JP2021088643A - Inorganic particle-dispersion slurry and dispersant for inorganic particle-dispersion slurry - Google Patents
Inorganic particle-dispersion slurry and dispersant for inorganic particle-dispersion slurry Download PDFInfo
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- JP2021088643A JP2021088643A JP2019218966A JP2019218966A JP2021088643A JP 2021088643 A JP2021088643 A JP 2021088643A JP 2019218966 A JP2019218966 A JP 2019218966A JP 2019218966 A JP2019218966 A JP 2019218966A JP 2021088643 A JP2021088643 A JP 2021088643A
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- parts
- acid
- dispersant
- inorganic particle
- water
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- 239000002002 slurry Substances 0.000 title claims abstract description 95
- 239000002270 dispersing agent Substances 0.000 title claims abstract description 92
- 239000006185 dispersion Substances 0.000 title claims abstract description 71
- 239000010954 inorganic particle Substances 0.000 claims abstract description 130
- 229920000642 polymer Polymers 0.000 claims abstract description 86
- 239000000178 monomer Substances 0.000 claims abstract description 37
- 239000002253 acid Substances 0.000 claims abstract description 36
- 150000003839 salts Chemical class 0.000 claims abstract description 32
- VVJKKWFAADXIJK-UHFFFAOYSA-N Allylamine Chemical compound NCC=C VVJKKWFAADXIJK-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-DYCDLGHISA-N deuterium hydrogen oxide Chemical compound [2H]O XLYOFNOQVPJJNP-DYCDLGHISA-N 0.000 claims abstract description 16
- 239000000470 constituent Substances 0.000 claims abstract description 14
- DYUWTXWIYMHBQS-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCNCC=C DYUWTXWIYMHBQS-UHFFFAOYSA-N 0.000 claims abstract description 14
- OSSNTDFYBPYIEC-UHFFFAOYSA-N 1-ethenylimidazole Chemical compound C=CN1C=CN=C1 OSSNTDFYBPYIEC-UHFFFAOYSA-N 0.000 claims abstract description 12
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 64
- 239000007864 aqueous solution Substances 0.000 description 60
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 57
- 239000002245 particle Substances 0.000 description 32
- -1 satin white Chemical compound 0.000 description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- 238000003756 stirring Methods 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 16
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 14
- 239000012299 nitrogen atmosphere Substances 0.000 description 13
- 239000007787 solid Substances 0.000 description 13
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 12
- 229910017604 nitric acid Inorganic materials 0.000 description 12
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 10
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 10
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 229910001873 dinitrogen Inorganic materials 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 239000002244 precipitate Substances 0.000 description 9
- 150000007524 organic acids Chemical class 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 7
- 239000002518 antifoaming agent Substances 0.000 description 7
- 125000004432 carbon atom Chemical group C* 0.000 description 7
- 239000011976 maleic acid Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 6
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000003125 aqueous solvent Substances 0.000 description 6
- 150000001735 carboxylic acids Chemical class 0.000 description 6
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 5
- 235000015165 citric acid Nutrition 0.000 description 5
- 235000019253 formic acid Nutrition 0.000 description 5
- 239000001530 fumaric acid Substances 0.000 description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 5
- 150000007522 mineralic acids Chemical class 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 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 description 4
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 125000000129 anionic group Chemical group 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 229920001577 copolymer Polymers 0.000 description 4
- 239000003480 eluent Substances 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 4
- 238000005227 gel permeation chromatography Methods 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 235000005985 organic acids Nutrition 0.000 description 4
- 230000003449 preventive effect Effects 0.000 description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- XLXCHZCQTCBUOX-UHFFFAOYSA-N 1-prop-2-enylimidazole Chemical compound C=CCN1C=CN=C1 XLXCHZCQTCBUOX-UHFFFAOYSA-N 0.000 description 3
- IRQWEODKXLDORP-UHFFFAOYSA-N 4-ethenylbenzoic acid Chemical compound OC(=O)C1=CC=C(C=C)C=C1 IRQWEODKXLDORP-UHFFFAOYSA-N 0.000 description 3
- 101150096839 Fcmr gene Proteins 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- VRQIXCOIBHRSSE-UHFFFAOYSA-N acetic acid;prop-2-en-1-amine Chemical compound CC([O-])=O.[NH3+]CC=C VRQIXCOIBHRSSE-UHFFFAOYSA-N 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 150000007529 inorganic bases Chemical class 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 150000002736 metal compounds Chemical class 0.000 description 3
- 150000007530 organic bases Chemical class 0.000 description 3
- 150000002894 organic compounds Chemical class 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 2
- DURRSEGFTCZKMK-UHFFFAOYSA-N 1-prop-2-enylpyrrolidin-2-one Chemical compound C=CCN1CCCC1=O DURRSEGFTCZKMK-UHFFFAOYSA-N 0.000 description 2
- MZNSQRLUUXWLSB-UHFFFAOYSA-N 2-ethenyl-1h-pyrrole Chemical compound C=CC1=CC=CN1 MZNSQRLUUXWLSB-UHFFFAOYSA-N 0.000 description 2
- DCSJOYUSHGVMFL-UHFFFAOYSA-N 2-prop-2-enyl-1h-pyrrole Chemical compound C=CCC1=CC=CN1 DCSJOYUSHGVMFL-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
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- 239000002585 base Substances 0.000 description 2
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- ZDZVKPXKLLLOOA-UHFFFAOYSA-N Allylmalonic acid Chemical compound OC(=O)C(C(O)=O)CC=C ZDZVKPXKLLLOOA-UHFFFAOYSA-N 0.000 description 1
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- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 1
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- 229910002651 NO3 Inorganic materials 0.000 description 1
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- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004111 Potassium silicate Substances 0.000 description 1
- 102100038239 Protein Churchill Human genes 0.000 description 1
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- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
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- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
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- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910001593 boehmite Inorganic materials 0.000 description 1
- ABBZJHFBQXYTLU-UHFFFAOYSA-N but-3-enamide Chemical compound NC(=O)CC=C ABBZJHFBQXYTLU-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
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- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 125000006297 carbonyl amino group Chemical group [H]N([*:2])C([*:1])=O 0.000 description 1
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- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 1
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- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000012718 coordination polymerization Methods 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
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- 238000002050 diffraction method Methods 0.000 description 1
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- 229940043276 diisopropanolamine Drugs 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- LDCRTTXIJACKKU-ONEGZZNKSA-N dimethyl fumarate Chemical compound COC(=O)\C=C\C(=O)OC LDCRTTXIJACKKU-ONEGZZNKSA-N 0.000 description 1
- LDCRTTXIJACKKU-ARJAWSKDSA-N dimethyl maleate Chemical compound COC(=O)\C=C/C(=O)OC LDCRTTXIJACKKU-ARJAWSKDSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- VKFAUCPBMAGVRG-UHFFFAOYSA-N dipivefrin hydrochloride Chemical compound [Cl-].C[NH2+]CC(O)C1=CC=C(OC(=O)C(C)(C)C)C(OC(=O)C(C)(C)C)=C1 VKFAUCPBMAGVRG-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
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- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 238000012690 ionic polymerization Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000007561 laser diffraction method Methods 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910001960 metal nitrate Inorganic materials 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000005397 methacrylic acid ester group Chemical group 0.000 description 1
- JFZUABNDWZQLIJ-UHFFFAOYSA-N methyl 2-[(2-chloroacetyl)amino]benzoate Chemical compound COC(=O)C1=CC=CC=C1NC(=O)CCl JFZUABNDWZQLIJ-UHFFFAOYSA-N 0.000 description 1
- NUMHUJZXKZKUBN-UHFFFAOYSA-N methyl 4-ethenylbenzoate Chemical compound COC(=O)C1=CC=C(C=C)C=C1 NUMHUJZXKZKUBN-UHFFFAOYSA-N 0.000 description 1
- NKHAVTQWNUWKEO-IHWYPQMZSA-N methyl hydrogen fumarate Chemical compound COC(=O)\C=C/C(O)=O NKHAVTQWNUWKEO-IHWYPQMZSA-N 0.000 description 1
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 150000002762 monocarboxylic acid derivatives Chemical class 0.000 description 1
- NKHAVTQWNUWKEO-NSCUHMNNSA-N monomethyl fumarate Chemical compound COC(=O)\C=C\C(O)=O NKHAVTQWNUWKEO-NSCUHMNNSA-N 0.000 description 1
- QRWZCJXEAOZAAW-UHFFFAOYSA-N n,n,2-trimethylprop-2-enamide Chemical compound CN(C)C(=O)C(C)=C QRWZCJXEAOZAAW-UHFFFAOYSA-N 0.000 description 1
- JWAJUTZQGZBKFS-UHFFFAOYSA-N n,n-diethylprop-2-en-1-amine Chemical compound CCN(CC)CC=C JWAJUTZQGZBKFS-UHFFFAOYSA-N 0.000 description 1
- OVHHHVAVHBHXAK-UHFFFAOYSA-N n,n-diethylprop-2-enamide Chemical compound CCN(CC)C(=O)C=C OVHHHVAVHBHXAK-UHFFFAOYSA-N 0.000 description 1
- LQFLWKPCQITJIH-UHFFFAOYSA-N n-allyl-aniline Chemical compound C=CCNC1=CC=CC=C1 LQFLWKPCQITJIH-UHFFFAOYSA-N 0.000 description 1
- RHUCQDQRNUUMKY-UHFFFAOYSA-N n-benzylprop-2-en-1-amine Chemical compound C=CCNCC1=CC=CC=C1 RHUCQDQRNUUMKY-UHFFFAOYSA-N 0.000 description 1
- BGDTWOQNFJNCKH-UHFFFAOYSA-N n-ethyl-n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCN(CC)CC=C BGDTWOQNFJNCKH-UHFFFAOYSA-N 0.000 description 1
- PUUULGNNRPBVBA-UHFFFAOYSA-N n-ethylprop-2-en-1-amine Chemical compound CCNCC=C PUUULGNNRPBVBA-UHFFFAOYSA-N 0.000 description 1
- SWPMNMYLORDLJE-UHFFFAOYSA-N n-ethylprop-2-enamide Chemical compound CCNC(=O)C=C SWPMNMYLORDLJE-UHFFFAOYSA-N 0.000 description 1
- WGESLFUSXZBFQF-UHFFFAOYSA-N n-methyl-n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCN(C)CC=C WGESLFUSXZBFQF-UHFFFAOYSA-N 0.000 description 1
- IOXXVNYDGIXMIP-UHFFFAOYSA-N n-methylprop-2-en-1-amine Chemical compound CNCC=C IOXXVNYDGIXMIP-UHFFFAOYSA-N 0.000 description 1
- KTTAXOZHFOSJFB-UHFFFAOYSA-N n-octyl-n-prop-2-enyloctan-1-amine Chemical compound CCCCCCCCN(CC=C)CCCCCCCC KTTAXOZHFOSJFB-UHFFFAOYSA-N 0.000 description 1
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000006353 oxyethylene group Chemical group 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- HVAMZGADVCBITI-UHFFFAOYSA-M pent-4-enoate Chemical compound [O-]C(=O)CCC=C HVAMZGADVCBITI-UHFFFAOYSA-M 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 229910052913 potassium silicate Inorganic materials 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Landscapes
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
本発明は、無機粒子分散スラリー及び無機粒子分散スラリー用分散剤に関する。 The present invention relates to an inorganic particle dispersion slurry and a dispersant for an inorganic particle dispersion slurry.
「（Ｉ）（ａ）アクリル酸４０?６０モル％と（ｂ）（無水）マレイン酸６０〜４０モル％とを含む共重合体の水溶性塩と、（ＩＩ）（ａ）アクリル酸８０〜９５モル％と（ｂ）（無水）マレイン酸２０?５モル％とを含む共重合体の水溶性塩を含有し、共重合体（Ｉ）１００重量部に対して、共重合体（ＩＩ）３０?３００重量部を含むことを特徴とする塗被紙用分散剤」、無機粒子（重質・軽質炭酸カルシウム、カオリン、クレー、水酸化アルミニウム、サチンホワイト、酸化チタン、タルク又はこれらの混合物）及び水からなる無機粒子分散スラリーが知られている（特許文献１）。 "A water-soluble salt of a copolymer containing 40 to 60 mol% of (I) (a) acrylic acid and 60 to 40 mol% of (b) (maleic anhydride) maleic acid, and (II) (a) acrylic acid 80 to 80 to The copolymer (II) contains a water-soluble salt of a copolymer containing 95 mol% and (b) 20 to 5 mol% of (maleic anhydride) maleic anhydride, and is based on 100 parts by weight of the copolymer (I). Dispersant for coated paper, characterized by containing 30-300 parts by weight ", inorganic particles (heavy / light calcium carbonate, kaolin, clay, aluminum hydroxide, satin white, titanium oxide, talc or a mixture thereof) And an inorganic particle dispersion slurry composed of water is known (Patent Document 1).
