CN112843797A - Preparation method of efficient water-based silicon polyether defoaming agent - Google Patents
Preparation method of efficient water-based silicon polyether defoaming agent Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910001868 water Inorganic materials 0.000 title claims abstract description 106
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 94
- 229920000570 polyether Polymers 0.000 title claims abstract description 94
- 239000002518 antifoaming agent Substances 0.000 title claims abstract description 52
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 47
- 239000010703 silicon Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000203 mixture Substances 0.000 claims description 147
- 238000003756 stirring Methods 0.000 claims description 79
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 66
- -1 polydimethylsiloxane Polymers 0.000 claims description 59
- 230000008719 thickening Effects 0.000 claims description 57
- 238000002156 mixing Methods 0.000 claims description 56
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 50
- 239000013530 defoamer Substances 0.000 claims description 39
- 238000001816 cooling Methods 0.000 claims description 38
- 229920001296 polysiloxane Polymers 0.000 claims description 34
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 30
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 30
- 239000007822 coupling agent Substances 0.000 claims description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims description 25
- 239000002736 nonionic surfactant Substances 0.000 claims description 25
- 239000007864 aqueous solution Substances 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 19
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 19
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 19
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 19
- 229920000053 polysorbate 80 Polymers 0.000 claims description 19
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 19
- 239000003995 emulsifying agent Substances 0.000 claims description 8
- 239000002562 thickening agent Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 claims description 3
- 239000006260 foam Substances 0.000 description 49
- 230000005764 inhibitory process Effects 0.000 description 21
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- 230000000052 comparative effect Effects 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
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- 230000007547 defect Effects 0.000 description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 4
- 238000005187 foaming Methods 0.000 description 4
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Classifications
-
- 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
Abstract
The invention is suitable for the technical field of defoaming agents, and provides a preparation method of a high-efficiency water-based silicon polyether defoaming agent.
Description
Technical Field
The invention relates to the technical field of defoaming agents, and particularly relates to a preparation method of a high-efficiency water-based silicon polyether defoaming agent.
Background
In many industrial processes, the generation of bubbles is involved, and most foams adversely affect the production, such as reducing the production capacity, causing waste of raw materials, reducing the product quality, causing operational fluctuations, etc., and causing economic losses of various degrees. Generally, a foam is a coarse dispersion of a gas in a liquid, belonging to a gas-liquid heterogeneous system, and having a bulk density close to that of a gas but not close to that of a liquid. When the liquid does not contain the surfactant, the bubbles can migrate to the surface of the liquid and break and disappear; when the liquid contains a surfactant, the surface of the bubbles forms a film sheet, and the foam becomes stable.
Defoamers are surfactants used to suppress or eliminate foam and are the most cost effective method of controlling foam; defoaming technology has been adopted at home and abroad in the fields of textile printing and dyeing, medicine, fermentation, food, paper making, mineral separation, coating, fiber and petroleum refining, etc. The defoaming agent mainly comprises active ingredients, an emulsifier, a carrier and an emulsifying aid, wherein the active ingredients are the most main core part and play roles in breaking foam and reducing surface tension; the emulsifier is used for dispersing the active ingredients into small particles so as to be better dispersed into oil or water and have better defoaming effect; the carrier accounts for a large proportion in the defoaming agent, the surface tension of the carrier is not high, the carrier mainly plays a role of supporting a medium, the foam inhibition and defoaming effects are favorable, and the cost can be reduced; the emulsifying auxiliary agent is used for ensuring that the emulsifying effect is better. The antifoaming agent may be classified into five types, i.e., solid particle type, emulsion type, dispersion type, oil type and paste type, according to various classification criteria; according to the application of the defoaming agent in different industrial production, the defoaming agent can be divided into a textile industry defoaming agent, a paper industry defoaming agent, a coating industry defoaming agent, a food industry defoaming agent, a petroleum industry defoaming agent and the like; the defoaming agents can be classified into mineral oil, alcohols, fatty acids and fatty acid esters, amides, phosphates, silicones and polyether defoaming agents according to their chemical structures and compositions, with silicone and polyether defoaming agents being the most common.
The main component of the silicone defoaming agent is polydimethylsiloxane, namely silicone oil, and compared with H2O and common oils, the silicone oil has smaller surface tension, so that the silicone defoaming agent is suitable for both a water-based foaming system and an oily foaming system. In H2O and common oil, the silicone oil has high activity and low solubility, and the basic characteristics are stable chemical property, wide application range, low volatility, no toxicity, prominent defoaming capability and the like, and the defect is poor foam inhibition performance.
