CN1692969A - High-temp. resistance organosilicon emulsion defoaming agents, and its synthetic method - Google Patents
High-temp. resistance organosilicon emulsion defoaming agents, and its synthetic method Download PDFInfo
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- CN1692969A CN1692969A CN 200510043567 CN200510043567A CN1692969A CN 1692969 A CN1692969 A CN 1692969A CN 200510043567 CN200510043567 CN 200510043567 CN 200510043567 A CN200510043567 A CN 200510043567A CN 1692969 A CN1692969 A CN 1692969A
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Abstract
A refractory organic silicon emulsion as defoamer is prepared from the modified siloxane with 0.5-2 pa.s viscosity and the mixed emulsifier containing at least one organic acid, alcohol, or amine through proportional mixing, adding water and emulsifying.
Description
Technical field
The present invention relates to surfactant and organic synthesis thereof, relate to a kind of high temperature resistant organosilicon emulsion defoaming agents and synthetic method thereof more specifically.
Background technology
At present, the defoamer of producing both at home and abroad mainly contains polyethers and silicone based.Because polyethers has the residual aldehydes that produces in residual oxyalkylene hydro carbons monomer and the production process, thus bacterial classification there is certain toxic and side effect, thereby gradually by silicone based replacement.Silicone based defoamer is mainly selected dimethicone for use, because dimethicone in its structural uniqueness, makes it that lower surface tension be arranged, thereby can be used as good defoamer.Though this defoamer has significant froth breaking ability at normal temperatures, breakdown of emulsion when heating makes water-oil separating, has lowered it and has pressed down bubble and antifoam performance, even can't use, especially should not be at pharmacy, food, brewage in the industry that needs high-temperature sterilization and use.In addition, owing to bad dispersibility in water, so when aqueous phase is used as defoamer, generally be mixed with O/w emulsion.
Summary of the invention
One of purpose of the present invention provides at when heating breakdown of emulsion not, keeps the unseparated novel fire resistant organosilicon emulsion defoaming agents of profit; Two of purpose provides the synthetic method of this defoamer.
One of purpose of the present invention can realize by following technical measures:
This novel fire resistant organosilicon emulsion defoaming agents is to be the modified siloxane of 0.5～2pas by viscosity: the liquid emulsion that blended emulsifier=1: 0.2～1.3 raw materials in weight portion that contain the polymer of oxyalkylene of a kind of organic acid or a kind of alcohol or a kind of amine and fatty acid glyceride at least are composite, form with water and milkization.
One of purpose of the present invention also can realize by following technical measures:
Described blended emulsifier is fatty acids polyoxyethylene ester or its polyoxyethylene polyoxypropylene ester: AEO or its polyoxyethylene polyoxypropylene ether: isomerous tridecanol atactic polyether: fatty acid glyceride=1: 0.1-1.5: 0.1-1.5: the mixture of 0.1-1.5 weight portion proportioning; Aliphatic acid is C in the described polyoxyethylene carboxylate
10～C
18Acid, polyoxyethylene segment-(O-C
2H
4-)
n-or its polyoxypropylene oxygen ethene segment-(O-C
3H
6-O-C
2H
4-) n among the n-is 5～20; Fatty alcohol is C in the described AEO
8～C
18Alcohol, polyoxyethylene segment-(O-CH
2-CH
2-)
n-or its polyoxyethylene polyoxypropylene segment-(O-C
3H
6-O-C
2H
4-)
n-in n be 5～20; Atactic polyether in the described isomerous tridecanol atactic polyether is meant the atactic polymer by ethylene oxide, propylene oxide, and alcohol is 5～25 with the mol ratio of oxyalkylene; Aliphatic acid in the described fatty acid glyceride is oleic acid, laurate and stearic acid, is respectively monoesters, dibasic acid esters and three esters of glycerine; Siloxanes can be dimethyl siloxane or Methylethyl siloxanes in the described modified siloxane, and its chain number is between 10-200; Contained methyl oxygen ethene silica chain number or oxygen ethene siloxane chain joint number or sum of the two are between 5-30 in the modified siloxane.
