CN113583624A - Preparation method of silicone sealant - Google Patents
Preparation method of silicone sealant Download PDFInfo
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- CN113583624A CN113583624A CN202111050752.5A CN202111050752A CN113583624A CN 113583624 A CN113583624 A CN 113583624A CN 202111050752 A CN202111050752 A CN 202111050752A CN 113583624 A CN113583624 A CN 113583624A
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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
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention relates to a preparation method of a silicone sealant, belonging to the technical field of silicone sealants, and comprising the following steps of firstly, weighing raw materials in parts by weight; secondly, mixing alpha, omega-dihydroxy polysiloxane, methyl silicone oil, modified silicone oil and a cross-linking agent for 1h in vacuum at the temperature of 30 ℃ under the vacuum condition, adding fumed silica, continuously mixing for 30min in vacuum, then adding a coupling agent and a catalyst, and continuously mixing for 30min in vacuum; obtaining a silicone sealant; according to the invention, the modified silicone oil is prepared from the modifier and the aminoethyl aminopropyl silicone oil, the modifier is quaternary ammonium salt containing an epoxy group, the effect of inhibiting yellowing is achieved after quaternary ammonium salt is introduced, meanwhile, the quaternary ammonium salt structure can adsorb bacteria with negative charges, and the modified silicone oil has a better sterilization and mildew-resistant effect.
Description
Technical Field
The invention belongs to the technical field of organosilicon sealants, and particularly relates to a preparation method of a silicone sealant.
Background
The silicone sealant is a paste formed by mixing polydimethylsiloxane as a main raw material, a cross-linking agent, a filler, a plasticizer, a coupling agent and a catalyst in a vacuum state, and the single-component silicone glass adhesive is similar to an ointment and can be solidified into a tough rubber solid material once contacting with moisture in the air. The silicone glass cement has the characteristics of strong bonding force, high tensile strength, weather resistance, vibration resistance, moisture resistance, odor resistance and large adaptability to cold and heat changes.
The silicone sealant is gradually decomposed and aged under long-term humid conditions, and the aged sealant frequently has quality problems of yellow appearance, color change and the like. The silicone sealant has a plurality of yellowing factors, and the neutral transparent silicone sealant has amino molecules which are easy to yellow and gradually yellow after being vulcanized for a period of time; furthermore, yellowing of silicone adhesives is strongly related to long storage periods or to reactions occurring later.
Disclosure of Invention
The invention aims to provide a preparation method of a silicone sealant.
The purpose of the invention can be realized by the following technical scheme:
the preparation method of the silicone sealant comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 55-70 parts of alpha, omega-dihydroxy polysiloxane, 7-8 parts of methyl silicone oil, 20-30 parts of modified silicone oil, 1.9-2.2 parts of cross-linking agent, 7-11 parts of fumed silica, 0.4-0.6 part of coupling agent and 0.2-0.3 part of catalyst;
secondly, mixing alpha, omega-dihydroxy polysiloxane, methyl silicone oil, modified silicone oil and a cross-linking agent for 1h in vacuum at the temperature of 30 ℃ under the vacuum condition, adding fumed silica, continuously mixing for 30min in vacuum, then adding a coupling agent and a catalyst, and continuously mixing for 30min in vacuum; a silicone sealant was obtained.
The modified silicone oil is prepared by the following steps:
mixing the aminoethyl aminopropyl silicone oil, the modifier and isopropanol, carrying out reflux reaction for 4 hours at the temperature of 85 ℃, then carrying out heat preservation for 2 hours, and then removing the isopropanol under the condition of 0.01MPa to obtain the modified silicone oil.
Further, the dosage ratio of the aminoethyl aminopropyl silicone oil to the modifier to the isopropanol is 1.2-1.5 g: 0.6 g: 10 mL.
