CN114149556B - Aldehyde ketone modified self-extinction aqueous polyurethane dispersion and preparation method thereof - Google Patents
Aldehyde ketone modified self-extinction aqueous polyurethane dispersion and preparation method thereof Download PDFInfo
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- CN114149556B CN114149556B CN202111371597.7A CN202111371597A CN114149556B CN 114149556 B CN114149556 B CN 114149556B CN 202111371597 A CN202111371597 A CN 202111371597A CN 114149556 B CN114149556 B CN 114149556B
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- -1 Aldehyde ketone Chemical class 0.000 title claims abstract description 50
- 229920003009 polyurethane dispersion Polymers 0.000 title claims description 13
- 238000002360 preparation method Methods 0.000 title claims description 12
- 229920002635 polyurethane Polymers 0.000 claims abstract description 49
- 239000004814 polyurethane Substances 0.000 claims abstract description 49
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 24
- 239000002562 thickening agent Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 125000005442 diisocyanate group Chemical group 0.000 claims abstract description 9
- 239000013530 defoamer Substances 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 32
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 22
- 150000002009 diols Chemical class 0.000 claims description 19
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000004970 Chain extender Substances 0.000 claims description 12
- 238000004945 emulsification Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 claims description 6
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 6
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 6
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- 229920001451 polypropylene glycol Polymers 0.000 claims description 6
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 claims description 5
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 5
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 5
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 5
- 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 5
- 229920000728 polyester Polymers 0.000 claims description 5
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 5
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- ACCCMOQWYVYDOT-UHFFFAOYSA-N hexane-1,1-diol Chemical compound CCCCCC(O)O ACCCMOQWYVYDOT-UHFFFAOYSA-N 0.000 claims description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- ORLQHILJRHBSAY-UHFFFAOYSA-N [1-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1(CO)CCCCC1 ORLQHILJRHBSAY-UHFFFAOYSA-N 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 239000006260 foam Substances 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 9
- 230000001070 adhesive effect Effects 0.000 abstract description 9
- 230000000704 physical effect Effects 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 230000008033 biological extinction Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000006224 matting agent Substances 0.000 description 4
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 3
- 229920001610 polycaprolactone Polymers 0.000 description 3
- 239000004632 polycaprolactone Substances 0.000 description 3
- 229920000515 polycarbonate Polymers 0.000 description 3
- 239000004417 polycarbonate Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000002313 adhesive film Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- VEIOBOXBGYWJIT-UHFFFAOYSA-N cyclohexane;methanol Chemical compound OC.OC.C1CCCCC1 VEIOBOXBGYWJIT-UHFFFAOYSA-N 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4027—Mixtures of compounds of group C08G18/54 with other macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
- C08G18/4269—Lactones
- C08G18/4277—Caprolactone and/or substituted caprolactone
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/54—Polycondensates of aldehydes
- C08G18/548—Polycondensates of aldehydes with ketones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
Abstract
The invention discloses an aldehyde ketone modified self-extinction aqueous polyurethane dispersoid which mainly comprises the following components in percentage by weight: 100 parts of aldehyde ketone modified self-extinction waterborne polyurethane, 0.01-0.05 part of defoamer, 0.5-1 part of pH regulator and 1-3 parts of thickener; according to the aldehyde ketone modified self-extinction waterborne polyurethane dispersoid, aldehyde ketone resin and diisocyanate are polymerized, so that the aldehyde ketone resin is introduced into a molecular chain structure of the waterborne self-extinction polyurethane, the aldehyde ketone resin is connected with the waterborne self-extinction polyurethane through chemical bonds, the combination of the aldehyde ketone resin and the waterborne self-extinction polyurethane on a molecular level is realized, and the defects of low film forming strength, poor adhesive force, poor physical property and the like of the resin of the waterborne self-extinction polyurethane are overcome, so that the novel modified waterborne self-extinction polyurethane with excellent water resistance, adhesive force and heat resistance is prepared.
