CN107469411B - 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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- 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 fields, and in particular to a kind of preparation method of organic silicon defoamer.The present invention is using silicone oil as base-material; it is modified using methylvinyldichlorosilane monomer; increase the silicon oxygen bond in silicone oil, reuses 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 under the action of ammonium glycyrrhetate, the strong hydro-oleophobicity for defoaming agent of having releived; stability is increased, the appearance of the lamination of defoaming agent is prevented.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of preparation method of organic silicon defoamer.
Background technique
Defoaming agent is a kind of widely used fine chemicals, is mainly used for eliminating and inhibiting various unwanted bubbles.As
Defoaming agent should have insoluble in foam liquid or indissoluble, surface tension lower than foam liquid, with foam liquid have certain compatibility, with
Chemical reaction and the small grade fundamental characteristics of volatility do not occur for foam liquid.There are many type of defoaming agent, common on general industry
It is broadly divided into three classes: organic defoaming agent (alcohols, lipid, amide 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,
The advantages that preferable chemistry and thermal stability, outstanding antifoaming performance, receives significant attention, 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 is subject to certain restrictions it in the application of the industries such as biofermentation, copy paper, printing and dyeing.Polyethers defoaming
Agent is by ethylene oxide, a kind of nonionic surfactant of function admirable made from propylene oxide ring-opening polymerisation.It is widely used in
In aqueous systems, there are good hydrophily and antifoaming ability.But its antifoaming speed is not good enough, and temperature sensitive, need to cloud point with
Upper use.Inhibiting the common method of these foams is addition polyether antifoam agent or organic silicon defoamer, the defoaming of polyethers defoaming agent
Ability is weak, and foam inhibition ability is strong, and organic silicon defoaming agent brokenly bubble power is strong, antifoaming speed is fast, but foam inhibition ability is weak.But individually make
With polyether antifoam agent or the defoaming agent of organosilicon, defoaming and foam inhibition persistence duality immediately can not be often had both 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 defoaming agents are simply mixed, not only comprehensive performance is still not ideal enough, but also this defoaming agent stability often exists
Problem, the generation for phenomena such as will lead to layering, when addition, will cause different periods antifoam content and the uneven situation of performance.
Summary of the invention
The technical problems to be solved by the invention: for current defoaming agent be by organic silicon defoamer and polyether antifoam agent into
Row is simply mixed, and easily leads to that defoaming agent is unstable, and the problem of layering, the present invention provides a kind of systems of organic silicon defoamer
Preparation Method.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of preparation method of organic silicon defoamer, the preparation method include the following steps:
(1) according to parts by weight, 80~90 parts of silicone oil, 30~35 parts of linolenic acids, 20~25 parts of methyl ethylene dichloros are taken
Silicone oil, linolenic acid and additive, are put by silane, 8~11 parts of maleic anhydrides, 4~7 parts of catalyst and 1~3 part of additive first
In reactor, using nitrogen protection, preheated at 60~65 DEG C；
(2) after preheating, methylvinyldichlorosilane, maleic anhydride, catalyst is added, is warming up to 90~95 DEG C
Under reacted, it is cooling, collect reaction mixture；
(3) reaction mixture, allyl polyethenoxy ether and dimethylbenzene are put into reaction kettle, use sodium hydroxide solution
PH to 8.0~8.5 is adjusted, 1.2~1.5MPa is boosted to using carbon dioxide, is stirred at 80~95 DEG C:
(4) after stirring, emulsifier and ammonium glycyrrhetate is added, is warming up at 108~115 DEG C, is reacted, out
Material, collects out material, filters, and collects filtered fluid, and distill to filtered fluid, recycles dimethylbenzene, collects distillation residue, i.e.,
Obtain organic silicon defoamer.
Catalyst is alumina silicate, any one in lewis acid in the step (1).
The step (1) is that additive is titanium dioxide, any one in phosphomolybdic acid.
The mass ratio of step (3) reaction mixture, allyl polyethenoxy ether and dimethylbenzene is 8~11:3~5:
13。
The additional amount of emulsifier is the 1~1.2% of reaction mixture quality, the addition of ammonium glycyrrhetate in the step (4)
Amount is the 0.6~1.0% of reaction mixture quality, and emulsifier is any one in stearoyl lactate or stearyl lactate
Kind.
The present invention is compared with other methods, and advantageous effects are:
The present invention is modified it using methylvinyldichlorosilane monomer using silicone oil as base-material, increases silicone oil
In silicon oxygen bond, reuse maleic anhydride and protected, increase its acid-proof alkaline, then by with allyl polyethenoxy ether
Carry out graft reaction, form Polyether Modified Polysiloxanes Defoaming Agent, while under the action of ammonium glycyrrhetate, defoaming agent of having releived it is strong
Hydro-oleophobicity increases stability, prevents the appearance of the lamination of defoaming agent.
Specific embodiment
Catalyst is selected as alumina silicate, any one in lewis acid.
Additive is selected as titanium dioxide, any one in phosphomolybdic acid.
