TW200803959A - Defoaming agent composition - Google Patents
Defoaming agent composition Download PDFInfo
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- TW200803959A TW200803959A TW096105962A TW96105962A TW200803959A TW 200803959 A TW200803959 A TW 200803959A TW 096105962 A TW096105962 A TW 096105962A TW 96105962 A TW96105962 A TW 96105962A TW 200803959 A TW200803959 A TW 200803959A
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- TW
- Taiwan
- Prior art keywords
- group
- mass
- organic
- polyoxyalkylene
- iii
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 56
- 239000002518 antifoaming agent Substances 0.000 title abstract description 35
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 13
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 13
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920000642 polymer Polymers 0.000 claims abstract description 11
- 125000003545 alkoxy group Chemical group 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 8
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 7
- 125000002462 isocyano group Chemical group *[N+]#[C-] 0.000 claims abstract description 4
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 claims abstract description 3
- 125000001183 hydrocarbyl group Chemical group 0.000 claims abstract 6
- -1 polysiloxane Polymers 0.000 claims description 34
- 239000000843 powder Substances 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 18
- 125000004432 carbon atom Chemical group C* 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 9
- 150000001721 carbon Chemical class 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- 125000000962 organic group Chemical group 0.000 claims description 7
- 239000013530 defoamer Substances 0.000 claims description 6
- 125000000219 ethylidene group Chemical group [H]C(=[*])C([H])([H])[H] 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 3
- 230000006866 deterioration Effects 0.000 abstract description 3
- 238000004381 surface treatment Methods 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 229920002545 silicone oil Polymers 0.000 abstract 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 17
- 229910000420 cerium oxide Inorganic materials 0.000 description 16
- 238000005187 foaming Methods 0.000 description 16
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 16
- 239000003921 oil Substances 0.000 description 15
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- 150000002430 hydrocarbons Chemical group 0.000 description 12
- 235000014113 dietary fatty acids Nutrition 0.000 description 10
- 239000000194 fatty acid Substances 0.000 description 10
- 229930195729 fatty acid Natural products 0.000 description 10
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 6
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 6
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 4
- 125000003342 alkenyl group Chemical group 0.000 description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 4
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000010730 cutting oil Substances 0.000 description 4
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 4
- 239000001508 potassium citrate Substances 0.000 description 4
- 229960002635 potassium citrate Drugs 0.000 description 4
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 4
- 235000011082 potassium citrates Nutrition 0.000 description 4
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- SZIFAVKTNFCBPC-UHFFFAOYSA-N 2-chloroethanol Chemical compound OCCCl SZIFAVKTNFCBPC-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 229910002012 Aerosil® Inorganic materials 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 125000000753 cycloalkyl group Chemical group 0.000 description 3
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 230000001804 emulsifying effect Effects 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- 229920002098 polyfluorene Polymers 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 125000003944 tolyl group Chemical group 0.000 description 3
- 125000001731 2-cyanoethyl group Chemical group [H]C([H])(*)C([H])([H])C#N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 125000002947 alkylene group Chemical group 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 125000004106 butoxy group Chemical group [*]OC([H])([H])C([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 2
- 239000004359 castor oil Substances 0.000 description 2
- 235000019438 castor oil Nutrition 0.000 description 2
- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 125000004218 chloromethyl group Chemical group [H]C([H])(Cl)* 0.000 description 2
- 125000004093 cyano group Chemical group *C#N 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 2
- 125000005843 halogen group Chemical group 0.000 description 2
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 125000006038 hexenyl group Chemical group 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 125000005504 styryl group Chemical group 0.000 description 2
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 1
- 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 1
- FJKROLUGYXJWQN-UHFFFAOYSA-M 4-hydroxybenzoate Chemical compound OC1=CC=C(C([O-])=O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-M 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- 235000014443 Pyrus communis Nutrition 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- ABBQHOQBGMUPJH-UHFFFAOYSA-M Sodium salicylate Chemical compound [Na+].OC1=CC=CC=C1C([O-])=O ABBQHOQBGMUPJH-UHFFFAOYSA-M 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- DHXVGJBLRPWPCS-UHFFFAOYSA-N Tetrahydropyran Chemical compound C1CCOCC1 DHXVGJBLRPWPCS-UHFFFAOYSA-N 0.000 description 1
- 235000010724 Wisteria floribunda Nutrition 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 125000004450 alkenylene group Chemical group 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000005037 alkyl phenyl group Chemical group 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 229960004365 benzoic acid Drugs 0.000 description 1
- 125000004369 butenyl group Chemical group C(=CCC)* 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- SURLGNKAQXKNSP-DBLYXWCISA-N chlorin Chemical compound C\1=C/2\N/C(=C\C3=N/C(=C\C=4NC(/C=C\5/C=CC/1=N/5)=CC=4)/C=C3)/CC\2 SURLGNKAQXKNSP-DBLYXWCISA-N 0.000 description 1
- DIOQZVSQGTUSAI-NJFSPNSNSA-N decane Chemical compound CCCCCCCCC[14CH3] DIOQZVSQGTUSAI-NJFSPNSNSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- UTBDYLQPXTWUDG-UHFFFAOYSA-N ethene;octadecanoic acid Chemical compound C=C.CCCCCCCCCCCCCCCCCC(O)=O UTBDYLQPXTWUDG-UHFFFAOYSA-N 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 125000006125 ethylsulfonyl group Chemical group 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- DIOQZVSQGTUSAI-UHFFFAOYSA-N n-butylhexane Natural products CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- QEHKBHWEUPXBCW-UHFFFAOYSA-N nitrogen trichloride Chemical compound ClN(Cl)Cl QEHKBHWEUPXBCW-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000004302 potassium sorbate Substances 0.000 description 1