Further, the modifier is prepared by the following steps:
step S1, preparing component A;
the reaction process is as follows:
step S11, mixing chlorobenzene, deionized water and 2- (methylthio) benzonitrile, adding sulfonyl chloride at the temperature of 0 ℃, heating to 35 ℃ after the addition, reacting for 15min, heating to 75 ℃, reacting for 40min, cooling to 0 ℃ after the reaction, precipitating a solid, performing suction filtration under reduced pressure, and recrystallizing the obtained solid with absolute ethyl alcohol to obtain an intermediate 1; wherein the dosage ratio of chlorobenzene to deionized water to the 2- (methylthio) benzonitrile to the sulfonyl chloride is 150 mL: 3.4 g: 25g of: 28g of a mixture;
step S12, mixing deionized water, the intermediate 1 and potassium hydroxide, stirring for reaction for 20min, heating to 115 ℃, dropwise adding a sodium chloroacetate aqueous solution, reacting for 8h after addition, cooling to room temperature after the reaction is finished, performing reduced pressure suction filtration, adjusting the pH value of filtrate to 1 by using concentrated hydrochloric acid, precipitating a solid, performing reduced pressure suction filtration, washing a filter cake by using deionized water, absolute ethyl alcohol and acetone in sequence, and drying to constant weight at 70 ℃ after washing is finished to obtain an intermediate 2; wherein the sodium chloroacetate aqueous solution is sodium chloroacetate and deionized water 6 g: 10 mL; the dosage ratio of the deionized water, the intermediate 1, the potassium hydroxide and the sodium chloroacetate aqueous solution is 50 mL: 8 g: 3.5 g: 10 mL;
step S13, mixing the intermediate 2, thionyl chloride and N, N-dimethylformamide, heating and refluxing for 5 hours, and evaporating the thionyl chloride after the reaction is finished to obtain a component A; wherein the dosage ratio of the intermediate 2, the thionyl chloride and the N, N-dimethylformamide is 21 g: 100 g: 2 mL.
Step S2, preparing component B;
the reaction process is as follows:
step S21, mixing magnesium powder and tetrahydrofuran, adding 3, 4-dichlorobromobenzene at the temperature of 20 ℃, heating to 45 ℃ after adding, stirring for reaction for 2 hours, then cooling to-5 ℃, adding trimethyl borate, keeping the temperature unchanged for reaction for 3 hours, adding a hydrochloric acid solution with the mass fraction of 10% of that of the tetrahydrofuran after the reaction is finished, mixing and standing for layering, extracting an organic phase with toluene, washing with water, drying and concentrating to obtain an intermediate 3; wherein the dosage ratio of the magnesium powder, the tetrahydrofuran, the 3, 4-dichlorobromobenzene and the trimethyl borate is 12 g: 300 mL: 90 g: 50g of the total weight of the mixture;
step S22, mixing the intermediate 3, 2-bromo-5-fluoroaniline, potassium carbonate and toluene, adding bis (triphenylphosphine) palladium dichloride under the conditions of 65 ℃ and nitrogen protection, carrying out reflux reaction for 5 hours after the addition is finished, extracting with water and ethyl acetate after the reaction is finished, and washing, drying and concentrating an organic phase to obtain a component B; wherein the dosage ratio of the intermediate 3, the 2-bromo-5-fluoroaniline, the potassium carbonate, the toluene and the bis-triphenylphosphine palladium dichloride is 13 g: 12 g: 33 g: 50mL of: 1g of the total weight of the composition.
Step S3, mixing the component A, the component B and toluene, heating to 60 ℃, dropwise adding triethylamine, refluxing and reacting for 5 hours after dropwise adding, cooling to room temperature after reaction, extracting with toluene, and washing, drying and concentrating an organic phase to obtain an intermediate 4; wherein the dosage ratio of the component A, the component B, toluene and triethylamine is 15.3 g: 15 g: 100mL of: 9.1 g;
step S4, mixing the intermediate 4, p-iodotoluene, potassium carbonate and toluene, and reacting for 7h at the temperature of 70 ℃ to obtain an intermediate 5; wherein the dosage ratio of the intermediate 4 to the p-iodotoluene to the potassium carbonate to the toluene is 2 g: 1.1 g: 0.2 g: 20 mL;
the reaction process is as follows:
and step S5, mixing the intermediate 5 with toluene, adding epoxy chloropropane, heating and refluxing for 5 hours after the addition is finished, cooling to room temperature after the reaction is finished, then carrying out vacuum filtration, and drying the obtained filter cake to constant weight at 40 ℃ to obtain the modifier. Wherein the dosage ratio of the intermediate 5, the epichlorohydrin to the toluene is 5.3 g: 1 g: 40 mL.