Any one being selected as in stearoyl lactate or stearyl lactate of emulsifier.
A kind of preparation method of organic silicon defoamer, the preparation method include the following steps:
(1) according to parts by weight, 80~90 parts of silicone oil, 30~35 parts of linolenic acids, 20~25 parts of methyl ethylene dichloros are taken
Silicone oil, linolenic acid and additive, are put by silane, 8~11 parts of maleic anhydrides, 4~7 parts of catalyst and 1~3 part of additive first
In reactor, using nitrogen protection, 30~35min is preheated at 60~65 DEG C；
(2) after preheating, methylvinyldichlorosilane, maleic anhydride, catalyst is added, is warming up to 90~95 DEG C
Under carry out 2~4h of reaction, it is cooling, collect reaction mixture；
(3) it is in mass ratio 8~11:3~5:13, reaction mixture, allyl polyethenoxy ether and dimethylbenzene is put into
In reaction kettle, pH to 8.0~8.5 is adjusted using sodium hydroxide solution, 1.2~1.5MPa is boosted to using carbon dioxide, 80
1~3h is stirred at~95 DEG C:
(4) after stirring, emulsifier and ammonium glycyrrhetate is added, the additional amount of emulsifier is reaction mixture quality
1~1.2%, the additional amount of ammonium glycyrrhetate is the 0.6~1.0% of reaction mixture quality, is warming up at 108~115 DEG C, is carried out
4~6h is reacted, material is collected out in discharging, is filtered, and collects filtered fluid, and distill to filtered fluid, recycles dimethylbenzene, is collected
Residue is distilled to get organic silicon defoamer.
Example 1
Catalyst is selected as alumina silicate.
Additive is selected as phosphomolybdic acid.
Emulsifier is selected as stearyl lactate.
A kind of preparation method of organic silicon defoamer, the preparation method include the following steps:
(1) according to parts by weight, 85 parts of silicone oil, 33 parts of linolenic acids, 23 parts of methylvinyldichlorosilanes, 10 parts of Malaysias are taken
Silicone oil, linolenic acid and additive, are put into reactor by acid anhydrides, 5 parts of catalyst and 2 parts of additives first, using nitrogen protection,
33min is preheated at 63 DEG C；
(2) after preheating, be added methylvinyldichlorosilane, maleic anhydride, catalyst, be warming up at 93 DEG C into
Row reaction 3h, cooling, collection reaction mixture；
(3) it is in mass ratio 9:4:13, reaction mixture, allyl polyethenoxy ether and dimethylbenzene is put into reaction kettle
In, pH to 8.3 is adjusted using sodium hydroxide solution, 1.3MPa is boosted to using carbon dioxide, stirs 2h at 85 DEG C:
(4) after stirring, emulsifier and ammonium glycyrrhetate is added, the additional amount of emulsifier is reaction mixture quality
1.1%, the additional amount of ammonium glycyrrhetate is the 0.8% of reaction mixture quality, is warming up at 140 DEG C, carries out reaction 5h, is discharged,
Collect out material, filter, collect filtered fluid, and filtered fluid is distilled, recycle dimethylbenzene, collect distillation residue to get
Organic silicon defoamer.
Example 2
Catalyst is selected as alumina silicate, any one in lewis acid.
Additive is selected as titanium dioxide, any one in phosphomolybdic acid.
Any one being selected as in stearoyl lactate or stearyl lactate of emulsifier.
A kind of preparation method of organic silicon defoamer, the preparation method include the following steps:
(1) according to parts by weight, 90 parts of silicone oil, 35 parts of linolenic acids, 25 parts of methylvinyldichlorosilanes, 11 parts of Malaysias are taken
Silicone oil, linolenic acid and additive, are put into reactor by acid anhydrides, 7 parts of catalyst and 3 parts of additives first, using nitrogen protection,
35min is preheated at 65 DEG C；
(2) after preheating, be added methylvinyldichlorosilane, maleic anhydride, catalyst, be warming up at 95 DEG C into
Row reaction 4h, cooling, collection reaction mixture；
(3) it is in mass ratio 11:5:13, reaction mixture, allyl polyethenoxy ether and dimethylbenzene is put into reaction kettle
In, pH to 8.5 is adjusted using sodium hydroxide solution, 1.5MPa is boosted to using carbon dioxide, stirs 3h at 95 DEG C:
(4) after stirring, emulsifier and ammonium glycyrrhetate is added, the additional amount of emulsifier is reaction mixture quality
1.2%, the additional amount of ammonium glycyrrhetate is the 1.0% of reaction mixture quality, is warming up at 115 DEG C, carries out reaction 6h, is discharged,
Collect out material, filter, collect filtered fluid, and filtered fluid is distilled, recycle dimethylbenzene, collect distillation residue to get
Organic silicon defoamer.
Example 3
Catalyst is selected as alumina silicate.
Additive is selected as titanium dioxide.
Emulsifier is selected as stearoyl lactate.