Description
Technical Field
The invention belongs to the field of production and preparation of extinction resins, and particularly relates to an aldehyde-ketone modified self-extinction waterborne polyurethane dispersion and a preparation method thereof.
Background
The aqueous polyurethane matting resin has the characteristics of soft luster and strong high-grade feel by taking matting as surface decoration, and is increasingly popular in the fields of leather finishing, printing ink, papermaking, food packaging and the like in recent years. The addition of matting agents to aqueous polyurethane resins is the most common way to achieve a matting effect. However, most of the conventional matting agents are inorganic substances, the compatibility of the matting agents and an organic polyurethane matrix is poor, the dispersion is difficult to be uniform, the film formation is discontinuous, the matting agents and the matrix do not realize the combination of molecular level, and the physical properties such as scratch resistance, bending resistance, hand feeling and the like of the adhesive film are affected.
The self-extinction type aqueous polyurethane has extinction effect without externally adding an extinction agent, and overcomes the problem of inorganic extinction agent compatibility, but the conventional aqueous self-extinction polyurethane forms larger emulsion particles to obtain extinction effect by controlling the emulsification process, and the resin has low film forming strength, poor adhesive force, poor physical property and poor heat resistance, and influences the widening of application fields.
Disclosure of Invention
The invention aims to provide an aldehyde ketone modified self-extinction waterborne polyurethane dispersoid and a preparation method thereof, wherein aldehyde ketone resin and diisocyanate are polymerized to introduce the aldehyde ketone resin into a molecular chain structure of the waterborne self-extinction polyurethane, the aldehyde ketone resin is connected with the waterborne self-extinction polyurethane through chemical bonds to realize the combination of the aldehyde ketone resin and the waterborne self-extinction polyurethane on a molecular level, and the defects of low film forming strength, poor adhesive force, poor physical property and the like of the resin of the waterborne self-extinction polyurethane are overcome, so that the novel modified waterborne self-extinction polyurethane with excellent water resistance, adhesive force and heat resistance is prepared.
The technical scheme of the invention relates to an aldehyde-ketone modified self-extinction aqueous polyurethane dispersoid, which mainly comprises the following components in percentage by weight:
the preparation method of the aldehyde ketone modified self-extinction aqueous polyurethane dispersoid comprises the following steps:
firstly, aldehyde-ketone modified self-extinction waterborne polyurethane with the weight of the formula components and a defoaming agent are fully mixed at a high speed;
secondly, reducing the rotating speed and stirring the mixed solution at a low speed, and adding a pH regulator and a thickener into the mixed solution in a mode of adding the pH regulator and the thickener in batches for many times after eliminating foam in the mixed solution:
firstly, adding a first batch of pH regulator into the mixed solution, and regulating the pH value of the mixed solution to be 8-10; then adding a first batch of thickener, and uniformly mixing; and then adding the pH regulator and the thickener of the next batch in sequence until the weight of the components of the formula is added.
Preferably: the preparation method of the aldehyde ketone modified self-extinction waterborne polyurethane comprises the following steps:
s1, mixing 60-80 parts of macromolecular diol, 5-20 parts of aldehyde ketone resin, 10-30 parts of butanone, 3-6 parts of hydrophilic chain extender, 0-2 parts of micromolecular dihydric alcohol and 40-60 parts of diisocyanate, and reacting for 2-3 hours at 70-95 ℃ to obtain a prepolymer;
s2, cooling the prepolymer to 65 ℃, and then adding 30-60 parts of acetone into the prepolymer for viscosity reduction;
s3, adding 2-4 parts of neutralizer for neutralization for 30min, and then adding 250-350 parts of deionized water for emulsification while stirring;
s4, adding 8-15 parts of chain extender after emulsification is completed, reacting at 20-60 ℃ until the reaction is complete, and then distilling under reduced pressure to remove acetone to obtain aldehyde ketone modified self-extinction waterborne polyurethane.
