CN112724718A - Preparation method of inorganic mineral material modified inorganic silicone resin - Google Patents
Preparation method of inorganic mineral material modified inorganic silicone resin Download PDFInfo
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- CN112724718A CN112724718A CN202011592111.8A CN202011592111A CN112724718A CN 112724718 A CN112724718 A CN 112724718A CN 202011592111 A CN202011592111 A CN 202011592111A CN 112724718 A CN112724718 A CN 112724718A
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- silica sol
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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
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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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
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1687—Use of special additives
Abstract
The invention discloses a preparation method of inorganic mineral material modified inorganic silicon resin, which comprises the following steps: placing the silica sol solution with the pH value of 8-11 in a reaction kettle, heating to 50-80 ℃, and continuously stirring; after hydrophilic organic silicon monomer accounting for 1.5-3% of the mass of the silica sol solution is dripped, the temperature in S1 is kept unchanged, and the copolymerization is completed after the reaction is carried out for 3-4 h; reducing the temperature to 50-60 ℃, dropwise adding 1-3% of hydrophobic organic silicon monomer, reacting for 5-6h, and finishing copolymerization again; adding flaky or needle-shaped inorganic mineral powder accounting for 5-20% of the mass of the silica sol solution into the resin in S3, increasing the rotating speed to 500-1000 r/min, and continuously reacting for 1-2 h. Through the arrangement, the nano inorganic silicon resin prepared by the method has good film forming property and hydrophobicity, can be used for preparing pure inorganic building coatings, and can also be compounded with common emulsion to produce inorganic building coatings meeting the industrial standard.
Description
Technical Field
The invention relates to the field of inorganic coatings, in particular to a preparation method of inorganic mineral material modified inorganic silicone resin.
Background
The inorganic coating is an inorganic polymer coating which is composed of inorganic polymer, metal subjected to dispersion activation, metal oxide nano material and rare earth ultrafine powder, can quickly react with iron atoms on the surface of a steel structure to generate an inorganic polymer anticorrosive coating which has physical and chemical double protection effects and is firmly combined with a matrix through a chemical bond, has no pollution to the environment, long service life and anticorrosive performance reaching the international advanced level, and is a high-tech upgrading product meeting the requirement of environmental protection.
Potassium silicate inorganic exterior wall coatings and silica sol inorganic exterior wall coatings have been developed in recent years in China. Inorganic coatings have also begun to be used in China in a large amount as exterior wall decoration and protection, and the excellent weather resistance and color retention and air permeability of the inorganic coatings are accepted by people.
However, after long-term use and testing, the two inorganic exterior wall coatings respectively have the following disadvantages: the potassium silicate inorganic paint has poor compatibility, needs special emulsion, auxiliary agent, color paste and powder, has poor storage stability, slow film forming, early water resistance, poor scrubbing resistance and long curing time, and is accompanied with salting-out phenomenon to cause blooming. The silica sol inorganic paint has fast filming, violent shrinkage in drying process, too strong rigidity, water resistance, compatibility and color development property slightly superior to potassium silicate, but has difference from actual requirements.
In order to solve the problems, the application provides a preparation method of nano inorganic silicon resin.
Disclosure of Invention
The invention aims to provide a preparation method of inorganic mineral material modified inorganic silicone resin, and the nano inorganic silicone resin prepared by the method has good film forming property and hydrophobicity, can be used for preparing pure inorganic building coating, and can also be compounded with common emulsion to produce inorganic building coating meeting the industrial standard.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of inorganic mineral material modified inorganic silicone resin comprises the following steps:
s1, placing the silica sol solution with the pH value of 8-11 in a reaction kettle, heating to 50-80 ℃, and continuously stirring at the rotating speed of 60-80 revolutions;
s2, dropwise adding a hydrophilic organic silicon monomer accounting for 1.5-3% of the mass of the silica sol solution, keeping the temperature in the S1 unchanged, and reacting for 3-4 hours to complete copolymerization;
s3, reducing the temperature to 50-60 ℃, dropwise adding 1-3% of hydrophobic organic silicon monomer, increasing the rotation speed to 80-120 r, reacting for 5-6h, and finishing copolymerization again;
s4, adding flaky or needle-shaped inorganic mineral powder accounting for 5-20% of the mass of the silica sol solution into the resin in the S3, increasing the rotating speed to 500-1000 r/min, and continuously reacting for 1-2 h.
