CN117209690A - Carboxylate polymer, preparation method thereof and coating dispersing agent - Google Patents
Carboxylate polymer, preparation method thereof and coating dispersing agent Download PDFInfo
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- CN117209690A CN117209690A CN202311249171.3A CN202311249171A CN117209690A CN 117209690 A CN117209690 A CN 117209690A CN 202311249171 A CN202311249171 A CN 202311249171A CN 117209690 A CN117209690 A CN 117209690A
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- 150000007942 carboxylates Chemical class 0.000 title claims abstract description 54
- 229920000642 polymer Polymers 0.000 title claims abstract description 45
- 239000002270 dispersing agent Substances 0.000 title claims abstract description 43
- 239000011248 coating agent Substances 0.000 title claims abstract description 26
- 238000000576 coating method Methods 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000178 monomer Substances 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 15
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 15
- 239000003999 initiator Substances 0.000 claims abstract description 15
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 14
- 229920000570 polyether Polymers 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 14
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- DYDWKSVZHZNBLO-UHFFFAOYSA-N 4-prop-2-enoxybenzoic acid Chemical compound OC(=O)C1=CC=C(OCC=C)C=C1 DYDWKSVZHZNBLO-UHFFFAOYSA-N 0.000 claims description 7
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 229920003086 cellulose ether Polymers 0.000 claims description 6
- GZNJJEODYYLYSA-UHFFFAOYSA-N diethyl prop-2-enyl phosphate Chemical compound CCOP(=O)(OCC)OCC=C GZNJJEODYYLYSA-UHFFFAOYSA-N 0.000 claims description 6
- CPJRRXSHAYUTGL-UHFFFAOYSA-N isopentenyl alcohol Chemical compound CC(=C)CCO CPJRRXSHAYUTGL-UHFFFAOYSA-N 0.000 claims description 6
- 239000000176 sodium gluconate Substances 0.000 claims description 6
- 229940005574 sodium gluconate Drugs 0.000 claims description 6
- 235000012207 sodium gluconate Nutrition 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- 230000003472 neutralizing effect Effects 0.000 claims description 5
- BYDRTKVGBRTTIT-UHFFFAOYSA-N 2-methylprop-2-en-1-ol Chemical compound CC(=C)CO BYDRTKVGBRTTIT-UHFFFAOYSA-N 0.000 claims description 4
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- UCWBKJOCRGQBNW-UHFFFAOYSA-M sodium;hydroxymethanesulfinate;dihydrate Chemical compound O.O.[Na+].OCS([O-])=O UCWBKJOCRGQBNW-UHFFFAOYSA-M 0.000 claims description 4
- AEUVIXACNOXTBX-UHFFFAOYSA-N 1-sulfanylpropan-1-ol Chemical compound CCC(O)S AEUVIXACNOXTBX-UHFFFAOYSA-N 0.000 claims description 3
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 3
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 3
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 3
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- 239000005913 Maltodextrin Substances 0.000 claims description 3
- 229920002774 Maltodextrin Polymers 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 235000010323 ascorbic acid Nutrition 0.000 claims description 3
- 229960005070 ascorbic acid Drugs 0.000 claims description 3
- 239000011668 ascorbic acid Substances 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 3
- BLCKNMAZFRMCJJ-UHFFFAOYSA-N cyclohexyl cyclohexyloxycarbonyloxy carbonate Chemical compound C1CCCCC1OC(=O)OOC(=O)OC1CCCCC1 BLCKNMAZFRMCJJ-UHFFFAOYSA-N 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 3
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 3
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 3
- -1 isobutenyl alcohol Chemical compound 0.000 claims description 3
- 229940035034 maltodextrin Drugs 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 claims description 3
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 3
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 3
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 3
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 3
- 229940001584 sodium metabisulfite Drugs 0.000 claims description 3
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 3
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 3
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 3
