CN114231246A - Ketoxime-removing type transparent sealant and preparation method thereof - Google Patents
Ketoxime-removing type transparent sealant and preparation method thereof Download PDFInfo
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- CN114231246A CN114231246A CN202111651253.1A CN202111651253A CN114231246A CN 114231246 A CN114231246 A CN 114231246A CN 202111651253 A CN202111651253 A CN 202111651253A CN 114231246 A CN114231246 A CN 114231246A
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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Abstract
The invention provides a deketoxime type transparent sealant and a preparation method thereof, and relates to the technical field of silicone sealants. The ketoxime-removing type transparent sealant comprises the following raw materials in parts by weight: 1.5-17.5 parts of base material, 40-70 parts of alpha, omega-dihydroxy polydimethylsiloxane, 8-35 parts of plasticizer, 5-30 parts of filler, 1-8 parts of cross-linking agent, 1-5 parts of coupling agent, 1-5 parts of mildew preventive and 0.05-1 part of catalyst; the base material is prepared by the following method: according to the mass ratio (6-7.5): (2.5-4) heating alpha, omega-dihydroxy polydimethylsiloxane and precipitated white carbon black to 125-135 ℃, uniformly mixing in a vacuum state, and stirring at a rotating speed of 45-50 rpm to obtain the base material. The ketoxime-removing type transparent sealant has the advantage of low cost.
Description
Technical Field
The invention relates to the technical field of silicone sealants, in particular to a deketoxime type transparent sealant and a preparation method thereof.
Background
The room temperature vulcanized silicone rubber has excellent oxidation resistance, high and low temperature resistance, aging resistance, water resistance, moisture resistance and other performances, and the deketoxime type transparent sealant as one kind of room temperature vulcanized silicone rubber also has the performances. Meanwhile, because the construction is convenient and efficient, the operation is simple, the ketoxime removing type transparent sealant is widely used for sealing doors and windows of buildings and glass lighting sheds and bonding various materials such as stone, and is popular among consumers in the building industry.
At present, the transparent sealant has large demand on the market and has very strong competition. In order to reduce the cost of the sealant, a large amount of white oil is added into some products, but the service life of the sealant is greatly reduced, and the environment can be polluted due to the exudation of the white oil. In the prior art, fumed silica is usually added into the sealant as a filler to improve the strength of the sealant, and precipitated silica with almost similar reinforcing performance and much lower price is not used, because the precipitated silica has higher moisture content and quicker moisture regain, the moisture is difficult to effectively remove even if the precipitated silica is baked by an oven, and the situation that the sealant is thickened or even dried can be caused if the fumed silica is directly used. If the problem of high water content of the precipitated white carbon black can be solved, the production cost of the sealant can be greatly reduced, and the competitiveness of enterprises is improved.
Disclosure of Invention
In view of the above, there is a need to provide a ketoxime-removing type transparent sealant which has the advantage of low cost.
The ketoxime-removing type transparent sealant comprises the following raw materials in parts by weight: 1.5-17.5 parts of base material, 40-70 parts of alpha, omega-dihydroxy polydimethylsiloxane, 8-35 parts of plasticizer, 5-30 parts of filler, 1-8 parts of cross-linking agent, 1-5 parts of coupling agent, 1-5 parts of mildew preventive and 0.05-1 part of catalyst;
the base material is prepared by the following method: according to the mass ratio (6-7.5): (2.5-4) taking alpha, omega-dihydroxy polydimethylsiloxane and precipitated white carbon black, heating to 125 ℃ and 135 ℃, and uniformly mixing in a vacuum state at the stirring speed of 45-50 rpm to obtain the base material.
