CN107469411A - A kind of preparation method of organic silicon defoamer - Google Patents
A kind of preparation method of organic silicon defoamer Download PDFInfo
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- CN107469411A CN107469411A CN201710873378.6A CN201710873378A CN107469411A CN 107469411 A CN107469411 A CN 107469411A CN 201710873378 A CN201710873378 A CN 201710873378A CN 107469411 A CN107469411 A CN 107469411A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
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Abstract
The invention belongs to chemical technology field, and in particular to a kind of preparation method of organic silicon defoamer.The present invention is used as base-material using silicone oil; it is modified using methylvinyldichlorosilane monomer; increase the silicon oxygen bond in silicone oil, reuse maleic anhydride and protected, increase its acid-proof alkaline; then by carrying out graft reaction with allyl polyethenoxy ether; Polyether Modified Polysiloxanes Defoaming Agent is formed, while in the presence of ammonium glycyrrhetate, the strong hydro-oleophobicity for defoamer of having releived; stability is added, prevents the appearance of the lamination of defoamer.
Description
Technical field
The invention belongs to chemical technology field, and in particular to a kind of preparation method of organic silicon defoamer.
Background technology
Defoamer is a kind of widely used fine chemicals, is mainly used in eliminating and suppresses various unwanted bubbles.As
Defoamer should possess insoluble in foam liquid or indissoluble, surface tension less than foam liquid, with foam liquid have certain compatibility, with
Foam liquid does not occur to chemically react and the fundamental characteristics such as volatility is small.The species of defoamer is a lot, is commonly used on general industry
It is broadly divided into three classes：Organic defoamer（Alcohols, lipid, acid amides etc.）, organic silicon defoamer and polyether antifoam agent.It is wherein organic
Silicon and polyether antifoam agent application field are the most extensive, and dosage is also larger.Organic silicon defoamer with its slightly solubility, low surface tension,
Preferably chemistry and receive significant attention the advantages that heat endurance, outstanding antifoaming performance, whether aqueous systems or
There are defoaming suds suppressing properties well in non-aqueous system.But due to its siloxane main chain in the environment of strong acid and strong base easy fracture and
The strong hydro-oleophobicity of itself makes it be subject to certain restrictions in the application of the industries such as biofermentation, copy paper, printing and dyeing.Polyethers defoams
Agent is by oxirane, a kind of nonionic surfactant of function admirable made from expoxy propane ring-opening polymerisation.It is widely used in
In aqueous systems, there is good hydrophily and suds.But its antifoaming speed is not good enough, and temperature sensitive, need to cloud point with
Upper use.It is addition polyether antifoam agent or organic silicon defoamer to suppress the conventional method of these foams, and polyethers defoamer defoams
Ability is weak, and suds ability is strong, and organic silicon defoamer brokenly bubble power is strong, antifoaming speed is fast, but suds ability is weak.But individually make
With polyether antifoam agent or the defoamer of organosilicon, defoaming and suds persistence duality immediately can not be often had concurrently simultaneously
Matter.Therefore the producer having sells after mixing organic silicon defoamer and polyether antifoam agent, to obtain preferable resultant effect, but
Only two kinds of defoamers are simply mixed, not only combination property is still not ideal enough, and this defoamer stability is often present
Problem, the generation for phenomena such as causing layering, can cause different periods antifoam content and performance uneven situation during addition.
The content of the invention
The technical problems to be solved by the invention：It is to enter organic silicon defoamer and polyether antifoam agent for current defoamer
Row is simply mixed, and is easily caused that defoamer is unstable, and the problem of layering, the invention provides a kind of system of organic silicon defoamer
Preparation Method.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
A kind of preparation method of organic silicon defoamer, the preparation method comprise the following steps：
（1）Count in parts by weight, take 80~90 parts of silicone oil, 30~35 parts of leukotrienes, 20~25 parts of methylvinyldichlorosilanes,
8~11 parts of maleic anhydrides, 4~7 parts of catalyst and 1~3 part of additive, are put into reaction by silicone oil, leukotrienes and additive first
In device, protected using nitrogen, preheated at 60~65 DEG C；
（2）After preheating terminates, methylvinyldichlorosilane, maleic anhydride, catalyst are added, is warming up at 90~95 DEG C
Row reaction, cooling, collects reactant mixture；
（3）Reactant mixture, allyl polyethenoxy ether and dimethylbenzene are put into reactor, adjusted using sodium hydroxide solution
PH to 8.0~8.5,1.2~1.5MPa is boosted to using carbon dioxide, stirred at 80~95 DEG C：
（4）After stirring terminates, emulsifying agent and ammonium glycyrrhetate are added, is warming up at 108~115 DEG C, is reacted, discharged, received
Collect material, filter, collect filtered fluid, and filtered fluid is distilled, reclaim dimethylbenzene, collect distillation residue, produced
Machine silicon defoaming agent.
