CN110713790A - Preparation method of silicon dioxide-organic silicon composite system, product and application thereof - Google Patents

Preparation method of silicon dioxide-organic silicon composite system, product and application thereof Download PDF

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CN110713790A
CN110713790A CN201910933706.6A CN201910933706A CN110713790A CN 110713790 A CN110713790 A CN 110713790A CN 201910933706 A CN201910933706 A CN 201910933706A CN 110713790 A CN110713790 A CN 110713790A
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composite system
silicon
sol
methyltrimethoxysilane
temperature
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黄颖杰
卢静
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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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
    • 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
    • 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
    • C08G77/14—Polysiloxanes containing silicon bound to oxygen-containing groups
    • C08G77/18—Polysiloxanes containing silicon bound to oxygen-containing groups to alkoxy or aryloxy groups
    • 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
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F21—LIGHTING
    • F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
    • F21V9/00—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters
    • F21V9/40—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters with provision for controlling spectral properties, e.g. colour, or intensity
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/10—Transparent films; Clear coatings; Transparent materials

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Engineering & Computer Science (AREA)
  • Silicon Polymers (AREA)

Abstract

The invention provides a preparation method of a silicon dioxide-organic silicon composite system, a product and an application thereof, the silicon dioxide-organic silicon composite system is a coating material, takes organic siloxane and aluminum-silicon sol as raw materials, takes zinc oxide acetic acid as a catalyst, and comprises the following steps: putting a proper amount of methyltrimethoxysilane and dimethyldimethoxysilane into a flask, adding a proper amount of water, aluminum-silicon sol, zinc oxide acetic acid solution and isopropanol, stirring uniformly, and heating and hydrolyzing in a constant-temperature water bath; adding a silane coupling agent KH560, stirring at a constant temperature, and mixing the coupling agents; after mixing completely, keeping for a certain time at 60-90 ℃ to complete the polycondensation reaction; and (3) putting the substrate cleaned in advance into the sol, slowly pulling out at a constant speed, and drying and curing to obtain the nano-composite material. Through experiments and estimation, the proper distribution ratio of each component is designed. The method can prepare a proper light filtering coating film for the bulb, so that the light filtering coating film has strong adhesive force and good high-temperature resistance.