The deketoxime type transparent sealant is prepared by mixing precipitated white carbon black with alpha, omega-dihydroxy polydimethylsiloxane to prepare a base material in advance, the precipitated white carbon black can be dehydrated more fully by high-speed stirring, and a part of residual two-dimensional network structures in the structure can be removed at high temperature, so that the problem that the precipitated white carbon black is easy to structurize when added into the sealant due to high moisture regain is solved, the precipitated white carbon black is successfully added into the sealant, the using amount of gas phase white carbon black in the filler is reduced, the raw material cost of the sealant is greatly reduced, and the conditions of thickening and dry sealant can be avoided.
When the base material is prepared, if the stirring rotating speed is too low, the precipitated white carbon black is not sufficiently dehydrated, and if the stirring rotating speed is too high, the stirring paddle and the base material are sheared too fast, the temperature is increased sharply, and the temperature exceeds the range, so that the components in the base material are attenuated, and even the base material is structured.
In one embodiment, in the preparation method of the base material, the pressure is 0.09-0.1 MPa, and the mixing and stirring time is 140-160 min.
In one embodiment, the dosage of the base material is 3-10% of the total weight of the deketoxime type transparent sealant.
In one embodiment, the α, ω -dihydroxypolydimethylsiloxane has a viscosity of 10000 to 150000mPa.s at 25 ℃. The alpha, omega-dihydroxy polydimethylsiloxane with the viscosity range can be better compounded, so that the sealant has moderate consistency, the tensile strength and the elongation at break are further improved, the construction is more convenient, and the phenomena of flowing and drooping are not easy to occur.
In one embodiment, the plasticizer is selected from: one or more than two of simethicone and epoxidized soybean oil.
In one embodiment, the filler is selected from: one or two of fumed silica and precipitated silica. Wherein, the fumed silica needs to be baked in an oven for 10-14 h at 140-160 ℃ to ensure that the volatile component is less than 1.2%.
Preferably, the filler is fumed silica. The specific surface area of the fumed silica is usually 100-150 m2The specific surface area of the precipitated white carbon black is usually 50-100 m2And/g, two kinds of white carbon black with different specific surface areas are added into the sealant, so that gaps among particle sizes can be effectively filled, the strength of the sealant is improved, and the cost of the sealant is reduced.
In one embodiment, the cross-linking agent is selected from: one or more of vinyl tributyrinoxime silane, methyl tributyrinoxime silane and phenyl tributyrinoxime silane.
In one embodiment, the cross-linking agent is vinyl tributyrinoxime silane and methyl tributyrinoxime silane, and the mass ratio of the vinyl tributyrinoxime silane to the methyl tributyrinoxime silane is 2: (8-10). The compound cross-linking agent can improve the curing speed of the sealant, prevent the adhesive tape from breaking after the sealant is applied, and simultaneously can control the surface drying time of the sealant, thereby being more convenient for construction.
In one embodiment, the coupling agent is selected from: one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane and N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane.
In one embodiment, the coupling agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and N-beta- (aminoethyl) -gamma-aminopropyl trimethoxy silane, and the mass of the two is (0.5-1.5): 2. the compound coupling agent can ensure that the soaking and bonding effects of the sealant are better, the compound coupling agent is suitable for a humid environment, and meanwhile, the curing speed of the sealant can be improved.
In one embodiment, the catalyst is selected from: one or more than two of dibutyltin dilaurate, dibutyltin dioctoate, dibutyltin diacetate, dibutyltin dimethoxide and dibutyltin oxide.
In one embodiment, the mildew inhibitor is selected from: one or more than two of 5-chlorine-2-methyl-4-isothiazoline-3-ketone, benzyl trimethyl ammonium chloride, benzyl trimethyl ammonium bromide and phenyl trimethyl ammonium chloride.
The sealant is commonly used in high-temperature and high-humidity places such as kitchens and toilets, so that mildew can grow after long-time use, and the attractiveness is affected. The mildew preventive can improve the mildew preventive effect of the sealant, ensure the attractiveness of the sealant and be more suitable for high-temperature and high-humidity environments.