上記の無機粒子分散スラリーは、ｐＨ（２５℃）を１〜６に調整した場合、十分な流動性が得られないという問題がある。本発明の目的は、ｐＨ（２５℃）が１〜６（好ましくは１〜５、さらに好ましくは１．６〜４．５）であっても優れた流動性を有する無機粒子分散スラリー及びこのスラリー用の分散剤を提供することである。 The above-mentioned inorganic particle-dispersed slurry has a problem that sufficient fluidity cannot be obtained when the pH (25 ° C.) is adjusted to 1 to 6. An object of the present invention is an inorganic particle-dispersed slurry having excellent fluidity even when the pH (25 ° C.) is 1 to 6 (preferably 1 to 5, more preferably 1.6 to 4.5) and this slurry. Is to provide a dispersant for.
本発明の無機粒子分散スラリーの特徴は、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）及び水（Ｄ）を含有してなり、
ｐＨ（２５℃）が１〜６であり、
分散剤（Ｃ）がアリルアミン（塩）、ジアリルアミン（塩）、Ｎ−ビニルイミダゾール（塩）及びＮ−ビニルピロリドンからなる群より選ばれる少なくとも１種を必須構成単量体としてなるポリマーを含有してなる点を要旨とする。
The characteristic of the inorganic particle dispersion slurry of the present invention is that it contains inorganic particles (A), acid (B), dispersant (C) and water (D).
The pH (25 ° C) is 1-6,
The dispersant (C) contains a polymer in which at least one selected from the group consisting of allylamine (salt), diallylamine (salt), N-vinylimidazole (salt) and N-vinylpyrrolidone is an essential constituent monomer. The point is to be the gist.
本発明の分散剤の特徴は、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）及び水（Ｄ）を含有し、ｐＨ（２５℃）が１〜６である無機粒子分散スラリー用の分散剤であって、
アリルアミン（塩）、ジアリルアミン（塩）、Ｎ−ビニルイミダゾール（塩）及びＮ−ビニルピロリドンからなる群より選ばれる少なくとも１種を必須構成単量体としてなるポリマーを含有してなる点を要旨とする。
The characteristics of the dispersant of the present invention are for inorganic particle dispersion slurry containing inorganic particles (A), acid (B), dispersant (C) and water (D) and having a pH (25 ° C.) of 1 to 6. Dispersant
The gist is that it contains a polymer in which at least one selected from the group consisting of allylamine (salt), diallylamine (salt), N-vinylimidazole (salt) and N-vinylpyrrolidone is an essential constituent monomer. ..
本発明の無機粒子分散スラリーは、ｐＨ（２５℃）が１〜６（好ましくは１〜５、さらに好ましくは１．６〜４．５）であっても優れた流動性を有する。 The inorganic particle-dispersed slurry of the present invention has excellent fluidity even when the pH (25 ° C.) is 1 to 6 (preferably 1 to 5, more preferably 1.6 to 4.5).
本発明の分散剤は、ｐＨ（２５℃）が１〜６（好ましくは１〜５、さらに好ましくは１．６〜４．５）である無機粒子分散スラリーに適用した場合でも優れた流動性を発揮する。 The dispersant of the present invention has excellent fluidity even when applied to an inorganic particle dispersion slurry having a pH (25 ° C.) of 1 to 6 (preferably 1 to 5, more preferably 1.6 to 4.5). Demonstrate.
無機粒子（Ａ）としては、ｐＨ１〜６の水に対して安定に分散できるものであれば特に制限はなく、金属酸化物及びカーボンが含まれる。 The inorganic particles (A) are not particularly limited as long as they can be stably dispersed in water having a pH of 1 to 6, and include metal oxides and carbon.
金属酸化物としては、酸化アルミニウム、酸化ケイ素及び酸化チタン等が挙げられる。 Examples of the metal oxide include aluminum oxide, silicon oxide and titanium oxide.
カーボンとしては、グラファイト及びカーボンブラック等が挙げられる。 Examples of carbon include graphite and carbon black.
無機粒子（Ａ）として、金属酸化物及びカーボン以外に、金属硫酸塩（硫酸カルシウム、硫酸バリウム及び硫酸セリウム等）、金属ケイ酸塩（ケイ酸アルミニウム、ケイ酸カリウム、ケイ酸カルシウム及びケイ酸マグネシウム等）、金属（金、ロジウム、パラジウム及び白金等）、窒化物（窒化アルミニウム、窒化ホウ素及び窒化ケイ素等）及びこれらを含む複合体（セピオライト、ゼオライト、コージェライト、ベーマイト、イモゴライト、セリサイト、合金、珪藻土、ハイドロタルサイト、クレー、タルク、マイカ及びガラス等）等も使用できる。 As the inorganic particles (A), in addition to metal oxide and carbon, metal sulfate (calcium sulfate, barium sulfate, cerium sulfate, etc.), metal silicate (aluminum silicate, potassium silicate, calcium silicate and magnesium silicate) Etc.), metals (gold, rhodium, palladium and platinum, etc.), nitrides (aluminum nitride, boron nitride, silicon nitride, etc.) and composites containing them (sepiolite, zeolite, cordierite, boehmite, imogolite, cericite, alloys, etc.) , Silicic acid soil, hydrotalcite, clay, talc, mica, glass, etc.) can also be used.
無機粒子（Ａ）の含有量（重量％）は、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）中のポリマー及び水（Ｄ）の重量に基づいて、１〜８０が好ましく、さらに好ましくは１０〜７０、特に好ましくは２８〜６０である。この範囲であると流動性がさらに良好となる。 The content (% by weight) of the inorganic particles (A) is preferably 1 to 80 based on the weights of the inorganic particles (A), the acid (B), the polymer in the dispersant (C) and the water (D). It is more preferably 10 to 70, and particularly preferably 28 to 60. Within this range, the fluidity becomes even better.
酸（Ｂ）としては、無機粒子分散スラリーのｐＨ（２５℃）を１〜６にすることができるものであれば特に制限はなく、無機酸及び有機酸のいずれでもよく、これらを単独で使用しても混合物にしてもよい。 The acid (B) is not particularly limited as long as the pH (25 ° C.) of the inorganic particle dispersion slurry can be adjusted to 1 to 6, and either an inorganic acid or an organic acid may be used, and these may be used alone. It may be a mixture.
無機酸としては、塩酸、硫酸、硝酸、リン酸、クロム酸及びホウ酸等が挙げられる。 Examples of the inorganic acid include hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, chromic acid, boric acid and the like.
有機酸としては、カルボン酸（酢酸、トリフルオロ酢酸、リンゴ酸、クエン酸、ギ酸、グルコン酸、乳酸、シュウ酸、マロン酸、コハク酸、グルタル酸、マレイン酸、フマル酸及び酒石酸等）及びスルホン酸（メタンスルホン酸、エタンスルホン酸、ベンゼンスルホン酸及びｐ−トルエンスルホン）等が挙げられる。 Organic acids include carboxylic acids (acetic acid, trifluoroacetic acid, malic acid, citric acid, formic acid, gluconic acid, lactic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, maleic acid, fumaric acid, tartrate acid, etc.) and sulfonic acid. Acids (methane sulfonic acid, ethane sulfonic acid, benzene sulfonic acid and p-toluene sulfonic acid) and the like can be mentioned.
これらの酸のうち、硝酸及び有機酸が好ましく、さらに好ましくは硝酸及びカルボン酸、特に好ましくは硝酸、ギ酸、酢酸及びクエン酸である。 Among these acids, nitric acid and organic acids are preferable, and nitric acid and carboxylic acids are more preferable, and nitric acid, formic acid, acetic acid and citric acid are particularly preferable.
酸（Ｂ）の含有量（重量％）は、無機粒子分散スラリーのｐＨ（２５℃）を１〜６にすることができれば制限はないが、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）中のポリマー及び水（Ｄ）の重量に基づいて、０．１〜５が好ましく、さらに好ましくは０．５〜４、特に好ましくは１．５〜３である。 The content (% by weight) of the acid (B) is not limited as long as the pH (25 ° C.) of the inorganic particle dispersion slurry can be set to 1 to 6, but the inorganic particles (A), the acid (B), and the dispersant Based on the weight of the polymer in (C) and water (D), it is preferably 0.1 to 5, more preferably 0.5 to 4, and particularly preferably 1.5 to 3.
分散剤（Ｃ）は、アリルアミン（塩）、ジアリルアミン（塩）、Ｎ−ビニルイミダゾール（塩）及びＮ−ビニルピロリドンからなる群より選ばれる少なくとも１種を必須構成単量体としてなるポリマーを含有するが、これらの必須構成単量体以外にＮ−アリルイミダゾール（塩）やＮ−アリルピロリドン、２−ビニルピロール、２−アリルピロール等を必須構成単量体とするポリマーも効果的である。 The dispersant (C) contains a polymer containing at least one selected from the group consisting of allylamine (salt), diallylamine (salt), N-vinylimidazole (salt) and N-vinylpyrrolidone as an essential constituent monomer. However, in addition to these essential constituent monomers, polymers containing N-allylimidazole (salt), N-allylpyrrolidone, 2-vinylpyrrole, 2-allylpyrrole and the like as essential constituent monomers are also effective.
ポリマーは、本発明の効果を阻害しない限り、必須単量体以外に、必須単量体と共重合できる他の単量体を構成単量体とすることができるが、必須構成単量体がＮ−ビニルイミダゾール、Ｎ−ビニルピロリドン、Ｎ−アリルイミダゾール、Ｎ−アリルピロリドン、２−ビニルピロール又は２−アリルピロールの場合、他の単量体を構成単量体として含まないことが好ましい。 As long as the effect of the present invention is not impaired, the polymer may be composed of other monomers that can be copolymerized with the essential monomer in addition to the essential monomer. In the case of N-vinylimidazole, N-vinylpyrrolidone, N-allylimidazole, N-allylpyrrolidone, 2-vinylpyrrole or 2-allylpyrrole, it is preferable that no other monomer is contained as a constituent monomer.
共重合可能な他の単量体としてとくに制限はないが、アニオン単量体、カチオン単量体及びノニオン単量体が含まれる。 The other copolymerizable monomer is not particularly limited, and includes an anion monomer, a cation monomer, and a nonionic monomer.
アニオン単量体としては、アリル基又はビニル基を持つカルボン酸｛脂肪族モノカルボン酸（アクリル酸及びメタクリル酸等）、芳香族モノカルボン酸（４−ビニル安息香酸等）、脂肪族ジカルボン酸（マレイン酸、フマル酸及びアリルマロン酸等）、これらカルボン酸の分子内無水物（マレイン酸無水物及びフマル酸無水物等）、ジカルボン酸モノエステル（マレイン酸モノメチルエステル、フマル酸モノメチルエステル、フマル酸モノブチルセロソルブエステル及びマレイン酸モノブチルセロソルブエステル等）及びジカルボン酸モノアミド（マレイン酸モノアミド及びフマル酸モノアミド等）等｝；及びアリル基又はビニル基を持つスルホン酸｛ビニルスルホン酸及びアリルスルホン酸等｝等が挙げられる。 Examples of the anionic monomer include carboxylic acids having an allyl group or a vinyl group {aliphatic monocarboxylic acids (acrylic acid, methacrylic acid, etc.), aromatic monocarboxylic acids (4-vinylbenzoic acid, etc.), aliphatic dicarboxylic acids (4-vinylbenzoic acid, etc.). Maleic acid, fumaric acid, allylmalonic acid, etc.), intramolecular anhydrides of these carboxylic acids (maleic acid anhydride, fumaric acid anhydride, etc.), dicarboxylic acid monoesters (maleic acid monomethyl ester, fumaric acid monomethyl ester, fumaric acid monoester, etc.) Butyl cellosolve ester and monobutyl cellosolve ester of maleic acid, etc.) and dicarboxylic acid monoamide (monoamide of maleic acid, monoamide of fumaric acid, etc.), etc.}; Be done.
