CN1931417A - Prepn process of active defoaming agent composition - Google Patents
Prepn process of active defoaming agent composition Download PDFInfo
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- CN1931417A CN1931417A CN 200610040821 CN200610040821A CN1931417A CN 1931417 A CN1931417 A CN 1931417A CN 200610040821 CN200610040821 CN 200610040821 CN 200610040821 A CN200610040821 A CN 200610040821A CN 1931417 A CN1931417 A CN 1931417A
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- Prior art keywords
- defoaming composition
- active defoaming
- active
- defoamer
- catalyst
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- 239000000203 mixture Substances 0.000 title claims abstract description 42
- 239000002518 antifoaming agent Substances 0.000 title description 14
- 238000000034 method Methods 0.000 title description 10
- 230000008569 process Effects 0.000 title description 2
- 239000002245 particle Substances 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 11
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 11
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 6
- 229920001296 polysiloxane Polymers 0.000 claims description 29
- 229920002545 silicone oil Polymers 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- -1 trimethylsiloxy group Chemical group 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 6
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Chemical compound [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 4
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 125000005375 organosiloxane group Chemical group 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000012423 maintenance Methods 0.000 claims description 3
- 238000002454 metastable transfer emission spectrometry Methods 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- 125000002947 alkylene group Chemical group 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 150000003863 ammonium salts Chemical class 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000004093 cyano group Chemical group *C#N 0.000 claims description 2
- 229940008099 dimethicone Drugs 0.000 claims description 2
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 2
- RSIHJDGMBDPTIM-UHFFFAOYSA-N ethoxy(trimethyl)silane Chemical compound CCO[Si](C)(C)C RSIHJDGMBDPTIM-UHFFFAOYSA-N 0.000 claims description 2
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 claims description 2
- 125000004494 ethyl ester group Chemical group 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000005843 halogen group Chemical group 0.000 claims description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims 1
- 239000006260 foam Substances 0.000 abstract description 25
- 238000005406 washing Methods 0.000 abstract description 10
- 238000010438 heat treatment Methods 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 3
- 229920002050 silicone resin Polymers 0.000 abstract 2
- 229920001131 Pulp (paper) Polymers 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000013530 defoamer Substances 0.000 description 44
- 230000003254 anti-foaming effect Effects 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000839 emulsion Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000005587 bubbling Effects 0.000 description 5
- 239000002480 mineral oil Substances 0.000 description 5
- 235000010446 mineral oil Nutrition 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000004964 aerogel Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 150000001408 amides Chemical class 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229910008051 Si-OH Inorganic materials 0.000 description 2
- 229910006358 Si—OH Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000002283 diesel fuel Substances 0.000 description 2
- 239000003866 digestant Substances 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-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
- 241001465754 Metazoa Species 0.000 description 1
- 229920002367 Polyisobutene Polymers 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 239000003849 aromatic solvent Substances 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- OSXYHAQZDCICNX-UHFFFAOYSA-N dichloro(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](Cl)(Cl)C1=CC=CC=C1 OSXYHAQZDCICNX-UHFFFAOYSA-N 0.000 description 1
- GNEPOXWQWFSSOU-UHFFFAOYSA-N dichloro-methyl-phenylsilane Chemical compound C[Si](Cl)(Cl)C1=CC=CC=C1 GNEPOXWQWFSSOU-UHFFFAOYSA-N 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 239000005055 methyl trichlorosilane Substances 0.000 description 1
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000005054 phenyltrichlorosilane Substances 0.000 description 1
- HOKBIQDJCNTWST-UHFFFAOYSA-N phosphanylidenezinc;zinc Chemical compound [Zn].[Zn]=P.[Zn]=P HOKBIQDJCNTWST-UHFFFAOYSA-N 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000035479 physiological effects, processes and functions Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000004537 pulping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Degasification And Air Bubble Elimination (AREA)
- Paper (AREA)
Abstract
The present invention is one kind of active defoaming composition suitable for eliminating harmful foams under high temperature and strong alkaline condition in high efficiency, and may be used in washing paper pulp, treating metal surface and other fields. The active defoaming composition is prepared with organic siloxane, silicone resin, inorganic oxide particle, hydrophobic treating agent, catalyst and other material. The preparation process includes the following steps: 1. mixing organic siloxane, silicone resin and catalyst, and heating the mixture to 80-200 deg.c for controllable polymerization; 2. adding inorganic oxide particle and hydrophobic treating agent; and 3. further heating to reaction at 80-200 deg.c temperature and 0.01-0.08 MPa vacuum for 2-10 hr, and cooling to room temperature to obtain white polymer as the active defoaming composition.
