CN115594850A - Preparation method of T-type alkoxy silicone oil and application of T-type alkoxy silicone oil in room-temperature vulcanized silicone rubber - Google Patents
Preparation method of T-type alkoxy silicone oil and application of T-type alkoxy silicone oil in room-temperature vulcanized silicone rubber Download PDFInfo
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 56
- 125000003545 alkoxy group Chemical group 0.000 title claims abstract description 48
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 29
- 239000004945 silicone rubber Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 18
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004014 plasticizer Substances 0.000 claims abstract description 18
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 14
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 14
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 12
- GKTNLYAAZKKMTQ-UHFFFAOYSA-N n-[bis(dimethylamino)phosphinimyl]-n-methylmethanamine Chemical compound CN(C)P(=N)(N(C)C)N(C)C GKTNLYAAZKKMTQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 9
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLUBVTJUEUUZMR-UHFFFAOYSA-B silicon(4+);tetraphosphate Chemical compound [Si+4].[Si+4].[Si+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XLUBVTJUEUUZMR-UHFFFAOYSA-B 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 230000007062 hydrolysis Effects 0.000 claims abstract description 6
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 5
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 230000008707 rearrangement Effects 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 19
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 6
- 238000012544 monitoring process Methods 0.000 claims description 4
- 238000006462 rearrangement reaction Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 abstract description 5
- 238000001556 precipitation Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 12
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 10
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 6
- 239000000463 material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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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
- C08G77/38—Polysiloxanes modified by chemical after-treatment
-
- 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
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Silicon Polymers (AREA)
Abstract
The invention discloses a preparation method of T-type alkoxy silicone oil, which comprises the following steps: mixing DMC and hexamethyldisiloxane, heating, dripping phosphoric acid, refluxing and removing water to obtain a silicophosphate terminator; heating the linear body, adding a potassium hydroxide aqueous solution, stirring for polycondensation reaction, and adding a silicon phosphate terminator to obtain alpha, omega-dihydroxy polydimethylsiloxane; weighing methyltrimethoxysilane and hexamethyldisiloxane, adding alpha, omega-dihydroxy polydimethylsiloxane, stirring and heating; heating to a specified temperature, and adding a phosphazene catalyst; adding water for hydrolysis after the partial reaction, and then adding dimethyl dimethoxy silane for rearrangement and end capping again; after the full reaction is finished, adding a terminator and stirring; and continuously heating to remove low volatile matters to obtain the T-type alkoxy silicone oil. The obtained T-type alkoxy silicone oil is used as a plasticizer in room-temperature vulcanized silicone rubber, so that the problem of silicone oil precipitation is solved, the storage stability is improved, and the mechanical properties of the silicone rubber are greatly improved.
Description
Technical Field
The invention relates to the technical field of silicone rubber, in particular to a preparation method of T-type alkoxy silicone oil and application of the T-type alkoxy silicone oil in room-temperature vulcanized silicone rubber.
Background
The silicon rubber is a high molecular elastic material with molecular chains having both inorganic and organic properties, has unique comprehensive properties such as high and low temperature resistance, excellent electrical property and chemical stability, water resistance, ozone resistance and weather aging resistance, is simple in use and strong in process applicability, and is widely applied as an adhesive material when room temperature vulcanized silicone Rubber (RTV) is used as a building sealant commonly called glass cement. However, the traditional room temperature vulcanized silicone rubber generally uses dimethyl silicone oil as a plasticizer, and during storage, the dimethyl silicone oil is easy to precipitate, and the storage stability is poor, so that the performance of the room temperature vulcanized silicone rubber is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of T-type alkoxy silicone oil and application of the T-type alkoxy silicone oil in room-temperature vulcanized silicone rubber, which solves the problem of silicone oil precipitation, improves the storage stability and greatly improves the mechanical properties of the silicone rubber.
