WO2013000249A1 - 一种颗粒消泡剂及其制备方法 - Google Patents
一种颗粒消泡剂及其制备方法 Download PDFInfo
- Publication number
- WO2013000249A1 WO2013000249A1 PCT/CN2011/083984 CN2011083984W WO2013000249A1 WO 2013000249 A1 WO2013000249 A1 WO 2013000249A1 CN 2011083984 W CN2011083984 W CN 2011083984W WO 2013000249 A1 WO2013000249 A1 WO 2013000249A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- added
- silicone
- stirring
- silicone emulsion
- defoamer
- Prior art date
Links
- 239000002245 particle Substances 0.000 title claims abstract description 28
- 239000013530 defoamer Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 102
- 238000003756 stirring Methods 0.000 claims abstract description 72
- 239000000839 emulsion Substances 0.000 claims abstract description 65
- 239000000203 mixture Substances 0.000 claims abstract description 58
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000002518 antifoaming agent Substances 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000004519 grease Substances 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 18
- 229920000570 polyether Polymers 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 15
- 229920002472 Starch Polymers 0.000 claims description 14
- 235000019698 starch Nutrition 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000008107 starch Substances 0.000 claims description 12
- 239000008187 granular material Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 3
- 235000010980 cellulose Nutrition 0.000 claims description 3
- 229920003086 cellulose ether Polymers 0.000 claims description 3
- 239000003995 emulsifying agent Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 229920000388 Polyphosphate Polymers 0.000 claims description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 2
- 239000000969 carrier Substances 0.000 claims description 2
- 235000021317 phosphate Nutrition 0.000 claims description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 239000001205 polyphosphate Substances 0.000 claims description 2
- 235000011176 polyphosphates Nutrition 0.000 claims description 2
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 2
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 2
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract 1
- 239000006260 foam Substances 0.000 description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 20
- 238000005406 washing Methods 0.000 description 16
- 229920002125 Sokalan® Polymers 0.000 description 13
- 239000007787 solid Substances 0.000 description 13
- 238000004140 cleaning Methods 0.000 description 11
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 10
- 239000004584 polyacrylic acid Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 description 10
- 229910052938 sodium sulfate Inorganic materials 0.000 description 10
- 235000011152 sodium sulphate Nutrition 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 8
- 239000001768 carboxy methyl cellulose Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 8
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 239000011149 active material Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- 239000001509 sodium citrate Substances 0.000 description 6
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 6
- 230000001629 suppression Effects 0.000 description 6
- 239000000084 colloidal system Substances 0.000 description 5
- 239000007762 w/o emulsion Substances 0.000 description 5
- JSYPRLVDJYQMAI-ODZAUARKSA-N (z)-but-2-enedioic acid;prop-2-enoic acid Chemical compound OC(=O)C=C.OC(=O)\C=C/C(O)=O JSYPRLVDJYQMAI-ODZAUARKSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 239000007764 o/w emulsion Substances 0.000 description 4
- 239000010457 zeolite Substances 0.000 description 4
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000003254 anti-foaming effect Effects 0.000 description 3
- 239000003599 detergent Substances 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 239000001593 sorbitan monooleate Substances 0.000 description 3
- 235000011069 sorbitan monooleate Nutrition 0.000 description 3
- 229940035049 sorbitan monooleate Drugs 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000013405 beer Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012459 cleaning agent Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 polysiloxane Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 229920002126 Acrylic acid copolymer Polymers 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229920002323 Silicone foam Polymers 0.000 description 1
- 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 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229920006243 acrylic copolymer Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 150000002191 fatty alcohols Chemical class 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- 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 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000013514 silicone foam Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000012265 solid product Substances 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
- 238000003860 storage Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0026—Low foaming or foam regulating compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/825—Mixtures of compounds all of which are non-ionic
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0008—Detergent materials or soaps characterised by their shape or physical properties aqueous liquid non soap compositions
- C11D17/0017—Multi-phase liquid compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/0034—Fixed on a solid conventional detergent ingredient
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
- C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
- C11D3/3738—Alkoxylated silicones
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D9/00—Compositions of detergents based essentially on soap
- C11D9/04—Compositions of detergents based essentially on soap containing compounding ingredients other than soaps
- C11D9/22—Organic compounds, e.g. vitamins
- C11D9/36—Organic compounds, e.g. vitamins containing silicon
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/82—Compounds containing silicon
Definitions
- the invention relates to a preparation of a particle defoaming agent and a preparation method thereof.
- Defoamers are fine chemical additives and, therefore, the invention belongs to the field of fine chemical technology.
- Defoamers are mainly classified into silicone defoamers and non-silicone defoamers according to the active components. Most of the heavy-duty detergents and heavy-duty laundry detergents used in drum washing machines are silicone defoamers. Silicone defoamers are considered to be very effective in this application because they can be added very little. The amount is not affected by the hardness of water, and conventional defoamer compositions, such as soaps, have certain requirements on the hardness of water. The best-selling silicone defoamers in the market are mainly liquid types. Because they contain a large amount of water, they cannot be added to solid products, and there are problems such as poor compatibility with defoamed products and limited use range. Solid defoamers have unique advantages in the cleaning industry.
- EP0496510A1 introduces fatty acids, fatty alcohols, alkylphosphoric acids and hydrocarbon non-polar additives with a melting point of 30 ⁇ 100 °C as defoaming ingredients.
- the waxy substance of the discontinuous coating encloses the active material, but the problem of uneven distribution of the antifoaming active material cannot be completely solved;
- EP1075863 and WO2005058454 enhance the defoaming performance by introducing a hydrophobic organic liquid;
- WO2005058455 simultaneously introduces a melting point of 35 ⁇ 100 °C non-polar additive and non-silicon organic liquid to enhance the defoaming performance,
- EP1118655A1 introduces the addition of oleyl alcohol to improve the foam inhibition performance of silicone foam control components;
- EP1075864A2 WO2008043512 highlights the activity of silicone
- the fraction of the material is not limited by the size of the carrier such as sodium carbonate, sodium sulfate, sodium tripolyphosphate or sodium borate.
