laurate, stannous octoate, two (dodecyl sulphur) dibutyl tin, dibutyltin diacetate, N-methylmorpholine, N-ethylmorpholine, dual-morpholinyl diethyl ether, dimorpholine triethyl ether, N-(dimethylaminoethyl) morpholine; Thinner is Virahol, ethylene glycol, propylene glycol, one or more in butyleneglycol, hexylene glycol, glycol ether, diethylene glycol dimethyl ether, ethylene glycol monomethyl ether, bisphenol F epoxy resin, diacetone alcohol, methyl aceto acetate; Sterilant is the one in dimethyl fumarate, sodium Diacetate, phenylformic acid, nitrous acid hydrogen sodium, oxyacetic acid, benzotriazole.
The further technical scheme of the present invention is to provide a kind of preparation method of high performance pigments ink, it is characterized in that, adopts the raw materials of above-mentioned high performance pigments ink and weight percent thereof and following operation steps:
Step one: preparation wetting ability dihydroxy compound, be specially: in stirred vessel, add 2-chloroethyl sulfonic acid or 3-chloropropionic acid successively, diethanolamine, add sodium hydroxide again and react 1-2 hour, finally remove sodium hydroxide with hydrogen ion exchange resin, and concentrated, be drying to obtain described wetting ability dihydroxy compound;
Step 2: prepare multifunctional polyurethane oligomer, be specially: in stirred vessel, add polyester or polyether Glycols, diisocyanate monomer, wetting ability dihydroxy compound successively, 2-3h is reacted under the effect of 80 DEG C and catalyzer, obtain the base polyurethane prepolymer for use as of NCO end-blocking, the mol ratio of NCO/OH is 1.1 ~ 1.4; Cool to 70 DEG C and add end-capping reagent Hydroxyethyl acrylate again, finally add water and the mixing of salt forming agent rapid stirring, namely isothermal reaction obtains multifunctional polyurethane oligomer half an hour;
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add nano dye, reaction monomers, light trigger, thinner, sterilant successively, under the high-speed stirring of 1000-2000 rev/min, finally add the multifunctional polyurethane oligomer obtained by step 2 and deionized water, abundant stirring, after 0.5-3 hour, namely obtains described high performance pigments ink with the membrane filtration in 0.1-0.3 μm of aperture;
Principle of the present invention is: the ink prepared by the present invention, adopt aqurous ployurethane oligopolymer, organic reaction monomer and water as moving phase, good wetting and dispersing effect can be played to nano dye, thus ensure that the viscosity of ink is applicable to the requirement of ink-jet printer.
In Conventional decal tackiness agent, polyurethane binding has splendid over-all properties, can pass through the preferred of polyisocyanates, polyethers, polyester, small molecule chain extender etc. and combination, prepare the tackiness agent of ideal performance, make it have higher tensile strength, low temperature flexibility, good elasticity, hydrolytic resistance and weathering resistance, excellent tear-resistant, wear resistance, high temperature adhesion and chemical resistance etc.
The method that tradition prepares aqueous polyurethane has outer emulsion process and self-emulsification.Outer emulsion process needs additional emulsifying agent, and this is the extremely strong tensio-active agent of a class water absorbability, introduce this tensio-active agent water-intake rate after glue curing film forming higher, and the glue stability outward appearance of preparation is poor.Internal emulsification method introduces water soluble group in polyurethane macromolecular chain, makes it have self-emulsifying ability, do not need additional emulsifying agent with regard to energy stable dispersion in aqueous phase, but still there is the higher problem of water-intake rate after film forming.
In ink, the colour fastness of water-intake rate on Printing of tackiness agent has crucial impact, and then affects the over-all properties of ink.Patent of the present invention sets about improving this problem from two aspects:
A) reduce the introduction volume of water soluble group, adopt water-soluble better sulfonic group, less consumption just can play dissemination; Adopt volatilizable salt forming agent simultaneously, in subsequent cure, decompose with the ionic group of sulfonic group salify, at this time free sulfonic group dewaters with the hydroxyl condensation on fiber, and the group that absorbs water is closed, and greatly can reduce the water-retaining capacity of film.
B) on polyurethane molecular chain, double bond is introduced, adopt water tolerance good acrylate monomer under certain condition with its copolymerization, improve its water tolerance, simultaneously can performance between comprehensive two kinds of differing materials, overcome respective shortcoming, greatly improve the over-all properties of ink.
Compared with existing paint ink, the distinguishing feature of paint ink provided by the present invention has:
1. ink viscosity is low, and fluency, dispersion stabilization are good;
2. cured film has excellent mechanical endurance and snappiness, excellent chemical-resistant and high-and low-temperature resistance performance;
3. the Printing color clear obtained, reflecting feel is strong, and colour fastness is high.
Embodiment
Below in conjunction with concrete case study on implementation, explanation is described in detail to the present invention.
