CN113121938A - Silicon dioxide acrylic resin composite particle and preparation method thereof - Google Patents
Silicon dioxide acrylic resin composite particle and preparation method thereof Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- 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
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/32—Radiation-absorbing paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/65—Additives macromolecular
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- C08L2201/00—Properties
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Abstract
The invention relates to a silicon dioxide acrylic resin composite particle and a preparation method thereof, wherein the silicon dioxide acrylic resin composite particle is of a core-shell structure, namely acrylic resin coats nano silicon dioxide; the nano silicon dioxide is processed by gamma-methacryloxypropyltrimethoxysilane modified nano-silica. The invention prepares the silicon dioxide acrylic resin composite particles with core-shell structures by a dispersion polymerization method. SiO 22The modification of the particle surface is to realize the complete coating of SiO by AA2Precondition for the particles, SiO2The particles can only be coated with SiO by AA after being modified by gamma-methacryloxypropyltrimethoxysilane2And (3) granules.
Description
Technical Field
The invention relates to a coating heat insulation component, in particular to a silicon dioxide acrylic resin composite particle.
Background
The heat insulating material, a material capable of retarding heat flow transmission, and the early heat insulating material are mostly used in buildings and industries, and are mostly barrier heat insulating materials, and the transparency and the lighting property are not high. If the nano transparent heat insulation coating can be successfully applied to the building glass, the infrared radiation and the ultraviolet rays of sunlight passing through the transparent glass can be effectively blocked, the transparency of visible light can not be changed when the visible light enters the room, and long waves radiated by indoor objects can be kept indoors in winter, so that a new way for building energy conservation is opened up.
The heat insulation coating which can be well applied to the glass surface of a building needs to ensure the heat insulation effect, needs a coating layer with good adhesive force and has good transparency. Most of the existing preparation methods of the heat-insulating coating are to add inorganic substances or a plurality of nano materials with heat-insulating property as fillers, which not only increases the process difficulty and the dispersion time, but also has great influence on the transparency of an organism.
In recent years, silica aerogel has been studied as a hot spot, and although the heat insulation performance and transparency can be greatly improved, the stability and workability of the coating are greatly affected.
Disclosure of Invention
The purpose of the invention is: the problem of lack an excellent coating heat insulation functional component among the prior art is solved, can solve current heat insulation coating transparency, adhesive force after using this heat insulation functional component, the constructability is not good problem. The invention provides a silicon dioxide acrylic resin composite particle and a preparation method thereof.
The technical scheme for realizing the purpose of the invention is as follows:
a silicon dioxide acrylic resin composite particle is of a core-shell structure and comprises two types of matrix particles, namely nano silicon dioxide and acrylic resin, wherein the nano silicon dioxide is coated by the acrylic resin; the nano silicon dioxide is modified nano silicon dioxide modified by gamma-methacryloxypropyltrimethoxysilane.
The particle size of one nano-silica of the matrix of the silicon dioxide acrylic resin composite particle is 1-10nm, and the modified nano-silica is prepared from the following reactants: nano silicon dioxide, water, ammonia water and gamma-methacryloxypropyltrimethoxysilane, wherein the molar ratio of the nano silicon dioxide to the gamma-methacryloxypropyltrimethoxysilane is 1:10-20, and the most preferable ratio is 1: 18.
The silicon dioxide acrylic resin composite particle is prepared by the following components: 0.05-0.3 mol.L of modified nano silicon dioxide-1(ii) a 0.1-1 mol.L of acrylic resin-1(ii) a 0.1-0.5 mmol.L of stabilizer-1(ii) a 1-10 mmol. L of initiator-1(ii) a 1-10ml/L of water; the remaining volume of the formulation is alcohol. Wherein the stabilizer is polyvinylpyrrolidone, and the initiator is azobisisobutyronitrile. The alcohol is selected from the group consisting of methanol, ethanol, propanol and isomers thereof, butanol and isomers thereof, and most preferably ethanol.
The optimal formula is as follows: 0.1 mol.L of modified nano silicon dioxide-1(ii) a Acrylic resin 0.6 mol. L-1(ii) a 0.23 mmol. L of stabilizer-1(ii) a Initiator 6.1 mmol. L-1(ii) a 5.5ml/L of water, and the rest volume of the component ethanol in the formula.
By combining the preparation method of the invention, the formula has good monodispersity, smooth surface and SiO coating2The number of particles is close to SiO2a/AA composite particle.
