CN114736546A - Lithium silicate-based inorganic resin and synthesis method and application thereof - Google Patents
Lithium silicate-based inorganic resin and synthesis method and application thereof Download PDFInfo
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- CN114736546A CN114736546A CN202210281702.6A CN202210281702A CN114736546A CN 114736546 A CN114736546 A CN 114736546A CN 202210281702 A CN202210281702 A CN 202210281702A CN 114736546 A CN114736546 A CN 114736546A
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- lithium silicate
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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
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
- C09D1/04—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates with organic additives
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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
- 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
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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
- 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
- C09D7/63—Additives non-macromolecular organic
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a lithium silicate-based inorganic resin and a synthesis method and application thereof, wherein the inorganic resin comprises the following components: 30-60 parts of lithium silicate solution, 1-5 parts of 3-urea propyl triethoxysilane, 10-30 parts of lithium hydroxide solution, 5-20 parts of gamma-aminopropyl triethoxysilane and 5-20 parts of methyl triethoxysilane. The obtained inorganic resin has good stability and weather resistance. In the synthesis method of the lithium silicate-based inorganic resin, firstly, adding a lithium silicate solution and stirring, then, adding 3-urea propyl triethoxysilane for coupling reaction, then, adding a lithium hydroxide solution to adjust the pH value, then, sequentially adding gamma-amino propyl triethoxysilane and methyl triethoxysilane for hydrolysis reaction, and cooling to obtain the lithium silicate-based inorganic resin. The inorganic resin is used for preparing the paint, does not cause wall surface efflorescence and whitening and flowering, obviously improves the aesthetic effect of the wall surface, and can also improve the weather resistance of the paint.
Description
Technical Field
The invention relates to the technical field of inorganic coating resin, in particular to lithium silicate-based inorganic resin and a synthesis method and application thereof.
Background
The lithium silicate-based inorganic paint belongs to silicate inorganic paint, and also belongs to silicate inorganic paint, and potassium silicate-based inorganic paint and sodium silicate-based inorganic paint. Sodium silicate is almost rarely used in inorganic coatings because of its poor water resistance. Potassium silicate is most widely used. However, potassium silicate has a defect in water resistance, and when an interior and exterior wall coating using the potassium silicate as a base material encounters moisture or humid air, potassium ions migrate to the surface of the coating, so that a layer of white frost is slowly generated on the wall surface, which not only affects the appearance effect, but also affects the performance of the coating due to the ion migration, so that the potassium silicate base material is mostly suitable for being used in the interior wall white coating. The lithium silicate-based inorganic coating has excellent water resistance, and can overcome the defects of sodium silicate and potassium silicate-based inorganic coatings. However, the inorganic coating prepared by the inorganic coating serving as the base material is brittle and easy to crack, and because the binding power of lithium silicate is weak, the dosage of pigment and filler is relatively small, the covering power of the coating is low, most importantly, the storage stability of the lithium silicate-based inorganic coating is poor, the product which is stable for a long time (the quality guarantee period is 12 months) is difficult to prepare, and the workability is not good enough. Thus, very few lithium silicate-based inorganic coating products are on the market.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a lithium silicate-based inorganic resin which has the advantages of high strength, high toughness and good stability, can be self-dried to form a film and can avoid the phenomenon of white frost; the second purpose of the invention is to provide a synthesis method of lithium silicate-based inorganic resin, which has simple steps and mild reaction conditions; the invention also aims to provide application of the lithium silicate-based inorganic resin, and the coating produced by using the resin as a base material has excellent coating performance.
One of the purposes of the invention is realized by adopting the following technical scheme:
the lithium silicate-based inorganic resin comprises the following raw materials in parts by weight: 30-60 parts of lithium silicate solution, 1-5 parts of 3-urea propyl triethoxysilane, 10-30 parts of lithium hydroxide solution, 5-20 parts of gamma-aminopropyl triethoxysilane and 5-20 parts of methyl triethoxysilane.
Further, the concentration of the lithium silicate solution is 20-25%, and the modulus is 4-10.
Further, the concentration of the lithium hydroxide solution is 5-15%.
Further, the lithium silicate-based inorganic resin also comprises 0.1-10 parts of organic silicon resin.
Still further, the organic silicon resin is organic silicon resin emulsion with methyl and phenyl.
Further, the lithium silicate-based inorganic resin also comprises 0.1-10 parts of silicone-acrylic emulsion.
