CN118079469A - Polysiloxane defoamer and preparation method thereof - Google Patents
Polysiloxane defoamer and preparation method thereof Download PDFInfo
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- -1 Polysiloxane Polymers 0.000 title claims abstract description 122
- 239000013530 defoamer Substances 0.000 title claims abstract description 54
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 113
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 53
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 53
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 50
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002270 dispersing agent Substances 0.000 claims abstract description 28
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 28
- PQPVPZTVJLXQAS-UHFFFAOYSA-N hydroxy-methyl-phenylsilicon Chemical compound C[Si](O)C1=CC=CC=C1 PQPVPZTVJLXQAS-UHFFFAOYSA-N 0.000 claims abstract description 19
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims abstract description 19
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract 7
- 238000003756 stirring Methods 0.000 claims description 45
- 238000010438 heat treatment Methods 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 32
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 16
- 229910000077 silane Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 229940014800 succinic anhydride Drugs 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 7
- 229920001228 polyisocyanate Polymers 0.000 claims description 7
- 239000005056 polyisocyanate Substances 0.000 claims description 7
- 229920006389 polyphenyl polymer Polymers 0.000 claims description 7
- HEBRGEBJCIKEKX-UHFFFAOYSA-M sodium;2-hexadecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HEBRGEBJCIKEKX-UHFFFAOYSA-M 0.000 claims description 7
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 8
- 238000013329 compounding Methods 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 125000004356 hydroxy functional group Chemical group O* 0.000 description 43
- 239000006260 foam Substances 0.000 description 19
- 239000000243 solution Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 12
- 230000005764 inhibitory process Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 239000004721 Polyphenylene oxide Substances 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000005187 foaming Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 239000004753 textile Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003599 detergent Substances 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 239000004604 Blowing Agent Substances 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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
-
- 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
-
- 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
- B01D19/0413—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing N-atoms
-
- 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
- B01D19/0422—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing S-atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a polysiloxane defoamer and a preparation method thereof, wherein the polysiloxane defoamer comprises the following components in parts by mass: 35-45 parts of polyborosiloxane, 10-15 parts of phenyl methyl siloxane, 3-8 parts of modified hydroxy polydimethylsiloxane, 4-6 parts of modified nano silicon dioxide, 0.1-0.3 part of carboxylated graphene oxide, 0.1-0.2 part of methacrylamide and 0.3-0.7 part of dispersing agent. The invention, through compounding of multiple components, synergistic, the defoaming agent prepared has good defoaming effect and good stability, by adding the modified hydroxy polydimethylsiloxane and the modified nano silicon dioxide into the system, not only improves the defoaming effect, but also improves the stability of the system, so that the stability of the defoaming agent at high temperature is improved, the centrifugal stability is stronger, the problem of poor stability of the existing defoaming agent is solved, and the quality of the product is improved.
Description
Technical Field
The invention belongs to the technical field of defoamers, and particularly relates to a polysiloxane defoamer and a preparation method thereof.
Background
The chemical methods for eliminating foam mainly include a chemical reaction method and a method of adding an antifoaming agent. The chemical reaction method is to add some reagents to make the reagents and the foaming agent react chemically to generate water-insoluble substances, so as to reduce the concentration of the surfactant in the liquid film and promote the foam to break. However, this method has some drawbacks, such as uncertainty of the blowing agent composition and the creation of hazards to the system equipment from poorly soluble substances. The most widely used defoaming method in various industries is a method of adding a defoaming agent. The method has the greatest advantages of high defoaming efficiency and convenient use.
The defoaming agent, also called as an antifoaming agent, can generate a plurality of harmful foams in the industrial production process, needs to be added, and is widely applied to the removal of the harmful foams generated in the production process of industries such as paint production, textile sizing, food fermentation, biological medicine, paint, petrochemical industry, papermaking, industrial cleaning and the like. The defoaming agent is a substance capable of reducing the surface tension of water, solution, suspension and the like, preventing foam from forming or reducing or eliminating original foam, has the following properties of strong defoaming force, small dosage, no influence on the basic properties of a system when being added into a foaming system, namely no reaction with the system to be defoamed, small surface tension, good balance with the surface, good heat resistance, no physiological activity, high safety and very wide application of the defoaming agent.