- EP0636685A2, EP0718018A2, EP0995473AK EP329842, USP5861368, USP6165968, W09716519AK US6610752 is a defoamer based on zeolite. From the composition of zeolite itself, it is a porous "cage" structure, and the defoaming active material is easily "trapped" and cannot play its role.
- CN1177630A describes a solid carrier particle antifoaming agent which is capable of producing an alkaline pH value in contact with water, but such an antifoaming agent is placed to absorb moisture;
- EP142910 discloses a water-soluble or water-dispersible organic vehicle.
- the organic vehicle comprises a first organic carrier component having a melting point of 38 to 90 ° C, and an ethoxylated nonionic group selected from the group consisting of a hydrophilic-lipophilic balance of 9.5 to 13.5 ° C and a melting point of 5 to 36 ° C. a second carrier component of a surfactant; US Pat. No.
- the solid antifoaming agent in the above patents mostly uses the choice of carrier or the combination of silicone grease and other auxiliaries to achieve the balance of defoaming and antifoaming, while the silicone grease which has not been pre-emulsified and dispersed is difficult to be in the carrier. Evenly distributed, so the foam control effect is not ideal in the early stage of washing and in the late stage of washing, and it is difficult to ensure the defoaming stability of the product. How to balance the foam control and the defoaming stability of the product in the early stage of washing and in the late stage of washing is a concern of many experts and scholars.
- the inventors used a silicone emulsion instead of the silicone grease, and agglomerated the silicone emulsion onto the carrier in a stepwise manner to form a two-layer "silicone" adsorption, which reduced the concentration of the silicone grease produced by the one-time agglomeration mixing.
- the problem of large and uneven distribution of silicone grease makes the defoamer particles have sufficient defoaming components on the outside and inside, which can play a slow release effect, thereby improving the defoaming, foam suppression and stability of the product.
- the prepared solid particle defoamer is good in beer bottle cleaning, cleaning of various heat exchange equipment, boiler, heat exchange pipeline, steel plate cleaning, mechanical cleaning, cement, starch gelatinization, cleaning process in the detergent industry. Eliminate the bubble effect.
- the present invention provides a method for preparing a solid particle defoaming agent, which provides better defoaming, foam suppression and stability of the obtained solid particle defoaming agent.
- the antifoaming agent of the present invention maintains a good defoaming effect both in the initial stage of washing and in the late stage of washing when applied to washing powder. And the product has better defoaming stability.
- the invention provides a particle defoaming agent and a preparation method thereof, which are formed by stepwise agglomeration of a silicone emulsion onto a carrier to form two layers of "silicone" adsorption, thereby reducing active substances produced by one-time agglomeration mixing.
- the concentration gradient is too large and the distribution of the silicone grease is not uniform, thereby improving the defoaming, foam suppression and stability properties of the product.
- the particulate antifoaming agent of the present invention consists of the following components:
- sulfates carbonates, phosphates, polyphosphates, starches, celluloses or aluminosilicates.
- These carriers are solid at room temperature, preferably starch and sulfates, carbonates, particles having a particle size of more than 300 mesh. Sulfate and carbonate having a diameter of less than 300 mesh have little adsorption force and are not recommended as a carrier of the present invention. They are used singly or in combination in an amount of 55 to 75% of the total mass of the particulate antifoaming agent.
- the carrier of the present invention is added in two parts, represented by A1 and A2, respectively, and the mass ratio of A1 to A2 is 4:1-15:1.
- the silicone emulsion is prepared from silicon grease, silicon polyether, emulsifier, deionized water, and the specific preparation method can be found from the existing professional literature.
- the silicone emulsion is used in an amount of 15 to 35% by weight based on the total mass of the particulate antifoaming agent.
- Silicone grease obtained by a reaction of an organopolysiloxane, a silicone resin, a silica, a hydrophobic treatment agent, a basic catalyst or the like.
- the specific preparation method can be found from the existing professional literature.
- the amount of silicone grease is 20% to 40% of the total mass of the silicone emulsion.
- Silicone polyether is prepared by the addition reaction of hydrogen-containing polysiloxane and unsaturated polyether under the action of acidic catalyst.
- the specific preparation method can be found from the existing professional literature.
- the silicone polyether has a dynamic viscosity at 25 ° C of 10 to 30,000 mPa's, preferably 60 to 5,000 mPa's at 25 °C. The amount is 5% to 10.5% of the total amount of the silicone emulsion.
- Emulsifier which is a nonionic surfactant.
- the amount is 2% to 7.5% of the total amount of the silicone emulsion.
- the silicone emulsion is added in two parts, represented by B1 and B2, respectively, and the mass ratio of B1 to B2 is 4: 1-10: 1.
- Commonly used structurants are: 1 Acrylic polymers, including polyacrylic acid and its sodium salt, maleic acid acrylic copolymer. 2 Cellulose ether, referring to water-soluble or water-swellable cellulose ethers, including sodium carboxymethylcellulose. 3 Lemon acid or citrate, including sodium citrate, potassium citrate. 4 polyvinylpyrrolidone.
- compositions may be used singly or in combination in any ratio.
- the amount is 3 to 10% of the total mass of the particle defoamer.
- the solvent includes alcohols and water such as methanol, ethanol, isopropanol, preferably ethanol and water. They can be used alone or in any ratio. The amount is 2% to 10% of the total mass of the particle defoamer.