The second purpose of the invention is realized by adopting the following technical scheme:
the synthesis method of the lithium silicate-based inorganic resin comprises the following steps:
1) adding lithium silicate solution into a constant temperature device, and stirring;
2) adding 3-urea propyl triethoxysilane, and then adding a lithium hydroxide solution to adjust the pH to 11-12.5;
3) and (3) continuously adding gamma-aminopropyl triethoxysilane, adding methyl triethoxysilane, stirring for reaction, and cooling to obtain the lithium silicate-based inorganic resin.
Further, in the step 1), controlling the temperature of a constant temperature device to be 50-60 ℃; and 3) adding methyltriethoxysilane, and stirring for reacting for 1-2 h.
And further, in the step 3), after adding the methyltriethoxysilane and stirring for reaction, adding the silicone resin and/or the silicone acrylic emulsion and stirring for reaction for 2-3 hours.
The third purpose of the invention is realized by adopting the following technical scheme:
in the application of the lithium silicate-based inorganic resin, the lithium silicate-based inorganic resin is used for preparing the coating.
Compared with the prior art, the invention has the beneficial effects that:
(1) the main component of the lithium silicate-based inorganic resin of the present invention is a lithium silicate solution in which lithium ions are dissolved in water together with CO dissolved in water2The lithium carbonate which is difficult to dissolve in water is generated by the reaction, the solubility is almost negligible at normal temperature, and 3-urea propyl triethoxy silane, gamma-amino propyl triethoxy silane and methyl triethoxy silane are utilizedOxoxysilanesTo pairThe lithium silicate is modified, so that the stability of the inorganic resin is greatly improved. 3-urea propyl triethoxysilane is used as a coupling agent, the lithium hydroxide solution has good stability and is not easy to volatilize and is used for adjusting the pH value, and the gamma-amino propyl triethoxysilane and the methyl triethoxysilane are used for initiating a hydrolysis reaction, so that the stability of the inorganic resin is improved.
(2) The lithium silicate-based inorganic resin is added with organic silicon resin and silicone-acrylate emulsion, and due to the physicochemical action of a silane coupling agent and a silane hydrolysate in the lithium silicate-based inorganic resin, the long-chain organic silicon resin or the silicone-acrylate emulsion is bonded with the inorganic resin to form longer-chain inorganic composite resin which has better toughness and adhesion to a base material. And the addition of the organic silicon resin or the silicone-acrylate emulsion forms longer-chain lithium silicate-based inorganic composite resin, so that the resin and the inorganic coating prepared from the resin have better performance stability.
(3) According to the synthesis method of the lithium silicate-based inorganic resin, firstly, a lithium silicate solution is added and stirred, then, 3-urea propyl triethoxysilane is added for coupling reaction, then, a lithium hydroxide solution is added to adjust the pH value to be 11-12.5, then, gamma-amino propyl triethoxysilane and methyl triethoxysilane are sequentially added for hydrolysis reaction, and after cooling, the lithium silicate-based inorganic resin is prepared. The silane coupling agent is added into the lithium silicate solution firstly, so that the coupling agent and the lithium silicate generate a coupling effect firstly, the stability of the lithium silicate in the change of temperature and pH value can be improved, and the lithium silicate can be bonded with a hydrolysate in time in the subsequent hydrolysis of silane to form longer-chain inorganic resin. The long-chain inorganic resin has better toughness, high strength and stable performance than single lithium silicate, so that the coating prepared from the synthesized lithium silicate-based inorganic resin has better stability than the coating prepared from the lithium silicate, and the product stability of the lithium silicate-based series inorganic coating is greatly improved.
The pH value is adjusted by adopting the lithium hydroxide solution, and the lithium hydroxide solution is not easy to volatilize, so that the phenomenon of alkali return caused by the fact that potassium ions and sodium ions are easily introduced by adopting potassium hydroxide and sodium hydroxide can be avoided.
(4) The lithium silicate-based inorganic resin is used for preparing the coating, and lithium ions are stable and cannot migrate from the interior of the coating to the surface of the coating along with water. Therefore, the defects of wall surface efflorescence, blushing and the like caused by the precipitation of potassium ions of most of the prior potassium silicate inorganic coatings are fundamentally avoided, the aesthetic effect of the wall surface is obviously improved, in addition, the lithium silicate is modified by utilizing 3-urea propyl triethoxysilane, gamma-amino propyl triethoxysilane and methyl triethoxysilane, so that the stability of the coating is greatly enhanced, the weather resistance of the coating is improved, and the inorganic coating has excellent self-cleaning effect and stain resistance, thereby having great application prospect in practical application.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, any combination between the embodiments or technical features described below may form a new embodiment.