- 235000010241 potassium sorbate Nutrition 0.000 description 1
- 229940069338 potassium sorbate Drugs 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 150000003304 ruthenium compounds Chemical class 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 229960003885 sodium benzoate Drugs 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 229960005076 sodium hypochlorite Drugs 0.000 description 1
- 229960004025 sodium salicylate Drugs 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 239000001587 sorbitan monostearate Substances 0.000 description 1
- 235000011076 sorbitan monostearate Nutrition 0.000 description 1
- 229940035048 sorbitan monostearate Drugs 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000006276 transfer reaction Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
- A47K—SANITARY EQUIPMENT NOT OTHERWISE PROVIDED FOR; TOILET ACCESSORIES
- A47K7/00—Body washing or cleaning implements
- A47K7/02—Bathing sponges, brushes, gloves, or similar cleaning or rubbing implements
- A47K7/03—Bathing sponges, brushes, gloves, or similar cleaning or rubbing implements containing soap or other cleaning ingredients, e.g. impregnated
-
- A—HUMAN NECESSITIES
- A47—FURNITURE; DOMESTIC ARTICLES OR APPLIANCES; COFFEE MILLS; SPICE MILLS; SUCTION CLEANERS IN GENERAL
- A47K—SANITARY EQUIPMENT NOT OTHERWISE PROVIDED FOR; TOILET ACCESSORIES
- A47K10/00—Body-drying implements; Toilet paper; Holders therefor
- A47K10/24—Towel dispensers, e.g. for piled-up or folded textile towels; Toilet paper dispensers; Dispensers for piled-up or folded textile towels provided or not with devices for taking-up soiled towels as far as not mechanically driven
- A47K10/32—Dispensers for paper towels or toilet paper
- A47K10/42—Dispensers for paper towels or toilet paper dispensing from a store of single sheets, e.g. stacked
- A47K10/421—Dispensers for paper towels or toilet paper dispensing from a store of single sheets, e.g. stacked dispensing from the top of the dispenser
-
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Abstract
Description
200803959 (1) 九、發明說明 【發明所屬之技術領域】 本發明係關於發泡液，尤其是關於鹼性之內添於發泡 液後，即使長期保存亦少有性能之隨時間劣化之聚矽氧系 之去泡劑組成物。 【先前技術】 Φ 聚矽氧系去泡劑，與其他之去泡劑比較因具有各種優 異性質，故在伴隨化學工業，食品工業，石油工業，織物 工業，製紙工業，紙漿工業或醫藥品工業等發泡之步驟中 被廣泛使用，例如在將二甲基聚矽氧烷，甲基苯基聚矽氧 烷，甲基乙烯聚矽氧烷等聚矽氧油與微粉末二氧化矽混合 之油複合物（oil compound)型去泡劑，將該等油複合物與 界面活性劑一起分散於水中所成乳液型去泡劑則被廣泛使 用。但是，此乳液型去泡劑，在高溫，高鹼性，高剪斷力 φ 等的過苛條件下乳化粒子被破壞，由於會有去泡能力降低 之問題，而作爲此之替代之物，則有關於以聚氧化烯烴基 所改性之有機聚矽氧烷與油-複合物加以倂用之自我乳化型 去泡劑〔特公昭5 1 -7 1 8 86.號，特公昭54-43 0 1 5號，特公 * 昭52- 1 983 6號，特公昭52-2263 8號，特公昭55-23 084號 公報（專利文獻1〜5)〕之提案被發表。 但是’該等聚砂氧系去泡劑，在與發泡液長時間接觸 下，會有去泡性能降低，分離·沈澱物發生等問題產生， 此種問題在發泡液爲鹼性之情形尤其顯著。 -5- 200803959 (2) 又，在伴隨發泡之步驟經過長時間之情形，於經時變 化下，去泡性能與初期比較因降低，故追加去泡劑並添加 成爲必要，而有生產率降低，或因去泡劑之多量添加所致 各種不便產生。 爲改善該等問題，使得去泡性能更爲提高則有各種提 μ 案被發表，可例舉例如將使用於油複合物之二氧化矽預先 以氯矽烷等疏水化準備之方法（特公昭52-3 1836號公報： φ 專利文獻6)，使二氧化矽以含氮有機矽化合物處理之方法 .(特公昭5 1 -3 5 5 5 6號公報：專利文獻7)等，然而其特性之 更加提高則爲所求。 〔專利文獻1〕特公昭5 1 -7 1 8 86號公報 〔專利文獻2〕特公昭54-430 1 5號公報 〔專利文獻3〕特公昭52- 1 9 836號公報 〔專利文獻4〕特公昭52-22638號公報 〔專利文獻5〕特公昭5 5-23 084號公報 φ 〔專利文獻6〕特公昭52-3 1 836號公報 〔專利文獻7〕特公昭5 1 -3 5 5 5 6號公報200803959 (1) IX. INSTRUCTIONS OF THE INVENTION [Technical Fields According to the Invention] The present invention relates to a foaming liquid, and in particular, to a foaming liquid which is added to a foaming liquid after alkali, even if it is stored for a long period of time, there is little performance degradation with time. A defoaming defoamer composition. [Prior Art] Φ Polyoxane defoamer, compared with other defoamers, has various excellent properties, so it is associated with the chemical industry, food industry, petroleum industry, fabric industry, paper industry, pulp industry or pharmaceutical industry. It is widely used in the step of foaming, for example, mixing polyoxyxane oil such as dimethyl polyoxyalkylene, methylphenyl polyoxyalkylene or methylvinyl polyoxyalkylene with fine powder of cerium oxide. An oil compound type defoaming agent which is widely used as an emulsion type defoaming agent which is dispersed in water together with a surfactant. However, in the emulsion type defoaming agent, the emulsified particles are destroyed under excessively high conditions such as high temperature, high alkalinity, high shearing force φ, and the like, as a substitute for the defoaming ability, There is a self-emulsifying defoaming agent for the use of an organopolyoxane modified with a polyoxyalkylene group and an oil-complex. [Special Proclamation 5 1 -7 1 8 86., Special Gong Sho 54-43 Proposal No. 0 1 5, No. 4, No. 5, No. 983, No. 5, No. 983, No. 52-2263, and No. Sho 55-23 084 (Patent Documents 1 to 5). However, in the case of such a polyoxo-based defoaming agent, when it is in contact with the foaming liquid for a long period of time, there are problems such as a decrease in defoaming performance and a problem such as separation and precipitation, and the problem is that the foaming liquid is alkaline. Especially remarkable. -5- 200803959 (2) In addition, when the step of foaming has passed for a long period of time, the defoaming performance is lowered as compared with the initial period due to the change over time. Therefore, it is necessary to add a defoaming agent and add it, and the productivity is lowered. Or inconvenience caused by the addition of a large amount of defoaming agent. In order to improve the problem, the defoaming performance is further improved, and various types of preparations have been disclosed. For example, a method of hydrophobizing a cerium oxide used in an oil compound in advance is prepared by using a chlorin or the like. -3 1836: φ Patent Document 6), a method in which ruthenium dioxide is treated with a nitrogen-containing organic ruthenium compound, etc. (Japanese Patent Publication No. 5 1 -3 5 5 5 6: Patent Document 7), etc. If you improve even more, you will be asked for it. [Patent Document 1] Japanese Laid-Open Patent Publication No. Hei. No. Hei. No. Hei. No. Hei. Japanese Laid-Open Patent Publication No. Hei. No. 5-5-23 084 (Patent Document 6) Japanese Patent Publication No. 52-3 No. 836 (Patent Document 7) Japanese Patent Publication No. 5 1 -3 5 5 5 6 Bulletin