A kind of high performance pigments ink, is characterized in that, its composition of described paint ink and content are:
(1) the multifunctional polyurethane oligomer of weight percent 5-15%; Described multifunctional polyurethane oligomer has structure shown in formula (I), in formula (I), and R
1=H, OH, CH
3; R
2for vulcabond; R
3for wetting ability dihydroxy compound; R
4for polyester or polyether Glycols, M is volatilizable salt forming agent, and m is 1-3, n is 10-40;
(2) reaction monomers of weight percent 5-15%;
(3) light trigger of weight percent 1-3%w;
(4) nano dye of weight percent 8-20%;
(5) related auxiliaries of weight percent 1-7%;
(6) deionized water of weight percent 40-80%.
In technical solution of the present invention:
Described vulcabond is the one in hexamethylene diisocyanate (HDI), xylylene diisocyanate (XDI), cyclohexanedimethyleterephthalate vulcabond (HXDI), trimethylammonium-1,6-hexamethylene diisocyanate (TMHDI), tetramethyl-m-xylylene diisocyanate (TMXDI), dicyclohexyl methane diisocyanate (HMDI), isoflurane chalcone diisocyanate (IPDI).
The structural formula of described wetting ability dihydroxy compound is (HO)
xq (COOH)
y, (HO)
xq (SO
3h)
y, (NH
2)
xq (COOH)
yor (NH
2)
xq (SO
3h)
y, wherein Q is carbochain containing 1-12 carbon atom or aromatic ring, and x, y are 1-3.Preferred structure is such as formula the wetting ability dihydroxy compound shown in (II).
Described polyester or polyether Glycols are Polyoxypropylene diol (PPG-200, PPG-400, PPG-600, PPG-700, PPG-1000 or PPG-2000), polytetrahydrofuran diol (PTHF-250, PTHF-650, PTHF-1000, PTHF-1400, PTHF-1800 or PTHF-2000), polyoxyethylene glycol (PEG-200, PEG-400, PEG-600, PEG-800, PEG-1000 or PEG-2000), hexylene glycol system polyester glycol (PHA-200, PHA-580, PHA-1000, PHA-1500 or PHA-2000), polycaprolactone glycol (HDO-300, HDO-500, HDO-830, BDO-1000 or BDO-2000), polycarbonate diol (PCDL-500, PCDL-1000 or PCDL-2000) in one.
Described salt forming agent is Trimethylamine 99, triethylamine, diisopropylethylamine, triisopropylamine, tributylamine, N, N-dimethylcyclohexylam,ne, N-methylmorpholine, N, N-dimethylethanolamine, the one in N-methyl-N-(2-hydroxyethyl)-1,3-propylene diamine.
Described reaction monomers is furfuralcohol glycidyl ether, ethylene glycol diglycidylether, glycidyl allyl ether, glycidyl methacrylate, isobornyl acrylate, condensed ethandiol diacrylate, 1, one or more in the Viscoat 295 of 6-hexanediyl ester, ethoxylation, propenoxylated Viscoat 295,1,6-hexylene glycol methoxyl group mono acrylic ester, cyclohexyl acrylate, the just own ester of vinylformic acid, Isooctyl acrylate monomer, vinylformic acid bicyclopentyl 2-ethoxyethyl acetate, vinylformic acid ester in the positive last of the ten Heavenly stems.
Described light trigger is the one in benzoin isopropyl ether, the two methyl ether of benzil, diphenylthanedione, 1-hydroxycyclohexyl phenyl ketone, methyl o-benzoylbenzoate, thiophenyl benzophenone, sulfonic group thia anthraquinone.
Described nano dye is the one that particle diameter is less than in the mineral dye of 300nm, azo pigment, anthraquinone pigment, phthalocyanine pigment, high-visibility pigment.
Described related auxiliaries is thinner and sterilant.Wherein, thinner is Virahol, ethylene glycol, propylene glycol, one or more in butyleneglycol, hexylene glycol, glycol ether, diethylene glycol dimethyl ether, ethylene glycol monomethyl ether, bisphenol F epoxy resin, diacetone alcohol, methyl aceto acetate; Sterilant is the one in dimethyl fumarate, sodium Diacetate, phenylformic acid, nitrous acid hydrogen sodium, oxyacetic acid, benzotriazole.
