CN111057240A - Method for preparing resin from phenyl alkoxy silane high-boiling residues - Google Patents
Method for preparing resin from phenyl alkoxy silane high-boiling residues Download PDFInfo
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- CN111057240A CN111057240A CN201911194517.8A CN201911194517A CN111057240A CN 111057240 A CN111057240 A CN 111057240A CN 201911194517 A CN201911194517 A CN 201911194517A CN 111057240 A CN111057240 A CN 111057240A
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- phenylalkoxysilane
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a method for preparing resin from phenyl alkoxy silane high-boiling residues, which comprises the following steps: step (1): pressing phenyl alkoxy silane high-boiling residues, a chlorosilane monomer and a part of solvent into a dropwise adding kettle for later use by a feed pump; step (2): adding part of solvent, water and alcohol into a reaction kettle, adding the material drops in the dropping kettle into the reaction kettle, controlling the reaction temperature at 15-55 ℃ and the dropping time at 3-8 h; stirring for 1-3h after the dropwise addition is finished, standing to separate an acid water layer, washing the silicon resin prepolymer for 3-6 times until the prepolymer is neutral, filtering, evaporating the solvent, adding a catalyst for polymerization, and adding the solvent for cooling to obtain a finished product of phenyl silicon resin; the prepared silicone resin has good heat resistance, flexibility and insulation moisture resistance, and is suitable for electric insulating paint, high-temperature-resistant paint, coil impregnating varnish and the like.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a method for preparing resin from phenyl alkoxy silane high-boiling residues.
Background
The organic silicon material has the advantages of high refractive index, good light transmittance, good thermal stability, strong ultraviolet resistance, small internal stress, low hygroscopicity and the like, and the performance of the organic silicon material is obviously superior to that of epoxy resin, and the organic silicon material becomes an ideal choice of power type LED packaging materials. The research and development and production of power type LED packaging materials are relatively laggard in China, and the requirements of domestic markets for the power type LED packaging materials mostly depend on import, for example, products of international three silica gel enterprises, namely Corning, Mitigo and Xinyue, mainly use high-refractive-index organic silicon packaging materials and have absolute advantages in domestic high-end packaging markets. Besides the requirements of high refractive index, light transmittance and ultraviolet radiation resistance, the power type LED packaging material also needs to have certain basic mechanical properties. The unreinforced vulcanized rubber has poor physical and mechanical properties and cannot meet the requirements, so reinforcing filler must be added to reinforce the packaging material, but the addition of the filler easily has negative influence on the refractive index and the light transmittance of the packaging material, and thus higher requirements are provided for the selection of the reinforcing filler.
Phenyl silicone resin has excellent electrical insulation, hydrophobicity, weather resistance, high temperature and low temperature resistance, radiation resistance and physiological inertia, however, the following problems are mostly existed in the preparation process of the existing phenyl silicone resin: a large amount of acidic wastewater is generated in the preparation process; the preparation process is complex and is not easy to control.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing resin from high-boiling-point substance of phenyl alkoxy silane, the high-boiling-point substance of phenyl alkoxy silane used by the invention is a byproduct for producing phenyl trialkoxy silane, mainly contains tripolymer and dimer of phenyl trialkoxy silane, contains a small amount of phenyl alkoxy silane, has low price, and can be used for replacing common phenyl trichlorosilane, so that the produced product has low cost and high yield; the prepared silicone resin has good heat resistance, flexibility and insulation moisture resistance, and is suitable for electric insulating paint, high-temperature-resistant paint, coil impregnating varnish and the like.
In order to achieve the purpose, the invention provides the following technical scheme: a method for preparing resin from phenyl alkoxy silane high-boiling residues comprises the following steps:
step (1): pressing phenyl alkoxy silane high-boiling residues, a chlorosilane monomer and a part of solvent into a dropwise adding kettle for later use by a feed pump;
step (2): adding part of solvent, water and alcohol into a reaction kettle, adding the material drops in the dropping kettle into the reaction kettle, controlling the reaction temperature at 15-55 ℃ and the dropping time at 3-8 h; stirring for 1-3h after the dropwise addition is finished, standing to separate an acid water layer, washing the silicon resin prepolymer for 3-6 times until the prepolymer is neutral, filtering, evaporating the solvent, adding a catalyst for polymerization, adding the solvent, and cooling to obtain the finished product of the phenyl silicon resin.
Preferably, the phenyl alkoxy silane high-boiling substance comprises a high-boiling substance which is a byproduct in the production of phenyl trimethoxy silane and phenyl triethoxy silane.