The polyether defoamer is a copolymer of ethylene oxide and propylene oxide, and the defoaming effect is achieved mainly by utilizing different characteristics of solubility of the polyether defoamer shown at different temperatures. At low temperatures, the polyether is dispersed in water, and as the temperature is increased, the hydrophilicity of the polyether gradually decreases, and the polyether is rendered insoluble until the cloud point, thus exerting defoaming action. The cloud point can be changed by adjusting the types of the polyether and the proportion of the raw materials in the preparation process, so that the polyether can be applied to different industries. The polyether type defoaming agent has the advantages of strong foam inhibition capability, high temperature resistance and the like, and has the defects of certain toxicity, limited use condition by temperature, low foam breaking rate and narrow use field. If the amount of the foam generated is large, the foam cannot be quickly eliminated, and the defoaming effect can be shown only by adding the defoaming agent into the foam again.
In many industrial production fields, such as papermaking, textile printing and dyeing, oil processing, sewage treatment, petroleum exploitation and transportation, the defoaming agent required to be used has good defoaming and foam inhibiting functions, and the organosilicon defoaming agent has strong defoaming force, high defoaming speed and weak foam inhibiting capability; the polyether defoamer has weak defoaming capability and strong foam inhibiting capability, and both cannot well meet the production requirements.
Disclosure of Invention
The embodiment of the invention provides a preparation method of a high-efficiency water-based silicon polyether defoaming agent, which is characterized in that polydimethylsiloxane and polyether modified polysiloxane are blended into the same system, the defoaming capability of the polydimethylsiloxane and the foam inhibition capability of the polyether modified polysiloxane are fully exerted, and the synergistic effect of the polydimethylsiloxane and the polyether modified polysiloxane is utilized, so that the defoaming time of the prepared high-efficiency water-based silicon polyether defoaming agent is greatly shortened, and the foam inhibition time is greatly prolonged, thereby having excellent defoaming and foam inhibition performances and meeting the production requirement under a lower concentration.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a high-efficiency water-based silicon polyether defoaming agent comprises the following steps:
1) uniformly mixing polydimethylsiloxane and polyether modified polysiloxane to obtain a mixture A;
2) adding the mixture A, a nonionic surfactant and deionized water into a stirring kettle, heating to 75-80 ℃, stirring for 1-2 h, and cooling to room temperature to obtain a mixture B;
3) adding 3% and 5% of coupling agent and emulsifier by mass percent into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C;
4) uniformly mixing a thickening agent and a sodium hydroxide aqueous solution, and adjusting the pH value to 7 to obtain thickening water;
5) and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 1-2 h at 50-65 ℃, then cooling to room temperature, and homogenizing for 0.5-1 h to obtain the high-efficiency water-based silicon polyether defoamer.
Further, the mass ratio of the polydimethylsiloxane to the polyether modified polysiloxane in the step 1) is (1-7): 9.
further, the mass ratio of the mixture A, the nonionic surfactant and the deionized water in the step 2) is (1-5): 1: (3-7).
Further, the rotating speed of the stirring kettle in the step 2) is 800-1200 r/min.
Further, the hydrophilic-lipophilic balance value of the nonionic surfactant in the step 2) is 1-3.
Further, the coupling agent in the step 3) is a titanate coupling agent.
Further, the emulsifier in the step 3) is polyoxyethylene sorbitan monooleate.
Further, the mass concentration of the sodium hydroxide aqueous solution in the step 4) is 10%.
Further, the thickener in the step 4) is sodium polyacrylate.
Further, the homogenization pressure in the step 5) is 80-100 MPa.
The invention has the following beneficial effects:
according to the invention, the polydimethylsiloxane and the polyether modified polysiloxane are blended into the same system, so that the defoaming capability of the polydimethylsiloxane and the foam inhibition capability of the polyether modified polysiloxane are fully exerted, and the synergistic effect of the polydimethylsiloxane and the polyether modified polysiloxane is utilized, so that the defoaming time of the prepared high-efficiency water-based silicon polyether defoaming agent is greatly shortened, and the foam inhibition time is greatly improved, and therefore, the high-efficiency water-based silicon polyether defoaming agent has excellent defoaming and foam inhibition performances, and can meet the production requirement at a lower concentration.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The main component of the silicone defoaming agent is polydimethylsiloxane, namely silicone oil, and compared with H2O and common oils, the silicone oil has smaller surface tension, so that the silicone defoaming agent is suitable for both a water-based foaming system and an oily foaming system. In H2O and common oil, the silicone oil has high activity and low solubility, and the basic characteristics are stable chemical property, wide application range, low volatility, no toxicity, prominent defoaming capability and the like, and the defect is poor foam inhibition performance.