Description

Preparation method of silicon dioxide-organic silicon composite system, product and application thereof
Technical Field
The invention belongs to the technical field of paint preparation, and particularly relates to a preparation method of a silicon dioxide-organic silicon composite system, a product and application thereof.
Background
The coating has wide application in various aspects, but the coating needs to have light transmission and high temperature resistance in many cases, for example, a headlamp for a vehicle needs to have high temperature resistance of four to five hundred degrees, and many coating products can not meet the requirements, for example, pure silicone resin, polyester modified silicone resin and the like can obviously turn yellow and are not durable at high temperature of five to five degrees. Therefore, the light transmission and high temperature resistance are always the research direction. Therefore, it is necessary to develop such products.
The Shandong university Xiesheng is prepared by mixing organic silicon resin obtained by hydrolytic condensation of MTES after hydrolytic condensation under certain conditions, and copolymerizing to obtain inorganic-organic silicon resin. The two resins have high temperature resistance, can be cured at room temperature and moisture state, keep stable performance in wide temperature, humidity and frequency ranges, and have good chemical weather resistance stability and transparency.
Mixing organosilicon monomer (CH) with tetraethoxysilane TEOS such as Yanwei3）Si(OC2H5)3And (C)6H5）2Si(OCH3)2Firstly, preparing SiO from tetraethoxysilane TEOS by a sol-gel method2The sol reacts with active body, and then the active body and organic silicon monomer are subjected to graft copolymerization reaction, so that the obtained copolymer coating has higher heat resistance and high hardness than the traditional high-temperature resistant coatings such as pure organic silicon, epoxy modified organic silicon and the like, and simultaneously keeps good impact strength.
The above coating materials also have improved high-temperature heat resistance, but do not simultaneously achieve properties such as light-transmitting adhesion, and therefore, further modification is required to obtain a good coating material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method of a silicon dioxide-organic silicon composite system.
Yet another object of the present invention is to: provides a silicon dioxide-organic silicon composite system product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of a silicon dioxide-organic silicon composite system, wherein the silicon dioxide-organic silicon composite system is a coating material, organic siloxane and aluminum-silicon sol are used as raw materials, zinc oxide acetic acid is used as a catalyst, and the preparation method comprises the following steps:
(1) putting a proper amount of methyltrimethoxysilane and dimethyldimethoxysilane into a flask, adding a proper amount of water, aluminum-silicon sol, zinc oxide acetic acid solution and isopropanol, stirring uniformly, and then heating and hydrolyzing in a constant-temperature water bath, wherein: the ratio of methyltrimethoxysilane to dimethyldimethoxysilane is (30-5) to 1; the ratio of the aluminum-silicon sol to the methyltrimethoxysilane is (2-5) to 1; the adding amount of the silane coupling agent is 0.1 to 0.5 percent of the total amount, and the adding amount of the zinc oxide acetic acid is 0.5 to 2 percent of the total amount; the ratio of methyltrimethoxysilane to isopropanol is (5-30) to 1;
(2) adding a silane coupling agent KH560, stirring at a constant temperature, and mixing the coupling agents;
(3) after mixing completely, keeping for a certain time at 60-90 ℃ to complete the polycondensation reaction;
(4) and (3) putting the substrate cleaned in advance into the sol, slowly pulling out at a constant speed, and drying and curing to obtain the nano-composite material.
The temperature of the constant-temperature water bath in the step (1) is 35-60 ℃.
The step (2) is as follows: the ratio of the methyltrimethoxysilane to the silane coupling agent is (20-100): 1.
The temperature in the step (3) is 60-90 ℃.
The drying temperature in the step (4) is 60 ℃; the curing temperature was 200 ℃.
The invention also provides a silicon dioxide-organic silicon composite system prepared by any one of the methods.
The invention provides an application of a silicon dioxide-organic silicon composite system as a proper light filtering coating film for a bulb.
Organic siloxane and aluminum-silicon sol are used as raw materials, zinc oxide acetic acid is used as a catalyst, a coating material is prepared, and drying and curing are carried out after coating. Through experiments and estimation, the proper distribution ratio of each component is designed. The method can prepare the proper light filtering coating film for the bulb, so that the light filtering coating film has strong adhesive force and good high-temperature resistance. The invention takes the organic siloxane as the raw material to prepare the coating with good light transmission and high temperature resistance, and the coating resists the high temperature of 500 ℃ at 400 ℃, has good adhesive force and strong light transmission.
Detailed Description
The present invention is described in detail by the following specific examples, but the scope of the present invention is not limited to these examples.
Example 1