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000003973 paint Substances 0.000 abstract description 32
- 239000006185 dispersion Substances 0.000 abstract description 13
- 239000000945 filler Substances 0.000 abstract description 12
- 230000009471 action Effects 0.000 abstract description 8
- 230000014759 maintenance of location Effects 0.000 abstract description 6
- 239000004568 cement Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- 239000000049 pigment Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 101000908015 Homo sapiens Putative inactive carboxylesterase 4 Proteins 0.000 description 3
- 102100023322 Putative inactive carboxylesterase 4 Human genes 0.000 description 3
- 230000002688 persistence Effects 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 description 2
- 125000001165 hydrophobic group Chemical group 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- WCASXYBKJHWFMY-UHFFFAOYSA-N crotyl alcohol Chemical group CC=CCO WCASXYBKJHWFMY-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention relates to the technical field of paint, in particular to a carboxylate polymer, a preparation method thereof and a paint dispersing agent. The carboxylate polymer comprises, by weight, 600-800 parts of unsaturated polyether, 1.1-1.4 parts of functional monomer A, 6.0-10.0 parts of functional monomer B, 6.9-9.0 parts of initiator, 0.6-1.0 parts of reducing agent, 2.1-2.6 parts of chain transfer agent, 40.0-60.0 parts of C solution, 40.0-50.0 parts of neutralizer and 200.0-220.0 parts of water. The carboxylate polymer and the coating dispersing agent provided by the invention have better dispersibility and viscosity reduction effect than the common coating dispersing agent; the dispersing action process of carboxylate molecules on cement-based filler in the paint is controlled in a chemical and physical mode, so that the dispersing action of carboxylate molecules on cement-based filler in the paint is continuously and slowly carried out within a certain time, and the aim of prolonging the dispersion retention is fulfilled.
Description
Technical Field
The invention relates to the technical field of paint, in particular to a carboxylate polymer, a preparation method thereof and a paint dispersing agent.
Background
The dispersing agent is an auxiliary agent which can uniformly disperse solid particles in a solvent, one end of the dispersing agent is a hydrophilic group, and the other end of the dispersing agent is a hydrophobic group; hydrophilic groups are often polar groups such as carboxylic, sulfonic, sulfuric, amino or amine groups and salts, while hydrophobic groups are often nonpolar hydrocarbon chains such as hydrocarbon chains of 8 carbon atoms or more. The existing coating dispersing agent on the market has good dispersing effect, but hydrophilic groups are not firmly combined on the surfaces of particles with lower polarity or nonpolar, and the lipophilic groups do not have enough carbon chain length and cannot generate enough steric hindrance effect in an aqueous dispersing system so as to play a role in stabilizing, so that sediment is easily formed in equipment in production and use, and the equipment use is affected.
Therefore, it is necessary to find a dispersant having good dispersing performance and a long duration of dispersing action.
Disclosure of Invention
In order to solve the persistence defect of the existing dispersing agent, the invention provides a carboxylate polymer, which comprises, by weight, 600-800 parts of unsaturated polyether, 1.1-1.4 parts of functional monomer A, 6.0-10.0 parts of functional monomer B, 6.9-9.0 parts of initiator, 0.6-1.0 parts of reducing agent, 2.1-2.6 parts of chain transfer agent, 40.0-60.0 parts of C solution, 40.0-50.0 parts of neutralizer and 200.0-220.0 parts of water.
Further, the unsaturated polyether is one or more of allyl polyoxyethylene ether, isopentenyl alcohol polyoxyethylene ether, isobutenyl alcohol polyoxyethylene ether and methallyl alcohol polyoxyethylene ether.
Further, the functional monomer A is one or more of allyl diethyl phosphate, phosphoric acid, phosphorous acid, pyrophosphoric acid and disodium hydrogen phosphate.
Further, the functional monomer B is one or more of 4- (allyloxy) benzoic acid, vinyl acetate and methyl methacrylate.
