CN101274242B - Method for preparing polymer ceramic dispersants - Google Patents
Method for preparing polymer ceramic dispersants Download PDFInfo
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- CN101274242B CN101274242B CN2008100172587A CN200810017258A CN101274242B CN 101274242 B CN101274242 B CN 101274242B CN 2008100172587 A CN2008100172587 A CN 2008100172587A CN 200810017258 A CN200810017258 A CN 200810017258A CN 101274242 B CN101274242 B CN 101274242B
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- 239000002270 dispersing agent Substances 0.000 title claims abstract description 42
- 239000000919 ceramic Substances 0.000 title claims abstract description 35
- 229920000642 polymer Polymers 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title description 4
- 239000000178 monomer Substances 0.000 claims abstract description 89
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000003999 initiator Substances 0.000 claims abstract description 37
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 31
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 31
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 17
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 17
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 164
- 239000000203 mixture Substances 0.000 claims description 53
- 239000007858 starting material Substances 0.000 claims description 26
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 24
- 239000002253 acid Substances 0.000 claims description 21
- 239000012670 alkaline solution Substances 0.000 claims description 14
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229920001577 copolymer Polymers 0.000 claims description 12
- 230000032050 esterification Effects 0.000 claims description 12
- 238000005886 esterification reaction Methods 0.000 claims description 12
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 10
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 10
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 8
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 8
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 8
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 8
- 235000006408 oxalic acid Nutrition 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 7
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 6
- 235000019253 formic acid Nutrition 0.000 claims description 6
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical group CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- 235000019394 potassium persulphate Nutrition 0.000 claims description 4
- ARGZBGBUZXUAHM-UHFFFAOYSA-L potassium sodium hydrogen sulfite sulfooxy sulfate Chemical compound [Na+].[K+].OS([O-])=O.OS(=O)(=O)OOS([O-])(=O)=O ARGZBGBUZXUAHM-UHFFFAOYSA-L 0.000 claims description 4
- JLBJTVDPSNHSKJ-UHFFFAOYSA-N 4-Methylstyrene Chemical compound CC1=CC=C(C=C)C=C1 JLBJTVDPSNHSKJ-UHFFFAOYSA-N 0.000 claims description 3
- GHUXAYLZEGLXDA-UHFFFAOYSA-N 8-azido-5-ethyl-6-phenylphenanthridin-5-ium-3-amine;bromide Chemical compound [Br-].C12=CC(N=[N+]=[N-])=CC=C2C2=CC=C(N)C=C2[N+](CC)=C1C1=CC=CC=C1 GHUXAYLZEGLXDA-UHFFFAOYSA-N 0.000 claims description 3
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- -1 acrylic ester Chemical class 0.000 claims description 3
- LNCPIMCVTKXXOY-UHFFFAOYSA-N hexyl 2-methylprop-2-enoate Chemical compound CCCCCCOC(=O)C(C)=C LNCPIMCVTKXXOY-UHFFFAOYSA-N 0.000 claims description 3
- LNMQRPPRQDGUDR-UHFFFAOYSA-N hexyl prop-2-enoate Chemical compound CCCCCCOC(=O)C=C LNMQRPPRQDGUDR-UHFFFAOYSA-N 0.000 claims description 3
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims description 3
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 claims description 3
- AZRPQPHRMNCMTN-UHFFFAOYSA-L potassium sodium dioxido-oxo-sulfanylidene-lambda6-sulfane sulfooxy hydrogen sulfate Chemical compound S(=S)(=O)([O-])[O-].[Na+].S(=O)(=O)(O)OOS(=O)(=O)O.[K+] AZRPQPHRMNCMTN-UHFFFAOYSA-L 0.000 claims description 3
- 125000003277 amino group Chemical group 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulphite Substances [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims 1
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims 1