The step（1）Middle catalyst is any one in alumina silicate, lewis acid.
The step（1）It is any one in titanium dioxide, phosphomolybdic acid for additive.
The step（3）The mass ratio of reactant mixture, allyl polyethenoxy ether and dimethylbenzene is 8~11：3~5：
13。
The step（4）The addition of middle emulsifying agent is the 1~1.2% of reactant mixture quality, the addition of ammonium glycyrrhetate
Measure as the 0.6~1.0% of reactant mixture quality, emulsifying agent is any one in stearoyl lactate or CSL
Kind.
Compared with other method, advantageous effects are the present invention：
The present invention is modified using silicone oil as base-material using methylvinyldichlorosilane monomer to it, is increased in silicone oil
Silicon oxygen bond, reuse maleic anhydride and protected, increase its acid-proof alkaline, then by being carried out with allyl polyethenoxy ether
Graft reaction, form Polyether Modified Polysiloxanes Defoaming Agent, while in the presence of ammonium glycyrrhetate, defoamer of having releived it is strong hydrophobic
Oleophobic property, stability is added, prevent the appearance of the lamination of defoamer.
Embodiment
The selection of catalyst is any one in alumina silicate, lewis acid.
The selection of additive is any one in titanium dioxide, phosphomolybdic acid.
The selection of emulsifying agent is any one in stearoyl lactate or CSL.
A kind of preparation method of organic silicon defoamer, the preparation method comprise the following steps：
（1）Count in parts by weight, take 80~90 parts of silicone oil, 30~35 parts of leukotrienes, 20~25 parts of methylvinyldichlorosilanes,
8~11 parts of maleic anhydrides, 4~7 parts of catalyst and 1~3 part of additive, are put into reaction by silicone oil, leukotrienes and additive first
In device, protected using nitrogen, 30~35min is preheated at 60~65 DEG C；
（2）After preheating terminates, methylvinyldichlorosilane, maleic anhydride, catalyst are added, is warming up at 90~95 DEG C
Row 2~4h of reaction, cooling, collects reactant mixture；
（3）It is 8~11 in mass ratio：3~5：13, reactant mixture, allyl polyethenoxy ether and dimethylbenzene are put into reaction
In kettle, pH to 8.0~8.5 is adjusted using sodium hydroxide solution, 1.2~1.5MPa is boosted to using carbon dioxide, 80~95
1~3h is stirred at DEG C：
（4）After stirring terminates, add emulsifying agent and ammonium glycyrrhetate, the addition of emulsifying agent for reactant mixture quality 1~
1.2%, the addition of ammonium glycyrrhetate is the 0.6~1.0% of reactant mixture quality, is warming up at 108~115 DEG C, is carried out anti-
4~6h is answered, discharges, collects out material, is filtered, collects filtered fluid, and filtered fluid is distilled, reclaims dimethylbenzene, collects and steams
Residue is evaporated, produces organic silicon defoamer.
Example 1
The selection of catalyst is alumina silicate.
The selection of additive is phosphomolybdic acid.
The selection of emulsifying agent is CSL.
A kind of preparation method of organic silicon defoamer, the preparation method comprise the following steps：
（1）Count in parts by weight, take 85 parts of silicone oil, 33 parts of leukotrienes, 23 parts of methylvinyldichlorosilanes, 10 parts of maleic acids
Silicone oil, leukotrienes and additive, are put into reactor, are protected using nitrogen by acid anhydride, 5 parts of catalyst and 2 parts of additives first,
33min is preheated at 63 DEG C；
（2）After preheating terminates, methylvinyldichlorosilane, maleic anhydride, catalyst are added, is warming up at 93 DEG C and carries out instead
3h is answered, is cooled down, collects reactant mixture；
（3）It is 9 in mass ratio：4：13, reactant mixture, allyl polyethenoxy ether and dimethylbenzene are put into reactor, made
PH to 8.3 is adjusted with sodium hydroxide solution, 1.3MPa is boosted to using carbon dioxide, 2h is stirred at 85 DEG C：
（4）After stirring terminates, emulsifying agent and ammonium glycyrrhetate are added, the addition of emulsifying agent is reactant mixture quality
1.1%, the addition of ammonium glycyrrhetate is the 0.8% of reactant mixture quality, is warming up at 140 DEG C, carries out reaction 5h, is discharged,
Material is collected out, is filtered, collects filtered fluid, and filtered fluid is distilled, reclaims dimethylbenzene, distillation residue is collected, produces
Organic silicon defoamer.
