CN104628989A - Aqueous jet ink for cotton fabric and preparation method thereof - Google Patents
Aqueous jet ink for cotton fabric and preparation method thereof Download PDFInfo
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- CN104628989A CN104628989A CN201510082208.7A CN201510082208A CN104628989A CN 104628989 A CN104628989 A CN 104628989A CN 201510082208 A CN201510082208 A CN 201510082208A CN 104628989 A CN104628989 A CN 104628989A
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- polyaminoester emulsion
- jet
- chitin modified
- ink
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 64
- 239000004744 fabric Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title description 2
- 239000000839 emulsion Substances 0.000 claims abstract description 106
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229920001661 Chitosan Polymers 0.000 claims abstract description 44
- 239000008367 deionised water Substances 0.000 claims abstract description 27
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 27
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000178 monomer Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 229920002101 Chitin Polymers 0.000 claims description 64
- 239000000049 pigment Substances 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 12
- 150000001718 carbodiimides Chemical class 0.000 claims description 11
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 7
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 4
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003002 pH adjusting agent Substances 0.000 claims description 4
- 230000006196 deacetylation Effects 0.000 claims description 3
- 238000003381 deacetylation reaction Methods 0.000 claims description 3
- 230000004048 modification Effects 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 3
- 239000004971 Cross linker Substances 0.000 claims description 2
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 abstract description 12
- 229920002635 polyurethane Polymers 0.000 abstract description 11
- 238000006116 polymerization reaction Methods 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 229920000728 polyester Polymers 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 125000005442 diisocyanate group Chemical group 0.000 abstract 1
- 229920000223 polyglycerol Polymers 0.000 abstract 1
- 150000005846 sugar alcohols Polymers 0.000 abstract 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 30
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 26
- 238000007639 printing Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 13
- 239000000835 fiber Substances 0.000 description 12
- 229920001451 polypropylene glycol Polymers 0.000 description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 10
- 239000007921 spray Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 7
- DQFBYFPFKXHELB-UHFFFAOYSA-N Chalcone Natural products C=1C=CC=CC=1C(=O)C=CC1=CC=CC=C1 DQFBYFPFKXHELB-UHFFFAOYSA-N 0.000 description 6
- 235000005513 chalcones Nutrition 0.000 description 6
- 229960002725 isoflurane Drugs 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 5
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 5
- 230000000149 penetrating effect Effects 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- NIHJEJFQQFQLTK-UHFFFAOYSA-N butanedioic acid;hexanedioic acid Chemical compound OC(=O)CCC(O)=O.OC(=O)CCCCC(O)=O NIHJEJFQQFQLTK-UHFFFAOYSA-N 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 230000032050 esterification Effects 0.000 description 3
- 238000005886 esterification reaction Methods 0.000 description 3
- 229920000909 polytetrahydrofuran Polymers 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000004144 decalcomania Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000000176 photostabilization Effects 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- -1 acrylic ester Chemical class 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000001261 hydroxy acids Chemical group 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 125000003010 ionic group Chemical group 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229960004418 trolamine Drugs 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Abstract
The invention relates to aqueous jet ink for a cotton fabric and a preparation method thereof. The invention relates to a chitosan modified polyurethane emulsion and a preparation method thereof. The chitosan modified polyurethane emulsion is prepared from the following raw materials in parts by weight by the following steps: firstly mixing 15-22 parts of diisocyanate, 51-66 parts of polyhydric alcohols and 2-6 parts of a carboxylic hydrophilic monomer for pre-polymerization reaction and adding 10-20 parts of polyglycerol to block and adding 0.5-4 parts of a salifying auxiliary to obtain a polyurethane prepolymer; then, adding 135-180 parts of deionized water for ionization reaction to obtain the polyurethane emulsion; and finally adding 1.5-5 parts of chitosan and 100-150 parts of a citric acid aqueous solution into every 100 parts of the polyurethane prepolymer to be modified to obtain the chitosan modified polyurethane emulsion. The invention further relates to application of the chitosan modified polyurethane emulsion in preparation of the aqueous jet ink for the cotton fabric. The aqueous jet ink provided by the invention has a strong adhesive force on purified cotton and cotton-polyester blended fabrics, the fabric needs not to be pre-treated, and a printed product is bright in color, high in wet-dye rubbing fastness and washing fastness and flexible in hand feel.
Description
Technical field
The present invention relates to polymer chemistry and textile inkjet printing technical field, be specifically related to a kind of cotton fabric use ink-jet and preparation method thereof, relate more specifically to a kind of cotton fabric use pigment inkjet containing chitin modified polyaminoester emulsion and preparation method thereof.
