CN101632908A - Method for preparing defoaming agent composition - Google Patents
Method for preparing defoaming agent composition Download PDFInfo
- Publication number
- CN101632908A CN101632908A CN200910184385A CN200910184385A CN101632908A CN 101632908 A CN101632908 A CN 101632908A CN 200910184385 A CN200910184385 A CN 200910184385A CN 200910184385 A CN200910184385 A CN 200910184385A CN 101632908 A CN101632908 A CN 101632908A
- Authority
- CN
- China
- Prior art keywords
- polysiloxane
- defoaming agent
- agent composition
- polyether
- filler particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 55
- 239000002518 antifoaming agent Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title abstract description 18
- -1 polysiloxane Polymers 0.000 claims abstract description 86
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 81
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000000945 filler Substances 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 13
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 12
- 239000007822 coupling agent Substances 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 229920000570 polyether Polymers 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000010703 silicon Substances 0.000 claims abstract description 6
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 11
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 6
- YDQGDERWZVTINN-UHFFFAOYSA-N [K].C[SiH2]O Chemical compound [K].C[SiH2]O YDQGDERWZVTINN-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000003517 fume Substances 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- NTWZYMJGDYYGNL-UHFFFAOYSA-N [Na].C[Si] Chemical compound [Na].C[Si] NTWZYMJGDYYGNL-UHFFFAOYSA-N 0.000 claims description 3
- 239000008119 colloidal silica Substances 0.000 claims description 3
- 238000002454 metastable transfer emission spectrometry Methods 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 3
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 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
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 3
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 2
- PYSGFFTXMUWEOT-UHFFFAOYSA-N 3-(dimethylamino)propan-1-ol Chemical compound CN(C)CCCO PYSGFFTXMUWEOT-UHFFFAOYSA-N 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 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
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 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
- 239000000463 material Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- RPDAUEIUDPHABB-UHFFFAOYSA-N potassium ethoxide Chemical compound [K+].CC[O-] RPDAUEIUDPHABB-UHFFFAOYSA-N 0.000 claims description 2
- BDAWXSQJJCIFIK-UHFFFAOYSA-N potassium methoxide Chemical compound [K+].[O-]C BDAWXSQJJCIFIK-UHFFFAOYSA-N 0.000 claims description 2
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 230000001413 cellular effect Effects 0.000 claims 1
- 238000012512 characterization method Methods 0.000 claims 1
- 238000010276 construction Methods 0.000 claims 1
- 239000006260 foam Substances 0.000 abstract description 8
- 238000004132 cross linking Methods 0.000 abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 239000012847 fine chemical Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000011149 active material Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 abstract 1
- 239000013530 defoamer Substances 0.000 description 16
- 239000012808 vapor phase Substances 0.000 description 9
- 230000003254 anti-foaming effect Effects 0.000 description 8
- 239000004964 aerogel Substances 0.000 description 7
- 230000002209 hydrophobic effect Effects 0.000 description 7
- 238000010792 warming Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000002585 base Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 229920013822 aminosilicone Polymers 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 125000000596 cyclohexenyl group Chemical group C1(=CCCCC1)* 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
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 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
- 238000004043 dyeing Methods 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 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
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000005054 phenyltrichlorosilane Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 125000002769 thiazolinyl group Chemical group 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
- HADKRTWCOYPCPH-UHFFFAOYSA-M trimethylphenylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C1=CC=CC=C1 HADKRTWCOYPCPH-UHFFFAOYSA-M 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
The invention discloses a method for preparing a defoaming agent composition, belonging to the technical field of fine chemical preparation. The invention provides a defoaming agent composition widely used for removing harmful foams in industrial production. The defoaming agent composition comprises the following components: (1) polysiloxane RaSiO(4-a)/2; (2) a coupling agent; (3) fine filler particles such as silicon dioxide and the like; (4) organic silicon resin; (5) polyether modified polysiloxane MDx(CH3GSiO)yM, wherein M is chain link R'2SiO1/2, D is chain link R'2SiO2/2, G is polyether radical-(CH2)z(EO)g(PO)hR'' and (6) an alkaline catalyst. The preparation method comprises the following steps: (1) heating the polysiloxane and the coupling agent together in a stirring machine, adding the alkaline catalyst to carry out a polymerization reaction at the temperature of 40-140 DEG C; (2) after crosslinking the mixture, adding the organic silicon resin and the polyether modified polysiloxane, carrying out a reaction again for 1-7 h at the temperature of 80-140 DEG C, and then adding the fine filler particles to mix uniformly, carrying out a reaction for 1-6 h at temperature of 90-180 DEG C; (3) after finishing the reaction, keeping the mixture for 0.1-1.5 h at the vacuum degree of -0.01 to -0.08 MPa, and finally, cooling to the room temperature to obtain white active materials that are defoaming agent compositions.
Description
Technical field
The present invention relates to a kind ofly based on polysiloxane, and introduce the preparation of the universal defoaming agent composition of polyether-modified polysiloxanes therein, said composition has excellent antifoaming performance in anion, nonionic foaming system.Defoaming agent composition belongs to fine chemicals, therefore, the invention belongs to technical field of fine chemical preparations.
Technical background
Foam is a common phenomena in the live and work.But foam can bring great harm sometimes in 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, and the defoamer froth breaking is one of chemical method.Along with the significantly raising of industrial enterprise's production scale and production efficiency, the defoamer froth breaking is more widely used.At present, defoamer has been widely used in the industries such as papermaking, textile printing and dyeing, oil exploitation and refining, coating, emulsion polymerisation, sewage disposal, metal cleaning, and defoamer has become indispensable functional aid in the production process.