The reaction process is as follows:
furthermore, the coupling agent is one or two of gamma-aminopropyltriethoxysilane and gamma- (2, 3-glycidoxy) propyltrimethoxysilane which are mixed according to any proportion.
Further, the cross-linking agent is one or two of methyl tributyl ketoxime silane and vinyl tributyrinoxime silane which are mixed according to any proportion.
Further, the catalyst was dibutyltin dilaurate.
The invention has the beneficial effects that:
the modified silicone oil is prepared by the modifier and the aminoethyl aminopropyl silicone oil, wherein the modifier is quaternary ammonium salt containing epoxy group, the epoxy group in the modifier is easy to open-loop connect with the amino group in the aminoethyl aminopropyl silicone oil, after the quaternary ammonium salt is introduced, nitrogen atoms are positively charged and are not easy to oxidize, so as to achieve the effect of inhibiting yellowing, meanwhile, the quaternary ammonium salt structure can adsorb bacteria with negative charges, so as to have better sterilization and anti-mildew effects, the obtained modified silicone oil can replace common silicone oil, so as to have long-term sterilization and anti-yellowing performance, in addition, the added mildew preventive is easy to separate out from the sealant, the modifier contains a component A which has the quaternary ammonium salt structure, can resist bacteria, also contains five-membered heterocycle of N and S groups and has the mildew-proof effect, the modifier containing the structure has more stable effect, the mildew-proof performance is improved, and the component A is not easy to lose efficacy due to the introduction of the modifier, the mildew-proof effect is more durable.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
Example 1
Preparation of component A:
step S11, mixing chlorobenzene, deionized water and 2- (methylthio) benzonitrile, adding sulfonyl chloride at the temperature of 0 ℃, heating to 35 ℃ after the addition, reacting for 15min, heating to 75 ℃, reacting for 40min, cooling to 0 ℃ after the reaction, precipitating a solid, performing suction filtration under reduced pressure, and recrystallizing the obtained solid with absolute ethyl alcohol to obtain an intermediate 1; wherein the dosage ratio of chlorobenzene to deionized water to the 2- (methylthio) benzonitrile to the sulfonyl chloride is 150 mL: 3.4 g: 25g of: 28g of a mixture;
step S12, mixing deionized water, the intermediate 1 and potassium hydroxide, stirring for reaction for 20min, heating to 115 ℃, dropwise adding a sodium chloroacetate aqueous solution, reacting for 8h after addition, cooling to room temperature after the reaction is finished, performing reduced pressure suction filtration, adjusting the pH value of filtrate to 1 by using concentrated hydrochloric acid, precipitating a solid, performing reduced pressure suction filtration, washing a filter cake by using deionized water, absolute ethyl alcohol and acetone in sequence, and drying to constant weight at 70 ℃ after washing is finished to obtain an intermediate 2; wherein the sodium chloroacetate aqueous solution is sodium chloroacetate and deionized water 6 g: 10 mL; the dosage ratio of the deionized water, the intermediate 1, the potassium hydroxide and the sodium chloroacetate aqueous solution is 50 mL: 8 g: 3.5 g: 10 mL;
step S13, mixing the intermediate 2, thionyl chloride and N, N-dimethylformamide, heating and refluxing for 5 hours, and evaporating the thionyl chloride after the reaction is finished to obtain a component A; wherein the dosage ratio of the intermediate 2, the thionyl chloride and the N, N-dimethylformamide is 21 g: 100 g: 2 mL.