- the preparation method of the granular antifoaming agent is as follows:
- the mixture obtained in (3) is granulated and dried to obtain a granule defoaming agent prepared.
- Advantageous Effects The present invention pre-emulsifies silicone grease into a silicone emulsion, which reduces the problem that the silicone grease is not easily dispersed and agglomerated onto the carrier, and the quality uniformity of the defoaming agent is ensured; and the silicone emulsion is stepwise.
- the carrier is added to solve the problem that the concentration gradient of the silicone grease generated by the one-time agglomeration mixing is too large, and the initial defoaming is sufficient and the active agent is released in the whole process for a long time, so that the entire washing process can fully defoam and inhibit the foaming, thereby Improve the continuous defoaming stability of the product.
- the obtained antifoaming actives were respectively a high viscosity silicone grease mixture G1 and a high viscosity silicone grease mixture G2.
- silicone emulsion S5 20 parts G2, 20 parts Gl, 4.5 parts flat plus 0-20, 3 parts sorbitan monostearate, 4.5 parts silicon polyether E 6 parts silicon polyether E at room temperature 5 , warmed to 80 ° C while stirring, fully mixed at 80 ° C for 40 min; after completion, the temperature of the system will be slowly added to the water, increase the stirring speed to change from water-in-oil emulsion to oil-in-water emulsion Phase, continue to add water to the required mass concentration of 50%.
- the above mixture is further emulsified by a colloid mill to obtain the desired silicone emulsion S5.
- Example 3 of the prepared particulate antifoaming agent 50 g of sodium sulfate (1250 mesh) was added to the mixer, 29 g of the silicone emulsion S3 was added thereto, and the mixture was uniformly stirred; then 9 g of sodium carbonate (300 mesh) was added thereto, and after stirring, 2 g of the silicone emulsion S1 and 4 g of organic were added. Silicone emulsion S2, stir well. Then, 3 g of polyacrylic acid was added, stirring was continued, and after stirring, 3 g of deionized water was added, and after stirring uniformly, the obtained mixture was granulated and dried to obtain Example 3 of the prepared particulate antifoaming agent.
- Example 8 of the prepared particulate antifoaming agent 55 g of sodium carbonate (800 mesh) was added to the mixer, 13 g of the silicone emulsion S2 was added thereto, and the mixture was uniformly stirred; 10 g of cationic starch was further added thereto, and after stirring, 2 g of the silicone emulsion S5 was added, and the mixture was uniformly stirred. Then, 10 g of maleic acid acrylic acid polymer was added, stirring was continued, and after stirring, 10 g of deionized water was added thereto, and after stirring uniformly, the resulting mixture was granulated and dried to obtain Example 8 of the prepared particulate antifoaming agent.
- Example 10 of the prepared particulate antifoaming agent 50 g of sodium carbonate (800 mesh) was added to the mixer, and 12 g of the silicone emulsions S1 and 18 g were added thereto. Silicone emulsion S2, stir well; add 5g sodium carbonate (800 mesh) to it, stir evenly, add 5g silicone emulsion S3, stir evenly. Then, 4 g of polyacrylic acid was added, stirring was continued, and after stirring uniformly, 6 g of deionized water was added, and after stirring uniformly, the obtained mixture was granulated and dried to obtain Example 10 of the prepared particulate antifoaming agent.
- sample granule defoamer and the comparative example, a solid antifoam sample abroad were tested as follows.
- Test method 50 g of commercially available washing powder, 0.3 g of solid particle defoamer were added to a drum washing machine with a capacity of 6 kg, and the test procedure was standard washing.
- the door of the washing machine is marked with five metrics, which are 0, 25%, 50%, 75%, and 100% of the door height. And each record is "0", “1", “2", “3", “4".
- "0" is the starting point, indicating no foam, and "4" means full of foam.
- the foam height was recorded every 5 minutes and recorded at the time of shutdown. The larger the value, the higher the foam height in the washing machine and the worse the foam inhibition; the lower the foam height in the same time, the better the foam inhibition performance of the product.
- the test results are as follows: M 0 0 ⁇ 1 ⁇ 2 ⁇ 2 ⁇ 2 ⁇ 3 >3 4 Embodiment 1
- Test method Horizontal auditing bubbler (manufactured by Nanjing Sixin Technology Application Research Institute Co., Ltd.) The glass audition superscript 0, 1, 2, 3 four metrics. "0" is the starting point, indicating no foam, and "3" means full of foam.
- the foam rises to a certain height the time to rise to a certain height is the blank time
- 0.5 g of defoamer is added thereto to record the change of the foam height with time. The longer it takes for the foam to rise to the same scale, the better the foam suppression performance.
- Table 4 The test results are shown in Table 4:
- the initial defoaming is sufficient and the active agent is released in a delayed manner throughout the process, ensuring sufficient defoaming and foam suppression throughout the washing process. And after being placed at 40 °C for four weeks, the performance of the defoaming performance is not obvious, and it has good anti-attenuation performance.