Background technology
Textiles is digital ink-jet printed is that the pattern of design is inputted computer in digital form, by computer control sprayed printed system, is directly injected on fabric by printing ink, thus prints out various pattern.Compared with Conventional decal technique, it saves lithography process, and production efficiency is high, achieves short run, personalized stamp.Digital ink-jet printed ink mainly comprises type of dye ink and pigment ink two kinds, and type of dye ink is reacted by dyestuff and fiber and combined, and need select different dyestuffs for different fibers, versatility is low.And also needing the operation such as decatize, water-based, oven dry after type of dye ink spray printing, complex process, wastewater discharge is large, and fabric photostabilization is poor.Pigment ink versatility is high, photostabilization good, and printing technology is relatively simple, is just becoming the main development direction that weaving is ink-jet printed.
Pigment in pigment ink does not react with fiber, and the combination of pigment and fiber is realized by the binder in ink.Therefore, the performance of binder has material impact to the soft degree of stamp, colour brightness, crock fastness and washing fastness.Generally, binder consumption is high, and stamp feel is poor, but when binder consumption is low, pigment Bearable dry and wet wipe fastness is low, and therefore, pigment jetting exists the contradiction between feel and color fastness.
For solving the deficiency that pigment ink of the prior art exists, domestic and international patent documentation has proposed many solutions.US Patent No. 6902780 discloses one and carries out pre-treatment to fabric coating, thus improves the method for ink-jet printed color fastness.Chinese patent CN103834233A discloses and a kind of adopts branched polymer coated pigment nanoparticle to be tinting material, without the need to added binding agents, and bright-colored degree and the good ink-jet of colour fastness.Chinese patent CN1687260A discloses a kind of ink-jet adopting polyocarboxy acid type polymer to do dispersion agent and sticking agent, by the hydroxyl generation esterification and crosslinking of the carboxyl in poly carboxylic acid and polyol solvent, pigment particles is made to anchor on base material, tool color fastness in need.Chinese patent CN1803913A discloses a kind of cross-linked acrylic acid that adopts and provides solid space network structure, is firmly attached on fabric fibre by pigment, thus improves the ink-jet of the water-fastness fastness to rubbing of textile printing; But above-mentioned prior art still cannot take into account the requirement of soft degree and color fast degree, still need the cotton fabric use ink-jet seeking a kind of excellent property.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of chitin modified polyaminoester emulsion is provided, described chitin modified polyaminoester emulsion is applied to after preparing the ink-jet of cotton fabric use, the cotton fabric use ink-jet prepared can directly be greater than in the BLENDED FABRIC of 50% in pure cotton fabric or cotton content by spray printing, decalcomania is bright-colored, dry wet rubbing fastness and washing are firmly high, soft.
Another object of the present invention is to the preparation method that above-mentioned chitin modified polyaminoester emulsion is provided.
Another object of the present invention is to provide above-mentioned chitin modified polyaminoester emulsion preparing the application in the ink-jet of cotton fabric use.
Another object of the present invention is to provide the ink-jet of a kind of cotton fabric use.
Another object of the present invention is to the preparation method that the ink-jet of above-mentioned cotton fabric use is provided.
For achieving the above object, the present invention adopts following technical scheme:
A kind of chitin modified polyaminoester emulsion, described chitin modified polyaminoester emulsion is prepared from by following raw material by weight: first by vulcabond 15 ~ 22 parts, polyvalent alcohol 51 ~ 66 parts, prepolymerization is carried out in 2 ~ 6 parts of mixing of carboxylic acid type hydrophilic monomer, add Polyglycerine 10 ~ 20 parts and carry out end-blocking, and add into salt assitant 0.5 ~ 4 part polyurethane prepolymer; Then add deionized water 135 ~ 180 parts to carry out ion reaction and obtain polyaminoester emulsion, finally add the chitosan of 1.5 ~ 5 parts by every 100 parts of polyurethane prepolymers, the aqueous citric acid solution of 100 ~ 150 parts carries out modification to polyaminoester emulsion and namely obtains chitin modified polyaminoester emulsion; Wherein, the mean polymerisation degree of described Polyglycerine is 4 ~ 10; The molecular weight of described chitosan is 5000 ~ 30000.