Description
Technical field:
The present invention relates to a kind of active defoaming agent composition preparation method, the present invention relates to a kind of preparation method who is suitable for eliminating under the high temperature highly basic condition active defoaming composition of harmful foam more precisely, as be applied in fields such as pulping and paper-making, metal surface cleaning, defoamer is a kind of fine chemicals additive, therefore, the invention belongs to the fine chemistry industry auxiliary agent
Technical field.
Background technology:
Foam is a common phenomena in people's live and work, brings very big harm to industrial production, for example reduce machine operating efficiency, incur loss through delay working time, influence the quality of product etc.The method of eliminating harmful foam mainly contains physical method and chemical method froth breaking, and comparatively speaking, chemical method is promptly used the method froth breaking of defoamer to have widely and used.At present, the application of defoamer has been penetrated into paper industry, textile printing and dyeing, oil exploitation and refining, coating, emulsion polymerisation, sewage disposal, Chemical cleaning, Treatment of Metal Surface etc.
Facts have proved: because the particularity of foaming system itself, the difference of foam liquid chemical composition for example, differences such as temperature, shear rate, pH value, so do not have a kind of defoamer can be common to every profession and trade.Even the defoamer that the different operations in the same industry are used is also inequality, more useful two kinds of defoamers are in the situation of same operation, the quick froth breaking of a kind of embodiment, and another kind ofly embody the long-time bubble effect that presses down.
Defoamer can be divided into mineral oil origin, animals and plants oil type, polyether-type and several main types such as silicone based according to the difference of active matter.Because methyl-silicone oil has more special chemical property, as low surface tension, water insoluble, volatility is low, no physiology toxicity and itself can not produce pollution etc. to environment, thereby in the raw material of defoamer usually as first-selected material.But light has silicone oil can not realize froth breaking well, and this is because have electrostatic repulsion between silicone oil particle and the foam film, and " the entering energy barrier (entry barrier) " that makes silicone oil enter into the vacuolar membrane surface becomes big.Even the silicone oil particle enters into the surface of vacuolar membrane, froth breaking well also differs surely, silicone oil particulate that Here it is is not enough " the entering the degree of depth (entry depth) " on foam film surface, therefore, viewpoint according to people such as Denkov proposition, only enter coefficient E, spreading coefficient S and bridge formation coefficient B and all work energetically zero, could guarantee that a defoamer has good antifoaming performance.Based on a lot of basic research and analysis, the discovery white carbon joins to deenergize in the silicone oil and significantly improves antifoaming performance, mensuration by FTT (FilmTrapped Technology) technology finds that the effect of white carbon is to reduce " entering energy barrier (entrybarrier) " and increases " entering the degree of depth (entry depth) ".
Slurrying workshop section in paper industry, most important operation is an alkaline cooking, adds a lot of digestants, the purpose that adds digestant is that remove or protect fiber and half fiber that quicken lignin make it not dissolve.In addition, also must add some chemical assistants such as anthraquinone and derivative and surface-active substance in the digestion process, and will add some surfactants such as sodium alkyl sulfonate in the washing process.These auxiliary agents and the resin that removes out, wax, sodium soap etc. are easy to produce foam, therefore finish can produce a large amount of foams in the pulp washing process of back in boiling.These foams are not as eliminating, and all can produce very big influence to indexs such as the pulp washing speed of wash engine, washability, operational efficiency, even can cause the idle running of wash engine.Commonly used defoamer mainly contains two types in the pulp washing operation, and a kind of is that mineral oil and acid amides are composite, and another kind is the defoamer of organosilicon type.The defoamer that mineral oil and acid amides are formed has been used decades, for example domestic OTD product comes to this, but deposition can appear in acid amides when temperature is low, can produce two chalk English in the use, add mineral oil and adopt materials such as kerosene, diesel oil mostly, their existence meeting exerts an adverse impact to environment and people's physical and mental health.Comparatively speaking, silicone defoaming agent has high efficiency, is friendly to environment.