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims 1
- 229920002582 Polyethylene Glycol 600 Polymers 0.000 claims 1
- 229920002593 Polyethylene Glycol 800 Polymers 0.000 claims 1
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 claims 1
- 229920002523 polyethylene Glycol 1000 Polymers 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000049 pigment Substances 0.000 abstract description 3
- 239000002002 slurry Substances 0.000 abstract description 3
- 238000007865 diluting Methods 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 238000010526 radical polymerization reaction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 28
- 238000000465 moulding Methods 0.000 description 8
- 229920002521 macromolecule Polymers 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 description 2
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 2
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 235000019795 sodium metasilicate Nutrition 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 0 *C(c1ccccc1)=C Chemical compound *C(c1ccccc1)=C 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- XEEYSDHEOQHCDA-UHFFFAOYSA-N 2-methylprop-2-ene-1-sulfonic acid Chemical compound CC(=C)CS(O)(=O)=O XEEYSDHEOQHCDA-UHFFFAOYSA-N 0.000 description 1
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 description 1
- YWHSNUQRJHAQQR-UHFFFAOYSA-L S(=O)([O-])[O-].[K+].S(=O)(=O)(O)OOS(=O)(=O)O.[K+] Chemical compound S(=O)([O-])[O-].[K+].S(=O)(=O)(O)OOS(=O)(=O)O.[K+] YWHSNUQRJHAQQR-UHFFFAOYSA-L 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 238000012660 binary copolymerization Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- CEYULKASIQJZGP-UHFFFAOYSA-L disodium;2-(carboxymethyl)-2-hydroxybutanedioate Chemical compound [Na+].[Na+].[O-]C(=O)CC(O)(C(=O)O)CC([O-])=O CEYULKASIQJZGP-UHFFFAOYSA-L 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- BEGBSFPALGFMJI-UHFFFAOYSA-N ethene;sodium Chemical group [Na].C=C BEGBSFPALGFMJI-UHFFFAOYSA-N 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- 229930015698 phenylpropene Natural products 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
Landscapes
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
本发明公开了一种高分子陶瓷分散剂的制备方法，首先将聚乙二醇、马来酸酐混合均匀后聚合制得半酯化产物；然后将半酯化产物、乙烯基类单体和水混合均匀后，在引发剂引发下进行自由基聚合即可得到高分子陶瓷分散剂。采用本发明制得的产品对陶瓷浆料具有优良的分散稀释作用和助磨作用；可提高坯体强度和成坯率，从而降低生产成本；同时使陶瓷制品密度，抗折强度等指标大大增强。此外，此产品亦可用于颜料、涂料等的分散。The invention discloses a preparation method of a polymer ceramic dispersant. Firstly, polyethylene glycol and maleic anhydride are uniformly mixed and then polymerized to obtain a half-esterified product; then the half-esterified product, vinyl monomers and water After mixing evenly, the polymer ceramic dispersant can be obtained by free radical polymerization under the trigger of the initiator. The product prepared by adopting the present invention has excellent dispersing and diluting effect and grinding-aiding effect on ceramic slurry; it can increase the green body strength and green body forming rate, thereby reducing production cost; at the same time, the density, flexural strength and other indicators of ceramic products are greatly enhanced . In addition, this product can also be used for the dispersion of pigments, coatings, etc.
Description
Technical field
The present invention relates to a kind of preparation method of macromolecule dispersing agent, relate in particular to a kind of preparation method of polymer ceramic dispersants.
Background technology
The development that becomes more meticulous along with ceramics, new moulding process emerges in an endless stream, annotate film moulding, colloidal vibration moulding, LOW TEMPERATURES moulding, directly solidify and annotate film moulding, infiltration solidification moulding etc. as the moulding of centrifugal notes film, gel, and numerous moulding process all requires to prepare the ceramic size of low-viscosity, high dispersive, high stability, high solid loading.Solution mainly is to use dispersant in processing procedure, improves the rheological characteristic of slip, improves the uniformity of its microstructure and improves its intensity.