カチオン単量体としては、アリル基又はビニル基を持つアミン｛アリル脂肪族アミン（アリルメチルアミン、アリルジメチルアミン、アリルエチルアミン、アリルジエチルアミン、アリルエチルメチルアミン、アリルブチルアミン、アリルジブチルアミン、アリルブチルメチルアミン、アリルジヘキシルアミン、アリルヘキシルメチルアミン、アリルエチルヘキシルアミン、アリルオクチルアミン、アリルジオクチルアミン、アリルオクチルメチルアミン及びアリルオクチルエチルアミン等）、アリル芳香族アミン（アリルベンジルアミン、アリルベンジルメチルアミン、アリルベンジルエチルアミン、Ｎ−アリルアニリン、３−アミノスチレン及び４−アミノスチレン等）、ジアリル脂肪族アミン（ジアリルメチルアミン、ジアリルエチルアミン、ジアリルブチルアミン、ジアリルヘキシルアミン及びジアリルオクチルアミン等）｝；及びアリル基又はビニル基を持つ複素環式アミン｛ビニルピリジン、２−ビニルイミダゾリン及びＮ−アリルイミダゾール等｝等が挙げられる。 As the cationic monomer, an amine having an allyl group or a vinyl group {allyl aliphatic amine (allylmethylamine, allyldimethylamine, allylethylamine, allyldiethylamine, allylethylmethylamine, allylbutylamine, allyldibutylamine, allylbutylmethyl) Amin, allyldihexylamine, allylhexylmethylamine, allylethylhexylamine, allyloctylamine, allyldioctylamine, allyloctylmethylamine, allyloctylethylamine, etc.), allyl aromatic amines (allylbenzylamine, allylbenzylmethylamine, allylbenzyl) Ethylamine, N-allylaniline, 3-aminostyrene and 4-aminostyrene, etc.), diallyl aliphatic amines (diallylmethylamine, diallylethylamine, diallylbutylamine, diallylhexylamine, diallyloctylamine, etc.)}; and allyl groups or vinyl. Examples thereof include heterocyclic amines having a group {vinylpyridine, 2-vinylimidazoline, N-allylimidazole, etc.}.
ノニオン単量体としては、ビニル基を持つアミド｛脂肪族モノカルボン酸アミド（アクリルアミド及びメタクリルアミド等）、脂肪族ジカルボン酸ジアミド（マレイン酸ジアミド等）、脂肪族モノカルボン酸モノアルキルアミド（Ｎ−メチルアクリルアミド、Ｎ−メチルメタクリルアミド、Ｎ−エチルアクリルアミド、Ｎ−エチルメタクリルアミド、Ｎ−ｔｅｒｔ−ブチルメタクリルアミド、Ｎ−ｎ−プロピルメタクリルアミド、Ｎ−イソプロピルアクリルアミド及びＮ−シクロヘキシルメタクリルアミド）、芳香族モノカルボン酸モノアルキルアミド（Ｎ−メチル−４−ビニル安息香酸アミド）、脂肪族ジカルボン酸ジアルキルアミド（Ｎ，Ｎ’−ジメチルマレイン酸ジアミド等）、脂肪族モノカルボン酸ジアルキルアミド（Ｎ，Ｎ−ジメチル−アクリルアミド、Ｎ，Ｎ−ジメチル−メタクリルアミド、Ｎ，Ｎ−ジエチルアクリルアミド及びＮ，Ｎ−ジエチルメタクリルアミド等）、芳香族モノカルボン酸ジアルキルアミド（Ｎ，Ｎ−ジメチル−４−ビニル安息香酸アミド等）、Ｎ−ヒドロキシメチルアクリルアミド及びアリルアミド（ＣＨ２＝ＣＨＣＨ２ＣＯＮＨ２）等｝；アリル基又はビニル基を持つエステル｛脂肪族モノカルボン酸アルキルエステル（アクリル酸メチル、メタクリル酸メチル、アクリル酸エチル及びメタクリル酸エチル等）、芳香族モノカルボン酸アルキルエステル（４−ビニル安息香酸メチルエステル等）、脂肪族ジカルボン酸ジアルキルエステル（マレイン酸ジメチルエステル及びフマル酸ジメチルエステル等）、ポリオキシアルキレン脂肪族モノカルボン酸エステル（ポリオキシエチレングリコールアクリル酸ジエステル、ポリオキシエチレングリコールメタクリル酸ジエステル、メトキシポリオキシエチレンアクリル酸モノエステル、メトキシポリオキシエチレンメタクリル酸モノエステル、メトキシポリオキシプロピレンアクリル酸モノエステル及びメトキシポリオキシプロピレンメタクリル酸モノエステル等）、ポリオキシアルキレン芳香族モノカルボン酸エステル（メトキシポリオキシエチレン４−ビニル安息香酸モノエステル等）、アルコキシポリオキシアルキレン脂肪族ジカルボン酸ジエステル（メトキシポリオキシエチレンマレイン酸ジエステル等）、カルボン酸アリル（酢酸アリル、プロピオン酸アリル及び酪酸アリル等）等｝；ビニル基を持つオキサゾリドン｛N−ビニル−２−オキサゾリドン等｝；ビニル基を持つオキサゾリン（２−ビニル−２−オキサゾリン及び５−ビニルイソオキサゾリン等）；及びアリル基を持つエーテル（アリルメチルエーテル、アリルエチルエーテル及びアリルベンジルエーテル等）等が挙げられる。 Examples of the nonionic monomer include amides having a vinyl group {aliphatic monocarboxylic acid amides (acrylamide and methacrylic acid amides, etc.), aliphatic dicarboxylic acid diamides (maleic acid diamides, etc.), and aliphatic monocarboxylic acid monoalkylamides (N-). Methylacrylamide, N-methylmethacrylate, N-ethylacrylamide, N-ethylmethacrylate, N-tert-butylmethacrylate, Nn-propylmethacrylate, N-isopropylacrylamide and N-cyclohexylmethacrylate), aromatics Monocarboxylic acid monoalkylamide (N-methyl-4-vinylbenzoic acid amide), aliphatic dicarboxylic acid dialkylamide (N, N'-dimethylmaleic acid dialkylamide, etc.), aliphatic monocarboxylic acid dialkylamide (N, N-) Dimethyl-acrylamide, N, N-dimethyl-methacrylamide, N, N-diethylacrylamide and N, N-diethylmethacrylate, etc.), aromatic monocarboxylic acid dialkylamide (N, N-dimethyl-4-vinylbenzoic acid amide, etc.) Etc.), N-hydroxymethylacrylamide and allylamide (CH 2 = CHCH 2 CONH 2 ), etc.}; Estel having an allyl group or a vinyl group {aliphatic monocarboxylic acid alkyl ester (methyl acrylate, methyl methacrylate, ethyl acrylate) And ethyl methacrylate), aromatic monocarboxylic acid alkyl ester (4-vinylbenzoic acid methyl ester, etc.), aliphatic dicarboxylic acid dialkyl ester (maleic acid dimethyl ester, fumaric acid dimethyl ester, etc.), polyoxyalkylene aliphatic mono Carous acid esters (polyoxyethylene glycol acrylic acid diester, polyoxyethylene glycol methacrylate diester, methoxypolyoxyethylene acrylic acid monoester, methoxypolyoxyethylene methacrylate monoester, methoxypolyoxypropylene acrylic acid monoester and methoxypolyoxy (Propine methacrylic acid monoester, etc.), polyoxyalkylene aromatic monocarboxylic acid ester (methoxypolyoxyethylene 4-vinyl benzoic acid monoester, etc.), alkoxypolyoxyalkylene aliphatic dicarboxylic acid diester (methoxypolyoxyethylene maleic acid diester, etc.) ), Allyl carboxylate (allyl acetate, allyl propionate, allyl butyrate, etc.), etc.}; Oxazolide having a vinyl group {N-vinyl-2-oxazoline, etc.}; Oxazoline with vinyl group (2-vinyl-2-oxazoline, 5-vinylisoxazoline, etc.); and ether with allyl group (allyl methyl ether, allyl ethyl ether, and allyl). Benzyl ether, etc.) and the like.
これらの他の単量体のうち、カチオン単量体及びノニオン単量体が好ましく、さらに好ましくは（メタ）アリル基又はビニル基を持つアミン、アリル基又はビニル基を持つアミド及びアリル基又はビニル基を持つエステルである。 Among these other monomers, a cationic monomer and a nonionic monomer are preferable, and more preferably an amine having a (meth) allyl group or a vinyl group, an amide having an allyl group or a vinyl group, and an allyl group or vinyl. It is an ester with a group.
アリルアミン（塩）、ジアリルアミン（塩）、Ｎ−ビニルイミダゾール（塩）において塩を形成できる酸としては、無機酸及び有機酸のいずれでもよく、アニオン単量体も含まれる。これらを単独で使用してもよいし、複数種類用いてもよい。また、共重合可能な他の単量体のうちカチオン単量体も同じように塩を形成してもよい。 The acid capable of forming a salt in allylamine (salt), diallylamine (salt), and N-vinylimidazole (salt) may be any of an inorganic acid and an organic acid, and also includes an anionic monomer. These may be used alone or in a plurality of types. Further, among the other copolymerizable monomers, the cationic monomer may also form a salt in the same manner.
無機酸としては、塩酸、硫酸、硝酸、リン酸、クロム酸及びホウ酸等が挙げられる。 Examples of the inorganic acid include hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, chromic acid, boric acid and the like.
有機酸としては、炭素数１〜６のカルボン酸（酢酸、トリフルオロ酢酸、リンゴ酸、クエン酸、ギ酸、グルコン酸、乳酸、シュウ酸、マロン酸、コハク酸、グルタル酸、マレイン酸、フマル酸及び酒石酸等）及び炭素数１〜７のスルホン酸（メタンスルホン酸、エタンスルホン酸、ベンゼンスルホン酸及びｐ−トルエンスルホン酸）等が挙げられる。 Organic acids include carboxylic acids with 1 to 6 carbon atoms (acetic acid, trifluoroacetic acid, malic acid, citric acid, formic acid, gluconic acid, lactic acid, oxalic acid, malonic acid, succinic acid, glutaric acid, maleic acid, fumaric acid). And tartrate acid, etc.) and sulfonic acids having 1 to 7 carbon atoms (methane sulfonic acid, ethane sulfonic acid, benzene sulfonic acid, p-toluene sulfonic acid) and the like.
これらの酸のうち、硝酸及び有機酸が好ましく、さらに好ましくは硝酸及びカルボン酸、特に好ましくは硝酸、ギ酸、酢酸及びクエン酸である。 Among these acids, nitric acid and organic acids are preferable, and nitric acid and carboxylic acids are more preferable, and nitric acid, formic acid, acetic acid and citric acid are particularly preferable.
共重合可能な他の単量体のうちアニオン単量体も塩を形成してもよく、アニオン単量体と塩を形成できる塩基としては、無機塩基及び有機塩基のいずれでもよく、アリルアミン、ジアリルアミン、Ｎ−ビニルイミダゾール及び／又はカチオン単量体も含まれる。これらを単独で使用してもよいし、複数種類用いてもよい。 Of the other copolymerizable monomers, the anionic monomer may also form a salt, and the base capable of forming a salt with the anionic monomer may be either an inorganic base or an organic base, and allylamine and diallylamine. , N-vinylimidazole and / or cationic monomers are also included. These may be used alone or in a plurality of types.
無機塩基としては、アンモニア及びアルカリ金属の水酸化物（水酸化カリウム及び水酸化ナトリウム等）等が挙げられる。 Examples of the inorganic base include ammonia and alkali metal hydroxides (potassium hydroxide, sodium hydroxide, etc.) and the like.
有機塩基としては、炭素数２〜９のアミン（モノエタノールアミン、トリエタノールアミン、モノイソプロパノールアミン、ジイソプロパノールアミン及びトリイソプロパノールアミン等）等が挙げられる。 Examples of the organic base include amines having 2 to 9 carbon atoms (monoethanolamine, triethanolamine, monoisopropanolamine, diisopropanolamine, triisopropanolamine, etc.).
ポリマーに他の単量体単位を含む場合、必須単量体｛アリルアミン（塩）、ジアリルアミン（塩）、Ｎ−ビニルイミダゾール（塩）及び／又はＮ−ビニルピロリドン｝単位の含有量（モル％）は、必須単量体単位及び他の単量体単位のモル数に基づいて、２０〜９５が好ましく、さらに好ましくは３０〜９０である。この場合、他の単量体単位の含有量（モル％）は、必須単量体単位及び他の単量体単位のモル数に基づいて、５〜８０が好ましく、さらに好ましくは１０〜７０である。 If the polymer contains other monomeric units, the content (mol%) of the essential monomeric {allylamine (salt), diallylamine (salt), N-vinylimidazole (salt) and / or N-vinylpyrrolidone} units. Is preferably 20 to 95, more preferably 30 to 90, based on the number of moles of the essential monomer unit and the other monomer unit. In this case, the content (mol%) of the other monomer unit is preferably 5 to 80, more preferably 10 to 70, based on the number of moles of the essential monomer unit and the other monomer unit. is there.