Example 2
Preparation of component B:
step S21, mixing magnesium powder and tetrahydrofuran, adding 3, 4-dichlorobromobenzene at the temperature of 20 ℃, heating to 45 ℃ after adding, stirring for reaction for 2 hours, then cooling to-5 ℃, adding trimethyl borate, keeping the temperature unchanged for reaction for 3 hours, adding a hydrochloric acid solution with the mass fraction of 10% of that of the tetrahydrofuran after the reaction is finished, mixing and standing for layering, extracting an organic phase with toluene, washing with water, drying and concentrating to obtain an intermediate 3; wherein the dosage ratio of the magnesium powder, the tetrahydrofuran, the 3, 4-dichlorobromobenzene and the trimethyl borate is 12 g: 300 mL: 90 g: 50g of the total weight of the mixture;
step S22, mixing the intermediate 3, 2-bromo-5-fluoroaniline, potassium carbonate and toluene, adding bis (triphenylphosphine) palladium dichloride under the conditions of 65 ℃ and nitrogen protection, carrying out reflux reaction for 5 hours after the addition is finished, extracting with water and ethyl acetate after the reaction is finished, and washing, drying and concentrating an organic phase to obtain a component B; wherein the dosage ratio of the intermediate 3, the 2-bromo-5-fluoroaniline, the potassium carbonate, the toluene and the bis-triphenylphosphine palladium dichloride is 13 g: 12 g: 33 g: 50mL of: 1g of the total weight of the composition.
Example 3
Preparing a modifier:
step S3, mixing the component A prepared in the embodiment 1 and the component B prepared in the embodiment 2 with toluene, heating to 60 ℃, dropwise adding triethylamine, carrying out reflux reaction for 5 hours after dropwise adding, cooling to room temperature after reaction, extracting with toluene, and washing, drying and concentrating an organic phase to obtain an intermediate 4; wherein the dosage ratio of the component A, the component B, toluene and triethylamine is 15.3 g: 15 g: 100mL of: 9.1 g;
step S4, mixing the intermediate 4, p-iodotoluene, potassium carbonate and toluene, and reacting for 7h at the temperature of 70 ℃ to obtain an intermediate 5; wherein the dosage ratio of the intermediate 4 to the p-iodotoluene to the potassium carbonate to the toluene is 2 g: 1.1 g: 0.2 g: 20 mL;
step S5, mixing the intermediate 5 with toluene, adding epoxy chloropropane, heating and refluxing for 5 hours after the addition is finished, cooling to room temperature after the reaction is finished, then carrying out vacuum filtration, and drying the obtained filter cake to constant weight at 40 ℃ to obtain a modifier; wherein the dosage ratio of the intermediate 5, the epichlorohydrin to the toluene is 5.3 g: 1 g: 40 mL.
Example 4
Preparing modified silicone oil:
mixing the aminoethyl aminopropyl silicone oil, the modifier and isopropanol, carrying out reflux reaction for 4 hours at the temperature of 85 ℃, then carrying out heat preservation for 2 hours, and then removing the isopropanol under the condition of 0.01MPa to obtain the modified silicone oil. Wherein the dosage ratio of the aminoethyl aminopropyl silicone oil to the modifier to the isopropanol is 1.2 g: 0.6 g: 10mL, modifier from example 3.
Example 5
Preparing modified silicone oil:
mixing the aminoethyl aminopropyl silicone oil, the modifier and isopropanol, carrying out reflux reaction for 4 hours at the temperature of 85 ℃, then carrying out heat preservation for 2 hours, and then removing the isopropanol under the condition of 0.01MPa to obtain the modified silicone oil. Wherein the dosage ratio of the aminoethyl aminopropyl silicone oil to the modifier to the isopropanol is 1.5 g: 0.6 g: 10mL, modifier from example 3.