Common silicone defoaming agent generally is at high temperature to handle by silicone oil and hydrophobic silicic aerogels to form, and the processing under the high temperature mainly is that tiny white carbon particle is dispersed in the middle of the silicone oil, improves whole froth breaking effect, and the someone is referred to as synergistic effect.But common silicone defoaming agent disappearing under this particular surroundings of pulp washing (high temperature highly basic) pressed down the bubble effect and showed by force inadequately, and especially on suds suppressing properties, this just makes has to increase use amount when the user uses defoamer, thereby causes cost to rise.
Suds suppressing properties at defoamer improves, and the researcher made a lot of research and report both at home and abroad.Introduced with dimethyl polysiloxane as Japan Patent JP45-261 3 (23,613/70), and special siloxane resin and white carbon are the defoamer of component; People such as Ai zawa are at United States Patent (USP) the 4th, 639, have introduced a kind of method for preparing organosilicon froth breaking active matter in No. 489, and this method is 50-300 ℃ of heating down with methyl-silicone oil, filler, organic siliconresin and catalyst; Mention with organosilicon crosslinked thing among the patent US5153258 of people such as the HidekiNakahara of Dow corning company invention and make the suds suppressing properties that important component improves active matter, and the preparation method of five kinds of cross-linking agents proposed, these cross-linking agents and silicone grease are mixed obtaining pressing down the lasting active matter of bubble again; Kremer, mainly introduce spent glycol, polyisobutene, mineral oil, kerosene, diesel oil, gasoline, naphtha, aromatic solvent in the patent US2005/0109675A1 literary composition of people such as Lawrence N. invention and made carrier, dissolving viscosity 60,000～1,000,000 straight or branched silicone oil or silicone grease, the crosslinked silicone grease of HMW or both compounds, crosslinked silicone grease has the bubble ability that better presses down, cross-linking agent be by-OH ,-OCH3 ,-(CH3) polysiloxanes of 3 end-blockings, the prepared froth breaking active matter of this method has extremely strong suds suppressing properties; The patent US6207722 of the people such as Juen. of Dow corning company invention has set forth a kind of preparation method who contains the active matter of silicones, makes organic hydrophobic particles with methyl MQ resin or the methyl MQ resin that contains the part vinyl and mixes pyroreaction with methyl-silicone oil and white carbon etc. and prepare suds suppressing properties active matter preferably; U.S. Pat 4186104, US4690713, US4741861, US4919843, US5531929 and US5283004 etc. have done detailed introduction at the preparation of the organosilicon active matter of alkaline system use in addition, mainly being the suds suppressing properties that how to improve defoamer under the highly basic system, all is to adopt modified silicon oil, MQ resin, white carbon and base catalyst and organo-silicon coupling agent etc. to make the organosilicon active matter in the hot conditions reaction mostly.But the organosilicon active matter that all these patents are mentioned suds suppressing properties in strong alkali environment is all unsatisfactory, and particularly in the high temperature strong alkali environment, it disappears but the bubble activity is all not ideal.People such as Nanjing Sixin Science Application Research Institute Co., Ltd's Cao Zhiping also design at high temperature highly basic system in the patent of invention " Thermostable alkali resistance organosilicon defoaming agent latex emulsion composite and preparation method " of application in 2004, and be applied to embody good suds suppressing properties in beer bottle cleaning, the scouring agent.
Experience and IR infrared analysis according to some researchers, find that disappearing of silicone defoaming agent press down that the active basic reason that decay takes place is that small white carbon particle is assembled after bubble effect a period of time, the white carbon particle content is very high in some defoamer particulates, reach 15～17%, the white carbon particle content that has only 1～2%.And for defoamer, these two kinds of white carbon solids content are not the defoamer optimal selections.
