CN111057241A - MT hydrogen-containing methyl phenyl silicone resin and preparation method thereof - Google Patents
MT hydrogen-containing methyl phenyl silicone resin and preparation method thereof Download PDFInfo
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- CN111057241A CN111057241A CN201911424152.3A CN201911424152A CN111057241A CN 111057241 A CN111057241 A CN 111057241A CN 201911424152 A CN201911424152 A CN 201911424152A CN 111057241 A CN111057241 A CN 111057241A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/70—Siloxanes defined by use of the MDTQ nomenclature
Abstract
The invention relates to MT hydrogen-containing methyl phenyl silicone resin and a preparation method thereof, wherein phenyl trimethoxy silane and hydrochloric acid aqueous solution are mixed or phenyl trimethoxy silane, water and acidic cationic resin are mixed, reaction is carried out under the heating condition to obtain a reactant, and hydrochloric acid or acidic cationic resin is removed to obtain a hydroxyl-containing phenyl polysiloxane intermediate; mixing the hydroxyl-containing phenyl polysiloxane intermediate with an end-capping agent and an acidic cationic resin, reacting under heating conditions, removing the acidic cationic resin, and distilling under reduced pressure to remove low-boiling-point substances. The method is simple to operate, good in repeatability and controllability, energy-saving and environment-friendly, and a large amount of organic solvent is not required to be used.
Description
Technical Field
The invention relates to the technical field of organic silicon materials, in particular to MT hydrogen-containing methyl phenyl silicone resin and a preparation method thereof.
Background
The organic silicon material becomes one of the key research directions of the LED packaging materials at home and abroad by virtue of the advantages of excellent thermal stability, aging resistance, mechanical property, optical property, moisture resistance and the like. Therefore, the development of the organic silicon material with excellent performance has great significance for the promotion of the LED packaging technology and the development of the LED industry in China.
One key in the development of organosilicon materials is to synthesize methyl phenyl silicone resin with high light transmittance and refractive index and good thermal stability, such as: the MT hydrogen-containing methyl phenyl silicone resin is suitable for LED packaging glue. The traditional MT hydrogen-containing methyl phenyl silicone resin is prepared by hydrolytic polycondensation of hydrogen-containing chlorosilane and non-hydrogen-containing chlorosilane, a large amount of organic solvent is needed in the preparation process, and the repeatability and controllability are poor, so that the defects of complex synthesis process and high pollution and energy consumption in the production process exist.
Disclosure of Invention
Accordingly, there is a need for a method for preparing MT hydrogen-containing methylphenyl silicone resin and MT hydrogen-containing methylphenyl silicone resin which have simple synthesis process and do not need to use a large amount of organic solvent.
A preparation method of MT hydrogen-containing methyl phenyl silicone resin comprises the following steps:
mixing phenyltrimethoxysilane and hydrochloric acid aqueous solution;
mixing phenyltrimethoxysilane, water and acidic cationic resin, reacting under heating to obtain a reactant, and removing hydrochloric acid or the acidic cationic resin to obtain a hydroxyl-containing phenyl polysiloxane intermediate;
mixing the hydroxyl-containing phenyl polysiloxane intermediate with an end-capping agent and an acidic cationic resin, reacting under heating conditions, removing the acidic cationic resin, and distilling under reduced pressure to remove low-boiling-point substances.
The preparation process of the MT hydrogen-containing methyl phenyl silicone resin starts from phenyl trimethoxy silane, firstly a hydroxyl-containing phenyl polysiloxane intermediate is synthesized through a hydrolytic condensation reaction, and then the MT hydrogen-containing methyl phenyl silicone resin is obtained under the action of an end-capping agent and acidic cation resin, is colorless transparent viscous liquid, and compared with the preparation process of the MT hydrogen-containing methyl phenyl silicone resin through hydrolytic polycondensation of hydrogen-containing chlorosilane and non-hydrogen-containing chlorosilane, the method is simple to operate, good in repeatability and controllability, energy-saving and environment-friendly, and does not need to use a large amount of organic solvent.
In one embodiment, in the step of mixing phenyltrimethoxysilane and the aqueous hydrochloric acid solution, the mass ratio of phenyltrimethoxysilane to the aqueous hydrochloric acid solution is (1:2) - (2: 1); the mass concentration of the hydrochloric acid aqueous solution is 1-3%.