Preferably: the macromolecular diol is at least one of polypropylene glycol, polytetrahydrofuran glycol, polyester diol, polycaprolactone diol and polycarbonate diol, and the molecular weight of the macromolecular diol is 1000-3000;
the aldehyde ketone resin is at least one of KR-120 and KR-120A, KR-120B;
the hydrophilic chain extender is at least one of dimethylolpropionic acid or dimethylolbutyric acid;
the small molecular dihydric alcohol is at least one of ethylene glycol, butanediol, neopentyl glycol, hexanediol, cyclohexanedimethanol and trimethylolpropane;
the diisocyanate is at least one of isophorone diisocyanate, hexamethylene diisocyanate, 4' -dicyclohexylmethane diisocyanate and toluene diisocyanate;
the neutralizing agent is at least one of triethylamine and N, N-dimethylethanolamine;
the chain extender is at least one of hydrazine hydrate, ethylenediamine, isophorone diamine and diethylenetriamine.
Preferably: the defoamer is at least one of Tego Foamex825, tego Foamex8030 and Tego Foamex 1488;
the pH regulator is at least one of triethylamine, ethanolamine, diethanolamine and triethanolamine;
the thickener is at least one of acrysolASE60, RM-8W and acrysolSCT-275.
The aldehyde ketone modified self-extinction aqueous polyurethane dispersoid has the beneficial effects that: the aldehyde ketone modified self-extinction waterborne polyurethane dispersoid has the advantages of low glossiness, good water resistance, good adhesive force and the like
The preparation method of the aldehyde ketone modified self-extinction waterborne polyurethane dispersoid has the beneficial effects that: the aldehyde ketone resin and the diisocyanate are polymerized to realize that the aldehyde ketone resin is introduced into a molecular chain structure of the water-based self-extinction polyurethane, the aldehyde ketone resin is connected with the water-based self-extinction polyurethane through chemical bonds to realize the combination of the two resins on a molecular level, and the defects of low film forming strength, poor adhesive force, poor physical property and the like of the resin of the water-based self-extinction polyurethane are overcome, so that the novel modified water-based self-extinction polyurethane with excellent water resistance, adhesive force and heat resistance is prepared.
Detailed Description
In order to facilitate the understanding of the technical scheme of the present invention by those skilled in the art, the technical scheme of the present invention will be further described with reference to the embodiments of the specification.
The technical scheme of the invention relates to an aldehyde-ketone modified self-extinction aqueous polyurethane dispersoid, which mainly comprises the following components in percentage by weight:
the preparation method of the aldehyde ketone modified self-extinction aqueous polyurethane dispersoid comprises the following steps:
and firstly, fully mixing the aldehyde-ketone modified self-extinction waterborne polyurethane and the defoamer in high speed according to the weight of the formula components.
And secondly, reducing the rotating speed, stirring the mixed solution at a low speed, and adding the pH regulator and the thickener into the mixed solution in a mode of adding the pH regulator and the thickener in batches for many times after eliminating foam in the mixed solution. Firstly, adding a first batch of pH regulator into the mixed solution, and regulating the pH value of the mixed solution to be 8-10; then adding a first batch of thickener, and uniformly mixing; and then adding the pH regulator and the thickener of the next batch in sequence until the weight of the components of the formula is added.
In the technical scheme of the invention, the preparation method of the aldehyde-ketone modified self-extinction waterborne polyurethane comprises the following steps:
s1, mixing 60-80 parts of macromolecular diol, 5-20 parts of aldehyde ketone resin, 10-30 parts of butanone, 3-6 parts of hydrophilic chain extender, 0-2 parts of micromolecular dihydric alcohol and 40-60 parts of diisocyanate, and reacting for 2-3 hours at 70-95 ℃ to obtain a prepolymer.