At present, ceramic dispersants is divided into inorganic dispersant, organic dispersing agent and macromolecule dispersing agent three classes.Inorganic dispersant mainly is an inorganic electrolyte, as sodium chloride, sodium metasilicate, sodium metasilicate, calgon, sodium carbonate, sodium phosphate trimer (STPP) etc., mainly is applicable to aluminium oxide and zirconia slurry.Organic dispersing agent mainly is organic bath class dispersant and surfactant-dispersed agent, as natrium citricum, sodium humate, sodium ethylene diamine tetracetate (EDTA), odium stearate, sodium alkyl sulfonate, AEO etc.Little dispersal agent molecule is owing to be subjected to the influence of factors such as molecular structure, relative molecular mass, and its dispersion effect is often very limited, and large usage quantity.And macromolecule dispersing agent is because hydrophilic group, hydrophobic group position and adjustable size, and molecular structure can be pectination, can present highly branched chainization again, to the disperse particles surface coverage and to seal effect better than the former.Its dispersion is easier in addition tends towards stability, flows, and macromolecule dispersing agent will become a rising class ceramic dispersants, and it synthesizes and application study causes extensive attention.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of polymer ceramic dispersants, it has good dispersion diluting effect and grinding aid effect to ceramic slurry; Improved blank strength and billet yield, thereby reduced production costs; Make ceramic density simultaneously, indexs such as rupture strength strengthen greatly but also can be used for the dispersion of pigment, coating etc.
For achieving the above object, the technical solution used in the present invention is: polyethylene glycol and maleic anhydride are pressed 1: the mixed in molar ratio of 0.1-1.2 is even, makes solution A; Add acid solution in solution A, the mass ratio of solution A and acid solution is 100: 0.5-10, be warming up to 30-90 ℃ then, and reacted 0.5-4 hour, make esterification products B; With product B, functional monomer and vinyl monomer by 1: the mass ratio of 1-10: 0.1-1.5 mixes, and makes monomer solution C, and wherein, functional monomer is the monomer of 1. being represented by general formula; Described vinyl monomer is acrylic ester monomer of 2. being represented by general formula or the styrene monomer of 3. being represented by general formula:
1. R in the formula
1Be hydrogen atom or alkyl, M
1Be hydrogen atom or carboxyl; M
2For hydrogen atom or carboxylic side chain or contain sulfonic side chain or the organic amine group;
2. the R in the formula
2Be hydrogen atom or methyl, M
3Be alkyl;
3. the R in the formula
3Be hydrogen atom or methyl; With solution C, molecular weight regulator and water by 1: the mass ratio of 0-0.5: 1-10 mixes, and makes monomer mixture solution D; With water and water soluble starter by 1: the mass ratio of 0.002-1 mixes, and obtains initiator solution E; At 40-90 ℃, in monomer mixture solution D, add and drip initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 0.05-20, the dropping time is 0.1-4 hour, after dropwising, adjust the temperature to 50-95 ℃, reacted 1-6 hour, make aqueous copolymers solution F; With alkaline solution the pH value of solution F is adjusted to 7-13, sub-ceramic dispersants promptly secures satisfactory grades.
It is PEG200, PEG400, PEG600, PEG800, the PEG1000 of 200-8000 that polyethylene glycol of the present invention adopts molecular weight; Acid solution is a kind of in sulfuric acid, formic acid, acetate, the oxalic acid; Functional monomer is acrylic or methacrylic acid; Described vinyl monomer is a kind of in methyl acrylate, methyl methacrylate, ethyl acrylate, EMA, butyl acrylate, butyl methacrylate, Hexyl 2-propenoate, hexyl methacrylate, octadecyl acrylate, octadecyl methacrylate, styrene, the methyl styrene; Molecular weight regulator is lauryl mercaptan, ethyl mercaptan, triethanolamine or isopropyl alcohol; Water soluble starter is ammonium persulfate, potassium peroxydisulfate, ammonium persulfate-sodium sulfite or ammonium persulfate-sodium bisulfite, potassium peroxydisulfate-sodium sulfite or potassium peroxydisulfate-sodium hydrogensulfite, ammonium persulfate-sodium thiosulfate or potassium peroxydisulfate-sodium thiosulfate; Alkaline solution is a kind of in ammoniacal liquor, NaOH, potassium hydroxide, sodium carbonate, sodium acid carbonate, trimethylamine, triethylamine or the triethanolamine.