According to the difference of froth breaking active matter, defoamer is divided into mineral oil origin, polyether-type and several main types such as silicone based.Compare with other defoamers, poly organo siloxane defoamer stable chemical performance, side effect is little, and good froth breaking ability and the lasting bubble ability that presses down are also arranged under the very low situation of consumption simultaneously, thereby, favored very much.
The froth breaking active matter is the core of defoamer, and its antifoaming speed and suds suppressing properties directly influence the performance of final products.For silicone based defoamer, the improvement of the antifoaming performance of its active matter is the improvement direction of silicone defoaming agent.The most original polysiloxane defoamers active matter is handled through specific process technology by dimethyl silicone polymer and silica and is obtained, and the defoaming agent composition of introducing as US3383327 comes to this.But because it can not press down bubble lastingly, promptly suds suppressing properties is poor, and therefore, domestic and international research personnel have carried out large-scale expansion research to its performance.US4338217A1 replaces common polysiloxanes and silicon dioxide granule mixed processing to make the froth breaking active matter with the alkoxyl polysiloxanes; US5824739 introducing amino silicones or carboxyl polysiloxanes obtain defoaming composition as the main body of froth breaking active matter with the silica mixed processing; EP163541B1 introduces with the polysiloxanes that contains terminal hydroxyl and form the side chain polysiloxane with the polysiloxane reaction that contains other active function groups under the effect of catalyst, and replace common polysiloxanes and hydrophilic silicon dioxide mixed processing with this, prepared defoamer formulations has very high viscosity, is difficult to this emulsification is dispersed in the water.US5153258 introduces and introduce the antifoaming performance that lightly crosslinked polysiloxane can improve composition in system, for example contain vinyl polysiloxane and hydrogeneous polysiloxane, hydroxyl polysiloxane and alkyl silicate and under the effect of catalyst, cross-linking reaction takes place, but crosslinking degree is difficult to control.CN1931417A discloses a kind of defoaming agent composition of high temperature resistant anti-highly basic, it is obtained by polysiloxanes and organic siliconresin cross-linking reaction, active matter is prepared into after the emulsion bubbling test performance in black liquor, it has suds suppressing properties preferably, but antifoaming speed remains further to be improved, and, because froth breaking active matter viscosity is bigger, be dispersed in the water it quite difficult.
The silicone antifoam agent of EP-A341952 introduction use branching and the composition of polyethers one polysiloxane copolymer are used for pulp production as defoamer.US5523019 introduces the composition of mineral oil and polyether-polysiloxane copolymers as defoamer, it is said to have positive effect.According to WO 98/000216, the siloxanes that contains dimethyl-3-hydroxypropyl-polyoxyethylene polyoxypropylene group is a specially suitable surfactant in the defoamer formulation.
In sum, the improvement of present existing froth breaking active matter mainly comprises the following aspects: (1) replaces methyl polysiloxane with modified polyorganosiloxane (for example hydroxyl polysiloxanes, contain amino silicones); (2) the cancellated polysiloxanes in space replaces the straight chain polysiloxane; (3) in the system of polysiloxanes and silicon dioxide granule, introduce organic siliconresin etc.; (4) as wherein adding polyethers or polyether-modified polysiloxanes.
The present invention reacts under the effect of catalyst by dimethyl silicone polymer, coupling agent, silicon polyethers, the silicones of trimethylsiloxy group end-blocking, with silica-treated, the froth breaking active matter that obtains has good antifoaming speed and suds suppressing properties in anion, nonionic foaming system then.The formation principle of froth breaking active matter still imperfectly understands at present, analyze its mechanism and may be and wherein contain the affinity that has increased froth breaking active matter and water behind the silicon polyethers, the froth breaking active matter can be dispersed into the defoamer particulate of required size with fast speeds in water, therefore, has antifoaming speed faster.
Summary of the invention
A kind of preparation of defoaming agent composition provides a kind of defoaming composition based on polysiloxanes, it is low to have viscosity, easily disperse, in various systems, have very fast antifoaming speed and good characteristics such as suds suppressing properties, can be widely used in harmful foam of eliminating in the industrial production.
Technical scheme
A kind of defoaming agent composition is characterized in that it is made up of following material:
A, polysiloxane.The general structure of polysiloxane is as follows:
R
aSiO
(4-a)/2
Wherein the value of a is 1.9～2.2, R in the molecular structure is identical or different, and the carbon number that it comprises the replacement of hydrogen atom, monovalence or non-replacement is 1～20 alkyl, and R is an alkyl, specifically comprise: alkyl, as methyl, ethyl, propyl group, n-pro-pyl, butyl, isobutyl group; Aryl is as phenyl, benzyl; Thiazolinyl is as vinyl, acrylic, pi-allyl, cyclohexenyl group.Consider that from the angle that raw material are easy to get preferred radicals R more than 80% is a methyl.The dynamic viscosity of this polysiloxane in the time of 25 ℃ is 1,000～300,000mPas, and the polysiloxane that the present invention adopts is the dimethyl silicone polymer of trimethylsiloxy group end-blocking.
B, coupling agent.The coupling agent that adds 0.5～20 part in per 100 parts polysiloxane, preferred 1～10 part.Coupling agent from following selection one or more, comprise MTMS, MTES, phenyl triethoxysilane, methyl triacetic acid base silane, tetraethoxysilane, ethyl orthosilicate, dimethyl diethoxy siloxanes, ethyl triethoxysilane.
C, meticulous filler particles.Meticulous filler particles is meant the oxide of silicon, magnesium, zinc, aluminium, i.e. silica, magnesia, zinc oxide, alundum (Al.These meticulous filler particles use separately or mix and use.Silica is commonly called as white carbon, and it is divided into two kinds of precipitated silica and fume colloidal silicas by manufacture method, is divided into two kinds of hydrophilic white carbon and hydrophobic silicic aerogels by surface nature.The meticulous filler particles that adds 0.1～20 part in per 100 parts polysiloxane, preferred 4～10 parts.The preferred meticulous filler particles of the present invention is a fume colloidal silica, can be the hydrophilic white carbon of vapor phase method, also can be the vapor phase method hydrophobic silicic aerogels, and its specific area is 20～800m
2/ g, preferred 50～500m
2/ g.