The invention also provides a preparation method of the deketoxime type transparent sealant, which comprises the steps of uniformly mixing the base material, alpha, omega-dihydroxy polydimethylsiloxane and part of the plasticizer in a vacuum state, sequentially adding the cross-linking agent, the filler, the coupling agent, the mildew preventive, the catalyst and the rest of the plasticizer, and carrying out mixing reaction to obtain the deketoxime type transparent sealant.
In one embodiment, the preparation method comprises the following steps:
s1, adding a base material, alpha, omega-dihydroxy polydimethylsiloxane and a part of plasticizer into a reaction kettle, and stirring for 6-10 min under the pressure of 0.03-0.04 MPa, wherein the stirring speed is 15-25 r/min;
s2, adding a cross-linking agent, stirring at a rotation speed of 20-30 r/min and a temperature below 50 ℃ under a pressure of-0.01-0.095 MPa for 18-22 min;
s3, adding a filler, stirring at a speed of 10-45 r/min and a temperature of below 60 ℃ under a pressure of-0.01-0.095 MPa for 26-30 min;
s4, adding a coupling agent and a mildew preventive, stirring at a rotation speed of 20-30 r/min and a temperature of below 60 ℃ for 13-17 min under the pressure of-0.01-0.095 MPa;
and S5, adding a catalyst and the rest of plasticizer, stirring at a speed of 20-30 r/min under the pressure of-0.01-0.095 MPa and at a temperature of below 60 ℃, stirring for 23-27 min, and completing the reaction to obtain the deketoxime type transparent sealant.
In one embodiment, the plasticizer used in S1 is 55% to 65% of the total weight of the plasticizer.
Compared with the prior art, the invention has the following beneficial effects:
according to the deketoxime type transparent sealant disclosed by the invention, the precipitated white carbon black and the alpha, omega-dihydroxy polydimethylsiloxane are mixed to prepare the base material in advance, so that the problem that the precipitated white carbon black is easy to structurize when being added into the sealant due to high moisture regain is solved, the precipitated white carbon black is successfully added into the sealant, the using amount of gas phase white carbon black in the filler is reduced, the raw material cost of the sealant is greatly reduced, and the situations of thickening and drying the sealant can be avoided. The preparation method of the ketoxime removing type transparent sealant is simple, and the prepared ketoxime removing type transparent sealant has the advantages of low cost, good mildew-proof effect and the like.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the preferred embodiments. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The starting materials in the following examples and comparative examples were all commercially available unless otherwise specified. The viscosity of the α, ω -dihydroxypolydimethylsiloxane at 25 ℃ was 80000 mPas. And baking the fumed silica in an oven at 150 ℃ for 12h for later use.
Example 1
The deketoxime type transparent sealant is prepared by the following steps:
(1) mixing the components in a weight ratio of 6.5: 3.5 of alpha, omega-dihydroxy polydimethylsiloxane and precipitated white carbon black are placed in a kneader, the temperature is increased to 125-135 ℃, the pressure is 0.095MPa, the mixture is stirred for 150min at 50rpm, and the mixture is cooled to room temperature to prepare the base material.
(2) Weighing a base material accounting for 6 percent of the total weight of the sealant, adding the base material, 62 parts of alpha, omega-dihydroxy polydimethylsiloxane and 15 parts of simethicone into a reaction kettle with a stirrer, stirring for 8min under 0.03-0.04 MPa, and rotating at the revolution and rotation speed of the stirrer of 15-25 r/min.
(3) Adding 4 parts of a mixture of 2: 9, stirring the vinyl tributyrinoxime silane and methyl tributyrinoxime silane compounded cross-linking agent for 20min under-0.01-0.095 MPa, rotating at the revolution and rotation speeds of 20-30 r/min by using a stirrer, and introducing cooling water into a jacket of a reaction kettle to control the temperature of the sizing agent to be below 50 ℃.