Further, the initiator is one or more of hydrogen peroxide, ammonium persulfate, azodiisobutyronitrile, diisopropyl peroxydicarbonate, benzoyl peroxide, di-tert-butyl peroxide, dicyclohexyl peroxydicarbonate and potassium persulfate.
Further, the reducing agent is one or more of ascorbic acid, BRUGGOLITE 51, sodium formaldehyde sulfoxylate, maltodextrin, sodium metabisulfite, sodium hypophosphite and sodium dithionite;
further, the chain transfer agent is one or more of thioglycollic acid, mercaptopropionic acid, mercaptoethanol, mercaptopropanol and sodium hypophosphite.
Further, the liquid C is one or more of acrylic acid, methacrylic acid, hydroxyethyl acrylate and hydroxypropyl acrylate.
Further, the neutralizer is one or more of sodium hydroxide, potassium hydroxide and cesium hydroxide.
Further, the carboxylate polymer has the structural formula
The structure represents carboxylate polymer when unsaturated polyether is methyl allyl alcohol polyoxyethylene ether, functional monomer A is allyl diethyl phosphate, functional monomer B is 4- (allyloxy) benzoic acid and C solution is acrylic acid.
The invention also provides a preparation method of the carboxylate polymer, which comprises the following steps:
(1) Charging unsaturated polyether and a first portion of water into a reaction vessel, and stirring;
(2) Adding the functional monomer A into the reaction container, and stirring for 10-20 min;
(3) Dropwise adding an initiator, a reducing agent, a chain transfer agent, functional monomers B and C into the reaction container, controlling the dropwise adding time to be 150-210 min, controlling the material temperature to be less than or equal to 40 ℃, and keeping the temperature for 50-70 min after the dropwise adding is finished;
(4) Adding a neutralizing agent and a second part of water into the reaction vessel, and adjusting the pH to 5-7 and the solid content to 50 percent.
It is understood that in the step (3), the initiator, the reducing agent, the chain transfer agent, the functional monomer B and the functional monomer C are all prepared in the form of a solution for dropwise addition, wherein the solvent is water.
The sum of the first part of water amount, the second part of water amount and the water solvent amount of the initiator, the reducing agent, the chain transfer agent, the functional monomers B and C in the step (3) is the total amount of water.
The invention also provides a coating dispersing agent, which comprises 650.0-800.0 parts by weight of carboxylate polymer, 80.0-110.0 parts by weight of polycarboxylic acid slump retaining agent, 14.0-18.0 parts by weight of sodium gluconate, 30.0-40.0 parts by weight of cellulose ether and 160.0-190.0 parts by weight of deionized water, wherein the carboxylate polymer is the carboxylate polymer or is prepared by adopting the preparation method.
Preferably, the polycarboxylic acid slump retaining agent is Point-T4404 from the New Material group Co., ltd.
The invention also provides a preparation method of the paint dispersing agent, which comprises the following steps: weighing the raw materials, and mixing uniformly.
Compared with the prior art, the carboxylate polymer and the coating dispersing agent containing the carboxylate polymer provided by the invention have the following beneficial effects:
the carboxylate polymer provided by the invention has the advantages that the prepared carboxylate has lower molecular weight by introducing lipophilic groups, so that the viscosity of the cement-based filler can be reduced. In addition, one end of the carboxylate active group can be adsorbed on the surface of the pigment and filler, and the other end of the carboxylate active group enters the base material to form an adsorption layer (the adsorption layer is thicker as the adsorption group is more and the chain length is longer), so that pigment and filler particles are in a dispersed and suspended state in a coating system for a long time by virtue of the repulsive force and steric hindrance of the load; can maintain low mixing amount and has better dispersibility and viscosity reduction effect than common coating dispersing agent. The coating dispersing agent containing carboxylate polymer is characterized by that it utilizes chemical and physical mode to control the dispersion action process of carboxylate molecule on cement-base filler in the coating material, and can make the dispersion action of carboxylate molecule on cement-base filler in the coating material be continuously and slowly implemented in a certain time, and can not completely quickly release all the dispersing power of said coating material, i.e. can be uniformly mixed and slowly released, so that the concentration of carboxylate coating dispersing agent in the system can be continuously raised so as to attain the goal of prolonging dispersion retention property.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a carboxylate polymer, which comprises 600-800 parts by weight of unsaturated polyether, 1.1-1.4 parts by weight of functional monomer A, 6.0-10.0 parts by weight of functional monomer B, 6.9-9.0 parts by weight of initiator, 0.6-1.0 parts by weight of reducing agent, 2.1-2.6 parts by weight of chain transfer agent, 40.0-60.0 parts by weight of C solution, 40.0-50.0 parts by weight of neutralizer and 200.0-220.0 parts by weight of water.