Two of purpose of the present invention can realize by following technical measures:
The synthetic method of this organosilicon emulsion defoaming agents is
Synthesizing of a, modified siloxane
Conventional method is that the synthetic viscosity of raw material is the modified siloxane of 0.5～2pas with octamethylcy-clotetrasiloxane, highly basic, absolute ethyl alcohol, hydrochloric acid, propylene oxide, ethylene oxide;
The preparation of b, blended emulsifier
With various emulsifying agent polyoxyethylene carboxylates or its polyoxyethylene polyoxypropylene ester: AEO or its polyoxyethylene polyoxypropylene ether: isomerous tridecanol atactic polyether: fatty acid glyceride=1: 0.1-1.5: 0.1-1.5: in the mixing kettle that 0.1-1.5 weight portion proportioning input band stirs, heating and melting, stirring and evenly mixing is incubated standby.
The preparation of c, defoamer
Modified siloxane with a, the preparation of b operation: blended emulsifier=1: 0.2～1.3 weight portion proportionings join in the reactor, be heated to 40～80 ℃, the water that in batches adds 40～80 ℃ again, mix the back and add polyvinyl alcohol or methylcellulose class thickening stabilizing agent, cross homogenizer, it is 10-60%, H that emulsification gets solid content
2O is the defoamer of 90-40%.
Two of purpose of the present invention also can realize by following technical measures:
Described highly basic is sodium methoxide, caustic alcohol, KOH and NaOH.
One aspect of the present invention adds the component of high immersion immersion oil equilibrium valve (HLB value) in blended emulsifier, improve its heat resistance; Be equipped with corresponding stabilizing agent on the other hand again, make organic silicon emulsion stable under normal temperature condition, behind high temperature (130 ℃), still keep good pressing down to steep and antifoam performance.
Organosilicon emulsion defoaming agents good stability of the present invention at the 130 ℃ of heating half an hour of breakdown of emulsion not, keeps profit not separate, and places and is cooled to room temperature, still keeps good stable and presses down bubble, antifoam performance.Therefore, be suitable for especially medicine, food, industry (because of before adding defoamer, all needing to carry out high-temperature sterilization in the production process of these industries) such as brewage to it.Also be suitable for industries such as chemical industry, papermaking.
The specific embodiment
Embodiment 1:
Synthesizing of a, modified siloxane
Conventional method is that the synthetic viscosity of raw material is the modified siloxane of 0.5pas with octamethylcy-clotetrasiloxane, potassium hydroxide, absolute ethyl alcohol, hydrochloric acid, propylene oxide and ethylene oxide;
Synthesizing of b, blended emulsifier
Getting aliphatic acid respectively is C
10Acid, fatty alcohol are C
8The pure and mild catalyst potassium hydroxide that accounts for gross weight 0.1% is inserted in the reactor, and heat fused is evacuated to behind the 2700pa with nitrogen sweep still secondary, each inflated with nitrogen to 0.2Mpa, vacuumizes then; Press organic acid again: the proportioning of oxirane=1: 20mol adds oxirane, stirring also is heated to 70 ℃, treat that ethylene oxide reaction finishes the logical nitrogen in back to the vexed still of 0.2Mpa 60 minutes, blowing, be neutralized to PH=5 with oxalic acid again, add 0.1% active carbon that accounts for the reactant gross weight, press filtration gets emulsifying agent; Be C with various emulsifying agents according to aliphatic acid again
10Acid, polyethylene glycol-(O-CH
2-CH
2-)
n-n be 20 fatty acid polyethylene glycol ester: fatty alcohol is C
8Alcohol, polyethylene glycol-(O-CH
2-CH
2-)
n-in n be 20 AEO: the atactic polymer of isomerous tridecanol ethylene oxide: glyceryl oleate=1: 0.1: 1.5: 0.1 ratio mix blended emulsifier, standby.