A silicon dioxide-organic silicon composite system is a coating material, which takes organic siloxane and aluminum-silicon sol as raw materials and zinc oxide acetic acid as a catalyst and is prepared by the following steps:
(1) adding 10g of methyltrimethoxysilane, 1g of dimethyldimethoxysilane, 30g of aluminum-silicon sol and 30g of water into a three-neck flask provided with a stirrer, a condenser, a thermometer and a dropping funnel, stirring and uniformly dispersing, dropwise adding zinc oxide acetic acid solution to adjust the pH to be =6, then adding 1g of isopropanol, stirring at high speed in a 35 ℃ water bath, homogenizing for 30min, and hydrolyzing;
(2) adding 0.1g of silane coupling agent KH560 into a dropping funnel, and accelerating and stirring for 1 hour at constant temperature;
(3) heating to 60 ℃ after complete mixing and keeping for 30min to complete polycondensation reaction to obtain sol;
(4) putting the glass cleaned in advance into the sol, slowly pulling out the glass at a constant speed, drying the lower surface at 60 ℃, and thermally curing at 200 ℃. The effect of the ratio of methyltrimethoxysilane to Si-Al-OOH is shown in Table 1.
Example 2
A silicon dioxide-organic silicon composite system is a coating material and is prepared by the following steps:
(1) adding 10g of methyltrimethoxysilane, 0.5g of dimethyldimethoxysilane, 50g of aluminum-silicon sol and 30g of water into a three-neck flask provided with a stirrer, a condenser, a thermometer and a dropping funnel, stirring and uniformly dispersing, dropwise adding zinc oxide acetic acid solution to adjust the pH to be =6, then adding 1g of isopropanol, stirring at high speed in a water bath at 50 ℃, homogenizing for 60min, and hydrolyzing;
(2) adding 0.2g of silane coupling agent KH560 into a dropping funnel, accelerating and stirring at constant temperature for 1h, and mixing the coupling agent;
(3) heating to 70 ℃ after complete mixing and keeping for 60min to complete polycondensation reaction to obtain sol;
(4) putting the glass cleaned in advance into the sol, slowly pulling out the glass at a constant speed, drying the lower surface at 60 ℃, and thermally curing at 200 ℃. The effect of the ratio of methyltrimethoxysilane to Si-Al-OOH is shown in Table 1.
Example 3
A silicon dioxide-organic silicon composite system is a coating material and is prepared by the following steps:
(1) adding 10g of methyltrimethoxysilane, 2g of dimethyldimethoxysilane, 20g of aluminum-silicon sol and 30g of water into a three-neck flask provided with a stirrer, a condenser, a thermometer and a dropping funnel, stirring and uniformly dispersing, dropwise adding zinc oxide-acetic acid solution to adjust the pH to be =6, then adding 2g of isopropanol, stirring at high speed in a water bath at 60 ℃, homogenizing for 90min, and hydrolyzing;
(2) adding 0.3g of silane coupling agent KH560 into a dropping funnel, accelerating and stirring at constant temperature for 1h, and mixing the coupling agent;
(3) heating to 90 ℃ after complete mixing and keeping for 90min to complete polycondensation reaction to obtain sol;
(4) putting the glass cleaned in advance into the sol, slowly pulling out the glass at a constant speed, drying the lower surface at 60 ℃, and thermally curing at 200 ℃. The effect of the ratio of methyltrimethoxysilane to Si-Al-OOH is shown in Table 1.
Example 4
A silicon dioxide-organic silicon composite system is a coating material and is prepared by the following steps:
(1) adding 10g of methyltrimethoxysilane, 0.8g of dimethyldimethoxysilane, 10g of aluminum-silicon sol and 30g of water into a three-neck flask provided with a stirrer, a condenser, a thermometer and a dropping funnel, stirring and uniformly dispersing, dropwise adding zinc oxide acetic acid solution to adjust the pH to be =6, then adding 1.2g of isopropanol, stirring at high speed in a water bath at 40 ℃, homogenizing for 50min, and hydrolyzing;
(2) adding 0.4g of silane coupling agent KH560 into a dropping funnel, accelerating and stirring at constant temperature for 1h, and mixing the coupling agent;
(3) heating to 75 ℃ after complete mixing and keeping for 40 min to complete polycondensation reaction to obtain sol;
(4) putting the glass cleaned in advance into the sol, slowly pulling out the glass at a constant speed, drying the lower surface at 60 ℃, and thermally curing at 200 ℃. The effect of the ratio of methyltrimethoxysilane to Si-Al-OOH is shown in Table 1.
Example 5
A silicon dioxide-organic silicon composite system is a coating material and is prepared by the following steps:
(1) adding 10g of methyltrimethoxysilane, 0.9g of dimethyldimethoxysilane, 50g of aluminum-silicon sol and 30g of water into a three-neck flask provided with a stirrer, a condenser, a thermometer and a dropping funnel, stirring and uniformly dispersing, dropwise adding zinc oxide acetic acid solution to adjust the pH to be =6, then adding 0.7g of isopropanol, stirring at high speed in a water bath at 55 ℃, homogenizing for 70min, and hydrolyzing;
(2) adding 0.5g of silane coupling agent KH560 into a dropping funnel, accelerating and stirring at constant temperature for 1h, and mixing the coupling agent;
(3) heating to 85 ℃ after complete mixing and keeping for 80 min to complete polycondensation reaction to obtain sol;
(4) putting the glass cleaned in advance into the sol, slowly pulling out the glass at a constant speed, drying the lower surface at 60 ℃, and thermally curing at 200 ℃. The effect of the methyltrimethoxysilane to Si-Al-OOH ratio is shown in Table 1:
Figure RE-RE-DEST_PATH_IMAGE001
。