Example 6
Preparing a silicone sealant:
firstly, weighing the following raw materials in parts by weight: 55 parts of alpha, omega-dihydroxy polysiloxane, 7 parts of methyl silicone oil, 20 parts of modified silicone oil, 1.9 parts of cross-linking agent, 7 parts of fumed silica, 0.4 part of coupling agent and 0.2 part of catalyst;
secondly, mixing alpha, omega-dihydroxy polysiloxane, methyl silicone oil, modified silicone oil and a cross-linking agent for 1h in vacuum at the temperature of 30 ℃ under the vacuum condition, adding fumed silica, continuously mixing for 30min in vacuum, then adding a coupling agent and a catalyst, and continuously mixing for 30min in vacuum; a silicone sealant was obtained.
Wherein the coupling agent is gamma-aminopropyl triethoxysilane; the cross-linking agent is methyl tributyl ketoxime silane; the catalyst is dibutyltin dilaurate; the modified silicone oil was obtained in example 4.
Example 7
Preparing a silicone sealant:
firstly, weighing the following raw materials in parts by weight: 60 parts of alpha, omega-dihydroxy polysiloxane, 7 parts of methyl silicone oil, 25 parts of modified silicone oil, 2 parts of cross-linking agent, 9 parts of fumed silica, 0.5 part of coupling agent and 0.2 part of catalyst;
secondly, mixing alpha, omega-dihydroxy polysiloxane, methyl silicone oil, modified silicone oil and a cross-linking agent for 1h in vacuum at the temperature of 30 ℃ under the vacuum condition, adding fumed silica, continuously mixing for 30min in vacuum, then adding a coupling agent and a catalyst, and continuously mixing for 30min in vacuum; a silicone sealant was obtained.
Wherein the coupling agent is gamma-aminopropyl triethoxysilane; the cross-linking agent is methyl tributyl ketoxime silane; the catalyst is dibutyltin dilaurate; the modified silicone oil was obtained in example 4.
Example 8
Preparing a silicone sealant:
firstly, weighing the following raw materials in parts by weight: 70 parts of alpha, omega-dihydroxy polysiloxane, 8 parts of methyl silicone oil, 30 parts of modified silicone oil, 2.2 parts of cross-linking agent, 11 parts of fumed silica, 0.6 part of coupling agent and 0.3 part of catalyst;
secondly, mixing alpha, omega-dihydroxy polysiloxane, methyl silicone oil, modified silicone oil and a cross-linking agent for 1h in vacuum at the temperature of 30 ℃ under the vacuum condition, adding fumed silica, continuously mixing for 30min in vacuum, then adding a coupling agent and a catalyst, and continuously mixing for 30min in vacuum; a silicone sealant was obtained.
Wherein the coupling agent is gamma-aminopropyl triethoxysilane; the cross-linking agent is methyl tributyl ketoxime silane; the catalyst is dibutyltin dilaurate; the modified silicone oil was obtained in example 4.
Comparative example 1
The modified silicone oil in comparative example 7 was changed to aminoethylaminopropyl silicone oil, and the remaining raw materials and preparation process were kept unchanged.
Comparative example 2
The modified silicone oil in comparative example 7 was replaced with dimethyl silicone oil, and the remaining raw materials and preparation process were kept unchanged.
The samples prepared in examples 6 to 8 and comparative examples 1 to 2 were subjected to the test; and (3) mildew-proof grade: according to the test in GB/T1741-2007, according to JC/T885-2001, the building mildew-proof sealant, the grade 0 does not have obvious mildew growth under the magnification of about 50 times; grade 1 is where no or very little mold growth is visible to the naked eye, but is evident under a magnifying glass. And (4) placing the completely cured transparent adhesive tape in an oven at 90 ℃ for treatment for 3d, and observing the color change.