The present invention adopts anchoring group to replace the lipophilic group of traditional dispersant, and be polymer chain, and select the group of opposed polarity according to the surface nature of oversubscription loose powder body, with the firm absorption of assurance dispersant on solid particles surface, and this absorption is generally Irreversible Adsorption, is difficult to desorption, replace hydrophilic radical with solvent chain, main chain and side chain adjustable length have been introduced new polymerization single polymerization monomer, and the product that makes has good dispersion effect and humidification; Use the monomer of maleic anhydride one polyethylene glycol half ester product as polymerisation, both can in product, introduce an amount of relative molecular mass as requested as side chain, can regulate the side chain relative molecular mass according to application conditions again, guarantee that dispersant forms the protective layer of adequate thickness in solid particles surface, this has just widened the application of product greatly, has improved the application performance of product; Change tradition and produce the means of the binary copolymerization of macromolecule dispersing agent, add a small amount of hydrophobic monomer, as polymer hydrophile-lipophile balance group, to strengthen the dispersive property of end product as the 3rd monomer.
Embodiment 1: polyethylene glycol (PEG200) and maleic anhydride is even by 1: 0.8 mixed in molar ratio, make solution A; Add bright sulfur acid in solution A, solution A is 100: 3 with the mass ratio of acid, is warming up to 30 ℃ then, reacts 4 hours, makes esterification products B; Product B, functional monomer acrylic acid and the vinyl monomer methyl acrylate mass ratio by 1: 1: 1.5 is mixed, make monomer solution C; Solution C and the water mass ratio by 1: 8 is mixed, make monomer mixture solution D; Water and the water soluble starter ammonium persulfate mass ratio by 1: 0.002 is mixed, obtain initiator solution E; At 80 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 10, the dropping time is 2 hours, after dropwising, adjusts the temperature to 50 ℃, reacted 6 hours, and made aqueous copolymers solution F; With alkaline solution ammoniacal liquor the pH value of solution F is adjusted to 8, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 2: polyethylene glycol (PEG400) and maleic anhydride is even by 1: 0.5 mixed in molar ratio, make solution A; Add pure formic acid in solution A, solution A is 100: 5 with the mass ratio of acid, is warming up to 40 ℃ then, reacts 3.5 hours, makes esterification products B; Product B, functional monomer methacrylic acid and the vinyl monomer methyl methacrylate mass ratio by 1: 3: 1.2 is mixed, make monomer solution C; Solution C, molecular weight regulator ethyl mercaptan and the water mass ratio by 1: 0.04: 5 is mixed, make monomer mixture solution D; Water and the water soluble starter potassium peroxydisulfate mass ratio by 1: 0.005 is mixed, obtain initiator solution E; At 50 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 5, the dropping time is 1 hour, after dropwising, adjusts the temperature to 55 ℃, reacted 5.5 hours, and made aqueous copolymers solution F; With alkaline solution NaOH the pH value of solution F is adjusted to 12, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 3: polyethylene glycol (PEG600) and maleic anhydride are evenly made solution A by 1: 1.0 mixed in molar ratio; Add pure acetate in solution A, solution A is 100: 8 with the mass ratio of acid, is warming up to 50 ℃ then, reacts 3 hours, makes esterification products B; Product B, functional monomer itaconic acid and the vinyl monomer ethyl acrylate mass ratio by 1: 8: 0.8 is mixed, make monomer solution C; Solution C, molecular weight regulator triethanolamine and the water mass ratio by 1: 0.01: 3 is mixed, make monomer mixture solution D; Water and water soluble starter ammonium persulfate-sulfurous acid (hydrogen) sodium mass ratio by 1: 0.009 is mixed, obtain initiator solution E; At 70 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 0.5, the dropping time is 4 hours, after dropwising, adjusts the temperature to 60 ℃, reacted 5 hours, and made aqueous copolymers solution F; With alkaline solution potassium hydroxide the pH value of solution F is adjusted to 7, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 4: polyethylene glycol (PEG800) and maleic anhydride is even by 1: 0.9 mixed in