Storage-stable, fast-curing dealcoholized silicone sealant and method of making same
By preparing cyclodextrin metal framework materials and combining them with alkoxy-terminated 107 adhesive and other components, the problems of slow curing speed and poor storage stability of de-alcoholized silicone sealants were solved, achieving rapid curing and high stability, making them suitable for the construction and industrial fields.
Patent Information
- Application Number
- CN202411646444.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-18
- Publication Date
- 2025-12-16
- Estimated Expiration
- 2044-11-18
AI Technical Summary
The slow curing speed and poor storage stability of alcohol-based silicone sealants limit their further application.
Cyclodextrin was used to prepare cyclodextrin metal framework materials, which were then combined with alkoxy-terminated 107 adhesive, dimethyl silicone oil, inorganic fillers, and other components to prepare de-alcoholized silicone sealant through vacuum dehydration blending and mixing reaction. The component ratio and process conditions were optimized.
It significantly improves the storage stability and deep curing speed of de-alcoholized silicone sealants, making them suitable for industrial production.
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Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the technical field of sealant, and particularly relates to a storage-stable and fast-curing dealcoholized silicone sealant and a preparation method thereof. BACKGROUND
[0002] Silicone sealant is widely used in the fields of building and industry due to its good weather resistance and high and low temperature resistance. The dealcoholized silicone sealant is more in demand in recent years because it releases alcohol small molecules in the curing process, has no irritating odor, is green and environmentally friendly, and has no corrosivity to metal substrates, and has wide adhesion to substrates.
[0003] However, the dealcoholized silicone sealant has the shortcomings of slow curing speed and obvious decay of curing performance in the storage process, and poor storage stability, which restricts its further promotion. Therefore, it is necessary to prepare a storage-stable and fast-curing dealcoholized silicone sealant. SUMMARY
[0004] Based on this, the purpose of the present application is to provide a storage-stable and fast-curing dealcoholized silicone sealant.
[0005] The technical solutions for achieving the above-mentioned purposes include the following.
[0006] On the one hand, the present application provides a dealcoholized silicone sealant, which is prepared from raw materials including the following components by mass fraction:
[0007]
[0008] The preparation method of the cyclodextrin metal framework material includes the following steps:
[0009] (1) filter the aqueous solution containing cyclodextrin and potassium hydroxide into methanol, and stand still at 40-60 DEG C for 4-8 hours;
[0010] (2) add cetyltrimethylammonium bromide to the mixed solution obtained in step (1), stir uniformly, and stand still at 20-30 DEG C for 8-24 hours to obtain the cyclodextrin metal framework material.
[0011] On the other hand, the present application provides a preparation method of the dealcoholized silicone sealant, which includes the following steps:
[0012] The alkoxy-terminated 107 glue, dimethyl silicone oil, cyclodextrin metal framework material and inorganic filler are dehydrated and blended under the condition of temperature of 90-130 DEG C, vacuum degree of-0.08-0.099 MPa for 60-180 min, and then cooled to 40-50 DEG C, and the crosslinking agent, coupling agent and catalyst are added and mixed under the condition of vacuum degree of-0.08-0.099 MPa and stirring speed of 100-800 rpm for 40-120 min, to obtain the dealcoholized silicone sealant.
[0013] The present application has the following beneficial effects:
[0014] The present application prepares cyclodextrin into cyclodextrin metal framework material, and then prepares dealcoholized silicone sealant by combining the cyclodextrin metal framework material with alkoxy-terminated 107 glue and other components, which can significantly improve the storage stability of the dealcoholized silicone sealant, and the cyclodextrin metal framework material has strong affinity to water, which can improve the permeation rate of water vapor in the glue, thereby significantly improving the deep curing speed of the dealcoholized silicone sealant. The dealcoholized silicone sealant of the present application has excellent storage stability and deep curing speed under the combination of various components.
[0015] By optimizing the specific selection and ratio of each preparation raw material, the storage stability and deep curing speed of the obtained alcohol type silicone sealant are further improved.