The test results are shown in table 1 below:
TABLE 1
As can be seen from the above Table 1, the silicone sealant prepared by the invention has good mildew resistance and good yellowing inhibition.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (8)
1. The preparation method of the silicone sealant is characterized by comprising the following steps:
mixing alpha, omega-dihydroxy polysiloxane, methyl silicone oil, modified silicone oil and a cross-linking agent for 1h in vacuum at the temperature of 30 ℃ under the vacuum condition, adding fumed silica, continuously mixing for 30min in vacuum, then adding a coupling agent and a catalyst, and continuously mixing for 30min in vacuum; obtaining a silicone sealant;
the modified silicone oil is prepared by the following steps:
mixing reactive aminoethyl aminopropyl silicone oil, a modifier and isopropanol, carrying out reflux reaction for 4 hours at the temperature of 85 ℃, then carrying out heat preservation for 2 hours, and then removing the isopropanol under the condition of 0.01MPa to obtain the modified silicone oil.
2. The method of claim 1, wherein the modifier is prepared by the steps of:
step S1, preparing component A;
step S2, preparing component B;
step S3, mixing the component A, the component B and toluene, heating to 60 ℃, dropwise adding triethylamine, and after dropwise adding, carrying out reflux reaction for 5 hours to obtain an intermediate 4;
step S4, mixing the intermediate 4, p-iodotoluene, potassium carbonate and toluene, and reacting for 7h at the temperature of 70 ℃ to obtain an intermediate 5;
and step S5, mixing the intermediate 5 with toluene, then adding epoxy chloropropane, and heating and refluxing for 5h after the addition is finished to obtain the modifier.
3. The preparation method of the silicone sealant according to claim 1, wherein the weight parts of the materials are as follows: 55-70 parts of alpha, omega-dihydroxy polysiloxane, 7-8 parts of methyl silicone oil, 20-30 parts of modified silicone oil, 1.9-2.2 parts of cross-linking agent, 7-11 parts of fumed silica, 0.4-0.6 part of coupling agent and 0.2-0.3 part of catalyst.
4. The method for preparing a silicone sealant according to claim 2, wherein the component A is prepared by the following steps:
step S11, mixing chlorobenzene, deionized water and 2- (methylthio) benzonitrile, adding sulfonyl chloride at the temperature of 0 ℃, heating to 35 ℃ after the addition, reacting for 15min, heating to 75 ℃, and reacting for 40min to obtain an intermediate 1;
step S12, mixing deionized water, the intermediate 1 and potassium hydroxide, stirring and reacting for 20min, then heating to 115 ℃, dropwise adding a sodium chloroacetate aqueous solution, and reacting for 8h after the addition to obtain an intermediate 2;
and step S13, mixing the intermediate 2, thionyl chloride and N, N-dimethylformamide, heating and refluxing for 5 hours, and evaporating the thionyl chloride after the reaction is finished to obtain the component A.
5. The method of claim 2 wherein component B is prepared by the steps of:
step S21, mixing magnesium powder and tetrahydrofuran, adding 3, 4-dichlorobromobenzene at the temperature of 20 ℃, heating to 45 ℃ after the addition, stirring for reaction for 2 hours, then cooling to-5 ℃, adding trimethyl borate, and keeping the temperature unchanged for reaction for 3 hours to obtain an intermediate 3;
and step S22, mixing the intermediate 3, 2-bromo-5-fluoroaniline, potassium carbonate and toluene, adding bis (triphenylphosphine) palladium dichloride under the conditions of 65 ℃ and nitrogen protection, and performing reflux reaction for 5 hours to obtain a component B.
6. The method for preparing a silicone sealant according to claim 1, wherein the coupling agent is one or two of γ -aminopropyltriethoxysilane and γ - (2, 3-glycidoxy) propyltrimethoxysilane, which are mixed in an arbitrary ratio.
7. The method for preparing a silicone sealant according to claim 1, wherein the crosslinking agent is one or two of methyltributanoxime silane and vinyltributoxime silane mixed in an arbitrary ratio.
8. The method of claim 1 wherein the catalyst is dibutyltin dilaurate.
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| CN115157111A (en) * | 2022-07-13 | 2022-10-11 | 安徽禾臣新材料有限公司 | Polishing pad for glass processing and preparation method thereof |
| CN115784928A (en) * | 2022-12-08 | 2023-03-14 | 济宁正东化工有限公司 | Method for synthesizing 3,4-dichlorobenzonitrile |
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