W 【發明內容】 ^ 〔發明揭示〕 〔發明欲解決課題〕 本發明係鑑於上述情事而完成者，其目的在於提供一 種發泡液，尤其是內添於鹼性之發泡液後，即使長期保存 則少有分離·沈澱物之發生或去泡性能之隨時間劣化，又 -6- 200803959 (3) 爲去泡持續性優異之去泡劑組成物。 〔解決課題之手段〕 本發明人等’爲達成上述目的經一再重複戮力檢討， 結果首先發現以有機聚矽氧烷經表面處理之微粉末二氧化 • 砂與具有特定物性之有機聚矽氧烷之混合物在鹼性觸媒存 在下予以處理所得聚矽氧油複合物，含有具有特定構造及 φ 物性之聚氧乙烯改性有機聚矽氧烷及水，進而依需要含有 ’具有特定構造及物性之聚氧化烯烴改性有機聚矽氧烷， 聚氧化烯烴聚合物，非離子性界面活性劑之去泡劑組成物 ’發泡液，尤其是相對於鹼性發泡液爲內添穩定性及去泡 持續性優異者，因而完成本發明。 因此，本發明係提供一種，含有： (A)使下述⑴〜（iii)成分於室溫〜200°C進行混合處理 ，依需要進行中和及/或低沸點餾份之除去所得聚矽氧油 φ 複合物：1〜4 0質量％ (i) 25°C中黏度爲10〜1 00,000mm2/s之本質上疏水性的有 機聚矽氧烷：100質量份 (ii) 以有機聚矽氧烷經表面處理之微粉末二氧化矽·· 1〜20 ‘ 質量份 (iii) 鹼性觸媒：0.01〜5質量份 (B)下述一般式⑴ R12R3Si〇-(R12SiO)x-(R1R2SiO)y-SiRl2R3 ⑴ 200803959 (4) [式中，R1互爲同種或不同種之取代或者非取代之碳數1 〜18之一價烴基，R2爲下述一般式（II) -R4-0(CH2CH20)a-(CH2(CH3)CH0)b-R5 (II)[Explanation] ^ [Disclosure of the Invention] [Problem to be Solved by the Invention] The present invention has been made in view of the above circumstances, and an object thereof is to provide a foaming liquid, particularly after being added to an alkaline foaming liquid, even if it is long-term There is little separation, precipitation, or defoaming performance deterioration over time, and -6-200803959 (3) is a defoaming agent composition excellent in defoaming durability. [Means for Solving the Problem] The inventors of the present invention have repeatedly reviewed the results of the above-mentioned purposes. The results firstly found that the micro-powder dioxide and the organic poly-oxygen with specific physical properties were treated with an organic polysiloxane. The polyoxo-oxygen oil compound obtained by treating the mixture of the alkane in the presence of a basic catalyst contains a polyoxyethylene-modified organopolyoxane having a specific structure and φ physical properties, and water, and further contains 'specific structure and Physical properties of polyalkylene oxide modified organopolyoxane, polyoxyalkylene polymer, nonionic surfactant defoamer composition 'foaming liquid, especially for the internal foaming solution And the excellent defoaming persistence, thus completing the present invention. Therefore, the present invention provides a method comprising: (A) mixing the following components (1) to (iii) at room temperature to 200 ° C, and if necessary, neutralizing and/or removing the low-boiling fraction; Oxygen oil φ composite: 1 to 40% by mass (i) Organic hydrophobic polysiloxane having a viscosity of 10 to 1 00,000 mm 2 /s at 25 ° C: 100 parts by mass (ii) with organic polyfluorene Oxane surface-treated fine powder ceria · 1~20 ' parts by mass (iii) basic catalyst: 0.01 to 5 parts by mass (B) the following general formula (1) R12R3Si〇-(R12SiO)x-(R1R2SiO y-SiRl2R3 (1) 200803959 (4) wherein R1 is a substituted or unsubstituted carbon number of 1 to 18, and R2 is a general formula (II)-R4-0 ( CH2CH20)a-(CH2(CH3)CH0)b-R5 (II)
(式中，R4爲碳數2〜6之二價烴基，r5爲選自氫原子或碳 數1〜6之烷基，乙醯基及異氰基之一價有機基，a及b爲 3 ga + bg 80，且滿足a/b = 2/8〜8/2之正數）所示之一價有機 基’ R3爲R1，R2，羥基或碳數1〜6之烷氧基，X爲5〜 2Q() ’ y爲1〜3〇之整數]。 所示之25°c中黏度爲10〜1 0,000mm2/s之聚氧化烯烴改性 有機聚矽氧烷之1種或2種以上之混合物·· 〇〜3 0質量％ (C)下述一般式（III) R62R8SiO-(R62SiO)m-(R6R7SiO)n-SiR62R8 (III) [式中’ R6互爲同種或不同種之取代或者非取代之碳數！ 〜18之一價烴基，R7爲下述一般式（IV) 'R9-0(CH2CH2〇)c-R10 (IV) [式中，R9爲碳數2〜6之二價烴基，R1()爲選自氫原子或 碳數1〜6之烷基，乙醯基及異氰基之一價有機基，R8爲 -8 - 200803959 (5) R6，R7，羥基或碳數1〜6之烷氧基，C爲3〜50之正數， m爲5〜200之整數，η爲1〜30之整數]。 所示之聚氧乙烯改性有機聚矽氧烷之1種或2種以上之混 合物：1〜40質量％ (D)聚氧化烯烴聚合物之1種或2種以上之混合物：0〜40 * 質量％ (Ε)非離子性界面活性劑之1種或2種以上之混合物：0〜 φ 2 0質量％ (F)水：剩餘部分 爲其特徵之去泡劑組成物。 〔發明效果〕 本發明之去泡劑組成物，在內添於發泡液後，即使長 期保存亦少有性能之隨時間劣化，而爲去泡持續性優異者 〔實施發明之最佳型態〕 構成本發明之去泡劑組成物之（Α)成分之聚矽氧油複 合物，係作爲對此組成物賦予去泡性用之主成分者，本質 上係疏水性之有機聚矽氧烷（i)，與以有機聚矽氧烷經表面 處理之微粉末二氧化矽（Π)爲主成分，將該等於鹼性觸媒 (iii)之存在下進行處理所得者。 使用於（A)成分之有機聚矽氧烷（i)，本質上爲疏水性 之物。在此，本質上疏水性係指，即使在一部份官能基含 -9- 200803959 (6) 有親水性基但有機聚矽氧烷全體則顯示疏水性者。 本質上疏水性之有機聚矽氧烷（i)可爲直鏈狀或爲分支 鏈狀之物，尤以下述平均組成式（V)所示者爲恰當。 R1 ^810(4^)/2 (V) 上述式（V)中，R11係取代或者非取代之碳數丨〜18之 φ 一價烴基，該等可爲相同或相異。R11之一價烴基方面， 具體而3 ’可例舉甲基’乙基，丙基，丁基，戊基，己基 ’庚基’半基，壬基，癸基，十二基，十三基，十四基， 十六基，十八基等之烷基，環己基等之環烷基，乙烯基， 烯丙基等之鏈烯基，苯基，甲苯基等之芳基，苯乙烯基， α -甲基苯乙烯基等之芳烷基等，或將鍵結於該等基之碳原 子的氫原子一部份或全部以鹵原子，氰基，胺基，經基等 所取代之氯甲基，3-氯丙基，·3,3,3-三氟丙基，氰乙基， 馨 3 -胺基丙基，Ν-(β -胺基乙基）-γ -胺基丙基等，而就去泡性 及經濟性之面觀之以全R11之8〇莫耳％以上，尤其是90 莫耳％以上爲甲基者爲佳。又，Ρ爲1·9^ρ^2·2，較佳爲 1·95$ρ^2·15之正數。此外，有機聚矽氧烷之末端，可以 R^sSi-所示之三有機單矽烷基所封端，亦可以HORi'Si·· 所示二有機羥基單矽烷基所封端。 此本質上疏水性之有機聚矽氧烷（i)之以奧氏（ostwald) 黏度計測定之於25 °C中之黏度’就以去泡性，作業性之面 而言以 1 〇 〜1 00,000mm2/s，較佳爲 50 〜I0,000inm2/s。在 -10- 200803959 (7) 未達10mm2/s時去泡性能劣化，超過1 00,000mm2/s時聚 矽氧油複合物之黏度增大使得作業性惡化。 一方面，以有機聚矽氧烷經表面處理之微粉末二氧化 矽（ii)，例如，雖可藉由將微粉末二氧化矽原粉以下述組 成式（VI)所示之有機聚矽氧烷進行表面處理而得，然而亦 * 可使用市售之物。 _ R122R13SiO_(R122SiO)w-SiR122R13 (VI) 上述式（VI)中，R12互爲同種或不同種之碳數1〜18 之一價烴基，具體言之，可例舉甲基，乙基，丙基，丁基 ，戊基，己基，庚基，辛基，壬基，癸基，十二基，十三 基’十四基，十六基，十八基等之烷基，環己基等之環烷 基，苯基，甲苯基等之芳基等，而就去泡性及經濟性而言 以全R12之80莫耳％以上，尤其是90莫耳％以上爲甲基較 # 佳。R13係R12 ’羥基或甲氧基，乙氧基，丙氧基，丁氧基 等碳數1〜6之烷氧基。又，w係以有機聚矽氧烷之奧氏 (ostwald)黏度計測定之25°C中-之黏度，自作業性觀之，較 佳爲10〜l，000mm2/s’更佳爲20〜100mni2/s之數。 微粉末二氧化矽原粉可爲周知之物，可爲濕式二氧化 矽’乾式二氧化矽之任一種。在該等微粉末二氧化矽原粉 方面，可例舉沈澱二氧化矽，二氧化矽乾凝膠（xer〇gel)， 煙燻（fumed)二氧化矽等，具體言之可例舉 Nipsil(T〇s〇hSilica 公司製），SYLYSIA(富士 Silysia 化學 200803959 (8) 公司製），Aerosil(日本Aerosil公司製）等之市售品。又， 以BET法所計算之比表面積爲100m2/g以上700m2/g以下 ，尤以150m2/g以上5 00m2/g以下之物爲佳。 微粉末二氧化矽之表面處理可以周知之方法，例如， 使用Henschel混合機，樂帝克混合機（Loedige Mixer)，高 ' 速機 （high-speeder)等之混合·分散裝置來進行，在上述 裝置裝入微粉末二氧化矽原粉，在攪拌前或一邊攪拌一邊 φ 藉由有機聚矽氧烷之噴霧來製造。依需要可進行加熱，氨 水等鹼性觸媒之添加。在此情形，較佳爲於室溫〜1 00 °c ，尤其是在50〜80 °c經1〇分〜2小時，尤其是進行15分 〜1小時之處理爲所望。 此外，相對於微粉末二氧化矽之表面處理劑（有機聚 矽氧烷）量，因微粉末二氧化矽之比表面積而異，而BET 比表面積在100〜700m2/g相對於微粉末二氧化矽100質 量份爲1〜50質量份，較佳爲5〜30質量份。 φ 以有機聚矽氧烷經表面處理之微粉末二氧化矽（Π)之 添加量，相對於有機聚矽氧烷（i) 100質量份爲1〜20質量 份，較佳爲5〜15質量份。添加量在未達1質量份時，去 泡性能劣化，若比20質量份更多時，聚矽氧油複合物之 * 黏度增加，使得作業性惡化。 又，本發明之（A)成分所使用之鹼性觸媒（iii)，可爲聚 矽氧烷之轉移反應所使用之周知鹼性觸媒，例如鹼金屬或 鹼土類金屬之氧化物，氫氧化物，醇鹽或矽酸鹽 (SILICONATE)等，較佳爲矽酸鉀及氫氧化鉀。 -12- 200803959 (9) 鹼性觸媒（iii)之使用量，相對於有機聚矽氧烷（i)100 質量份爲0 · 0 1〜5質量份，較佳爲0.1〜3質量份。在未達 〇·〇1質量份時作爲觸媒之效果弱，即使超過5質量份之量 亦無法使觸媒之效果提高，在成本上爲不利。 又，本發明（A)成分之聚矽氧油複合物，係使用本質 ' 上疏水性之有機聚矽氧烷（i)與以上述有機聚矽氧烷經表面 處理之微粉末二氧化矽（ii)與鹼性觸媒（iii)之設定量，於 φ 室溫〜200°C，較佳爲 100〜200°C，更佳爲 150〜200°C之 溫度進行混合處理之後，可因應需要藉由中和及/或低沸 點餾份之除去來製造。 此外，混合處理時間以1 0分〜5小時，尤以1〜3小 時爲佳。又，混合處理以在氮等惰性氛圍下進行爲佳。 中和可使用2-氯乙醇，甲酸，乙酸等有機酸，稀鹽酸 ，稀硫酸等無機酸等來進行。又，低沸點餾份之除去，可 以減壓餾除等方法來進行。 φ 本發明之去泡劑組成物中，上述聚矽氧油複合物（A) 之含量，爲去泡劑組成物全體之1〜40質量％，較佳爲5 〜30質量％。含量比1質量％更少時，則去泡性能並非充 分，若比40質量％更多時製品之穩定性及內添穩定性則惡 ’ 化。 (B)成分之聚氧化烯烴改性有機聚矽氧烷，係將前述 聚矽氧油複合物予以乳化分散用之物，係以下述一般式（I) 所示。 200803959 (10) R12R3SiO-(Rl2SiO)x«(R1R2si〇)y-SiRl2R3 (I) 上述式（I)中’ R1互爲同種或不同種之取代或者非取 代之碳數1〜1 8之一價烴基，具體言之，可例舉甲基，乙 基，丙基，丁基，戊基，己基，庚基，辛基，壬基，癸基 、，十二基，十三基’十四基，十六基，十八基等烷基，環 己基等之環烷基，乙烯基，烯丙基等之鏈烯基，苯基，甲 φ 苯基等之芳基，苯乙烯基，α-甲基苯乙烯基等之芳烷基等 ’或將鍵結於該等基之碳原子的氫原子一部份或全部以鹵 原子，氰基，胺基等取代之氯甲基，3 -氯丙基，3，3,3 -三 氟丙基，氰乙基，3-胺基丙基，Ν-(β-胺基乙基）-γ-胺基丙 基等之一價烴基。 又’ R2係下述一般式（II)所示之聚氧化烯烴基。 -R4,0(CH2CH20)a，（CH2(CH3)CH0)b-R5 (II) 上述式（II)中，R4爲碳數2〜6之二價烴基，可例舉烷 撐基，亞鏈烯基等，可例舉例如乙烯基，丙烯基，丁#基 ，戊烯基，己烯基等。又，R5爲氫原子，碳數1〜6之烷 ’ 基，乙醯基或異氰基，烷基方面可例舉甲基，乙基，丙基 ，丁基，戊基等。a及 b 爲 3Sa + bS80，較佳爲 5$a + b$60，且 a/b = 2/8 〜8/2，較佳爲可滿足 a/b = 2.5/7.5 〜7.5/2.5之正數。 一方面，R3係與R1或者R2同樣之基，羥基或碳數1 -14- 200803959 (11) 〜6之烷氧基，具體言之以該R1及R2而例示之基，烷氧 基方面，可例舉甲氧基，乙氧基，丙氧基，丁氧基等。 此外，上述式（I)中之X爲5〜200，較佳爲20〜150 之整數，y爲1〜30，較佳爲1〜20之整數。 * 此聚氧化烯烴改性有機聚矽氧烷，可爲單獨1種’亦 ， 可使用2種以上之混合物，而以奧氏（ostwald)黏度計所測 定之 25°C中之黏度，爲1〇〜1〇,〇〇〇1111112/3，較佳爲50〜 8,000mm2/s，更佳爲 500 〜5,000mm2/s 之物。 本發明之去泡劑組成物中，上述聚氧化烯烴改性有機 聚矽氧烷（B)之含量爲去泡劑組成物全體之0〜3 0質量％， 較佳爲1〜20質量％。含量超過30質量％時組成物之去泡 特性則惡化。 (C)成分之聚氧乙烯改性有機聚矽氧烷，係用來使去 泡劑組成物之內添穩定性，保存穩定性，稀釋穩定性，高 溫穩定性，去泡性提高之物， φ 以下述一般式（ΙΠ)所示。 R62R8SiO-(R62SiO)m-(R6R7SiO)n-SiR62R8 (III) 上述式（III)中，R6係互爲同種或不同種之取代或者非 取代之碳數1〜1 8之一價烴基，具體言之可例舉以該R1 所例示之基，而就以去泡性及經濟性而言以全R6之80莫 耳％以上，尤以90莫耳％以上爲甲基者爲佳。 又，R7係下述一般式（IV)所示之聚氧乙烯基。 -15- 200803959 (12) -r9-o(ch2ch2o)c_r10 (IV) 上述式（IV)中，R9爲碳數2〜6之二價烴基，可例舉 烷撐基，亞鏈烯基等，可例舉例如乙烯基，丙烯基，丁烯 基，戊烯基，己烯基等。又，R1G可例舉氫原子，碳數1 〜6之烷基，乙醯基或異氰基，烷基方面可例舉甲基，乙 基，丙基，丁基，戊基等。c爲3〜5 0，較佳爲可滿足4〜 φ 3 0之正數。c比3更小時對內添穩定性，保存穩定性，稀 釋穩定性，高溫穩定性，去泡性會有不良影響。又，若比 5 〇更大時，熔點及熔融黏度變高，使得作業性，去泡性降 低。 一方面，R8係與R6或者R7同樣之基，羥基或碳數1 〜6之烷氧基，具體言之以該R6及R7例示之基，烷氧基 方面，可例舉甲氧基，乙氧基，丙氧基，丁氧基等。 此外，上述式（ΠΙ)中m爲 5〜200，較佳爲10〜150 • 之整數。m比200更大時乳化分散性降低，對內添穩定性 ，保存穩定性，稀釋穩定性，高溫穩定性，去泡性產生不 良影響。η爲1〜30，較佳爲1〜20之整數。 