The preparation method of above-mentioned chitin modified polyaminoester emulsion, specifically comprises the steps:
S1: the polyvalent alcohol after processed, carboxylic acid type hydrophilic monomer and vulcabond are reacted 3 ~ 5 hours at 70 ~ 90 DEG C, then adds Polyglycerine end-blocking, continues reaction 1 ~ 2 hour; After reaction terminates, product is down to below room temperature, then adds into salt assitant ionization 10 ~ 15min and obtain polyurethane prepolymer;
S2. add in deionized water by step S1 gained polyurethane prepolymer, emulsify at a high speed 0.5 ~ 1.0 hour, 60 DEG C vacuumize de-acetone, obtain polyaminoester emulsion;
S3. be dissolved in aqueous citric acid solution by chitosan, then slowly joined by the aqueous citric acid solution of chitosan in the polyaminoester emulsion in step S2, stirring at room temperature 2 ~ 5 hours, obtains chitin modified polyaminoester emulsion;
Wherein, the rotating speed of the emulsify at a high speed in step S2 is 1000 ~ 1500rpm.
Chitin modified polyaminoester emulsion provided by the invention is particularly useful for preparing the ink-jet of cotton fabric use, contriver finds when the ink-jet of cotton fabric use being prepared by chitin modified polyaminoester emulsion, the attachment fastness of selection on aqueous jet and cotton of the molecular weight of chitosan affects larger, when the molecular weight of the chitosan selected is 5000 ~ 30000, the fastness between the aqueous jet of preparation and cotton is moderate and be beneficial to ink-jet; Select other molecular weight chitin modified after the aqueous jet poor-performing prepared of polyaminoester emulsion; This is because when the molecular weight of chitosan is less than 5000, the attachment fastness of chitin modified polyaminoester emulsion to cotton can be affected; And when the molecular weight of chitosan is greater than 30000, chitosan solution viscosity is comparatively large, more deionized water need be added and reduce viscosity, be unfavorable for the design of inkjet formulation.
Preferably, the deacetylation of described chitosan is greater than 70%.The deacetylation of chitosan is low, not only can affect the solubility property of chitosan, and due to ionizable-NH
2reduce, cause and-COO
-interactional-the NH of negatively charged ion
3 +positive ion reduces, thus affects the covered effect of chitosan at polyurethane surface, the consistency of both reductions.
Preferably, described carboxylic acid type hydrophilic monomer is any monomer that this area is commonly used, and in the present invention, can select one or both the mixture in dimethylol propionic acid, dimethylolpropionic acid.
Preferably, the massfraction of described aqueous citric acid solution is 1 ~ 3%.The massfraction of aqueous citric acid solution is less than 1%, be then unfavorable for the dissolving of chitosan; Massfraction is greater than 3%, can affect again the pH value of emulsion, thus affect stability of emulsion.
Preferably, described vulcabond is one or more in isophorone diisocyanate, hexamethylene diisocyanate, tolylene diisocyanate, diphenylmethanediisocyanate; The molecular weight of described polyvalent alcohol is 1000 ~ 3000, further preferably, described polyvalent alcohol is one or more in polyethylene glycol adipate, poly adipate succinic acid ester, PCDL, polycaprolactone diols, polypropylene glycol, polytetrahydrofuran dibasic alcohol.
The ink-jet of a kind of cotton fabric use, the ink-jet of described cotton fabric use is prepared from by following raw material by weight: chitin modified polyaminoester emulsion 25 ~ 50 parts, water nano dispersible pigment color paste 13 ~ 30 parts, carbodiimide cross-linker 1 ~ 3 part, pH adjusting agent 0.2 ~ 0.5 part, organic blend solvent 12 ~ 30 parts, deionized water 10 ~ 18 parts;
Wherein, described chitin modified polyaminoester emulsion is prepared from by following raw material by weight: first by vulcabond 15 ~ 22 parts, polyvalent alcohol 51 ~ 66 parts, prepolymerization is carried out in 2 ~ 6 parts of mixing of carboxylic acid type hydrophilic monomer, add Polyglycerine 10 ~ 20 parts and carry out end-blocking, and add into salt assitant 0.5 ~ 4 part polyurethane prepolymer; Then add deionized water 135 ~ 180 parts to carry out ion reaction and obtain polyaminoester emulsion, finally add the chitosan of 1.5 ~ 5 parts by every 100 parts of polyurethane prepolymers, the aqueous citric acid solution of 100 ~ 150 parts carries out modification to polyaminoester emulsion and namely obtains chitin modified polyaminoester emulsion.
The preparation method of above-mentioned cotton fabric use ink-jet is as follows:
Mixed with deionized water by organic blend solvent, add chitin modified polyaminoester emulsion, water nano dispersible pigment color paste successively, dispersed with stirring is even, be 7.5 ~ 8.0 by pH adjusting agent adjust ph, add carbodiimide again, stir evenly, obtain the ink-jet of cotton fabric use.