C. the preparation of defoamer
Modified siloxane with a, the preparation of b operation: blended emulsifier=the weight portion proportioning joined in the reactor in 1: 0.2, be warming up to 60 ℃, add 40 ℃ water more in three batches, mix the back and add the polyvinyl alcohol thickening stabilizing agent, cross homogenizer, emulsification gets that solid content is 10%, H
2O is 90% defoamer.
Embodiment 2:
Synthesizing of a, modified siloxane
Conventional method is that the synthetic viscosity of raw material is the modified siloxane of 2pas with octamethylcy-clotetrasiloxane, potassium hydroxide, absolute ethyl alcohol, hydrochloric acid, oxyalkylene;
Synthesizing of b, blended emulsifier
Getting aliphatic acid respectively is C
18Acid, fatty alcohol are C
12The pure and mild catalyst NaOH that accounts for gross weight 1.0% is inserted in the reactor, and heat fused is evacuated to behind the 2800pa with nitrogen sweep still four times, each inflated with nitrogen to 0.5Mpa, vacuumizes then; Again by alcohol: the proportioning of oxirane=1: 5mol adds oxirane, stirs and be heated to 100 ℃, treats that reacting ethylene oxide finishes the logical nitrogen in back to the vexed still of 0.5Mpa 10 minutes, blowing, be neutralized to PH=6 with oxalic acid again, add 1.0% atlapulgite that accounts for the reactant gross weight, press filtration gets emulsifying agent; Be C with various emulsifying agents according to aliphatic acid again
18Acid, polyethylene glycol-(O-CH
2-CH
2-)
n-n be 5 fatty acid polyethylene glycol ester: fatty alcohol is C
12Alcohol, polyethylene glycol-(O-CH
2-CH
2-)
n-in n be 10 AEO: the atactic polymer of isomerous tridecanol propylene oxide: glycerol monolaurate=1: 1.5: 0.1: 1.5 ratio mix blended emulsifier, standby.
C. the preparation of defoamer
Modified siloxane with a, the preparation of b operation: blended emulsifier=the weight portion proportioning joined in the reactor in 1: 1.3, be warming up to 40 ℃, add 60 ℃ water more in four batches, mix the back and add the methylcellulose thickening stabilizing agent, cross homogenizer, emulsification gets that solid content is 60%, H
2O is 40% defoamer.
Embodiment 3:
Synthesizing of a, modified siloxane
Conventional method is that the synthetic viscosity of raw material is the modified siloxane of 1.0pas with octamethylcy-clotetrasiloxane, potassium hydroxide, absolute ethyl alcohol, hydrochloric acid, oxyalkylene;
Synthesizing of b, blended emulsifier
Getting aliphatic acid respectively is C
15Acid, fatty alcohol are C
12The pure and mild catalyst potassium hydroxide that accounts for gross weight 0.5% is inserted in the reactor, and heat fused is evacuated to behind the 2700pa with nitrogen sweep still three times, each inflated with nitrogen to 0.2Mpa, vacuumizes then; Press organic acid again: the proportioning of oxirane=1: 10mol adds oxirane, stirring also is heated to 90 ℃, treat that reacting ethylene oxide finishes the logical nitrogen in back to the vexed still of 0.2Mpa 30 minutes, blowing, be neutralized to PH=5 with oxalic acid again, add 0.5% active carbon that accounts for the reactant gross weight, press filtration gets emulsifying agent; Be C with various emulsifying agents according to aliphatic acid again
15Acid, polyethylene glycol-(O-CH
2-CH
2-)
n-n be 12 fatty acid polyethylene glycol ester: fatty alcohol is C
12Alcohol, polyethylene glycol-(O-CH
2-CH
2-)
n-in n be 13 AEO: the atactic polymer of isomerous tridecanol ethylene oxide: stearine=1: 1: 1: 1 ratio mix blended emulsifier, standby.