In another aspect of the present invention, a method for preparing silica acrylic resin composite particles comprises the steps of: (1) preparing modified nano silicon dioxide; (2) preparing silicon dioxide acrylic resin composite particles;
adding an alcoholic solution of nano-silica into a reaction container with a cooling device, adding water, dropwise adding ammonia water, adding gamma-methacryloxypropyl trimethoxysilane, stirring and heating under the protection of inert gas, preferably nitrogen, reacting, performing post-treatment to obtain modified nano-silica, and storing the modified nano-silica in alcohol, preferably ethanol, for later use;
and (2) sequentially adding a stabilizer, an alcohol solution of modified nano-silica, water and alcohol, preferably absolute ethyl alcohol, into a reaction solvent, then slowly dropwise adding acrylic resin dissolved with an initiator under the protection of inert gas, preferably nitrogen, stirring, heating, reacting, and performing post-treatment to obtain the silicon dioxide acrylic resin composite particles.
According to the preparation method of the silicon dioxide acrylic resin composite particles, the reaction temperature in the step (1) is 30-70 ℃, preferably 50-60 ℃, and most preferably 50 ℃; the reaction temperature in the step (2) is 50-90 ℃, preferably 70-75 ℃, and most preferably 70 ℃.
According to the preparation method of the silicon dioxide acrylic resin composite particles, the dropping speed in the step (2) is 0.2-8ml/min, preferably 0.3-6ml/min, and more preferably 0.5-3 ml/min.
The invention has the positive effects that:
the invention prepares the silicon dioxide acrylic resin (SiO) with a core-shell structure by a dispersion polymerization method2/AA) composite particles. SiO 22The modification of the particle surface is to realize the complete coating of SiO by AA2Precondition for the particles, SiO2The particles can only be coated with SiO by AA after being modified by gamma-Methacryloxypropyltrimethoxysilane (MPS)2Particles; SiO 22Hydroxyl on the surface of the particle is combined with carboxyl of MPS, and then is condensed and grafted with the group on the surface of acrylic acid to form a hand-pulled structure.
In the present invention, silica acrylic resin (SiO)2the/AA composite particles are used in coatings due to the silica/acrylic resin (SiO)2the/AA) composite particles have good wetting contact between the acrylic resin and the glass substrate, so that the adhesion can be increased; simultaneously, the transparency is increased because of the nano SiO2The particles have the ability to absorb ultraviolet light and can be considered substantially completely transparent. According to the reference PVDF fluorocarbon coating detection standard GB/T5237.5-2000, the pencil hardness (scratch) is measured to be more than or equal to F; the adhesive force is less than or equal to grade 1; the film-forming material has a thickness of nanometer (e.g., 30nm and 75nm), a light transmittance of greater than 91.0%, and a haze of less than 0.4%.
Drawings
FIG. 1 shows a modified SiO of the present invention2Transmission electron micrograph
FIG. 2 shows a silica acrylic resin (SiO) of the present invention2Transmission electron micrograph of/AA) composite particle
Detailed Description
(example 1)
A1000 mL four-necked flask equipped with a condenser was charged with 6gSiO250mL of the ethanol solution of the particles was added with 5mL of water, about 5 drops of ammonia water were added dropwise, and 320.4g of modified coupling agent MPS was added. Then the four-necked flask is moved into a constant-temperature oil bath pot in N2Under the protection of (2), stirring and heating, the reaction temperature is 50 ℃, after 24 hours of reaction, centrifugal separation is carried out, and the obtained grafted SiO2The granules were kept in ethanol for further use.
0.58g of stabilizer (PVP) and 166.8g of modified SiO were sequentially added to a four-necked flask2Then 72.2g of acrylic resin dissolved with 0.164g of initiator (AIBN) is slowly dripped under the condition of introducing nitrogen, the dripping speed is 3.5ml/min, the mixture is stirred for about 2 hours, heated to 75 ℃, reacted for 12 hours, centrifugally separated and stored in ethanol.
The resulting silica/acrylic resin (SiO)2and/AA) composite particles 8.25g are added into a polyvinylidene fluoride dispersion system 5.5kg, then defoaming agent (commercially available, Germany BYK-141)11g and leveling agent (commercially available, Germany BYK-333) 9.9g are added and evenly mixed to obtain the application coating of the invention. The resulting coating was sprayed on glass to obtain a coating film having a thickness of about 50 to 60 μm, and the surface of the coating film was dried. The resulting coatings were tested and the results are shown in table 1.