(4) Adding 24 parts of fumed silica, stirring for 8min under-0.01-0.095 MPa, rotating at revolution and rotation speeds of 10-15 r/min by using a stirrer, lifting a stirring paddle, cleaning the unstirred fumed silica by using a quick scraping rod, continuously stirring for 20min under-0.01-0.095 MPa, rotating at revolution and rotation speeds of 35-45 r/min by using the stirrer, and simultaneously controlling the temperature of the sizing material to be below 60 ℃.
(5) Adding 3 parts of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane and 1 part of 5-chloro-2-methyl-4-isothiazolin-3-one, stirring for 25min under the pressure of-0.01-0.095 MPa, and controlling the revolution and rotation speeds of a stirrer to be 20-30 r/min and the temperature of the rubber material to be below 60 ℃.
(6) Adding 0.5 part of dibutyltin dilaurate and 10 parts of dimethyl silicone oil, stirring for 25min under-0.01-0.095 MPa, and controlling the revolution and rotation speed of a stirrer to be 20-30 r/min and the temperature of the rubber material to be below 60 ℃.
(7) Stopping stirring, introducing nitrogen into the reaction kettle, and removing vacuum to obtain the product.
Example 2
The deketoxime type transparent sealant is prepared by the following steps:
(1) mixing the components in a weight ratio of 6.5: 3.5 of alpha, omega-dihydroxy polydimethylsiloxane and precipitated white carbon black are placed in a kneader, the temperature is increased to 125-135 ℃, the pressure is 0.095MPa, the mixture is stirred for 150min at 50rpm, and the mixture is cooled to room temperature to prepare the base material.
(2) Weighing a base material accounting for 10 percent of the total weight of the sealant, adding the base material, 60 parts of alpha, omega-dihydroxy polydimethylsiloxane and 15 parts of simethicone into a reaction kettle with a stirrer, stirring for 8min under 0.03-0.04 MPa, and rotating at the revolution and rotation speed of the stirrer of 15-25 r/min.
(3) Adding 4 parts of a mixture of 2: 9, stirring the vinyl tributyrinoxime silane and methyl tributyrinoxime silane compounded cross-linking agent for 20min under-0.01-0.095 MPa, rotating at the revolution and rotation speeds of 20-30 r/min by using a stirrer, and introducing cooling water into a jacket of a reaction kettle to control the temperature of the sizing agent to be below 50 ℃.
(4) Adding 23 parts of fumed silica, stirring for 8min under-0.01-0.095 MPa, rotating at revolution and rotation speeds of 10-15 r/min by using a stirrer, lifting a stirring paddle, cleaning the unstirred fumed silica by using a quick scraping rod, continuously stirring for 20min under-0.01-0.095 MPa, rotating at revolution and rotation speeds of 35-45 r/min by using the stirrer, and simultaneously controlling the temperature of the sizing material to be below 60 ℃.
(5) Adding 3 parts of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane and 1 part of 5-chloro-2-methyl-4-isothiazolin-3-one, stirring for 25min under the pressure of-0.01-0.095 MPa, and controlling the revolution and rotation speeds of a stirrer to be 20-30 r/min and the temperature of the rubber material to be below 60 ℃.
(6) Adding 0.5 part of dibutyltin dilaurate and 10 parts of dimethyl silicone oil, stirring for 25min under-0.01-0.095 MPa, and controlling the revolution and rotation speed of a stirrer to be 20-30 r/min and the temperature of the rubber material to be below 60 ℃.
(7) Stopping stirring, introducing nitrogen into the reaction kettle, and removing vacuum to obtain the product.
Example 3
The difference between the ketoxime-removed transparent sealant and the embodiment 1 is that 4 parts of compound crosslinking agent is replaced by 4 parts of methyl tributyl ketoxime silane.
Example 4
The difference between the deketoxime type transparent sealant and the embodiment 1 is that a coupling agent is replaced by a compound coupling agent which is a composition of gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and N-beta- (aminoethyl) -gamma-aminopropyl trimethoxy silane, and the mass ratio of the two is 1: 2.
comparative example 1
A deketoxime type transparent sealant is different from that in example 1 in that no mildew preventive is added.