The formulations of the lithium silicate-based inorganic resins of examples 1 to 5 are shown in Table 1.
TABLE 1 lithium silicate-based inorganic resin formulations of examples 1 to 5 (parts by mass)
The organic silicon resin is an organic silicon resin emulsion with methyl and phenyl, wherein the manufacturer is Wake, and the model is 50E.
The method for synthesizing the lithium silicate-based inorganic resin of embodiments 1 to 2 includes the steps of:
1) adding a lithium silicate solution into a constant temperature device, controlling the temperature to be 50-60 ℃, and stirring;
2) adding 3-urea propyl triethoxysilane, and then adding a lithium hydroxide solution to adjust the pH to 11-12.5;
3) and continuously adding gamma-aminopropyl triethoxysilane, adding methyl triethoxysilane, stirring for reacting for 2h, and cooling to obtain the lithium silicate-based inorganic resin.
The method for synthesizing the lithium silicate-based inorganic resin of embodiments 3 to 4 includes the steps of:
1) adding a lithium silicate solution into a constant temperature device, controlling the temperature to be 50-60 ℃, and stirring;
2) adding 3-urea propyl triethoxysilane, and then adding a lithium hydroxide solution to adjust the pH to 11-12.5;
3) continuously adding gamma-aminopropyl triethoxysilane, adding methyl triethoxysilane, stirring and reacting for 2 h;
4) and adding silicon resin and/or silicone acrylic emulsion, stirring for reaction for 3 hours, and cooling to obtain the lithium silicate-based inorganic resin.
Comparative example 1
Comparative example 1 differs from example 5 in that: comparative example 1 the lithium silicate solution was replaced with a potassium silicate solution. The remaining components and the synthesis method were the same as in example 5.
Comparative example 2
Comparative example 2 differs from example 5 in that: comparative example 2 the lithium hydroxide solution was replaced with ammonia water, and the remaining components and the synthesis method were the same as in example 5.
Comparative example 3
Comparative example 3 differs from example 5 in that: comparative example 3 the lithium hydroxide solution was replaced with a potassium hydroxide solution, and the remaining components and the synthesis method were the same as in example 5.
Comparative example 4
Comparative example 4 differs from example 5 in that: the synthesis of comparative example 4, which was hydrolyzed and then coupled, included the following steps:
1) adding a lithium silicate solution into a constant temperature device, controlling the temperature to be 50-60 ℃, and stirring;
2) adding gamma-aminopropyltriethoxysilane and methyltriethoxysilane, stirring and reacting for 2 h; in this comparative example 4, the resin had gelled and solidified at the time of step 2), so that the subsequent coupling step could not be performed. I.e., hydrolysis followed by coupling, does not result in a coating material in a fluid state.
Performance testing
20 parts of the inorganic resin of examples 1 to 5 and comparative examples 1 to 3 were added with 30 parts of deionized water, 0.1 part of a dispersant, 0.32 part of a wetting agent, 5 parts of diatomaceous earth, 10 parts of an acrylic acid solution, 0.5 part of a film-forming aid and 0.5 part of a leveling agent to prepare a coating, and the coating was subjected to performance tests, the results of which are shown in table 2. The coatings of examples 1 to 5 were then allowed to stand at room temperature (20 to 30 ℃) for 3 months, 6 months, 8 months, 12 months and 18 months, respectively, and the presence of caking, agglomeration and molding of the coatings in the container was observed, and the results are shown in Table 3.
TABLE 2 Performance data testing of the coatings of examples 1-5 and comparative examples 1-3
TABLE 3 cases of the coatings of examples 1 to 5 after a long period of standing
As shown in Table 2, comparative example 1 replaces the lithium silicate solution with a potassium silicate solution, which reacts with CO2 dissolved in water to form potassium carbonate, which has high solubility and thus migrates to the surface of the paint along with water, so that comparative example 1 has failed in water resistance. Comparative example 2 lithium hydroxide was replaced with ammonia, which was easily volatilized and was not good in heat resistance, and the coating was delaminated after volatilization. Comparative example 3 the lithium hydroxide solution was substituted for potassium hydroxide, and potassium ions were introduced, which were easily dissolved in water, resulting in poor water resistance of the coating. Comparative example 4, which is hydrolyzed before coupling, affects the stability and heat resistance of the coating. Therefore, the coatings using the inorganic resins of examples 1 to 5 as raw materials all have good weather resistance and stability, and meet the standards of the coatings.