Preferably, the chlorosilane monomer comprises one or more of methyltrichlorosilane, dimethyldichlorosilane and diphenyldichlorosilane.
Preferably, the solvent comprises one or more of toluene, xylene aromatic hydrocarbon solvent or ethyl acetate and butyl acetate environment-friendly solvent.
Preferably, the alcohol comprises one or more of methanol, ethanol, isopropanol and butanol.
Preferably, the catalyst comprises naphthenate, carboxylate, titanate.
Compared with the prior art, the invention has the following beneficial effects:
1. the high-boiling-point substance of the phenyl alkoxy silane used by the invention is a byproduct for producing the phenyl trialkoxy silane, mainly contains tripolymer and dimer of the phenyl trialkoxy silane, contains a small amount of phenyl alkoxy silane, has low price, replaces the common phenyl trichlorosilane with the phenyl alkoxy silane, and produces the product with low cost and high yield; the prepared silicone resin has good heat resistance, flexibility and insulation moisture resistance, and is suitable for electric insulating paint, high-temperature-resistant paint, coil impregnating varnish and the like.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1, a method for preparing a resin from a phenylalkoxysilane high boiling material, comprising the steps of:
pressing phenyl alkoxy silane high-boiling residues, a chlorosilane monomer and a part of solvent into a dropwise adding kettle for later use by a feed pump; adding part of solvent, water and alcohol into a reaction kettle, dropwise adding the material in the kettle into the reaction kettle, controlling the reaction temperature at 15-55 ℃, and dropwise adding for 3-8 h; stirring for 1-3h after the dropwise addition is finished, standing to separate an acid water layer, washing the silicon resin prepolymer for 3-6 times until the prepolymer is neutral, filtering, evaporating the solvent, adding a catalyst for polymerization, adding the solvent, and cooling to obtain the finished product of the phenyl silicon resin.
Wherein, the phenylalkoxysilane high-boiling residues comprise high-boiling residues which are byproducts in the production of phenyltrimethoxysilane and the production of phenyltriethoxysilane;
wherein, the chlorosilane monomer refers to one or more of methyltrichlorosilane, dimethyldichlorosilane and diphenyldichlorosilane;
wherein, the solvent is one or more of aromatic solvents such as toluene, xylene and the like or environment-friendly solvents such as ethyl acetate, butyl acetate and the like;
wherein, the alcohol refers to one or more of methanol, ethanol, isopropanol and butanol;
wherein the catalyst comprises naphthenate, carboxylate, titanate and the like.
Example 2, a method for preparing resin from phenyl alkoxy silane high boiling substance, comprising the following steps: 212 parts of phenyl alkoxy silane high-boiling residue, 45 parts of methyl trichlorosilane, 67 parts of dimethyl dichlorosilane and 430 parts of xylene are pressed into a dropwise adding kettle by a feed pump for later use; 210 parts of toluene, 561 parts of water and 242 parts of ethanol are added into a reaction kettle, and a material drop in the reaction kettle is added into the reaction kettle in a dropping manner, wherein the reaction temperature is controlled to be 25-35 ℃, and the dropping time is about 4 hours; stirring for 2h after the dropwise addition is finished, standing to separate lower-layer acid water, washing the upper-layer silicon resin prepolymer for 6 times until the prepolymer is neutral, filtering, evaporating at low temperature to remove the solvent, adding 0.006 part of manganese naphthenate, carrying out reduced pressure polymerization at 140 ℃, adding the solvent, and cooling to obtain a finished product of phenyl silicon resin, wherein the yield can reach 89%, and the elongation can reach 320%.
Example 3, a method for preparing a resin from a phenylalkoxysilane high boiling material comprising the steps of: 183 parts of phenylalkoxysilane high-boiling substance, 29 parts of methyltrichlorosilane, 76 parts of dimethyldichlorosilane, 51 parts of diphenyldichlorosilane and 418 parts of xylene are pressed into a dripping kettle by a feed pump for later use; 324 parts of toluene, 411 parts of water and 256 parts of methanol are added into a reaction kettle, the material in the dropwise adding kettle is added into the reaction kettle, the reaction temperature is controlled to be 20-30 ℃, and the dropwise adding time is about 5 hours; stirring for 2h after the dropwise addition is finished, standing to separate lower-layer acid water, washing upper-layer silicon resin prepolymer for 5 times to be neutral, filtering, evaporating at low temperature to remove the solvent, adding 0.01 part of butyl titanate, carrying out reduced pressure polymerization at 150 ℃, adding the solvent, and cooling to obtain a finished product of phenyl silicon resin, wherein the yield can reach 90%, and the elongation can reach 320%.