[0016] The preparation method of the cyclodextrin metal framework material and the dealcoholized silicone sealant of the present application is simple, which is beneficial to industrial production. DETAILED DESCRIPTION
[0017] In order to facilitate the understanding of the present application, the present application will be described more fully below. The present application can be realized in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present application more thorough and comprehensive.
[0018] The experimental methods in the following examples without specific conditions are usually carried out according to the conventional conditions or according to the conditions suggested by the manufacturers. The various common chemical reagents used in the examples are all commercially available products.
[0019] Unless otherwise defined, all technical and scientific terms used in the present application have the same meaning as commonly understood by one of ordinary skill in the art to which the present application belongs. The terms used in the specification of the present application are only for the purpose of describing the specific embodiments and are not used to limit the present application. The term "and / or" used in the present application includes any and all combinations of one or more related listed items.
[0020] Further, as used herein, the term "or" is the inclusive, not the exclusive, "or", and is equivalent to the term "and / or", unless the context clearly dictates otherwise. The term "based on" is not exclusive, and allows for other factors to be based on, unless the context clearly dictates otherwise. Further, throughout the specification, the meaning of "a", "an", and "the" include plural references. The meaning of "in" includes "in" and "on".
[0021] In some embodiments thereof relates to a dealcoholized silicone sealant, prepared from raw materials comprising the following components, in parts by mass:
[0022]
[0023] In some preferred embodiments thereof, the dealcoholized silicone sealant is prepared from raw materials comprising the following components, in parts by mass:
[0024]
[0025]
[0026] In some preferred embodiments thereof, the dealcoholized silicone sealant is prepared from raw materials comprising the following components, in parts by mass:
[0027]
[0028] In some preferred embodiments thereof, the method for preparing the cyclodextrin metal framework material comprises the following steps:
[0029] (1) filtering an aqueous solution containing cyclodextrin and potassium hydroxide into methanol, and standing at 40-60°C for 4-8h;
[0030] (2) adding cetyltrimethylammonium bromide to the mixture obtained in step (1), stirring to uniform, and standing at 20-30°C for 8-24h, to obtain the cyclodextrin metal framework material.
[0031] In some preferred embodiments thereof, the cyclodextrin is one or more of α-cyclodextrin, β-cyclodextrin and γ-cyclodextrin.
[0032] In some preferred embodiments thereof, the cyclodextrin is γ-cyclodextrin.
[0033] In some preferred embodiments thereof, the mass ratio of the cyclodextrin, potassium hydroxide and cetyltrimethylammonium bromide is 1g: 0.2-0.5g: 0.2-0.6mg.
[0034] In some preferred embodiments, the mass ratio of the cyclodextrin, potassium hydroxide and cetyltrimethylammonium bromide is 1g: 0.3g-0.4g: 0.3mg-0.5mg.
[0035] In some preferred embodiments, the concentration of the cyclodextrin in the aqueous solution is 25g / L-40g / L.
[0036] In some preferred embodiments, the concentration of the cyclodextrin in the aqueous solution is 30g / L-35g / L.
[0037] In some preferred embodiments, the volume ratio of the methanol and water is 1: 0.8-1.2.
[0038] In some preferred embodiments, the preparation method of the cyclodextrin metal framework material comprises the following steps:
[0039] (1) dissolving the cyclodextrin and potassium hydroxide in water, and then filtering the obtained solution into a reaction kettle containing methanol, and standing at 40℃-60℃ for 4h-8h;
[0040] (2) adding the cetyltrimethylammonium bromide to the mixed solution obtained in step (1), stirring uniformly, standing at 20℃-30℃ for 8h-24h, filtering, washing, and drying, to obtain the cyclodextrin metal framework material;
[0041] In some preferred embodiments, in step (1), standing at 45℃-55℃ for 4h-6h.
[0042] In some preferred embodiments, in step (2), standing at 25℃-30℃ for 12h-16h.
[0043] In some preferred embodiments, the drying is drying under vacuum at 40℃-60℃.