ポリマーの数平均分子量（Ｍｎ）は、５００〜１００万が好ましく、さらに好ましくは２０００〜１０万である。 The number average molecular weight (Mn) of the polymer is preferably 5 to 1,000,000, more preferably 20 to 100,000.
数平均分子量（Ｍｎ）は、分子量既知の（ポリ）エチレングリコールを標準物質として、ゲルパーミエーションクロマトグラフィー（ＧＰＣ）法で測定できる（たとえば、カラム温度４０℃、溶離液メタノール：イオン交換水：酢酸ナトリウム＝８００：１２００：１５（重量比）、流速０ ．８ｍｌ／分、試料濃度０ ．４重量％溶離液溶液で測定できる。）。 The number average molecular weight (Mn) can be measured by a gel permeation chromatography (GPC) method using (poly) ethylene glycol having a known molecular weight as a standard substance (for example, column temperature 40 ° C., eluent methanol: ion-exchanged water: acetic acid). Sodium = 800: 1200: 15 (weight ratio), flow velocity 0.8 ml / min, sample concentration 0.4 wt% eluent solution can be measured).
ポリマーの製造方法としては特に制限はなく、公知の方法（たとえば、ラジカル重合法、イオン重合法、配位重合法）が適用できるが、ラジカル重合法が好ましい。 The method for producing the polymer is not particularly limited, and known methods (for example, radical polymerization method, ionic polymerization method, coordination polymerization method) can be applied, but the radical polymerization method is preferable.
必須構成単量体及び必要により他の単量体を重合した後、無機酸及び／若しくは有機酸又は無機塩基及び／若しくは有機塩基で中和してもよい。 After polymerizing the essential constituent monomers and, if necessary, other monomers, they may be neutralized with an inorganic acid and / or an organic acid or an inorganic base and / or an organic base.
分散剤（Ｃ）は、水性溶媒を含有することが好ましい。水性溶媒としては、水、炭素数１?６のアルコール（エチルアルコール、メチルアルコール、エチレングリコール及びジエチレングリコール等）及び炭素数１?６のケトン（メチルイソブチルケトン及びアセトン等）等が挙げられ、これらは単独又は混合して用いてもよい。分散剤（Ｃ）は水を含むことが好ましい。 The dispersant (C) preferably contains an aqueous solvent. Examples of the aqueous solvent include water, alcohols having 1 to 6 carbon atoms (ethyl alcohol, methyl alcohol, ethylene glycol, diethylene glycol, etc.), ketones having 1 to 6 carbon atoms (methylisobutylketone, acetone, etc.), and the like. It may be used alone or in combination. The dispersant (C) preferably contains water.
分散剤（Ｃ）に水性溶媒を含む場合、水性溶媒の含有量(重量％)は、ポリマー及び水性溶媒の重量に基づいて、２０〜８０程度が好ましい。またこの場合、ポリマーの含有量(重量％)は、ポリマー及び水性溶媒の重量に基づいて、２０〜８０程度が好ましい。 When the dispersant (C) contains an aqueous solvent, the content (% by weight) of the aqueous solvent is preferably about 20 to 80 based on the weight of the polymer and the aqueous solvent. In this case, the content (% by weight) of the polymer is preferably about 20 to 80 based on the weight of the polymer and the aqueous solvent.
分散剤（Ｃ）の含有量は、ポリマーの含有量(重量％)として、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）中のポリマー及び水（Ｄ）の重量に基づいて、０．０５〜３０が好ましく、さらに好ましくは０．１〜１０、特に好ましくは０．５〜５である。この範囲であると流動性がさらに良好となる。 The content of the dispersant (C) is based on the weight of the inorganic particles (A), the acid (B), the polymer in the dispersant (C) and the water (D) as the content (% by weight) of the polymer. It is preferably 0.05 to 30, more preferably 0.1 to 10, and particularly preferably 0.5 to 5. Within this range, the fluidity becomes even better.
水（Ｄ）としては特に限定はないが、イオン交換水及び超純水等が好ましい。 The water (D) is not particularly limited, but ion-exchanged water, ultrapure water and the like are preferable.
水（Ｄ）の含有量（重量％）は、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）中のポリマー及び水（Ｄ）の重量に基づいて、１?９０が好ましく、さらに好ましくは２０?８０、特に好ましくは３８?６５である。この範囲であると流動性がさらに良好となる。
なお、分散剤（Ｃ）に水が含まれる場合、この水（Ｄ）の含有量には分散剤（Ｃ）中の水も含まれる。
The content (% by weight) of water (D) is preferably 1 to 90 based on the weight of the polymer in the inorganic particles (A), the acid (B), the dispersant (C) and the water (D), and more preferably. It is preferably 20 to 80, particularly preferably 38 to 65. Within this range, the fluidity becomes even better.
When the dispersant (C) contains water, the content of the water (D) also includes the water in the dispersant (C).
本発明の無機粒子分散スラリーには、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）及び水（Ｄ）以外に、他の構成成分（水溶性有機化合物及び水溶性金属化合物等）や他の添加剤（増粘剤、防錆剤及び消泡剤等）を含有してもよい。 In addition to the inorganic particles (A), acid (B), dispersant (C) and water (D), the inorganic particle dispersion slurry of the present invention contains other constituents (water-soluble organic compounds, water-soluble metal compounds, etc.). And other additives (thickening agent, rust preventive, defoaming agent, etc.) may be contained.
水溶性有機化合物としては、水（０〜１００℃、好ましくは５〜６０℃）に容易に溶解する有機化合物が含まれ、炭素数１〜４のアルコール及び炭素数３〜６のケトン等が挙げられる。 Examples of the water-soluble organic compound include an organic compound that is easily dissolved in water (0 to 100 ° C., preferably 5 to 60 ° C.), and examples thereof include alcohols having 1 to 4 carbon atoms and ketones having 3 to 6 carbon atoms. Be done.
水溶性金属化合物としては、水（０〜１００℃、好ましくは５〜６０℃）に容易に溶解する金属化合物が含まれ、有機酸金属塩、金属硝酸塩、金属オキシ硝酸塩、金属水酸化物及び金属亜硝酸塩等が挙げられる。 The water-soluble metal compound includes a metal compound that is easily dissolved in water (0 to 100 ° C, preferably 5 to 60 ° C), and includes an organic acid metal salt, a metal nitrate, a metal oxynitrite, a metal hydroxide and a metal. Examples include nitrite.
他の構成成分を含有する場合、他の構成成分の含有量（重量％）は、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）中のポリマー及び水（Ｄ）の重量に基づいて、０．１〜７０が好ましく、さらに好ましくは０．３〜６０、特に好ましくは７〜５４である。 When containing other constituents, the content (% by weight) of the other constituents is based on the weight of the polymer and water (D) in the inorganic particles (A), acid (B), dispersant (C). It is preferably 0.1 to 70, more preferably 0.3 to 60, and particularly preferably 7 to 54.
増粘剤としては、公知の天然又は合成の増粘剤（無機化合物、セルロース化合物、タンパク質、アクリルポリマー及びビニルポリマー等）が含まれる。 Thickeners include known natural or synthetic thickeners (inorganic compounds, cellulose compounds, proteins, acrylic polymers, vinyl polymers, etc.).
防錆剤としては、含窒素有機防錆剤又は多価アルコール部分エステル防錆剤等からなる群より選ばれる少なくとも一種が含まれる。 The rust preventive includes at least one selected from the group consisting of a nitrogen-containing organic rust preventive, a polyhydric alcohol partial ester rust preventive, and the like.
消泡剤としては、公知の水系用の消泡剤（シリコーン系消泡剤、鉱物油系消泡剤、ポリエーテル系消泡剤及びワックス系消泡剤等）が含まれる。 Examples of the defoaming agent include known water-based defoaming agents (silicone-based defoaming agents, mineral oil-based defoaming agents, polyether-based defoaming agents, wax-based defoaming agents, and the like).
他の添加剤を含有する場合、他の添加剤の含有量（重量％）は、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）中のポリマー及び水（Ｄ）の重量に基づいて、好ましくは０．１〜５、さらに好ましくは０．５〜３、特に好ましくは０．５〜１である。 When containing other additives, the content (% by weight) of the other additives is based on the weight of the polymer and water (D) in the inorganic particles (A), acid (B), dispersant (C). It is preferably 0.1 to 5, more preferably 0.5 to 3, and particularly preferably 0.5 to 1.
本発明の無機粒子分散スラリーは、無機粒子（Ａ）、酸（Ｂ）、分散剤（Ｃ）及び水（Ｄ）、並びに必要に応じて他の構成成分及び／又は他の添加剤を均一混合分散できれば、製造方法に制限はなく、公知の混合分散機を用いて得ることができる。無機粒子（Ａ）以外の成分を均一混合してから、無機粒子（Ａ）を分散させることが好ましい。なお、均一混合分散する際、無機粒子が粉砕や破砕を受けてもよい。 The inorganic particle dispersion slurry of the present invention is a uniform mixture of inorganic particles (A), acid (B), dispersant (C) and water (D), and if necessary, other constituents and / or other additives. If it can be dispersed, there is no limitation on the production method, and it can be obtained by using a known mixing and dispersing machine. It is preferable to uniformly mix the components other than the inorganic particles (A) and then disperse the inorganic particles (A). In addition, when uniformly mixed and dispersed, the inorganic particles may be crushed or crushed.
本発明の無機粒子分散スラリー中の無機粒子（Ａ）の個数平均粒子径（μｍ）は、０．０１〜１００が好ましく、さらに好ましくは０．０２〜５０、特に好ましくは０．０８〜３６である。 The number average particle diameter (μm) of the inorganic particles (A) in the inorganic particle dispersion slurry of the present invention is preferably 0.01 to 100, more preferably 0.02 to 50, and particularly preferably 0.08 to 36. is there.
個数平均粒子径は、ＪＩＳ Ｘ８８２５：２０１３（粒子径解析−レーザー回折・散乱法）に準拠したレーザー回折分析式粒度分布計（たとえば、ＬＡ−９５０Ｖ２、株式会社堀場製作所）を用いて求められる。 The number average particle size is determined using a laser diffraction analysis type particle size distribution meter (for example, LA-950V2, Horiba Seisakusho Co., Ltd.) based on JIS X 8825: 2013 (particle size analysis-laser diffraction / scattering method).
本発明の無機粒子分散スラリーは、各種基材（プラスチック、木、皮革、金属及びセラミックス等）に塗布してもよく、乾燥成型してもよい。また、バインダー等と混合して各種基材に塗布したり、乾燥成形してもよい。さらに、塗布や成型した後に焼結してもよい。 The inorganic particle dispersion slurry of the present invention may be applied to various base materials (plastic, wood, leather, metal, ceramics, etc.) or may be dry-molded. Further, it may be mixed with a binder or the like and applied to various substrates, or may be dry-molded. Further, it may be sintered after being coated or molded.
以下、特記しない限り、部は重量部を、％は重量％を意味する。
＜実施例１＞
アリルアミン酢酸塩（６０％水溶液）１６７部（０．９モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）１６部（０．０２モル部）を加え、窒素雰囲気下で８０℃にて４時間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（１）を得た。ポリマー（１）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ１）を得た。ポリマー（１）の数平均分子量は２万であった。
Hereinafter, unless otherwise specified, parts mean parts by weight and% means% by weight.
<Example 1>
After raising the temperature to 80 ° C. while flowing nitrogen gas into 167 parts (0.9 mol parts) of allylamine acetate (60% aqueous solution), 16 parts (0.02 mol parts) of ammonium persulfate (25% aqueous solution) was added. , The reaction was carried out at 80 ° C. for 4 hours in a nitrogen atmosphere to obtain a yellow liquid crude polymer aqueous solution. 90 parts of the crude polymer aqueous solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (1). .. 80 parts of the polymer (1) and 80 parts of water were uniformly mixed to obtain the dispersant (c1) of the present invention. The number average molecular weight of the polymer (1) was 20,000.
数平均分子量（Ｍｎ）は、分子量既知の（ポリ）エチレングリコールを標準物質として、ゲルパーミエーションクロマトグラフィー（ＧＰＣ）法（カラム温度４０℃、溶離液メタノール：イオン交換水：酢酸ナトリウム＝８００：１２００：１５（重量比）、流速０ ．８ｍｌ／分、試料濃度０ ．４重量％溶離液溶液）で測定した（以下、同じである。）。 The number average molecular weight (Mn) is a gel permeation chromatography (GPC) method (column temperature 40 ° C., eluent methanol: ion-exchanged water: sodium acetate = 800: 1200, using (poly) ethylene glycol having a known molecular weight as a standard substance. Measured at 15 (weight ratio), flow velocity 0.8 ml / min, sample concentration 0.4 wt% eluent solution) (the same applies hereinafter).