C. the preparation of defoamer
Modified siloxane with a, the preparation of b operation: blended emulsifier=the weight portion proportioning joined in the reactor in 1: 1, be warming up to 50 ℃, divide two batches of water that add 40 ℃ again, mix the back and add the polyvinyl alcohol thickening stabilizing agent, cross homogenizer, emulsification gets that solid content is 30%, H
2O is 70% defoamer.
Embodiment 4:
Synthesizing of a, modified siloxane
Conventional method is that the synthetic viscosity of raw material is the modified siloxane of 0.8pas with octamethylcy-clotetrasiloxane, potassium hydroxide, absolute ethyl alcohol, hydrochloric acid, oxyalkylene;
Synthesizing of b, blended emulsifier
Getting aliphatic acid respectively is C
10Acid, fatty alcohol are C
8The pure and mild catalyst NaOH that accounts for gross weight 01.0% is inserted in the reactor, and heat fused is evacuated to behind the 2800pa with nitrogen sweep still three times, each inflated with nitrogen to 0.3Mpa, vacuumizes then; Press organic acid again: the proportioning of oxirane=1: 15mol adds oxirane, stirring also is heated to 20 ℃, treat that reacting ethylene oxide finishes the logical nitrogen in back to the vexed still of 0.2Mpa 20 minutes, blowing, be neutralized to PH=5.5 with oxalic acid again, add 0.8% active carbon that accounts for the reactant gross weight, press filtration gets emulsifying agent; Be C with various emulsifying agents according to aliphatic acid again
10Acid, polyethylene glycol-(O-CH
2-CH
2-)
n-n be 20 fatty acid polyethylene glycol ester: fatty alcohol is C
8Alcohol, polyethylene glycol-(O-CH
2-CH
2-)
n-in n be 20 AEO: the atactic polymer of isomerous tridecanol propylene oxide: glycerol monolaurate=1: 1.5: 0.1: 1.5 ratio mix blended emulsifier, standby.
C. the preparation of defoamer
Modified siloxane with a, the preparation of b operation: blended emulsifier=the weight portion proportioning joined in the reactor in 1: 2, be warming up to 40 ℃, add 60 ℃ water more in three batches, mix the back and add the methylcellulose thickening stabilizing agent, cross homogenizer, emulsification gets that solid content is 60%, H
2O is 40% defoamer.
Embodiment 5:
Synthesizing of a, modified siloxane
Conventional method is that the synthetic viscosity of raw material is the modified siloxane of 1.2pas with octamethylcy-clotetrasiloxane, potassium hydroxide, absolute ethyl alcohol, hydrochloric acid, oxyalkylene;
Synthesizing of b, blended emulsifier
Getting aliphatic acid respectively is C
18Acid, fatty alcohol are C
18Alcohol, polyethylene glycol-(O-CH
2-CH
2-)
n-in n be that 5 AEO and the catalyst potassium hydroxide that accounts for gross weight 0.5% are inserted in the reactor, heat fused is evacuated to behind the 2500pa with nitrogen sweep still three times, each inflated with nitrogen to 0.4Mpa, vacuumizes then; Press amine again: the proportioning of oxirane=1: 10mol adds oxirane, stirs and be heated to 90 ℃, treats that reacting ethylene oxide finishes the logical nitrogen in back to the vexed still of 0.3Mpa 40 minutes, blowing, be neutralized to PH=6 with oxalic acid again, add 0.8% atlapulgite that accounts for the reactant gross weight, press filtration gets emulsifying agent; Be C with various emulsifying agents according to aliphatic acid again
18Acid, polyethylene glycol-(O-CH
2-CH
2-)
n-n be 5 fatty acid polyethylene glycol ester: fatty alcohol is C
18Alcohol, polyethylene glycol-(O-CH
2-CH
2-)
n-in n be 5 AEO: the atactic polymer of isomerous tridecanol ethylene oxide: glyceryl oleate=1: 0.7: 1.0: 0.2 ratio mix blended emulsifier, standby.