By adopting the technical scheme, the compatibility of the pure hydrophilic inorganic silicon resin and the hydrophobic organic silicon monomer is improved by copolymerizing the pure hydrophilic inorganic silicon resin and the hydrophilic inorganic silicon monomer; the film forming property and the hydrophobicity of the inorganic silicon resin are greatly improved through two times of polymerization; needle-like or flake-like inorganic mineral material to amorphous SiO2The inorganic coating is converted into a core-shell structure with an excellent crystal structure, and the core-shell structure is a crystal with a compact and regular structure, so that the film forming property, the construction property, the adhesive force, the contamination resistance and the water resistance of the prepared inorganic coating are greatly improved.
Preferably, the hydrophilic organosilicon monomer is gamma-glycidoxypropyltrimethoxysilane and/or gamma-methacryloxytrimethoxysilane.
Through the technical scheme, flexible selection can be performed according to the cost.
Preferably, the hydrophobic organosilicon monomer is methyl trioxysilane and/or isobutyl trioxysilane.
Through the technical scheme, flexible selection can be performed according to the cost.
Preferably, the silica sol solution is selected from LS-30 type silica sol solution of Zhejiang Uuda chemical company Limited, SiO2The content is 30 percent.
Preferably, the main material of the inorganic mineral powder is whisker containing calcium ions.
Preferably, the inorganic silicone resin is modified by an inorganic mineral material.
Through the technical scheme, the inorganic silicon resin has good film forming property and hydrophobicity.
Preferably, the nano inorganic silicone resin modified by organosilicon monomer.
Through the technical scheme, the inorganic silicon resin has good film forming property and hydrophobicity, and also has good mechanical strength, mechanical property, wear resistance, heat resistance, cracking resistance, chalking resistance and water resistance.
Preferably, a building emulsion is added as a film former.
Through the technical scheme, the building emulsion can improve the film forming property of the resin.
Preferably, one or more of titanium dioxide, kaolin and heavy calcium carbonate are added as pigments and fillers.
By the technical scheme, the titanium dioxide, kaolin and heavy calcium carbonate have the advantage of good effect as pigments and fillers.
Compared with the prior art, the invention has the beneficial effects that:
(1) the compatibility of the pure hydrophilic inorganic silicone resin and the hydrophobic organic silicon monomer is improved by copolymerization with the relatively hydrophilic organic silicon monomer;
(2) the film forming property, the hydrophobicity and the color development property of the inorganic silicon resin are greatly improved through two times of polymerization;
(3) needle-like or flake-like inorganic mineral material to amorphous SiO2The inorganic coating is converted into a core-shell structure with an excellent crystal structure, and the core-shell structure is a crystal with a compact and regular structure, so that the film forming property, the construction property, the adhesive force, the stain resistance and the water resistance of the inorganic coating prepared by the method are greatly improved.
Drawings
FIG. 1 is a graph showing the results of comparison between examples 3 to 6 of the present invention and comparative example 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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.
Referring to fig. 1, the following is an embodiment of the present invention:
example 1: a preparation method of inorganic mineral material modified inorganic silicone resin comprises the following steps:
s1, placing the silica sol solution with the pH value of 8-11 in a reaction kettle, and heating to 50-80 ℃; the silica sol solution is selected from LS-30 type silica sol solution of Zhejiang Uuda chemical Co., Ltd, SiO2The content is 30 percent; continuously stirring at the rotating speed of 60-80 revolutions;
s2, dripping hydrophilic organic silicon monomers accounting for 1.5-3% of the mass of the silica sol solution; the hydrophilic organic silicon monomer is gamma-glycidoxypropyltrimethoxysilane and/or gamma-methacryloyloxytrimethoxysilane; keeping the temperature in the S1 constant, and reacting for 3-4h to complete copolymerization;
s3, reducing the temperature to 50-60 ℃, and dropwise adding 1-3% of hydrophobic organic silicon monomer; the hydrophobic organic silicon monomer is methyl trioxysilane and/or isobutyl trioxysilane; increasing the rotating speed to 80-120 revolutions, reacting for 5-6h, and finishing copolymerization again;
s4, adding flaky or needle-shaped inorganic mineral powder which accounts for 5-20% of the mass of the silica sol solution into the resin in the S3, increasing the rotating speed to 500-1000 r/min, and continuously reacting for 1-2h, wherein the main material of the inorganic mineral powder is whisker containing calcium ions.
Example 2: an inorganic mineral material modified inorganic silicone resin. Prepared by the method of example one. When in use, the building emulsion can be added as a film forming material to improve the film forming property, and one or more of titanium dioxide, kaolin and heavy calcium carbonate are added as pigment and filler.