molar ratio, make solution A; Add pure oxalic acid in solution A, solution A is 100: 1 with the mass ratio of acid, is warming up to 60 ℃ then, reacts 2.5 hours, makes esterification products B; Product B, functional monomer hydroxy-ethyl acrylate and the vinyl monomer EMA mass ratio by 1: 5: 0.3 is mixed, make monomer solution C; Solution C, molecular weight regulator isopropyl alcohol and the water mass ratio by 1: 0.2: 1 is mixed, make monomer mixture solution D; Water and water soluble starter potassium peroxydisulfate-sulfurous acid (hydrogen) sodium mass ratio by 1: 0.5 is mixed, obtain initiator solution E; At 40 ℃, in monomer mixture solution D, add and drip initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 0.05, the dropping time is 4 hours, after dropwising, adjust the temperature to 65 ℃, reacted 4.5 hours, make aqueous copolymers solution F; With alkaline solution sodium carbonate the pH value of solution F is adjusted to 13, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 5: polyethylene glycol (PEG1000) and maleic anhydride is even by 1: 0.6 mixed in molar ratio, make solution A; The mixture that in solution A, adds bright sulfur acid and oxalic acid, solution A is 100: 0.8 with the mass ratio of acid, is warming up to 70 ℃ then, reacts 2 hours, makes esterification products B; Product B, functional monomer hydroxyethyl methacrylate and the vinyl monomer butyl acrylate mass ratio by 1: 4: 0.1 is mixed, make monomer solution C; Solution C, molecular weight regulator lauryl mercaptan and the water mass ratio by 1: 0.3: 10 is mixed, make monomer mixture solution D; Water and the water soluble starter ammonium persulfate-sodium thiosulfate mass ratio by 1: 0.8 is mixed, obtain initiator solution E; At 60 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 20, the dropping time is 0.1 hour, after dropwising, adjusts the temperature to 70 ℃, reacted 4 hours, and made aqueous copolymers solution F; With the alkaline solution sodium acid carbonate pH value of solution F is adjusted to 10, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 6: polyethylene glycol (PEG200) and maleic anhydride is even by 1: 1.1 mixed in molar ratio, make solution A; The mixture that in solution A, adds pure formic acid and acetate, solution A is 100: 10 with the mass ratio of acid, is warming up to 80 ℃ then, reacts 1.5 hours, makes esterification products B; With the mixture of the mixture of product B, functional monomer hydroxypropyl acrylate and hydroxy propyl methacrylate and vinyl monomer butyl methacrylate and Hexyl 2-propenoate by 1: 4: 4: 0.2: 0.8 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator ethyl mercaptan and the water mass ratio by 1: 0.5: 2 is mixed, make monomer mixture solution D; Water and the water soluble starter potassium peroxydisulfate-sodium thiosulfate mass ratio by 1: 0.2 is mixed, obtain initiator solution E; At 90 ℃, in monomer mixture solution D, add and drip initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 1, the dropping time is 3.5 hours, after dropwising, adjust the temperature to 75 ℃, reacted 3.5 hours, make aqueous copolymers solution F; With the alkaline solution trimethylamine pH value of solution F is adjusted to 9, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 7: polyethylene glycol (PEG400) and maleic anhydride is even by 1: 0.1 mixed in molar ratio, make solution A; The mixture that in solution A, adds bright sulfur acid, acetate and oxalic acid, solution A is 100: 7 with the mass ratio of acid, is warming up to 90 ℃ then, reacts 0.5 hour, makes esterification products B; With the mixture of product B, functional monomer methallyl sulfonic acid and allyl sulphonic acid and vinyl monomer hexyl methacrylate and octadecyl acrylate by 1: 2: 7: 0.3: 0.2 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator triethanolamine and the water mass ratio by 1: 0.1: 9 is mixed, make monomer mixture solution D; Water and the water soluble starter potassium peroxydisulfate mass ratio by 1: 1 is mixed, obtain initiator solution E; At 45 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 15, the dropping time is 0.5 hour, after dropwising, adjusts the temperature to 80 ℃, reacted 3 hours, and made aqueous copolymers solution F; With the alkaline solution triethylamine pH value of solution F is adjusted to 11, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 8: polyethylene glycol (PEG600) and maleic anhydride is even by 1: 1.2 mixed in molar ratio, make solution A; The