Claims (6)

1. a preparation method of a silicon dioxide-organic silicon composite system, the silicon dioxide-organic silicon composite system is a coating material, and is characterized in that organic siloxane and aluminum-silicon sol are used as raw materials, zinc oxide acetic acid is used as a catalyst, and the preparation method comprises the following steps:
(1) putting a proper amount of methyltrimethoxysilane and dimethyldimethoxysilane into a flask, adding a proper amount of water, aluminum-silicon sol, zinc oxide acetic acid solution and isopropanol, stirring uniformly, and heating and hydrolyzing in a constant-temperature water bath, wherein the ratio of the methyltrimethoxysilane to the dimethyldimethoxysilane is (30-5): 1; the ratio of the aluminum-silicon sol to the methyltrimethoxysilane is (2-5) to 1; the adding amount of the silane coupling agent is 0.1 to 0.8 percent of the total amount, and the adding amount of the zinc oxide acetic acid is 0.5 to 2 percent of the total amount; the ratio of methyltrimethoxysilane to isopropanol is (5-30) to 1;
(2) adding a silane coupling agent KH560, stirring at a constant temperature, and mixing the coupling agents;
(3) after mixing completely, keeping for a certain time at 60-90 ℃ to complete the polycondensation reaction;
(4) and (3) putting the substrate cleaned in advance into the sol, slowly pulling out at a constant speed, and drying and curing to obtain the nano-composite material.
2. The method for preparing a silica-organosilicon composite system according to claim 1, wherein: the temperature of the thermostatic water bath in the step (1) is 35-60 ℃.
3. The method for preparing a silica-organosilicon composite system according to claim 1, wherein: the step (2) is as follows: the ratio of the methyltrimethoxysilane to the silane coupling agent is (20-100): 1.
4. The method for preparing a silica-organosilicon composite system according to claim 1, wherein: the drying temperature in the step (4) is 60 ℃; the curing temperature was 200 ℃.
5. A silica-organosilicon composite system, characterized by being prepared according to the method of any of claims 1 to 4.
6. Use of the silica-silicone composite system according to claim 5 as a suitable light-filtering coating film for lamp bulbs.
CN201910933706.6A 2019-09-29 2019-09-29 Preparation method of silicon dioxide-organic silicon composite system, product and application thereof Pending CN110713790A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101955728A (en) * 2009-07-17 2011-01-26 黄祥道 Organic-inorganic hybrid wear-resistant transparent coating for reinforcing surface of optical plastics
CN102134411A (en) * 2011-01-18 2011-07-27 浙江大学 Method for preparing organic-inorganic composite sol used for preventing corrosion on surface of metal aluminum plate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101955728A (en) * 2009-07-17 2011-01-26 黄祥道 Organic-inorganic hybrid wear-resistant transparent coating for reinforcing surface of optical plastics
CN102134411A (en) * 2011-01-18 2011-07-27 浙江大学 Method for preparing organic-inorganic composite sol used for preventing corrosion on surface of metal aluminum plate

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