Wherein the unsaturated polyether is one or more of allyl polyoxyethylene ether, isopentenyl alcohol polyoxyethylene ether, isobutenyl alcohol polyoxyethylene ether and methallyl alcohol polyoxyethylene ether.
The functional monomer A is one or more of allyl diethyl phosphate, phosphoric acid, phosphorous acid, pyrophosphoric acid and disodium hydrogen phosphate.
The functional monomer B is one or more of 4- (allyloxy) benzoic acid, vinyl acetate and methyl methacrylate.
The initiator is one or more of hydrogen peroxide, ammonium persulfate, azodiisobutyronitrile, diisopropyl peroxydicarbonate, benzoyl peroxide, di-tert-butyl peroxide, dicyclohexyl peroxydicarbonate and potassium persulfate.
The reducing agent is one or more of ascorbic acid, BRUGGOLITE 51, sodium formaldehyde sulfoxylate, maltodextrin, sodium metabisulfite, sodium hypophosphite and sodium dithionite.
The chain transfer agent is one or more of thioglycollic acid, mercaptopropionic acid, mercaptoethanol, mercaptopropanol and sodium hypophosphite.
The neutralizer is one or more of sodium hydroxide, potassium hydroxide and cesium hydroxide.
The liquid C is one or more of acrylic acid, methacrylic acid, hydroxyethyl acrylate and hydroxypropyl acrylate.
The present invention also provides an operational example of the above-described method for preparing a carboxylate polymer, comprising the steps of:
(1) Charging unsaturated polyether and a first portion of water into a reaction vessel, and stirring;
(2) Adding the functional monomer A into the reaction container, and stirring for 10-20 min;
(3) Dropwise adding an initiator, a reducing agent, a chain transfer agent, functional monomers B and C into the reaction container, controlling the dropwise adding time to be 150-210 min, controlling the material temperature to be less than or equal to 40 ℃, and keeping the temperature for 50-70 min after the dropwise adding is finished;
(4) Adding a neutralizing agent and a second part of water into the reaction vessel, and adjusting the pH to 5-7 and the solid content to 50 percent.
The invention also provides a coating dispersing agent, which comprises 650.0-800.0 parts by weight of carboxylate polymer, 80.0-110.0 parts by weight of polycarboxylic acid slump retaining agent, 14.0-18.0 parts by weight of sodium gluconate, 30.0-40.0 parts by weight of cellulose ether and 160.0-190.0 parts by weight of deionized water, wherein the carboxylate polymer is the carboxylate polymer or is prepared by adopting the preparation method.