The present invention first synthesizes the base polyurethane prepolymer for use as that end group is isocyanic ester, by calculating the molar weight of-NCO in performed polymer, the Polyglycerine adding equimolar amount carries out end-blocking, Polyglycerine has multiple hydroxyl, Polyglycerine is introduced the wetting ability that can improve polymer molecular chain in urethane, thus improve the stability of polyaminoester emulsion; Secondly, the poly-hydroxy of Polyglycerine has stronger absorption or anchorage effect to granules of pigments, can improve the dispersion stabilization of pigment in ink-jet.
The present invention introduces carboxylic acid type hydrophilic monomer in polyurethane molecular chain, by ionization and emulsify at a high speed, forms surface arrangement and COO
-the emulsion particle of negatively charged ion, and the amino of chitosan formation-NH in citric acid solution
3 +positive ion, by both mix and blends, by the interaction between negative ions, define Chitosan-coated outside, urethane is at interior emulsion particle.Because chitosan is with comparatively polyamino and hydroxyl, there is interaction force with the hydroxyl of cotton fibre, therefore, by Chitosan-coated on emulsion particle surface, effectively can improve the sticking power of modified polyurethane to cotton fabric.In addition, select citric acid solution dissolve chitosan be because, citric acid both can with cotton fibre generation esterification, also can with the hydroxyl generation esterification of chitosan, the sticking power between the splicing of further reinforced company and cotton fibre.The consumption of preferred chitosan accounts for 1.5 ~ 5% of polyurethane prepolymer amount, when the consumption of chitosan is more than 5%, can affect the snappiness of polyaminoester emulsion, and then affect ink-jet printed feel.In the present invention, the mean polymerisation degree of described Polyglycerine is 4 ~ 10.When the polymerization degree of Polyglycerine is less than 4, enough anchorings or adsorption be there is no to pigment, cause spray printing product colour to grow dim, uneven; Along with the polymerization degree increases, Polyglycerine institute is hydroxyl to increase, in emulsifying polyurethane process, be with polyhydric Polyglycerine can be enriched in emulsion particle surface, when the polymerization degree of Polyglycerine is greater than 10, the hydroxyl of emulsion particle surface enrichment is too much, and the hydrogen bond action between emulsion particle is excessively strong, causes emulsion to store viscosity and increases.
The molecular weight of the polyvalent alcohol selected in the present invention is 1000 ~ 3000, this is because when the molecular weight of polyvalent alcohol is less than 1000, the snappiness through chitin modified polyaminoester emulsion can be caused to decline, affect the soft degree of cotton fabric printing product; And when molecular weight is greater than 3000, then can affect the tensile elasticity of cotton fabric printing product very little because of the isocyanic ester as hard section.
Organic blend solvent of the present invention is the mixture of one or more in ethylene glycol, propylene glycol, glycol ether, butyl glycol ether, butyl, glycerine, 2-Pyrrolidone etc.
Described one-tenth salt assitant in the present invention is can generate the reagent of salt or ionic group with carboxyl, preferably, can select one or both the mixture in triethylamine, ammoniacal liquor.Ink-jet printed in baking process, along with the volatilization of salt-forming reagent, hydroxy-acid group comes out, and the carbodiimide in ink-jet and carboxyl react, and the webbed crosslinking structure of shape, is firmly attached to pigment on fabric fibre.
Compared with prior art, the present invention has following beneficial effect:
(1) the present invention adopts Polyglycerine blocked polyurethane, the polyhydroxy structure of Polyglycerine can improve the hydrophilic stability of urethane, to pigment, there is absorption or anchorage effect again, be conducive to improving the dispersiveness of pigment in the chitin modified polyaminoester emulsion of binder, directly be sprayed on fabric after drying by aqueous jet of the present invention, hydroxyl and fibre-effects make pigment attachment fastness improve.
(2) the present invention is by-the COO of polyaminoester emulsion
-with-the NH of chitosan solution
3 +interact, form Chitosan-coated outside, urethane, at interior chitin modified polyaminoester emulsion, is conducive to the amino of chitosan, hydroxyl and cotton fibre effect, and under the effect of citric acid, strengthens chitin modified polyaminoester emulsion further to the sticking power of cotton fabric.
(3) the present invention selects chitin modified polyaminoester emulsion as binder, and described chitin modified polyaminoester emulsion can be good at pigment and fiber to couple together, and increases the firmness stamp good hand touch simultaneously of pigment; Cotton fabric use ink-jet prepared by the present invention can directly be greater than on the polyester cotton of 50% in pure cotton fabric or cotton content by spray printing, and decalcomania is bright-colored, dry wet rubbing fastness and washing fastness high, soft.