＜実施例２＞
アリルアミン（６０％水溶液）７４部（０．８モル部）及びアクリルアミド（４０％水溶液）１３９部（０．８モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）３０部（０．０３モル部）を加え、窒素雰囲気下で８０℃にて４時間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液を真空乾燥して淡黄色固状のポリマー（２）を得た。ポリマー（２）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ２）を得た。ポリマー（２）の数平均分子量は２万であった。
<Example 2>
Ammonium persulfate (25 parts) was heated to 80 ° C. while flowing nitrogen gas into 74 parts (0.8 mol parts) of allylamine (60% aqueous solution) and 139 parts (0.8 mol parts) of acrylamide (40% aqueous solution). % Aqueous solution) was added in an amount of 30 parts (0.03 mol parts) and reacted at 80 ° C. for 4 hours in a nitrogen atmosphere to obtain a yellow liquid crude polymer aqueous solution. The crude polymer aqueous solution was vacuum dried to obtain a pale yellow solid polymer (2). 80 parts of the polymer (2) and 80 parts of water were uniformly mixed to obtain the dispersant (c2) of the present invention. The number average molecular weight of the polymer (2) was 20,000.
＜実施例３＞
アリルアミン酢酸塩（６０％水溶液）１５６部（０．８モル部）及びアクリルアミド（４０％水溶液）１６部（０．０９モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）１７部（０．０２モル部）を加え、窒素雰囲気下で８０℃にて４時間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（３）を得た。ポリマー（３）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ３）を得た。ポリマー（３）の数平均分子量は２万であった。
<Example 3>
Ammonium persulfate was heated to 80 ° C. while flowing nitrogen gas into 156 parts (0.8 mol parts) of allylamine acetate (60% aqueous solution) and 16 parts (0.09 mol parts) of acrylamide (40% aqueous solution). 17 parts (0.02 mol parts) of (25% aqueous solution) was added and reacted at 80 ° C. for 4 hours in a nitrogen atmosphere to obtain a yellow liquid crude polymer aqueous solution. 90 parts of the crude polymer aqueous solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (3). .. 80 parts of the polymer (3) and 80 parts of water were uniformly mixed to obtain the dispersant (c3) of the present invention. The number average molecular weight of the polymer (3) was 20,000.
＜実施例４＞
ジアリルアミンクエン酸塩（６０％水溶液）１３４部（０．３モル部）及びアクリルアミド（４０％水溶液）４９部（０．３モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）１１部（０．０１モル部）を加え、窒素雰囲気下で８０℃にて４時間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（４）を得た。ポリマー（４）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ４）を得た。ポリマー（４）の数平均分子量は２万であった。
<Example 4>
After raising the temperature to 80 ° C. while flowing nitrogen gas into 134 parts (0.3 mol parts) of diallylamine citrate (60% aqueous solution) and 49 parts (0.3 mol parts) of acrylamide (40% aqueous solution), it is excessive. 11 parts (0.01 mol parts) of ammonium sulfate (25% aqueous solution) was added and reacted at 80 ° C. for 4 hours in a nitrogen atmosphere to obtain a yellow liquid crude polymer aqueous solution. 90 parts of the crude polymer aqueous solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (4). .. 80 parts of the polymer (4) and 80 parts of water were uniformly mixed to obtain the dispersant (c4) of the present invention. The number average molecular weight of the polymer (4) was 20,000.
＜実施例５＞
ジアリルアミン（６０％水溶液）７９部（０．５モル部）及びアクリルアミド（４０％水溶液）１３１部（０．７モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）６６部（０．０７モル部）を加え、窒素雰囲気下で８０℃にて４０分間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液を真空乾燥して淡黄色固状のポリマー（５）を得た。ポリマー（５）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ５）を得た。ポリマー（５）の数平均分子量は２０００であった。
<Example 5>
After raising the temperature to 80 ° C. while flowing nitrogen gas into 79 parts (0.5 mol part) of diallylamine (60% aqueous solution) and 131 parts (0.7 mol part) of acrylamide (40% aqueous solution), ammonium persulfate (25 parts) % Aqueous solution) was added in an amount of 66 parts (0.07 mol parts) and reacted at 80 ° C. for 40 minutes in a nitrogen atmosphere to obtain a yellow liquid crude polymer aqueous solution. The crude polymer aqueous solution was vacuum dried to obtain a pale yellow solid polymer (5). 80 parts of the polymer (5) and 80 parts of water were uniformly mixed to obtain the dispersant (c5) of the present invention. The number average molecular weight of the polymer (5) was 2000.
＜実施例６＞
ジアリルアミンギ酸塩（６０％水溶液）８７部（０．４モル部）及びアリルジメチルアミンギ酸塩（６０％水溶液）８０部（０．４モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）１４部（０．０２モル部）を加え、窒素雰囲気下で８０℃にて４時間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（６）を得た。ポリマー（６）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ６）を得た。ポリマー（６）の数平均分子量は１万であった。
<Example 6>
The temperature was raised to 80 ° C. while flowing nitrogen gas into 87 parts (0.4 mol part) of diallylamine formate (60% aqueous solution) and 80 parts (0.4 mol part) of allyldimethylamine formate (60% aqueous solution). After that, 14 parts (0.02 mol parts) of ammonium persulfate (25% aqueous solution) was added and reacted at 80 ° C. for 4 hours in a nitrogen atmosphere to obtain a yellow liquid crude polymer aqueous solution. 90 parts of the crude polymer aqueous solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (6). .. 80 parts of the polymer (6) and 80 parts of water were uniformly mixed to obtain the dispersant (c6) of the present invention. The number average molecular weight of the polymer (6) was 10,000.
＜実施例７＞
ジアリルアミン硝酸塩（６０％水溶液）１０３部（０．４モル部）及びメタクリル酸メチル（６０％水溶液）６４部（０．４モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）３部（３×１０−３モル部）を加え、窒素雰囲気下で８０℃にて８時間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（７）を得た。ポリマー（７）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ７）を得た。ポリマー（７）の数平均分子量は１０万であった。
<Example 7>
After raising the temperature to 80 ° C. while flowing nitrogen gas into 103 parts (0.4 mol part) of diallylamine nitrate (60% aqueous solution) and 64 parts (0.4 mol part) of methyl methacrylate (60% aqueous solution), it is excessive. 3 parts (3 × 10 -3 mol parts) of ammonium sulfate (25% aqueous solution) was added and reacted at 80 ° C. for 8 hours in a nitrogen atmosphere to obtain a yellow liquid crude polymer aqueous solution. 90 parts of the crude polymer aqueous solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (7). .. 80 parts of the polymer (7) and 80 parts of water were uniformly mixed to obtain the dispersant (c7) of the present invention. The number average molecular weight of the polymer (7) was 100,000.
＜実施例８＞
ジアリルアミン酢酸塩（６０％水溶液）１１５部（０．４モル部）及びアクリルアミド（４０％水溶液）７８部（０．４モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）６０部（０．０７モル部）を加え、窒素雰囲気下で８０℃にて３時間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（８）を得た。ポリマー（８）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ８）を得た。ポリマー（８）の数平均分子量は５０００であった。
<Example 8>
After raising the temperature to 80 ° C. while flowing nitrogen gas into 115 parts (0.4 mol part) of diallylamine acetate (60% aqueous solution) and 78 parts (0.4 mol part) of acrylamide (40% aqueous solution), ammonium persulfate 60 parts (0.07 mol parts) of (25% aqueous solution) was added and reacted at 80 ° C. for 3 hours in a nitrogen atmosphere to obtain a yellow liquid crude polymer aqueous solution. 90 parts of the crude polymer aqueous solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (8). .. 80 parts of the polymer (8) and 80 parts of water were uniformly mixed to obtain the dispersant (c8) of the present invention. The number average molecular weight of the polymer (8) was 5000.
＜実施例９＞
アリルアミン酢酸塩（６０％水溶液）７部（０．０４モル部）及びメトキシポリオキシエチレン（オキシエチレン：２３モル）メタクリル酸エステル（５０％水溶液）１９１部（０．０９モル部）に窒素ガスを流入させながら８０℃に昇温した後、過硫酸アンモニウム（２５％水溶液）８部（０．０１モル部）を加え、窒素雰囲気下で８０℃にて３時間反応させ、黄色液体状の粗重合体水溶液を得た。粗重合体水溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（９）を得た。ポリマー（９）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ９）を得た。ポリマー（９）の数平均分子量は２万であった。
<Example 9>
Nitrogen gas was added to 7 parts (0.04 mol parts) of allylamine acetate (60% aqueous solution) and 191 parts (0.09 mol parts) of methoxypolyoxyethylene (oxyethylene: 23 mol) methacrylic acid ester (50% aqueous solution). After raising the temperature to 80 ° C. while flowing in, 8 parts (0.01 mol parts) of ammonium persulfate (25% aqueous solution) is added and reacted at 80 ° C. for 3 hours in a nitrogen atmosphere to produce a yellow liquid crude polymer aqueous solution. Got 90 parts of the crude polymer aqueous solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (9). .. 80 parts of the polymer (9) and 80 parts of water were uniformly mixed to obtain the dispersant (c9) of the present invention. The number average molecular weight of the polymer (9) was 20,000.
＜実施例１０＞
Ｎ−ビニルイミダゾール（２０％トルエン溶液）５００部（１．１モル部）及びアゾビスイソブチロニトリル１２部（０．０７モル部）を均一混合し、窒素雰囲気下で６０℃にて４８時間反応させ、懸濁液状の粗重合体トルエン溶液を得た。粗重合体トルエン溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（１０）を得た。ポリマー（１０）８０部及び水２０部を均一混合して、本発明の分散剤（ｃ１０）を得た。ポリマー（１０）の数平均分子量は５０００であった。
<Example 10>
500 parts (1.1 mol parts) of N-vinylimidazole (20% toluene solution) and 12 parts (0.07 mol parts) of azobisisobutyronitrile were uniformly mixed and heated at 60 ° C. for 48 hours under a nitrogen atmosphere. The reaction was carried out to obtain a suspension-like crude polymer toluene solution. 90 parts of the crude polymer toluene solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (10). It was. 80 parts of the polymer (10) and 20 parts of water were uniformly mixed to obtain the dispersant (c10) of the present invention. The number average molecular weight of the polymer (10) was 5000.
＜実施例１１＞
Ｎ−ビニルイミダゾール（１０％トルエン溶液）１０００部（１．１モル部）及びアゾビスイソブチロニトリル０．６部（０．００４モル部）を均一混合し、窒素雰囲気下で６０℃にて４８時間反応させ、懸濁液状の粗重合体トルエン溶液を得た。粗重合体トルエン溶液９０部を１０００部のアセトン中に注いで、生じた白色沈殿を濾別しさらに２回５００部のアセトンで洗浄した後、真空乾燥して白色固状のポリマー（１１）を得た。ポリマー（１１）４９部、酢酸（ＥＰ規格、ナカライテスク株式会社）３１部及び水３２０部を均一混合して、本発明の分散剤（ｃ１１）を得た。ポリマー（１１）の数平均分子量は１０万であった。
<Example 11>
1000 parts (1.1 mol parts) of N-vinylimidazole (10% toluene solution) and 0.6 parts (0.004 mol parts) of azobisisobutyronitrile were uniformly mixed and at 60 ° C. under a nitrogen atmosphere. The reaction was carried out for 48 hours to obtain a suspension-like crude polymer toluene solution. 90 parts of the crude polymer toluene solution was poured into 1000 parts of acetone, the white precipitate formed was filtered off, washed twice with 500 parts of acetone, and then vacuum dried to obtain a white solid polymer (11). It was. 49 parts of the polymer (11), 31 parts of acetic acid (EP standard, Nacalai Tesque, Inc.) and 320 parts of water were uniformly mixed to obtain the dispersant (c11) of the present invention. The number average molecular weight of the polymer (11) was 100,000.