The polyether defoamer is a copolymer of ethylene oxide and propylene oxide, and the defoaming effect is achieved mainly by utilizing different characteristics of solubility of the polyether defoamer shown at different temperatures. At low temperatures, the polyether is dispersed in water, and as the temperature is increased, the hydrophilicity of the polyether gradually decreases, and the polyether is rendered insoluble until the cloud point, thus exerting defoaming action. The cloud point can be changed by adjusting the types of the polyether and the proportion of the raw materials in the preparation process, so that the polyether can be applied to different industries. The polyether type defoaming agent has the advantages of strong foam inhibition capability, high temperature resistance and the like, and has the defects of certain toxicity, limited use condition by temperature, low foam breaking rate and narrow use field. If the amount of the foam generated is large, the foam cannot be quickly eliminated, and the defoaming effect can be shown only by adding the defoaming agent into the foam again.
The polydimethylsiloxane and the polyether modified polysiloxane are blended into the same system, the defoaming capability of the polydimethylsiloxane and the foam inhibition capability of the polyether modified polysiloxane are fully exerted, and the synergistic effect of the polydimethylsiloxane and the polyether modified polysiloxane is utilized, so that the prepared silicon polyether defoaming agent has excellent defoaming and foam inhibition performances, and can meet the production requirement at lower concentration
Specifically, the embodiment of the invention provides a preparation method of a high-efficiency water-based silicon polyether defoaming agent, which comprises the following steps:
1) uniformly mixing polydimethylsiloxane and polyether modified polysiloxane to obtain a mixture A;
2) adding the mixture A, a nonionic surfactant and deionized water into a stirring kettle, heating to 75-80 ℃, stirring for 1-2 h, and cooling to room temperature to obtain a mixture B;
3) adding 3% and 5% of coupling agent and emulsifier by mass percent into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C;
4) uniformly mixing a thickening agent and a sodium hydroxide aqueous solution, and adjusting the pH value to 7 to obtain thickening water;
5) and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 1-2 h at 50-65 ℃, then cooling to room temperature, and homogenizing for 0.5-1 h to obtain the high-efficiency water-based silicon polyether defoamer.
In the embodiment of the invention, the mass ratio of the polydimethylsiloxane to the polyether modified polysiloxane in the step 1) is (1-7): 9.
in the embodiment of the invention, the mass ratio of the mixture A, the nonionic surfactant and the deionized water in the step 2) is (1-5): 1: (3-7).
In the embodiment of the invention, the rotating speed of the stirring kettle in the step 2) is 800-1200 r/min.
In the embodiment of the invention, the hydrophilic-lipophilic balance value of the nonionic surfactant in the step 2) is 1-3.
In the embodiment of the invention, the coupling agent in the step 3) is a titanate coupling agent.
In an embodiment of the present invention, the emulsifier in step 3) is polyoxyethylene sorbitan monooleate.
In the embodiment of the present invention, the mass concentration of the sodium hydroxide aqueous solution in the step 4) is 10%.
In the embodiment of the invention, the thickener in the step 4) is sodium polyacrylate.
In the embodiment of the invention, the homogenization pressure in the step 5) is 80-100 MPa.
The technical solution and the technical effect of the present invention will be further described by specific examples.
Example 1
The preparation method comprises the following steps of (1): 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 2
The preparation method comprises the following steps of (1) mixing polydimethylsiloxane and polyether modified polysiloxane according to a mass ratio of 2: 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 3
The preparation method comprises the following steps of (1): 3, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 4
The preparation method comprises the following steps of (1) mixing polydimethylsiloxane and polyether modified polysiloxane in a mass ratio of 4: 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 5
And (2) mixing polydimethylsiloxane and polyether modified polysiloxane according to the mass ratio of 5: 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 6
The preparation method comprises the following steps of (1) mixing polydimethylsiloxane and polyether modified polysiloxane according to a mass ratio of 2: 3, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 7
And (2) mixing polydimethylsiloxane and polyether modified polysiloxane according to the mass ratio of 7: 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 8
The preparation method comprises the following steps of (1): 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 3: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 9
The preparation method comprises the following steps of (1): 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 5: 1: 3, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 10
The preparation method comprises the following steps of (1): 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 5, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 11
The preparation method comprises the following steps of (1): 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 1: 1: 7, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 12
The preparation method comprises the following steps of (1): 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 3: 1: 5, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Example 13
The preparation method comprises the following steps of (1) mixing polydimethylsiloxane and polyether modified polysiloxane in a mass ratio of 4: 9, uniformly mixing to obtain a mixture A; mixing the mixture A, a nonionic surfactant and deionized water according to a mass ratio of 3: 1: 5, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Control group
Taking a common defoaming agent sold in the market.