Embodiment
Below in conjunction with specific embodiment, the present invention is further explained, but embodiments of the present invention is not limited in any way.Unless stated otherwise, involved in embodiment reagent, method are the conventional reagent in this area and method.The mill base that the water nano dispersible pigment color paste that the present invention uses is Cabot Co., Ltd, pigment content is about 15%.
Ink-jet printed performance test: measure ink jet viscosity with reference to the rotational method in GB/T 10247-2008; GB/T 19077.1-2008 measures the D50 granularity of ink-jet; With reference to GB/T 3920-2008 textiles colour fastness to rubbing testing method, colour fastness to rubbing tester is utilized to carry out doing/wet friction colour fastness detection, adopt GB/T 5713 to test the color fastness to water of textiles, and evaluate the staining progression of sample according to GB251 grey scale for assessing staining of colour.
the synthesis of the chitin modified polyaminoester emulsion of embodiment 1
Described chitin modified polyaminoester emulsion mainly composed as follows:
| Material title | Quality/g |
| Isoflurane chalcone diisocyanate | 16.0 |
| Polypropylene glycol (Mn=2000) | 65.9 |
| Dimethylolpropionic acid | 4.8 |
| Polyglycerine (mean polymerisation degree is 10) | 10.0 |
| Triethylamine | 3.3 |
| Deionized water | 155 |
| Chitosan (molecular weight 30000) | 3.0 |
| 2% aqueous citric acid solution | 150 |
The chitin modified polyaminoester emulsion of the present embodiment, its concrete preparation process is as follows
S1. the polypropylene glycol after processed, dimethylolpropionic acid and isoflurane chalcone diisocyanate are reacted 3 hours at 90 DEG C, then add Polyglycerine continuation reaction 2 hours; Thing to be polymerized is down to below room temperature, adds triethylamine ionization 10min, controls viscosity to avoid pole-climbing, obtain polyurethane prepolymer in reaction process with acetone;
S2. add in deionized water by polyurethane prepolymer, emulsify at a high speed is after 1.0 hours, and 60 DEG C vacuumize de-acetone, obtain polyaminoester emulsion;
S3. chitosan is dissolved in aqueous citric acid solution, and slowly joins in polyaminoester emulsion, stirring at room temperature 5 hours, obtains chitin modified polyaminoester emulsion.
The chitin modified polyaminoester emulsion of gained is micro-yellow half penetrating, and solid content is that at 25.3%, 25 DEG C, viscosity is 170mpa.s.
Above-mentioned chitin modified polyaminoester emulsion is applied to and prepares cotton fabric water-soluble ink-jet, described cotton fabric use ink-jet mainly composed as follows:
Organic blend solvent is mixed with deionized water, adds above-mentioned chitin modified polyaminoester emulsion, water nano 122 redness slurry successively, utilize stirrer to be uniformly dispersed, be 7.6 by Monoethanolamine MEA BASF adjust ph, add carbodiimide again, stir evenly, obtain the ink-jet of cotton fabric use.At 25 DEG C, the viscosity of ink-jet is 3.5 mpa.s, D50 particle diameter is 157nm.
Test shows, this ink-jet is bright-coloured through baking and banking up with earth gained printed color after spray printing on cotton fabric, xerotripsis fastness 4 grades, wet rubbing fastness 3 grades, and color fastness to water 4 grades, stamp is soft, smooth tack-free.
the synthesis of the chitin modified polyaminoester emulsion of embodiment 2
Described chitin modified polyaminoester emulsion mainly composed as follows:
| Material title | Quality/g |
| Diphenylmethanediisocyanate | 21.2 |
| Polypropylene glycol (Mn=2000) | 35.0 |
| PCDL (Mn=2000) | 16.8 |
| Dimethylol propionic acid | 6.0 |
| Polyglycerine (mean polymerisation degree is 8) | 17.2 |
| Triethylamine | 3.8 |
| Deionized water | 180 |
| Chitosan (molecular weight is 5000) | 5.0 |
| 3% aqueous citric acid solution | 150 |
The chitin modified polyaminoester emulsion of the present embodiment, its concrete preparation process is as follows
S1. the polypropylene glycol after processed, PCDL, dimethylol propionic acid and diphenylmethanediisocyanate are reacted 5 hours at 70 DEG C, then add Polyglycerine, 80 DEG C are reacted 1.5 hours; Thing to be polymerized is down to below room temperature, adds triethylamine ionization 15min, controls viscosity to avoid pole-climbing in reaction process with acetone; Obtain polyurethane prepolymer.
S2. add in deionized water by polyurethane prepolymer, emulsify at a high speed is after 1.0 hours, and 60 DEG C vacuumize de-acetone, obtain polyaminoester emulsion.