Many types of defoamers, organosiloxane, polyether, silicon and ether grafts, amine, imine and amide containing, have faster defoaming speed, longer foam suppressing time, and wider application range of medium, even harsh medium environments such as high temperature, strong acid and strong alkali. The common defoamers on the market at present comprise organic defoamers, polyether defoamers, organosilicon defoamers and polyether modified siloxane defoamers. The polyether defoamer has the greatest advantages that the foam inhibition capability is strong, part of products also have excellent performances such as high temperature resistance, strong acid resistance, strong alkali resistance and the like, but the products have the defects of limited use conditions, poor foam inhibition capability, low foam breaking rate and the like; the research of the organic defoaming agent is early, and the organic defoaming agent has the advantages of mature production process, easily available raw materials, high environmental protection performance, low production cost and the like, but has the defects of low defoaming efficiency, strong specialization, harsh use condition and the like; the polyether modified siloxane defoamer is an emerging product, and has the advantages of both polyether defoamer and organosilicon defoamer, but the products are still in the research and development stage, the products on the market are few in types, the production cost is high, and the foam inhibition and defoaming performance can be influenced when the products are stored for a long time; the organic silicon defoamer has the advantages of strong defoaming performance, quick foam breaking capability, low volatility, no toxicity to the environment, no physiological inertia, wide application range and the like, thus having wide application prospect and huge market potential, but poor foam inhibition performance.
The organic silicon defoamer is a novel defoamer and is widely applied to various fields due to excellent defoaming performance and foam inhibition performance. Common organic silicon defoamer, silicone oil defoamer: silicone oil is a liquid silicone polymer with good defoaming and foam inhibiting properties. It is commonly used in petroleum, chemical, paint, textile and other fields. Diatomite defoamer: diatomite is a natural siliceous rock, and the surface of the diatomite is provided with a plurality of micropores and functional groups, so that the diatomite has good defoaming performance and foam inhibition performance. It is generally used in the fields of detergents, cosmetics, pharmaceuticals, etc. Silicate defoamer: silicate is an inorganic compound whose main components are sodium silicate and silicate. It has good defoaming performance and foam inhibition performance, and is generally used in the fields of chemical industry, coating, textile and the like. Polysiloxane defoamer: polysiloxane is a polymer with high molecular weight, and the molecular structure of the polysiloxane contains a silicon-oxygen bond, so that the polysiloxane has good defoaming performance and foam inhibition performance. It is generally used in the fields of detergents, cosmetics, pharmaceuticals, etc. The commercially available silicone defoamer is not ideal in defoaming effect, and is poor in stability, so that the use effect is affected.
Disclosure of Invention
The invention aims to provide a polysiloxane defoamer and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
The polysiloxane defoamer comprises the following components in parts by mass: 35-45 parts of polyborosiloxane, 10-15 parts of phenyl methyl siloxane, 3-8 parts of modified hydroxy polydimethylsiloxane, 4-6 parts of modified nano silicon dioxide, 0.1-0.3 part of carboxylated graphene oxide, 0.1-0.2 part of methacrylamide and 0.3-0.7 part of dispersing agent.
Further, polyborosiloxanes are commercially available products with a viscosity of 240 Pa.S, phenylmethylsiloxanes are available from Dow Corning, and a kinematic viscosity at 20℃of 8000cSt.
Further, carboxylated graphene oxide sheet diameter: 0.5-5 microns, thickness: 0.8-1.2 nanometers. The material is purchased from the Qianfeng nanometer,
Further, the preparation method of the modified nano silicon dioxide comprises the following steps:
(1) Mixing nano silicon dioxide, a silane coupling agent and 50wt% ethanol water solution according to the mass ratio of 1:1:10-12, heating to 55 ℃, reacting for 1.5-2.5h, filtering, washing and drying to obtain silane modified silicon dioxide;
(2) Mixing silane modified silicon dioxide, succinic anhydride and 50wt% ethanol water solution according to the mass ratio of 1:3:8-10, heating to 40 ℃, reacting for 1-2h, centrifuging, and drying to obtain the modified nano silicon dioxide.
Further, the particle size of the nano silicon dioxide is 50-150nm, and the specific surface area is 150-200 m 2/g.