C. the preparation of defoamer
Modified siloxane with a, the preparation of b operation: blended emulsifier=the weight portion proportioning joined in the reactor in 1: 1.0, be warming up to 50 ℃, add 40 ℃ water more in three batches, mix the back and add the polyvinyl alcohol thickening stabilizing agent, cross homogenizer, emulsification gets that solid content is 30%, H
2O is 90% defoamer.
Claims (9)
1, novel fire resistant organosilicon emulsion defoaming agents is characterized in that it is is the modified siloxane of 0.5～2pas by viscosity: the liquid emulsion that blended emulsifier=1: 0.2～1.3 raw materials in weight portion that contain the polymer of oxyalkylene of a kind of organic acid or a kind of alcohol or a kind of amine and fatty acid glyceride at least are composite, form with water and milkization.
2, novel fire resistant organosilicon emulsion defoaming agents according to claim 1 is characterized in that described blended emulsifier is fatty acids polyoxyethylene ester or its polyoxyethylene polyoxypropylene ester: AEO or its polyoxyethylene polyoxypropylene ether: isomerous tridecanol atactic polyether: fatty acid glyceride=1: 0.1-1.5: 0.1-1.5: the mixture of 0.1-1.5 weight portion proportioning.
3, novel fire resistant organosilicon emulsion defoaming agents according to claim 2 is characterized in that aliphatic acid is C in the described polyoxyethylene carboxylate
10～C
18Acid, polyoxyethylene segment-(O-C
2H
4-)
n-or its polyoxypropylene oxygen ethene segment-(O-C
3H
6-O-C
2H
4-)
n-in n be 5～20.
4, novel fire resistant organosilicon emulsion defoaming agents according to claim 2 is characterized in that fatty alcohol is C in the described AEO
8～C
18Alcohol, polyoxyethylene segment-(O-CH
2-CH
2-)
n-or its polyoxyethylene polyoxypropylene segment-(O-C
3H
6-O-C
2H
4-)
n-in n be 5～20.
5, novel fire resistant organosilicon emulsion defoaming agents according to claim 2, it is characterized in that atactic polyether in the described isomerous tridecanol atactic polyether is meant the atactic polymer by ethylene oxide, propylene oxide, alcohol is 5～25 with the mol ratio of oxyalkylene.
6, novel fire resistant organosilicon emulsion defoaming agents according to claim 2 is characterized in that the aliphatic acid in the described fatty acid glyceride is oleic acid, laurate and stearic acid, is respectively monoesters, dibasic acid esters and three esters of glycerine.
7, novel fire resistant organosilicon emulsion defoaming agents according to claim 1 is characterized in that siloxanes can be dimethyl siloxane or Methylethyl siloxanes in the described modified siloxane, and its chain number is between 10-200; Contained methyl oxygen ethene silica chain number or oxygen ethene siloxane chain joint number or sum of the two are between 5-30 in the modified siloxane.
8, the synthetic method of the novel fire resistant organosilicon emulsion defoaming agents of claim 1 is characterized in that
Synthesizing of a, modified siloxane
Conventional method is that the synthetic viscosity of raw material is the modified siloxane of 0.5～2pas with octamethylcy-clotetrasiloxane, highly basic, absolute ethyl alcohol, hydrochloric acid, propylene oxide, ethylene oxide;
The preparation of b, blended emulsifier
With various emulsifying agent polyoxyethylene carboxylates or its polyoxyethylene polyoxypropylene ester: AEO or its polyoxyethylene polyoxypropylene ether: isomerous tridecanol atactic polyether: fatty acid glyceride=1: 0.1-1.5: 0.1-1.5: in the mixing kettle that 0.1-1.5 weight portion proportioning input band stirs, heating and melting, stirring and evenly mixing is incubated standby.