A preparation method for high performance pigments ink, is characterized in that, adopts the raw materials of above-mentioned high performance pigments ink and weight percent thereof and following operation steps:
Step one: preparation wetting ability dihydroxy compound, be specially: in stirred vessel, add 2-chloroethyl sulfonic acid or 3-chloropropionic acid successively, diethanolamine, add sodium hydroxide again and react 1-2 hour, finally remove sodium hydroxide with hydrogen ion exchange resin, and concentrated, be drying to obtain described wetting ability dihydroxy compound;
Step 2: prepare multifunctional polyurethane oligomer, be specially: in stirred vessel, add polyester or polyether Glycols, diisocyanate monomer, wetting ability dihydroxy compound successively, 2-3h is reacted under the effect of 80 DEG C and catalyzer, obtain the base polyurethane prepolymer for use as of NCO end-blocking, the mol ratio of NCO/OH is 1.1 ~ 1.4; Cool to 70 DEG C and add end-capping reagent Hydroxyethyl acrylate again, finally add water and the mixing of salt forming agent rapid stirring, namely isothermal reaction obtains multifunctional polyurethane oligomer half an hour;
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add nano dye, reaction monomers, light trigger, thinner, sterilant successively, under the high-speed stirring of 1000-2000 rev/min, finally add the multifunctional polyurethane oligomer obtained by step 2 and deionized water, abundant stirring, after 0.5-3 hour, namely obtains described high performance pigments ink with the membrane filtration in 0.1-0.3 μm of aperture;
Diisocyanate monomer described in step 2 is the one in hexamethylene diisocyanate (HDI), xylylene diisocyanate (XDI), cyclohexanedimethyleterephthalate vulcabond (HXDI), trimethylammonium-1,6-hexamethylene diisocyanate (TMHDI), tetramethyl-m-xylylene diisocyanate (TMXDI), dicyclohexyl methane diisocyanate (HMDI) or isoflurane chalcone diisocyanate (IPDI) monomer;
Catalyzer described in step 2 is dibutyl tin laurate, stannous octoate, two (dodecyl sulphur) dibutyl tin, oxalic acid diethyl) one in morpholine;
Salt forming agent described in step 2 is Trimethylamine 99, triethylamine, diisopropylethylamine, triisopropylamine, tributylamine, N, N-dimethylcyclohexylam,ne, N-methylmorpholine, N, one in N-dimethylethanolamine or N-methyl-N-(2-hydroxyethyl)-1,3-propylene diamine.
Embodiment 1
The present embodiment provides a kind of high performance pigments red ink and preparation method thereof.
Step one: preparation wetting ability dihydroxy compound, be specially: under room temperature, 200 grams of 2-chloroethyl sulfonic acid and 145.44 grams of diethanolamine are dissolved in 500 ml waters, then add 110.66 grams of sodium hydroxide to it and be warmed up to 80 DEG C of reactions and within one hour, obtain N, the mixed aqueous solution of N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid sodium.This aqueous solution hydrogen ion exchange resin is exchanged, and is concentrated, dry, obtain N, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid (DHESA) sterling.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polytetrahydrofuran diol PTHF-2000 and PTHF-250 respectively 125 grams and 15 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid (DHESA) 16.7 grams and isoflurane chalcone diisocyanate (IPDI) 49 grams, drip 1-2 and drip stannous octoate, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.1.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 4.6 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.882 grams, the water measured and salt forming agent diisopropylethylamine 10.1 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains transparent clear soln half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. Pigment reds 22 successively, isobornyl acrylate 15 grams, propenoxylated Viscoat 295 2 grams, benzoin isopropyl ether 0.8 gram, ethylene glycol 10 grams, diethylene glycol dimethyl ether 5 grams, dimethyl fumarate 0.1 gram, under the rotating speed of 1200 revs/min, finally add multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water, dispersion stirring 45 minutes, obtains Pigment red ink with 0.2 μm of aperture membrane filtration.Indices tested by ink at 25 DEG C: viscosity 6mPas, surface tension 35mN/m, electric conductivity 870s/m, Zeta potential-41.2mV, particle diameter 150nm, pH value 8.5.
By this ink spray printing to pure cotton fabric surface, through 140 DEG C of curing fixations 2 minutes, can obtain bright in colour, figure clarity was high, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 4 grades.During ink spray printing, fluency is good, deposits 7 months under room temperature, stable without sedimentation.
Embodiment 2:
The present embodiment provides a kind of high performance pigments blue ink and preparation method thereof.
Step one: wetting ability dihydroxy compound DHESA is prepared according to embodiment 1.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polyoxypropyleneglycol PPG-2000 and PPG-200 respectively 125 grams and 10 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid (DHESA) 16.7 grams and hexamethylene diisocyanate (HDI) 37 grams, drip 1-2 and drip dibutyl tin laurate, be warmed to 80 DEG C of reactions 3 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.2.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 4.6 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.814 grams, the water measured and salt forming agent triethylamine 10.1 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains transparent clear soln half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. pigment Blue 15s successively, furfuralcohol glycidyl ether 14 grams, cyclohexyl acrylate 3, the two methyl ether 0.9 gram of benzil, Virahol 9.9 grams, ethylene glycol monomethyl ether 5 grams, 0.1 gram, phenylformic acid, under the rotating speed of 1500 revs/min, finally add multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water, dispersion stirring 1 hour, filter with the filter bag in 0.2 μm of aperture and obtain Pigment blue ink.Indices tested by ink at 25 DEG C: viscosity 7mPas, surface tension 40mN/m, electric conductivity 850s/m, Zeta potential-38.7mV, particle diameter 120nm, pH value 8.2.
By this ink spray printing to bamboo pulp fiber fabric face, through 130 DEG C of curing fixations 3 minutes, can higher color depth, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 3-4 level.During ink spray printing, fluency is good, deposits 6 months under room temperature, stable without sedimentation.
Embodiment 3:
The present embodiment provides a kind of high performance pigments India ink and preparation method thereof.