[0044] In some preferred embodiments, the alkoxy-terminated 107 glue is at least one of methyl-dimethoxy-terminated 107 glue, methyl-diethoxy-terminated 107 glue, vinyl-dimethoxy-terminated 107 glue, vinyl-diethoxy-terminated 107 glue, trimethoxy-terminated 107 glue and triethoxy-terminated 107 glue.
[0045] In some preferred embodiments, the viscosity of the alkoxy-terminated 107 glue at 25℃ is 10000mPa·s-100000mPa·s.
[0046] In some preferred embodiments, the viscosity of the alkoxy-terminated 107 glue at 25℃ is 15000mPa·s-25000mPa·s.
[0047] In some preferred embodiments, the dimethicone has a viscosity of 100 mPa s to 500 mPa s at 25℃.
[0048] In some preferred embodiments, the dimethicone has a viscosity of 300 mPa s to 400 mPa s at 25℃.
[0049] In some preferred embodiments, the inorganic filler is at least one of nano active calcium carbonate, light calcium carbonate and heavy calcium carbonate.
[0050] In some preferred embodiments, the crosslinking agent is at least one of methyltrimethoxysilane, methyltriethoxysilane, propyltrimethoxysilane, octyltrimethoxysilane and phenyltrimethoxysilane.
[0051] In some preferred embodiments, the coupling agent is at least one of γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidoxypropyltrimethoxysilane, γ-mercaptopropyltrimethoxysilane and 3-isocyanatopropyltrimethoxysilane.
[0052] In some preferred embodiments, the titanate catalyst is at least one of tetraisopropyl titanate, tetrabutyl titanate, diisopropyl titanate bis(acetoacetate), dibutoxy bis(acetoacetate) titanate and diisobutyl titanate bis(acetoacetate).
[0053] In some embodiments, the preparation method of the dealcoholized silicone sealant is disclosed, comprising the following steps:
[0054] The alkoxyl-terminated 107 glue, dimethicone, cyclodextrin metal framework material and inorganic filler are dehydrated and blended at a temperature of 90℃ to 130℃ and a vacuum degree of -0.08 MPa to -0.099 MPa for 60 min to 180 min, and then cooled to 40℃ to 50℃, and the crosslinking agent, coupling agent and catalyst are added and mixed and reacted at a vacuum degree of -0.08 to -0.099 MPa and a stirring speed of 100 rpm to 800 rpm for 40 min to 120 min, to obtain the dealcoholized silicone sealant.
[0055] The application will be further described in detail in combination with specific embodiments.
[0056] In the following examples, "parts" refer to weight parts unless otherwise specified.
[0057] In the following examples, the viscosity refers to the viscosity tested at 25℃ unless otherwise specified.
[0058] Example 1
[0059] Dissolve 162 g of γ-cyclodextrin and 56 g of potassium hydroxide in 5.0 L of water, and then filter the solution through an organic filter membrane into a reaction kettle containing 4.5 L of methanol. After standing and diffusing at 50°C for 5 h, add 66.5 mg of cetyltrimethylammonium bromide, and after stirring uniformly, stand at 25°C for 12 h. Filter the above solution, and after washing the obtained crystals twice with 1.5 L of methanol, dry them under vacuum at 50°C to obtain a cyclodextrin metal-organic framework material (γ-CD-MOF).
[0060] Dehydrate and blend 100 parts of a 107 adhesive terminated with dimethoxymethyl groups having a viscosity of 20,000 mPa·s, 40 parts of dimethyl silicone oil having a viscosity of 350 mPa·s, 80 parts of γ-CD-MOF, and 160 parts of nano active calcium carbonate under the conditions of a temperature of 110°C and a vacuum degree of -0.098 MPa for 120 min, and after fully cooling to 45°C, add 0.8 parts of methyltrimethoxysilane, 0.5 parts of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, and 4 parts of titanium diisopropyl bis(acetoacetate) ethylate, and mix and react under the conditions of a vacuum degree of -0.098 MPa and a stirring speed of 300 rpm for 80 min to obtain a storage-stable fast-curing dealcoholized silicone sealant composition.