Example 3: an organic silicon monomer modified nano inorganic silicone resin is prepared by the following method:
s1, placing the silica sol solution with the pH value of 8-11 in a reaction kettle, and heating to 50-80 ℃; the silica sol solution is selected from LS-30 type silica sol solution of Zhejiang Uuda chemical Co., Ltd, SiO2The content is 30 percent; continuously stirring at the rotating speed of 60-80 revolutions;
s2, dropwise adding a hydrophilic organic silicon monomer accounting for 1.5% of the mass of the silica sol solution; the hydrophilic organic silicon monomer is gamma-glycidol ether oxygen propyl trimethoxy silane; keeping the temperature in the S1 constant, and reacting for 3-4h to complete copolymerization;
s3, reducing the temperature to 50-60 ℃, and dropwise adding 1% of hydrophobic organic silicon monomer; the hydrophobic organic silicon monomer is methyl trioxysilane; increasing the rotating speed to 80-120 revolutions, reacting for 5-6h, and finishing copolymerization again;
s4, adding flaky or needle-shaped inorganic mineral powder which accounts for 5% of the mass of the silica sol solution into the resin in the S3, increasing the rotating speed to 500-1000 r/min, and continuously reacting for 1-2h, wherein the main material of the inorganic mineral powder is whisker containing calcium ions.
Example 4: a preparation method of inorganic mineral material modified inorganic silicone resin is prepared by the following steps:
s1, placing the silica sol solution with the pH value of 8-11 in a reaction kettle, and heating to 50-80 ℃; the silica sol solution is selected from LS-30 type silica sol solution of Zhejiang Uuda chemical Co., Ltd, SiO2The content is 30 percent; continuously stirring at the rotating speed of 60-80 revolutions;
s2, dropwise adding hydrophilic organic silicon monomers accounting for 3% of the mass of the silica sol solution; the hydrophilic organic silicon monomer is gamma-methacryloxy trimethoxy silane; keeping the temperature in the S1 constant, and reacting for 3-4h to complete copolymerization;
s3, reducing the temperature to 50-60 ℃, and dropwise adding 3% of hydrophobic organic silicon monomer; the hydrophobic organic silicon monomer is isobutyl trioxysilane; increasing the rotating speed to 80-120 revolutions, reacting for 5-6h, and finishing copolymerization again;
s4, adding flaky or needle-shaped inorganic mineral powder accounting for 20% of the mass of the silica sol solution into the resin in the S3, increasing the rotating speed to 500-1000 r/min, and continuously reacting for 1-2h, wherein the main material of the inorganic mineral powder is whisker containing calcium ions.
Example 5: a preparation method of inorganic mineral material modified inorganic silicone resin is prepared by the following steps:
s1, placing the silica sol solution with the pH value of 8-11 in a reaction kettle, and heating to 50-80 ℃; the silica sol solution is selected from LS-30 of Zhejiang Uuda chemical Co., LtdSilica Sol solution, SiO2The content is 30 percent; continuously stirring at the rotating speed of 60-80 revolutions;
s2, dropwise adding hydrophilic organic silicon monomers accounting for 3% of the mass of the silica sol solution; the hydrophilic organic silicon monomer is gamma-glycidoxypropyltrimethoxysilane and gamma-methacryloyloxytrimethoxysilane, and the mass ratio of the gamma-glycidoxypropyltrimethoxysilane to the gamma-methacryloyloxytrimethoxysilane is 1: 1; keeping the temperature in the S1 constant, and reacting for 3-4h to complete copolymerization;
s3, reducing the temperature to 50-60 ℃, and dropwise adding 3% of hydrophobic organic silicon monomer; the hydrophobic organic silicon monomer is methyl trioxysilane and isobutyl trioxysilane, and the mass ratio of the methyl trioxysilane to the isobutyl trioxysilane is 1: 1; increasing the rotating speed to 80-120 revolutions, reacting for 5-6h, and finishing copolymerization again;
s4, adding flaky or needle-shaped inorganic mineral powder accounting for 15% of the mass of the silica sol solution into the resin in the S3, increasing the rotating speed to 500-1000 r/min, and continuously reacting for 1-2h, wherein the main material of the inorganic mineral powder is whisker containing calcium ions.
Example 6: a preparation method of inorganic mineral material modified inorganic silicone resin is prepared by the following steps:
s1, placing the silica sol solution with the pH value of 8-11 in a reaction kettle, and heating to 50-80 ℃; the silica sol solution is selected from LS-30 type silica sol solution of Zhejiang Uuda chemical Co., Ltd, SiO2The content is 30 percent; continuously stirring at the rotating speed of 60-80 revolutions;
s2, dropwise adding hydrophilic organic silicon monomers accounting for 2% of the mass of the silica sol solution; the hydrophilic organic silicon monomer is gamma-glycidoxypropyltrimethoxysilane and gamma-methacryloyloxytrimethoxysilane, and the mass ratio of the gamma-glycidoxypropyltrimethoxysilane to the gamma-methacryloyloxytrimethoxysilane is 1: 1; keeping the temperature in the S1 constant, and reacting for 3-4h to complete copolymerization;
s3, reducing the temperature to 50-60 ℃, and dropwise adding 2% of hydrophobic organic silicon monomer; the hydrophobic organic silicon monomer is methyl trioxysilane and isobutyl trioxysilane, and the mass ratio of the methyl trioxysilane to the isobutyl trioxysilane is 1: 1; increasing the rotating speed to 80-120 revolutions, reacting for 5-6h, and finishing copolymerization again;
s4, adding flaky or needle-shaped inorganic mineral powder accounting for 15% of the mass of the silica sol solution into the resin in the S3, increasing the rotating speed to 500-1000 r/min, and continuously reacting for 1-2h, wherein the main material of the inorganic mineral powder is whisker containing calcium ions.