Step one: wetting ability dihydroxy compound DHESA is prepared according to embodiment 1.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add poly-hexanodioic acid-1,6-hexylene glycol esterdiol PHA-2000 and PTHF-200 respectively 125 grams and 15 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid (DHESA) 16.7 grams and xylylene diisocyanate (XDI) 41.5 grams, drip 1-2 and drip stannous octoate, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.2.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 4.6 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.837 grams, the water measured and salt forming agent N-methylmorpholine 7.9 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains transparent clear soln half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. Pigment blacks 11 successively, ethylene glycol diglycidylether 14 grams, the just own ester of vinylformic acid 3 grams, diphenylthanedione 0.8 gram, propylene glycol 8, diethylene glycol dimethyl ether 7 grams, dimethyl fumarate 0.2 gram, under the rotating speed of 2000 revs/min, finally add multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water, dispersion stirring 30 minutes, filter with the filter bag in 0.1 μm of aperture and obtain Pigment black ink.Indices tested by ink at 25 DEG C: viscosity 6mPas, and surface tension is 41mN/m, and electric conductivity is 800s/m, Zeta potential-27.4mV, particle diameter 100nm, pH value 8.7.
By this ink spray printing to nonwoven surface, through 145 DEG C of curing fixations 2 minutes, can higher color depth, flower pattern is clear, soft printing bonded fabric.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4 grades and 3-4 level respectively, and fastness to washing reaches 4 grades, and sunlight fastness reaches 4 grades.During ink spray printing, fluency is good, deposits 4 months under room temperature, stable without sedimentation.
Embodiment 4:
The present embodiment provides yellow ink of a kind of high performance pigments and preparation method thereof.
Step one: wetting ability dihydroxy compound DHESA is prepared according to embodiment 1.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polycaprolactone glycol HDO-2000 and PTHF-300 respectively 125 grams and 10 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid (DHESA) 16.7 grams and cyclohexanedimethyleterephthalate vulcabond (HXDI) 42.7 grams, drip 1-2 and drip two (dodecyl sulphur) dibutyl tin, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.3.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 5 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.842 grams, the water measured and salt forming agent triisopropylamine 11.2 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains transparent clear soln half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. pigment Yellow 14s successively, glycidyl methacrylate 12 grams, propenoxylated Viscoat 295 5 grams, 1-hydroxycyclohexyl phenyl ketone 0.8 gram, butyleneglycol 9 grams, diacetone alcohol 6 grams, oxyacetic acid 0.1 gram, under the rotating speed of 1000 revs/min, finally add multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water, dispersion stirring 2 hours, obtains Pigment Yellow 73 ink with the membrane filtration in 0.1 μm of aperture.Indices tested by ink at 25 DEG C: viscosity 9mPas, surface tension 50mN/m, electric conductivity 750s/m, Zeta potential-35mV, particle diameter 100nm, pH value 9.
By this ink spray printing to nylon surface, through 130 DEG C of curing fixations 3 minutes, can obtain bright in colour, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 4 grades.During ink spray printing, fluency is good, deposits 5 months under room temperature, stable without sedimentation.
Embodiment 5:
The present embodiment provides a kind of high performance pigments blue ink and preparation method thereof.
Step one: wetting ability dihydroxy compound DHESA is prepared according to embodiment 1.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polycarbonate diol PCTL-2000 and PCTL-500 respectively 125 grams and 25 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid (DHESA) 16.7 grams and trimethylammonium-1,6-hexamethylene diisocyanate (TMHDI) 46.2 grams, drip 1-2 and drip dibutyltin diacetate, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.4.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 6 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.904 grams, the water measured and salt forming agent N, N-dimethylethanolamine 7 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains transparent clear soln half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. Pigment blues 56 successively, condensed ethandiol diacrylate 14.5 grams, Isooctyl acrylate monomer 2.5 grams, 1-hydroxycyclohexyl phenyl ketone 1 gram, butyleneglycol 11 grams, diethylene glycol dimethyl ether 4 grams, benzotriazole 0.2 gram, under the rotating speed of 1000 revs/min, finally add multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water, dispersion stirring 3 hours, obtains Pigment blue ink with the membrane filtration in 0.1 μm of aperture.Indices tested by ink at 25 DEG C: viscosity 6.3mPas, and surface tension is 45mN/m, and electric conductivity is 810s/m, Zeta potential-38.5mV, particle diameter 80nm, pH value 8.
By this ink spray printing to polyester-cotton blend surface, through 150 DEG C of curing fixations 3 minutes, can obtain bright in colour, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 4 grades.During ink spray printing, fluency is good, deposits 6 months under room temperature, stable without sedimentation.
Embodiment 6:
The present embodiment provides yellow ink of a kind of high performance pigments and preparation method thereof.