D, organic siliconresin.Organic siliconresin refers to the cancellated polysiloxane in highly cross-linked space, this cancellated polysiloxane is normally by various mixtures hydrolysis in organic solvent such as toluene of methyl trichlorosilane, dimethyldichlorosilane, phenyl trichlorosilane, diphenyl dichlorosilane or dichloromethyl phenylsilane, obtain the acidic hydrolysis thing, remove disacidify through washing then, obtain product.The organic siliconresin that the present invention uses is by chain link R '
3SiO
1/2(being called the M unit in the organosilicon chemistry) and chain link SiO
4/2The MQ resin that the unit of (Q unit) is formed, the mol ratio between the two is (0.4～1.2): 1.0, preferred (0.5～0.8): 1.0.In described M unit R '
3SiO
1/2, R ' wherein is identical or different, and R is consistent in the general structure of value and polysiloxane, is 1～20 alkyl for the carbon number of the replacement of hydrogen atom, monovalence or non-replacement.
The described organic siliconresin that in 100 parts polysiloxane, adds 1～20 part, preferred 4～15 parts.
E, polyether-modified polysiloxanes.Take place under the effect of catalyst by hydrogen containing siloxane and the polyethers that contains unsaturated bond that addition reaction prepares.The described polyether-modified polysiloxanes preferably average viscosity under 25 ℃ is 10～30, and 000mPas is preferably at 25 ℃ and descends 60～5,000mPas.The structural formula of polyether-modified polysiloxanes is as follows:
MD
x(CH
3GSiO)
yM
Wherein, M is identical with M unit in the organic siliconresin, is chain link R '
3SiO
1/2, D is chain link R '
2SiO
2/2, the R ' span of two structural formulas is identical; G is a polyether group, represents with following general structure :-(CH
2)
z(EO)
g(PO)
hR ", R in the formula " be-H or-CH
3Or-COCH
3Above-mentioned each structural formula subscript x, y, z, g, h are the degree of polymerization, x is 10～500 integer; Y is 1～50 integer; Z is 2～6 integer; G is 1～36 integer; H is 0～20 integer.
In 100 parts polysiloxane, add 0.1～50 part of described polyether-modified polysiloxanes, preferred 1～20 part.
F, base catalyst.Base catalyst is used for accelerating reacting between coupling agent and the polysiloxane.The hydroxide that comprises alkali metal hydroxide, alkali metal silane alkoxide, alkali metal alkyl oxide, quaternary ammonium salt, specifically refer to NaOH, potassium hydroxide, cesium hydroxide, methyl silanol potassium, methyl silicon sodium alcoholate, sodium methoxide, caustic alcohol, potassium methoxide, potassium ethoxide, beta-hydroxyethyl Trimethylamine, TMAH etc., preferable methyl silanol potassium.Add 0.1～10 part of base catalyst in per 100 parts polysiloxane, preferred 0.5～5 part.
The preparation method of defoaming agent composition of the present invention is as follows:
Polysiloxane and coupling agent heat up in stirrer for mixing, add the base catalyst polymerization reaction take place in the time of 40～140 ℃; Crosslinked back takes place and adds organic siliconresin and polyether-modified polysiloxanes in mixture, and reacts 1～7h again at 60～140 ℃, adds then after meticulous filler particles mixes, again at 90～180 ℃ of reaction 1～6h; After reaction finishes, mixture-0.01～-keep 0.1～1.5h under the 0.08MPa vacuum.At last, cool to room temperature obtains white active matter and is defoaming agent composition.
Specific implementation method
Comparative Examples 1: with reference to US5283004 example 1
Comparative Examples 2: with reference to US5283004 example 18
Embodiment 1
Add 1 in the 5L mixer, 000g viscosity is 1, the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 000mPas, 20g ethyl orthosilicate and 10g methyl silanol potassium, 1) and the polyether-modified polysiloxanes of 50g (x=100, y=20 mixes polymerization reaction take places at 80 ℃, add 90g MQ resin (M: Q=0.75: then, z=3, g=20, h=12, R "=-H); at 120 ℃ of hybrid reaction 4h, and then adding 80g specific area is 200m
2The vapor phase method hydrophobic silicic aerogels of/g, system are warming up to 160 ℃, and after keeping 2h under this temperature, keep 0.5h under the vacuum of-0.03MPa, and last cool to room temperature obtains white thickness silicone antifoam composition.
Embodiment 2
In the 5L mixer, add 1,000g viscosity is 10, the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 000mPas, 30g ethyl orthosilicate and 10g potassium hydroxide mix polymerization reaction take place at 100 ℃, 1) and the polyether-modified polysiloxanes (x=50 of 60g adds 100g MQ resin (M: Q=0.65: then, y=8, z=3, g=14, h=8, R "=-CH
3), at 100 ℃ of hybrid reaction 3.5h, adding the 90g specific area then is 300m
2The vapor phase method hydrophobic silicic aerogels of/g continues to be warming up to 180 ℃, and after keeping 2h under this temperature, keeps 0.5h under the vacuum of-0.03MPa, and last cool to room temperature obtains white thickness silicone antifoam composition.
Embodiment 3
In the 5L mixer, add 1,000g viscosity is 5, the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 000mPas, 20g MTES and 20g methyl silanol potassium, mix polymerization reaction take place at 120 ℃, 1) and the polyether-modified polysiloxanes of 40g (x=150, y=10, z=3 adds 80g MQ resin (M: Q=0.66: then, g=20, h=7, R "=-H), at 110 ℃ of hybrid reaction 3h; Adding the 100g specific area then is 200m
2The hydrophilic white carbon of the vapor phase method of/g continues to be warming up to 140 ℃, and after keeping 5h under this temperature, keeps 0.5h under the vacuum of-0.03MPa, and last cool to room temperature obtains white thickness silicone antifoam composition.