此聚氧乙烯改性有機聚矽氧烷，可單獨使用1種，亦 可使用2種以上之混合物。 本發明之去泡劑組成物中，上述聚氧乙烯改性有機聚 矽氧烷（C)之含量，爲去泡劑組成物全體之1〜40質量％， 較佳爲5〜2 0質量％。含量比1質量份更少時，則對穩定 性，去泡性之效果少，超過40質量％時，則去泡劑組成物 -16 - 200803959 (13) 之黏度變筒，水分散性變差。 此外’（B)成分之聚氧化烯烴改性有機聚矽氧烷及 成分之聚氧乙烯改性有機聚矽氧烷，例如，將含有Si-H 基之有機氫聚矽氧烷與分子鏈末端具有烯丙基等之脂肪族 不飽和基之聚氧化烯烴或聚氧乙烯化合物在鉑等觸媒之存 ~ 在下，進行加成反應而可得。 (D)成分之聚氧化烯烴聚合物，在本發明之去泡劑組 φ 成物中則成爲乳化助劑，故使用以下述一般式（VII)所示之 物爲恰當。 R140-(R150)z-R14 (VII) 上述式（VII)中，R14可例舉氫原子，或甲基，乙基， 丙基，丁基等之烷基，乙烯基，烯丙基等之鏈烯基，乙醯 基或硬脂醯基等之碳數1〜20，尤其是可例舉1〜18之一 φ 價有機基，該等可爲相同或相異。R15爲乙烯基，丙烯基 等之烷撐基等之碳數2〜6之二價烴基。在此情形，R15可 爲互爲相異之2種以上之基。 又，z係以此聚氧化烯烴聚合物之GPC所測定之聚苯 乙烯換算重量平均分子量，較佳爲5 0 0〜5，0 0 0，更佳爲 1，000〜4,000之數。在此，重量平均分子量未達500時所 得去泡劑組成物之乳化穩定性會有惡化之虞’超過5，0 0 0 時黏度變高而有作業性惡化之虞。此外’聚氧化烯烴聚合 物，可單獨使用1種，亦可使用2種以上之混合物。 -17 - 200803959 (14) 本發明之去泡劑組成物中，上述聚氧化烯烴聚合物 (D)之含量，爲去泡劑組成物全體之0〜40質量％，較佳爲 0〜20質量％。超過40質量％時去泡劑組成物之乳化特性 惡化。此外，配合之情形可成爲有效量，而以配合5質量 %以上爲佳。 * (E)成分之非離子性界面活性劑係用於將去泡成分[亦 即，（A)〜（D)成分]分散於水之物，但一般可爲周知之物， φ 例如山梨聚糖脂肪酸酯，甘油脂肪酸酯，聚甘油脂肪酸酯 ，丙二醇脂肪酸酯，蔗糖脂肪酸酯，聚乙二醇脂肪酸酯， 聚環氧乙烷醚，聚氧乙烯烷基苯基醚，聚環氧乙烷脂肪酸 酯，聚氧乙烯山梨聚糖脂肪酸酯，聚環氧乙烷甘油脂肪酸 酯’聚氧乙烯丙二醇脂肪酸酯，聚氧乙烯蓖麻油，聚氧乙 烯硬化蓖麻油等。 此外，本發明之去泡劑組成物中，此非離子性界面活 性劑，可單獨使用1種，亦可使用2種以上之混合物，其 • 含量爲〇〜20質量％，較佳爲1〜10質量％。在超過20質 量％時去泡劑組成物之黏度變高，作業性惡化。 在本發明之去泡劑組成物中，（F)成分係將上述（A)〜 (E)成分爲乳化而添加必要的水·爲必要，其量爲相對於（a) ’ 〜（E)各成分含有比率之合計的剩餘部分，較佳爲相對於 (A)〜（E)成分之合計1〇〇質量份添加50〜2,00〇質量份， 更佳爲80〜400質量份。 又，本發明之去泡劑組成物，係混合上述（A)〜（F)成 分之設定量，可因應必要一邊加熱，一邊以周知方法，例 -18- 200803959 (15) 如以均化混合器（homomixer)，均化器（homogenizer)，膠 體硏磨等之混合·分散機予以均一地攪拌·乳化而可調製’ 尤其是在使（A)〜（E)成分之設定量予以均一地混合·分散後 ，添加（F)成分之設定量之一部份，進行攪拌·乳化後進而 •添加殘留的（F)成分，予以均一地攪拌·混合，來調製去泡 ，劑組成物之方法爲佳。 再者，在本發明之去泡劑組成物，以防腐之目的可任 0 意添加少量保存料，殺菌料。在此保存料，殺菌料之具體 例方面，可例舉次氯酸鈉，山梨酸，山梨酸鉀，水楊酸’ 水楊酸鈉，苯甲酸，苯甲酸鈉，對羥基苯甲酯 (parahydroxybenzoate)類，異噻嗤啉化合物等。其添加量 相對於本發明之去泡劑組成物100質量份以0〜〇·5質量 份，尤以0.005〜0.5質量份爲佳。 如此所得本發明之去泡劑組成物，藉由發泡液，尤其 是添加於鹼性之發泡液，即使長期保存亦少有性能之隨時 φ 間劣化，可獲得內添穩定性及去泡持續性優異之物。此外 ，去泡劑組成物之添加量並無特別限定，相對於發泡液以 -添加0· 001〜3質量％，尤以添加0.01〜1質量％爲佳。又 ，鹼性之發泡液方面，可例示水性切削油，紙漿黑液 * (PULP BLACK LIQUOR)等。 【實施方式】 〔實施例〕 以下，例示實施例及比較例，具體說明本發明，但本 -19- 200803959 (16) 發明並非限制於下述實施例者。此外’下述例中，％示質 量％，黏度係以奧氏（ostwald)黏度計而測定之25°C中之値 [實施例1〜6，比較例1〜4] 下述（A)〜（E)成分係使用表1所示之量’加熱至70°C ，以均化器均一地混合後，緩緩添加（F)成分之水，來調 製去泡劑組成物。關於此組成物係藉由下述所示方法，來 評價去泡性，內添穩定性，製品穩定性。結果如表1所示 (A)聚矽氧油複合物[聚矽氧油複合物（a-1)] 本質上疏水性之有機聚矽氧烷係，黏度以8,000mm2/s ，CH3Si03/2單位爲含有0.01莫耳分率之分支鏈狀二甲基 聚矽氧烷100質量份，微粉末二氧化矽係將下述（甲）5質 φ 量份，鹼性觸媒係，氫氧化鉀含有3%之矽酸鉀3.3質量 份，在氮氛圍下於150°C，經3小時混合後，以2-氯乙醇 中和，接著將低沸點餾份除去之物。 [聚矽氧油複合物（a-2)] 本質上疏水性之有機聚矽氧烷係，黏度l〇,〇〇〇mm2/s 之二甲基聚矽氧烷100質量份，微粉末二氧化矽係下述（ 乙）1〇質量份，鹼性觸媒係使用含有氫氧化鉀3%之矽酸鉀 5質量份，在氮氛圍下於150°C，3小時混合後，以2-氯乙 -20- 200803959 (17) 醇中和，接著使低沸點餾份除去之物。 [聚矽氧油複合物（a-3)] 本質上疏水性之有機聚矽氧烷係以黏度8,000mm2/s， 使CH3Si03/2單位含有0·01莫耳分率之分支鏈狀二甲基聚 矽氧烷1〇〇質量份，微粉末二氧化矽係使用下述（甲）5質 量份，在氮氣體氛圍下於1 50 °C，經3小時混合者。(wherein R4 is a divalent hydrocarbon group having 2 to 6 carbon atoms, and r5 is an alkyl group selected from a hydrogen atom or a carbon number of 1 to 6, an ethylidene group and an isovalent organic group, and a and b are 3 Ga + bg 80, and satisfying a positive number of a/b = 2/8 to 8/2) The organic group 'R3 is R1, R2, a hydroxyl group or an alkoxy group having a carbon number of 1 to 6, X is 5 ~ 2Q() ' y is an integer from 1 to 3〇]. One or a mixture of two or more kinds of polyoxyalkylene-modified organopolyoxane having a viscosity of 10 to 10,000 mm 2 /s as shown in the above-mentioned 25 ° C. 〇 〜 30% by mass (C) Formula (III) R62R8SiO-(R62SiO)m-(R6R7SiO)n-SiR62R8 (III) [In the formula, R6 is the same or different kinds of substituted or unsubstituted carbon number! ～18 one-valent hydrocarbon group, R7 is the following general formula (IV) 'R9-0(CH2CH2〇)c-R10 (IV) [wherein, R9 is a divalent hydrocarbon group having a carbon number of 2 to 6, and R1() is It is selected from a hydrogen atom or an alkyl group having 1 to 6 carbon atoms, an acetyl group and an isovalent organic group, and R8 is -8 - 200803959 (5) R6, R7, a hydroxyl group or an alkoxy group having a carbon number of 1 to 6. Base, C is a positive number of 3 to 50, m is an integer of 5 to 200, and η is an integer of 1 to 30]. One or a mixture of two or more of the polyoxyethylene-modified organic polyoxyalkylenes shown: 1 to 40% by mass (D) one or a mixture of two or more kinds of polyoxyalkylene polymers: 0 to 40 * Mass% (Ε) One or a mixture of two or more kinds of nonionic surfactants: 0 to φ 2 0% by mass (F) Water: the remaining part of the defoaming agent composition. [Effect of the Invention] The defoamer composition of the present invention, after being added to the foaming liquid, has little performance deterioration over time even after long-term storage, and is excellent in defoaming durability (the best mode of the invention) The polyfluorene oxide oil composition constituting the (Α) component of the defoaming agent composition of the present invention is a hydrophobic organopolysiloxane which is a main component for imparting defoaming property to the composition. (i) It is obtained by treating the fine powder of cerium oxide (cerium) which is surface-treated with an organic polyoxyalkylene as a main component and treating it in the presence of the basic catalyst (iii). The organopolyoxane (i) used in the component (A) is substantially hydrophobic. Here, intrinsically hydrophobic means that even if a part of the functional group contains a hydrophilic group of -9-200803959 (6), the whole of the organopolyoxyalkylene shows hydrophobicity. The substantially hydrophobic organopolyoxane (i) may be linear or branched, and is particularly preferably represented by the following average composition formula (V). R1 ^ 810 (4^) / 2 (V) In the above formula (V), R11 is a substituted or unsubstituted φ monovalent hydrocarbon group having a carbon number of 丨 18 or more, and these may be the same or different. R11 is a monovalent hydrocarbon group, and specifically 3' may be exemplified by methyl 'ethyl, propyl, butyl, pentyl, hexyl'heptyl'-half group, fluorenyl, fluorenyl, dodecyl, thirteenthyl An alkyl group of a tetradecyl group, a hexadecyl group, an octadecyl group or the like, a cycloalkyl group such as a cyclohexyl group, an alkenyl group such as a vinyl group or an allyl group, an aryl group such as a phenyl group or a tolyl group, or a styryl group. An aralkyl group such as α-methylstyryl or the like, or a part or all of a hydrogen atom bonded to a carbon atom of the group is substituted with a halogen atom, a cyano group, an amine group, a group or the like. Chloromethyl, 3-chloropropyl, ·3,3,3-trifluoropropyl, cyanoethyl, octane 3-aminopropyl, Ν-(β-aminoethyl)-γ-aminopropyl Base, etc., and in terms of defoaming and economy, it is better to use more than 8% of all R11, especially 90% or more of methyl. Further, Ρ is 1·9^ρ^2·2, preferably a positive number of 1·95$ρ^2·15. Further, the terminal of the organopolyoxyalkylene may be blocked by a triorganomonoalkylene group represented by R^sSi- or may be blocked by a diorganohydroxymonoalkylene group represented by HORI'Si. The essentially hydrophobic organopolyoxane (i) has an viscosity determined by an ostwald viscometer at 25 ° C. It is defoamed, and the workability is 1 〇 to 1 00,000. Mm2/s, preferably 50 to I0,000 inm2/s. -10- 