The main purpose of this patent is to solve by novel method to press down the bubble problem.Main thought is under the effect of catalyst polymerization to take place by the silicone oil of high molecular weight and organic siliconresin, make it form the network structure in space, and then react with the white carbon particle, reducing the gathering of white carbon particle, thereby improve the suds suppressing properties of defoamer further.Experiment shows that the silicone defoaming agent of Xing Chenging possesses outstanding antifoaming performance in this way.
Summary of the invention:
The objective of the invention is for provide a kind of efficient, inexpensive active defoaming agent compositions, said composition as papermaking pulp washing operation, Treatment of Metal Surface etc. in high temperature highly basic is the organosilicon active defoaming composition with extremely strong froth breaking, suds suppressing properties.
[technical scheme]
Active defoaming composition of the present invention is by organosiloxane, organic siliconresin, inorganic oxide solid particle, hydrophobic treatment agent, catalyst and other material, obtains by chemical means such as modification processing, polymerisations.
Organopolysiloxane of the present invention, its chemical structure of general formula: R
aSiO
(4-a)/2
Wherein R is for replacing or the monovalence alkyl of non-replacement, and carbon number is 1-20, and these groups can be alkyl such as methyl, ethyl, propyl group, isopropyl, butyl etc.; Also can be aryl such as phenyl, benzyl etc. and alkylene such as vinyl, acrylic etc., the hydrogen atom in these groups can partly or entirely be replaced by halogen atom, cyano group.Wherein the value of a is 1.9-2.2.The organosiloxane that the present invention adopts generally speaking is the dimethicone of trimethylsiloxy group end-blocking.Organopolysiloxane is called for short silicone oil again, and suitable silicon oil viscosity is with 1,000-1, and 000,000MPas is good, is preferably 10,000-500,000MPas, the consumption of silicone oil is the 50-95% of active defoaming composition gross mass, is preferably 80-90%.
Organic siliconresin of the present invention is meant highly cross-linked cancellated polysiloxane.This cancellated polysiloxane is normally by the various mixtures of methyl trichlorosilane, dimethyldichlorosilane, phenyl trichlorosilane, diphenyl dichlorosilane or dichloromethyl phenylsilane, in organic solvent such as toluene, hydrolysis at a lower temperature, obtain the acidic hydrolysis thing, remove disacidify through washing then, then the heating or in the presence of catalyst polycondensation make performed polymer, performed polymer can further be transformed into the spacial framework that certain degree of cross linking is arranged.Be applied to the preferred MQ silicones of organic siliconresin of the present invention, M/Q value preferred 0.4～1.2: 1.0, they can solvent is arranged or without the situation of solvent under prepare by hydrolysis certain silane material, preferably in the presence of solvent toluene to the precursor of tetravalence siloxanes (as ethyl orthosilicate, poly-ethyl ester of silicic acid or sodium metasilicate) and the precursor of monovalence trialkyl silica base unit (as trimethylchloro-silicane institute, trimethylethoxysilane, HMDO or HMDS) hydrolysis and condensation, the MQ resin that generates is trimethyl silylization further, residual Si-OH is reacted away, but or the cancellation Si-OH group that under the highly basic condition, heats up, make resin from condensation.Organic siliconresin accounting example is preferably 4-15% in the active defoaming composition gross mass.
Inorganic oxide solid particle of the present invention is meant the oxide of particle diameter less than the silicon of 25um, magnesium, zinc, aluminium, i.e. white carbon, magnesia, titanium oxide, alundum (Al etc.Inorganic oxide can be used alone, but also also mix together, and its consumption is 1～15% of an active defoaming composition gross mass, preferred 4-8%, and consumption is less than 4%, then defoamer froth breaking efficiently; Consumption surpasses 8%, then can influence the emulsification and the dispersion of active matter, thereby influence antifoaming performance.The preferred white carbon of the present invention.