The invention also provides the formulations (unit: parts by weight) of the examples and comparative examples shown in table 1:
TABLE 1
| Raw materials | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 |
| Unsaturated polyether | 704.7 | 704.7 | 704.7 | 704.7 | 704.7 | 704.7 |
| Functional monomer A | 1.1 | 1.3 | 1.4 | 1.1 | 0 | 1.3 |
| Functional monomer B | 6.0 | 8.0 | 8.0 | 10.0 | 8.0 | 0 |
| Initiator(s) | 6.9 | 7.6 | 8.4 | 8.4 | 7.6 | 7.6 |
| Reducing agent | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
| Chain transfer agent | 2.3 | 2.1 | 2.6 | 2.6 | 2.1 | 2.1 |
| Liquid C | 50.4 | 50.4 | 50.4 | 50.4 | 50.4 | 50.4 |
| Neutralizing agent | 44.4 | 44.4 | 44.4 | 44.4 | 44.4 | 44.4 |
| Water and its preparation method | 213.4 | 210.7 | 209.3 | 207.6 | 212 | 218.7 |
Wherein the unsaturated polyether is methallyl alcohol polyoxyethylene ether with a molecular weight of 2400;
the functional monomer A is allyl diethyl phosphate;
the functional monomer B is 4- (allyloxy) benzoic acid;
the initiator is hydrogen peroxide;
the reducing agent is 0.7 part of BRUGGOLITE 51 and 0.1 part of sodium hypophosphite
The chain transfer agent is mercaptopropionic acid;
the solution C is acrylic acid;
the neutralizer is a 32wt% sodium hydroxide solution.
It should be noted that the specific parameters or some common reagents in the above embodiments are specific embodiments or preferred embodiments under the concept of the present invention, and are not limited thereto; and can be adaptively adjusted by those skilled in the art within the concept and the protection scope of the invention.
In addition, unless otherwise specified, the starting materials employed may also be commercially available products conventionally used in the art or may be prepared by methods conventionally used in the art.
The carboxylate polymers prepared in examples 1-4 have the structural formula:
the invention also provides the preparation methods of the above examples and comparative examples, which specifically comprise the following steps:
(1) Putting unsaturated polyether and 60 parts of water into a reaction kettle, and starting a stirring and temperature controlling device;
(2) Adding the functional monomer A into the reaction kettle, and stirring for 15min;
(3) Dropwise adding a solution A (containing an initiator and 30 parts of water), a solution B (containing a reducing agent, a chain transfer agent and 30 parts of water) and a solution D (containing a solution C, a functional monomer B and 30 parts of water) into a reaction kettle, controlling the dropwise adding time to be 150min, controlling the material temperature to be 40 ℃, and preserving the heat for 60min after the dropwise adding is finished;
(4) Adding a neutralizing agent and the rest water into the reaction kettle, and adjusting the pH value to 6 and the solid content to 50 percent to obtain the catalyst.
Coating dispersants were prepared using the carboxylate polymers prepared in examples 1-4 and comparative examples 1-2, respectively, to prepare coating dispersants KZJ-1, KZJ-2, KZJ-3, KZJ-4, PCE-1, and PCE-2 having a solids content of 40%.
Wherein, the raw materials of the coating dispersing agent comprise: 675.3 parts of a carboxylate polymer, 101.3 parts of a polycarboxylic acid slump retaining agent, 16.9 parts of sodium gluconate, 33.8 parts of a cellulose ether and 172.7 parts of deionized water;
the preparation method comprises the steps of uniformly mixing the raw materials to obtain the coating dispersing agent with the solid content of 40%.
Among them, the polycarboxylic acid slump retaining agent is Point-T4404 of Jie New Material group Co., ltd.
The dispersion properties of the paint dispersants and the commercially available paint dispersants provided in examples and comparative examples were evaluated by using viscosity values of the paint after mixing with the paint dispersant, as follows:
weighing 90 parts of acrylic emulsion, 9.5 parts of water, 0.3 part of defoamer and 0.2 part of paint dispersing agent, dispersing for 1min in a dispersing machine at the speed of 300r/min to prepare a liquid material, adding 230 parts of pigment and filler (pigment and filler is formed by mixing cement, heavy calcium and snow white at the speed of 5:2:3) according to a formula, dispersing for 5min at 800r/min, taking off, testing initial viscosity by using a stormer viscometer to obtain a dispersing capacity, and expressing the dispersing capacity by using a KU value (the smaller the KU value is, the better the dispersing capacity is indicated); then continuing to test viscosity for 60min, 90min and 120min, namely a dispersion retention test, and comparing viscosity rising conditions at 120min and at the initial time, wherein the viscosity rising conditions are expressed by delta KU values; the smaller the Δku value, the better the dispersion retention is indicated within the same period of time. The test results are shown in Table 2.