[0061] Example 2
[0062] Dissolve 100 g of α-cyclodextrin and 35 g of potassium hydroxide in 3.0 L of water, and then filter the solution through an organic filter membrane into a reaction kettle containing 3.0 L of methanol. After standing and diffusing at 60°C for 4 h, add 40 mg of cetyltrimethylammonium bromide, and after stirring uniformly, stand at 30°C for 18 h. Filter the above solution, and after washing the obtained crystals twice with 1.0 L of methanol, dry them under vacuum at 60°C to obtain a cyclodextrin metal-organic framework material (α-CD-MOF).
[0063] Dehydrate and blend 100 parts of a 107 adhesive terminated with diethoxy groups having a viscosity of 50,000 mPa·s, 20 parts of dimethyl silicone oil having a viscosity of 500 mPa·s, 50 parts of α-CD-MOF, and 100 parts of light calcium carbonate under the conditions of a temperature of 130°C and a vacuum degree of -0.090 MPa for 60 min, and after fully cooling to 50°C, add 0.5 parts of methyltriethoxysilane, 1.0 parts of γ-glycidoxypropyltrimethoxysilane, and 8 parts of dibutoxybis(acetoacetate) titanium ester, and mix and react under the conditions of a vacuum degree of -0.085 MPa and a stirring speed of 100 rpm for 120 min to obtain a storage-stable fast-curing dealcoholized silicone sealant composition.
[0064] Example 3
[0065] 200 g of β-cyclodextrin and 70 g of potassium hydroxide were dissolved in 6.0 L of water, and the solution was filtered through an organic filter membrane into a reaction kettle containing 5.0 L of methanol. After standing and diffusing at 40℃ for 8 h, 85 mg of cetyltrimethylammonium bromide was added, and after stirring to homogeneity, the solution was left to stand at 25℃ for 24 h. The resulting crystals were filtered, washed twice with 2.0 L of methanol, and dried at 40℃ under vacuum to obtain a cyclodextrin metal-organic framework material (β-CD-MOF).
[0066] 100 parts of end-trimethoxyl-terminated 107 glue with a viscosity of 100000 mPa·s, 50 parts of dimethyl silicone oil with a viscosity of 100 mPa·s, 30 parts of β-CD-MOF, 200 parts of heavy calcium carbonate were dehydrated and blended at a temperature of 90℃ and a vacuum degree of -0.080 MPa for 180 min. After being cooled to 40℃, 1.5 parts of propyltrimethoxysilane, 0.2 parts of γ-aminopropyltrimethoxysilane, and 2 parts of titanium diisobutoxide bis(acetylacetate) were added. The mixture was mixed and reacted at a vacuum degree of -0.095 MPa and a stirring speed of 800 rpm for 40 min to obtain a storage-stable fast-curing dealcoholized silicone sealant composition.
[0067] Example 4
[0068] The difference between this embodiment and Example 1 is that α-cyclodextrin is used instead of γ-cyclodextrin. The other raw materials and reaction conditions for preparing the cyclodextrin metal-organic framework material and the dealcoholized silicone sealant composition are the same as those of Example 1.
[0069] 162 g of α-cyclodextrin and 56 g of potassium hydroxide were dissolved in 5.0 L of water, and the solution was filtered through an organic filter membrane into a reaction kettle containing 4.5 L of methanol. After standing and diffusing at 50℃ for 5 h, 66.5 mg of cetyltrimethylammonium bromide was added, and after stirring to homogeneity, the solution was left to stand at 25℃ for 12 h. The resulting crystals were filtered, washed twice with 1.5 L of methanol, and dried at 50℃ under vacuum to obtain a cyclodextrin metal-organic framework material (α-CD-MOF).