Hydrophobic treatment agent of the present invention is mainly used in to be handled the hydrophobization of inorganic oxide solid particle, the hydrophobic treatment agent mainly includes machine silicone couplet (as: MTES, inferior silester, trimethyl one Ethoxysilane, dimethyldiethoxysilane etc.), silicone oil with low viscosity, inorganic ammonium salt, HMDS, Methyl Hydrogen Polysiloxane Fluid, hydroxy silicon oil, D3, D4, D5, D6 and DMC etc., and consumption is 1～5% of an active compound total amount;
It is to promote between viscous silicone fluid and the silicones that catalyst of the present invention mainly acts on, and and solids between the carrying out of reaction, generally can adopt the product that is made by alkaline matter such as KOH, NaOH, Me4NOH, CsOH and methyl-silicone oil reaction, its consumption is the 1-5% of active defoaming composition total amount;
The preparation of the active defoaming agent composition of a kind of papermaking pulp washing defoamer of the present invention takes following steps to realize:
1. organopolysiloxane and organic siliconresin solid particle in mixer fully premix and add catalyst after begin mixture is heated to 80-200 ℃ of polymerization reaction take place, the degree of polymerization can be controlled as required;
2. the inorganic agent that adds inorganic oxide and hydrophobically modified;
3. said mixture is heated down at 80 ℃-200 ℃, temperature is preferably at 100-180 ℃; Reaction time is 2-10h, and the preferred reaction time is 3-5h, and the high temperature maintenance stage in later stage of this reaction is preferably under the vacuum condition carries out, and makes reaction more thorough, and vacuum degree control is preferably 0.03-0.05MPa at 0.01-0.08MPa; Cool to room temperature obtains white polymerization shape froth breaking active matter then.
The above-mentioned organosilicon active compound that makes can be made signature well behaved emulsion type defoaming agent of bubble and solvent-borne type defoamer by suitable emulsification and dispersing technology.
The specific embodiment
Embodiment 1
(1) preparation of active defoaming composition:
Adding 2000g viscosity in 5L vacuum stirring device is 100, the silicone oil of 000MPas, 200gMQ resin (M/Q ratio is 0.40: 1.00), 20g catalyst A (annotating: make) by KOH and methyl-silicone oil reaction, add hydrophobic silicic aerogels 100g and 30g MTES after being warming up to the polymerization of 100-150 ℃ of question response thing section, stir, and 100-120 ℃ of insulation of control temperature of reaction system 4h, at last 160 ℃, react 2h when vacuum is 0.03-0.05MPa again, make reaction thoroughly.And then cool to room temperature obtains white crosslinked shape active defoaming composition.
(2) emulsion type defoaming agent preparation:
In above-mentioned prepared active defoaming composition, add 250g Pan of department, 100g tween, 800g223 polyethers, 700g400 polyethers, constantly be heated to 70 ℃ under the strong agitation, slowly add 1200g water, add 2% hydroxy ethyl fiber cellulose solution 50g again, slowly add 1300g water again, make emulsion pass through colloid mill behind 70 ℃ of insulation 30min, prepared emulsion is cooled to below 40 ℃ under stirring at a slow speed, add anticorrisive agent and promptly make the good emulsion type defoaming agent A of antifoaming performance.
Annotate: 223 polyethers, 400 polyethers, catalyst A are that Nanjing Sixin Science Application Research Institute Co., Ltd produces
(1) preparation of active defoaming composition:
Adding 2000g viscosity in the 5L de-airing mixer is 200, the silicone oil of 000MPas, 100gMQ resin (M/Q ratio is 1.0: 1.0), 20g catalyst B (annotating: make) by NaOH and methyl-silicone oil reaction, be warming up to the 80-140 ℃ of crosslinked back of reaction mass and add hydrophobic silicic aerogels 100g and 30g HMDS, stir, and 90-110 ℃ of insulation of control temperature of reaction system 4h, at last 160 ℃, react 2h when vacuum is 0.03-0.05MPa again, make reaction thoroughly.And then cool to room temperature obtains white polymerization shape active defoaming composition.
(2) preparation of solvent-borne type defoamer:
With being warming up to 100-105 ℃ of temperature maintenance 1h in the above-mentioned organosilicon active compound 100g adding 200g diethylene glycol (DEG) that makes it is fully dissolved, can make the good defoamer B of antifoaming performance.