S2, cooling the prepolymer to 65 ℃, and then adding 30-60 parts of acetone into the prepolymer for viscosity reduction.
S3, adding 2-4 parts of neutralizer for neutralization for 30min, and then adding 250-350 parts of deionized water for emulsification while stirring.
S4, adding 8-15 parts of chain extender after emulsification is completed, reacting at 20-60 ℃ until the reaction is complete, and then distilling under reduced pressure to remove acetone to obtain aldehyde ketone modified self-extinction waterborne polyurethane.
The technical scheme is as follows:
the macromolecular diol is at least one of polypropylene glycol, polytetrahydrofuran glycol, polyester diol, polycaprolactone diol and polycarbonate diol, and the molecular weight of the macromolecular diol is 1000-3000.
The aldehyde ketone resin is at least one of KR-120 and KR-120A, KR-120B.
The hydrophilic chain extender is at least one of dimethylolpropionic acid or dimethylolbutyric acid.
The small molecular dihydric alcohol is at least one of ethylene glycol, butanediol, neopentyl glycol, hexanediol, cyclohexanedimethanol and trimethylolpropane.
The diisocyanate is at least one of isophorone diisocyanate, hexamethylene diisocyanate, 4' -dicyclohexylmethane diisocyanate and toluene diisocyanate.
The neutralizing agent is at least one of triethylamine and N, N-dimethylethanolamine.
The chain extender is at least one of hydrazine hydrate, ethylenediamine, isophorone diamine and diethylenetriamine.
The defoamer is at least one of Tego Foamex825, tego Foamex8030 and Tego Foamex 1488.
The pH regulator is at least one of triethylamine, ethanolamine, diethanolamine and triethanolamine.
The thickener is at least one of acrysolASE60, RM-8W and acrysolSCT-275.
Based on the above technical solutions, several embodiments are provided below.
Example 1:
the aldehyde ketone modified self-extinction aqueous polyurethane dispersion comprises:
the aldehyde ketone modified self-extinction waterborne polyurethane in the example 1 is prepared according to the following steps:
a1, mixing 80 parts of polypropylene glycol (molecular weight 2000), 20 parts of KR-120A,20 parts of butanone, 6 parts of dimethylolbutanoic acid and 60 parts of hexamethylene diisocyanate, and reacting at 95 ℃ for 3 hours to obtain a prepolymer;
a2, cooling to 65 ℃, and adding 60 parts of acetone into the prepolymer to reduce the viscosity;
a3, adding 4 parts of N, N-dimethylethanolamine to neutralize for 30min, and then adding 320 parts of deionized water while stirring to emulsify;
and A4, adding 15 parts of hydrazine hydrate after emulsification is completed, reacting at 60 ℃ to completion, and then distilling under reduced pressure to remove acetone to obtain aldehyde ketone modified self-extinction waterborne polyurethane.
Example 2:
the aldehyde ketone modified self-extinction aqueous polyurethane dispersion comprises:
the aldehyde ketone modified self-extinction waterborne polyurethane in the example 2 is prepared according to the following steps:
b1, mixing 20 parts of polytetrahydrofuran glycol (molecular weight 2000), 10 parts of polypropylene glycol (molecular weight 1000), 50 parts of polyester diol (molecular weight 3000), 5 parts of KR-120, 10 parts of butanone, 3 parts of dimethylolpropionic acid, 2 parts of ethylene glycol and 40 parts of isophorone diisocyanate, and reacting at 95 ℃ for 2 hours to obtain a prepolymer;
b2, cooling to 65 ℃, and adding 30 parts of acetone into the prepolymer to reduce the viscosity;
b3, adding 2 parts of triethylamine to neutralize for 30min, and then adding 250 parts of deionized water while stirring to emulsify;
and B4, adding 8 parts of isophorone diamine after emulsification is completed, reacting at 40 ℃ to completion, and then distilling under reduced pressure to remove acetone to obtain aldehyde ketone modified self-extinction waterborne polyurethane.