(example 2)
A1000 mL four-necked flask equipped with a condenser was charged with 6gSiO250mL of ethanol solution of the particles was added with 5mL of water, about 5 drops of ammonia water were added dropwise, and 356g of modified coupling agent MPS was added. Then will beTransferring the four-necked bottle into a constant-temperature oil bath pot in a nitrogen atmosphere2Under the protection of (2), stirring and heating, the reaction temperature is 50 ℃, after 24 hours of reaction, centrifugal separation is carried out, and the obtained grafted SiO2The granules were kept in ethanol for further use.
0.87g of stabilizer (PVP) and 166.8g of modified SiO were sequentially added to a four-necked flask2Then 72.5g of acrylic resin dissolved with 0.492g of initiator (AIBN) is slowly dripped under the condition of introducing nitrogen, the dripping speed is 0.5ml/min, the mixture is stirred for about 2 hours, the temperature is started to be 75 ℃, the mixture is reacted for 12 hours, and the mixture is centrifugally separated and stored in ethanol.
The resulting silica/acrylic resin (SiO)2The coating is prepared by adding 8.25g of/AA) composite particles into 10.8kg of vinylidene fluoride-hexafluoropropylene copolymer dispersion system, adding 15.2g of defoaming agent (commercially available, ByK-141 in Germany) and 21.6g of flatting agent (commercially available, ByK-333 in Germany) and uniformly mixing. The resulting coating was sprayed on glass to obtain a coating film having a thickness of about 50 to 60 μm, and the surface of the coating film was dried. The resulting coatings were tested and the results are shown in table 1.
(example 3)
A1000 mL four-necked flask equipped with a condenser was charged with 6gSiO250mL of ethanol solution of the particles was added with 5mL of water, about 5 drops of ammonia water were added dropwise, and 89g of modified coupling agent MPS was added. Then transferring the four-necked bottle into a constant-temperature oil bath kettle, stirring and heating under the protection of helium, reacting at 50 ℃ for 24 hours, and performing centrifugal separation to obtain the grafted SiO2The granules were kept in ethanol for further use.
0.815g of stabilizer (PVP) and 250.2g of modified SiO were sequentially added to a four-necked flask2Then 72.2g of acrylic resin dissolved with 1.64g of initiator (AIBN) is slowly dripped under the condition of introducing helium, the dripping speed is 7.6ml/min, the mixture is stirred for about 2 hours, heated to 75 ℃, reacted for 12 hours, centrifugally separated and stored in ethanol.
The resulting silica/acrylic resin (SiO)2/AA) composite particle 8.25g, 12.75kg of tetrafluoroethylene-propylene were addedAnd (3) adding 17.3g of defoaming agent (commercially available, BYK-141, Germany) and 25.8g of flatting agent (commercially available, BYK-333, Germany) into the polymer dispersion system, and uniformly mixing to obtain the application coating. The resulting coating was sprayed on glass to obtain a coating film having a thickness of about 50 to 60 μm, and the surface of the coating film was dried. The resulting coatings were tested and the results are shown in table 1.
And (3) performance testing:
and (4) testing standard: GB/T6739-2006 GB/T9286-1998
And (3) testing items: hardness, adhesion, transmittance and haze of pencil
And (3) testing conditions are as follows: temperature (20. + -. 2 ℃), relative humidity (50. + -. 10)%
TABLE 1
| Hardness of pencil | Adhesion force | Light transmittance | Haze degree | |
| Example 1 | 1H | Level 0 | 91.4％ | 0.36％ |
| Example 2 | F | Level 0 | 92.3％ | 0.34％ |
| Example 3 | 1H | Level 0 | 91.7％ | 0.31％ |
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like 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 silica acrylic resin composite particle characterized by: the silicon dioxide acrylic resin composite particles are of a core-shell structure, namely, acrylic resin coats nano silicon dioxide; the nano silicon dioxide is modified nano silicon dioxide modified by gamma-methacryloxypropyltrimethoxysilane.
2. The silica acrylic resin composite particle according to claim 1, characterized in that: the modified nano silicon dioxide is prepared from the following reactants: nano silicon dioxide, water, ammonia water and gamma-methacryloxypropyl trimethoxysilane, wherein the molar ratio of the nano silicon dioxide to the gamma-methacryloxypropyl trimethoxysilane is 1: 10-20.