[0070] 100 parts of methyl-terminated dimethoxyl terminated 107 glue with a viscosity of 20000 mPa·s, 40 parts of dimethyl silicone oil with a viscosity of 350 mPa·s, 80 parts of α-CD-MOF, and 160 parts of nano active calcium carbonate are dehydrated and blended under the condition of a temperature of 110°C and a vacuum degree of -0.098 MPa for 120 min. After being fully cooled to 45°C, 0.8 parts of methyl trimethoxysilane, 0.5 parts of N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane, and 4 parts of titanium diisopropyl bis(acetoacetate) ethyl ester are added. Mixing reaction is carried out under the condition of a vacuum degree of -0.098 MPa and a stirring speed of 300 rpm for 80 min. A storage-stable fast-curing dealcoholized silicone sealant composition is obtained.
[0071] Example 5
[0072] The difference between this example and Example 1 is that β-cyclodextrin is used instead of γ-cyclodextrin. The other preparation raw materials and reaction conditions of the cyclodextrin metal framework material and the dealcoholized silicone sealant composition are the same as those of Example 1.
[0073] 162 g of β-cyclodextrin and 56 g of potassium hydroxide are dissolved in 5.0 L of water. Then, the solution is filtered through an organic filter membrane into a reaction kettle containing 4.5 L of methanol. After being left to diffuse at 50°C for 5 h, 66.5 mg of cetyltrimethylammonium bromide is added. After being stirred uniformly, the solution is left to stand at 25°C for 12 h. The obtained crystals are filtered. After being washed twice with 1.5 L of methanol, the crystals are dried under vacuum at 50°C. A cyclodextrin metal framework material (β-CD-MOF) is obtained.
[0074] 100 parts of methyl-terminated dimethoxyl terminated 107 glue with a viscosity of 20000 mPa·s, 40 parts of dimethyl silicone oil with a viscosity of 350 mPa·s, 80 parts of β-CD-MOF, and 160 parts of nano active calcium carbonate are dehydrated and blended under the condition of a temperature of 110°C and a vacuum degree of -0.098 MPa for 120 min. After being fully cooled to 45°C, 0.8 parts of methyl trimethoxysilane, 0.5 parts of N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane, and 4 parts of titanium diisopropyl bis(acetoacetate) ethyl ester are added. Mixing reaction is carried out under the condition of a vacuum degree of -0.098 MPa and a stirring speed of 300 rpm for 80 min. A storage-stable fast-curing dealcoholized silicone sealant composition is obtained.
[0075] Comparative Example 1
[0076] The difference between this comparative example and Example 1 is that no cyclodextrin metal framework material is added to the dealcoholized silicone sealant composition. The other preparation raw materials and reaction conditions of the dealcoholized silicone sealant composition are the same as those of Example 1.
[0077] 100 parts of methyl terminated dimethoxy terminated 107 silicone with viscosity of 20000 mPa·s, 40 parts of dimethyl silicone oil with viscosity of 350 mPa·s, 160 parts of nano active calcium carbonate were dehydrated and blended under the condition of temperature of 110°C and vacuum degree of -0.098 MPa for 120 min, and then fully cooled to 45°C, 0.8 parts of methyl trimethoxysilane, 0.5 parts of N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane and 4 parts of titanium diisopropyl bis(acetoacetate) ethyl ester were added, and mixed and reacted under the condition of vacuum degree of -0.098 MPa and stirring speed of 300 rpm for 80 min, to obtain the dealcoholized silicone sealant composition.
[0078] Comparative Example 2
[0079] The difference between the present comparative example and Example 1 is that γ-cyclodextrin is used to replace γ-CD-MOF, and other raw materials and reaction conditions of the dealcoholized silicone sealant composition are the same as those of Example 1.
[0080] 100 parts of methyl terminated dimethoxy terminated 107 silicone with viscosity of 20000 mPa·s, 40 parts of dimethyl silicone oil with viscosity of 350 mPa·s, 80 parts of γ-cyclodextrin, 160 parts of nano active calcium carbonate were dehydrated and blended under the condition of temperature of 110°C and vacuum degree of -0.098 MPa for 120 min, and then fully cooled to 45°C, 0.8 parts of methyl trimethoxysilane, 0.5 parts of N-(β-aminoethyl)-γ-aminopropyl trimethoxysilane and 4 parts of titanium diisopropyl bis(acetoacetate) ethyl ester were added, and mixed and reacted under the condition of vacuum degree of -0.098 MPa and stirring speed of 300 rpm for 80 min, to obtain the dealcoholized silicone sealant composition.