Step one: wetting ability dihydroxy compound DHESA is prepared according to embodiment 1.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, adds polyoxyethylene glycol (PEG-2000 and PEG-400) each 125 grams and 20 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-aminoethyl sulfonic acid (DHESA) 16.7 grams and tetramethyl-m-xylylene diisocyanate (TMXDI) 53.7 grams, drip 1-2 dual-morpholinyl diethyl ether, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.4.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 5.8 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.925 grams, the water measured and salt forming agent N, N-dimethylcyclohexylam,ne 9.9 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains transparent clear soln half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. Pigment Yellow 73s 65 successively, 1,6-hexanediyl ester 13.5 grams, the Viscoat 295 of ethoxylation 3.5 grams, thiophenyl benzophenone 1.1 grams, glycol ether 10 grams, hexylene glycol 5 grams, dimethyl fumarate 0.1 gram, finally adds multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water under the rotating speed of 1600 revs/min, dispersion stirring 1.5 hours, obtains Pigment Yellow 73 ink with 0.2 μm of aperture membrane filtration.Indices tested by ink at 25 DEG C: viscosity 5.8mPas, surface tension 42mN/m, electric conductivity 820s/m, Zeta potential-43.5mV, particle diameter 190nm, pH value 8.5.
By this ink spray printing to paper surface, through 120 DEG C of curing fixations 2 minutes, can obtain bright in colour, the clear solid of flower pattern, soft calico paper.Through colour fastness test, its dry fastness reaches 4-5 level, and sunlight fastness reaches 4 grades.During ink spray printing, fluency is good, deposits 8 months under room temperature, stable without sedimentation.
Embodiment 7:
The present embodiment provides a kind of high performance pigments red ink and preparation method thereof.
Step one: preparation wetting ability dihydroxy compound, be specially: under room temperature, 168.8 grams of 3-chloropropionic acids and 145.44 grams of diethanolamine are dissolved in 500 ml waters, then add 110.66 grams of sodium hydroxide to it and be warmed up to 90 DEG C of reactions and within 2 hours, obtain N, the mixed aqueous solution of N-bis-(2-hydroxyethyl)-2-alanine sodium.This aqueous solution hydrogen ion exchange resin is exchanged, and is concentrated, dry, obtain N, N-bis-(2-hydroxyethyl)-2-alanine (HEAPA) sterling.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polytetrahydrofuran diol PTHF-2000 and PTHF-250 respectively 125 grams and 15 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-alanine (HEAPA) 19 grams and isoflurane chalcone diisocyanate (IPDI) 49 grams, drip 1-2 and drip stannous octoate, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.1.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 7 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.900 grams, the water measured and salt forming agent diisopropylethylamine 10.1 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains white micro-blueing light emulsion half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. pigment red 3s 8 successively, 1,6-hexanediyl ester 14.5 grams, propenoxylated Viscoat 295 3.5 grams, the two methyl ether 0.9 gram of benzil, butyleneglycol 11 grams, ethylene glycol monomethyl ether 4.5 grams, 0.15 gram, nitrous acid hydrogen sodium, adds multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water under finally stirring at 1800 revs/min, dispersion stirring 50 minutes, obtains Pigment red ink with 0.2 μm of aperture membrane filtration.Indices tested by ink at 25 DEG C: viscosity is 7mPas, surface tension 75mN/m, and electric conductivity is 700s/m, Zeta potential-39.5mV, particle diameter 160nm, pH value 8.5.
By this ink spray printing on polyester-cotton fabric, through 160 DEG C of curing fixations 3 minutes, can obtain bright in colour, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 4 grades.During ink spray printing, fluency is good, deposits 6 months under room temperature, stable without sedimentation.
Embodiment 8:
The present embodiment provides a kind of high performance pigments blue ink and preparation method thereof.
Step one: wetting ability dihydroxy compound HEAPA is prepared according to embodiment 7.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polyoxypropyleneglycol PTHF-2000 and PTHF-200 respectively 125 grams and 10 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-alanine (HEAPA) 18 grams and dicyclohexyl methane diisocyanate (HMDI) 57.7 grams, drip 1-2 and drip stannous octoate, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.2.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 7 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.933 grams, the water measured and salt forming agent tributylamine 14.5 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains white emulsion half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. pigment blue 1s 6 successively, 1,6-hexylene glycol methoxyl group mono acrylic ester 16 grams, propenoxylated Viscoat 295 3 grams, thiophenyl benzophenone 0.9 gram, Virahol 10 grams, benzotriazole 3.5 grams, 0.15 gram, nitrous acid hydrogen sodium, adds multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water under finally stirring at 1200 revs/min, dispersion stirring 1 hour, obtains Pigment blue ink with 0.2 μm of aperture membrane filtration.The viscosity of ink is 7mPas, and surface tension is 62mN/m, and electric conductivity is 860s/m, Zeta potential-26.6mV, particle diameter 130nm, pH value 8.5.
By this ink spray printing on real silk fabric, through 120 DEG C of curing fixations 3 minutes, can obtain bright in colour, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 4 grades.During ink spray printing, fluency is good, deposits 6 months under room temperature, stable without sedimentation.
Embodiment 9:
The present embodiment provides a kind of high performance pigments India ink and preparation method thereof.