In order to achieve the purpose, the invention provides a preparation method of T-type alkoxy silicone oil, which comprises the following steps:
s1, mixing DMC and hexamethyldisiloxane, heating to 160-180 ℃, dropwise adding phosphoric acid, stirring for 6-8 hours, refluxing and removing water to obtain a silicophosphate terminator;
s2, heating the linear body to 130-150 ℃, adding a potassium hydroxide aqueous solution, stirring for polycondensation reaction, monitoring the viscosity on line, adding a silicon phosphate terminating agent before reaching the target viscosity, continuing to react for 5-50 minutes, vacuumizing, decompressing and distilling to remove low-boiling-point substances to obtain alpha, omega-dihydroxy polydimethylsiloxane;
s3, weighing methyltrimethoxysilane and hexamethyldisiloxane in a certain proportion, adding alpha and omega-dihydroxy polydimethylsiloxane, fully stirring and mixing for 30 minutes at normal temperature, and heating to 50-60 ℃;
s4, after the temperature is raised to the specified temperature, adding a phosphazene catalyst, and continuously stirring for reaction for 2-3 hours;
s5, adding water for hydrolysis after full reaction, carrying out hydrolysis reaction for 2-3 hours, and then adding dimethyl dimethoxy silane for rearrangement and end sealing again;
s6, after the full reaction is finished, adding a terminator, and stirring to terminate the reaction;
and S7, continuously heating to 150-160 ℃, vacuumizing and removing low volatile matters to obtain the T-type alkoxy silicone oil.
Preferably, in the step S1, the mass ratio of DMC, hexamethyldisiloxane to phosphoric acid is (60-80): 5-15): 10-20, and the stirring speed is 200-400r/min.
Preferably, in the step S2, the mass concentration of the aqueous solution of potassium hydroxide is 10%, the mass ratio of the linear body, the aqueous solution of potassium hydroxide and the silicon phosphate terminating agent is 40000 (1.5-2.0), and the target viscosity is 1000-80000 mPas.
Preferably, the mass ratio of the methyltrimethoxysilane to the hexamethyldisiloxane in the step S3 is (1.0-3.0): (0.5-1.5), and the stirring speed during the stirring reaction is 400-800r/min.
Preferably, the proportion of the phosphazene added in the step S4 is 15ppm to 20ppm, the temperature is raised to 50 ℃ to 60 ℃, and a phosphazene catalyst is added.
Preferably, the amount of water added in the hydrolysis reaction in the step S5 is 2.5 to 3.5 times of that of the methyltrimethoxysilane.
Preferably, the dimethyldimethoxysilane added in the rearrangement reaction in the step S5 is 1.5-2.5 times of the methyltrimethoxysilane.
Preferably, the reaction is continued for 1 hour after the addition of the terminator in the step S6.
Preferably, the temperature in the step S7 is raised to 150-160 ℃ and then the reduction is carried out for 2.0-3.0 hours.
The prepared T-type alkoxy silicone oil is applied to room temperature vulcanized silicone rubber as a plasticizer, the addition amount of the T-type alkoxy silicone oil is less than that of other plasticizers, the mechanical property is greatly improved, and deep curing is better.
Therefore, the preparation method of the T-type alkoxy silicone oil and the application of the T-type alkoxy silicone oil in room-temperature vulcanized silicone rubber have the following beneficial effects:
(1) According to the invention, methyltrimethoxysilane and hexamethyldisiloxane are used as end sealing agents, phosphazene is used as a catalyst, a linear body is used as a basic raw material to prepare alpha-dihydroxy polydimethylsiloxane, omega-dihydroxy polydimethylsiloxane is obtained, and then the hydrolysis is carried out, and then the functional material is used for carrying out modified end sealing on T-type polydimethylsiloxane, so that the T-type alkoxy end-blocked polydimethylsiloxane is prepared.
(2) T-type alkoxy silicone oil is used as a plasticizer, and the T-type alkoxy silicone oil has an alkoxy active functional group which can react with substances in the silicone rubber, cannot be dissociated in the silicone rubber, and is better in deep curing. And secondly, the T-shaped structure can form a net structure in the cross-linking process, so that the mechanical property of the room-temperature vulcanized silicone rubber is greatly improved.
The technical solution of the present invention is further described in detail by the following examples.