Comparative example 2
The deketoxime type transparent sealant is prepared by the following steps:
(1) adding 65 parts of alpha, omega-dihydroxy polydimethylsiloxane and 15 parts of simethicone into a reaction kettle with a stirrer, and stirring for 8min under 0.03-0.04 MPa, wherein the revolution and rotation speed of the stirrer is 15-25 r/min.
(2) Adding 4 parts of a mixture of 2: 9, stirring the vinyl tributyrinoxime silane and methyl tributyrinoxime silane compounded cross-linking agent for 20min under-0.01-0.095 MPa, rotating at the revolution and rotation speeds of 20-30 r/min by using a stirrer, and introducing cooling water into a jacket of a reaction kettle to control the temperature of the sizing agent to be below 50 ℃.
(3) Adding 24 parts of fumed silica, stirring for 8min under-0.01-0.095 MPa, rotating at revolution and rotation speeds of 10-15 r/min by using a stirrer, lifting a stirring paddle, cleaning the unstirred fumed silica by using a quick scraping rod, continuously stirring for 20min under-0.01-0.095 MPa, rotating at revolution and rotation speeds of 35-45 r/min by using the stirrer, and simultaneously controlling the temperature of the sizing material to be below 60 ℃.
(4) Adding 3 parts of N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane and 1 part of 5-chloro-2-methyl-4-isothiazolin-3-one, stirring for 25min under the pressure of-0.01-0.095 MPa, and controlling the revolution and rotation speeds of a stirrer to be 20-30 r/min and the temperature of the rubber material to be below 60 ℃.
(5) Adding 0.5 part of dibutyltin dilaurate and 10 parts of dimethyl silicone oil, stirring for 25min under-0.01-0.095 MPa, and controlling the revolution and rotation speed of a stirrer to be 20-30 r/min and the temperature of the rubber material to be below 60 ℃.
(6) Stopping stirring, introducing nitrogen into the reaction kettle, and removing vacuum to obtain the product.
Comparative example 3
A deketoxime type transparent sealant is different from that of comparative example 2 in that step (3):
adding 24 parts of fumed silica and 4 parts of precipitated silica, stirring for 8min under-0.01-0.095 MPa, rotating at the revolution and rotation speeds of 10-15 r/min by a stirrer, lifting a stirring paddle, cleaning the unstirred fumed silica and the precipitated silica by a quick scraping rod, continuously stirring for 20min under-0.01-0.095 MPa, rotating at the revolution and rotation speeds of 35-45 r/min by the stirrer, and simultaneously controlling the temperature of the sizing material to be below 60 ℃.
Experimental example 1
The samples prepared in the above examples and comparative examples were subjected to performance tests for elongation at break, tensile strength, open time, shore a hardness, storage stability and mildew resistance rating. The test methods and test results are as follows.
(1) Elongation at break and tensile strength were tested according to GB/T528-2009.
(2) The tack free time and the post-immersion tensile adhesion were determined according to GB/T13477-2017.
(3) Shore A hardness was tested according to GB/T531.1-2008.
(4) The mildew resistance rating is tested according to GB/T1741-2007.
(5) And (4) testing the storage stability: and (3) placing the prepared sealant sample in an air drying oven at 90 ℃ for a certain time, and testing the surface drying time, the curing condition and the appearance of the adhesive tape.
TABLE 1 sealant Performance test results
As can be seen from the table above, the ketoxime removing type transparent sealant prepared by the embodiment of the invention has a good mildew-proof effect, can be used in high-temperature and high-humidity places in kitchens and toilets, and is not easy to generate mildew so as to influence the overall attractiveness of the environment. The precipitated white carbon black is used in the formula of the embodiment, so that the production cost is greatly reduced, and the phenomena of thickening and glue drying do not occur in the use process of the sealant. Moreover, example 3, due to the use of a single crosslinker, exhibited a longer open time than the use of a compounded crosslinker strip. Example 4 because of the use of the compound coupling agent, the sealant after soaking in water is 100% cohesive failure for both aluminum and glass, indicating that the water-soaking adhesion performance of the sealant is relatively good.
