CN112807756A - Silyl ether defoaming agent and preparation method thereof - Google Patents
Silyl ether defoaming agent and preparation method thereof Download PDFInfo
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- CN112807756A CN112807756A CN202011588593.XA CN202011588593A CN112807756A CN 112807756 A CN112807756 A CN 112807756A CN 202011588593 A CN202011588593 A CN 202011588593A CN 112807756 A CN112807756 A CN 112807756A
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- ether
- defoaming
- polysiloxane
- defoaming agent
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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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- 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
Abstract
The invention provides a silicon ether defoaming agent and a preparation method thereof, wherein the silicon ether defoaming agent is mainly prepared from the following raw materials: the adhesive comprises, by mass, 25-40 parts of polyethylene glycol ether, 30-50 parts of dimethyl silicone oil, 8-15 parts of polysiloxane, 9-11 parts of sorbitol polyoxyethylene ether stearate and 1-5 parts of a thickening agent. The silicon ether defoaming agent disclosed by the invention adopts a compound formula, and multiple components are matched for use, so that the synergistic effect is obviously increased, and the defoaming and foam inhibiting effects are excellent.
Description
Technical Field
The invention relates to the field of defoaming agents, and particularly relates to a silyl ether defoaming agent and a preparation method thereof.
Background
In the industrial production process, if a large amount of foam exists, a lot of troubles are brought to the production process, and the production capacity is greatly limited; waste of raw materials and products is caused; the quality of the product is influenced; environmental pollution, etc. Therefore, how to effectively control the foam in the production process becomes a focus of attention of researchers. Defoaming agents are now commonly used to eliminate foam generated in industrial processes.
The defoaming agents commonly used in industry can be generally classified into organic defoaming agents, silicone defoaming agents, polyether defoaming agents, and the like.
The organic silicon defoaming agent generally comprises products such as polydimethylsiloxane and the like, has the characteristics of high defoaming speed, good foam inhibition and the like, but is generally limited in application due to the defects of high price, water insolubility and the like; the silicon ether defoaming agent belongs to a nonionic surfactant, has excellent defoaming and foam inhibiting functions, is non-toxic, is insoluble in water, is soluble in an organic solvent, can be used independently, and can be prepared into emulsion for use. Among them, GPE type is particularly suitable for fermentation industry, and PPE is suitable for high temperature use. The product has the advantages of polyether and silicone defoaming agents, can defoam and inhibit foams in different media, has a defoaming effect which is 2-3 times stronger than that of a conventional defoaming agent, and has the characteristics of low toxicity, high surface activity, wide pH application range, low surface tension, high spreading speed and the like. The product can be dissolved in water in any proportion, can be subjected to high-temperature sterilization treatment, and can be widely applied to defoaming treatment in the fields of fermentation manufacturing of antibiotics, vitamins, food processing, papermaking, chemical industry, coatings, building materials, detergents and the like.
The silicon ether active agent exists in water in a molecular state, has high stability, no toxicity, good compatibility with other types of surfactants, good foam inhibition effect, emulsifying capacity and washing effect, and is widely applied to various fields of industrial departments, civil washing and the like. With the development of the petroleum industry, the yield and variety of the silicon ether active agent are continuously increasing. The molecular weight of the silicon ether active agent is generally changed greatly, the composition and the structure of the silicon ether active agent are complex, and the physical and chemical properties of the polymer are obviously changed due to the difference, so that the stability is poor.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a silicon ether defoaming agent with a simple formula, wherein the silicon ether defoaming agent has a higher boiling point, good heat resistance, good stability at high temperature, and good defoaming performance and foam inhibition performance. The problem that the foam arouses in satisfying high temperature waste water that can be fine reaches the defoaming demand, effectively prolongs the defoaming and lasts the usable time, has improved defoaming speed and production efficiency.