Detailed Description
The invention provides a preparation method of T-type alkoxy silicone oil, which comprises the following steps:
s1, heating DMC and hexamethyldisiloxane to 160-180 ℃, dropwise adding phosphoric acid, stirring for 6-8 hours, refluxing for dewatering, and obtaining a silicophosphate terminator, wherein the stirring speed is 200-400 r/min; wherein the mass ratio of DMC, hexamethyldisiloxane to phosphoric acid is (60-80): (5-15): 10-20).
S2, heating the linear body to 130-150 ℃, adding a potassium hydroxide aqueous solution, stirring for polycondensation reaction, monitoring the viscosity on line, adding a silicon phosphate terminating agent before the target viscosity is 1000-80000mPa & S, continuing to react for 5-50 minutes, vacuumizing, decompressing and distilling to remove low-boiling-point substances to obtain alpha, omega-dihydroxy polydimethylsiloxane; wherein the mass concentration of the potassium hydroxide aqueous solution is 10 percent, and the mass ratio of the linear body, the potassium hydroxide aqueous solution and the silicon phosphate terminator is 40000 (1.5-2.0).
S3, weighing methyltrimethoxysilane and hexamethyldisiloxane in a certain proportion, adding alpha and omega-dihydroxy polydimethylsiloxane, fully stirring and mixing for 30 minutes at normal temperature, wherein the stirring speed is 400-800r/min, and heating to 50-60 ℃; wherein the mass ratio of the methyltrimethoxysilane to the hexamethyldisiloxane is (1.0-3.0) to (0.5-1.5).
S4, after the temperature is raised to 50-60 ℃, 15-20 ppm of phosphazene catalyst is added, and the mixture is continuously stirred and reacts for 2-3 hours;
and S5, after full reaction, adding water for hydrolysis, wherein the added water amount is 2.5-3.5 times of that of the methyltrimethoxysilane, performing hydrolysis reaction for 2-3 hours, then adding the dimethyldimethoxysilane for rearrangement end capping again, and the added dimethyldimethoxysilane is 1.5-2.5 times of that of the methyltrimethoxysilane.
S6, after the full reaction is finished, adding a terminator, stirring to terminate the reaction, and continuing the reaction for 1 hour;
and S7, continuously heating to 150-160 ℃, vacuumizing to remove low volatile matter for 2.0-3.0 hours, and obtaining the T-type alkoxy silicone oil.
The prepared T-type alkoxy silicone oil is applied to room temperature vulcanized silicone rubber as a plasticizer, the addition amount of the T-type alkoxy silicone oil is less than that of other plasticizers, the mechanical property is greatly improved, and deep curing is better.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
The preparation method comprises the following steps of preparing T-type alkoxy silicone oil and the application of the T-type alkoxy silicone oil as a plasticizer in room-temperature vulcanized silicone rubber:
the preparation method of the T-type alkoxy silicone oil comprises the following steps:
(1) Heating DMC and hexamethyldisiloxane to 170 ℃, dropwise adding phosphoric acid, stirring at the speed of 300r/min for 7 hours, refluxing and removing water to obtain a silicophosphate terminator, wherein the mass ratio of DMC to hexamethyldisiloxane to phosphoric acid is 70;
(2) Heating the linear body to 150 ℃, adding a potassium hydroxide aqueous solution with the mass concentration of 10%, stirring for polycondensation reaction, monitoring the viscosity on line, adding the silicon phosphate terminating agent obtained in the step (1) before the target viscosity is 1000mPa & s, continuing to react for 50 minutes, vacuumizing, decompressing and distilling to remove low-boiling-point substances to obtain hydroxyl silicone oil, wherein the mass ratio of the linear body to the potassium hydroxide aqueous solution to the silicon phosphate terminating agent is 40000;
(3) Adding 2 parts of methyltrimethoxysilane and 1.7 parts of hexamethyldisiloxane into a 100 parts of alpha, omega-dihydroxy polydimethylsiloxane reaction kettle, fully stirring and mixing for 30 minutes at normal temperature, and heating to 50-60 ℃;
(4) After the temperature reaches 60 ℃, adding 20ppm of self-made phosphazene catalyst, and continuously stirring for reaction for 3 hours;
(5) After the rearrangement reaction is finished, adding 2.0 parts of water into the reaction kettle for hydrolysis, and carrying out hydrolysis reaction for 2 hours; after the reaction is finished, continuously adding 6.5 parts of dimethyldimethoxysilane, and then continuously carrying out rearrangement reaction;
(6) After the full reaction is finished, adding 60ppm of terminator into the reaction kettle, and continuing stirring for 1 hour;
(7) Continuously heating to 150 ℃, and vacuumizing to remove volatile matters. Vacuumizing for 2 hours;
(8) And (3) adding the T-type alkoxy silicone oil prepared in the step (7) into room-temperature vulcanized silicone rubber as a plasticizer to prepare the room-temperature vulcanized silicone rubber.