TABLE 2
From table 2 it can be obtained:
the initial viscosity values of the paint dispersing agent and the paint provided by the examples 1-4 are lower than those of the comparative example and the commercial sample, and the viscosity rising value of the paint after 120min is also lower than those of the comparative example and the commercial sample, so that the carboxylate polymer and the paint dispersing agent containing the carboxylate polymer provided by the invention have better dispersing performance and viscosity reduction effect, and the dispersing action duration time is long.
The comparison of PCE-1 and KZJ-2 shows that when allyl diethyl phosphate is not added into carboxylate polymer, the initial dispersibility of the paint is obviously reduced, the viscosity of the paint is obviously thickened along with the extension of the standing time, and the dispersion retention is shortened to a certain extent, so that the introduction of phosphate groups is beneficial to enhancing the dispersion performance of the dispersing agent.
The comparison result of PCE-2 and KZJ-2 shows that when 4- (allyloxy) benzoic acid is not added into carboxylate polymer, the initial KU value of the paint is obviously increased, which indicates that the dispersibility of the paint dispersing agent is poor, and the viscosity thickening of the paint is obvious along with the extension of the standing time, which indicates that 4- (allyloxy) benzoic acid is added into the paint dispersing agent, the lipophilic group benzene ring is successfully introduced, and the molecular weight of the side chain of carboxylate is effectively reduced, so that the dispersion performance of the dispersing agent is enhanced.
The present invention also provides the following coating dispersants of comparative examples 3 to 5:
comparative example 3
Unlike KZJ-2, which was prepared using the carboxylate polymer of example 2, the polycarboxylic acid slump retaining agent in the raw material was replaced with an equal amount of deionized water to prepare a paint dispersant PCE-3.
Comparative example 4
Unlike KZJ-2, which was prepared using the carboxylate polymer of example 2, sodium gluconate in the feed was replaced with an equal amount of deionized water to prepare the coating dispersant PCE-4.
Comparative example 5
Unlike KZJ-2, which was prepared using the carboxylate polymer of example 2, the cellulose ether in the starting material was replaced with an equal amount of deionized water to prepare the coating dispersant PCE-5.
The prepared coating dispersants KZJ-1, KZJ-2, KZJ-3, KZJ-4, PCE-3, PCE-4, PCE-5 and commercial products were subjected to powder opening capability and dispersibility test. The dispersibility test was as above. The powder opening capability test method comprises the following steps: 180 parts of emulsion, 9.5 parts of water, 0.3 part of defoamer and 0.2 part of paint dispersing agent are weighed and dispersed for 1min in a dispersing machine at the speed of 300r/min to prepare a liquid material, 180 parts of pigment and filler (pigment and filler is formed by mixing cement, heavy calcium carbonate and snow white according to the ratio of 5:2:3) are added, the mixture is dispersed for 3min at the speed of 350r/min, and a paint sample is poured on a glass plate for flattening, and the particle size and the number of dry films are observed. The smaller the number of dry film particles, the better the powder opening ability of the added coating dispersant. The test results are shown in Table 3.
TABLE 3 Table 3
From table 3 it is possible to obtain:
the paint dispersants provided in examples 1 to 4 of the present invention are used to effectively improve the powder-opening ability of the paint, and the initial dispersibility and dispersion retention of the paint after the paint is added are superior to those of the comparative example and the commercial sample.
The comparison result of PCE-3 and KZJ-2 shows that when the carboxylic acid slump retaining agent Point-T4404 is not added, the influence on the powder opening capability of the paint is small, the number of dry film particles is not obviously increased, but the dispersibility and dispersion action persistence are greatly influenced.