200803959 (7) The defoaming performance deteriorates when it is less than 10 mm 2 /s, and the viscosity of the polyoxygenated oil compound increases when it exceeds 100,000 mm 2 /s, which deteriorates workability. In one aspect, the surface-treated fine powder of cerium oxide (ii) is an organopolysiloxane, for example, by using the fine powder of cerium oxide as the organic polyoxygen oxide represented by the following composition formula (VI). The alkane is obtained by surface treatment, however, * commercially available materials can also be used. _ R122R13SiO_(R122SiO)w-SiR122R13 (VI) In the above formula (VI), R12 is a monovalent hydrocarbon group having the same or different carbon number of 1 to 18, and specifically, a methyl group, an ethyl group, and a C group. Base, butyl, pentyl, hexyl, heptyl, octyl, decyl, decyl, dodecyl, thirteenyl'tetradecyl, hexadecyl, octadecyl, etc., cyclohexyl, etc. An aryl group such as a cycloalkyl group, a phenyl group or a tolyl group, etc., and more than 80 mol% of the total R12 in terms of defoaming property and economic efficiency, especially 90 mol% or more is preferably a methyl group. R13 is an alkoxy group having 1 to 6 carbon atoms such as R12'hydroxy or methoxy, ethoxy, propoxy or butoxy. Further, w is a viscosity at 25 ° C measured by an ostwald viscometer of an organic polyoxane, and from the viewpoint of workability, preferably 10 to 1,000 mm 2 /s' is more preferably 20 to 100 mni 2 /s number. The fine powder of cerium oxide powder may be a well-known one, and may be any of wet cerium cerium lanthanum cerium. The fine powder of cerium oxide raw material may, for example, be precipitated cerium oxide, cerium dioxide dry gel (xer〇gel), fumed cerium oxide, etc., specifically, Nipsil ( Commercial products such as SYLYSIA (Fuji Silysia Chemicals 200203959 (8)), Aerosil (made by Nippon Aerosil Co., Ltd.), etc., are available from T〇s〇hSilica Co., Ltd.). Further, the specific surface area calculated by the BET method is preferably from 100 m 2 /g to 700 m 2 /g, more preferably from 150 m 2 /g to more than 500 m 2 /g. The surface treatment of the fine powder of cerium oxide can be carried out by a known method, for example, using a mixing/dispersing device such as a Henschel mixer, a Loedige Mixer, or a high-speeder. The apparatus was charged with a fine powder of cerium oxide as a raw material, and was sprayed by spraying of an organic polyoxane before or while stirring. Heating, addition of an alkaline catalyst such as ammonia can be carried out as needed. In this case, it is preferably at room temperature to 1 00 ° C, especially at 50 to 80 ° C for 1 Torr to 2 hours, especially for 15 minutes to 1 hour. Further, the amount of the surface treatment agent (organic polyoxymethane) relative to the fine powder of ceria is different depending on the specific surface area of the fine powder of ceria, and the BET specific surface area is 100 to 700 m 2 /g with respect to the micropowder. 100 parts by mass of 矽 is 1 to 50 parts by mass, preferably 5 to 30 parts by mass. φ The amount of the finely-treated cerium oxide (cerium) which is surface-treated with the organopolysiloxane is 1 to 20 parts by mass, preferably 5 to 15 parts by mass based on 100 parts by mass of the organopolysiloxane (i). Share. When the amount of addition is less than 1 part by mass, the defoaming performance is deteriorated, and when it is more than 20 parts by mass, the viscosity of the polyoxygenated oil composite increases, which deteriorates workability. Further, the basic catalyst (iii) used in the component (A) of the present invention may be a known basic catalyst used for the transfer reaction of polyoxyalkylene, such as an oxide of an alkali metal or an alkaline earth metal, hydrogen. Oxide, alkoxide or citrate (SILICONATE), etc., preferably potassium citrate and potassium hydroxide. -12- 200803959 (9) The amount of the basic catalyst (iii) to be used is 0.1 to 1 part by mass, preferably 0.1 to 3 parts by mass, per 100 parts by mass of the organopolysiloxane (i). When the amount is less than 1 part by mass, the effect as a catalyst is weak, and even if it exceeds 5 parts by mass, the effect of the catalyst cannot be improved, which is disadvantageous in terms of cost. Further, the polyasoxy oil composite of the component (A) of the present invention is an organic polysiloxane (i) which is hydrophobic in nature and a fine powder of cerium oxide which is surface-treated with the above organic polyoxyalkylene ( Ii) and the amount of the alkaline catalyst (iii), after mixing at φ room temperature to 200 ° C, preferably 100 to 200 ° C, more preferably 150 to 200 ° C, may be required Manufactured by removal of neutralized and/or low boiling fractions. Further, the mixing treatment time is from 10 minutes to 5 hours, particularly preferably from 1 to 3 hours. Further, the mixing treatment is preferably carried out under an inert atmosphere such as nitrogen. The neutralization can be carried out using an organic acid such as 2-chloroethanol, formic acid or acetic acid, or an inorganic acid such as dilute hydrochloric acid or dilute sulfuric acid. Further, the removal of the low-boiling fraction can be carried out by a method such as distillation under reduced pressure. φ In the defoaming agent composition of the present invention, the polyfluorene oxide compound (A) is contained in an amount of 1 to 40% by mass, preferably 5 to 30% by mass based on the total of the defoaming agent composition. When the content is less than 1% by mass, the defoaming performance is not sufficient, and if it is more than 40% by mass, the stability and internal stability of the product are deteriorated. The polyoxyalkylene-modified organopolyoxane of the component (B) is obtained by emulsifying and dispersing the above-mentioned polyoxyxylene oil composite, and is represented by the following general formula (I). 200803959 (10) R12R3SiO-(Rl2SiO)x«(R1R2si〇)y-SiRl2R3 (I) In the above formula (I), R1 is the same or different type of substituted or unsubstituted carbon number 1~1 8 The hydrocarbon group, specifically, may be exemplified by methyl, ethyl, propyl, butyl, pentyl, hexyl, heptyl, octyl, decyl, decyl, dodecyl, thirteenyl 'tetradecyl , an alkyl group such as a hexadecanyl group, an octadecyl group or the like, a cycloalkyl group such as a cyclohexyl group, an alkenyl group such as a vinyl group or an allyl group, an aryl group such as a phenyl group or a phenyl group, a styryl group, and an α- An aralkyl group such as a methylstyryl group or the like or a chloromethyl group or a 3-methyl group in which a hydrogen atom bonded to a carbon atom of the group is partially or wholly substituted with a halogen atom, a cyano group, an amine group or the like. a monovalent hydrocarbon group such as propyl, 3,3,3-trifluoropropyl, cyanoethyl, 3-aminopropyl, fluorene-(β-aminoethyl)-γ-aminopropyl. Further, R2 is a polyoxyalkylene group represented by the following general formula (II). -R4,0(CH2CH20)a, (CH2(CH3)CH0)b-R5 (II) In the above formula (II), R4 is a divalent hydrocarbon group having 2 to 6 carbon atoms, and may be an alkylene group or a subchain The alkenyl group or the like may, for example, be a vinyl group, a propenyl group, a butyl group, a pentenyl group or a hexenyl group. Further, R5 is a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, an ethylidene group or an isocyano group, and the alkyl group may, for example, be a methyl group, an ethyl group, a propyl group, a butyl group or a pentyl group. a and b are 3Sa + bS80, preferably 5$a + b$60, and a/b = 2/8 to 8/2, preferably a positive number satisfying a/b = 2.5/7.5 to 7.5/2.5. In one aspect, R3 is the same group as R1 or R2, a hydroxyl group or an alkoxy group having a carbon number of from 1 to 14 to 200803959 (11) to 6 and, in particular, a group exemplified by the R1 and R2, in terms of an alkoxy group, A methoxy group, an ethoxy group, a propoxy group, a butoxy group, etc. are mentioned. Further, X in the above formula (I) is an integer of from 5 to 200, preferably from 20 to 150, and y is an integer of from 1 to 30, preferably from 1 to 20. * The polyoxyalkylene-modified organopolyoxane may be used alone or in combination of two or more kinds, and the viscosity at 25 ° C measured by an ostwald viscometer is 1 〇~1〇, 〇〇〇1111112/3, preferably 50 to 8,000 mm2/s, more preferably 500 to 5,000 mm2/s. In the defoaming agent composition of the present invention, the content of the polyoxyalkylene-modified organopolyoxane (B) is 0 to 30% by mass, preferably 1 to 20% by mass based on the total of the defoaming agent composition. When the content exceeds 30% by mass, the defoaming property of the composition deteriorates. The polyoxyethylene modified organopolyoxyalkylene of the component (C) is used for the stability, storage stability, dilution stability, high temperature stability, and defoaming property of the defoaming agent composition. φ is shown by the following general formula (ΙΠ). R62R8SiO-(R62SiO)m-(R6R7SiO)n-SiR62R8 (III) In the above formula (III), R6 is a substituted or unsubstituted carbon number of 1 to 18 monovalent hydrocarbon groups of the same kind or different species, specifically The exemplified by the above R1 may be preferably 80 mol% or more of the total R6, and particularly preferably 90 mol% or more of the methyl group in terms of defoaming property and economy. Further, R7 is a polyoxyethylene group represented by the following general formula (IV). -15- 200803959 (12) -r9-o(ch2ch2o)c_r10 (IV) In the above formula (IV), R9 is a divalent hydrocarbon group having 2 to 6 carbon atoms, and examples thereof include an alkylene group and an alkenylene group. For example, a vinyl group, a propenyl group, a butenyl group, a pentenyl group, a hexenyl group, etc. may be mentioned. Further, R1G may, for example, be a hydrogen atom, an alkyl group having 1 to 6 carbon atoms, an ethylidene group or an isocyano group, and the alkyl group may, for example, be a methyl group, an ethyl group, a propyl group, a butyl group or a pentyl group. c is 3 to 50, preferably a positive number satisfying 4 to φ 3 0 . When c is smaller than 3, it adds stability, storage stability, dilution stability, high temperature stability, and defoaming. Further, when it is larger than 5 Å, the melting point and the melt viscosity are increased, so that workability and defoaming property are lowered. In one aspect, R8 is the same group as R6 or R7, a hydroxyl group or an alkoxy group having 1 to 6 carbon atoms, specifically, the groups represented by R6 and R7, and the alkoxy group may, for example, a methoxy group, Oxyl, propoxy, butoxy, and the like. Further, in the above formula (ΠΙ), m is an integer of 5 to 200, preferably 10 to 150 ?. When m is larger than 200, the emulsifying dispersibility is lowered, and internal stability, storage stability, dilution stability, high temperature stability, and defoaming are adversely affected. η is an integer of 1 to 30, preferably 1 to 20. The polyoxyethylene-modified organopolyoxane may be used singly or in combination of two or more. In the defoaming agent composition of the present invention, the content of the polyoxyethylene-modified organopolyoxane (C) is from 1 to 40% by mass, preferably from 5 to 20% by mass based on the total of the defoaming agent composition. . When the content is less than 1 part by mass, the effect on stability and defoaming property is small, and when it exceeds 40% by mass, the viscosity of the defoaming agent composition-16 - 200803959 (13) becomes a cylinder, and water dispersibility is deteriorated. . Further, the polyoxyalkylene-modified organopolyoxane of the component (B) and the polyoxyethylene-modified organopolyoxane of the component, for example, an organohydrogenpolyoxyalkylene having a Si-H group and a molecular chain end A polyalkylene oxide or a polyoxyethylene compound having an aliphatic unsaturation such as an allyl group can be obtained by an addition reaction in the presence of a catalyst such as platinum. The polyoxyalkylene polymer of the component (D) is an emulsifying aid in the defoaming agent group φ of the present invention. Therefore, it is preferable to use a compound represented by the following general formula (VII). R140-(R150)z-R14 (VII) In the above formula (VII), R14 may, for example, be a hydrogen atom or an alkyl group such as a methyl group, an ethyl group, a propyl group or a butyl group, a vinyl group, an allyl group or the like. The alkenyl group, the ethyl sulfonyl group or the stearyl group or the like has a carbon number of 1 to 20, and particularly one of the 1 to 18 valence organic groups may be exemplified, and these may be the same or different. R15 is a divalent hydrocarbon group having 2 to 6 carbon atoms such as an alkyl group such as a vinyl group or a propylene group. In this case, R15 may be two or more types which are different from each other. Further, z is a polystyrene-equivalent weight average molecular weight measured by GPC of the polyoxyalkylene polymer, preferably from 50,000 to 5,000, more preferably from 1,000 to 4,000. Here, when the weight average molecular weight is less than 500, the emulsion stability of the defoaming agent composition is deteriorated. When the viscosity exceeds 5,000, the viscosity is high and the workability is deteriorated. Further, the polyoxyalkylene polymer may be used singly or in combination of two or more. -17 - 200803959 (14) The content of the polyoxyalkylene polymer (D) in the defoaming agent composition of the present invention is 0 to 40% by mass, preferably 0 to 20% by mass based on the entire defoaming agent composition. %. When it exceeds 40% by mass, the emulsification characteristics of the defoaming agent composition deteriorate. Further, the case of blending may be an effective amount, and it is preferably 5 mass% or more. * The nonionic surfactant of the component (E) is used to disperse the defoaming component [that is, the components (A) to (D)] in water, but generally