The defoaming agents prepared in the above examples 1 to 13 and the control group were numbered, and the defoaming performance and foam suppressing performance of each group of defoaming agents were tested as follows:
and (3) defoaming performance test: pouring 200mL of sodium dodecyl benzene sulfonate solution with the mass fraction of 0.5% into a l000mL measuring cylinder, introducing nitrogen, bubbling to a certain height, then respectively adding equivalent defoaming agents, recording the time required for reducing the foam from 800mL scale to 300mL scale, repeating for 3 times, and taking the average value, namely the defoaming time of the group of defoaming agents; the shorter the time, the better the defoaming effect.
And (3) testing the foam inhibition performance: adding 200mL of sodium dodecyl benzene sulfonate solution with the mass fraction of 0.5% and an equivalent amount of corresponding defoaming agent into a L000mL measuring cylinder, introducing nitrogen for continuous bubbling, keeping the nitrogen flow at 1L/min, recording the time required by the foam to rise from a 300mL scale to a 800mL scale, repeating for 3 times, and taking the average value of the times, namely the foam inhibition time of the group of defoaming agent; the longer the time, the better the foam suppressing effect.
See table 1 below for specific assay results:
TABLE 1
As can be seen from table 1, compared with the use of a commercially available common defoamer, the defoaming time of the high-efficiency aqueous silicon polyether defoamer prepared according to the present invention is greatly reduced, and the foam suppressing time is greatly increased, wherein the defoaming and foam suppressing performance of the high-efficiency aqueous silicon polyether defoamer prepared according to example 13 is the best.
Further, the present invention was carried out by a single factor deletion comparative experiment on polydimethylsiloxane and polyether modified polysiloxane based on the preparation procedure of example 13, and the experimental results found that different factors were deleted and that the finally prepared silicon polyether defoamer had a certain degree of difference in defoaming and foam suppressing properties, specifically, see the following comparative examples.
Comparative example 1
Polyether modified polysiloxane, a nonionic surfactant and deionized water are mixed according to a mass ratio of 3: 1: 5, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Comparative example 2
The preparation method comprises the following steps of (1) mixing polydimethylsiloxane, a nonionic surfactant and deionized water in a mass ratio of 3: 1: 5, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
Comparative example 3
Mixing a nonionic surfactant and deionized water according to a mass ratio of 3: 1: 5, adding the mixture into a stirring kettle, heating to 75 ℃, stirring at the rotating speed of 1000r/min for 2 hours, and cooling to room temperature to obtain a mixture B; adding 3% and 5% of titanate coupling agent and polyoxyethylene sorbitan monooleate in percentage by mass into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C; uniformly mixing sodium polyacrylate and a 10% sodium hydroxide aqueous solution by mass concentration, and adjusting the pH value to 7 to obtain thickening water; and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 2h at 55 ℃, then cooling to room temperature, homogenizing for 0.5h, and homogenizing under 100MPa to obtain the high-efficiency water-based silicon polyether defoamer.
The defoaming agents prepared in the comparative examples 1 to 3 are numbered, and the defoaming performance and foam inhibition performance of each group of defoaming agents are tested as follows:
and (3) defoaming performance test: pouring 200mL of sodium dodecyl benzene sulfonate solution with the mass fraction of 0.5% into a l000mL measuring cylinder, introducing nitrogen, bubbling to a certain height, then respectively adding equivalent defoaming agents, recording the time required for reducing the foam from 800mL scale to 300mL scale, repeating for 3 times, and taking the average value, namely the defoaming time of the group of defoaming agents; the shorter the time, the better the defoaming effect.