Further, the silane coupling agent is selected from one or more of KH550, KH560 and KH 570.
Further, the preparation method of the modified hydroxy polydimethylsiloxane comprises the following steps: mixing the hydroxy polydimethylsiloxane and polymethylene polyphenyl polyisocyanate (CAS: 9016-87-9) with the mass ratio of 4-6:1, heating to 70-80 ℃ in nitrogen atmosphere, and reacting for 4-6h under stirring condition to obtain the modified hydroxy polydimethylsiloxane.
Further, the stirring speed is 90-100r/min.
Further, the molecular weight of the hydroxy polydimethylsiloxane is 500-20000. Purchased from wuhank biomedical technologies limited.
Further, the dispersing agent is at least one selected from sodium hexadecyl benzene sulfonate, sodium dodecyl benzene sulfonate and sodium lignin sulfonate.
The invention also provides a preparation method of the polysiloxane defoamer, which comprises the following steps: mixing polyborosiloxane, phenyl methyl siloxane, modified hydroxy polydimethylsiloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 85-90 ℃, stirring and reacting for 3-4 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
Compared with the prior art, the invention has the advantages that: the invention, through compounding of multiple components, synergistic, the defoaming agent prepared has good defoaming effect and good stability, by adding the modified hydroxy polydimethylsiloxane and the modified nano silicon dioxide into the system, not only improves the defoaming effect, but also improves the stability of the system, so that the stability of the defoaming agent at high temperature is improved, the centrifugal stability is stronger, the problem of poor stability of the existing defoaming agent is solved, and the quality of the product is improved.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a polysiloxane defoamer, which comprises the following components in parts by mass: 40 parts of polyborosiloxane, 13 parts of phenyl methyl siloxane, 5 parts of modified hydroxy polydimethylsiloxane, 5 parts of modified nano silicon dioxide, 0.2 part of carboxylated graphene oxide, 0.2 part of methacrylamide and 0.5 part of dispersing agent.
Polyborosiloxanes are commercially available products with a viscosity of 240 Pa.S, phenylmethylsiloxanes are available from Dow Corning, and a kinematic viscosity at 20℃of 8000cSt.
Carboxylated graphene oxide sheet diameter: 0.5-5 microns, thickness: 0.8-1.2 nanometers. The material is purchased from the Qianfeng nanometer,
The preparation method of the modified nano silicon dioxide comprises the following steps:
(1) Mixing nano silicon dioxide, a silane coupling agent and an ethanol water solution with the weight ratio of 50wt% in the mass ratio of 1:1:11, heating to 55 ℃, reacting for 2 hours, filtering, washing and drying to obtain silane modified silicon dioxide;
(2) And mixing silane modified silicon dioxide, succinic anhydride and 50wt% ethanol water solution according to the mass ratio of 1:3:9, heating to 40 ℃, reacting for 1.5 hours, centrifuging, and drying to obtain the modified nano silicon dioxide.
The particle size of the nano silicon dioxide is 50-150nm, and the specific surface area is 150-200 m 2/g.
The silane coupling agent is KH550.
The preparation method of the modified hydroxy polydimethylsiloxane comprises the following steps: mixing the hydroxy polydimethylsiloxane and polymethylene polyphenyl polyisocyanate (CAS: 9016-87-9) in a mass ratio of 5:1, heating to 75 ℃ in a nitrogen atmosphere, and reacting for 5 hours under the stirring condition of 95r/min to obtain the modified hydroxy polydimethylsiloxane.
The molecular weight of the hydroxy polydimethylsiloxane is 500-20000. Purchased from wuhank biomedical technologies limited.
The dispersing agent is sodium hexadecyl benzene sulfonate.
The preparation method of the polysiloxane defoamer comprises the following steps: mixing polyborosiloxane, phenyl methyl siloxane, modified hydroxy polydimethylsiloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 86 ℃, stirring and reacting for 3.5 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
Example 2
The embodiment provides a polysiloxane defoamer, which comprises the following components in parts by mass: 35 parts of polyborosiloxane, 10 parts of phenyl methyl siloxane, 3 parts of modified hydroxy polydimethylsiloxane, 4 parts of modified nano silicon dioxide, 0.1 part of carboxylated graphene oxide, 0.1 part of methacrylamide and 0.3 part of dispersing agent.