In one embodiment, in the step of mixing phenyltrimethoxysilane, water and the acidic cationic resin, the mass ratio of phenyltrimethoxysilane to water is (1:2) to (2: 1); the mass of the acidic cation resin is 0.5-2% of the total mass of reactants formed by the phenyltrimethoxysilane and the water.
In one embodiment, the acidic cationic resin is a CH-01 type acidic cationic resin.
In one embodiment, in the step of mixing the hydroxyl-containing phenyl polysiloxane intermediate with the end-capping agent and the acidic cationic resin, the mass ratio of the hydroxyl-containing phenyl polysiloxane intermediate to the end-capping agent is (10:6) - (10:1), and the mass of the acidic cationic resin is 0.5% -2% of the total mass of reactants consisting of the hydroxyl-containing phenyl polysiloxane intermediate and the end-capping agent.
In one embodiment, the capping agent comprises a hydrogen-containing double head.
In one embodiment, in the step of removing hydrochloric acid to obtain the hydroxyl group-containing phenyl polysiloxane intermediate, the reaction product is washed with water to a pH of 6.8-7.2, and subjected to dehydration treatment to obtain the hydroxyl group-containing phenyl polysiloxane intermediate.
In one embodiment, in the step of carrying out the reaction under the heating condition to obtain the reactant, the heating temperature is 30-70 ℃, the reaction time is 2-4 h, and/or;
in the step of mixing the hydroxyl-containing phenyl polysiloxane intermediate with an end-capping reagent and acidic cationic resin and reacting under a heating condition, the heating temperature is 50-80 ℃; the reaction time is 4-6 h.
The invention also provides MT hydrogen-containing methylphenyl silicone resin prepared by the preparation method of MT hydrogen-containing methylphenyl silicone resin.
In one embodiment, the MT hydrogenous methylphenyl silicone resin has a refractive index of 1.50-1.55, and the viscosity of the MT hydrogenous methylphenyl silicone resin is 2000mPa.s-5000mPa.s at 24-26 ℃.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
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. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The embodiment of the invention provides a preparation method of MT hydrogen-containing methyl phenyl silicone resin, which comprises the following steps:
s1, mixing phenyltrimethoxysilane and hydrochloric acid aqueous solution, or
Mixing phenyltrimethoxysilane, water and acidic cationic resin, reacting under heating to obtain a reactant, and removing hydrochloric acid or the acidic cationic resin to obtain a hydroxyl-containing phenyl polysiloxane intermediate.
Wherein, the hydrochloric acid aqueous solution and the acidic cation resin mainly play a role in catalyzing the phenyltrimethoxysilane to perform hydrolytic condensation reaction. In addition, the aqueous hydrochloric acid solution can also provide water necessary for the hydrolysis condensation reaction, and after the reaction, the hydrochloric acid in the aqueous hydrochloric acid solution needs to be removed.
It is to be understood that the above-mentioned water is not limited, and preferably, the water is distilled water.
The preparation process starts from phenyl trimethoxy silane, and synthesizes the phenyl polysiloxane intermediate containing hydroxyl through hydrolytic condensation reaction under the heating condition, the hydrolytic condensation process is single and easy to control, and few by-products are formed. Compared with the preparation process of MT hydrogen-containing methyl phenyl silicone resin by hydrolytic polycondensation of hydrogen-containing chlorosilane and non-hydrogen-containing chlorosilane, the method has the advantages of simple operation, good repeatability and controllability, no need of using organic solvent, energy conservation and environmental protection.
In one embodiment, in the step of carrying out the reaction under the heating condition to obtain the reactant, the heating temperature is 30-70 ℃, the reaction time is 2-4 h,
in one embodiment, in the step of mixing phenyltrimethoxysilane and the aqueous hydrochloric acid solution, the mass ratio of phenyltrimethoxysilane to the aqueous hydrochloric acid solution is (1:2) - (2: 1); the mass concentration of the hydrochloric acid aqueous solution is 1-3%.
In one embodiment, in the step of mixing phenyltrimethoxysilane, water and the acidic cationic resin, the mass ratio of phenyltrimethoxysilane to water is (1:2) to (2: 1); the mass of the acidic cation resin is 0.5-2% of the total mass of reactants formed by the phenyltrimethoxysilane and the water.
In one embodiment, in the step of removing hydrochloric acid to obtain the hydroxyl group-containing phenyl polysiloxane intermediate, the reaction product is washed with water until the pH of the reaction product is 6.8-7.2 to remove hydrochloric acid, and then subjected to dehydration treatment to obtain the hydroxyl group-containing phenyl polysiloxane intermediate. Further, the water removal agent is anhydrous calcium chloride.