Step one: wetting ability dihydroxy compound HEAPA is prepared according to embodiment 7.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add poly-hexanodioic acid-1,6-hexylene glycol esterdiol PHA-2000 and PTHF-200 respectively 125 grams and 15 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-alanine (HEAPA) 19 grams and hexamethylene diisocyanate (HDI) 38 grams, drip 1-2 and drip dimorpholine triethyl ether, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.2.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 7 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.856 grams, the water measured and salt forming agent triethylamine 10.1 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains white emulsion half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. Pigment blacks 11 successively, 1,6-hexanediyl ester 15 grams, Isooctyl acrylate monomer 3 grams, sulfonic group thia anthraquinone 1.2 grams, Virahol 9.5 grams, ethylene glycol monomethyl ether 4.5 grams, sodium Diacetate 0.15 gram, adds multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water under finally stirring at 1500 revs/min, dispersion stirring 1 hour, obtains Pigment black ink with 0.3 μm of aperture membrane filtration.The viscosity of ink is 8mPas, and surface tension is 40mN/m, and electric conductivity is 950s/m, Zeta potential-30.8mV, particle diameter 200nm, pH value 9.
By this ink spray printing on spun rayon piece goods, through 140 DEG C of curing fixations 3 minutes, can obtain bright in colour, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 4 grades.During ink spray printing, fluency is good, deposits 6 months under room temperature, stable without sedimentation.
Embodiment 10:
The present embodiment provides yellow ink of a kind of high performance pigments and preparation method thereof.
Step one: wetting ability dihydroxy compound HEAPA is prepared according to embodiment 7.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polycaprolactone glycol HDO-2000 and PTHF-300 respectively 125 grams and 10 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-alanine (HEAPA) 19 grams and dicyclohexyl methane diisocyanate (HMDI) 57.7 grams, drip 1-2 and drip dual-morpholinyl diethyl ether, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.2.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 7 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.915 grams, the water measured and salt forming agent diisopropylethylamine 10.1 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains white blueing light emulsion half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. pigment yellow 17s successively, condensed ethandiol diacrylate 16 grams, Isooctyl acrylate monomer 3 grams, diphenylthanedione 0.9 gram, diacetone alcohol 10 grams, ethylene glycol monomethyl ether 5.5 grams, 0.15 gram, nitrous acid hydrogen sodium, add multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water under finally stirring at 1000 revs/min, dispersion stirring 2 hours, obtains Pigment Yellow 73 ink with 0.3 μm of aperture membrane filtration.The viscosity of ink is 8mPas, and surface tension is 54mN/m, and electric conductivity is 860s/m, Zeta potential-25.8mV, particle diameter 220nm, pH value 9.
By this ink spray printing on nitrile cotton fabric, through 150 DEG C of curing fixations 3 minutes, can obtain bright in colour, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 3-4 level.During ink spray printing, fluency is good, deposits 6 months under room temperature, stable without sedimentation.
Embodiment 11:
The present embodiment provides a kind of high performance pigments red ink and preparation method thereof.
Step one: wetting ability dihydroxy compound HEAPA is prepared according to embodiment 7.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polycarbonate diol PCDL-2000 and PCDL-500 respectively 125 grams and 25 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-alanine (HEAPA) 19 grams and dicyclohexyl methane diisocyanate (HMDI) 57.7 grams, drip 1-2 and drip N-ethylmorpholine, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.3.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 7 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.975 grams, the water measured and salt forming agent diisopropylethylamine 10.1 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains oyster white blueing light emulsion half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. pigment red 4s 8 successively, glycidyl allyl ether 17 grams, vinylformic acid bicyclopentyl 2-ethoxyethyl acetate 2 grams, methyl o-benzoylbenzoate 0.9 gram, butyleneglycol 11 grams, methyl aceto acetate 4.5 grams, dimethyl fumarate 0.15 gram, add multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water under finally stirring at 1200 revs/min, dispersion stirring 1 hour, obtains Pigment red ink with 0.2 μm of aperture membrane filtration.The viscosity of ink is 7mPas, and surface tension is 55mN/m, and electric conductivity is 790s/m, Zeta potential-35mV, particle diameter 180nm, pH value 8.8.
By this ink spray printing on sodolin, through 140 DEG C of curing fixations 3 minutes, can obtain bright in colour, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 4 grades.During ink spray printing, fluency is good, deposits 5 months under room temperature, stable without sedimentation.
Embodiment 12:
The present embodiment provides a kind of high performance pigments blue ink and preparation method thereof.
Step one: wetting ability dihydroxy compound HEAPA is prepared according to embodiment 7.
Step 2: prepare multifunctional polyurethane oligomer, be specially: in the four-hole boiling flask that agitator, thermometer and prolong are housed, add polyoxyethylene glycol PEG-2000 and PEG-400 respectively 125 grams and 20 grams in 110 DEG C of vacuum hydro-extractions 1 hour.The N measured is added after cooling, N-bis-(2-hydroxyethyl)-2-alanine (HEAPA) 19 grams and isoflurane chalcone diisocyanate (IPDI) 49 grams, drip 1-2 and drip stannous octoate, be warmed to 80 DEG C of reactions 2 hours, obtain the base polyurethane prepolymer for use as of NCO end-blocking, R value (mol ratio of NCO/OH) is 1.4.Then temperature of reaction is down to 70 DEG C, adds Hydroxyethyl acrylate 7 grams reaction 1 hour, thus obtain the base polyurethane prepolymer for use as of double bond end-blocking.920 grams, the water measured and salt forming agent N-methyl-N-(2-hydroxyethyl)-1,3-propylene diamine 10.4 grams are slowly added to rapid stirring mixing in above-mentioned performed polymer, isothermal reaction obtains oyster white blueing light emulsion half an hour.