S3. chitosan is dissolved in aqueous citric acid solution, and slowly joins in polyaminoester emulsion, stirring at room temperature 2 hours, obtains chitin modified polyaminoester emulsion.
The chitin modified polyaminoester emulsion of gained is micro-yellow half penetrating, and solid content is that at 23.9%, 25 DEG C, viscosity is 195mpa.s.
Above-mentioned chitin modified polyaminoester emulsion is applied to and prepares cotton fabric water-soluble ink-jet, described cotton fabric use ink-jet mainly composed as follows:
Organic blend solvent is mixed with deionized water, adds above-mentioned chitin modified polyaminoester emulsion, water nano 074 yellow pulp successively, utilize stirrer to be uniformly dispersed, be 8.0 by Monoethanolamine MEA BASF adjust ph, add carbodiimide again, stir evenly, obtain the ink-jet of cotton fabric use.At 25 DEG C, the viscosity of ink-jet is 4.2 mpa.s, D50 particle diameter is 134nm.
Test shows, this ink-jet is bright-coloured through baking and banking up with earth gained printed color after spray printing on cotton fabric, xerotripsis fastness 4 grades, wet rubbing fastness 4 grades, and color fastness to water 4 grades, stamp is soft, smooth tack-free.
the synthesis of the chitin modified polyaminoester emulsion of embodiment 3
Described chitin modified polyaminoester emulsion mainly composed as follows:
| Material title | Quality/g |
| Hexamethylene diisocyanate | 15.6 |
| Polypropylene glycol (Mn=1000) | 32.0 |
| Polytetrahydrofuran dibasic alcohol (Mn=2000) | 30.3 |
| Dimethylol propionic acid | 2.0 |
| Polyglycerine (mean polymerisation degree is 4) | 19.5 |
| Ammoniacal liquor | 0.6 |
| Deionized water | 135 |
| Chitosan (molecular weight is 15000) | 1.5 |
| 1.0% aqueous citric acid solution | 100 |
The chitin modified polyaminoester emulsion of the present embodiment, its concrete preparation process is as follows
S1. the polypropylene glycol after processed, polytetrahydrofuran dibasic alcohol, dimethylol propionic acid and hexamethylene diisocyanate are reacted 4 hours at 85 DEG C, then add Polyglycerine continuation reaction 1.0 hours; Thing to be polymerized is down to below room temperature, adds triethylamine ionization 10min, controls viscosity to avoid pole-climbing in reaction process with acetone; Obtain polyurethane prepolymer.
S2. add in deionized water by prepolymer, emulsify at a high speed 0.5 hour, 60 DEG C vacuumize de-acetone, obtain polyaminoester emulsion.
S3. chitosan is dissolved in aqueous citric acid solution, and slowly joins in polyaminoester emulsion, stirring at room temperature 3 hours, obtains chitin modified polyaminoester emulsion.
The chitin modified polyaminoester emulsion of gained is micro-yellow half penetrating, and solid content is that at 29.9%, 25 DEG C, viscosity is 210mpa.s.
Above-mentioned chitin modified polyaminoester emulsion is applied to and prepares cotton fabric water-soluble ink-jet, described cotton fabric use ink-jet mainly composed as follows:
Organic blend solvent is mixed with deionized water, adds above-mentioned chitin modified polyaminoester emulsion, water nano black slurry successively, utilize stirrer to be uniformly dispersed, be 7.8 by trolamine adjust ph, add carbodiimide again, stir evenly, obtain the ink-jet of cotton fabric use.At 25 DEG C, the viscosity of ink-jet is 3.8 mpa.s, D50 particle diameter is 163nm.
Test shows, this ink-jet is bright-coloured through baking and banking up with earth gained printed color after spray printing on cotton fabric, xerotripsis fastness 4 grades, wet rubbing fastness 4 grades, and color fastness to water 4 grades, stamp is soft, smooth tack-free.
the synthesis of the chitin modified polyaminoester emulsion of embodiment 4
Described chitin modified polyaminoester emulsion mainly composed as follows:
| Material title | Quality/g |
| Isoflurane chalcone diisocyanate | 17.9 |
| Poly adipate succinic acid ester (Mn=3000) | 22.0 |
| Polypropylene glycol (Mn=2000) | 34.4 |
| Dimethylol propionic acid | 5.0 |
| Polyglycerine (mean polymerisation degree is 6) | 17.1 |
| Triethylamine | 3.6 |
| Deionized water | 160 |
| Chitosan (molecular weight is 10000) | 4.0 |
| 2.0% aqueous citric acid solution | 140 |
The chitin modified polyaminoester emulsion of the present embodiment, its concrete preparation process is as follows
S1. the poly adipate succinic acid ester after processed, polypropylene glycol, dimethylol propionic acid and isoflurane chalcone diisocyanate are reacted 4 hours at 85 DEG C, then add Polyglycerine continuation reaction 1.5 hours; Thing to be polymerized is down to below room temperature, adds triethylamine ionization 10min, controls viscosity to avoid pole-climbing in reaction process with acetone; Obtain polyurethane prepolymer.