Comparative example 1: as a comparative example, a conventional inorganic silicone resin coating material commercially available on the market was used.
The properties of the inorganic silicone resins prepared in examples 3 to 6, which were diluted so that the solid content was the same as that of comparative example 1, were compared, and the results are shown in fig. 1. From the above results, it can be seen that the inorganic silicone resin prepared according to the method of the present application has good film forming property, workability, adhesion, stain resistance, and water resistance.
In conclusion, the beneficial effects of the invention are as follows: (1) the compatibility of the pure hydrophilic inorganic silicone resin and the hydrophobic organic silicon monomer is improved by copolymerization with the relatively hydrophilic organic silicon monomer; (2) the film forming property and the hydrophobicity of the inorganic silicon resin are greatly improved through two times of polymerization; (3) needle-like or flake-like inorganic mineral material to amorphous SiO2The inorganic coating is converted into a core-shell structure with an excellent crystal structure, and the core-shell structure is a crystal with a compact and regular structure, so that the film forming property, the construction property, the adhesive force, the stain resistance and the water resistance of the inorganic coating prepared by the method are greatly improved.
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. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. A preparation method of inorganic mineral material modified inorganic silicone resin is characterized by comprising the following steps: the method comprises the following steps:
s1, placing the silica sol solution with the pH value of 8-11 in a reaction kettle, and heating to 50-80 ℃;
continuously stirring at the rotating speed of 60-80 r/min;
s2, dripping hydrophilic organic silicon monomers accounting for 1.5-3% of the mass of the silica sol solution;
keeping the temperature in the S1 constant, and reacting for 3-4h to complete copolymerization;
s3, reducing the temperature to 50-60 ℃, and dropwise adding 1-3% of hydrophobic organic silicon monomer;
increasing the rotating speed to 80-120 r/min, reacting for 5-6h, and finishing copolymerization again;
s4, adding flaky or needle-shaped inorganic mineral powder accounting for 5-20% of the mass of the silica sol solution into the resin in the S3, increasing the rotating speed to 500-1000 r/min, and continuously reacting for 1-2 h.
2. The method for preparing inorganic mineral material modified inorganic silicone resin according to claim 1, wherein: the hydrophilic organosilicon monomer is gamma-glycidoxypropyltrimethoxysilane and/or gamma-methacryloyloxytrimethoxysilane.
3. The method for preparing inorganic mineral material modified inorganic silicone resin according to claim 2, wherein: the hydrophobic organic silicon monomer is methyl trioxysilane and/or isobutyl trioxysilane.
4. The method for preparing inorganic mineral material modified inorganic silicone resin according to claim 3, wherein: the silica sol solution is selected from LS-30 type silica sol solution and SiO of Zhejiang Uuda chemical company Limited2The content is 30 percent.
5. The method for preparing inorganic mineral material modified inorganic silicone resin according to claim 4, wherein: the main material of the inorganic mineral powder is whisker containing calcium ions.
6. An inorganic mineral material-modified inorganic silicone resin produced by any one of claims 1 to 5.
7. The inorganic mineral material modified inorganic silicone resin according to claim 6, wherein: adding the building emulsion as a film forming material.
8. The inorganic mineral material modified inorganic silicone resin according to claim 7, wherein: one or more of titanium dioxide, kaolin and heavy calcium carbonate are added as pigment and filler.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115612301A (en) * | 2022-09-27 | 2023-01-17 | 江西联锴科技有限公司 | Hydrophilic organic/inorganic composite spherical silicon resin and preparation method and application thereof |
| CN115627086A (en) * | 2022-09-29 | 2023-01-20 | 广州先进技术研究所 | High-temperature-resistant wide-spectrum super-lyophobic coating and preparation method thereof |
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| US20100062200A1 (en) * | 2007-03-09 | 2010-03-11 | Heribert Domes | Method for coating metal surfaces using an aqueous compound having polymers, the aqueous compound, and use of the coated substrates |
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