Polyborosiloxanes are commercially available products with a viscosity of 240 Pa.S, phenylmethylsiloxanes are available from Dow Corning, and a kinematic viscosity at 20℃of 8000cSt.
Carboxylated graphene oxide sheet diameter: 0.5-5 microns, thickness: 0.8-1.2 nanometers. The material is purchased from the Qianfeng nanometer,
The preparation method of the modified nano silicon dioxide comprises the following steps:
(1) Mixing nano silicon dioxide, a silane coupling agent and an ethanol water solution with the weight ratio of 50wt% in the mass ratio of 1:1:10, heating to 55 ℃, reacting for 1.5 hours, filtering, washing and drying to obtain silane modified silicon dioxide;
(2) And mixing silane modified silicon dioxide, succinic anhydride and 50wt% ethanol water solution according to the mass ratio of 1:3:8, heating to 40 ℃, reacting for 1h, centrifuging, and drying to obtain the modified nano silicon dioxide.
The particle size of the nano silicon dioxide is 50-150nm, and the specific surface area is 150-200 m 2/g.
The silane coupling agent is KH560.
The preparation method of the modified hydroxy polydimethylsiloxane comprises the following steps: mixing the hydroxy polydimethylsiloxane and polymethylene polyphenyl polyisocyanate (CAS: 9016-87-9) in a mass ratio of 4:1, heating to 70 ℃ in a nitrogen atmosphere, and reacting for 4 hours under a stirring condition of 90r/min to obtain the modified hydroxy polydimethylsiloxane.
The molecular weight of the hydroxy polydimethylsiloxane is 500-20000. Purchased from wuhank biomedical technologies limited.
The dispersing agent is sodium dodecyl benzene sulfonate.
The preparation method of the polysiloxane defoamer comprises the following steps: mixing polyborosiloxane, phenyl methyl siloxane, modified hydroxy polydimethylsiloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 85 ℃, stirring and reacting for 3 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
Example 3
The embodiment provides a polysiloxane defoamer, which comprises the following components in parts by mass: 45 parts of polyborosiloxane, 15 parts of phenyl methyl siloxane, 8 parts of modified hydroxy polydimethylsiloxane, 6 parts of modified nano silicon dioxide, 0.3 part of carboxylated graphene oxide, 0.2 part of methacrylamide and 0.7 part of dispersing agent.
Polyborosiloxanes are commercially available products with a viscosity of 240 Pa.S, phenylmethylsiloxanes are available from Dow Corning, and a kinematic viscosity at 20℃of 8000cSt.
Carboxylated graphene oxide sheet diameter: 0.5-5 microns, thickness: 0.8-1.2 nanometers. The material is purchased from the Qianfeng nanometer,
The preparation method of the modified nano silicon dioxide comprises the following steps:
(1) Mixing nano silicon dioxide, a silane coupling agent and 50wt% of ethanol water solution according to the mass ratio of 1:1:12, heating to 55 ℃, reacting for 2.5 hours, filtering, washing and drying to obtain silane modified silicon dioxide;
(2) And mixing silane modified silicon dioxide, succinic anhydride and 50wt% ethanol water solution according to the mass ratio of 1:3:10, heating to 40 ℃, reacting for 2 hours, centrifuging, and drying to obtain the modified nano silicon dioxide.
The particle size of the nano silicon dioxide is 50-150nm, and the specific surface area is 150-200 m 2/g.
The silane coupling agent is KH570.
The preparation method of the modified hydroxy polydimethylsiloxane comprises the following steps: mixing the hydroxy polydimethylsiloxane and polymethylene polyphenyl polyisocyanate (CAS: 9016-87-9) in a mass ratio of 6:1, heating to 80 ℃ in a nitrogen atmosphere, and reacting for 6 hours under a stirring condition of 100r/min to obtain the modified hydroxy polydimethylsiloxane.
The molecular weight of the hydroxy polydimethylsiloxane is 500-20000. Purchased from wuhank biomedical technologies limited.
The dispersing agent is sodium lignin sulfonate.