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add 10 grams of C.I. Pigment blues 63 successively, 1,6-hexanediyl ester 15 grams, vinylformic acid ester in the positive last of the ten Heavenly stems 3.5 grams, the two methyl ether 0.9 gram of benzil, butyleneglycol 11 grams, bisphenol F epoxy resin 4.5 grams, 0.15 gram, nitrous acid hydrogen sodium, adds multifunctional polyurethane oligomer solution prepared in step 2 and each 50 grams of water under finally stirring at 1800 revs/min, dispersion stirring 1 hour, obtains Pigment blue ink with 0.3 μm of aperture membrane filtration.The viscosity of ink is 10mPas, and surface tension is 33mN/m, and electric conductivity is 690s/m, Zeta potential-25mV, particle diameter 240nm, pH value 9.5.
By this ink spray printing in viscose fabric, through 130 DEG C of curing fixations 3 minutes, can obtain bright in colour, the clear solid of flower pattern, soft PRINTED FABRIC.Through colour fastness test, it is dry, fastness to wet rubbing reaches 4-5 level and 4 grades respectively, and fastness to washing reaches 4 grades.During ink spray printing, fluency is good, deposits 4 months under room temperature, stable without sedimentation.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also change above-mentioned embodiment and revise.Therefore, the present invention is not limited to embodiment disclosed and described above, also should fall in the protection domain of claim of the present invention modifications and changes more of the present invention.In addition, although employ some specific terms in this specification sheets, these terms just for convenience of description, do not form any restriction to the present invention.
The present invention does not address part and is applicable to prior art.
Claims (10)
1. a high performance pigments ink, it is characterized in that its raw materials and weight percent as follows:
(1) the multifunctional polyurethane oligomer of weight percent 5-15%; Described multifunctional polyurethane oligomer has structure shown in formula (I), in formula (I), and R
1=H, OH, CH
3; R
2for vulcabond; R
3for wetting ability dihydroxy compound; R
4for polyester or polyether Glycols, M is salt forming agent, and m is 1-3, n is 10-40;
(2) reaction monomers of weight percent 5-15%;
(3) light trigger of weight percent 1-3%w;
(4) nano dye of weight percent 8-20%;
(5) related auxiliaries of weight percent 1-7%;
(6) deionized water of weight percent 40-80%.
2. high performance pigments ink according to claim 1, it is characterized in that, described vulcabond is the one in hexamethylene diisocyanate (HDI), xylylene diisocyanate (XDI), cyclohexanedimethyleterephthalate vulcabond (HXDI), trimethylammonium-1,6-hexamethylene diisocyanate (TMHDI), tetramethyl-m-xylylene diisocyanate (TMXDI), dicyclohexyl methane diisocyanate (HMDI) or isoflurane chalcone diisocyanate (IPDI).
3. high performance pigments ink according to claim 1, is characterized in that, the structural formula of described wetting ability dihydroxy compound is (HO)
xq (COOH)
y, (HO)
xq (SO
3h)
y, (NH
2)
xq (COOH)
yor (NH
2)
xq (SO
3h)
yin one; Wherein Q is carbochain containing 1-12 carbon atom or aromatic ring, and x, y are 1-3.
4. a kind of high performance pigments ink according to claim 1, it is characterized in that, described polyester or polyether Glycols are at least one in Polyoxypropylene diol, polytetrahydrofuran diol, polyoxyethylene glycol, hexylene glycol system polyester glycol, polycaprolactone glycol and polycarbonate diol;
Described Polyoxypropylene diol is that one in PPG-200, PPG-400, PPG-600, PPG-700, PPG-1000 and PPG-2000 at least plants;
Described polytetrahydrofuran diol is at least one in PTHF-250, PTHF-650, PTHF-1000, PTHF-1400, PTHF-1800 and PTHF-2000;
Described polyoxyethylene glycol is at least one in PEG-200, PEG-400, PEG-600, PEG-800, PEG-1000 and PEG-2000;
Described hexylene glycol system polyester glycol is at least one in PHA-200, PHA-580, PHA-1000, PHA-1500 and PHA-2000;
Described polycaprolactone glycol is at least one in HDO-300, HDO-500, HDO-830, BDO-1000 and BDO-2000;
Described polycarbonate diol is at least one in PCDL-500, PCDL-1000 and PCDL-2000.
5. a kind of high performance pigments ink according to claim 1, it is characterized in that, described salt forming agent is Trimethylamine 99, triethylamine, diisopropylethylamine, triisopropylamine, tributylamine, N, N-dimethylcyclohexylam,ne, N-methylmorpholine, N, one in N-dimethylethanolamine or N-methyl-N-(2-hydroxyethyl)-1,3-propylene diamine.