＜実施例１２＞
水１００部及び硫酸銅（ＩＩ）（１０００ｐｐｍ水溶液）５×１０−４部（３×１０−９モル部）を均一混合し、これを窒素雰囲気下で６０℃に昇温した後、これに、Ｎ−ビニルピロリドン１００部（０．９モル部）、アンモニア（２８％水溶液）４．７部（０．０８モル部）及び過酸化水素（３５％水溶液）３１部（０．３モル部）を、夫々別々に３時間かけて滴下した。滴下終了後、アンモニア（２８％水溶液）１．６部（０．０３モル部）を添加混合し１時間後、８０℃に昇温し、過酸化水素（３５％水溶液）４．４部（０．０４モル部）を添加混合した。１．５時間後、過酸化水素（３５％水溶液）４．４部（０．０４モル部）を添加混合した後、さらに８０℃で１時間保持して粗重合体水溶液を得た。粗重合体水溶液を真空乾燥して淡黄色固状のポリマー（１２）を得た。ポリマー（１２）８０部及び水８０部を均一混合して、本発明の分散剤（ｃ１２）とした。ポリマー（１２）の数平均分子量は９０００であった。
<Example 12>
100 parts of water and 5 × 10 -4 parts (3 × 10 -9 mol parts) of copper (II) sulfate (1000 ppm aqueous solution) were uniformly mixed, and the temperature was raised to 60 ° C. in a nitrogen atmosphere. 100 parts (0.9 mol parts) of N-vinylpyrrolidone, 4.7 parts (0.08 mol parts) of ammonia (28% aqueous solution) and 31 parts (0.3 mol parts) of hydrogen peroxide (35% aqueous solution). , Each of which was added dropwise over 3 hours. After completion of the dropping, 1.6 parts (0.03 mol parts) of ammonia (28% aqueous solution) was added and mixed, and after 1 hour, the temperature was raised to 80 ° C. and 4.4 parts (0) of hydrogen peroxide (35% aqueous solution) was added. .04 mol parts) was added and mixed. After 1.5 hours, 4.4 parts (0.04 mol parts) of hydrogen peroxide (35% aqueous solution) was added and mixed, and the mixture was further held at 80 ° C. for 1 hour to obtain a crude polymer aqueous solution. The crude polymer aqueous solution was vacuum dried to obtain a pale yellow solid polymer (12). 80 parts of the polymer (12) and 80 parts of water were uniformly mixed to obtain the dispersant (c12) of the present invention. The number average molecular weight of the polymer (12) was 9000.
＜実施例１３＞
水１００部及び硫酸銅（ＩＩ）（１０００ｐｐｍ水溶液）５×１０−４部（３×１０−９モル部）を均一混合し、これを窒素雰囲気下で６０℃に昇温した後、Ｎ−ビニルピロリドン１００部（０．９モル部）、アンモニア（２８％水溶液）０．８２部（０．０１モル部）及び過酸化水素（３５％水溶液）５．４部（０．０６モル部）を、夫々別々に３時間かけて滴下した。滴下終了後、アンモニア（２８％水溶液）０．２８部（０．００５モル部）を添加混合し１時間後、８０℃に昇温し、過酸化水素（３５％水溶液）０．８部（０．００８モル部）を添加混合した。１．５時間後、過酸化水素（３５％水溶液）０．８部（０．００８モル部）を添加混合した後、さらに８０℃で１時間保持して粗重合体水溶液を得た。粗重合体水溶液を真空乾燥して淡黄色固体のポリマー（１３）を得た。ポリマー（１３）８０部及び水３２０部を均一混合して、本発明の分散剤（ｃ１３）を得た。ポリマー（１３）の数平均分子量は５万であった。
<Example 13>
100 parts of water and 5 × 10 -4 parts (3 × 10 -9 mol parts) of copper (II) sulfate (1000 ppm aqueous solution) are uniformly mixed, and this is heated to 60 ° C. in a nitrogen atmosphere and then N-vinyl. 100 parts (0.9 mol parts) of pyrrolidone, 0.82 parts (0.01 mol parts) of ammonia (28% aqueous solution) and 5.4 parts (0.06 mol parts) of hydrogen peroxide (35% aqueous solution). Each was dropped separately over 3 hours. After completion of the dropping, 0.28 part (0.005 mol part) of ammonia (28% aqueous solution) was added and mixed, and after 1 hour, the temperature was raised to 80 ° C. and 0.8 part (0 part) of hydrogen peroxide (35% aqueous solution) was added. .008 mol parts) was added and mixed. After 1.5 hours, 0.8 part (0.008 mol part) of hydrogen peroxide (35% aqueous solution) was added and mixed, and the mixture was further maintained at 80 ° C. for 1 hour to obtain a crude polymer aqueous solution. The crude polymer aqueous solution was vacuum dried to obtain a pale yellow solid polymer (13). 80 parts of the polymer (13) and 320 parts of water were uniformly mixed to obtain the dispersant (c13) of the present invention. The number average molecular weight of the polymer (13) was 50,000.
＜実施例１４＞
分散剤（ｃ１）４部と水（ｄ１；イオン交換水）５３部と酸（ｂ１；酢酸、ＥＰ規格、ナカライテスク株式会社）３部を均一混合し、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，０００ｒｐｍで攪拌しながら、無機粒子（アルミナ、Ａ−１１、住友化学株式会社）４０部を徐々に加え、加え終わってから１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（１）を得た。無機粒子分散スラリー（１）中の無機粒子（ａ１０１）の個数平均粒子径は３３μｍであった。
<Example 14>
4 parts of dispersant (c1), 53 parts of water (d1; ion-exchanged water) and 3 parts of acid (b1; acetic acid, EP standard, Nacalai Tesque Co., Ltd.) are uniformly mixed, and a homomixer (HIGH-FLEX DISPERSER, Co., Ltd.) While stirring at 1,000 rpm using SMT), 40 parts of inorganic particles (alumina, A-11, Sumitomo Chemical Co., Ltd.) were gradually added, and after the addition was completed, stirring was performed at 1,500 rpm for 5 minutes. The inorganic particle dispersion slurry (1) of the present invention was obtained. The number average particle diameter of the inorganic particles (a101) in the inorganic particle dispersion slurry (1) was 33 μm.
個数平均粒子径は、レーザー回折式粒度分析計（ＬＡ−９５０Ｖ２、株式会社堀場製作所）を用い、電気伝導度０．１ｍＳ／ｍ以下の水に、測定試料濃度０．１％となるように測定試料を添加して、測定温度２５±１０℃で測定した。なお、循環液（水）の屈折率１．３３、アルミナの屈折率１．６６、カーボンブラックの屈折率１．９２、酸化チタンの屈折率２．５０、親水性シリカの屈折率１．４５を用いた（以下同様である。）。 The number average particle size is measured using a laser diffraction type particle size analyzer (LA-950V2, HORIBA, Ltd.) in water with an electrical conductivity of 0.1 mS / m or less so that the measurement sample concentration is 0.1%. A sample was added and the measurement was performed at a measurement temperature of 25 ± 10 ° C. The refractive index of the circulating fluid (water) is 1.33, the refractive index of alumina is 1.66, the refractive index of carbon black is 1.92, the refractive index of titanium oxide is 2.50, and the refractive index of hydrophilic silica is 1.45. Used (the same applies hereinafter).
＜実施例１５＞
分散剤（ｃ２）８部と水（ｄ１；イオン交換水）６１部と酸（ｂ２；クエン酸、ＥＰ規格、ナカライテスク株式会社）３部を均一混合し、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，０００ｒｐｍで攪拌しながら、無機粒子（アルミナ、Ａ−１１、住友化学株式会社）２８部を徐々に加え、加え終わってから１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（２）を得た。無機粒子分散スラリー（２）中の無機粒子（ａ１０２）の個数平均粒子径は３３μｍであった。
<Example 15>
8 parts of dispersant (c2), 61 parts of water (d1; ion-exchanged water) and 3 parts of acid (b2; citric acid, EP standard, Nacalai Tesque Co., Ltd.) are uniformly mixed, and a homomixer (HIGH-FLEX DISPERSER) is used. While stirring at 1,000 rpm using the company SMT), gradually add 28 parts of inorganic particles (alumina, A-11, Sumitomo Chemical Co., Ltd.), and after the addition is completed, stir at 1,500 rpm for 5 minutes. , The inorganic particle dispersion slurry (2) of the present invention was obtained. The number average particle diameter of the inorganic particles (a102) in the inorganic particle dispersion slurry (2) was 33 μm.
＜実施例１６＞
分散剤（ｃ１）を分散剤（ｃ３）に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（３）を得た。無機粒子分散スラリー（３）中の無機粒子（ａ１０３）の個数平均粒子径は３３μｍであった。
<Example 16>
The inorganic particle dispersion slurry (3) of the present invention was obtained in the same manner as in Example 14 except that the dispersant (c1) was changed to the dispersant (c3). The number average particle diameter of the inorganic particles (a103) in the inorganic particle dispersion slurry (3) was 33 μm.
＜実施例１７＞
分散剤（ｃ４）１０部と水（ｄ１；イオン交換水）４７部と酸（ｂ３；ギ酸、ＥＰ規格、ナカライテスク株式会社）３部を均一混合し、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，０００ｒｐｍで攪拌しながら、無機粒子（アルミナ、Ａ−１１、住友化学株式会社）４０部を徐々に加え、加え終わってから１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（４）を得た。無機粒子分散スラリー（４）中の無機粒子（ａ１０４）の個数平均粒子径は３３μｍであった。
<Example 17>
10 parts of dispersant (c4), 47 parts of water (d1; ion-exchanged water) and 3 parts of acid (b3; formic acid, EP standard, Nacalai Tesque Co., Ltd.) were uniformly mixed, and a homomixer (HIGH-FLEX DISPERSER, Co., Ltd.) was mixed. While stirring at 1,000 rpm using SMT), 40 parts of inorganic particles (alumina, A-11, Sumitomo Chemical Co., Ltd.) were gradually added, and after the addition was completed, stirring was performed at 1,500 rpm for 5 minutes. The inorganic particle dispersion slurry (4) of the present invention was obtained. The number average particle diameter of the inorganic particles (a104) in the inorganic particle dispersion slurry (4) was 33 μm.
＜実施例１８＞
分散剤（ｃ１）を分散剤（ｃ５）に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（５）を得た。無機粒子分散スラリー（５）中の無機粒子（ａ１０５）の個数平均粒子径は３３μｍであった。
<Example 18>
The inorganic particle dispersion slurry (5) of the present invention was obtained in the same manner as in Example 14 except that the dispersant (c1) was changed to the dispersant (c5). The number average particle diameter of the inorganic particles (a105) in the inorganic particle dispersion slurry (5) was 33 μm.
＜実施例１９＞
分散剤（ｃ６）１部と水（ｄ１；イオン交換水）３７．５部と酸（ｂ４；硝酸、ＪＩＳ試薬特級、ナカライテスク株式会社）１．５部を均一混合し、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，０００ｒｐｍで攪拌しながら、無機粒子（アルミナ、Ａ−１１、住友化学株式会社）６０部を徐々に加え、加え終わってから１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（６）を得た。無機粒子分散スラリー（６）中の無機粒子（ａ１０６）の個数平均粒子径は３７μｍであった。
<Example 19>
1 part of dispersant (c6), 37.5 parts of water (d1; ion-exchanged water) and 1.5 parts of acid (b4; nitric acid, JIS reagent special grade, Nacalai Tesque Co., Ltd.) were uniformly mixed, and a homomixer (HIGH-) was mixed. While stirring at 1,000 rpm using FLEX DISPERSER (SMT Co., Ltd.), gradually add 60 parts of inorganic particles (alumina, A-11, Sumitomo Chemical Co., Ltd.), and after the addition is completed, add 60 parts at 1,500 rpm for 5 minutes. Stirring was performed to obtain the inorganic particle dispersion slurry (6) of the present invention. The number average particle diameter of the inorganic particles (a106) in the inorganic particle dispersion slurry (6) was 37 μm.
＜実施例２０＞
分散剤（ｃ１）を分散剤（ｃ７）に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（７）を得た。無機粒子分散スラリー（７）中の無機粒子（ａ１０７）の個数平均粒子径は３４μｍであった。
<Example 20>
The inorganic particle dispersion slurry (7) of the present invention was obtained in the same manner as in Example 14 except that the dispersant (c1) was changed to the dispersant (c7). The number average particle diameter of the inorganic particles (a107) in the inorganic particle dispersion slurry (7) was 34 μm.
＜実施例２１＞
分散剤（ｃ１）を分散剤（ｃ８）に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（８）を得た。無機粒子分散スラリー（８）中の無機粒子（ａ１０８）の個数平均粒子径は３３μｍであった。
<Example 21>
The inorganic particle dispersion slurry (8) of the present invention was obtained in the same manner as in Example 14 except that the dispersant (c1) was changed to the dispersant (c8). The number average particle diameter of the inorganic particles (a108) in the inorganic particle dispersion slurry (8) was 33 μm.