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Abstract
一种颗粒消泡剂的制备方法,该颗粒消泡剂由占总质量的55-75%的载体、15-35%的有机硅乳液、3-10%的结构剂和2-10%的溶剂组成,制备该颗粒消泡剂的方法为:(1)先将载体A1加入到混合器中,然后向其中加入有机硅乳液B1,搅拌均勾;(2)将载体组分A2加入到(1)得到的混合物中,并搅拌均勾;(3)往(2)得到的混合物中加入有机硅乳液B2,搅拌混合均勾后,加入溶剂搅拌均勾;(4)将(3)得到的混合物造粒、烘干,即得。
Description
一种颗粒消泡剂及其制备方法
技术领域
本发明涉及一种制备颗粒消泡剂及其制备方法。 消泡剂属于精细化学品添加剂, 因 此, 本发明隶属于精细化工技术领域。 技术背景
在工业清洗中, 需要用到工业清洗剂来去除污垢, 降低油水间表面张力。 清洗剂中 含有大量的表面活性剂, 在搅动过程中, 表面活性剂会吸附在气泡的周围稳定气泡, 从 而产生大量泡沫。 这种情形在啤酒瓶清洗, 各类换热设备、 锅炉、 换热管道的清洗, 钢 板清洗, 机械清洗, 水泥, 淀粉糊化等工业过程中都比较突出。 泡沫的存在会降低生产 能力, 造成原料和产品的浪费, 延长反应周期, 影响产品品质, 污染环境等。 因此, 泡 沫的消除变得非常重要, 工业过程中一般通过添加消泡剂来消泡。
按照活性组份的不同, 消泡剂主要分为有机硅消泡剂和非有机硅消泡剂。 用于滚筒 洗衣机的重垢型洗衣粉和重垢型洗衣液中的多为有机硅消泡剂, 硅氧烷消泡剂被认为在 这一应用中是很有效的, 因为它们可添加很少的数量且不受水的硬度的影响, 而传统的 消泡剂组合物, 例如皂类, 则对水的硬度有一定的要求。 市场畅销的有机硅消泡剂主要 是液体类型的, 由于含有大量水分而不能加入到固体类产品中, 存在与被消泡的产品相 容性差、 使用范围不广等问题。 在清洗行业中, 固体消泡剂有独特的优势。
关于固体消泡剂的研制有很多介绍: EP0496510A1、EP1070526A2介绍了熔点为 30〜 100°C的脂肪酸、 脂肪醇、 烷基磷酸及烃类非极性添加剂为助消泡成分, 这些成分虽然能 形成间断涂层的蜡状物质将活性物包住, 但无法彻底解决消泡活性物分布不均的问题; EP1075863、 WO2005058454通过疏水有机液体的引入来增强消泡性能; WO2005058455 同时引入熔点为 35〜100°C的非极性添加剂和非硅有机液体两种物质来增强消抑泡性能, EP1118655A1 介绍了加入油醇来改进硅酮控泡组份的抑泡性能; EP1075864A2、 WO2008043512 重点介绍了有机硅活性物部分, 且没有对载体部分如碳酸钠、 硫酸钠、 三聚磷酸钠、 硼酸钠进行出粒径大小的限制。 因为粒径太小, 不能足量吸附活性物, 无 法达到预期的消泡效果, 且如何使活性物更易分散及更均匀的附聚到载体上涉及较少; EP0636685A2 、 EP0718018A2、 EP0995473AK EP329842、 USP5861368、 USP6165968、
W09716519AK US6610752都是以沸石为载体的消泡剂,从沸石自身的组成结构上看,其 是一个多孔的 "笼式"结构, 消泡活性物质很容易被 "陷"其中, 不能发挥其作用。 大 量的文献表明以沸石为载体的消泡剂的活性会随着存放时间的延长而衰减, 解决的措施 很多: 如通过保护膜的方法将活性物包住、 引入硅聚醚先吸附到载体上以堵住沸石的多 孔结构、 加入能形成间断涂层的蜡状物质的材料, 但这些方法都不能彻底解决消泡剂的 衰减问题。 CN1177630A介绍了以一种含有与水接触式能产生碱性 pH值的固体载体颗粒 消泡剂, 但是这种消泡剂放置易吸潮; EP142910 公开了水溶性的或水可分散的有机载 体的使用, 有机载体含有熔点为 38〜90°C的第一有机载体组分, 以及选自亲水亲油平衡 为 9.5〜13.5 °C和熔点为 5〜36°C的乙氧基化的非离子表面活性剂的第二载体组分; US4894177介绍了一种改性纤维素为载体的颗粒消泡剂; US2003211961介绍了以一种或 多种丙烯酸树脂的聚合物、 共聚物或它们的混合体为载体的消泡剂。 上述这些消泡剂, 消泡剂的性能需进一步提高。
上述专利中的固体消泡剂, 多为利用载体的选择或者是利用硅脂和其它助剂的组合 来达到消泡和抑泡的平衡, 而没经过预先乳化分散的硅脂很难在载体中均匀分布, 所以 在洗涤初期和洗涤后期的泡沫控制效果都不太理想, 也很难保证产品的消泡稳定性。 如 何兼顾到洗涤初期和洗涤后期中的泡沫控制和产品的消泡稳定性是很多专家和学者关心 的问题。
本发明人采用有机硅乳液来代替硅脂, 并将有机硅乳液分步附聚到载体上, 形成两 个 硅脂 "层面"吸附, 减少了一次性附聚混合所产生的硅脂浓度梯度太大、 硅脂分布不 均匀的问题, 使得消泡剂颗粒外部和内部都有足够的消泡组分, 能起到缓慢释放的作用, 从而提高产品的消泡、 抑泡和稳定性能。 制备的固体颗粒消泡剂在啤酒瓶清洗, 各类换 热设备、 锅炉、 换热管道的清洗, 钢板清洗, 机械清洗, 水泥, 淀粉糊化, 洗衣粉行业 的清洗过程中都有较好的消抑泡效果。