Embodiment 4
In the 5L mixer, add 1,000g viscosity is 100, the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 000mPas, 25g dimethyldiethoxysilane and 10g sodium methoxide mix polymerization reaction take place at 100 ℃, 1) and the polyether-modified polysiloxanes (x=70 of 80g adds 120gMQ resin (M: Q=0.8: then, y=5, z=3, g=10, h=0, R "=-CH
3), at 120 ℃ of hybrid reaction 5h; Adding the 70g specific area then is 380m
2The hydrophilic white carbon of the vapor phase method of/g continues to be warming up to 180 ℃, and after keeping 1.5h under this temperature, keeps 1h under the vacuum of-0.03MPa, and last cool to room temperature obtains white thickness silicone antifoam composition.
Embodiment 5
In the 5L mixer, add 1,000g viscosity is 60, the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 000mPas, 45g ethyl orthosilicate and 15g methyl silicon sodium alcoholate mix polymerization reaction take place at 100 ℃, 1) and the polyether-modified polysiloxanes (x=100 of 78g adds 120gMQ resin (M: Q=0.75: then, y=40, z=3, g=18, h=6, R "=-CH
3), at 100 ℃ of hybrid reaction 5h; Adding the 60g specific area then is 150m
2The vapor phase method hydrophobic silicic aerogels of/g continues to be warming up to 170 ℃, and after keeping 1.5h under this temperature, keeps 0.5h under the vacuum of-0.03MPa, and last cool to room temperature obtains white thickness silicone antifoam composition.
Embodiment 6
In the 5L mixer, add 1,000g viscosity is 1, the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 000mPas, 25g phenyl triethoxysilane and 10g potassium hydroxide mix polymerization reaction take place at 100 ℃, 1) and the polyether-modified polysiloxanes (x=150 of 35g adds 60g MQ resin (M: Q=0.65: then, y=40, z=3, g=4, h=6, R "=-COCH
3), at 100 ℃ of hybrid reaction 5h; Adding the 80g specific area then is 200m
2The vapor phase method hydrophobic silicic aerogels of/g continues to be warming up to 130 ℃, and after keeping 4h under this temperature, keeps 0.5h under the vacuum of-0.03MPa, and last cool to room temperature obtains white thickness silicone antifoam composition.
Embodiment 7
Add 1 in the 5L mixer, 000g viscosity is 80, the dimethyl silicone polymer of the trimethylsiloxy group end-blocking of 000mPas, 25g ethyl triethoxysilane and 10g sodium methoxide, 1) and the polyether-modified polysiloxanes of 35g (x=200, y=10 mixes polymerization reaction take places at 120 ℃, add 100gMQ resin (M: Q=0.75: then, z=3, g=7, h=3, R "=-H); at 110 ℃ of hybrid reaction 3.5h, adding the 100g specific area then is 200m
2The vapor phase method hydrophobic silicic aerogels of/g continues to be warming up to 150 ℃, and after keeping 3.5h under this temperature, keeps 0.5h under the vacuum of-0.03MPa, and last cool to room temperature obtains white thickness silicone antifoam composition.
The defoaming agent composition performance test
Sodium dodecyl benzene sulfonate aqueous solution with 0.5% (mass percent) is the foaming medium, adopts and shakes a bottle method test.Method of testing is as follows: the above-mentioned foaming medium of addition 50mL in the 100mL tool plug graduated cylinder, and then add the test defoaming agent composition of 0.010g, leave standstill behind the shake 50 times in vertical direction, and it is foam time T that the record foam disappears to the liquid level time occurring
50, shake writes down foam time T 50 times again
100, reaching till 400 times until always shaking a bottle number of times, the time is short more, and then defoaming agent composition disappears, and to press down the bubble effect good more.
The antifoam performance test result of the various defoaming agent compositions that embodiment and Comparative Examples are prepared is as shown in table 1, the data by table 1 as can be seen, the antifoam performance of example 1～7 is all good than Comparative Examples.From table 2 with the result of the test of the defoaming agent composition of the technical program preparation and the contrast of the defoamer sample antifoam performance on the market as can be seen, the antifoam performance of example 5 obviously is better than the defoamer sample W and the Z of market appearance again.This just illustrates that defoaming agent composition of the present invention has stronger froth breaking ability in the anion system.