[0081] The dealcoholized silicone sealant compositions prepared in Examples 1-5 and Comparative Examples 1-2 were tested for the following properties:
[0082] 1. Surface dry time: detected according to B method of GB / T 13477.5-2002 “Test methods for building sealants Part 5: Determination of surface dry time”.
[0083] 2. 24h curing depth (mm) detection: two square glass pieces with side length of 50 mm were taken, the surfaces were washed with ethanol and dried, then a glue lump was punched on one of the glass pieces, and the other glass piece was pressed on the glue lump to make the two glass pieces parallel, and the distance between the two glass pieces was controlled to be 6 mm. The glue material overflowing from the edges of the two parallel glass pieces was scraped off with a scraper, and the surface of the glue material was ensured to be flat. After the test piece was cured in an environment of 23°C and 50% RH for 24 h, the glue material was cut along the parallel surface. After removing the uncured glue material, the thickness of the cured glue material around the edges of the test piece was measured, and the average value was taken as the 24h curing depth value.
[0084] The test results are shown in Table 1: from Comparative Example 1 and Example 1, it can be seen that the addition of the cyclodextrin metal framework material can significantly improve the storage stability of the dealcoholized silicone sealant and increase the deep curing speed of the dealcoholized silicone sealant.
[0085] From Comparative Example 2 and the comparison of Comparative Example 1 and Example 1, it can be seen that cyclodextrin can also improve the storage stability and increase the deep curing speed of the dealcoholized silicone sealant to a certain extent, but its effect is far inferior to that of the cyclodextrin metal framework material of the present application, and the dealcoholized silicone sealant added with the cyclodextrin metal framework material has better storage stability and higher deep curing speed.
[0086] From the comparison of Examples 1, 4 and 5, it can be seen that the γ-CD-MOF has a better effect on improving the storage stability of the dealcoholized silicone sealant than the β-CD-MOF and the α-CD-MOF.
[0087] Table 1
[0088]
[0089]
[0090] The above examples only express several embodiments of the present application, and the description is more specific and detailed, but it cannot be understood as a limitation on the scope of the patent. It should be noted that for ordinary skilled persons in the art, several modifications and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the present application patent should be subject to the appended claims.
Claims
1. A de-alcoholized silicone sealant, characterized in that, It is prepared from raw materials comprising the following components, in parts by weight:
2. The de-alcoholized silicone sealant according to claim 1, characterized in that, It is prepared from raw materials comprising the following components, in parts by weight:
3. The de-alcoholized silicone sealant according to claim 1 or 2, characterized in that, The preparation method of the cyclodextrin metal framework material includes the following steps: (1) Filter the aqueous solution containing cyclodextrin and potassium hydroxide into methanol and let it stand at 40℃-60℃ for 4h-8h. (2) Add hexadecyltrimethylammonium bromide to the mixture obtained in step (1), stir evenly, and let stand at 20℃-30℃ for 8h-24h to obtain the cyclodextrin metal framework material.
4. The de-alcoholized silicone sealant according to claim 3, characterized in that, The cyclodextrin is one or more of α-cyclodextrin, β-cyclodextrin, and γ-cyclodextrin.
5. The de-alcoholized silicone sealant according to claim 4, characterized in that, The cyclodextrin is γ-cyclodextrin.
6. The de-alcoholized silicone sealant according to claim 3, characterized in that, The mass ratio of the cyclodextrin, potassium hydroxide, and hexadecyltrimethylammonium bromide is 1g:0.2g-0.5g:0.2mg-0.6mg.
7. The de-alcoholized silicone sealant according to claim 6, characterized in that, The mass ratio of the cyclodextrin, potassium hydroxide, and hexadecyltrimethylammonium bromide is 1g:0.3g-0.4g:0.3mg-0.5mg.
8. The de-alcoholized silicone sealant according to claim 3, characterized in that, The concentration of the cyclodextrin in the aqueous solution is 25 g / L to 40 g / L; and / or the volume ratio of methanol to water is 1:0.8-1.