Comparative example 1
The amounts of dimethyl silicone oil and T-type alkoxy silicone oil added as plasticizers are shown in Table 1, and the amounts of the rest are the same as those in example 1.
Comparative example 2
The amount of the plasticizer used was the same as that in example 1 except that the amount of the plasticizer used was dimethyl silicone oil shown in Table 1.
The room temperature vulcanized silicone rubbers obtained in example 1, comparative document 1, and comparative document 2 were subjected to a performance test.
The stability test method comprises the following steps: the mechanical properties of each product after 3 days and after 7 days were measured, respectively, and the test results are shown in tables 2 and 3.
Table 1 shows the parts of room temperature vulcanized silicone rubber added
| Material(s) | Example 1 | Comparative example 1 | Comparative example 2 |
| Polymer and method of making same | 100 | 100 | 100 |
| Dimethyl silicone oil | 0 | 10 | 30 |
| T-type alkoxy silicone oil | 30 | 20 | 0 |
| Gas silicon | 15 | 15 | 15 |
| Methyltrimethoxysilane | 3 | 3 | 3 |
| KH-792 | 1 | 1 | 1 |
| Catalyst and process for preparing same | 0.3 | 0.3 | 0.3 |
Mechanical Properties after 3 days of curing as shown in Table 2
| 3 days of detection | Example 1 | Comparative example 1 | Comparative example 2 |
| Strength of | 1.51 | 1.18 | 0.89 |
| Elongation percentage | 378 | 374 | 299 |
| 100% modulus | 0.2559 | 0.2379 | 0.1993 |
Mechanical properties after 7 days of curing as shown in Table 3
| 7 days of detection | Example 1 | Comparative example 1 | Comparative example 2 |
| Strength of | 2.11 | 1.35 | 0.96 |
| Elongation percentage | 452 | 399 | 275 |
| 100% modulus | 0.3004 | 0.2206 | 0.2665 |
| Hardness of | 21 | 19 | 17 |
As can be seen from Table 1, in inventive example 1, the room temperature vulcanized silicone rubber was prepared entirely using T-type alkoxy silicone oil as a plasticizer; in contrast, in comparative example 1, part of T-type alkoxy silicone oil and dimethyl silicone oil were used as plasticizers; while comparative example 2 used all dimethicone as the plasticizer. As can be seen from Table 2, the mechanical properties of the three formulations have been pulled apart after three days of curing of the room temperature vulcanizable silicone rubber prepared. The T-type alkoxy silicone oil is used as a plasticizer, and the mechanical property is improved. As can be seen from Table 3, the mechanical properties of the prepared room temperature vulcanized silicone rubber are greatly improved by using T-type alkoxy silicone oil as a plasticizer after curing for 7 days.
Therefore, the preparation method of the T-type alkoxy silicone oil and the application of the T-type alkoxy silicone oil in room-temperature vulcanized silicone rubber solve the problem of silicone oil precipitation, improve the storage stability and greatly improve the mechanical properties of the silicone rubber.
Finally, it should be noted that: the above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention is described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the invention without departing from the spirit and scope of the invention.