The second purpose of the invention is to provide the preparation method of the silyl ether antifoaming agent, which has the advantages of simple operation, mild operation conditions, no pollution, no discharge of three wastes, safety and environmental protection.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a silicon ether defoaming agent, which is mainly prepared from the following raw materials: the adhesive comprises, by mass, 25-40 parts of polyethylene glycol ether, 30-50 parts of dimethyl silicone oil, 8-15 parts of polysiloxane, 9-11 parts of sorbitol polyoxyethylene ether stearate and 1-5 parts of a thickening agent.
Preferably, as a further practicable scheme, by mass, the silicone oil comprises 30-38 parts of polyethylene glycol ether, 35-45 parts of dimethyl silicone oil, 10-13 parts of polysiloxane, 10-13 parts of sorbitol polyoxyethylene ether stearate and 2-4 parts of a thickening agent.
Preferably, as a further practicable scheme, by mass, the silicone oil comprises 35 parts of polyethylene glycol ether, 40 parts of dimethyl silicone oil, 11 parts of polysiloxane, 11 parts of sorbitol polyoxyethylene ether stearate and 3 parts of thickening agent.
In the formula of the silicon ether defoaming agent, the polyethylene glycol ether has certain hydrophilicity and extensibility, and the defoaming activity is not influenced by heating and repeated cyclic heating at a higher temperature. The defoaming agent of the invention takes polyglycol ether as a main agent, the dimethyl silicone oil mainly plays a role in coordination, the dimethyl silicone oil and polysiloxane have low molecular weight, easy diffusion and spreading, high surface activity and strong defoaming force, and the defoaming agent has the functions of foam inhibition and foam breaking for all bubble systems. The combination of the two components enhances the defoaming and foam inhibiting effect, and the practice shows that the two components are controlled in a proper addition range, so that the defoaming agent has good defoaming speed, and if the addition is too large, the hydrophilic property and the ductility of the polyethylene glycol ether are influenced.
In addition, in order to be matched with the formula to have a good defoaming and foam inhibiting effect, the sorbitol polyoxyethylene ether stearate is added, the property is stable, the lasting usable time of defoaming is effectively prolonged, the sorbitol polyoxyethylene ether stearate has excellent stability but is not easy to diffuse, so that the defects of the sorbitol polyoxyethylene ether stearate are just made up by the added polysiloxane, the defoaming and foam inhibiting effect of the sorbitol polyoxyethylene ether stearate can be improved by enhancing the ductility of the sorbitol polyoxyethylene ether stearate, the consumption of the polysiloxane and the stearate is generally kept equal in the added amount, the effect of other components can be covered if the added amount of any component is too large, the activity is reduced, the foam inhibiting and defoaming effect is influenced if the added amount of any component is increased, and the compatibility relationship among the consumption is also noticed besides the specific collocation among the formulas.
The thickener in the formula of the invention has no toxicity or irritation, good water solubility, good intermiscibility with a plurality of organic matter components and excellent dispersion thickening effect.
Preferably, as a further practical scheme, the thickening agent is any one or a mixture of several of starch, pectin, agar, methylcellulose and carboxymethyl cellulose.
The invention provides a formula of a silicon ether defoaming agent and a preparation method thereof, and the preparation method comprises the following steps:
stirring polyglycol ether and polysiloxane at 80-120 deg.C, adding other raw materials, and stirring.
Preferably, as a further practicable aspect, the addition of the other raw materials is in order polyethylene glycol ether, sorbitan polyoxyethylene ether stearate, and thickener.
Preferably, as a further practicable embodiment, the sorbitol polyoxyethylene ether stearate and the thickener are added and then stirred for 4 to 6 hours.
Preferably, as a further possibility, the polyethylene glycol ether is stirred with the polysiloxane at a temperature of 80-120 ℃ for 1-3 h.
Preferably, as a further practical scheme, after adding the polyethylene glycol ether and fully mixing, reducing the temperature to 50-70 ℃, and adding the sorbitol polyoxyethylene ether stearate and the thickening agent.
The preparation method has the advantages that the quality of the prepared silyl ether defoamer is improved by limiting the operation parameters in the preparation method, the silyl ether defoamer is good in stability and high in defoaming strength, the defoaming speed is greatly improved while low toxicity is eliminated, and the silyl ether defoamer is resistant to heat, acid, alkali and salt and a high-temperature system.