And (3) testing the foam inhibition performance: adding 200mL of sodium dodecyl benzene sulfonate solution with the mass fraction of 0.5% and an equivalent amount of corresponding defoaming agent into a L000mL measuring cylinder, introducing nitrogen for continuous bubbling, keeping the nitrogen flow at 1L/min, recording the time required by the foam to rise from a 300mL scale to a 800mL scale, repeating for 3 times, and taking the average value of the times, namely the foam inhibition time of the group of defoaming agent; the longer the time, the better the foam suppressing effect.
See table 2 below for specific assay results:
TABLE 2
| Numbering | Item of implementation | Polydimethylsiloxane | Polyether modified polysiloxane | Defoaming time(s) | Bubble suppressing time(s) |
| 13 | Example 9 | √ | √ | 61 | 211 |
| 15 | Comparative example 1 | √ | 86 | 172 | |
| 16 | Comparative example 2 | √ | 93 | 168 | |
| 17 | Comparative example 3 | 121 | 133 |
As can be seen from Table 2, the defoaming and foam inhibiting performance of the high-efficiency water-based silicon polyether defoamer prepared by the method is greatly improved compared with that of the high-efficiency water-based silicon polyether defoamer prepared by singly using polydimethylsiloxane and polyether modified polysiloxane.
In general, the polydimethylsiloxane and the polyether modified polysiloxane are blended into the same system, the defoaming capability of the polydimethylsiloxane and the foam inhibition capability of the polyether modified polysiloxane are fully exerted, and the synergistic effect of the polydimethylsiloxane and the polyether modified polysiloxane is utilized, so that the defoaming time of the prepared high-efficiency water-based silicon polyether defoaming agent is greatly shortened, and the foam inhibition time is greatly prolonged, and therefore, the high-efficiency water-based silicon polyether defoaming agent has excellent defoaming and foam inhibition performances, and can meet the production requirement at a lower concentration.
It should be understood that the above-mentioned embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a high-efficiency water-based silicon polyether defoaming agent is characterized by comprising the following steps:
1) uniformly mixing polydimethylsiloxane and polyether modified polysiloxane to obtain a mixture A;
2) adding the mixture A, a nonionic surfactant and deionized water into a stirring kettle, heating to 75-80 ℃, stirring for 1-2 h, and cooling to room temperature to obtain a mixture B;
3) adding 3% and 5% of coupling agent and emulsifier by mass percent into the mixture B, introducing nitrogen, and continuously stirring for 20-30 min to obtain a mixture C;
4) uniformly mixing a thickening agent and a sodium hydroxide aqueous solution, and adjusting the pH value to 7 to obtain thickening water;
5) and slowly adding thickening water into the mixture C, wherein the mass ratio of the thickening water to the mixture C is 1:20, stirring for 1-2 h at 50-65 ℃, then cooling to room temperature, and homogenizing for 0.5-1 h to obtain the high-efficiency water-based silicon polyether defoamer.
2. The preparation method of the high-efficiency water-based silicon polyether defoamer as claimed in claim 1, wherein the mass ratio of the polydimethylsiloxane to the polyether modified polysiloxane in the step 1) is (1-7): 9.
3. the preparation method of the high-efficiency water-based silicon polyether defoamer as claimed in claim 1, wherein the mass ratio of the mixture A, the nonionic surfactant and the deionized water in the step 2) is (1-5): 1: (3-7).
4. The preparation method of the high-efficiency water-based silicon polyether defoamer as claimed in claim 1, wherein the rotation speed of the stirring kettle in the step 2) is 800-1200 r/min.
5. The preparation method of the high-efficiency water-based silicon polyether defoamer as claimed in claim 1, wherein the hydrophilic-lipophilic balance value of the nonionic surfactant in the step 2) is 1-3.
6. The preparation method of the high-efficiency aqueous silicon polyether defoamer as claimed in claim 1, wherein the coupling agent in step 3) is a titanate coupling agent.
7. The method for preparing the high-efficiency aqueous silicon polyether defoamer as claimed in claim 1, wherein the emulsifier in step 3) is polyoxyethylene sorbitan monooleate.
8. The method for preparing the high-efficiency aqueous silicon polyether defoamer as claimed in claim 1, wherein the mass concentration of the sodium hydroxide aqueous solution in the step 4) is 10%.
9. The preparation method of the high-efficiency water-based silicon polyether defoamer as claimed in claim 7, wherein the thickener in the step 4) is sodium polyacrylate.
10. The preparation method of the high-efficiency water-based silicon polyether defoamer as claimed in claim 7, wherein the homogenization pressure in the step 5) is 80-100 MPa.
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