Annotate: catalyst B is that Nanjing Sixin Science Application Research Institute Co., Ltd produces
The test of defoamer:
The method of testing that defoamer disappears, suds suppressing properties has adopted circulation bubbling under stationary temperature and flow of test this patent invention is described in detail below:
Main tester: 2500ml graduated cylinder, water pump, spinner flowmeter, thermometer, stopwatch, temperature automatically controlled heater etc. (the device schematic diagram is seen Figure of description).
Add foam liquid 1500g behind l, the cleaning bubbling device;
2, open attemperating unit, make system be raised to 90 ℃ of temperature, and keep constant temperature;
3, open water pump and begin impact to bubble, and regulate spinner flowmeter with flow-control at 0.175m3/h, and write down 0 second, 15 seconds, 30 seconds, 45 seconds ... foam height when not adding defoamer;
4, take by weighing in the defoamer adding foam liquid system of metering, write down 15 seconds, 30 seconds, 45 seconds ... add the foam height behind the defoamer;
5, test result compares with pressing down the bubble rate.Pressing down bubble rate computing formula is: press down bubble rate (%)=(H blank-H test)/H blank * 100%
The H blank---do not add the foam height of defoamer, ml
H test---the foam height behind the adding defoamer, ml
Annotate: used foam liquid is paper mill, a Shenzhen black liquor of pulp making in the test, this black liquor pH 〉=13
The test case of defoamer sees Table 1 and table 2, from test result as can be seen, defoamer A and defoamer B obviously are better than external defoamer sample on antifoaming performance, and then have illustrated that the active compound of this papermaking pulp washing defoamer has good froth breaking, suds suppressing properties.
Table 1, defoamer A and the contrast of outer sample antifoaming performance
| Bubbling time/s | Outer sample | Defoamer A | ||||
| Blank foam height/ml | Foam height/ml behind the adding defoamer | Press down bubble rate/% | Blank foam height/ml | Foam height/ml behind the adding defoamer | Press down bubble rate/% | |
| 0 | 1300 | 1300 | ||||
| 15 | 1600 | 1950 | 1650 | 1920 | ||
| 30 | 1750 | 1950 | 1800 | 1890 | ||
| 45 | 1750 | 1800 | 1820 | 1550 | ||
| 60 | 1800 | 1400 | 80.00 | 1900 | 1390 | 85.00 |
| 90 | 1850 | 1400 | 81.80 | 2000 | 1366 | 90.60 |
| 120 | 1900 | 1410 | 81.70 | 2100 | 1388 | 89.00 |
| 180 | 2020 | 1460 | 77.80 | 2230 | 1393 | 90.00 |
| 240 | 2150 | 1500 | 76.50 | 2400 | 1406 | 90.40 |
| 300 | 1550 | 1430 | ||||
| 360 | 1600 | 1460 | ||||
| 420 | 1650 | 1490 | ||||
| 480 | 1680 | 1490 | ||||
Table 2, defoamer B and the contrast of outer sample antifoaming performance
| Bubbling time/s | Outer sample | Defoamer B | ||||
| Blank foam height/ml | Foam height/ml behind the adding defoamer | Press down bubble rate/% | Blank foam height/ml | Foam height/ml behind the adding defoamer | Press down bubble rate/% | |
| 0 | 1300 | 1300 | ||||
| 15 | 1600 | 1950 | 1650 | 1920 | ||
| 30 | 1750 | 1950 | 1800 | 1890 | ||
| 45 | 1750 | 1800 | 1820 | 1550 | ||
| 60 | 1800 | 1400 | 80.00 | 1900 | 1372 | 88.00 |
| 90 | 1850 | 1400 | 81.80 | 2000 | 1370 | 90.00 |
| 120 | 1900 | 1410 | 81.70 | 2100 | 1384 | 89.50 |
| 180 | 2020 | 1460 | 77.80 | 2230 | 1383 | 91.00 |
| 240 | 2150 | 1500 | 76.50 | 2400 | 1384 | 92.40 |
| 300 | 1550 | 1400 | ||||
| 360 | 1600 | 1440 | ||||
| 420 | 1650 | 1480 | ||||
| 480 | 1680 | 1480 | ||||
Description of drawings:
Accompanying drawing is circulation bubbling test isolated plant and instrument:
Wherein: 1, graduated cylinder
2, water pump
3, flowmeter
4, shower nozzle
5, temperature automatically controlled heater.