S2. add in deionized water by prepolymer, emulsify at a high speed 0.5 hour, 60 DEG C vacuumize de-acetone, obtain polyaminoester emulsion.
S3. chitosan is dissolved in aqueous citric acid solution, and slowly joins in polyaminoester emulsion, stirring at room temperature 3 hours, obtains chitin modified polyaminoester emulsion.
The chitin modified polyaminoester emulsion of gained is micro-yellow half penetrating, and solid content is that at 25.5%, 25 DEG C, viscosity is 200mpa.s.
Above-mentioned chitin modified polyaminoester emulsion is applied to and prepares cotton fabric water-soluble ink-jet, described cotton fabric use ink-jet mainly composed as follows:
Organic blend solvent is mixed with deionized water, adds chitin modified polyaminoester emulsion, water nano 15:3 phthalocyanine blue mill base successively, utilize stirrer to be uniformly dispersed, be 7.8 by Monoethanolamine MEA BASF adjust ph, add carbodiimide again, stir evenly, obtain the ink-jet of cotton fabric use.At 25 DEG C, the viscosity of ink-jet is 4.2 mpa.s, D50 particle diameter is 188nm.
Test shows, this ink-jet is bright-coloured through baking and banking up with earth gained printed color after spray printing on cotton fabric, xerotripsis fastness 4 grades, wet rubbing fastness 4 grades, and color fastness to water 4 grades, stamp is soft, smooth tack-free.
Reference examples 1 acrylatcs systems aqueous jet
Ink-jet mainly composed as follows:
Organic blend solvent is mixed with deionized water, adds 148 acrylic ester emulsions, water nano 122 mill base successively, utilize stirrer to be uniformly dispersed, be 7.5 by Monoethanolamine MEA BASF adjust ph, then add carbodiimide, stir evenly, obtain the ink-jet of cotton fabric use.At 25 DEG C, the viscosity of ink-jet is 4.7 mpa.s, D50 particle diameter is 195nm.
Test shows, this ink-jet is bright-coloured through baking and banking up with earth gained printed color after spray printing on cotton fabric, xerotripsis fastness 4 grades, wet rubbing fastness 2 grades, color fastness to water 3 grades, and stamp feel is comparatively hard, a little sticky hand.
reference examples 2polyurethane system aqueous jet
Described polyaminoester emulsion mainly composed as follows:
| Material title | Quality/g |
| Isoflurane chalcone diisocyanate | 16.0 |
| Polypropylene glycol (Mn=2000) | 65.9 |
| Dimethylolpropionic acid | 4.8 |
| Triethylamine | 3.3 |
| Deionized water | 250 |
| Quadrol | 0.18 |
The polyaminoester emulsion of the present embodiment, its concrete preparation process is as follows
Polypropylene glycol after processed, dimethylolpropionic acid and isoflurane chalcone diisocyanate are reacted 4 hours at 90 DEG C; Thing to be polymerized is down to below room temperature, changes ice-water bath into, adds triethylamine ionization 10min; Control viscosity to avoid pole-climbing with acetone in reaction process, obtain polyurethane prepolymer.
Less than 5 DEG C, polyurethane prepolymer is added in deionized water, after emulsify at a high speed 5min, add quadrol, chain extending reaction 2h.60 DEG C vacuumize de-acetone, obtain polyaminoester emulsion.
Gained polyaminoester emulsion is milky white, half penetrating, and solid content is that at 26.0%, 25 DEG C, viscosity is 205mpa.s.
Above-mentioned polyaminoester emulsion is applied to and prepares cotton fabric water-soluble ink-jet, described cotton fabric use ink-jet mainly composed as follows:
Organic blend solvent is mixed with deionized water, adds above-mentioned polyaminoester emulsion, water nano 122 redness slurry successively, utilize stirrer to be uniformly dispersed, be 7.5 by Monoethanolamine MEA BASF adjust ph, then add carbodiimide, stir evenly, obtain the ink-jet of cotton fabric use.At 25 DEG C, the viscosity of ink-jet is 4.0 mpa.s, D50 particle diameter is 197nm.
Test shows, this ink-jet is bright-coloured through baking and banking up with earth gained printed color after spray printing on cotton fabric, xerotripsis fastness 3 grades, wet rubbing fastness 1 grade, and color fastness to water 2 grades, stamp is soft, smooth tack-free.