6. a kind of high performance pigments ink according to claim 1, it is characterized in that, described reaction monomers is furfuralcohol glycidyl ether, ethylene glycol diglycidylether, glycidyl allyl ether, glycidyl methacrylate, isobornyl acrylate, condensed ethandiol diacrylate, 1, 6-hexanediyl ester, the Viscoat 295 of ethoxylation, propenoxylated Viscoat 295, 1, 6-hexylene glycol methoxyl group mono acrylic ester, cyclohexyl acrylate, the just own ester of vinylformic acid, Isooctyl acrylate monomer, one or more in vinylformic acid bicyclopentyl 2-ethoxyethyl acetate and vinylformic acid ester in the positive last of the ten Heavenly stems.
7. a kind of high performance pigments ink according to claim 1, it is characterized in that, described light trigger is one or both in benzoin isopropyl ether, benzil two methyl ether, diphenylthanedione, 1-hydroxy-cyclohexyl phenyl ketone, methyl o-benzoylbenzoate, thiophenyl benzophenone and sulfonic group thia anthraquinone.
8. a kind of high performance pigments ink according to claim 1, is characterized in that, described nano dye is the one that particle diameter is less than in the mineral dye of 300nm, azo pigment, anthraquinone pigment, phthalocyanine pigment or high-visibility pigment.
9. a kind of high performance pigments ink according to claim 1, it is characterized in that, described related auxiliaries comprises thinner and sterilant; Described thinner is Virahol, ethylene glycol, propylene glycol, one or more in butyleneglycol, hexylene glycol, glycol ether, diethylene glycol dimethyl ether, ethylene glycol monomethyl ether, bisphenol F epoxy resin, diacetone alcohol and methyl aceto acetate; Described sterilant is the one in dimethyl fumarate, sodium Diacetate, phenylformic acid, nitrous acid hydrogen sodium, oxyacetic acid or benzotriazole.
10. a preparation method for high performance pigments ink, is characterized in that, adopts the raw materials of the high performance pigments ink described in any one of claim 1-9 and weight percent thereof and following operation steps:
Step one: preparation wetting ability dihydroxy compound, be specially: in stirred vessel, add 2-chloroethyl sulfonic acid or 3-chloropropionic acid successively, diethanolamine, add sodium hydroxide again and react 1-2 hour, finally remove sodium hydroxide with hydrogen ion exchange resin, and concentrated, be drying to obtain described wetting ability dihydroxy compound;
Step 2: prepare multifunctional polyurethane oligomer, be specially: in stirred vessel, add polyester or polyether Glycols, diisocyanate monomer, wetting ability dihydroxy compound successively, 2-3h is reacted under the effect of 80 DEG C and catalyzer, obtain the base polyurethane prepolymer for use as of NCO end-blocking, the mol ratio of NCO/OH is 1.1 ~ 1.4; Cool to 70 DEG C and add end-capping reagent Hydroxyethyl acrylate again, finally add water and the mixing of salt forming agent rapid stirring, namely isothermal reaction obtains multifunctional polyurethane oligomer half an hour;
Step 3: preparation high performance pigments ink, be specially: in stirred vessel, add nano dye, reaction monomers, light trigger, thinner, sterilant successively, under the high-speed stirring of 1000-2000 rev/min, finally add the multifunctional polyurethane oligomer obtained by step 2 and deionized water, abundant stirring, after 0.5-3 hour, namely obtains described high performance pigments ink with the membrane filtration in 0.1-0.3 μm of aperture;
Diisocyanate monomer described in step 2 is the one in hexamethylene diisocyanate (HDI), xylylene diisocyanate (XDI), cyclohexanedimethyleterephthalate vulcabond (HXDI), trimethylammonium-1,6-hexamethylene diisocyanate (TMHDI), tetramethyl-m-xylylene diisocyanate (TMXDI), dicyclohexyl methane diisocyanate (HMDI) or isoflurane chalcone diisocyanate (IPDI) monomer;
Catalyzer described in step 2 is dibutyl tin laurate, stannous octoate, two (dodecyl sulphur) dibutyl tin, oxalic acid diethyl) one in morpholine;
Salt forming agent described in step 2 is Trimethylamine 99, triethylamine, diisopropylethylamine, triisopropylamine, tributylamine, N, N-dimethylcyclohexylam,ne, N-methylmorpholine, N, one in N-dimethylethanolamine or N-methyl-N-(2-hydroxyethyl)-1,3-propylene diamine.
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| CN107286751A (en) * | 2017-08-23 | 2017-10-24 | 王金桢 | A kind of preparation method of painting ink-jetting printing oil ink |
| CN109403091A (en) * | 2018-10-30 | 2019-03-01 | 浙江蓝宇数码科技股份有限公司 | A kind of environment-friendly digital weaving inking printing pigment ink and preparation method |
| CN110483722A (en) * | 2019-07-25 | 2019-11-22 | 南通万顺化工科技有限公司 | A kind of dedicated Water/oil dual-purpose polyurethane dispersant of synthetic leather and preparation method thereof |
| CN115286957A (en) * | 2021-09-16 | 2022-11-04 | 浙江理工大学 | Preparation method and application of photocuring self-emulsifying waterborne polyurethane composite pigment ink |
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