2.
9. The de-alcoholized silicone sealant according to claim 8, characterized in that, The concentration of the cyclodextrin in the aqueous solution is 30 g / L to 35 g / L.
10. The de-alcoholized silicone sealant according to claim 3, characterized in that, The preparation method of the cyclodextrin metal framework material includes the following steps: (1) Dissolve the cyclodextrin and potassium hydroxide in water, then filter the resulting solution into a reaction vessel containing methanol, and let it stand at 40℃-60℃ for 4h-8h. (2) Add the hexadecyltrimethylammonium bromide to the mixture obtained in step (1), stir evenly, let stand at 20℃-30℃ for 8h-24h, filter, wash, and dry to obtain the cyclodextrin metal framework material.
11. The de-alcoholized silicone sealant according to claim 10, characterized in that, In step (1), the mixture is left to stand at 45℃-55℃ for 4-6 hours.
12. The de-alcoholized silicone sealant according to claim 10, characterized in that, In step (2), let it stand at 25℃-30℃ for 12h-16h.
13. The de-alcoholized silicone sealant according to claim 10, characterized in that, The drying process is carried out under vacuum conditions at 40℃-60℃.
14. The de-alcoholized silicone sealant according to claim 1 or 2, characterized in that, The alkoxy-terminated 107 adhesive is at least one of methyldimethoxy-terminated 107 adhesive, methyldiethoxy-terminated 107 adhesive, vinyldimethoxy-terminated 107 adhesive, vinyldiethoxy-terminated 107 adhesive, trimethoxy-terminated 107 adhesive, and triethoxy-terminated 107 adhesive.
15. The de-alcoholized silicone sealant according to claim 14, characterized in that, The viscosity of the alkoxy-terminated 107 adhesive at 25°C is 10000 mPa·s to 100000 mPa·s.
16. The de-alcoholized silicone sealant according to claim 15, characterized in that, The viscosity of the alkoxy-terminated 107 adhesive at 25°C is 15000 mPa·s to 25000 mPa·s.
17. The de-alcoholized silicone sealant according to claim 1 or 2, characterized in that, The dimethyl silicone oil has a viscosity of 100 mPa·s to 500 mPa·s at 25°C; and / or, The inorganic filler is at least one of nano-activated calcium carbonate, light calcium carbonate, and heavy calcium carbonate; and / or, The crosslinking agent is at least one selected from methyltrimethoxysilane, methyltriethoxysilane, propyltrimethoxysilane, octyltrimethoxysilane, and phenyltrimethoxysilane; and / or, The coupling agent is at least one selected from γ-aminopropyltrimethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidyl ether oxypropyltrimethoxysilane, γ-mercaptopropyltrimethoxysilane, and 3-isocyanate propyltrimethoxysilane; and / or, The titanate catalyst is selected from at least one of tetraisopropyl titanate, tetrabutyl titanate, diisopropyl titanate (ethyl acetoacetate), dibutoxybis(ethyl acetoacetate) titanate, and diisobutyl titanate (ethyl acetoacetate).
18. The de-alcoholized silicone sealant according to claim 17, characterized in that, The viscosity of the dimethyl silicone oil at 25°C is 300 mPa·s to 400 mPa·s.
19. A method for preparing a dealcohol-type silicone sealant according to any one of claims 1-18, characterized in that, Includes the following steps: The alkoxy-terminated 107 adhesive, dimethyl silicone oil, cyclodextrin metal framework material, and inorganic filler are dehydrated and blended for 60 min to 180 min at a temperature of 90℃ to 130℃ and a vacuum degree of -0.08 MPa to -0.099 MPa. After cooling to 40℃ to 50℃, the crosslinking agent, coupling agent, and catalyst are added, and the mixture is stirred for 40 min to 120 min at a vacuum degree of -0.08 to -0.099 MPa and a stirring speed of 100 rpm to 800 rpm to obtain the de-alcoholized silicone sealant.
Citation Information
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