A kind of preparation method of organic silicon defoamer, the preparation method include the following steps:
(1) according to parts by weight, 80 parts of silicone oil, 30 parts of linolenic acids, 20 parts of methylvinyldichlorosilanes, 8 parts of Malaysias are taken
Silicone oil, linolenic acid and additive, are put into reactor by acid anhydrides, 4 parts of catalyst and 1 part of additive first, using nitrogen protection,
30min is preheated at 60 DEG C；
(2) after preheating, be added methylvinyldichlorosilane, maleic anhydride, catalyst, be warming up at 90 DEG C into
Row reaction 2h, cooling, collection reaction mixture；
(3) it is in mass ratio 8:3:13, reaction mixture, allyl polyethenoxy ether and dimethylbenzene is put into reaction kettle
In, pH to 8.0 is adjusted using sodium hydroxide solution, 1.2MPa is boosted to using carbon dioxide, stirs 1h at 80 DEG C；
(4) after stirring, emulsifier and ammonium glycyrrhetate is added, the additional amount of emulsifier is reaction mixture quality
1%, the additional amount of ammonium glycyrrhetate is the 0.6% of reaction mixture quality, is warming up at 108 DEG C, carries out reaction 4h, is discharged, and is received
Collect material out, filter, collect filtered fluid, and distill to filtered fluid, recycle dimethylbenzene, collects distillation residue to get having
Machine silicon defoaming agent.
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 compared into test, in the amount of 100ml
The expanding foam solution of 50ml is added in cylinder, adds the defoaming liquid of 0.2g, closes the lid, rock, observation comparison.
Defoaming agent 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 foam inhibition time/min | 16.8 | 18.5 | 20.0 | 12.3 |
| High-temperature stability | There is floating oil | There is oil slick | Stablize | Floating oil is obvious |
| Low-temperature stability | Stablize | Stablize | Stablize | There is precipitate |
| Centrifugal stability | 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 problem of present invention defoaming agent performance produced is stablized, is not susceptible to layering, is worthy to be popularized and makes
With.
Claims (5)
1. a kind of preparation method of organic silicon defoamer, which is characterized in that the preparation method includes the following steps:
Step (1): according to parts by weight, 80~90 parts of silicone oil, 30~35 parts of linolenic acids, 20~25 parts of methyl ethylene dichloros are taken
Silicone oil, linolenic acid and additive, are put by silane, 8~11 parts of maleic anhydrides, 4~7 parts of catalyst and 1~3 part of additive first
In reactor, using nitrogen protection, preheated at 60~65 DEG C；
Step (2): after preheating, methylvinyldichlorosilane, maleic anhydride, catalyst is added, is warming up to 90~95
It is reacted at DEG C, it is cooling, collect reaction mixture；
Step (3): reaction mixture, allyl polyethenoxy ether and dimethylbenzene are put into reaction kettle, molten using sodium hydroxide
Liquid adjusts pH to 8.0~8.5, boosts to 1.2~1.5MPa using carbon dioxide, stirs at 80~95 DEG C:
Step (4): after stirring, emulsifier and ammonium glycyrrhetate is added, the additional amount of the ammonium glycyrrhetate is reaction mixing
The 0.6~1.0% of amount of substance；It is warming up at 108~115 DEG C, is reacted, discharge, collect out material, filter, collect filtering
Liquid, and filtered fluid is distilled, dimethylbenzene is recycled, collects distillation residue to get organic silicon defoamer.
2. the preparation method of organic silicon defoamer according to claim 1, which is characterized in that catalyst in the step (1)
For any one in alumina silicate, lewis acid.
3. the preparation method of organic silicon defoamer according to claim 1, which is characterized in that step (1) additive is
Any one in titanium dioxide, phosphomolybdic acid.
4. the preparation method of organic silicon defoamer according to claim 1, which is characterized in that step (3) the reaction mixing
The mass ratio of object, allyl polyethenoxy ether and dimethylbenzene is 8~11:3~5:13.
5. the preparation method of organic silicon defoamer according to claim 1, which is characterized in that emulsifier in the step (4)
Additional amount be the 1~1.2% of reaction mixture quality, emulsifier is any in stearoyl lactate or stearyl lactate
It is a kind of.
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| 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 |
| CN111748327B (en) * | 2020-06-30 | 2022-10-18 | 中国石油天然气集团有限公司 | Environment-friendly defoaming agent for drilling fluid and preparation method thereof |
| CN111713493B (en) * | 2020-07-23 | 2021-10-29 | 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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| 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 |
| CN100457803C (en) * | 2006-11-28 | 2009-02-04 | 苏州大学 | Fluoric alkoxyl propyl methyl silicone oil and its prepn process |
| CN105531005B (en) * | 2013-08-13 | 2018-12-28 | 美国陶氏有机硅公司 | The method for forming defoaming agent particle |
| CN104436767B (en) * | 2014-12-24 | 2016-05-18 | 江苏四新科技应用研究所股份有限公司 | A kind of silicon composition and preparation thereof, application |
| 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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