The antifoam performance contrast of the various silicone antifoam compositions of table 1
Table 2 contrasts with the defoaming agent composition and the defoamer sample antifoam performance on the market of the technical program preparation
Claims (5)
1, a kind of defoaming agent composition is characterized in that it is made up of following material:
(1) polysiloxane, the general structure of polysiloxane is as follows:
R
aSiO
(4-a)/2
Wherein, the value of a is 1.9～2.2, and R is identical or different in the molecular structure, and the carbon number that it comprises the replacement of hydrogen atom, monovalence or non-replacement is 1～20 alkyl; The dynamic viscosity of described polysiloxane in the time of 25 ℃ is 1,000～300,000mPas;
(2) coupling agent, be selected from MTMS, MTES, phenyl triethoxysilane, methyl triacetic acid base silane, tetraethoxysilane, ethyl orthosilicate, dimethyl diethoxy siloxanes, the ethyl triethoxysilane one or more, per 100 parts polysiloxane adds 0.5～20 part coupling agent;
(3) meticulous filler particles is meant the oxide of silicon, magnesium, zinc, aluminium to comprise silica, magnesia, zinc oxide, alundum (Al that these meticulous filler particles use separately or mix and use; Per 100 parts polysiloxane adds 0.1～20 part meticulous filler particles;
(4) organic siliconresin is for by chain link M unit R '
3SiO
1/2With chain link Q cell S iO
4/2The MQ resin of forming, the mol ratio between the two is (0.4～1.2): 1.0, wherein the R ' in the M cellular construction formula is identical or different, and the carbon number that comprises the replacement of hydrogen atom, monovalence or non-replacement is 1～20 alkyl; Per 100 parts polysiloxane adds 1～20 part organic siliconresin;
(5) polyether-modified polysiloxanes, its molecular structural formula is as follows: MD
x(CH
3GSiO)
yM
Wherein, M is identical with M unit in the organic siliconresin, is chain link R '
3SiO
1/2, D is chain link R '
2SiO
2/2, the R ' span of two structural formulas is identical; G is a polyether group, and general structure is-(CH
2)
z(EO)
g(PO)
hR ", R in the formula " be-H or-CH
3Or-COCH
3Subscript x in above-mentioned each structural formula, y, z, g, h are the degree of polymerization, x is 10～500 integer; Y is 1～50 integer; Z is 2～6 integer; G is 1～36 integer; H is 0～20 integer; The average viscosity of described polyether-modified polysiloxanes under 25 ℃ is 10～30,000mPas; Add 0.1～50 part of described polyether-modified polysiloxanes in per 100 parts polysiloxane;
(6) base catalyst, be selected from NaOH, potassium hydroxide, cesium hydroxide, methyl silanol potassium, methyl silicon sodium alcoholate, sodium methoxide, caustic alcohol, potassium methoxide, potassium ethoxide, beta-hydroxyethyl Trimethylamine or TMAH, will add 0.1～10 part of base catalyst in per 100 parts polysiloxane.
2, the described a kind of defoaming agent composition of claim 1 is characterized in that (1) described polysiloxane is the dimethyl silicone polymer of trimethylsiloxy group end-blocking.
3, the described a kind of defoaming agent composition of claim 1 is characterized in that (3) described meticulous filler particles is a silica, is commonly called as white carbon, comprises precipitated silica, fume colloidal silica.
4, the described a kind of defoaming agent composition of claim 3 is characterized in that described meticulous filler particles is a fume colloidal silica, and its specific area is 20～800m
2/ g.
5, the described a kind of defoaming agent composition of preparation claim 1, its characterization step comprises:
(1) polysiloxane and coupling agent heat up in stirrer for mixing, add the base catalyst polymerization reaction take place in the time of 40～140 ℃;
(2) crosslinked back takes place and adds organic siliconresin and polyether-modified polysiloxanes in mixture, and reacts 1～7h again at 60～140 ℃, adds then after meticulous filler particles mixes, again at 90～180 ℃ of reaction 1～6h;
(3) after reaction finishes, mixture-0.01～-keep 0.1～1.5h under the 0.08MPa vacuum, last, cool to room temperature obtains white active matter and is defoaming agent composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101843850A CN101632908B (en) | 2009-08-19 | 2009-08-19 | Method for preparing defoaming agent composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101843850A CN101632908B (en) | 2009-08-19 | 2009-08-19 | Method for preparing defoaming agent composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101632908A true CN101632908A (en) | 2010-01-27 |
| CN101632908B CN101632908B (en) | 2011-07-20 |
Family
ID=41592339
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101843850A Active CN101632908B (en) | 2009-08-19 | 2009-08-19 | Method for preparing defoaming agent composition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101632908B (en) |
Cited By (36)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101884852A (en) * | 2010-06-30 | 2010-11-17 | 南京四新科技应用研究所有限公司 | Method for improving properties of polyether defoaming agent |
| CN102489048A (en) * | 2011-12-26 | 2012-06-13 | 滁州四新科技有限责任公司 | Antifoaming agent composition and preparation method thereof |