The preparation method of the polysiloxane defoamer comprises the following steps: mixing polyborosiloxane, phenyl methyl siloxane, modified hydroxy polydimethylsiloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 90 ℃, stirring and reacting for 4 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
Comparative example 1
The difference between this comparative example and example 1 is: the modified hydroxy polydimethylsiloxane is replaced by hydroxy polydimethylsiloxane.
The polysiloxane defoamer comprises the following components in parts by mass: 40 parts of polyborosiloxane, 13 parts of phenyl methyl siloxane, 5 parts of hydroxy polydimethylsiloxane, 5 parts of modified nano silicon dioxide, 0.2 part of carboxylated graphene oxide, 0.2 part of methacrylamide and 0.5 part of dispersing agent.
Polyborosiloxanes are commercially available products with a viscosity of 240 Pa.S, phenylmethylsiloxanes are available from Dow Corning, and a kinematic viscosity at 20℃of 8000cSt.
Carboxylated graphene oxide sheet diameter: 0.5-5 microns, thickness: 0.8-1.2 nanometers. The material is purchased from the Qianfeng nanometer,
The preparation method of the modified nano silicon dioxide comprises the following steps:
(1) Mixing nano silicon dioxide, a silane coupling agent and an ethanol water solution with the weight ratio of 50wt% in the mass ratio of 1:1:11, heating to 55 ℃, reacting for 2 hours, filtering, washing and drying to obtain silane modified silicon dioxide;
(2) And mixing silane modified silicon dioxide, succinic anhydride and 50wt% ethanol water solution according to the mass ratio of 1:3:9, heating to 40 ℃, reacting for 1.5 hours, centrifuging, and drying to obtain the modified nano silicon dioxide.
The particle size of the nano silicon dioxide is 50-150nm, and the specific surface area is 150-200 m 2/g.
The silane coupling agent is KH550.
The molecular weight of the hydroxy polydimethylsiloxane is 500-20000. Purchased from wuhank biomedical technologies limited.
The dispersing agent is sodium hexadecyl benzene sulfonate.
The preparation method of the polysiloxane defoamer comprises the following steps: mixing polyborosiloxane, phenyl methyl siloxane, hydroxy polydimethylsiloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 86 ℃, stirring and reacting for 3.5 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
Comparative example 2
The difference between this comparative example and example 1 is: the modified nano-silica is replaced with nano-silica.
The polysiloxane defoamer comprises the following components in parts by mass: 40 parts of polyborosiloxane, 13 parts of phenyl methyl siloxane, 5 parts of modified hydroxy polydimethylsiloxane, 5 parts of nano silicon dioxide, 0.2 part of carboxylated graphene oxide, 0.2 part of methacrylamide and 0.5 part of dispersing agent.
Polyborosiloxanes are commercially available products with a viscosity of 240 Pa.S, phenylmethylsiloxanes are available from Dow Corning, and a kinematic viscosity at 20℃of 8000cSt.
Carboxylated graphene oxide sheet diameter: 0.5-5 microns, thickness: 0.8-1.2 nanometers. The material is purchased from the Qianfeng nanometer,
The particle size of the nano silicon dioxide is 50-150nm, and the specific surface area is 150-200 m 2/g.
The preparation method of the modified hydroxy polydimethylsiloxane comprises the following steps: mixing the hydroxy polydimethylsiloxane and polymethylene polyphenyl polyisocyanate (CAS: 9016-87-9) in a mass ratio of 5:1, heating to 75 ℃ in a nitrogen atmosphere, and reacting for 5 hours under the stirring condition of 95r/min to obtain the modified hydroxy polydimethylsiloxane.
The molecular weight of the hydroxy polydimethylsiloxane is 500-20000. Purchased from wuhank biomedical technologies limited.
The dispersing agent is sodium hexadecyl benzene sulfonate.
The preparation method of the polysiloxane defoamer comprises the following steps: mixing polyborosiloxane, phenyl methyl siloxane, modified hydroxy polydimethylsiloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 86 ℃, stirring and reacting for 3.5 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
Comparative example 3
The difference between this comparative example and example 1 is: the addition amounts of the components are different.
The polysiloxane defoamer comprises the following components in parts by mass: 40 parts of polyborosiloxane, 5 parts of phenyl methyl siloxane, 13 parts of modified hydroxy polydimethylsiloxane, 2 parts of modified nano silicon dioxide, 0.2 part of carboxylated graphene oxide, 0.2 part of methacrylamide and 0.5 part of dispersing agent.