The preparation of c, defoamer
Modified siloxane with a, the preparation of b operation: blended emulsifier=1: 0.2～1.3 weight portion proportionings join in the reactor, be heated to 40～80 ℃, the water that in batches adds 40～80 ℃ again, mix the back and add polyvinyl alcohol or methylcellulose class thickening stabilizing agent, cross homogenizer, it is 10-60%, H that emulsification gets solid content
2O is the defoamer of 90-40%.
9, the synthetic method of novel fire resistant organosilicon emulsion defoaming agents according to claim 8 is characterized in that described highly basic is sodium methoxide, caustic alcohol, KOH and NaOH.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903951B (en) * | 2006-07-28 | 2010-05-12 | 南京四新科技应用研究所有限公司 | Improved non-organic silicone paint antifoaming agent and its preparation method |
| CN101602977B (en) * | 2009-05-26 | 2012-06-20 | 锦州康泰润滑油添加剂有限公司 | Defoaming agent composition for lubricating oil and preparation method thereof |
| CN103768833A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Delay coking high temperature defoaming agent and its application |
| CN107106939A (en) * | 2014-12-30 | 2017-08-29 | 凯米罗总公司 | Defoaming composition and its preparation and application comprising hydroxy-end capped siloxanes |
| CN109745738A (en) * | 2017-11-08 | 2019-05-14 | 丹阳市博元安全生产服务有限公司 | A kind of high temperature resistant defoaming agent and preparation method thereof |
| CN109836593A (en) * | 2019-02-15 | 2019-06-04 | 龙口市易久化工科技有限公司 | A kind of silicone-modified low-molecular-weight polyolefin water-borne dispersions and its preparation process |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SE9301347A0 (en) * | 1992-04-27 | 1993-10-28 | Nikko Chemical Inst Inc | Anti-foaming composition of emulsion type and anti-foaming method using the same |
| US6083998A (en) * | 1998-04-24 | 2000-07-04 | Betzdearborn Inc. | Defoamer and methods of use thereof |
| DE60204222T2 (en) * | 2001-03-21 | 2006-01-26 | Dow Corning Asia, Ltd. | SILICON ANTIFOAMS |
| WO2004101103A1 (en) * | 2003-05-15 | 2004-11-25 | San Nopco Ltd. | Surfactant and process for producing the same |
| CN1250313C (en) * | 2004-09-22 | 2006-04-12 | 曹治平 | High-temperature defoamer and its preparation |
-
2005
- 2005-05-20 CN CNB2005100435678A patent/CN100355478C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903951B (en) * | 2006-07-28 | 2010-05-12 | 南京四新科技应用研究所有限公司 | Improved non-organic silicone paint antifoaming agent and its preparation method |
| CN101602977B (en) * | 2009-05-26 | 2012-06-20 | 锦州康泰润滑油添加剂有限公司 | Defoaming agent composition for lubricating oil and preparation method thereof |
| CN103768833A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Delay coking high temperature defoaming agent and its application |
| CN103768833B (en) * | 2012-10-24 | 2015-06-17 | 中国石油化工股份有限公司 | Delay coking high temperature defoaming agent and its application |
| CN107106939A (en) * | 2014-12-30 | 2017-08-29 | 凯米罗总公司 | Defoaming composition and its preparation and application comprising hydroxy-end capped siloxanes |
| CN107106939B (en) * | 2014-12-30 | 2019-04-12 | 凯米罗总公司 | Defoaming composition and its preparation and application comprising hydroxy-end capped siloxanes |
| CN109745738A (en) * | 2017-11-08 | 2019-05-14 | 丹阳市博元安全生产服务有限公司 | A kind of high temperature resistant defoaming agent and preparation method thereof |
| CN109836593A (en) * | 2019-02-15 | 2019-06-04 | 龙口市易久化工科技有限公司 | A kind of silicone-modified low-molecular-weight polyolefin water-borne dispersions and its preparation process |
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