The sealant of the comparative example 1 is not added with a mildew preventive, and has poor mildew preventive effect. The sealant of comparative example 2, without addition of a base material, is compared with example 1, and it can be seen that the tensile strength is lower than that of example, the elongation at break is higher than that of example, the properties such as open time and storage life are not much different, and the Shore hardness is slightly lower than that of example. In the comparative example 3, the precipitated silica is not added into the rubber material in a base material mode, so that the sealant is easy to have a structurization problem.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The deketoxime type transparent sealant is characterized by comprising the following raw materials in parts by weight: 1.5-17.5 parts of base material, 40-70 parts of alpha, omega-dihydroxy polydimethylsiloxane, 8-35 parts of plasticizer, 5-30 parts of filler, 1-8 parts of cross-linking agent, 1-5 parts of coupling agent, 1-5 parts of mildew preventive and 0.05-1 part of catalyst;
the base material is prepared by the following method: according to the mass ratio (6-7.5): (2.5-4) heating alpha, omega-dihydroxy polydimethylsiloxane and precipitated white carbon black to 125-135 ℃, uniformly mixing in a vacuum state, and stirring at a rotating speed of 45-50 rpm to obtain the base material.
2. The deketoxime type transparent sealant as claimed in claim 1, wherein the base material is prepared by mixing at a pressure of 0.09-0.1 MPa and a temperature of 125-135 ℃ for 140-160 min.
3. The transparent sealant of claim 1, wherein the α, ω -dihydroxy polydimethylsiloxane has a viscosity of 10000 to 150000mPa.s at 25 ℃.
4. The deoketiminate type transparent sealant according to claim 1 wherein said plasticizer is selected from the group consisting of: one or more than two of simethicone and epoxidized soybean oil.
5. The deoketiminate type transparent sealant according to claim 1 wherein said filler is selected from the group consisting of: one or two of fumed silica and precipitated silica.
6. The deoketiminate type transparent sealant according to claim 1, wherein said crosslinking agent is selected from the group consisting of: one or more of vinyl tributyrinoxime silane, methyl tributyrinoxime silane and phenyl tributyrinoxime silane; the coupling agent is selected from: one or more of gamma-aminopropyltriethoxysilane, gamma- (2, 3-glycidoxy) propyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane and N-beta- (aminoethyl) -gamma-aminopropyltrimethoxysilane.
7. The ketoxime-removing transparent sealant as claimed in claim 6, wherein the cross-linking agent is vinyl tributyrinoxime silane and methyl tributyrinoxime silane in a mass ratio of 2: (8-10); the coupling agent is gamma- (2, 3-epoxypropoxy) propyl trimethoxy silane and N-beta- (aminoethyl) -gamma-aminopropyl trimethoxy silane, and the mass of the coupling agent is (0.5-1.5): 2.
8. the deoketiminate type transparent sealant according to any one of claims 1 to 7, wherein the catalyst is selected from the group consisting of: one or more than two of dibutyltin dilaurate, dibutyltin dioctoate, dibutyltin diacetate, dibutyltin dimethoxide and dibutyltin oxide; the mildew preventive is selected from: one or more than two of 5-chlorine-2-methyl-4-isothiazoline-3-ketone, benzyl trimethyl ammonium chloride, benzyl trimethyl ammonium bromide and phenyl trimethyl ammonium chloride.
9. The method for preparing the deketoxime type transparent sealant as claimed in any one of claims 1 to 8, wherein the base material, the α, ω -dihydroxy polydimethylsiloxane and a part of the plasticizer are uniformly mixed under vacuum, and then the cross-linking agent, the filler, the coupling agent, the mildew preventive, the catalyst and the rest of the plasticizer are sequentially added for mixing reaction, thereby obtaining the deketoxime type transparent sealant.