In a word, the silyl ether defoaming agent prepared by the preparation method is environment-friendly, good in defoaming effect and excellent in stability.
Compared with the prior art, the invention has the beneficial effects that:
(1) the silicon ether defoaming agent disclosed by the invention adopts a compound formula, and multiple components are matched for use, so that the synergistic effect is obviously increased, and the defoaming and foam inhibiting effects are excellent.
(2) The silicon ether defoaming agent has the advantages of good stability, high defoaming strength, low toxicity elimination, greatly improved defoaming speed, heat resistance, acid and alkali resistance and high temperature system.
(3) The silicon ether defoaming agent disclosed by the invention has the characteristics of no toxicity, no harm, simple process, lasting effect, environmental friendliness and the like. The defoaming agent is suitable for defoaming agents used in normal working procedures and discharged sewage in various processing industries, such as food industry, fiber industry, rubber industry, paper pulp industry, chemical industry and the like.
(4) The preparation method of the silyl ether antifoaming agent is simple to operate, the whole preparation method is mild in operation condition, free of pollution, free of three-waste discharge, safe and environment-friendly.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The specific preparation process of the silicon ether defoaming agent comprises the following steps:
1. the raw materials are mixed according to the following parts by mass:
25 parts of polyglycol ether, 50 parts of dimethyl silicone oil, 8 parts of polysiloxane, 11 parts of sorbitol polyoxyethylene ether stearate and 1 part of thickening agent.
2. Adding dimethyl silicone oil and polysiloxane into a reaction device with heating and stirring functions, heating and stirring at the stirring speed of 60rpm for 2h, and simultaneously heating to 100 ℃.
3. Polyethylene glycol ether was put into the reaction apparatus at a temperature of 100 ℃ and stirred at 60rpm for 1 hour.
4. After the temperature of the reaction device is adjusted to 50 ℃, adding the sorbitol polyoxyethylene ether stearate and the thickening agent starch, and stirring at the stirring speed of 60rpm for 5 hours.
5. Stopping heating after homogenizing, naturally cooling to normal temperature to obtain the defoaming agent, packaging, detecting and forming a product for sale.
Example 2
The specific preparation process of the silicon ether defoaming agent comprises the following steps:
1. the raw materials are mixed according to the following parts by mass:
40 parts of polyglycol ether, 30 parts of dimethyl silicone oil, 15 parts of polysiloxane, 9 parts of sorbitol polyoxyethylene ether stearate and 5 parts of thickening agent.
2. Adding dimethyl silicone oil and polysiloxane into a reaction device with heating and stirring functions, heating and stirring at the stirring speed of 60rpm for 2h, and simultaneously heating to 80 ℃.
3. On the basis of the temperature of 80 ℃, polyethylene glycol ether is put into the reaction device for stirring, the stirring speed is 60rpm, and the stirring time is 2 hours.
4. After the temperature of the reaction device is adjusted to 70 ℃, the sorbitol polyoxyethylene ether stearate and the thickening agent starch are added and stirred, wherein the stirring speed is 60rpm, and the stirring time is 4 hours.
5. Stopping heating after homogenizing, naturally cooling to normal temperature to obtain the defoaming agent, packaging, detecting and forming a product for sale.
Example 3
The specific preparation process of the silicon ether defoaming agent comprises the following steps:
1. the raw materials are mixed according to the following parts by mass:
30 parts of polyglycol ether, 45 parts of dimethyl silicone oil, 10 parts of polysiloxane, 13 parts of sorbitol polyoxyethylene ether stearate and 2 parts of thickening agent.
2. Adding dimethyl silicone oil and polysiloxane into a reaction device with heating and stirring functions, heating and stirring at the stirring speed of 60rpm for 2h, and simultaneously heating to 120 ℃.
3. Polyethylene glycol ether was put into the reaction apparatus at a temperature of 120 ℃ and stirred at a rotation speed of 60rpm for 3 hours.