| CN102527096A (en) * | 2011-05-12 | 2012-07-04 | 湖北新四海化工股份有限公司 | Organic silicon defoaming agent and preparation method thereof |
| CN102698475A (en) * | 2012-06-29 | 2012-10-03 | 南京四新科技应用研究所有限公司 | Defoaming composition |
| CN102716600A (en) * | 2012-07-12 | 2012-10-10 | 南京四新科技应用研究所有限公司 | Method for improving foam suppression performance of organosilicone emulsion |
| CN102718978A (en) * | 2012-07-12 | 2012-10-10 | 南京四新科技应用研究所有限公司 | Method for reducing viscosity of organic silicone emulsion |
| CN103627175A (en) * | 2013-12-11 | 2014-03-12 | 武汉大学 | Hydrophilic room temperature vulcanized silicone rubber |
| WO2015003407A1 (en) * | 2013-07-11 | 2015-01-15 | 南京四新科技应用研究所有限公司 | Organosilicon composition, preparation method and use thereof |
| CN104560109A (en) * | 2013-10-24 | 2015-04-29 | 中国石油化工股份有限公司 | Delayed coking method |
| CN106215467A (en) * | 2016-08-27 | 2016-12-14 | 合肥普庆新材料科技有限公司 | A kind of organic silicon defoamer |
| CN106215466A (en) * | 2016-08-27 | 2016-12-14 | 合肥普庆新材料科技有限公司 | A kind of preparation method of high stability of siloxane defoamer |
| CN106237662A (en) * | 2016-08-27 | 2016-12-21 | 合肥普庆新材料科技有限公司 | A kind of preparation method of organic silicon defoamer |
| CN106267913A (en) * | 2016-08-27 | 2017-01-04 | 合肥普庆新材料科技有限公司 | A kind of high stability of siloxane defoamer |
| CN106693453A (en) * | 2016-12-28 | 2017-05-24 | 广东中联邦精细化工有限公司 | Defoaming agent for producing industrial detergent and preparation method of defoaming agent |
| CN106731033A (en) * | 2016-12-14 | 2017-05-31 | 东至绿洲环保化工有限公司 | A kind of organic silicon defoamer |
| CN106799069A (en) * | 2016-12-28 | 2017-06-06 | 广东中联邦精细化工有限公司 | A kind of articles for washing produces special defoamer and preparation method thereof |
| CN106807119A (en) * | 2016-12-28 | 2017-06-09 | 广东中联邦精细化工有限公司 | The special defoamer of one kind sugaring and preparation method |
| CN106999804A (en) * | 2015-03-31 | 2017-08-01 | 圣诺普科有限公司 | Defoamer, the water soluble resin composite comprising it and the water-soluble resin aqueous solution |
| CN107050935A (en) * | 2016-12-27 | 2017-08-18 | 广东中联邦精细化工有限公司 | A kind of special defoamer of power plant desulfurization |
| CN107512863A (en) * | 2016-06-16 | 2017-12-26 | 苏州市兴邦化学建材有限公司 | A kind of solid defoaming agent and preparation method thereof of strength cement-based grouting material |
| CN109011719A (en) * | 2018-08-23 | 2018-12-18 | 南京瑞思化学技术有限公司 | A kind of silicon composition and preparation method thereof |
| CN109107229A (en) * | 2018-08-23 | 2019-01-01 | 南京瑞思化学技术有限公司 | Silicon composition |
| CN109248473A (en) * | 2018-11-05 | 2019-01-22 | 南京瑞思化学技术有限公司 | A kind of deaeration composition |
| CN109260771A (en) * | 2018-10-17 | 2019-01-25 | 南京瑞思化学技术有限公司 | A kind of organosilicon foam control composition |
| CN109776806A (en) * | 2019-01-11 | 2019-05-21 | 湖北新四海化工股份有限公司 | A kind of hydrophily MQ silicone resin and its synthetic method |
| CN110124360A (en) * | 2019-06-04 | 2019-08-16 | 江苏四新科技应用研究所股份有限公司 | A kind of defoaming composition |
| CN110478950A (en) * | 2019-05-14 | 2019-11-22 | 江苏四新科技应用研究所股份有限公司 | A kind of defoaming agent for transparent liquid detergent |
| CN110636891A (en) * | 2016-10-10 | 2019-12-31 | 索理思科技开曼公司 | Novel antifoam formulations for use in thermal desalination processes of water |
| CN110898467A (en) * | 2019-12-05 | 2020-03-24 | 浙江新安化工集团股份有限公司 | Defoaming active substance, preparation method thereof and defoaming agent |
| CN113797600A (en) * | 2020-06-16 | 2021-12-17 | 江苏四新科技应用研究所股份有限公司 | Organosilicon defoaming composition and preparation method thereof |
| CN114082227A (en) * | 2021-11-18 | 2022-02-25 | 湖北兴发环保科技有限公司 | Modified organic silicon defoaming agent and preparation method thereof |
| CN114307260A (en) * | 2021-11-06 | 2022-04-12 | 南京瑞思化学技术有限公司 | Preparation method of polyether composition |
| CN115105868A (en) * | 2022-07-01 | 2022-09-27 | 佛山市南海大田化学有限公司 | Organic silicon defoaming agent and preparation method thereof |
| CN115155113A (en) * | 2022-07-01 | 2022-10-11 | 佛山市南海大田化学有限公司 | Structure for organic silicon defoaming agent and synthetic method thereof |
| CN115317961A (en) * | 2022-08-24 | 2022-11-11 | 哈药集团技术中心 | Preparation method of dimethyl silicone oil defoaming agent |
| CN117467243A (en) * | 2023-12-05 | 2024-01-30 | 昆山兴凯半导体材料有限公司 | High-heat-conductivity and high-insulativity epoxy composition and application thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106345146A (en) * | 2016-08-27 | 2017-01-25 | 合肥普庆新材料科技有限公司 | Defoaming agent for strong-basic metal degreasing agents and preparation method of defoaming agent |
-
2009
- 2009-08-19 CN CN2009101843850A patent/CN101632908B/en active Active
Cited By (52)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101884852A (en) * | 2010-06-30 | 2010-11-17 | 南京四新科技应用研究所有限公司 | Method for improving properties of polyether defoaming agent |
| CN102527096A (en) * | 2011-05-12 | 2012-07-04 | 湖北新四海化工股份有限公司 | Organic silicon defoaming agent and preparation method thereof |
| CN102527096B (en) * | 2011-05-12 | 2015-02-18 | 湖北新四海化工股份有限公司 | Organic silicon defoaming agent and preparation method thereof |
| CN102489048A (en) * | 2011-12-26 | 2012-06-13 | 滁州四新科技有限责任公司 | Antifoaming agent composition and preparation method thereof |