10. The process for preparing a deketoxime type transparent sealant according to claim 9, which comprises the steps of:
s1, adding a base material, alpha, omega-dihydroxy polydimethylsiloxane and a part of plasticizer into a reaction kettle, and stirring for 6-10 min under the pressure of 0.03-0.04 MPa, wherein the stirring speed is 15-25 r/min;
s2, adding a cross-linking agent, stirring at a rotation speed of 20-30 r/min and a temperature below 50 ℃ under a pressure of-0.01-0.095 MPa for 18-22 min;
s3, adding a filler, stirring at a speed of 10-45 r/min and a temperature of below 60 ℃ under a pressure of-0.01-0.095 MPa for 26-30 min;
s4, adding a coupling agent and a mildew preventive, stirring at a rotation speed of 20-30 r/min and a temperature of below 60 ℃ for 13-17 min under the pressure of-0.01-0.095 MPa;
and S5, adding a catalyst and the rest of plasticizer, stirring at a speed of 20-30 r/min under the pressure of-0.01-0.095 MPa and at a temperature of below 60 ℃, stirring for 23-27 min, and completing the reaction to obtain the deketoxime type transparent sealant.
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| CN114854204A (en) * | 2022-06-29 | 2022-08-05 | 广东高士高科实业有限公司 | Room-temperature vulcanized silicone rubber and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436215A (en) * | 2013-09-05 | 2013-12-11 | 江苏天辰硅材料有限公司 | Condensed-type dual-ingredient organic silica gel for encapsulation |
| CN110272713A (en) * | 2018-03-13 | 2019-09-24 | 佛山市南海祥盛建筑材料有限公司 | Silicone sealant and its preparation method and application |
| CN111004604A (en) * | 2019-12-30 | 2020-04-14 | 广州市白云化工实业有限公司 | Organosilicon sealant and preparation method thereof |
| CN112239645A (en) * | 2020-09-07 | 2021-01-19 | 广州凌玮科技股份有限公司 | Silicone adhesive with antibacterial and mildewproof effects and preparation method thereof |
| CN112239643A (en) * | 2020-09-07 | 2021-01-19 | 广州凌玮科技股份有限公司 | Neutral transparent silicone adhesive and preparation method thereof |
| CN113150737A (en) * | 2021-02-07 | 2021-07-23 | 广东莱雅新化工科技有限公司 | Two-component organic silicon pouring sealant and preparation method thereof |
-
2021
- 2021-12-30 CN CN202111651253.1A patent/CN114231246A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103436215A (en) * | 2013-09-05 | 2013-12-11 | 江苏天辰硅材料有限公司 | Condensed-type dual-ingredient organic silica gel for encapsulation |
| CN110272713A (en) * | 2018-03-13 | 2019-09-24 | 佛山市南海祥盛建筑材料有限公司 | Silicone sealant and its preparation method and application |
| CN111004604A (en) * | 2019-12-30 | 2020-04-14 | 广州市白云化工实业有限公司 | Organosilicon sealant and preparation method thereof |
| CN112239645A (en) * | 2020-09-07 | 2021-01-19 | 广州凌玮科技股份有限公司 | Silicone adhesive with antibacterial and mildewproof effects and preparation method thereof |
| CN112239643A (en) * | 2020-09-07 | 2021-01-19 | 广州凌玮科技股份有限公司 | Neutral transparent silicone adhesive and preparation method thereof |
| CN113150737A (en) * | 2021-02-07 | 2021-07-23 | 广东莱雅新化工科技有限公司 | Two-component organic silicon pouring sealant and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘植榕 等: "《橡胶工业手册》", 30 September 1992, 化学工业出版社 * |
| 黄文润: "《液体硅橡胶》", 30 June 2009, 四川科学技术出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114854204A (en) * | 2022-06-29 | 2022-08-05 | 广东高士高科实业有限公司 | Room-temperature vulcanized silicone rubber and preparation method and application thereof |
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