＜実施例２２＞
分散剤（ｃ１）を分散剤（ｃ９）に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（９）を得た。無機粒子分散スラリー（９）中の無機粒子（ａ１０９）の個数平均粒子径は３４μｍであった。
<Example 22>
The inorganic particle dispersion slurry (9) of the present invention was obtained in the same manner as in Example 14 except that the dispersant (c1) was changed to the dispersant (c9). The number average particle diameter of the inorganic particles (a109) in the inorganic particle dispersion slurry (9) was 34 μm.
＜実施例２３＞
分散剤（ｃ１）４部を分散剤（ｃ１０）２．５部に変更し、水（ｄ１）５３部を５４．５部に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（１０）を得た。無機粒子分散スラリー（１０）中の無機粒子（ａ１１０）の個数平均粒子径は３３μｍであった。
<Example 23>
Inorganic of the present invention in the same manner as in Example 14, except that 4 parts of the dispersant (c1) was changed to 2.5 parts of the dispersant (c10) and 53 parts of water (d1) was changed to 54.5 parts. A particle dispersion slurry (10) was obtained. The number average particle diameter of the inorganic particles (a110) in the inorganic particle dispersion slurry (10) was 33 μm.
＜実施例２４＞
分散剤（ｃ１）４部を分散剤（ｃ１１）１０部に変更し、水（ｄ１）５３部を４７部に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（１１）を得た。無機粒子分散スラリー（１１）中の無機粒子（ａ１１１）の個数平均粒子径は３４μｍであった。
<Example 24>
Inorganic particle dispersion slurry of the present invention in the same manner as in Example 14, except that 4 parts of the dispersant (c1) was changed to 10 parts of the dispersant (c11) and 53 parts of water (d1) was changed to 47 parts. 11) was obtained. The number average particle diameter of the inorganic particles (a111) in the inorganic particle dispersion slurry (11) was 34 μm.
＜実施例２５＞
分散剤（ｃ１）を分散剤（ｃ１２）に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（１２）を得た。無機粒子分散スラリー（１２）中の無機粒子（ａ１１２）の個数平均粒子径は３４μｍであった。
<Example 25>
The inorganic particle dispersion slurry (12) of the present invention was obtained in the same manner as in Example 14 except that the dispersant (c1) was changed to the dispersant (c12). The number average particle diameter of the inorganic particles (a112) in the inorganic particle dispersion slurry (12) was 34 μm.
＜実施例２６＞
分散剤（ｃ１）４部を分散剤（ｃ１３）１０部に変更し、水（ｄ１）５３部を４７部に変更したこと以外、実施例１４と同様にして、本発明の無機粒子分散スラリー（１３）を得た。無機粒子分散スラリー（１３）中の無機粒子（ａ１１３）の個数平均粒子径は３５μｍであった。
<Example 26>
Inorganic particle dispersion slurry of the present invention in the same manner as in Example 14, except that 4 parts of the dispersant (c1) was changed to 10 parts of the dispersant (c13) and 53 parts of water (d1) was changed to 47 parts. 13) was obtained. The number average particle diameter of the inorganic particles (a113) in the inorganic particle dispersion slurry (13) was 35 μm.
＜実施例２７＞
分散剤（ｃ３）１部と水（ｄ１；イオン交換水）３７．５部と酸（ｂ４；硝酸、ＪＩＳ試薬特級、ナカライテスク株式会社）１．５部と無機粒子（カーボンブラック、ＭＡ１００、三菱化学株式会社）６０部を均一混合し、撹拌・脱泡装置（マゼルスターＫＫ−ＶＴ３００、倉敷紡績株式会社）を用いて撹拌し、超音波分散装置（ＵＰ４００Ｓ、ヒールッシャー社）で３０秒間出力２４０Ｗで分散させ、本発明の無機粒子分散スラリー（１４）を得た。無機粒子分散スラリー（１４）中の無機粒子（ａ２０１）の個数平均粒子径は０．１９μｍであった。
<Example 27>
Dispersant (c3) 1 part, water (d1; ion-exchanged water) 37.5 parts, acid (b4; nitric acid, JIS reagent special grade, Nacalai Tesque Co., Ltd.) 1.5 parts and inorganic particles (carbon black, MA100, Mitsubishi) Chemical Co., Ltd.) 60 parts are uniformly mixed, stirred using a stirring / defoaming device (Mazelstar KK-VT300, Kurashiki Spinning Co., Ltd.), and dispersed at an output of 240 W for 30 seconds with an ultrasonic disperser (UP400S, Heelser Co., Ltd.). Then, the inorganic particle dispersion slurry (14) of the present invention was obtained. The number average particle diameter of the inorganic particles (a201) in the inorganic particle dispersion slurry (14) was 0.19 μm.
＜実施例２８＞
分散剤（ｃ１０）６．３部と水（ｄ１；イオン交換水）６２．７部と酸（ｂ４；硝酸、ＪＩＳ試薬特級、ナカライテスク株式会社）３部と無機粒子（カーボンブラック、ＭＡ１００、三菱化学株式会社）２８部を均一混合し、撹拌・脱泡装置（マゼルスターＫＫ−ＶＴ３００、倉敷紡績株式会社）を用いて撹拌し、超音波分散装置（ＵＰ４００Ｓ、ヒールッシャー社）で３０秒間出力２４０Ｗで分散させ、本発明の無機粒子分散スラリー（１５）を得た。無機粒子分散スラリー（１５）中の無機粒子（ａ２０２）の個数平均粒子径は０．０８μｍであった。
<Example 28>
6.3 parts of dispersant (c10), 62.7 parts of water (d1; ion-exchanged water), 3 parts of acid (b4; nitric acid, JIS reagent special grade, Nacalai Tesque Co., Ltd.) and inorganic particles (carbon black, MA100, Mitsubishi) (Chemical Co., Ltd.) 28 parts are uniformly mixed, stirred using a stirring / defoaming device (Mazelstar KK-VT300, Kurashiki Spinning Co., Ltd.), and dispersed at an output of 240 W for 30 seconds with an ultrasonic disperser (UP400S, Heelser Co., Ltd.). Then, the inorganic particle dispersion slurry (15) of the present invention was obtained. The number average particle size of the inorganic particles (a202) in the inorganic particle dispersion slurry (15) was 0.08 μm.
＜実施例２９＞
分散剤（ｃ１２）１０部と水（ｄ１；イオン交換水）６０部と酸（ｂ４；硝酸、ＪＩＳ試薬特級、ナカライテスク株式会社）２部と無機粒子（カーボンブラック、ＭＡ１００、三菱化学株式会社）２８部を均一混合し、撹拌・脱泡装置（マゼルスターＫＫ−ＶＴ３００、倉敷紡績株式会社）を用いて撹拌し、超音波分散装置（ＵＰ４００Ｓ、ヒールッシャー社）で３０秒間出力２４０Ｗで分散させ、本発明の無機粒子分散スラリー（１６）を得た。無機粒子分散スラリー（１６）中の無機粒子（ａ２０３）の個数平均粒子径は０．０８μｍであった。
<Example 29>
10 parts of dispersant (c12), 60 parts of water (d1; ion-exchanged water), 2 parts of acid (b4; nitric acid, JIS reagent special grade, Nacalai Tesque Co., Ltd.) and inorganic particles (carbon black, MA100, Mitsubishi Chemical Co., Ltd.) 28 parts are uniformly mixed, stirred using a stirring / defoaming device (Mazelstar KK-VT300, Kurashiki Spinning Co., Ltd.), and dispersed at an output of 240 W for 30 seconds with an ultrasonic disperser (UP400S, Heelsher Co., Ltd.). Inorganic particle dispersion slurry (16) was obtained. The number average particle size of the inorganic particles (a203) in the inorganic particle dispersion slurry (16) was 0.08 μm.
＜実施例３０＞
無機粒子（酸化チタン、Ｒ−８２０、石原産業株式会社）６０部、酸（ｂ１）１．５部、分散剤（ｃ３）１部及び水（ｄ１）３７．５部を均一混合した後、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（１７）を得た。無機粒子分散スラリー（１７）中の無機粒子（ａ３０１）の個数平均粒子径は０．５０μｍであった。
<Example 30>
After uniformly mixing 60 parts of inorganic particles (titanium oxide, R-820, Ishihara Sangyo Co., Ltd.), 1.5 parts of acid (b1), 1 part of dispersant (c3) and 37.5 parts of water (d1), homo The inorganic particle dispersion slurry (17) of the present invention was obtained by stirring at 1,500 rpm for 5 minutes using a mixer (HIGH-FLEX DISPERSER, SMT Co., Ltd.). The number average particle diameter of the inorganic particles (a301) in the inorganic particle dispersion slurry (17) was 0.50 μm.
＜実施例３１＞
無機粒子（酸化チタン、Ｒ−８２０、石原産業株式会社）５５．５部、酸（ｂ１）１．５部、分散剤（ｃ８）１０部及び水（ｄ１）３３部を均一混合した後、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（１８）を得た。無機粒子分散スラリー（１８）中の無機粒子（ａ３０２）の個数平均粒子径は０．４９μｍであった。
<Example 31>
After uniformly mixing 55.5 parts of inorganic particles (titanium oxide, R-820, Ishihara Sangyo Co., Ltd.), 1.5 parts of acid (b1), 10 parts of dispersant (c8) and 33 parts of water (d1), homo The inorganic particle dispersion slurry (18) of the present invention was obtained by stirring at 1,500 rpm for 5 minutes using a mixer (HIGH-FLEX DISPERSER, SMT Co., Ltd.). The number average particle diameter of the inorganic particles (a302) in the inorganic particle dispersion slurry (18) was 0.49 μm.
＜実施例３２＞
無機粒子（酸化チタン、Ｒ−８２０、石原産業株式会社）２８部、酸（ｂ１）３部、分散剤（ｃ１２）８部及び水（ｄ１）６１部を均一混合した後、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（１９）を得た。無機粒子分散スラリー（１９）中の無機粒子（ａ３０３）の個数平均粒子径は０．４９μｍであった。
<Example 32>
After uniformly mixing 28 parts of inorganic particles (titanium oxide, R-820, Ishihara Sangyo Co., Ltd.), 3 parts of acid (b1), 8 parts of dispersant (c12) and 61 parts of water (d1), a homomixer (HIGH-) The inorganic particle dispersion slurry (19) of the present invention was obtained by stirring at 1,500 rpm for 5 minutes using FLEX DISPERSER (SMT Co., Ltd.). The number average particle size of the inorganic particles (a303) in the inorganic particle dispersion slurry (19) was 0.49 μm.
＜実施例３３＞
無機粒子（親水性シリカ、ニップシールＮＡ、東ソー・シリカ株式会社）３５部、酸（ｂ１）２部、分散剤（ｃ３）６部及び水（ｄ１）５７部を均一混合した後、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（２０）を得た。無機粒子分散スラリー（２０）中の無機粒子（ａ４０１）の個数平均粒子径は１０μｍであった。
<Example 33>
After uniformly mixing 35 parts of inorganic particles (hydrophilic silica, nip seal NA, Toso Silica Co., Ltd.), 2 parts of acid (b1), 6 parts of dispersant (c3) and 57 parts of water (d1), a homomixer (HIGH) The inorganic particle-dispersed slurry (20) of the present invention was obtained by stirring at 1,500 rpm for 5 minutes using −FLEX DISPERSER, SMT Co., Ltd.). The number average particle diameter of the inorganic particles (a401) in the inorganic particle dispersion slurry (20) was 10 μm.
＜実施例３４＞
無機粒子（親水性シリカ、ニップシールＮＡ、東ソー・シリカ株式会社）２８部、酸（ｂ１）３部、分散剤（ｃ８）８部及び水（ｄ１）６１部を均一混合した後、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（２１）を得た。無機粒子分散スラリー（２１）中の無機粒子（ａ４０２）の個数平均粒子径は１０μｍであった。
<Example 34>
After uniformly mixing 28 parts of inorganic particles (hydrophilic silica, nip seal NA, Tosoh Silica Co., Ltd.), 3 parts of acid (b1), 8 parts of dispersant (c8) and 61 parts of water (d1), a homomixer (HIGH) The inorganic particle-dispersed slurry (21) of the present invention was obtained by stirring at 1,500 rpm for 5 minutes using −FLEX DISPERSER, SMT Co., Ltd.). The number average particle diameter of the inorganic particles (a402) in the inorganic particle dispersion slurry (21) was 10 μm.