| CN102489048B (en) * | 2011-12-26 | 2014-01-15 | 滁州四新科技有限责任公司 | Antifoaming agent composition and preparation method thereof |
| CN102698475A (en) * | 2012-06-29 | 2012-10-03 | 南京四新科技应用研究所有限公司 | Defoaming composition |
| CN102698475B (en) * | 2012-06-29 | 2014-02-26 | 南京四新科技应用研究所有限公司 | Defoaming composition |
| CN102716600A (en) * | 2012-07-12 | 2012-10-10 | 南京四新科技应用研究所有限公司 | Method for improving foam suppression performance of organosilicone emulsion |
| CN102718978A (en) * | 2012-07-12 | 2012-10-10 | 南京四新科技应用研究所有限公司 | Method for reducing viscosity of organic silicone emulsion |
| CN102718978B (en) * | 2012-07-12 | 2014-02-19 | 南京四新科技应用研究所有限公司 | Method for reducing viscosity of organic silicone emulsion |
| WO2015003407A1 (en) * | 2013-07-11 | 2015-01-15 | 南京四新科技应用研究所有限公司 | Organosilicon composition, preparation method and use thereof |
| CN104560109A (en) * | 2013-10-24 | 2015-04-29 | 中国石油化工股份有限公司 | Delayed coking method |
| CN104560109B (en) * | 2013-10-24 | 2016-03-02 | 中国石油化工股份有限公司 | A kind of coking delay process |
| CN103627175B (en) * | 2013-12-11 | 2016-03-02 | 武汉大学 | A kind of hydrophilic room temperature vulcanized silicone rubber |
| CN103627175A (en) * | 2013-12-11 | 2014-03-12 | 武汉大学 | Hydrophilic room temperature vulcanized silicone rubber |
| CN106999804A (en) * | 2015-03-31 | 2017-08-01 | 圣诺普科有限公司 | Defoamer, the water soluble resin composite comprising it and the water-soluble resin aqueous solution |
| CN106999804B (en) * | 2015-03-31 | 2020-10-16 | 圣诺普科有限公司 | Defoaming agent, water-soluble resin composition containing same, and water-soluble resin aqueous solution |
| CN107512863A (en) * | 2016-06-16 | 2017-12-26 | 苏州市兴邦化学建材有限公司 | A kind of solid defoaming agent and preparation method thereof of strength cement-based grouting material |
| CN106237662A (en) * | 2016-08-27 | 2016-12-21 | 合肥普庆新材料科技有限公司 | A kind of preparation method of organic silicon defoamer |
| CN106267913A (en) * | 2016-08-27 | 2017-01-04 | 合肥普庆新材料科技有限公司 | A kind of high stability of siloxane defoamer |
| CN106215466A (en) * | 2016-08-27 | 2016-12-14 | 合肥普庆新材料科技有限公司 | A kind of preparation method of high stability of siloxane defoamer |
| CN106215467A (en) * | 2016-08-27 | 2016-12-14 | 合肥普庆新材料科技有限公司 | A kind of organic silicon defoamer |
| CN110636891A (en) * | 2016-10-10 | 2019-12-31 | 索理思科技开曼公司 | Novel antifoam formulations for use in thermal desalination processes of water |
| CN110636891B (en) * | 2016-10-10 | 2022-09-02 | 索理思科技开曼公司 | Novel antifoam formulations for use in thermal desalination processes of water |
| CN106731033A (en) * | 2016-12-14 | 2017-05-31 | 东至绿洲环保化工有限公司 | A kind of organic silicon defoamer |
| CN107050935A (en) * | 2016-12-27 | 2017-08-18 | 广东中联邦精细化工有限公司 | A kind of special defoamer of power plant desulfurization |
| CN106693453A (en) * | 2016-12-28 | 2017-05-24 | 广东中联邦精细化工有限公司 | Defoaming agent for producing industrial detergent and preparation method of defoaming agent |
| CN106799069A (en) * | 2016-12-28 | 2017-06-06 | 广东中联邦精细化工有限公司 | A kind of articles for washing produces special defoamer and preparation method thereof |
| CN106807119A (en) * | 2016-12-28 | 2017-06-09 | 广东中联邦精细化工有限公司 | The special defoamer of one kind sugaring and preparation method |
| CN109011719A (en) * | 2018-08-23 | 2018-12-18 | 南京瑞思化学技术有限公司 | A kind of silicon composition and preparation method thereof |
| CN109107229A (en) * | 2018-08-23 | 2019-01-01 | 南京瑞思化学技术有限公司 | Silicon composition |
| CN109011719B (en) * | 2018-08-23 | 2020-08-18 | 南京瑞思化学技术有限公司 | Organic silicon composition and preparation method thereof |
| CN109260771B (en) * | 2018-10-17 | 2021-04-27 | 南京瑞思化学技术有限公司 | Organic silicon foam control composition |
| CN109260771A (en) * | 2018-10-17 | 2019-01-25 | 南京瑞思化学技术有限公司 | A kind of organosilicon foam control composition |
| CN109248473A (en) * | 2018-11-05 | 2019-01-22 | 南京瑞思化学技术有限公司 | A kind of deaeration composition |
| CN109776806A (en) * | 2019-01-11 | 2019-05-21 | 湖北新四海化工股份有限公司 | A kind of hydrophily MQ silicone resin and its synthetic method |
| CN110478950A (en) * | 2019-05-14 | 2019-11-22 | 江苏四新科技应用研究所股份有限公司 | A kind of defoaming agent for transparent liquid detergent |
| CN110478950B (en) * | 2019-05-14 | 2021-08-06 | 江苏四新科技应用研究所股份有限公司 | Defoaming agent for transparent liquid detergent |
| CN110124360B (en) * | 2019-06-04 | 2021-11-19 | 江苏四新科技应用研究所股份有限公司 | Defoaming composition |
| CN110124360A (en) * | 2019-06-04 | 2019-08-16 | 江苏四新科技应用研究所股份有限公司 | A kind of defoaming composition |
| CN110898467A (en) * | 2019-12-05 | 2020-03-24 | 浙江新安化工集团股份有限公司 | Defoaming active substance, preparation method thereof and defoaming agent |
| CN110898467B (en) * | 2019-12-05 | 2021-02-05 | 浙江新安化工集团股份有限公司 | Defoaming active substance, preparation method thereof and defoaming agent |
| CN113797600B (en) * | 2020-06-16 | 2023-10-31 | 江苏四新科技应用研究所股份有限公司 | Organic silicon defoaming composition and preparation method thereof |
| CN113797600A (en) * | 2020-06-16 | 2021-12-17 | 江苏四新科技应用研究所股份有限公司 | Organosilicon defoaming composition and preparation method thereof |
| CN114307260A (en) * | 2021-11-06 | 2022-04-12 | 南京瑞思化学技术有限公司 | Preparation method of polyether composition |