Claims (10)
1. A preparation method of T-type alkoxy silicone oil is characterized by comprising the following steps:
s1, mixing DMC and hexamethyldisiloxane, heating to 160-180 ℃, dropwise adding phosphoric acid, stirring for 6-8 hours, refluxing and removing water to obtain a silicophosphate terminator;
s2, heating the linear body to 130-150 ℃, adding a potassium hydroxide aqueous solution, stirring for polycondensation reaction, monitoring the viscosity on line, adding a silicon phosphate terminating agent before reaching the target viscosity, continuing to react for 5-50 minutes, vacuumizing, decompressing and distilling to remove low-boiling-point substances to obtain alpha, omega-dihydroxy polydimethylsiloxane;
s3, weighing methyltrimethoxysilane and hexamethyldisiloxane in a certain proportion, adding alpha and omega-dihydroxy polydimethylsiloxane, fully stirring and mixing for 30 minutes at normal temperature, and heating to 50-60 ℃;
s4, after the temperature is raised to the specified temperature, adding a phosphazene catalyst, and continuously stirring and reacting for 2-3 hours;
s5, adding water for hydrolysis after full reaction, carrying out hydrolysis reaction for 2-3 hours, and then adding dimethyl dimethoxy silane for rearrangement and end sealing again;
s6, after the full reaction is finished, adding a terminator, and stirring to terminate the reaction;
and S7, continuously heating to 150-160 ℃, vacuumizing to remove low volatile matters, and obtaining the T-type alkoxy silicone oil.
2. The method for preparing T-type alkoxy silicone oil according to claim 1, wherein the method comprises the following steps: in the step S1, the mass ratio of DMC, hexamethyldisiloxane to phosphoric acid is (60-80): 5-15): 10-20, and the stirring speed is 200-400r/min.
3. The method for preparing T-type alkoxy silicone oil according to claim 1, wherein the method comprises the following steps: in the step S2, the mass concentration of the potassium hydroxide aqueous solution is 10%, the mass ratio of the linear body to the potassium hydroxide aqueous solution to the silicophosphate terminator is 40000 (1.5-2.0), and the target viscosity is 1000-80000 mPas.
4. The method for preparing T-type alkoxy silicone oil according to claim 1, wherein the method comprises the following steps: in the step S3, the mass ratio of the methyltrimethoxysilane to the hexamethyldisiloxane is (1.0-3.0) to (0.5-1.5), and the stirring speed during the stirring reaction is 400-800r/min.
5. The method for preparing T-type alkoxy silicone oil according to claim 1, wherein the method comprises the following steps: and (3) the proportion of the phosphazene added in the step (S4) is 15ppm-20ppm, the temperature is raised to 50 ℃ -60 ℃, and a phosphazene catalyst is added.
6. The method for preparing T-type alkoxy silicone oil according to claim 1, wherein the method comprises the following steps: the water amount added in the hydrolysis reaction in the step S5 is 2.5 to 3.5 times of that of the methyltrimethoxysilane.
7. The method for preparing T-type alkoxy silicone oil according to claim 1, wherein the method comprises the following steps: the dimethyl dimethoxy silane added in the rearrangement reaction in the step S5 is 1.5 to 2.5 times of the methyl trimethoxy silane.
8. The method for preparing T-type alkoxy silicone oil according to claim 1, wherein the method comprises the following steps: and (5) after adding the terminating agent in the step S6, continuing the reaction for 1 hour.
9. The method for preparing T-type alkoxy silicone oil according to claim 1, wherein the method comprises the following steps: and after the temperature is raised to 150-160 ℃ in the step S7, the reduction is carried out for 2.0-3.0 hours.
10. Use of a T-type alkoxy silicone oil according to any one of claims 1 to 9 as a plasticizer in room temperature vulcanizing silicone rubber.
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| CN103044920A (en) * | 2011-12-07 | 2013-04-17 | 北京天山新材料技术股份有限公司 | One-component room temperature vulcanized and methyl alcohol-removed silicon rubber of starting-resistant engine oil and preparation method of rubber |
| CN104151558A (en) * | 2014-08-08 | 2014-11-19 | 广东省工业技术研究院(广州有色金属研究院) | Preparation method for MDTQ type methyl phenyl vinyl silicone resin |
| CN113512197A (en) * | 2021-07-30 | 2021-10-19 | 新纳奇材料科技江苏有限公司 | Preparation method of alkoxy-terminated polydimethylsiloxane |
| CN113652193A (en) * | 2021-08-30 | 2021-11-16 | 江苏矽时代材料科技有限公司 | High-strength flowing silica gel and preparation method and application thereof |
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