Example 4, a method for preparing a resin from a phenylalkoxysilane high boiling material comprising the steps of: 183 parts of phenylalkoxysilane high-boiling substance, 29 parts of methyltrichlorosilane, 76 parts of dimethyldichlorosilane, 51 parts of diphenyldichlorosilane and 418 parts of xylene are pressed into a dripping kettle by a feed pump for later use; 324 parts of toluene, 411 parts of water, 200 parts of methanol and 156 parts of ethanol are added into a reaction kettle, a material drop in the dropping kettle is added into the reaction kettle, the reaction temperature is controlled to be 20-30 ℃, and the dropping time is about 5 hours; stirring for 2h after the dropwise addition is finished, standing to separate lower-layer acid water, washing upper-layer silicon resin prepolymer for 5 times to be neutral, filtering, evaporating at low temperature to remove the solvent, adding 0.01 part of butyl titanate, carrying out reduced pressure polymerization at 150 ℃, adding the solvent, and cooling to obtain a finished product of phenyl silicon resin, wherein the yield can reach 92%, and the elongation can reach 310%.
Example 5, a method for preparing a resin from a phenylalkoxysilane high boiling material, comprising the steps of: 183 parts of phenylalkoxysilane high-boiling substance, 29 parts of methyltrichlorosilane, 76 parts of dimethyldichlorosilane, 51 parts of diphenyldichlorosilane and 418 parts of xylene are pressed into a dripping kettle by a feed pump for later use; 324 parts of toluene, 411 parts of water and 256 parts of methanol are added into a reaction kettle, the material in the dropwise adding kettle is added into the reaction kettle, the reaction temperature is controlled to be 20-30 ℃, and the dropwise adding time is about 5 hours; stirring for 2h after the dropwise addition is finished, standing to separate lower-layer acid water, washing upper-layer silicon resin prepolymer for 5 times to be neutral, filtering, evaporating at low temperature to remove a solvent, adding 0.01 part of butyl titanate and 0.01 part of naphthenate, carrying out reduced pressure polymerization at 150 ℃, adding the solvent, and cooling to obtain a finished product of phenyl silicone resin, wherein the yield can reach 96%, and the elongation can reach 360%.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (6)
1. A method for preparing resin from phenyl alkoxy silane high-boiling residues is characterized by comprising the following steps: step (1): pressing phenyl alkoxy silane high-boiling residues, a chlorosilane monomer and a part of solvent into a dropwise adding kettle for later use by a feed pump;
step (2): adding part of solvent, water and alcohol into a reaction kettle, adding the material drops in the dropping kettle into the reaction kettle, controlling the reaction temperature at 15-55 ℃ and the dropping time at 3-8 h; stirring for 1-3h after the dropwise addition is finished, standing to separate an acid water layer, washing the silicon resin prepolymer for 3-6 times until the prepolymer is neutral, filtering, evaporating the solvent, adding a catalyst for polymerization, adding the solvent, and cooling to obtain the finished product of the phenyl silicon resin.
2. The method for preparing resin from phenylalkoxysilane according to claim 1, wherein said phenylalkoxysilane comprises high boiling substance by-produced from the production of phenyltrimethoxysilane and the production of phenyltriethoxysilane.
3. The method for preparing resin from phenylalkoxysilane according to claim 2, wherein said chlorosilane monomer comprises one or more of methyltrichlorosilane, dimethyldichlorosilane and diphenyldichlorosilane.
4. The method for preparing resin from phenylalkoxysilane according to claim 2, wherein said solvent comprises one or more of toluene, xylene aromatic solvent or environment friendly solvent of ethyl acetate and butyl acetate.
5. The method for preparing resin from phenylalkoxysilane according to claim 4, wherein said alcohol comprises one or more of methanol, ethanol, isopropanol and butanol.
6. The method for preparing resin from phenylalkoxysilane according to claim 4, wherein said catalyst comprises naphthenate, carboxylate, titanate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911194517.8A CN111057240A (en) | 2019-11-28 | 2019-11-28 | Method for preparing resin from phenyl alkoxy silane high-boiling residues |
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| CN201911194517.8A CN111057240A (en) | 2019-11-28 | 2019-11-28 | Method for preparing resin from phenyl alkoxy silane high-boiling residues |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111978545A (en) * | 2020-09-10 | 2020-11-24 | 江西星火狮达科技有限公司 | Special waterproof and mildewproof resin for wood and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111978545A (en) * | 2020-09-10 | 2020-11-24 | 江西星火狮达科技有限公司 | Special waterproof and mildewproof resin for wood and preparation method thereof |
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