In one embodiment, in the step of removing the acidic cationic resin to obtain the hydroxyl-containing phenyl polysiloxane intermediate, the acidic cationic resin is removed by suction filtration.
In one embodiment, the acidic cationic resin is a CH-01 type acidic cationic resin. The advantage of selecting this catalyst is that no other impurity ions are introduced into the system.
S2, mixing the hydroxyl-containing phenyl polysiloxane intermediate with an end-capping agent and an acidic cationic resin, reacting under heating conditions, removing the acidic cationic resin, and removing low-boiling-point substances by reduced pressure distillation to obtain the MT hydrogen-containing methylphenyl silicone resin.
MT-class silicone is a class of silicone resins consisting of organosilicon trifunctional units (T-linkages) and organosilicon monofunctional units (M-linkages).
In one embodiment, the mass ratio of the hydroxyl-containing phenyl polysiloxane intermediate to the end-capping agent is (10:6) - (10:1), and the mass of the acidic cationic resin is 0.5% -2% of the total mass of the reactants consisting of the hydroxyl-containing phenyl polysiloxane intermediate and the end-capping agent.
In one embodiment, the capping agent comprises a hydrogen-containing double head (MM)H). Further, the end-capping agent further comprises hexamethyldisiloxane (MM). Further, the end capping agent is composed of a hydrogen-containing double end cap (MM)H) And hexamethyldisiloxane (MM), preferably hydrogen-containing bis-end-caps (MM)H) And hexamethyldisiloxane (MM) in a mass ratio of (10-30) to (10-15).
In one embodiment, the acidic cationic resin is a CH-01 type acidic cationic resin, and the catalyst is selected to have the advantage of not introducing other impurity ions into the system.
In one embodiment, in the step of mixing the hydroxyl-containing phenyl polysiloxane intermediate with the end-capping agent and the acidic cationic resin and reacting under heating, the heating temperature is 50-80 ℃; the reaction time is 4-6 h.
In one embodiment, in the step of removing low boiling substances by distillation under reduced pressure, the substances removed under the conditions of 130 ℃ to 160 ℃ and vacuum degree of-0.096 MPa are low boiling substances.
The preparation process of the MT hydrogen-containing methyl phenyl silicone resin starts from phenyl trimethoxy silane, firstly a hydroxyl-containing phenyl polysiloxane intermediate is synthesized through a hydrolysis condensation reaction, and then under the action of an end-capping reagent and an acidic cation resin, the obtained MT hydrogen-containing methyl phenyl silicone resin is a colorless transparent viscous liquid, has high light transmittance and good thermal stability, has a refractive index of 1.50-1.55, an active hydrogen (mass percentage) content of 0.1-0.5% and a viscosity of 2000-5000mPa.s, and can be applied to LED packaging adhesive materials.
The embodiment of the invention also provides MT hydrogen-containing methylphenyl silicone resin prepared by the preparation method of the MT hydrogen-containing methylphenyl silicone resin.
In one embodiment, the MT hydrogenous methylphenyl silicone resin has a refractive index of 1.50-1.55, and the viscosity of the MT hydrogenous methylphenyl silicone resin is 2000mPa.s-5000mPa.s at 24-26 ℃. Further, the refractive index of the MT hydrogenous methylphenyl silicone resin is 1.511-1.518, and the viscosity of the MT hydrogenous methylphenyl silicone resin is 2700mPa.s-4500mPa.s at 24-26 ℃.
Compared with the traditional MT hydrogen-containing methyl phenyl silicone resin, the MT hydrogen-containing methyl phenyl silicone resin has high refractive index, so that the luminous flux of the MT hydrogen-containing methyl phenyl silicone resin is improved, the light transmission is good, and the light transmission of an LED product packaged by the resin is good. Further, the above MT hydrogenmethylphenyl silicone resin is suitable in viscosity.
It is understood that the preparation method of the MT hydrogen-containing methylphenyl silicone resin includes, but is not limited to, the preparation method of the MT hydrogen-containing methylphenyl silicone resin provided in the present application, and other preparation methods capable of obtaining the MT hydrogen-containing methylphenyl silicone resin are also possible.