The comparison result of PCE-4 and KZJ-2 shows that when the retarder sodium gluconate is not added, the powder opening capability, the dispersibility and the dispersion action persistence of the coating dispersing agent are all influenced.
The comparison result of PCE-5 and KZJ-2 shows that when the water-retaining agent cellulose ether is not added, the powder-opening capability of the paint is obviously deteriorated, pigment and filler are easy to agglomerate, so that the paint is not uniformly dispersed and is not easy to construct.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. A carboxylate polymer characterized by: the raw materials comprise 600 to 800 parts of unsaturated polyether, 1.1 to 1.4 parts of functional monomer A, 6.0 to 10.0 parts of functional monomer B, 6.9 to 9.0 parts of initiator, 0.6 to 1.0 parts of reducing agent, 2.1 to 2.6 parts of chain transfer agent, 40.0 to 60.0 parts of C solution, 40.0 to 50.0 parts of neutralizer and 200.0 to 220.0 parts of water by weight.
2. The carboxylate polymer according to claim 1, characterized in that: the unsaturated polyether is one or more of allyl polyoxyethylene ether, isopentenyl alcohol polyoxyethylene ether, isobutenyl alcohol polyoxyethylene ether and methallyl alcohol polyoxyethylene ether.
3. The carboxylate polymer according to claim 1, characterized in that: the functional monomer A is one or more of allyl diethyl phosphate, phosphoric acid, phosphorous acid, pyrophosphoric acid and disodium hydrogen phosphate.
4. The carboxylate polymer according to claim 1, characterized in that: the functional monomer B is one or more of 4- (allyloxy) benzoic acid, vinyl acetate and methyl methacrylate.
5. The carboxylate polymer according to claim 1, characterized in that: the initiator is one or more of hydrogen peroxide, ammonium persulfate, azodiisobutyronitrile, diisopropyl peroxydicarbonate, benzoyl peroxide, di-tert-butyl peroxide, dicyclohexyl peroxydicarbonate and potassium persulfate.
6. The carboxylate polymer according to claim 1, characterized in that: the reducing agent is one or more of ascorbic acid, BRUGGOLITE 51, sodium formaldehyde sulfoxylate, maltodextrin, sodium metabisulfite, sodium hypophosphite and sodium dithionite;
and/or the chain transfer agent is one or more of thioglycollic acid, mercaptopropionic acid, mercaptoethanol, mercaptopropanol and sodium hypophosphite;
and/or the neutralizer is one or more of sodium hydroxide, potassium hydroxide and cesium hydroxide.
7. The carboxylate polymer according to claim 1, characterized in that: the liquid C is one or more of acrylic acid, methacrylic acid, hydroxyethyl acrylate and hydroxypropyl acrylate.
8. The carboxylate polymer according to claim 1, characterized in that: the carboxylate polymer has the structural formula
9. The process for preparing a carboxylate polymer according to any one of claims 1 to 8, comprising the steps of:
(1) Charging unsaturated polyether and a first portion of water into a reaction vessel, and stirring;
(2) Adding the functional monomer A into the reaction container, and stirring for 10-20 min;
(3) Dropwise adding an initiator, a reducing agent, a chain transfer agent, functional monomers B and C into the reaction container, controlling the dropwise adding time to be 150-210 min, controlling the material temperature to be less than or equal to 40 ℃, and keeping the temperature for 50-70 min after the dropwise adding is finished;
(4) Adding a neutralizing agent and a second part of water into the reaction vessel, and adjusting the pH to 5-7 and the solid content to 50 percent.
10. A coating dispersant, characterized in that: the raw materials comprise 650.0-800.0 parts by weight of carboxylate polymer, 80.0-110.0 parts by weight of polycarboxylic acid slump retaining agent, 14.0-18.0 parts by weight of sodium gluconate, 30.0-40.0 parts by weight of cellulose ether and 160.0-190.0 parts by weight of deionized water, wherein the carboxylate polymer is the carboxylate polymer according to any one of claims 1-8 or prepared by the preparation method of claim 9.
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