mixture that in solution A, adds bright sulfur acid, formic acid and oxalic acid, solution A is 100: 2 with the mass ratio of acid, is warming up to 45 ℃ then, reacts 3.8 hours, makes esterification products B; With the mixture of the mixture of product B, functional monomer allyl benzene sulfonic acid and methacrylic acid and vinyl monomer octadecyl methacrylate, styrene and methyl styrene by 1: 3: 7: 0.2: 0.4: 0.7 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator isopropyl alcohol and the water mass ratio by 1: 0.4: 7 is mixed, make monomer mixture solution D; Water and water soluble starter ammonium persulfate-sulfurous acid (hydrogen) sodium mass ratio by 1: 0.1 is mixed, obtain initiator solution E; At 65 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 8, the dropping time is 2 hours, after dropwising, adjusts the temperature to 85 ℃, reacted 2.5 hours, and made aqueous copolymers solution F; With the alkaline solution triethanolamine pH value of solution F is adjusted to 12, sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 9: polyethylene glycol (PEG800) and maleic anhydride is even by 1: 0.3 mixed in molar ratio, make solution A; The mixture that in solution A, adds pure formic acid, acetate and oxalic acid, solution A is 100: 0.5 with the mass ratio of acid, is warming up to 65 ℃ then, reacts 2.7 hours, makes esterification products B; With the mixture of the mixture of product B, functional monomer itaconic acid and hydroxy-ethyl acrylate and vinyl monomer methyl methacrylate and ethyl acrylate by 1: 5: 2: 0.8: 0.4 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator lauryl mercaptan and the water mass ratio by 1: 0.05: 4 is mixed, make monomer mixture solution D; Water and the water soluble starter ammonium persulfate-sodium thiosulfate mass ratio by 1: 0.7 is mixed, obtain initiator solution E; At 85 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 13, the dropping time is 1.5 hours, after dropwising, adjusts the temperature to 90 ℃, reacted 2 hours, and made aqueous copolymers solution F; Mixture with alkaline solution ammoniacal liquor and NaOH) the pH value with solution F is adjusted to 10.5, and sub-ceramic dispersants promptly secures satisfactory grades.
Embodiment 10: polyethylene glycol (PEG1000) and maleic anhydride is even by 1: 0.7 mixed in molar ratio, make solution A; The mixture that in solution A, adds bright sulfur acid, acetate and oxalic acid, solution A is 100: 7 with the mass ratio of acid, is warming up to 85 ℃ then, reacts 1 hour, makes esterification products B; With the mixture of the mixture of product B, functional monomer hydroxy-ethyl acrylate, hydroxyethyl methacrylate and hydroxypropyl acrylate and vinyl monomer butyl acrylate and butyl methacrylate by 1: 2: 3: 4: 0.2: 0.6 mass ratio mixes, and makes monomer solution C; Solution C, molecular weight regulator triethanolamine and the water mass ratio by 1: 0.09: 6 is mixed, make monomer mixture solution D; Water and the water soluble starter ammonium persulfate mass ratio by 1: 0.4 is mixed, obtain initiator solution E; At 55 ℃, in monomer mixture solution D, add dropping initiator solution E, wherein the mass ratio of monomer mixture solution D and initiator solution E water soluble starter is 100: 3, the dropping time is 3 hours, after dropwising, adjusts the temperature to 95 ℃, reacted 1 hour, and made aqueous copolymers solution F; With the mixture of alkaline solution potassium hydroxide and sodium carbonate, the pH value of solution F is adjusted to 8.5, sub-ceramic dispersants promptly secures satisfactory grades.
The present invention can form double electrical layers at particle surface, and simultaneously electrostatic stabilization own, the stable triple mechanism of macromolecule steric stabilization and room can make colloid-stabilised or make particle insoluble in solvent continue to keep the state of high degree of dispersion.It both can add in slip, again can be in glaze slip adapted, have good dispersiveness and grinding aid effect, make slip under the situation of low moisture content, have suitable viscosity, good flowability, be convenient to operation, can reach energy-saving and cost-reducing purpose.Improved blank strength and billet yield, thereby reduced production costs; Make ceramic density simultaneously, indexs such as rupture strength strengthen greatly.This invention product also can be used for fields such as papermaking, mud conditioning, pigment dispersion and coating dispersion.