As shown in Table 3, examples 1 and 2 showed the agglomeration phenomenon after 12 months of storage because no silicone resin or silicone-acrylate emulsion was added, while examples 3 and 4 each added only one of silicone resin and silicone-acrylate emulsion and were stable for only 12 months of storage. Example 5 is stable for 18 months due to the addition of the silicone resin and the silicone-acrylate emulsion, which shows that the silicone resin and the silicone-acrylate emulsion can effectively improve the stability of the coating.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (10)
1. The lithium silicate-based inorganic resin is characterized by comprising the following raw materials in parts by weight: 30-60 parts of lithium silicate solution, 1-5 parts of 3-urea propyl triethoxysilane, 10-30 parts of lithium hydroxide solution, 5-20 parts of gamma-aminopropyl triethoxysilane and 5-20 parts of methyl triethoxysilane.
2. The lithium silicate-based inorganic resin according to claim 1, wherein the concentration of the lithium silicate solution is 20 to 25%, and the modulus is 4 to 10.
3. The lithium silicate-based inorganic resin according to claim 1, wherein the concentration of the lithium hydroxide solution is 5 to 15%.
4. The lithium silicate-based inorganic resin according to claim 1, further comprising 0.1 to 10 parts of a silicone resin.
5. The lithium silicate-based inorganic resin according to claim 4, wherein the silicone resin is a silicone resin emulsion having methyl groups and phenyl groups.
6. The lithium silicate-based inorganic resin according to claim 1, further comprising 0.1 to 10 parts of silicone-acrylic emulsion.
7. The method for synthesizing a lithium silicate-based inorganic resin according to any one of claims 1 to 6, comprising the steps of:
1) adding lithium silicate solution into a constant temperature device, and stirring;
2) adding 3-urea propyl triethoxysilane, and then adding a lithium hydroxide solution to adjust the pH to 11-12.5;
3) and (3) continuously adding gamma-aminopropyl triethoxysilane, adding methyl triethoxysilane, stirring for reaction, and cooling to obtain the lithium silicate-based inorganic resin.
8. The method for synthesizing lithium silicate-based inorganic resin according to claim 7, wherein in the step 1), the temperature is controlled to be 50 to 60 ℃ by a thermostatic device; and 3) adding methyltriethoxysilane, and stirring for reacting for 1-2 h.
9. The method for synthesizing lithium silicate-based inorganic resin according to claim 7, wherein in the step 3), after the methyl triethoxysilane is added and stirred for reaction, the silicone resin and/or the silicone acrylic emulsion is added and stirred for reaction for 2-3 hours.
10. Use of the lithium silicate-based inorganic resin according to any one of claims 1 to 6, wherein the lithium silicate-based inorganic resin is used for preparing a coating material.
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| CN202210281702.6A CN114736546A (en) | 2022-03-21 | 2022-03-21 | Lithium silicate-based inorganic resin and synthesis method and application thereof |
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| CN202210281702.6A CN114736546A (en) | 2022-03-21 | 2022-03-21 | Lithium silicate-based inorganic resin and synthesis method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115895307A (en) * | 2022-12-12 | 2023-04-04 | 成都迪泰化工有限公司 | Sand-wall-shaped pure-color-texture natural stone coating and preparation method thereof |
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- 2022-03-21 CN CN202210281702.6A patent/CN114736546A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115895307A (en) * | 2022-12-12 | 2023-04-04 | 成都迪泰化工有限公司 | Sand-wall-shaped pure-color-texture natural stone coating and preparation method thereof |
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Address after: 528458 Longtang Management Zone, Wuguishan Town, Zhongshan City, Guangdong Province Applicant after: ZHONGSHAN HUASHAN HI-TECH CERAMIC MATERIAL CO.,LTD. Applicant after: Zhongshan Baoxin Coating Technology Co.,Ltd. Address before: 528400 card 1, office building a, plant a, No. 1, Futian Third Road, Gangkou Town, Zhongshan City, Guangdong Province Applicant before: Zhongshan Baoxin Coating Technology Co.,Ltd. Applicant before: ZHONGSHAN HUASHAN HI-TECH CERAMIC MATERIAL CO.,LTD. |