Example 2
The selection of catalyst is any one in alumina silicate, lewis acid.
The selection of additive is any one in titanium dioxide, phosphomolybdic acid.
The selection of emulsifying agent is any one in stearoyl lactate or CSL.
A kind of preparation method of organic silicon defoamer, the preparation method comprise the following steps：
（1）Count in parts by weight, take 90 parts of silicone oil, 35 parts of leukotrienes, 25 parts of methylvinyldichlorosilanes, 11 parts of maleic acids
Silicone oil, leukotrienes and additive, are put into reactor, are protected using nitrogen by acid anhydride, 7 parts of catalyst and 3 parts of additives first,
35min is preheated at 65 DEG C；
（2）After preheating terminates, methylvinyldichlorosilane, maleic anhydride, catalyst are added, is warming up at 95 DEG C and carries out instead
4h is answered, is cooled down, collects reactant mixture；
（3）It is 11 in mass ratio：5：13, reactant mixture, allyl polyethenoxy ether and dimethylbenzene are put into reactor, made
PH to 8.5 is adjusted with sodium hydroxide solution, 1.5MPa is boosted to using carbon dioxide, 3h is stirred at 95 DEG C：
（4）After stirring terminates, emulsifying agent and ammonium glycyrrhetate are added, the addition of emulsifying agent is reactant mixture quality
1.2%, the addition of ammonium glycyrrhetate is the 1.0% of reactant mixture quality, is warming up at 115 DEG C, carries out reaction 6h, is discharged,
Material is collected out, is filtered, collects filtered fluid, and filtered fluid is distilled, reclaims dimethylbenzene, distillation residue is collected, produces
Organic silicon defoamer.
Example 3
The selection of catalyst is alumina silicate.
The selection of additive is titanium dioxide.
The selection of emulsifying agent is stearoyl lactate.
A kind of preparation method of organic silicon defoamer, the preparation method comprise the following steps：
（1）Count in parts by weight, take 80 parts of silicone oil, 30 parts of leukotrienes, 20 parts of methylvinyldichlorosilanes, 8 parts of maleic anhydrides,
Silicone oil, leukotrienes and additive, are put into reactor, are protected using nitrogen, 60 by 4 parts of catalyst and 1 part of additive first
30min is preheated at DEG C；
（2）After preheating terminates, methylvinyldichlorosilane, maleic anhydride, catalyst are added, is warming up at 90 DEG C and carries out instead
2h is answered, is cooled down, collects reactant mixture；
（3）It is 8 in mass ratio：3：13, reactant mixture, allyl polyethenoxy ether and dimethylbenzene are put into reactor, made
PH to 8.0 is adjusted with sodium hydroxide solution, 1.2MPa is boosted to using carbon dioxide, 1h is stirred at 80 DEG C；
（4）After stirring terminates, emulsifying agent and ammonium glycyrrhetate are added, the addition of emulsifying agent is the 1% of reactant mixture quality,
The addition of ammonium glycyrrhetate is the 0.6% of reactant mixture quality, is warming up at 108 DEG C, carries out reaction 4h, discharges, collects out
Material, filtering, filtered fluid is collected, and filtered fluid is distilled, reclaim dimethylbenzene, collected distillation residue, produce organosilicon
Defoamer.
Comparative example：The organic silicon defoamer of Changzhou chemical company production
Method：Organic silicon defoamer prepared by embodiment 1,2,3 and comparative example is subjected to contrast test, in 100ml graduated cylinder
50ml expanding foam solution is added, 0.2g defoaming liquid is added, closes the lid, rock, observation contrast.
Defoamer detection case table such as table 1
Table 1
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Foam time/s | 18.2 | 19.6 | 22.5 | 15.4 |
| The suds time/min | 16.8 | 18.5 | 20.0 | 12.3 |
| High-temperature stability | There is floating oil | There is oil slick | It is stable | Floating oil is obvious |
| Low-temperature stability | It is stable | It is stable | It is stable | There is precipitate |
| Dewatering ability | It is not stratified | It is not stratified | It is not stratified | Slightly it is layered |
From the foregoing, it will be observed that the defoamer stable performance that the present invention is produced, the problem of being not susceptible to be layered, is worthy to be popularized and uses.