4. After the temperature of the reaction device is adjusted to 60 ℃, the sorbitol polyoxyethylene ether stearate and the thickening agent starch are added and stirred, wherein the stirring speed is 60rpm, and the stirring time is 6 hours.
5. Stopping heating after homogenizing, naturally cooling to normal temperature to obtain the defoaming agent, packaging, detecting and forming a product for sale.
Example 4
The specific operation steps are consistent with those of the embodiment 3, and the raw materials are mixed according to the following parts by weight:
38 parts of polyglycol ether, 35 parts of dimethyl silicone oil, 13 parts of polysiloxane, 10 parts of sorbitol polyoxyethylene ether stearate and 4 parts of thickening agent.
Example 5
The specific operation steps are consistent with those of the embodiment 3, and the raw materials are mixed according to the following parts by weight:
35 parts of polyglycol ether, 40 parts of dimethyl silicone oil, 11 parts of polysiloxane, 11 parts of sorbitol polyoxyethylene ether stearate and 3 parts of thickening agent.
Comparative example 1
The procedure was as in example 5 except that the polysiloxane was added in an amount of 4 parts.
Comparative example 2
The specific procedure was as in example 5 except that 3 parts of sorbitan polyoxyethylene ether stearate was added.
Comparative example 3
The procedure was as in example 5 except that 10 parts of dimethylsilicone oil was added.
Experimental example 1
The specific treatment effects of the silyl ether antifoaming agents of examples 1 to 5 and comparative examples 1 to 3 were evaluated, and the specific results are shown in table 1 below:
the main apparatus device: a shaking shaker and a 500mL measuring cylinder with a plug;
and (3) testing conditions are as follows: 25 ℃;
test medium: a standard foaming liquid;
the specific test method comprises the following steps: weighing 0.25g of nonylphenol polyoxyethylene (10) ether and 0.25g (30 percent content) of sodium dodecyl benzene sulfonate, dissolving in 50mL of water, mixing, stirring to obtain a uniform transparent liquid, and adding water to dilute to 100mL, thus obtaining a standard foaming liquid; pouring 500mL of standard foaming liquid into a measuring cylinder, placing the measuring cylinder into a shaking flask shaker to shake for 5min at the frequency of 200 times/min, stopping shaking when the height of foam reaches 400mL scale, adding 0.2mL of the foam obtained in the embodiment and the comparative example, and recording the time required by foam elimination by using a stopwatch, namely the defoaming time; the cylinder was again placed in the shaker and shaken, and the time required for the foam height to reach 400mL again was recorded.
TABLE 1 results of treatment
| Group of | Defoaming time | Foam inhibition time | Dispersibility |
| Example 1 | 71 | 67 | Good effect |
| Example 2 | 65 | 74 | Good effect |
| Example 3 | 66 | 73 | Good effect |
| Example 4 | 65 | 72 | Good effect |
| Example 5 | 63 | 81 | Good effect |
| Comparative example 1 | 78 | 62 | Unevenness of |
| Comparative example 2 | 77 | 64 | Unevenness of |
| Comparative example 3 | 79 | 63 | Unevenness of |
As can be seen from Table 1 above, the silicone ether defoaming agent of the present invention has greatly improved defoaming time and foam suppressing time, better defoaming and foam suppressing effects, and better dispersibility than those of comparative examples 1-3. Comparative examples 1 to 3 were poor in defoaming effect because the compounding ratio of the raw materials was not controlled within an appropriate range, and it was found that a specific amount of each component thereof was also necessary.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (9)
1. The silicon ether defoaming agent is characterized by being mainly prepared from the following raw materials: the adhesive comprises, by mass, 25-40 parts of polyethylene glycol ether, 30-50 parts of dimethyl silicone oil, 8-15 parts of polysiloxane, 9-11 parts of sorbitol polyoxyethylene ether stearate and 1-5 parts of a thickening agent.