3. The silica acrylic resin composite particle according to claim 2, characterized in that: the particle size of the nano silicon dioxide is 1-10 nm.
4. The silica acrylic resin composite particle according to claim 1, 2 or 3, characterized in that: the silicon dioxide acrylic resin composite particle is prepared by the following components: 0.05-0.3mol L of modified nano silicon dioxide-1(ii) a Acrylic resin 0.1-1.0mol L-1(ii) a Stabilizer 0.1-0.5mmol L-1(ii) a Initiator 1-10mmol L-1(ii) a Water 1-10mlL-1(ii) a The remaining volume of the formulation is alcohol.
5. The silica acrylic resin composite particle according to claim 4, characterized in that: the stabilizer is polyvinylpyrrolidone, and the initiator is azobisisobutyronitrile.
6. The silica acrylic resin composite particle according to claim 4, characterized in that: the alcohol is selected from methanol, ethanol, propanol and isomers thereof, butanol and isomers thereof.
7. A method for preparing the silica acrylic resin composite particle according to claim 1, 2 or 3, characterized by comprising the steps of: (1) preparing modified nano silicon dioxide; (2) preparing silicon dioxide acrylic resin composite particles;
adding an alcoholic solution of nano-silica into a reaction container with a cooling device, adding water, dropwise adding ammonia water, adding gamma-methacryloxypropyl trimethoxysilane, stirring and heating under the protection of inert gas for reaction, performing post-treatment after the reaction is finished to obtain modified nano-silica, and storing the modified nano-silica in alcohol for later use;
and (2) sequentially adding a stabilizer, an alcohol solution of modified nano-silica, water and alcohol into a reaction solvent, then slowly dropwise adding acrylic resin dissolved with an initiator under the protection of inert gas, stirring, heating, reacting, and performing post-treatment to obtain the silicon dioxide acrylic resin composite particles.
8. The method for producing silica acrylic resin composite particles according to claim 7, characterized in that: the adding amount of each reactant in the step (2) is as follows: 0.05-0.3mol L of modified nano silicon dioxide-1(ii) a Acrylic resin 0.1-1.0mol L-1(ii) a Stabilizer 0.1-0.5mol L-1(ii) a Initiator 1-10mmol L-1(ii) a Water 1-10mlL-1(ii) a The balance being alcohol.
9. The method for producing the silica acrylic resin composite particle according to claim 4, characterized in that: the reaction temperature in the step (1) is 30-70 ℃, and preferably 50-60 ℃; the reaction temperature in the step (2) is 50-90 ℃, and preferably 70-75 ℃.
10. The method for producing the silica acrylic resin composite particle according to claim 4, characterized in that: the dropping speed of the step (2) is 0.2-8ml/min, preferably 0.3-6ml/min, and more preferably 0.5-3 ml/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133499A (en) * | 2021-11-26 | 2022-03-04 | 上海金力泰化工股份有限公司 | Micro acrylic capsule resin and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108946A (en) * | 2007-07-12 | 2008-01-23 | 深圳清华大学研究院 | Nano transparent insulating paint and its preparing process |
| CN105061700A (en) * | 2015-08-14 | 2015-11-18 | 华南理工大学 | Nano-silica/polyacrylate organic and inorganic hybrid water-dispersible resin and preparation method thereof |
| US20190046939A1 (en) * | 2017-08-09 | 2019-02-14 | Petrochina Company Limited | Nano-Silica Dispersion Having Amphiphilic Properties And A Double-Particle Structure And Its Production Method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101108946A (en) * | 2007-07-12 | 2008-01-23 | 深圳清华大学研究院 | Nano transparent insulating paint and its preparing process |
| CN105061700A (en) * | 2015-08-14 | 2015-11-18 | 华南理工大学 | Nano-silica/polyacrylate organic and inorganic hybrid water-dispersible resin and preparation method thereof |
| US20190046939A1 (en) * | 2017-08-09 | 2019-02-14 | Petrochina Company Limited | Nano-Silica Dispersion Having Amphiphilic Properties And A Double-Particle Structure And Its Production Method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114133499A (en) * | 2021-11-26 | 2022-03-04 | 上海金力泰化工股份有限公司 | Micro acrylic capsule resin and preparation method and application thereof |
| CN114133499B (en) * | 2021-11-26 | 2024-04-23 | 上海金力泰化工股份有限公司 | Micro acrylic capsule resin and preparation method and application thereof |
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Application publication date: 20210716 |