As can be seen from embodiment and comparative example 1, adopt the aqueous jet that modified polyurethane of the present invention is obtained, the aqueous jet wet rubbing fastness more obtained than existing employing acrylate, color fastness to water, soft degree are all significantly improved; Comparative example 2 can be found out, its wet rubbing fastness of aqueous jet adopting conventional urethane obtained, color fastness to water are all poor, even also do not reach the effect of acrylate.
Claims (9)
1. a chitin modified polyaminoester emulsion, it is characterized in that, described chitin modified polyaminoester emulsion is prepared from by following raw material by weight: first by vulcabond 15 ~ 22 parts, polyvalent alcohol 51 ~ 66 parts, prepolymerization is carried out in 2 ~ 6 parts of mixing of carboxylic acid type hydrophilic monomer, add Polyglycerine 10 ~ 20 parts and carry out end-blocking, and add into salt assitant 0.5 ~ 4 part polyurethane prepolymer; Then add deionized water 135 ~ 180 parts to carry out ion reaction and obtain polyaminoester emulsion, finally add the chitosan of 1.5 ~ 5 parts by every 100 parts of polyurethane prepolymers, the aqueous citric acid solution of 100 ~ 150 parts carries out modification to polyaminoester emulsion and namely obtains chitin modified polyaminoester emulsion; Wherein, the mean polymerisation degree of described Polyglycerine is 4 ~ 10; The molecular weight of described chitosan is 5000 ~ 30000.
2. chitin modified polyaminoester emulsion according to claim 1, it is characterized in that, the deacetylation of described chitosan is greater than 70%.
3. chitin modified polyaminoester emulsion according to claim 1, it is characterized in that, described carboxylic acid type hydrophilic monomer is one or both the mixture in dimethylol propionic acid, dimethylolpropionic acid.
4. chitin modified polyaminoester emulsion according to claim 1, it is characterized in that, the massfraction of described aqueous citric acid solution is 1 ~ 3%.
5. chitin modified polyaminoester emulsion according to claim 1, it is characterized in that, described vulcabond is one or more in isophorone diisocyanate, hexamethylene diisocyanate, tolylene diisocyanate, diphenylmethanediisocyanate; The molecular weight of described polyvalent alcohol is 1000 ~ 3000.
6. the preparation method of chitin modified polyaminoester emulsion described in the arbitrary claim of claim 1 to 5, is characterized in that, specifically comprise the steps:
S1: the polyvalent alcohol after processed, carboxylic acid type hydrophilic monomer and vulcabond are reacted 3 ~ 5 hours at 70 ~ 90 DEG C, then adds Polyglycerine end-blocking, continues reaction 1 ~ 2 hour; After reaction terminates, product is down to below room temperature, then adds into salt assitant ionization 10 ~ 15min and obtain polyurethane prepolymer;
S2. add in deionized water by step S1 gained polyurethane prepolymer, emulsify at a high speed 0.5 ~ 1.0 hour, 60 DEG C vacuumize de-acetone, obtain polyaminoester emulsion;
S3. be dissolved in aqueous citric acid solution by chitosan, then slowly joined by the aqueous citric acid solution of chitosan in the polyaminoester emulsion in step S2, stirring at room temperature 2 ~ 5 hours, obtains chitin modified polyaminoester emulsion.
7. chitin modified polyaminoester emulsion described in the arbitrary claim of claim 1 to 5 is preparing the application in the ink-jet of cotton fabric use.
8. cotton fabric use ink-jet, it is characterized in that, the ink-jet of described cotton fabric use is prepared from by following raw material by weight: chitin modified polyaminoester emulsion 25 ~ 50 parts described in the arbitrary claim of claim 1 to 5, water nano dispersible pigment color paste 13 ~ 30 parts, carbodiimide cross-linker 1 ~ 3 part, pH adjusting agent 0.2 ~ 0.5 part, organic blend solvent 12 ~ 30 parts, deionized water 10 ~ 18 parts.
9. cotton fabric use ink-jet described in claim 8, it is characterized in that, the preparation method of described cotton fabric use ink-jet is as follows: mixed with deionized water by organic blend solvent, add chitin modified polyaminoester emulsion, water nano dispersible pigment color paste successively, dispersed with stirring is even, is 7.5 ~ 8.0, then adds carbodiimide by pH adjusting agent adjust ph, stir evenly, obtain the ink-jet of cotton fabric use.
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| CN111117359A (en) * | 2019-12-30 | 2020-05-08 | 珠海天威新材料股份有限公司 | Water-based pigment ink for spinning and preparation method thereof |
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