发明内容
解决的技术问题: 本发明提供一种固体颗粒消泡剂的制备方法, 使得到的固体颗粒 消泡剂的消泡、 抑泡、 稳定性能更好。 本发明的消泡剂在应用于洗衣粉中时, 在洗涤初 期和洗涤后期都能保持很好的消抑泡效果。 且产品的消泡稳定性更优良。
技术方案:
本发明提供了一种颗粒消泡剂及其制备方法,通过将有机硅乳液分步附聚到载体上, 形成两个 硅脂 "层面"吸附, 减少了一次性附聚混合所产生的活性物浓度梯度太大、 硅 脂分布不均匀的问题, 从而提高产品的消泡、 抑泡和稳定性能。
本发明所述的颗粒消泡剂由以下组份组成:
A. 载体
选自硫酸盐、 碳酸盐、 磷酸盐、 聚磷酸盐、 淀粉、 纤维素或硅铝酸盐, 这些载体室温 下为固体, 优选淀粉和粒径为大于 300目的硫酸盐、 碳酸盐, 粒径小于 300目的硫酸盐、 碳酸盐的吸附力很小, 不建议作为本发明的载体。 它们单独使用或混合使用, 用量为颗 粒消泡剂总质量的 55〜75%。
本发明的载体分两部分添加, 分别用 A1和 A2表示, A1与 A2质量比为 4: 1-15: 1。
B. 有机硅乳液
所述有机硅乳液由硅脂、 硅聚醚、 乳化剂、 去离子水制备而成, 具体制备方法可以从 现有专业文献上查阅得知。 有机硅乳液的用量为颗粒消泡剂总质量的 15〜35%。
( 1 )硅脂, 由有机聚硅氧烷、 有机硅树脂、 二氧化硅、 疏水处理剂、 碱性催化剂等 通过反应获得。 具体制备方法可以从现有专业文献上查阅得知。 硅脂用量为有机硅乳液 总质量的 20%〜40%。
(2)硅聚醚, 是由含氢聚硅氧烷与不饱和聚醚在酸性催化剂的作用下发生加成反应 制备得到的, 具体制备方法可以从现有专业文献上查阅得知。 所述硅聚醚在 25 °C时的动 力粘度为 10〜30,000mPa's, 优选为在 25 下 60〜5,000mPa's。 用量为有机硅乳液总量的 5%〜10.5%。
( 3 ) 乳化剂, 为非离子表面活性剂。 用量为有机硅乳液总量的 2%〜7.5%。
(4) 去离子水, 用量占有机硅乳液总质量的 3%〜80%。
有机硅乳液分两部分添加, 分别用 B1和 B2表示, B1与 B2质量比为 4: 1-10: 1。
C.结构剂
常用的结构剂有: ① 丙烯酸类聚合物, 包括聚丙烯酸和其钠盐、 马来酸丙烯酸共聚 物。 ② 纤维素醚, 指水溶性的或可水溶胀的纤维素醚, 包括羧甲基纤维素钠。 ③ 柠檬 酸或柠檬酸盐类, 包括柠檬酸钠、 柠檬酸钾。 ④聚乙烯吡咯烷酮。
这些结构剂可以单独使用, 也可以任意比例混合使用。 用量为颗粒消泡剂总质量的 3〜10%。
D.溶剂
溶剂的蒸发会在固体颗粒内部形成空穴, 增加了固体颗粒的比表面积, 溶剂包括醇 类物质和水, 如甲醇、 乙醇、 异丙醇, 优选乙醇和水。 可以单独使用或以任意比例混合 使用。 用量为颗粒消泡剂总质量的 2%〜10%。
所述的颗粒消泡剂的制备方法, 具体操作步骤如下:
( 1 ) 先将载体 A1加入到混合器中, 然后向其中加入有机硅乳液 Bl, 搅拌均匀;
(2) 将载体组分 A2加入到 (1 ) 得到的混合物中, 并搅拌均匀;
(3 ) 往 (2) 得到的混合物中加入有机硅乳液 B2 , 搅拌混合均匀后, 加入结构剂 搅拌均匀后, 加入溶剂搅拌均匀;
(4) 将 (3 ) 得到的混合物造粒、 烘干, 得到的混合物即为所制备的颗粒消泡剂。 有益效果: 本发明将硅脂预先乳化成有机硅乳液, 减少了硅脂不易分散、 附聚到载 体上分布不均匀的问题, 保证了消泡剂的品质均一性; 并且分步将有机硅乳液加入载体, 解决了一次性附聚混合所产生的硅脂浓度梯度太大的问题, 达到初期消泡充分和整个过 程延时释放活性物, 使得整个洗涤过程都能充分消泡和抑泡, 从而提高产品的连续消泡 稳定性。
具体实施方式
按照 ZL200610040821.3的例 1和例 2的方法制备,得到的消泡活性物分别为高粘度 硅脂混合物 G1和高粘度硅脂混合物 G2。
制备硅聚醚 E E2、 E3、 E4、 E5和 E6, 其结构式为:
e、 f、 的取值见表 1 :
表 1 硅聚醚 E E2、 E3、 E4、 E5和 E6
1、 有机硅乳液制备
( 1 ) 有机硅乳液 SI的制备:
室温下, 将 20份的 Gl、 1.5份的平平加 0-25、 0.5份的失水山梨醇单油酸酯、 3份 的硅聚醚 E2、 3份的硅聚醚 边搅拌边升温至 70°C, 充分乳化混合 35min; 完成后体系 的温度保持在 70°C缓慢地加入水, 提高搅拌速度使其由油包水型乳液变为水包油型乳液 转相, 继续加水至所需要的质量浓度, 为 50%。 上述混合物通过胶体磨进一步乳化即得 所需的有机硅乳液 Sl。
( 2 ) 有机硅乳液 S2的制备:
室温下, 将 30份的 G2、 4.5份的平平加 0-15、 3份的失水山梨醇单油酸酯、 2.5份 的硅聚醚 E 4份的硅聚醚 E3, 边搅拌边升温至 80°C, 在下 80°C充分混合 40min; 完成 后将保持体系的温度缓慢地加入水, 提高搅拌速度使其由油包水型乳液变为水包油型乳 液转相, 继续加水至所需要的质量浓度, 为 60%。 上述混合物通过胶体磨进一步乳化即 得所需的有机硅乳液 S2。
( 3 ) 有机硅乳液 S3的制备:
室温下, 将 20份的 G2、 20份的 Gl、 4.5份的平平加 0-15、 3份的失水山梨醇单油 酸酯、 4.5份的硅聚醚 E3、 6份的硅聚醚 E4, 边搅拌边升温至 80°C, 在下 80°C充分混合 40min; 完成后将保持体系的温度缓慢地加入水, 提高搅拌速度使其由油包水型乳液变为 水包油型乳液转相, 继续加水至所需要的质量浓度, 为 70%。 上述混合物通过胶体磨进 一步乳化即得所需的有机硅乳液 S3。
( 4 ) 有机硅乳液 S4的制备:
室温下,将 20份的 G2、 20份的 Gl、 4.5份的平平加 0-15、 3份的油酸聚氧乙烯(6 ) 醚、 4.5份的硅聚醚 E5、6份的硅聚醚 E6,边搅拌边升温至 80°C,在下 80°C充分混合 40min; 完成后将保持体系的温度缓慢地加入水, 提高搅拌速度使其由油包水型乳液变为水包油 型乳液转相, 继续加水至所需要的质量浓度, 为 60%。 上述混合物通过胶体磨进一步乳 化即得所需的有机硅乳液 S4。
( 5 ) 有机硅乳液 S5的制备:
室温下, 将 20份的 G2、 20份的 Gl、 4.5份的平平加 0-20、 3份的失水山梨醇单硬 脂酸酯、 4.5份的硅聚醚 E 6份的硅聚醚 E5, 边搅拌边升温至 80°C, 在下 80°C充分混 合 40min; 完成后将保持体系的温度缓慢地加入水, 提高搅拌速度使其由油包水型乳液 变为水包油型乳液转相, 继续加水至所需要的质量浓度, 为 50%。 上述混合物通过胶体 磨进一步乳化即得所需的有机硅乳液 S5。
2、 固体颗粒消泡剂制备
实施例 1
将 70g淀粉加入到混合器中, 向其中加入 12.5g有机硅乳液 S2, 搅拌均匀; 再向其 中加入 5g淀粉, 搅拌均匀后加入 2.5g有机硅乳液 S4, 搅拌均匀。 然后加入 2g羧甲基纤 维素钠和 3g聚丙烯酸, 继续搅拌, 搅拌均匀后加入 5g无水乙醇, 搅拌均匀后将得到的 混合物造粒烘干, 即得到所制备的颗粒消泡剂实施例 1。
实施例 2
将 60g硫酸钠 (800目) 加入到混合器中, 向其中加入 16.5g有机硅乳液 S2, 搅拌 均匀; 再向其中加入 9g硫酸钠 (800 目) , 搅拌均匀后加入 3.5g有机硅乳液 S5, 搅拌 均匀。 然后加入 2g柠檬酸钠和 3g马来酸丙烯酸共聚物, 继续搅拌, 搅拌均匀后加入 3g 无水乙醇和 3g去离子水, 搅拌均匀后将得到的混合物造粒烘干, 即得到所制备的颗粒消 泡剂实施例 2。
实施例 3
将 50g硫酸钠 (1250目) 加入到混合器中, 向其中加入 29g有机硅乳液 S3, 搅拌 均匀; 再向其中加入 9g碳酸钠 (300 目) , 搅拌均匀后加入 2g有机硅乳液 S1和 4g有 机硅乳液 S2 , 搅拌均匀。 然后加入 3g聚丙烯酸, 继续搅拌, 搅拌均匀后加入 3g去离 子水, 搅拌均匀后将得到的混合物造粒烘干, 即得到所制备的颗粒消泡剂实施例 3。
实施例 4
将 63g硫酸钠 (300目)加入到混合器中, 向其中加入 14g有机硅乳液 Sl, 搅拌均 匀; 再向其中加入 10g阳离子淀粉, 搅拌均匀后加入 3g有机硅乳液 S2, 搅拌均匀。 然 后加入 8g聚丙烯酸, 继续搅拌, 搅拌均匀后加入 2g去离子水, 搅拌均匀后将得到的混 合物造粒烘干, 即得到所制备的颗粒消泡剂实施例 4。
实施例 5
将 65g硫酸钠 (800目)加入到混合器中, 向其中加入 17g有机硅乳液 Sl, 搅拌均
匀; 再向其中加入 7g阳离子淀粉, 搅拌均匀后加入 1.5g有机硅乳液 S3和 1.5g有机硅乳 液 S4, 搅拌均匀。 然后加入 3g羧甲基纤维素钠和 3g马来酸丙烯酸聚合物, 继续搅拌, 搅拌均匀后加入 2g无水乙醇, 搅拌均匀后将得到的混合物造粒烘干, 即得到所制备的颗 粒消泡剂实施例 5。
实施例 6
将 60g硫酸钠 (1250目) 加入到混合器中, 向其中加入 18g有机硅乳液 S2, 搅拌 均匀; 再向其中加入 5g硫酸钠 (1250目) , 搅拌均匀后加入 2g有机硅乳液 S3, 搅拌均 匀。 然后加入 3g羧甲基纤维素钠、 3g柠檬酸钠和 4g聚丙烯酸, 继续搅拌, 搅拌均匀后 加入 2g无水乙醇和 3g去离子水, 搅拌均匀后将得到的混合物造粒烘干, 即得到所制备 的颗粒消泡剂实施例 6。
实施例 7
将 50g硫酸钠 (1250目) 加入到混合器中, 向其中加入 12.6g有机硅乳液 S1和 12g 有机硅乳液 S2, 搅拌均匀; 再向其中加入 5g碳酸钠 (1250目) , 搅拌均匀后加入 2g有 机硅乳液 S4和 3.4g有机硅乳液 S5, 搅拌均匀。 然后加入 2g羧甲基纤维素钠、 5g柠檬 酸钠和 3g聚丙烯酸, 继续搅拌, 搅拌均匀后加入 5g无水乙醇, 搅拌均匀后将得到的混 合物造粒烘干, 即得到所制备的颗粒消泡剂实施例 7。