Polyborosiloxanes are commercially available products with a viscosity of 240 Pa.S, phenylmethylsiloxanes are available from Dow Corning, and a kinematic viscosity at 20℃of 8000cSt.
Carboxylated graphene oxide sheet diameter: 0.5-5 microns, thickness: 0.8-1.2 nanometers. The material is purchased from the Qianfeng nanometer,
The preparation method of the modified nano silicon dioxide comprises the following steps:
(1) Mixing nano silicon dioxide, a silane coupling agent and an ethanol water solution with the weight ratio of 50wt% in the mass ratio of 1:1:11, heating to 55 ℃, reacting for 2 hours, filtering, washing and drying to obtain silane modified silicon dioxide;
(2) And mixing silane modified silicon dioxide, succinic anhydride and 50wt% ethanol water solution according to the mass ratio of 1:3:9, heating to 40 ℃, reacting for 1.5 hours, centrifuging, and drying to obtain the modified nano silicon dioxide.
The particle size of the nano silicon dioxide is 50-150nm, and the specific surface area is 150-200 m 2/g.
The silane coupling agent is KH550.
The preparation method of the modified hydroxy polydimethylsiloxane comprises the following steps: mixing the hydroxy polydimethylsiloxane and polymethylene polyphenyl polyisocyanate (CAS: 9016-87-9) in a mass ratio of 5:1, heating to 75 ℃ in a nitrogen atmosphere, and reacting for 5 hours under the stirring condition of 95r/min to obtain the modified hydroxy polydimethylsiloxane.
The molecular weight of the hydroxy polydimethylsiloxane is 500-20000. Purchased from wuhank biomedical technologies limited.
The dispersing agent is sodium hexadecyl benzene sulfonate.
The preparation method of the polysiloxane defoamer comprises the following steps: mixing polyborosiloxane, phenyl methyl siloxane, modified hydroxy polydimethylsiloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 86 ℃, stirring and reacting for 3.5 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
Comparative example 4
The difference between this comparative example and example 1 is: no modified hydroxydimethicone was added.
The polysiloxane defoamer comprises the following components in parts by mass: 40 parts of polyborosiloxane, 18 parts of phenyl methyl siloxane, 5 parts of modified nano silicon dioxide, 0.2 part of carboxylated graphene oxide, 0.2 part of methacrylamide and 0.5 part of dispersing agent.
Polyborosiloxanes are commercially available products with a viscosity of 240 Pa.S, phenylmethylsiloxanes are available from Dow Corning, and a kinematic viscosity at 20℃of 8000cSt.
Carboxylated graphene oxide sheet diameter: 0.5-5 microns, thickness: 0.8-1.2 nanometers. The material is purchased from the Qianfeng nanometer,
The preparation method of the modified nano silicon dioxide comprises the following steps:
(1) Mixing nano silicon dioxide, a silane coupling agent and an ethanol water solution with the weight ratio of 50wt% in the mass ratio of 1:1:11, heating to 55 ℃, reacting for 2 hours, filtering, washing and drying to obtain silane modified silicon dioxide;
(2) And mixing silane modified silicon dioxide, succinic anhydride and 50wt% ethanol water solution according to the mass ratio of 1:3:9, heating to 40 ℃, reacting for 1.5 hours, centrifuging, and drying to obtain the modified nano silicon dioxide.
The particle size of the nano silicon dioxide is 50-150nm, and the specific surface area is 150-200 m 2/g.
The silane coupling agent is KH550.
The dispersing agent is sodium hexadecyl benzene sulfonate.
The preparation method of the polysiloxane defoamer comprises the following steps: mixing polyborosiloxane, phenyl methyl siloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 86 ℃, stirring and reacting for 3.5 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
Performance testing
At room temperature, 25 mL wt% of sodium dodecyl benzene sulfonate aqueous solution is poured into a measuring cylinder of 100mL, and the mixture is vibrated up and down for a plurality of times, so that the height of the foaming liquid reaches 100 mL. The defoaming agents of examples 1 to 3 and comparative examples 1 to 4 were added in an amount of 0.1 wt% of the foaming liquid, and the stop time was started until the foam was completely disappeared, and the defoaming performance of the defoaming agent was better as the stop time was shorter, and the experiment was repeated three times to take an average value.