2. The silicone ether defoaming agent according to claim 1, characterized by comprising, by mass, 30-38 parts of polyethylene glycol ether, 35-45 parts of dimethyl silicone oil, 10-13 parts of polysiloxane, 10-13 parts of sorbitol polyoxyethylene ether stearate, and 2-4 parts of a thickener.
3. The silicone ether defoaming agent according to claim 1, characterized by comprising, by mass, 35 parts of polyethylene glycol ether, 40 parts of dimethyl silicone oil, 11 parts of polysiloxane, 11 parts of sorbitan polyoxyethylene ether stearate, and 3 parts of a thickener.
4. The silicon ether defoamer according to any one of claims 1 to 3, wherein the thickener is any one or a mixture of starch, pectin, agar, methyl cellulose and carboxymethyl cellulose.
5. A method of preparing the silyl ether antifoam agent of any of claims 1-4, comprising the steps of:
stirring polyglycol ether and polysiloxane at 80-120 deg.C, adding other raw materials, and stirring.
6. The method according to claim 5, wherein the other raw materials are added in the order of polyethylene glycol ether, sorbitan polyoxyethylene ether stearate, and thickener.
7. The method according to claim 6, wherein the sorbitol polyoxyethylene ether stearate and the thickener are added and stirred for 4 to 6 hours.
8. A process according to claim 5, wherein the polyethylene glycol ether is stirred with the polysiloxane at a temperature of 80-120 ℃ for 1-3 hours.
9. The method according to claim 6, wherein after adding polyglycol ether and mixing, the temperature is lowered to 50-70 ℃, and sorbitol polyoxyethylene ether stearate and thickener are added.
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Citations (7)
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|---|---|---|---|---|
| US3746653A (en) * | 1972-05-15 | 1973-07-17 | Dow Corning | Jet dyeing foam control |
| CN105413251A (en) * | 2015-11-24 | 2016-03-23 | 宜兴市丰烨化学有限公司 | Polyether silicone oil tributyl phosphate defoaming agent and preparation method thereof |
| CN106731034A (en) * | 2016-12-22 | 2017-05-31 | 新疆水处理工程技术研究中心有限公司 | A kind of compound defoamer |
| CN107899274A (en) * | 2017-10-27 | 2018-04-13 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of self-emulsifying type defoamer and preparation method thereof |
| CN107899275A (en) * | 2017-11-15 | 2018-04-13 | 四川科立鑫新材料有限公司 | A kind of medicine production defoaming agent composition and preparation method thereof |
| CN110559696A (en) * | 2019-08-29 | 2019-12-13 | 安徽銮威化工科技开发有限公司 | Defoaming agent with high defoaming speed and preparation method thereof |
| CN110639241A (en) * | 2019-10-15 | 2020-01-03 | 武汉三友石化有限公司 | Petroleum defoaming agent and preparation method thereof |
-
2020
- 2020-12-29 CN CN202011588593.XA patent/CN112807756A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3746653A (en) * | 1972-05-15 | 1973-07-17 | Dow Corning | Jet dyeing foam control |
| CN105413251A (en) * | 2015-11-24 | 2016-03-23 | 宜兴市丰烨化学有限公司 | Polyether silicone oil tributyl phosphate defoaming agent and preparation method thereof |
| CN106731034A (en) * | 2016-12-22 | 2017-05-31 | 新疆水处理工程技术研究中心有限公司 | A kind of compound defoamer |
| CN107899274A (en) * | 2017-10-27 | 2018-04-13 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of self-emulsifying type defoamer and preparation method thereof |
| CN107899275A (en) * | 2017-11-15 | 2018-04-13 | 四川科立鑫新材料有限公司 | A kind of medicine production defoaming agent composition and preparation method thereof |
| CN110559696A (en) * | 2019-08-29 | 2019-12-13 | 安徽銮威化工科技开发有限公司 | Defoaming agent with high defoaming speed and preparation method thereof |
| CN110639241A (en) * | 2019-10-15 | 2020-01-03 | 武汉三友石化有限公司 | Petroleum defoaming agent and preparation method thereof |
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| Title |
|---|
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