实施例 8
将 55g碳酸钠 (800目)加入到混合器中, 向其中加入 13g有机硅乳液 S2, 搅拌均 匀; 再向其中加入 10g阳离子淀粉, 搅拌均匀后加入 2g有机硅乳液 S5, 搅拌均匀。 然 后加入 10g马来酸丙烯酸聚合物, 继续搅拌, 搅拌均匀后加入 10g去离子水, 搅拌均匀 后将得到的混合物造粒烘干, 即得到所制备的颗粒消泡剂实施例 8。
实施例 9
将 47g碳酸钠 (800目) 加入到混合器中, 向其中加入 10g有机硅乳液 S1和 12g有 机硅乳液 S2, 搅拌均匀; 再向其中加入 10g阳离子淀粉, 搅拌均匀后加入 3g有机硅乳 液 S3,搅拌均匀。然后加入 5g羧甲基纤维素钠、 2g柠檬酸钠和 3g聚丙烯酸, 继续搅拌, 搅拌均匀后加入 8g去离子水, 搅拌均匀后将得到的混合物造粒烘干, 即得到所制备的颗 粒消泡剂实施例 9。
实施例 10
将 50g碳酸钠 (800目) 加入到混合器中, 向其中加入 12g有机硅乳液 S1和 18g有
机硅乳液 S2, 搅拌均匀; 再向其中加入 5g碳酸钠 (800目) , 搅拌均匀后加入 5g有机 硅乳液 S3, 搅拌均匀。然后加入 4g聚丙烯酸, 继续搅拌, 搅拌均匀后加入 6g去离子水, 搅拌均匀后将得到的混合物造粒烘干, 即得到所制备的颗粒消泡剂实施例 10。
实施例 11
将 60g碳酸钠 (1250目)加入到混合器中, 向其中加入 13g有机硅乳液 S2, 搅拌均 匀; 再向其中加入 5g碳酸钠(1250目), 搅拌均匀后加入 2g有机硅乳液 S3, 搅拌均匀。 然后加入 3g羧甲基纤维素钠、 3g柠檬酸钠和 lg马来酸丙烯酸聚合物, 继续搅拌, 搅拌 均匀后加入 5g去离子水和 5g无水乙醇, 搅拌均匀后将得到的混合物造粒烘干, 即得到 所制备的颗粒消泡剂实施例 11。
对比例 1
将 75g淀粉加入到混合器中, 向其中加入 10g高粘度硅脂混合物 G1和 5g高粘度硅 脂混合物 G2, 混合均匀后加入 2g羧甲基纤维素钠和 3g聚丙烯酸。 搅拌均匀后加入 5g 无水乙醇, 搅拌均匀后将得到的混合物造粒烘干, 即得到所制备的颗粒消泡剂对比例 1。
对比例 2
将 25g淀粉、 25g硫酸钠 (1250目)和 25g碳酸钠 (800目)加入到混合器中, 向其 中加入 5g高粘度硅脂混合物 G1和 10g高粘度硅脂混合物 G2, 混合均匀后加入 2g羧甲 基纤维素钠和 3g聚丙烯酸。搅拌均匀后加入溶剂 3g无水乙醇和 2g去离子水, 搅拌均匀 后将得到的混合物造粒烘干, 即得到所制备的颗粒消泡剂对比例 2。
3、 消抑泡性能测试
将实施例颗粒消泡剂与对比例、 国外某固体消泡剂样品按下述方法进行测试。
① 洗衣机测试
测试方法: 在容量为 6kg的滚筒洗衣机里加入 50g市售的洗衣粉, 0.3g固体颗粒消 泡剂,测试程序为标准洗。洗衣机的门上标有 5个度量标示,分别为门高的 0, 25%, 50%, 75%, 100%。 并各记为 "0" , " 1 " , "2" , "3 " , "4" 。 "0"为起始, 表示无泡 沫, "4"表示充满泡沫。 每 5min记录一次泡沫高度, 停机时记录。 数值越大, 表明洗 衣机中的泡沫高度越高, 抑泡性就越差; 相同时间内泡沫高度越低, 说明产品抑泡性能 越好。 测试结果如下:
M 0 0 <1 <2 <2 <2 <3 >3 4 实施例 1
N 0 0 <1 <2 >2 >2 >3 4
M 0 0 <1 <1 >1 <2 >2 <3 <3 实施例 2
N 0 0 1 >1 >1 <2 >2 >3 >3
M 0 0 <1 <1 <2 <2 >2 2 <3 实施例 3
N 0 0 >1 <1 <2 >2 >3 3 >3
M 0 0 <1 <2 <2 <3 >3 >3 4 实施例 4
N 0 0 >1 >1 >2 >3 >3 4
M 0 0 <1 <1 <2 <3 >3 >3 4 实施例 5
N 0 0 <1 1 >2 <3 >3 4
M 0 0 <1 <1 <2 <2 >2 <3 <3 实施例 6
N 0 0 <1 <2 <2 <3 <3 <3 4
M 0 0 <1 <1 <1 <2 2 <3 <3 实施例 7
N 0 0 <1 <1 <2 <2 2 <3 <3
M 0 0 <1 <2 <2 <2 >3 >3 >3 实施例 8
N 0 0 1 <2 <2 <3 >3 3 4
M 0 0 <1 1 <2 <2 2 <3 <3 实施例 9
N 0 0 <1 1 <2 <3 3 >3 3
M 0 0 <1 <1 >1 <2 <2 <3 <3 实施例 10
N 0 0 <1 <1 <2 <2 <2 <3 <3
M 0 0 <1 <2 2 <2 <3 >3 >3 实施例 11
N 0 0 <1 2 >2 >2 >3 >3 4
M 0 <2 <2 <3 >3 <3 >3 4 对比例 1