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described in detail below with reference to examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of MT hydrogen-containing methyl phenyl silicone resin comprises the following steps:
(1) adding 80g of hydrochloric acid aqueous solution with the mass fraction of 2.0% into a four-neck flask provided with a mechanical stirrer, a temperature controller and a reflux condenser tube, preheating to 50 ℃, adding 80g of phenyltrimethoxysilane, reacting for 3 hours at 50 ℃, transferring the product into a separating funnel, washing for 3-4 times with distilled water until the pH value is 7, standing for layering, taking a lower-layer organic phase liquid product, drying with anhydrous calcium chloride to remove water, and performing suction filtration to remove the calcium chloride after the water removal, thereby preparing the colorless and transparent hydroxyl-containing phenyl polysiloxane intermediate.
(2) 50g of the hydroxyl-containing phenylpolysiloxane intermediate prepared above was charged into a four-neck flask equipped with a mechanical stirrer, a temperature controller and a reflux condenser, preheated to 60 ℃ and then charged with 10gMMHAnd 0.6g of CH-01 type acidic cation resin to react for 5 hours at the temperature of 60 ℃, after the reaction is finished, the CH-01 type acidic cation resin catalyst is removed by suction filtration, and then the product is transferred into a round bottom distillation flask to remove low-boiling-point substances by reduced pressure distillation under the conditions of 150 ℃ and 0.096MPa, thereby preparing the colorless, transparent and viscous MT hydrogen-containing methylphenyl silicon resin.
Example 2
A preparation method of MT hydrogen-containing methyl phenyl silicone resin comprises the following steps:
(1) 80g of hydrochloric acid solution with the mass fraction of 2.0 percent is added into a four-neck flask provided with a mechanical stirrer, a temperature controller and a reflux condenser tube to be preheated to 50 ℃, and then 80g of phenyltrimethoxysilane is added to react for 3 hours at the temperature of 50 ℃. And after the reaction is finished, transferring the product into a separating funnel, washing the product for 3-4 times by using distilled water until the product is neutral, standing and layering the product, taking a lower-layer organic phase liquid product, drying and dewatering the product by using anhydrous calcium chloride, and filtering and removing the calcium chloride after dewatering to obtain the colorless and transparent hydroxyl-containing phenyl polysiloxane intermediate.
(2) 50g of the hydroxyl-containing phenylpolysiloxane intermediate prepared above was charged into a four-neck flask equipped with a mechanical stirrer, a temperature controller and a reflux condenser, preheated to 60 ℃ and then charged with 15gMMH15gMM and 0.8gCH-01 type acidic cation resin at 60 ℃ for 5 hours. After the reaction is finished, removing the CH-01 type acidic cationic resin catalyst by suction filtration, transferring the product into a round bottom distillation flask, and removing low-boiling-point substances by reduced pressure distillation under the condition of 150 ℃/-0.096MPa, thereby preparing the colorless, transparent and viscous MT hydrogen-containing methylphenyl silicon resin.
Example 3
A preparation method of MT hydrogen-containing methyl phenyl silicone resin comprises the following steps:
(1) 80g of hydrochloric acid with the mass fraction of 2.0 percent is added into a four-neck flask provided with a mechanical stirrer, a temperature controller and a reflux condenser tube to be preheated to 50 ℃, and then 80g of phenyltrimethoxysilane is added to react for 3 hours at the temperature of 50 ℃. And after the reaction is finished, transferring the product into a separating funnel, washing the product for 3-4 times by using distilled water until the product is neutral, standing and layering the product, taking a lower-layer organic phase liquid product, drying and dewatering the product by using anhydrous calcium chloride, and filtering and removing the calcium chloride after dewatering to obtain the colorless and transparent hydroxyl-containing phenyl polysiloxane intermediate.
(2) 50g of the hydroxyl-containing phenylpolysiloxane intermediate prepared above was charged into a four-neck flask equipped with a mechanical stirrer, a temperature controller and a reflux condenser, preheated to 60 ℃ and then charged with 20gMMH10gMM and 0.8gCH-01 type acidic cation resin at 60 ℃ for 5 hours. After the reaction is finished, removing the CH-01 type acidic cationic resin catalyst by suction filtration, transferring the product into a round bottom distillation flask, and removing low-boiling-point substances by reduced pressure distillation under the condition of 150 ℃/-0.096MPa, thereby preparing the colorless, transparent and viscous MT hydrogen-containing methylphenyl silicon resin.