Example 3:
the aldehyde ketone modified self-extinction aqueous polyurethane dispersion comprises:
the aldehyde ketone modified self-extinction waterborne polyurethane in the example 3 is prepared according to the following steps:
c1, mixing 40 parts of polycarbonate dihydric alcohol (molecular weight 2000), 30 parts of polypropylene glycol (molecular weight 2000), 5 parts of KR-120A,20 parts of butanone, 5 parts of dimethylolpropionic acid, 1 part of cyclohexane dimethanol, 20 parts of hexamethylene diisocyanate and 30 parts of isophorone diisocyanate, and reacting at 95 ℃ for 3 hours to obtain a prepolymer;
c2, cooling to 65 ℃, and adding 55 parts of acetone into the prepolymer to reduce the viscosity;
adding 4 parts of N, N-dimethylethanolamine to neutralize for 30min, and then adding 350 parts of deionized water while stirring to emulsify;
and C4, adding 5 parts of hydrazine hydrate and 8 parts of isophorone diamine after emulsification is completed, reacting at 50 ℃ to completion, and then distilling off acetone under reduced pressure to obtain aldehyde ketone modified self-extinction waterborne polyurethane.
Example 4:
the aldehyde ketone modified self-extinction aqueous polyurethane dispersion comprises:
the aldehyde ketone modified self-extinction waterborne polyurethane in this example 4 was prepared according to the following steps:
d1, mixing 60 parts of polytetrahydrofuran glycol (molecular weight 2000), 10 parts of KR-120B, 15 parts of butanone, 4 parts of dimethylolpropionic acid, 1 part of butanediol, 0.5 part of trimethylolpropane and 50 parts of 4,4' -dicyclohexylmethane diisocyanate, and reacting at 95 ℃ for 2 hours to obtain a prepolymer;
d2, cooling to 65 ℃, and adding 40 parts of acetone into the prepolymer for viscosity reduction;
d3, adding 3 parts of triethylamine to neutralize for 30min, and then adding 300 parts of deionized water while stirring to emulsify;
and D4, adding 9 parts of ethylenediamine and 2 parts of isophorone diamine after emulsification is completed, reacting at 40 ℃ to completion, and then distilling off acetone under reduced pressure to obtain aldehyde ketone modified self-extinction waterborne polyurethane.
Example 5:
the aldehyde ketone modified self-extinction aqueous polyurethane dispersion comprises:
the aldehyde ketone modified self-extinction waterborne polyurethane in the example 5 is prepared according to the following steps:
e1, mixing 20 parts of polycaprolactone diol (molecular weight 1000), 40 parts of polyester diol (molecular weight 3000), 12 parts of KR-120, 18 parts of butanone, 4 parts of dimethylolbutanoic acid, 0.5 part of hexanediol, 0.5 part of neopentyl glycol and 40 parts of toluene diisocyanate, and reacting at 70 ℃ for 3 hours to obtain a prepolymer;
e2, cooling to 65 ℃, and adding 45 parts of acetone into the prepolymer to reduce the viscosity;
e3, adding 3 parts of N, N-dimethylethanolamine to neutralize for 30min, and then adding 300 parts of deionized water while stirring to emulsify;
and E4, adding 7 parts of hydrazine hydrate and 1 part of diethylenetriamine after emulsification is completed, reacting at 30 ℃ until the reaction is complete, and then distilling under reduced pressure to remove acetone to obtain the aldehyde ketone modified self-extinction waterborne polyurethane.
To further illustrate the properties of the present invention, such as matting effect and adhesion, the aldehyde-ketone modified self-matting aqueous polyurethane dispersions prepared according to the formulation components in examples 1 to 5 are compared with the commercial product performance index, and the comparison results are shown in table 1 below.