＜実施例３５＞
無機粒子（親水性シリカ、ニップシールＮＡ、東ソー・シリカ株式会社）６０部、酸（ｂ４）１．５部、分散剤（ｃ３）１部及び水（ｄ１）３７．５部を均一混合した後、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（２２）を得た。無機粒子分散スラリー（２２）中の無機粒子（ａ４０３）の個数平均粒子径は１１μｍであった。
<Example 35>
After uniformly mixing 60 parts of inorganic particles (hydrophilic silica, nip seal NA, Toso Silica Co., Ltd.), 1.5 parts of acid (b4), 1 part of dispersant (c3) and 37.5 parts of water (d1), The inorganic particle dispersion slurry (22) of the present invention was obtained by stirring at 1,500 rpm for 5 minutes using a homomixer (HIGH-FLEX DISPERSER, SMT Co., Ltd.). The number average particle diameter of the inorganic particles (a403) in the inorganic particle dispersion slurry (22) was 11 μm.
＜実施例３６＞
無機粒子（親水性シリカ、ニップシールＮＡ、東ソー・シリカ株式会社）３５部、酸（ｂ４）２部、分散剤（ｃ８）１０部及び水（ｄ１）５３部を均一混合した後、ホモミキサー（ＨＩＧＨ−ＦＬＥＸ ＤＩＳＰＥＲＳＥＲ、株式会社ＳＭＴ）を用いて１，５００ｒｐｍにて５分間攪拌を行って、本発明の無機粒子分散スラリー（２３）を得た。無機粒子分散スラリー（２３）中の無機粒子（ａ４０４）の個数平均粒子径は１１μｍであった。
<Example 36>
After uniformly mixing 35 parts of inorganic particles (hydrophilic silica, nip seal NA, Toso Silica Co., Ltd.), 2 parts of acid (b4), 10 parts of dispersant (c8) and 53 parts of water (d1), a homomixer (HIGH) The inorganic particle-dispersed slurry (23) of the present invention was obtained by stirring at 1,500 rpm for 5 minutes using −FLEX DISPERSER, SMT Co., Ltd.). The number average particle diameter of the inorganic particles (a404) in the inorganic particle dispersion slurry (23) was 11 μm.
＜比較例１＞
分散剤（ｃ１）を水（ｄ１）に変更したこと以外、実施例１４と同様にして、比較用の無機粒子分散スラリー（２４）の調製を試みたが、無機粒子が沈降してしまい無機粒子分散スラリーを得ることができなかった。
<Comparative example 1>
An attempt was made to prepare a comparative inorganic particle dispersion slurry (24) in the same manner as in Example 14 except that the dispersant (c1) was changed to water (d1), but the inorganic particles settled and the inorganic particles A dispersed slurry could not be obtained.
＜比較例２＞
分散剤（ｃ６）を水（ｄ１）に変更したこと以外、実施例１９と同様にして、比較用の無機粒子分散スラリー（２５）の調製を試みたが、全体が固化したため無機粒子分散スラリーを得ることができなかった。
<Comparative example 2>
An attempt was made to prepare an inorganic particle-dispersed slurry (25) for comparison in the same manner as in Example 19 except that the dispersant (c6) was changed to water (d1). I couldn't get it.
＜比較例３＞
分散剤（ｃ６）１部を比較用の分散剤（ｃ１４）１．４部に変更し、水（ｄ１）３７．５部を３７．１部に変更したこと以外、実施例１９と同様にして、比較用の無機粒子分散スラリー（２６）の調製を試みたが、全体が固化したため無機粒子分散スラリーを得ることができなかった。
<Comparative example 3>
Similar to Example 19 except that 1 part of the dispersant (c6) was changed to 1.4 parts of the comparative dispersant (c14) and 37.5 parts of water (d1) was changed to 37.1 parts. , An attempt was made to prepare an inorganic particle-dispersed slurry (26) for comparison, but an inorganic particle-dispersed slurry could not be obtained because the whole was solidified.
＜比較例４＞
分散剤（ｃ３）を水（ｄ１）に変更したこと以外、実施例２７と同様にして、比較用の無機粒子分散スラリー（２７）の調製を試みたが、全体が固化したため無機粒子分散スラリーを得ることができなかった。
<Comparative example 4>
An attempt was made to prepare an inorganic particle-dispersed slurry (27) for comparison in the same manner as in Example 27 except that the dispersant (c3) was changed to water (d1). I couldn't get it.
＜比較例５＞
分散剤（ｃ３）１部を比較用の分散剤（ｃ１４）１．４部に変更したこと及び水（ｄ１）３７．５部を３７．１部に変更したこと以外、実施例２７と同様にして、比較用の無機粒子分散スラリー（２８）の調製を試みたが、全体が固化したため無機粒子分散スラリーを得ることができなかった。
<Comparative example 5>
Same as in Example 27 except that 1 part of the dispersant (c3) was changed to 1.4 parts of the comparative dispersant (c14) and 37.5 parts of water (d1) was changed to 37.1 parts. Therefore, an attempt was made to prepare an inorganic particle-dispersed slurry (28) for comparison, but an inorganic particle-dispersed slurry could not be obtained because the whole was solidified.
＜比較例６＞
分散剤（ｃ３）を水（ｄ１）に変更したこと以外、実施例３０と同様にして、比較用の無機粒子分散スラリー（２９）を得た。無機粒子分散スラリー（２９）中の無機粒子（ａ３０４）の個数平均粒子径は１．１μｍであった。
<Comparative Example 6>
An inorganic particle-dispersed slurry (29) for comparison was obtained in the same manner as in Example 30 except that the dispersant (c3) was changed to water (d1). The number average particle size of the inorganic particles (a304) in the inorganic particle dispersion slurry (29) was 1.1 μm.
＜比較例７＞
分散剤（ｃ３）１部を比較用の分散剤（ｃ１４）１．４部に変更し、水（ｄ１）３７．５部を３７．１部に変更したこと以外、実施例３０と同様にして、比較用の無機粒子分散スラリー（３０）を得た。無機粒子分散スラリー（３０）中の無機粒子（ａ３０５）の個数平均粒子径は０．７２μｍであった。
<Comparative Example 7>
Similar to Example 30, except that 1 part of the dispersant (c3) was changed to 1.4 parts of the comparative dispersant (c14) and 37.5 parts of water (d1) was changed to 37.1 parts. , Inorganic particle dispersion slurry (30) for comparison was obtained. The number average particle size of the inorganic particles (a305) in the inorganic particle dispersion slurry (30) was 0.72 μm.
＜比較例８＞
分散剤（ｃ８）を水（ｄ１）に変更したこと以外、実施例３５と同様にして、比較用の無機粒子分散スラリー（３１）の調製を試みたが、全体が固化したため無機粒子分散スラリーを得ることができなかった。
<Comparative Example 8>
An attempt was made to prepare an inorganic particle-dispersed slurry (31) for comparison in the same manner as in Example 35, except that the dispersant (c8) was changed to water (d1). I couldn't get it.
＜比較例９＞
分散剤（ｃ８）１部を比較用の分散剤（ｃ１４）１．４部に変更し、水（ｄ１）３７．５部を３７．１部に変更したこと以外、実施例３５と同様にして、比較用の無機粒子分散スラリー（３２）の調製を試みたが、全体が固化したため無機粒子分散スラリーを得ることができなかった。
<Comparative Example 9>
Similar to Example 35, except that 1 part of the dispersant (c8) was changed to 1.4 parts of the comparative dispersant (c14) and 37.5 parts of water (d1) was changed to 37.1 parts. , An attempt was made to prepare an inorganic particle-dispersed slurry (32) for comparison, but an inorganic particle-dispersed slurry could not be obtained because the whole was solidified.
＜流動性評価１＞
実施例１４〜２６及び３０〜３６で調製した無機粒子分散スラリー（１）〜（１３）及び（１７）〜（２３）並びに、比較例６及び７で調製した無機粒子スラリー（２９）及び（３０）について、ＢＭ型粘度計（ＶＩＳＣＯＭＥＴＥＲ ＴＶ−２０、東機産業株式会社、２５℃、６０ｒｐｍ）を用いて粘度（ｍＰａ・ｓ）を測定した。さらに、同スラリーのｐＨをマルチ水質計（ＭＭ−４３Ｍ、東亜ディーケーケー株式会社、２５℃）を用いて測定した。これらの結果を下表に示す。
<Liquidity evaluation 1>
Inorganic particle dispersion slurries (1) to (13) and (17) to (23) prepared in Examples 14 to 26 and 30 to 36, and inorganic particle slurries (29) and (30) prepared in Comparative Examples 6 and 7. ), The viscosity (mPa · s) was measured using a BM type viscometer (VISCOMETER TV-20, Toki Sangyo Co., Ltd., 25 ° C., 60 rpm). Further, the pH of the slurry was measured using a multi-water quality meter (MM-43M, DKK-TOA CORPORATION, 25 ° C.). These results are shown in the table below.
「−」は無機粒子分散スラリーが得られなかったことを意味する。
"-" Means that the inorganic particle dispersion slurry was not obtained.
＜流動性評価２＞
実施例２７〜２９で調製した無機粒子分散スラリー（１４）〜（１６）について、Ｅ型粘度計（ＲＥ８０型、東機産業株式会社、２５℃、１０ｒｐｍ）を用いて粘度（ｍＰａ・ｓ）を測定した。さらに、同スラリーのｐＨをマルチ水質計（ＭＭ−４３Ｍ、東亜ディーケーケー株式会社、２５℃）を用いて測定した。これらの結果を下表に示す。
<Liquidity evaluation 2>
The viscosity (mPa · s) of the inorganic particle dispersion slurries (14) to (16) prepared in Examples 27 to 29 was measured using an E-type viscometer (RE80 type, Toki Sangyo Co., Ltd., 25 ° C., 10 rpm). It was measured. Further, the pH of the slurry was measured using a multi-water quality meter (MM-43M, DKK-TOA CORPORATION, 25 ° C.). These results are shown in the table below.
実施例で調製した無機粒子分散スラリーは、比較例で調製した無機粒子分散スラリーに比べて、ｐＨ（２５℃）が１〜６であっても優れた流動性であった。そして、本発明の分散剤は、ｐＨ（２５℃）が１〜６である無機粒子分散スラリーに適用した場合でも優れた流動性を発揮した。 The inorganic particle-dispersed slurry prepared in the examples had excellent fluidity even at a pH (25 ° C.) of 1 to 6 as compared with the inorganic particle-dispersed slurry prepared in the comparative example. The dispersant of the present invention exhibited excellent fluidity even when applied to an inorganic particle dispersion slurry having a pH (25 ° C.) of 1 to 6.
Claims (3)
ｐＨ（２５℃）が１〜６であり、
分散剤（Ｃ）がアリルアミン（塩）、ジアリルアミン（塩）、Ｎ−ビニルイミダゾール（塩）及びＮ−ビニルピロリドンからなる群より選ばれる少なくとも１種を必須構成単量体としてなるポリマーを含有してなることを特徴とする無機粒子分散スラリー。 It contains inorganic particles (A), acid (B), dispersant (C) and water (D).
The pH (25 ° C) is 1-6,
The dispersant (C) contains a polymer in which at least one selected from the group consisting of allylamine (salt), diallylamine (salt), N-vinylimidazole (salt) and N-vinylpyrrolidone is an essential constituent monomer. Inorganic particle dispersion slurry characterized by becoming.
アリルアミン（塩）、ジアリルアミン（塩）、Ｎ−ビニルイミダゾール（塩）及びＮ−ビニルピロリドンからなる群より選ばれる少なくとも１種を必須構成単量体としてなるポリマーを含有してなることを特徴とする分散剤。 A dispersant for an inorganic particle dispersion slurry containing inorganic particles (A), acid (B), dispersant (C) and water (D) and having a pH (25 ° C.) of 1 to 6.
It is characterized by containing a polymer containing at least one selected from the group consisting of allylamine (salt), diallylamine (salt), N-vinylimidazole (salt) and N-vinylpyrrolidone as an essential constituent monomer. Dispersant.
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| JP2001293872A (en) * | 2000-04-14 | 2001-10-23 | Minolta Co Ltd | Ink jet printer, ink for ink jet printer, and ink jet printing method |
| JP2013043893A (en) * | 2011-08-22 | 2013-03-04 | Jsr Corp | Aqueous dispersion for chemical and mechanical polishing and chemical and mechanical polishing method using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2001293872A (en) * | 2000-04-14 | 2001-10-23 | Minolta Co Ltd | Ink jet printer, ink for ink jet printer, and ink jet printing method |
| JP2013043893A (en) * | 2011-08-22 | 2013-03-04 | Jsr Corp | Aqueous dispersion for chemical and mechanical polishing and chemical and mechanical polishing method using the same |
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