Example 4
A preparation method of MT hydrogen-containing methyl phenyl silicone resin comprises the following steps:
(1) 80g of phenyltrimethoxysilane and 80g of distilled water are added into a four-neck flask provided with a mechanical stirrer, a temperature controller and a reflux condenser tube to be preheated to 40 ℃, and then 1.6gCH-01 type acidic cationic resin is added to react for 3 hours at the temperature of 40 ℃. And after the reaction is finished, performing suction filtration on the product to remove the CH-01 type acidic cationic resin, pouring the product into a separating funnel, standing for layering, taking a lower-layer organic phase liquid product, drying and dewatering by using anhydrous calcium chloride, and performing suction filtration to remove the calcium chloride after dewatering to obtain the colorless and transparent hydroxyl-containing phenyl polysiloxane intermediate.
(2) 50g of the hydroxyl-containing phenylpolysiloxane intermediate prepared above was charged into a four-neck flask equipped with a mechanical stirrer, a temperature controller and a reflux condenser, preheated to 60 ℃ and then charged with 10gMMH10gMM and 0.7gCH-01 type acidic cation resin is reacted for 5 hours at 60 ℃. After the reaction is finished, removing the CH-01 type acidic cationic resin catalyst by suction filtration, transferring the product into a round bottom distillation flask, and removing low-boiling-point substances by reduced pressure distillation under the condition of 150 ℃/-0.096MPa, thereby preparing the colorless, transparent and viscous MT hydrogen-containing methylphenyl silicon resin.
Example 5
A preparation method of MT hydrogen-containing methyl phenyl silicone resin comprises the following steps:
(1) 80g of phenyltrimethoxysilane and 80g of distilled water are added into a four-neck flask provided with a mechanical stirrer, a temperature controller and a reflux condenser tube to be preheated to 40 ℃, and then 1.6gCH-01 type acidic cationic resin is added to react for 3 hours at the temperature of 40 ℃. And after the reaction is finished, performing suction filtration on the product to remove the CH-01 type acidic cationic resin, pouring the product into a separating funnel, standing for layering, taking a lower-layer organic phase liquid product, drying and dewatering by using anhydrous calcium chloride, and performing suction filtration to remove the calcium chloride after dewatering to obtain the colorless and transparent hydroxyl-containing phenyl polysiloxane intermediate.
(2) 50g of the hydroxyl-containing phenylpolysiloxane intermediate prepared above was charged into a four-neck flask equipped with a mechanical stirrer, a temperature controller and a reflux condenser, preheated to 60 ℃ and then charged with 15gMMH10gMM and 0.75gCH-01 type acidic cation resin at 60 ℃ for 5 hours. After the reaction is finished, removing the CH-01 type acidic cationic resin catalyst by suction filtration, transferring the product into a round bottom distillation flask, and removing low-boiling-point substances by reduced pressure distillation under the condition of 150 ℃/-0.096MPa, thereby preparing the colorless, transparent and viscous MT hydrogen-containing methylphenyl silicon resin.
Example 6
A preparation method of MT hydrogen-containing methyl phenyl silicone resin comprises the following steps:
(1) 80g of phenyltrimethoxysilane and 80g of distilled water are added into a four-neck flask provided with a mechanical stirrer, a temperature controller and a reflux condenser tube to be preheated to 40 ℃, and then 1.6gCH-01 type acidic cationic resin is added to react for 3 hours at the temperature of 40 ℃. And after the reaction is finished, performing suction filtration on the product to remove the CH-01 type acidic cationic resin, pouring the product into a separating funnel, standing for layering, taking a lower-layer organic phase liquid product, drying and dewatering by using anhydrous calcium chloride, and performing suction filtration to remove the calcium chloride after dewatering to obtain the colorless and transparent hydroxyl-containing phenyl polysiloxane intermediate.
(2) 50g of the hydroxyl-containing phenylpolysiloxane intermediate prepared above was charged into a four-neck flask equipped with a mechanical stirrer, a temperature controller and a reflux condenser, preheated to 60 ℃ and then charged with 30gMMHAnd 0.8gCH-01 type acidic cation resin at 60 deg.C for 5 hr. After the reaction is finished, removing the CH-01 type acidic cationic resin catalyst by suction filtration, transferring the product into a round bottom distillation flask, and removing low-boiling-point substances by reduced pressure distillation under the condition of 150 ℃/-0.096MPa, thereby preparing the colorless, transparent and viscous MT hydrogen-containing methylphenyl silicon resin.
Effect verification
The refractive index, active hydrogen content and viscosity are used as the investigation indexes of MT hydrogen-containing methyl phenyl silicone resin for testing, and the test results are shown in table 1.