Claims (7)
1, active defoaming composition of the present invention is by organosiloxane, organic siliconresin, inorganic oxide solid particle, hydrophobic treatment agent, catalyst and other material, obtains by chemical means such as modification processing, polymerisations.
2, the described active defoaming composition of claim 1, its described organopolysiloxane, its chemical structure of general formula: R
aSiO
(4-a)/2
Wherein R is for replacing or the monovalence alkyl of non-replacement, and carbon number is 1-20, and these groups can be alkyl such as methyl, ethyl, propyl group, isopropyl, butyl etc.; Also can be aryl such as phenyl, benzyl etc. and alkylene such as vinyl, acrylic etc., the hydrogen atom in these groups can partly or entirely be replaced by halogen atom, cyano group.Wherein the value of a is 1.9-2.2.The organosiloxane that the present invention adopts generally speaking is the dimethicone of trimethylsiloxy group end-blocking.Organopolysiloxane is called for short silicone oil again, and the viscosity of silicone oil is 1,000-1, and 000,000MPas is good, consumption is the 50-95% of active defoaming composition gross mass.
3, the described active defoaming composition of claim 1, its described organic siliconresin is meant highly cross-linked cancellated polysiloxane.Be applied to the preferred MQ silicones of organic siliconresin of the present invention, M/Q value preferred 0.4～1.2: 1.0, it is to the hydrolysis of the precursor (as trimethylchloro-silicane institute, trimethylethoxysilane, HMDO or HMDS) of precursor of tetravalence siloxanes (as ethyl orthosilicate, the poly-ethyl ester of silicic acid or sodium metasilicate) and monovalence trialkyl silica base unit and condensation generation in the presence of solvent toluene.To account for the ratio of gross mass be 4-15% to organic siliconresin in active defoaming composition.
4, inorganic oxide solid particle of the present invention is meant the oxide of particle diameter less than the silicon of 25um, magnesium, zinc, aluminium, i.e. white carbon, magnesia, titanium oxide, alundum (Al etc.Inorganic oxide can be used alone, but also also mix together, and its consumption is 1～15% of an active defoaming composition gross mass.The preferred white carbon black of the present invention.
5, the described active defoaming composition of claim 1, its described hydrophobic treatment agent mainly includes machine silicone couplet (as: MTES, inferior silester, trimethyl one Ethoxysilane, dimethyldiethoxysilane etc.), silicone oil with low viscosity, inorganic ammonium salt, HMDS, Methyl Hydrogen Polysiloxane Fluid, hydroxy silicon oil, D3, D4, D5, D6 and DMC etc., and consumption is 1～5% of an active compound gross mass;
6, the described active defoaming composition of claim 1, its described catalyst are meant the product that is made by alkaline matter such as KOH, NaOH, Me4NOH, CsOH and methyl-silicone oil reaction, and catalyst amount is the 1-5% of active defoaming composition gross mass;
7, the preparation of a kind of active defoaming composition of the present invention takes following steps to realize:
1. organopolysiloxane and organic siliconresin solid particle in mixer fully premix and add catalyst after begin mixture is heated to 80-200 ℃ of polymerization reaction take place, the degree of polymerization can be controlled as required;
2. the inorganic agent that adds inorganic oxide and hydrophobically modified;
3. said mixture is heated down at 80 ℃-200 ℃, temperature is preferably at 100-180 ℃; Reaction time is 2-10h, and the preferred reaction time is 3-5h, and the high temperature maintenance stage in later stage of this reaction is preferably under the vacuum condition carries out, and makes reaction more thorough, and vacuum degree control is at 0.01-0.08MPa; Cool to room temperature obtains white polymerization shape active defoaming composition then.
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