it is a well-known thing, φ such as a pear Sugar fatty acid ester, glycerin fatty acid ester, polyglycerin fatty acid ester, propylene glycol fatty acid ester, sucrose fatty acid ester, polyethylene glycol fatty acid ester, polyethylene oxide ether, polyoxyethylene alkyl phenyl ether, Polyethylene oxide fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyethylene oxide glycerin fatty acid ester 'polyoxyethylene propylene glycol fatty acid ester, polyoxyethylene castor oil, polyoxyethylene hardened castor oil, etc. . Further, in the defoaming agent composition of the present invention, the nonionic surfactant may be used singly or in combination of two or more kinds, and the content thereof is 〇 20% by mass, preferably 1 〜 10% by mass. When the amount exceeds 20% by mass, the viscosity of the defoaming agent composition becomes high, and workability is deteriorated. In the defoaming agent composition of the present invention, the component (F) is required to emulsifie and add the necessary water to the components (A) to (E), and the amount thereof is relative to (a) ' to (E). The remainder of the total content of each component is preferably 50 to 2,00 parts by mass, more preferably 80 to 400 parts by mass, based on 1 part by mass of the total of the components (A) to (E). Further, the defoaming agent composition of the present invention is obtained by mixing the amounts of the above components (A) to (F), and heating them as necessary, and by a known method, for example, -18-200803959 (15) Mixing/dispersing machine such as homomixer, homogenizer, colloidal honing, etc., can be uniformly stirred and emulsified to prepare 'in particular, the setting amounts of (A) to (E) components are uniformly mixed. - After dispersing, one part of the set amount of the component (F) is added, and after stirring and emulsification, the residual component (F) is added, and the mixture is uniformly stirred and mixed to prepare a defoaming agent. good. Further, in the defoaming agent composition of the present invention, a small amount of a preservative and a sterilizing material may be added for the purpose of antiseptic. Specific examples of the septic material, such as sodium hypochlorite, sorbic acid, potassium sorbate, salicylic acid, sodium salicylate, benzoic acid, sodium benzoate, and parahydroxybenzoate, may be mentioned herein. Thiacorphyrin compounds and the like. The amount thereof to be added is preferably 0 to 5% by mass, particularly preferably 0.005 to 0.5 parts by mass, per 100 parts by mass of the defoaming agent composition of the present invention. The defoamer composition of the present invention thus obtained is degraded by a foaming liquid, especially an alkali foaming liquid, even if it is stored for a long period of time, and has little performance at all times, thereby obtaining internal stability and defoaming. Excellent for sustainability. Further, the amount of the defoaming agent to be added is not particularly limited, and is preferably 0.001 to 3% by mass based on the foaming liquid, and particularly preferably 0.01 to 1% by mass. Further, as the alkaline foaming liquid, aqueous cutting oil, pulp black liquor * (PULP BLACK LIQUOR) and the like can be exemplified. [Embodiment] [Embodiment] Hereinafter, the present invention will be specifically described by way of examples and comparative examples, but the invention is not limited to the following examples. Further, in the following examples, % shows % by mass, and the viscosity is 25 in 25 ° C measured by an ostwald viscosity meter [Examples 1 to 6, Comparative Examples 1 to 4] The following (A) ~ The component (E) was prepared by heating to 70 ° C in an amount shown in Table 1 and uniformly mixing the homogenizer, and then slowly adding water of the component (F) to prepare a defoaming agent composition. Regarding this composition, defoaming property, internal stability, and product stability were evaluated by the methods shown below. The results are shown in Table 1. (A) Polyoxygenated oil complex [polyanthracene oil complex (a-1)] An organic hydrophobic polyoxyalkylene system having a viscosity of 8,000 mm 2 /s, CH 3 Si 3 / 2 The unit is 100 parts by mass of a branched chain dimethyl polysiloxane having a content of 0.01 mol, and the fine powder of cerium oxide is the following (a) 5 mass φ parts, basic catalyst system, potassium hydroxide 3.3 parts by mass of 3% potassium citrate was mixed with nitrogen chloride at 150 ° C for 3 hours, and then neutralized with 2-chloroethanol, followed by removal of the low-boiling fraction. [Polyoxygenated oil complex (a-2)] An organic polyaerocycloxane which is hydrophobic in nature, has a viscosity of 10 〇, 〇〇〇mm2/s of dimethyl polyoxane, 100 parts by mass, and a fine powder The cerium oxide is 1 part by mass of the following (B), and the alkaline catalyst is used in an amount of 5 parts by mass of potassium citrate containing 3% of potassium hydroxide, and mixed at 150 ° C for 3 hours in a nitrogen atmosphere, and then 2- Chloroethyl-20- 200803959 (17) The alcohol is neutralized, followed by removal of the low-boiling fraction. [Polyoxygenated oil complex (a-3)] The organically hydrophobic organopolyoxane has a viscosity of 8,000 mm 2 /s, and the CH 3 Si 3 / 2 unit contains a branching dimethyl group of 0·01 molar fraction. 1 part by mass of the polyoxyalkylene oxide, the fine powder of cerium oxide was mixed with 5 parts by mass of the following (a), and mixed at 1,50 ° C for 3 hours under a nitrogen atmosphere.
[聚矽氧油複合物（a-4)] 本質上疏水性之有機聚矽氧烷係，黏度8,000mm2/s 使CH3Si03/2單位含有0.01莫耳分率之分支鏈狀之二甲基 聚矽氧烷1〇〇質量份，微粉末二氧化矽係Aer〇Sil200爲5 質量份，鹼性觸媒係含有氫氧化鉀3 %之矽酸鉀3.3質量 份，在氮氣體氛圍下於150°C，經3小時混合後，以2-氯 乙醇中和，接著除去低沸點餾份之物。 [微粉末二氧化矽] (甲）於樂帝克混合機裝入 Ae;rosil(AERΌSIL)3 00[日本 Aerosil公司製，比表面積300m2/g]100g，一邊攪拌，一 邊以霧狀添加兩末端羥基二甲基聚矽氧烷（黏度 5 0mm2/s)20g，在70°C經30分鐘攪拌者。 (乙）在樂帝克混合機裝入NipsilHD-2 [Tosoh二氧化 矽公司製，比表面積3 00m2/g] 100g，一邊攪拌一邊以霧 狀添加兩末端羥基二甲基聚矽氧烷（黏度50mm2/s)20g，於 -21 - 200803959 (18) 7 0°C經30分鐘攪拌者。 (B)聚氧化烯烴改性有機聚矽氧烷 [聚氧化烯烴改性有機聚矽氧烷（b-1)] 平均組成係以下述式 R12R3SiO-(R12SiO)x-(RlR2SiO)y-SiR12R3[Polyoxygenated oil complex (a-4)] An organic polyorganosiloxane which is hydrophobic in nature and has a viscosity of 8,000 mm 2 /s. The CH 3 Si 3 / 2 unit contains a branched dimethyl group of 0.01 mole fraction. 1 part by mass of decane, 5 parts by mass of fine powder of cerium oxide-based Aer〇Sil200, and 3.3 parts by mass of potassium citrate containing potassium hydroxide and 3% in a nitrogen atmosphere at 150° C, after mixing for 3 hours, neutralized with 2-chloroethanol, followed by removal of the low-boiling fraction. [Micro-powder cerium oxide] (A) Aer; rosil (AER Ό SIL) 3 00 [manufactured by Nippon Aerosil Co., Ltd., specific surface area: 300 m 2 /g] 100 g was placed in a Lectra mixer, and both ends were added in a mist while stirring. 20 g of hydroxydimethylpolysiloxane (viscosity 50 mm 2 /s), stirred at 70 ° C for 30 minutes. (B) In a Lectra mixer, NipsilHD-2 [Tosoh Sebacide Co., Ltd., specific surface area: 300 m2/g] 100 g, and a two-terminal hydroxydimethylpolyoxane (viscosity) was added in a mist while stirring. 50mm2/s) 20g, at -21 - 200803959 (18) 7 0 ° C stirred for 30 minutes. (B) Polyalkylene oxide modified organopolyoxane [Polyalkylene oxide modified organopolyoxane (b-1)] The average composition is as follows: R12R3SiO-(R12SiO)x-(RlR2SiO)y-SiR12R3