0.5G of the defoamers of examples 1-3 and comparative examples 1-4 were added to 100 mL of water, stirred well, centrifuged at 3000 r/min for 5min, and the centrifuge stability of the defoamers was observed, if no delamination was observed, the centrifuge stability was proved to be good.
0.5 G of the defoamers of examples 1-3 and comparative examples 1-4 are added into 100mL of water, and the mixture is kept stand at 60 ℃ to observe the high temperature resistance of the defoamers, and if no bleaching oil exists, the high temperature resistance is proved to be good.
TABLE 1 Performance test results
As is clear from examples 1 to 3, the defoamers prepared in examples 1 to 3 of the present invention have better overall properties, and as is clear from comparative examples 1 to 4, the defoamers have different degrees of performance degradation by changing the raw materials prepared. The invention, through compounding of multiple components, synergistic, the defoaming agent prepared has good defoaming effect and good stability, by adding the modified hydroxy polydimethylsiloxane and the modified nano silicon dioxide into the system, not only improves the defoaming effect, but also improves the stability of the system, so that the stability of the defoaming agent at high temperature is improved, the centrifugal stability is stronger, the problem of poor stability of the existing defoaming agent is solved, and the quality of the product is improved.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The polysiloxane defoamer is characterized by comprising the following components in parts by weight: 35-45 parts of polyborosiloxane, 10-15 parts of phenyl methyl siloxane, 3-8 parts of modified hydroxy polydimethylsiloxane, 4-6 parts of modified nano silicon dioxide, 0.1-0.3 part of carboxylated graphene oxide, 0.1-0.2 part of methacrylamide and 0.3-0.7 part of dispersing agent.
2. The polysiloxane defoamer of claim 1, wherein carboxylated graphene oxide flakes: 0.5-5 microns, thickness: 0.8-1.2 nanometers.
3. The polysiloxane defoamer of claim 1, wherein the preparation method of the modified nano-silica comprises the following steps:
(1) Mixing nano silicon dioxide, a silane coupling agent and 50wt% ethanol water solution according to the mass ratio of 1:1:10-12, heating to 55 ℃, reacting for 1.5-2.5h, filtering, washing and drying to obtain silane modified silicon dioxide;
(2) Mixing silane modified silicon dioxide, succinic anhydride and 50wt% ethanol water solution according to the mass ratio of 1:3:8-10, heating to 40 ℃, reacting for 1-2h, centrifuging, and drying to obtain the modified nano silicon dioxide.
4. A polysiloxane defoamer according to claim 3, wherein the nanosilica has a particle size of 50-150nm and a specific surface area of 150-200 m 2/g.
5. A polysiloxane defoamer according to claim 3, wherein the silane coupling agent is selected from one or more of KH550, KH560, KH 570.
6. A polysiloxane defoamer of claim 1, wherein the method of preparing the modified hydroxydimethicone comprises the steps of: mixing the hydroxy polydimethylsiloxane and polymethylene polyphenyl polyisocyanate with the mass ratio of 4-6:1, heating to 70-80 ℃ in a nitrogen atmosphere, and reacting for 4-6h under the stirring condition to obtain the modified hydroxy polydimethylsiloxane.
7. A silicone defoamer of claim 6, wherein the stirring is at a speed of 90-100r/min.
8. A silicone defoamer of claim 6, wherein the molecular weight of the hydroxy polydimethylsiloxane is 500-20000.
9. A silicone defoamer of claim 1, wherein said dispersant is selected from at least one of sodium hexadecyl benzene sulfonate, sodium dodecyl benzene sulfonate, sodium lignin sulfonate.
10. A process for the preparation of a silicone defoamer as claimed in any of claims 1to9, comprising the steps of: mixing polyborosiloxane, phenyl methyl siloxane, modified hydroxy polydimethylsiloxane, modified nano silicon dioxide and carboxylated graphene oxide, and uniformly stirring; continuously adding the methacrylamide, uniformly stirring, heating to 85-90 ℃, stirring and reacting for 3-4 hours, continuously adding the dispersing agent, uniformly stirring, and cooling to room temperature to obtain the polysiloxane defoamer.
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