Claims (5)
1. a kind of preparation method of organic silicon defoamer, it is characterised in that the preparation method comprises the following steps：
（1）Count in parts by weight, take 80~90 parts of silicone oil, 30~35 parts of leukotrienes, 20~25 parts of methylvinyldichlorosilanes,
8~11 parts of maleic anhydrides, 4~7 parts of catalyst and 1~3 part of additive, are put into reaction by silicone oil, leukotrienes and additive first
In device, protected using nitrogen, preheated at 60~65 DEG C；
（2）After preheating terminates, methylvinyldichlorosilane, maleic anhydride, catalyst are added, is warming up at 90~95 DEG C
Row reaction, cooling, collects reactant mixture；
（3）Reactant mixture, allyl polyethenoxy ether and dimethylbenzene are put into reactor, adjusted using sodium hydroxide solution
PH to 8.0~8.5,1.2~1.5MPa is boosted to using carbon dioxide, stirred at 80~95 DEG C：
（4）After stirring terminates, emulsifying agent and ammonium glycyrrhetate are added, is warming up at 108~115 DEG C, is reacted, discharged, received
Collect material, filter, collect filtered fluid, and filtered fluid is distilled, reclaim dimethylbenzene, collect distillation residue, produced
Machine silicon defoaming agent.
2. the preparation method of organic silicon defoamer according to claim 1, it is characterised in that the step（1）Middle catalyst
For any one in alumina silicate, lewis acid.
3. the preparation method of organic silicon defoamer according to claim 1, it is characterised in that the step（1）For additive
For any one in titanium dioxide, phosphomolybdic acid.
4. the preparation method of organic silicon defoamer according to claim 1, it is characterised in that the step（3）Reaction mixing
The mass ratio of thing, allyl polyethenoxy ether and dimethylbenzene is 8~11：3~5：13.
5. the preparation method of organic silicon defoamer according to claim 1, it is characterised in that the step（4）Middle emulsifying agent
Addition be the 1~1.2% of reactant mixture quality, the addition of ammonium glycyrrhetate for reactant mixture quality 0.6~
1.0%, emulsifying agent is any one in stearoyl lactate or CSL.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108654148A (en) * | 2018-06-27 | 2018-10-16 | 芜湖凌岳企业管理咨询有限公司 | Antifoaming agent and preparation method thereof for wastewater treatment |
| CN109200632A (en) * | 2018-09-11 | 2019-01-15 | 蓝凤祥 | Multi-functional nontoxic high temperature silicone modified polyether industrial defoaming agent of one kind and preparation method thereof |
| CN109364535A (en) * | 2018-10-29 | 2019-02-22 | 薛向东 | A kind of high temperature resistant defoaming agent |
| CN111569475A (en) * | 2020-05-28 | 2020-08-25 | 南京澳莉峰环保科技有限公司 | Organic silicon emulsion defoaming agent and preparation method thereof |
| CN111713493A (en) * | 2020-07-23 | 2020-09-29 | 陕西农塔生物数据研究有限公司 | Synergistic insecticidal auxiliary agent |
| CN111748327A (en) * | 2020-06-30 | 2020-10-09 | 中国石油天然气集团有限公司 | Environment-friendly defoaming agent for drilling fluid and preparation method thereof |
| CN112143342A (en) * | 2020-10-19 | 2020-12-29 | 徐州中捷环保科技有限公司 | Metal protective coating and preparation method thereof |
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| CN106621477A (en) * | 2016-10-18 | 2017-05-10 | 合肥新万成环保科技有限公司 | Hyperbranched polyether modified organic silicon defoamer with low dosage and preparation method of defoamer |
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| DE102005006962A1 (en) * | 2005-02-16 | 2006-08-24 | Goldschmidt Gmbh | Use of polysiloxane compound containing an organo silyloxycarbon bond, as antifoaming agent for liquid fuels e.g. hydraulic-, gear oil and fuel oil |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108654148A (en) * | 2018-06-27 | 2018-10-16 | 芜湖凌岳企业管理咨询有限公司 | Antifoaming agent and preparation method thereof for wastewater treatment |
| CN109200632A (en) * | 2018-09-11 | 2019-01-15 | 蓝凤祥 | Multi-functional nontoxic high temperature silicone modified polyether industrial defoaming agent of one kind and preparation method thereof |
| CN109364535A (en) * | 2018-10-29 | 2019-02-22 | 薛向东 | A kind of high temperature resistant defoaming agent |
| CN111569475A (en) * | 2020-05-28 | 2020-08-25 | 南京澳莉峰环保科技有限公司 | Organic silicon emulsion defoaming agent and preparation method thereof |
| CN111748327A (en) * | 2020-06-30 | 2020-10-09 | 中国石油天然气集团有限公司 | Environment-friendly defoaming agent for drilling fluid and preparation method thereof |
| CN111713493A (en) * | 2020-07-23 | 2020-09-29 | 陕西农塔生物数据研究有限公司 | Synergistic insecticidal auxiliary agent |
| CN112143342A (en) * | 2020-10-19 | 2020-12-29 | 徐州中捷环保科技有限公司 | Metal protective coating and preparation method thereof |
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| CN107469411B (en) | 2019-07-26 |
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