| CN114082227A (en) * | 2021-11-18 | 2022-02-25 | 湖北兴发环保科技有限公司 | Modified organic silicon defoaming agent and preparation method thereof |
| CN115105868A (en) * | 2022-07-01 | 2022-09-27 | 佛山市南海大田化学有限公司 | Organic silicon defoaming agent and preparation method thereof |
| CN115155113B (en) * | 2022-07-01 | 2023-09-29 | 佛山市南海大田化学有限公司 | Structure for organic silicon defoamer and synthesis method thereof |
| CN115155113A (en) * | 2022-07-01 | 2022-10-11 | 佛山市南海大田化学有限公司 | Structure for organic silicon defoaming agent and synthetic method thereof |
| CN115317961A (en) * | 2022-08-24 | 2022-11-11 | 哈药集团技术中心 | Preparation method of dimethyl silicone oil defoaming agent |
| CN117467243A (en) * | 2023-12-05 | 2024-01-30 | 昆山兴凯半导体材料有限公司 | High-heat-conductivity and high-insulativity epoxy composition and application thereof |
| CN117467243B (en) * | 2023-12-05 | 2024-04-09 | 昆山兴凯半导体材料有限公司 | High-heat-conductivity and high-insulativity epoxy composition and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101632908B (en) | 2011-07-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101632908B (en) | Method for preparing defoaming agent composition | |
| CN102337031B (en) | Organosilicon composition with low viscosity and preparation method thereof | |
| CN102489048B (en) | Antifoaming agent composition and preparation method thereof | |
| CN101422712A (en) | Preparation method of anti-foam additive | |
| CN101884852A (en) | Method for improving properties of polyether defoaming agent | |
| EP2393909B1 (en) | Foam control composition | |
| JP4664472B2 (en) | Silicone antifoam | |
| CN110898467B (en) | Defoaming active substance, preparation method thereof and defoaming agent | |
| US5914362A (en) | Silicone-based antifoam compositions cross-reference to related applications | |
| CN103275493B (en) | Organosilicon composition | |
| CN104130879A (en) | Defoaming agent for liquid detergent | |
| CN106215466A (en) | A kind of preparation method of high stability of siloxane defoamer | |
| CN105107237B (en) | A kind of organosilicon defoaming composition and preparation method thereof | |
| CN102698475A (en) | Defoaming composition | |
| JP2015525124A (en) | Carboxysilicone-containing composition and process for preparing the composition | |
| EP3494171A1 (en) | Foam control compositions comprising silicone materials | |
| WO2015003407A1 (en) | Organosilicon composition, preparation method and use thereof | |
| CN104784980A (en) | Defoaming composition | |
| KR20000048474A (en) | Foam control compositions having resin-fillers | |
| CN102000451A (en) | Silicone defoaming composition and preparation method thereof | |
| CN101780386B (en) | Self-emulsifying defoaming composition | |
| CN103669108A (en) | Organic silicon defoamer for paper making industry and preparation method thereof | |
| CN106215467A (en) | A kind of organic silicon defoamer | |
| CN102174778B (en) | Self-emulsifiable defoaming composition and preparation method thereof | |
| CN106267913A (en) | A kind of high stability of siloxane defoamer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Chuzhou Sixin Science and Technology Co., Ltd. Assignor: Sixin Science & Technology Applied Inst. Co., Ltd., Nanjing City Contract record no.: 2011320001116 Denomination of invention: Method for preparing defoaming agent composition Granted publication date: 20110720 License type: Exclusive License Open date: 20100127 Record date: 20110915 |
|
| C56 | Change in the name or address of the patentee | ||
| CP02 | Change in the address of a patent holder |
Address after: 210027, Nanjing, Jiangsu Province, Xiaguan Road, Shimonoseki District No. 199 Zijin venture special community building D11 Patentee after: Sixin Science & Technology Applied Inst. Co., Ltd., Nanjing City Address before: Huang Jia Wei Road Nanjing City, Jiangsu province 210037 Xiaguan District No. 41-1 building B4-2 Patentee before: Sixin Science & Technology Applied Inst. Co., Ltd., Nanjing City |
|
| C56 | Change in the name or address of the patentee |
Owner name: JIANGSU INSTITUTE OF FOUR NEW TECHNOLOGYAPPLICATIO Free format text: FORMER NAME: SIXIN SCIENCE + TECHNOLOGY APPLIED INST. CO., LTD., NANJING CITY |
|
| CP03 | Change of name, title or address |
Address after: 210027 Gulou District, Nanjing Province, east of the East Wing Road, No. 199 Zijin (Shimonoseki) science and technology venture special community D11 block Patentee after: JIANGSU SIXIN SCIENTIFIC-TECHNOLOGICAL APPLICATION RESEARCH INSTITUTE CO., LTD. Address before: 210027, Nanjing, Jiangsu Province, Xiaguan Road, Shimonoseki District No. 199 Zijin venture special community building D11 Patentee before: Sixin Science & Technology Applied Inst. Co., Ltd., Nanjing City |
|
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 210027 A22, 199 shogundong Road, Gulou District, Nanjing, Jiangsu. Patentee after: JIANGSU SIXIN SCIENTIFIC-TECHNOLOGICAL APPLICATION RESEARCH INSTITUTE CO., LTD. Address before: 210027 Nanjing, Jiangsu, Gulou District, No. 199 shogundong Road, purple gold (Xiaguan) technology entrepreneurship special community D11 Patentee before: JIANGSU SIXIN SCIENTIFIC-TECHNOLOGICAL APPLICATION RESEARCH INSTITUTE CO., LTD. |