N 0 <2 2 <3 >3 >3 4
对比例 2 M 0 1 <2 <3 <3 <3 >3 4
N 0 1 2 <3 <3 >3 4
M 0 <2 >2 <3 >3 4
外来样品
N 0 2 3 4
注: 上表中 "M"表示当时测试; "N"表示样品在 40°C放置四周后测试。
② 卧式循环鼓泡法:
测试方法: 卧式循环鼓泡仪 (南京四新科技应用研究所有限公司制造) 的玻璃试镜 上标 0, 1, 2, 3 四个度量标示。 "0"为起始, 表示无泡沫, "3" 表示充满泡沫。 在 卧式循环鼓泡仪里加入 14kg的 0.3%十二烷基苯磺酸钠水溶液(pH值为 13) , 然后打开 温控开关, 将起泡液加热至测试温度 80°C, 开启空气泵等泡沫升至一定高度 (升至一定 高度的时间即为空白时间) 时, 再向其中加入 0.5g消泡剂, 记录泡沫高度随着时间的变 化规律。 泡沫上升到同一刻度所用的时间越长, 说明抑泡性能越好。 测试结果见表 4:
表 4 卧式循环测试结果
实施例 1 3Ό3" 2'40" 6'24" 2830" 32'26" 实施例 2 3Ό7" 2'25" 6'37" 26'54" 3436" 实施例 3 3Ό9" 2'20" 5'58" 25 '21" 34'46" 实施例 4 3Ό6" 2'42" 5'30" 22'21" 33'40" 抑 实施例 5 3Ό7" 233" 6'30" 23 '21" 30'40" 实施例 6 3Ό3" 2'27" 4'30" 25 '21" 35 '45" 泡 实施例 7 3Ό6" 2'29" 6Ό1" 24'23" 36'43" 实施例 8 3Ό5" 2'25" 6Ό4" 2832" 32'40" 时 实施例 9 3Ό4" 2Ί5" 6'42" 2930" 34,06" 实施例 10 3Ό3" 2'20" 6'50" 30'23" 38 '43" 间 实施例 11 3Ό6" 235" 5 '25" 25 '21" 30Ί0" 对比例 1 3Ό9" 1'40" 5'40" 15'01" 17'46" 对比例 2 3Ό5" 1'45" 4'40" 14,07" 18 '23" 外来样品 3Ό7" 1Ί3" 4Ί8" 9'45" 1332" 通过上述测试, 可以看出有机硅乳液分步附聚到载体上的颗粒消泡剂样 品均一, 消泡稳定, 使用很少的添加量即可达到初期消泡充分和整个过程延 时释放活性物, 保证整个洗涤过程都能充分消泡和抑泡。 并且在 40 °C放置四 周后, 消抑泡性能变化不明显, 具有较好的抗衰减性能。
Claims
1、 一种颗粒消泡剂及其制备方法, 其特征在于, 所述的颗粒消泡剂由以下 组分组成:
A、 载体, 选自硫酸盐、 碳酸盐、 磷酸盐、 聚磷酸盐、 淀粉、 纤维素或硅铝 酸盐, 它们单独使用或混合使用, 用量为颗粒消泡剂总质量的 55〜75%, 所述的 载体分成 A1和 A2两部分使用, A1与 A2质量比为 4: 1-15: 1;
B、 有机硅乳液, 由硅脂、 硅聚醚、 乳化剂、 去离子水制备而成, 所述有机 硅乳液的用量为颗粒消泡剂总质量的 15~35%;有机硅乳液分为 B1和 B2两部分 使用, B1与 B2质量比为 4: 1-10: 1;
C、 结构剂, 选自丙烯酸类聚合物、 纤维素醚、 柠檬酸、 柠檬酸盐类或聚 乙烯吡咯烷酮, 所述结构剂可以单独使用, 也可以任意比例混合使用, 用量为颗 粒消泡剂总质量的 3~10%;
D、 溶剂, 为醇类物质和水, 单独使用或以任意比例混合使用, 用量为颗粒 消泡剂总质量的 2%〜10%;
制备方法如下:
( 1 ) 先将载体 A1加入到混合器中, 然后向其中加入有机硅乳液 Bl, 搅拌 均匀;
(2) 将载体组分 A2加入到 (1 ) 得到的混合物中, 并搅拌均匀;
(3)往 (2)得到的混合物中加入有机硅乳液 B2 , 搅拌混合均匀后, 加入 溶剂搅拌均匀;
(4) 将 (3) 得到的混合物造粒、 烘干, 即得。
2、 根据权利要求 1所述的一种颗粒消泡剂的制备方法, 其中, 所述的载体 为粒径为大于 300目的硫酸盐、 碳酸盐或淀粉。
3、 根据权利要求 1所述的一种颗粒消泡剂的制备方法, 其中, 所述的溶剂 为乙醇和 /或水。
4、 根据权利要求 1所述的一种颗粒消泡剂的制备方法, 其中, 所述的载体 A1和 A2两个部分组成可以相同或不同。
5、 根据权利要求 1所述的一种颗粒消泡剂的制备方法, 其中, 所述的有机 硅乳液 B1和 B2两个部分组成可以相同或不同。
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ES2602067T3 (es) | 2017-02-17 |
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US9023781B2 (en) | 2015-05-05 |
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