(但是，R1及R3爲-CH3，R2爲 -C3H60(C2H40)25.5(C3H60)8.5C4H9 ’ X 爲 30，y 爲 5。）表 示，且黏度爲l，〇〇〇mm2/s者。 [聚氧化烯烴改性以有機聚矽氧烷（b-2)] 平均組成爲以下述式(However, R1 and R3 are -CH3, and R2 is -C3H60(C2H40)25.5(C3H60)8.5C4H9' X is 30, y is 5), and the viscosity is l, 〇〇〇mm2/s. [Polyoxyalkylene modified with organopolyoxane (b-2)] The average composition is as follows
R12R3SiO-(R12SiO)x-(R1R2SiO)y-SiR12R3 (但是，R1及R3爲-CH3，R2爲 -C3H60(C2H40)21(C3H60)21CH3，X 爲 135，y 爲 15。）表示 ，且黏度爲2,5 00mm2/s之物。 [聚氧化烯烴改性有機聚砂氧院（b - 3 )] 平均組成爲下述式 -22- 200803959 (19) R12R3SiO-(R12SiO)x-(R1R2SiO)y-SiR12R3 (但是，R1 及 R3 爲-CH3，R2 爲·03Η60((：2Η40)8((：3Η60)24Η ’ x 爲 7 0 ’ y 爲 3) ’ 所示，且黏度爲8 00mm2/s之物。 [聚氧化烯烴改性有機聚矽氧烷（b-4)]R12R3SiO-(R12SiO)x-(R1R2SiO)y-SiR12R3 (however, R1 and R3 are -CH3, R2 is -C3H60(C2H40)21(C3H60)21CH3, X is 135, y is 15), and the viscosity is 2,5 00mm2/s. [Polyoxyalkylene modified organic polyoxate (b - 3 )] The average composition is the following formula-22-200803959 (19) R12R3SiO-(R12SiO)x-(R1R2SiO)y-SiR12R3 (however, R1 and R3 are -CH3, R2 is .03Η60((:2Η40)8((:3Η60)24Η ' x is 7 0 ' y is 3) ' and the viscosity is 800 mm 2 / s. [Polyoxyalkylene modified organic Polyoxane (b-4)]
平均組成爲以下述式 ， R12R3SiO-(R12SiO)x-(R1R2SiO)y-SiR12R3 (但是，R1及R3爲-CH3，R2爲 -C3H60(C2H40)24(C3H60)16H，X 爲 30，y 爲 5。） 所示，且黏度爲l，500mm2/s。 φ (C)聚氧乙烯改性有機聚矽氧烷 [聚氧乙烯改性有機聚矽氧烷（c-1)] 平均組成爲以下述式 R12R3SiO-(R12SiO)x-(R1R2SiO)y-SiR12R3 (但是，R1 及 R3 爲 _CH3，R2 爲-C3H60(C2H40)9.4H，X 爲 24 ， y 爲 4 。） 所示，且黏度爲4 5 0 m m 2 / s者。 - 23- 200803959 (20) [聚氧乙烯改性有機聚矽氧烷（c-2)] 平均組成爲以下述式 R^R^iO-CR^SiOOx-SiR^R3 (但是，R1 爲-CH3，R3 爲-C3H60(C2H40)32CH3，X 爲 60。） 所示，且熔點爲40°C者。 (D) 聚氧化烯烴聚合物 [聚氧化烯烴聚合物（d-1)] 平均組成爲以H0-(C3H60)3 5 -H所示者。 [聚氧化烯烴聚合物（d-2)] 平均組成爲以 CH2 = CHCH20-(C2H40)21(C3H60)21-CH3 所示者。 (E) 非離子性界面活性劑 (e-Ι)山梨聚糖單硬脂酸酯 (e-2)聚氧乙烯單月桂酸酯（EO加成莫耳數12) (e-3)聚氧乙烯單硬脂酸酯（EO加成莫耳數200) (e-4)聚氧乙烯十六基醚（EO加成莫耳數20) 《評價方法》 去泡性（添加之後）： - 24- 200803959 (21) 將各樣本以有效成分量0.2質量％添加於市售之水性 切削油劑之物以水稀釋3 0倍’以均化器經6，〇 〇 〇 rp mx2分 鐘攪拌，測定自攪拌停止至泡完全消失之時間。 ’ 去泡性（50°Cx7日後）： • 將各樣本以有效成分量〇·2質量％添加於市售之水性 切削油劑之物於5 0 °C保存7日，其後以水稀釋3 0倍，以 φ 均化器經6,000rpmx2分鐘攪拌，測定自攪拌停止至泡完 全消失之時間。 內添穩定性= 將各樣本 0 · 2質量％添加於市售之水性切削油劑之物 於5 0。(：保存7日時之外觀以目視依照下述基準觀察。 〇：無浮游·沈澱物，△:稍有浮游·沈澱物，X ··浮 游·沈澱物多 製品穩定性z 以目視依照下述基準觀察各樣本在45 °C保存7日後之 狀態。 〇：無分離，△:有濃淡分離，X:分離 -25- 200803959(22)The average composition is as follows: R12R3SiO-(R12SiO)x-(R1R2SiO)y-SiR12R3 (however, R1 and R3 are -CH3, R2 is -C3H60(C2H40)24(C3H60)16H, X is 30, y is 5 .), and the viscosity is l,500mm2 / s. φ (C) polyoxyethylene modified organopolyoxane [polyoxyethylene modified organopolyoxane (c-1)] The average composition is as follows: R12R3SiO-(R12SiO)x-(R1R2SiO)y-SiR12R3 (However, R1 and R3 are _CH3, R2 is -C3H60(C2H40)9.4H, X is 24, y is 4). The viscosity is 4 50 mm 2 / s. - 23- 200803959 (20) [Polyoxyethylene modified organopolyoxane (c-2)] The average composition is represented by the following formula: R^R^iO-CR^SiOOx-SiR^R3 (however, R1 is -CH3) , R3 is -C3H60(C2H40)32CH3, X is 60.), and the melting point is 40 °C. (D) Polyoxyalkylene polymer [Polyoxyalkylene polymer (d-1)] The average composition is represented by H0-(C3H60)3 5 -H. [Polyoxyalkylene polymer (d-2)] The average composition is as shown by CH2 = CHCH20-(C2H40)21(C3H60)21-CH3. (E) Nonionic surfactant (e-Ι) sorbitan monostearate (e-2) polyoxyethylene monolaurate (EO addition mole number 12) (e-3) polyoxygen Ethylene monostearate (EO addition mole number 200) (e-4) Polyoxyethylene hexadecyl ether (EO addition mole number 20) "Evaluation method" Defoaming property (after addition): - 24 - 200803959 (21) Each sample was added to a commercially available aqueous cutting oil agent in an amount of 0.2% by mass of the active ingredient, and diluted with water by 30 times to be stirred by a homogenizer at 6, 〇〇〇rp mx for 2 minutes. Stirring is stopped until the time when the bubble completely disappears. 'Defoaming property (50°C×7 days later): • Add each sample to the commercially available aqueous cutting oil at a concentration of 有效·2% by mass for 7 days at 50 °C, then dilute with water 3 At 0 times, the mixture was stirred at 6,000 rpm for 2 minutes in a φ homogenizer, and the time from the stop of stirring until the disappearance of the bubble was measured. Internal addition stability = 0. 2 mass% of each sample was added to a commercially available aqueous cutting oil agent at 50. (: The appearance of the 7th day was observed by visual observation according to the following criteria. 〇: No floating and sediment, △: slightly floating and sediment, X ··Floating and sediment multi-product stability z Visually according to the following criteria The state of each sample was observed after storage at 45 ° C for 7 days. 〇: no separation, △: separation of light and dark, X: separation -25 - 200803959 (22)
實預 g例 比較例 1 2 3 4 5 6 1 2 3 4 成 分 質 量 % (A) (a-1) 12 15 15 15 20 12 (a，2) 25 10 (a-3) 12 10 (a-4) 12 10 (B) (b-1) 5 3 3 2 5 5 5 5 (b-2) 5 (b-3) 2 1 2 2 (b-4) 3 2 5 3 (C) (c-1) 5 3 3 1 (c-2) 3 2 2 2 3 3 3 3 (D) (d-1) 12 5 5 10 12 12 10 15 (d-2) 2 10 5 (E) (e-1) 3 3 2 2 3 3 3 3 3 (e-2) 1 1 1 1 1 1 (e-3) 2 1 1 2 2 2 2 2 (e-4) 1 2 (F) 水 62 50 54 63 70 55 62 62 55 62 去泡性 添加 之後 0,45” 1，30” 0,30” 0,45” 1，00” 0,30” 1，00” Γ30” 0,45，， 1，00” 50°C x 7曰後 1，15” 3,00” Γ30” Γ30” 2,00” 2，15” 10分 以上 7,45” 9,00” 3,30” 內添安定性 〇 〇 〇 〇 〇 〇 X Δ X X 製品安定性 〇 〇 〇 〇 〇 〇 〇 X 〇 〇 -26-Pre-g example Comparative example 1 2 3 4 5 6 1 2 3 4 Component mass % (A) (a-1) 12 15 15 15 20 12 (a, 2) 25 10 (a-3) 12 10 (a- 4) 12 10 (B) (b-1) 5 3 3 2 5 5 5 5 (b-2) 5 (b-3) 2 1 2 2 (b-4) 3 2 5 3 (C) (c- 1) 5 3 3 1 (c-2) 3 2 2 2 3 3 3 3 (D) (d-1) 12 5 5 10 12 12 10 15 (d-2) 2 10 5 (E) (e-1 ) 3 3 2 2 3 3 3 3 3 (e-2) 1 1 1 1 1 1 (e-3) 2 1 1 2 2 2 2 2 (e-4) 1 2 (F) Water 62 50 54 63 70 55 62 62 55 62 After defoaming addition 0,45” 1,30” 0,30” 0,45” 1,00” 0,30” 1,00” Γ30” 0,45,, 1,00” 50 °C x 7曰1,15” 3,00” Γ30” Γ30” 2,00” 2,15” 10 points or more 7,45” 9,00” 3,30” Adding stability 〇〇〇〇〇 〇X Δ XX product stability 〇〇〇〇〇〇〇X 〇〇-26-
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|---|---|---|---|---|
| JP3974845B2 (en) * | 2002-12-05 | 2007-09-12 | 信越化学工業株式会社 | Antifoam composition |
| JP4232031B2 (en) * | 2004-05-14 | 2009-03-04 | 信越化学工業株式会社 | Antifoam composition and method for producing the same |
-
2006
- 2006-02-24 JP JP2006048504A patent/JP2007222812A/en active Pending
-
2007
- 2007-02-16 TW TW096105962A patent/TW200803959A/en unknown
- 2007-02-23 KR KR1020070018406A patent/KR20070088384A/en not_active Ceased
- 2007-02-25 CN CNA2007100058604A patent/CN101053797A/en active Pending
Also Published As
| Publication number | Publication date |
|---|---|
| KR20070088384A (en) | 2007-08-29 |
| JP2007222812A (en) | 2007-09-06 |
| CN101053797A (en) | 2007-10-17 |
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