Table 1:
as can be seen from the table 1, the performance such as extinction effect and adhesive force of the aldehyde-ketone modified self-extinction waterborne polyurethane dispersion prepared according to the technical scheme of the invention is superior to that of the commercially available product, and meanwhile, in the technical scheme of the invention, the effect of the aldehyde-ketone modified self-extinction waterborne polyurethane dispersion prepared according to the formula component in the example 2 is optimal.
While the invention has been described above with reference to exemplary embodiments, it should be apparent that the implementation of the invention is not limited by the foregoing, but rather is within the scope of the invention as long as various insubstantial modifications of the method concept and technical solution of the invention are adopted, or the inventive concept and technical solution are directly applied to other occasions without any modifications.
Claims (2)
1. An aldehyde ketone modified self-extinction aqueous polyurethane dispersion, which is characterized in that: the composition mainly comprises the following components:
the preparation method of the aldehyde ketone modified self-extinction aqueous polyurethane dispersoid comprises the following steps:
firstly, aldehyde-ketone modified self-extinction waterborne polyurethane with the weight of the formula components and a defoaming agent are fully mixed at a high speed;
secondly, reducing the rotating speed and stirring the mixed solution at a low speed, and adding a pH regulator and a thickener into the mixed solution in a mode of adding the pH regulator and the thickener in batches for many times after eliminating foam in the mixed solution:
firstly, adding a first batch of pH regulator into the mixed solution, and regulating the pH value of the mixed solution to be 8-10; then adding a first batch of thickener, and uniformly mixing; then, sequentially adding the pH regulator and the thickener of the next batch until the pH regulator and the thickener of the formula component weight are added;
the defoamer is at least one of Tego Foamex825, tego Foamex8030 and Tego Foamex 1488;
the pH regulator is at least one of triethylamine, ethanolamine, diethanolamine and triethanolamine;
the thickener is at least one of acrysolASE60, RM-8W and acrysolSCT-275;
the preparation method of the aldehyde ketone modified self-extinction waterborne polyurethane comprises the following steps:
s1, mixing 60-80 parts of macromolecular diol, 5-20 parts of aldehyde ketone resin, 10-30 parts of butanone, 3-6 parts of hydrophilic chain extender, 0-2 parts of micromolecular dihydric alcohol and 40-60 parts of diisocyanate, and reacting for 2-3 hours at 70-95 ℃ to obtain a prepolymer;
s2, cooling the prepolymer to 65 ℃, and then adding 30-60 parts of acetone into the prepolymer for viscosity reduction;
s3, adding 2-4 parts of neutralizer for neutralization for 30min, and then adding 250-350 parts of deionized water for emulsification while stirring;
s4, adding 8-15 parts of chain extender after emulsification is completed, reacting at 20-60 ℃ until the reaction is complete, and then distilling under reduced pressure to remove acetone to obtain aldehyde-ketone modified self-extinction waterborne polyurethane;
the macromolecular diol is at least one of polypropylene glycol, polytetrahydrofuran glycol and polyester diol, and the molecular weight of the macromolecular diol is 1000-3000;
the aldehyde ketone resin is at least one of KR-120 and KR-120A, KR-120B;
the hydrophilic chain extender is at least one of dimethylolpropionic acid or dimethylolbutyric acid.
2. The aldehyde ketone modified self-extinction waterborne polyurethane dispersion as claimed in claim 1, wherein:
the small molecular dihydric alcohol is at least one of ethylene glycol, butanediol, neopentyl glycol, hexanediol and cyclohexanedimethanol;
the diisocyanate is at least one of isophorone diisocyanate, hexamethylene diisocyanate, 4' -dicyclohexylmethane diisocyanate and toluene diisocyanate;
the neutralizer is at least one of triethylamine and N, N-dimethylethanolamine;
the chain extender is at least one of hydrazine hydrate, ethylenediamine, isophorone diamine and diethylenetriamine.
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