TABLE 1
As shown in Table 1, the MT hydrogen-containing methylphenyl silicone resin prepared by the preparation method of the MT hydrogen-containing methylphenyl silicone resin has the refractive index of 1.50-1.55, the active hydrogen (mass percentage) content of 0.1-0.5% and the viscosity of 2000-5000mPa.s, and can be applied to LED packaging adhesive materials.
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. A preparation method of MT hydrogen-containing methyl phenyl silicone resin is characterized by comprising the following steps:
mixing phenyltrimethoxysilane and hydrochloric acid aqueous solution;
mixing phenyltrimethoxysilane, water and acidic cationic resin, reacting under heating to obtain a reactant, and removing hydrochloric acid or the acidic cationic resin to obtain a hydroxyl-containing phenyl polysiloxane intermediate;
mixing the hydroxyl-containing phenyl polysiloxane intermediate with an end-capping agent and an acidic cationic resin, reacting under heating conditions, removing the acidic cationic resin, and distilling under reduced pressure to remove low-boiling-point substances.
2. The method for preparing MT hydrogenous methylphenyl silicon resin according to claim 1, wherein in the step of mixing phenyltrimethoxysilane and an aqueous hydrochloric acid solution, the mass ratio of phenyltrimethoxysilane to the aqueous hydrochloric acid solution is (1:2) - (2: 1); the mass concentration of the hydrochloric acid aqueous solution is 1-3%.
3. The method of claim 1, wherein the weight ratio of phenyltrimethoxysilane to water in the step of mixing phenyltrimethoxysilane, water and the acidic cationic resin is (1:2) - (2: 1); the mass of the acidic cation resin is 0.5-2% of the total mass of reactants formed by the phenyltrimethoxysilane and the water.
4. The method of any one of claims 1-3, wherein the acidic cationic resin is a CH-01 type acidic cationic resin.
5. The method for preparing MT hydrogen-containing methylphenyl silicone resin according to any one of claims 1 to 3, wherein in the step of mixing the hydroxyl-containing phenyl polysiloxane intermediate with the end-capping agent and the acidic cationic resin, the mass ratio of the hydroxyl-containing phenyl polysiloxane intermediate to the end-capping agent is (10:6) - (10:1), and the mass of the acidic cationic resin is 0.5% -2% of the total mass of reactants consisting of the hydroxyl-containing phenyl polysiloxane intermediate and the end-capping agent.
6. The method of any one of claims 1-3, wherein the end-capping agent comprises hydrogen-containing bis-heads.
7. The method of any one of claims 1 to 3, wherein the step of removing hydrochloric acid to obtain a hydroxy-containing phenyl polysiloxane intermediate comprises washing the reaction product with water to a pH of 6.8 to 7.2, and dehydrating the reaction product to obtain a hydroxy-containing phenyl polysiloxane intermediate.
8. The method for preparing MT hydrogen-containing methylphenyl silicone resin according to any one of claims 1 to 3, wherein in the step of carrying out the reaction under heating to obtain a reactant, the heating temperature is 30 ℃ to 70 ℃, the reaction time is 2h to 4h, and/or;
in the step of mixing the hydroxyl-containing phenyl polysiloxane intermediate with an end-capping reagent and acidic cationic resin and reacting under a heating condition, the heating temperature is 50-80 ℃; the reaction time is 4-6 h.
9. An MT hydrogenous methylphenyl silicone resin prepared by the method for preparing the MT hydrogenous methylphenyl silicone resin according to any one of claims 1-8.
10. The MT hydrogenous methylphenyl silicone resin according to claim 9, wherein the refractive index of the MT hydrogenous methylphenyl silicone resin is 1.50-1.55, and the viscosity of the MT hydrogenous methylphenyl silicone resin is 2000mpa.s-5000mpa.s at 24-26 ℃.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102936414A (en) * | 2012-08-27 | 2013-02-20 | 湖北环宇化工有限公司 | High refraction and high adhesion large power LED packaging organosilicon material and preparation method thereof |
| CN103242531A (en) * | 2013-05-09 | 2013-08-14 | 成都硅宝新材料有限公司 | Preparation method of phenyl hydrogen-containing MT silicone resin |
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2019
- 2019-12-31 CN CN201911424152.3A patent/CN111057241A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936414A (en) * | 2012-08-27 | 2013-02-20 | 湖北环宇化工有限公司 | High refraction and high adhesion large power LED packaging organosilicon material and preparation method thereof |
| CN103242531A (en) * | 2013-05-09 | 2013-08-14 | 成都硅宝新材料有限公司 | Preparation method of phenyl hydrogen-containing MT silicone resin |
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