Claims (8)
1. the preparation method of a polymer ceramic dispersants is characterized in that:
1) polyethylene glycol and maleic anhydride are pressed 1: the mixed in molar ratio of 0.1-1.2 is even, makes solution A;
2) add acid solution in solution A, the mass ratio of solution A and acid solution is 100: 0.5-10, be warming up to 30-90 ℃ then, and reacted 0.5-4 hour, make esterification products B;
3) with product B, functional monomer and vinyl monomer by 1: the mass ratio of 1-10: 0.1-1.5 mixes, and makes monomer solution C, and wherein, functional monomer is the monomer of 1. being represented by general formula; Described vinyl monomer is acrylic ester monomer of 2. being represented by general formula or the styrene monomer of 3. being represented by general formula:
1. R in the formula
1Be hydrogen atom or alkyl, M
1Be hydrogen atom or carboxyl; M
2For hydrogen atom or carboxylic side chain or contain sulfonic side chain or the organic amine group;
2. the R in the formula
2Be hydrogen atom or methyl, M
3Be alkyl;
3. the R in the formula
3Be hydrogen atom or methyl;
4) with solution C, molecular weight regulator and water by 1: the mass ratio of 0-0.5: 1-10 mixes, and makes monomer mixture solution D;
5) with water and water soluble starter by 1: the mass ratio of 0.002-1 mixes, and obtains initiator solution E;
6) at 40-90 ℃, in monomer mixture solution D, drip initiator solution E, wherein the mass ratio of the water soluble starter among monomer mixture solution D and the initiator solution E is 100: 0.05-20, the dropping time is 0.1-4 hour, after dropwising, adjust the temperature to 50-95 ℃, reacted 1-6 hour, make aqueous copolymers solution F;
7) with alkaline solution the pH value of solution F is adjusted to 7-13, sub-ceramic dispersants promptly secures satisfactory grades.
2. the preparation method of polymer ceramic dispersants according to claim 1 is characterized in that: it is PEG200, PEG400, PEG600, PEG800, the PEG1000 of 200-8000 that described polyethylene glycol adopts molecular weight.
3. the preparation method of polymer ceramic dispersants according to claim 1 is characterized in that: described acid solution is a kind of in sulfuric acid, formic acid, acetate, the oxalic acid.
4. the preparation method of polymer ceramic dispersants according to claim 1, it is characterized in that: said functional monomer is acrylic or methacrylic acid.
5. the preparation method of polymer ceramic dispersants according to claim 1 is characterized in that: said vinyl monomer is a kind of in methyl acrylate, methyl methacrylate, ethyl acrylate, EMA, butyl acrylate, butyl methacrylate, Hexyl 2-propenoate, hexyl methacrylate, octadecyl acrylate, octadecyl methacrylate, styrene, the methyl styrene.
6. the preparation method of polymer ceramic dispersants according to claim 1, it is characterized in that: said molecular weight regulator is lauryl mercaptan, ethyl mercaptan, triethanolamine or isopropyl alcohol.
7. the preparation method of polymer ceramic dispersants according to claim 1, it is characterized in that: said water soluble starter is ammonium persulfate, potassium peroxydisulfate, ammonium persulfate-sodium sulfite or ammonium persulfate-sodium bisulfite, potassium peroxydisulfate-sodium sulfite or potassium peroxydisulfate-sodium hydrogensulfite, ammonium persulfate-sodium thiosulfate or potassium peroxydisulfate-sodium thiosulfate.
8. the preparation method of polymer ceramic dispersants according to claim 1 is characterized in that: said alkaline solution is a kind of in ammoniacal liquor, NaOH, potassium hydroxide, sodium carbonate, sodium acid carbonate, trimethylamine, triethylamine or the triethanolamine.
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