CN111320755A - Polytitanosiloxane and preparation method thereof - Google Patents
Polytitanosiloxane and preparation method thereof Download PDFInfo
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- CN111320755A CN111320755A CN202010329975.4A CN202010329975A CN111320755A CN 111320755 A CN111320755 A CN 111320755A CN 202010329975 A CN202010329975 A CN 202010329975A CN 111320755 A CN111320755 A CN 111320755A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- -1 polysiloxane Polymers 0.000 claims abstract description 37
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 31
- 239000010936 titanium Substances 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000004821 distillation Methods 0.000 claims abstract description 21
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 19
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 16
- 239000000413 hydrolysate Substances 0.000 claims abstract description 15
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 11
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 12
- 230000003301 hydrolyzing effect Effects 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 2
- 229940083037 simethicone Drugs 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 7
- 238000009833 condensation Methods 0.000 abstract description 5
- 230000005494 condensation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 10
- 229920002545 silicone oil Polymers 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 6
- 238000009776 industrial production Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 239000011344 liquid material Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 description 1
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
- C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
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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)
- Silicon Polymers (AREA)
Abstract
The invention provides a titanium polysiloxane and a preparation method thereof, wherein the preparation method comprises the following steps: a) dropwise adding tetrabutyl titanate into the hydrolysate of the reaction raw material, and performing hydrolysis reaction to obtain an oligomer; the reaction raw material is dimethyl diethoxy silane and/or dimethyl dichlorosilane; b) and c) carrying out polymerization reaction on the oligomer obtained in the step a), a dimethyl cyclosiloxane mixture and a methyl silicone oil distillation light component under the action of a catalyst to obtain the titanium polysiloxane. Compared with the prior art, the titanium-containing polysiloxane provided by the invention is prepared by taking dimethyl diethoxy silane and/or dimethyl dichlorosilane as raw materials, is low in cost and adopting a specific preparation method, has a structure shown in a formula (I), is a colorless transparent liquid, and has excellent high-temperature resistance and low-temperature performance. Experimental results show that the initial oxidation temperature of the poly-titanium siloxane provided by the invention is above 312 ℃, the condensation point is below-52 ℃, and the poly-titanium siloxane has good industrial application prospects.
Description
Technical Field
The invention relates to the technical field of organic synthesis, in particular to a titanium polysiloxane and a preparation method thereof.
Background
Polysiloxane (silicone oil) is an organic polymer formed by combining an inorganic silica main chain and an organic branched chain, has more excellent heat resistance than other organic polymers, is an ideal high-temperature-resistant liquid material, and is widely applied to the high-temperature fields of heat conduction, adhesive transmission, demolding and the like. With the continuous advance of industrial development, the application field of high-temperature-resistant silicone oil products will continue to expand, and besides the traditional industry, the new development fields such as solar photo-thermal power generation and the like will also increase the use requirements on high-temperature heat-conducting silicone oil, and the requirements on the thermal stability, the service life and the like of the silicone oil will be further improved.
At present, the common polydimethylsiloxane (methyl silicone oil) product in China can only be used in an open system at the temperature of-50-180 ℃, when the use temperature exceeds 200 ℃, the oxidation reaction is easy to generate gel, and the service life is greatly shortened. The polymethylphenylsiloxane (methyl phenyl silicone oil) introduces phenyl in molecules, so that the high temperature resistance is improved compared with that of the methyl silicone oil, but the condensation point is correspondingly improved (> -50 ℃), the low-temperature use requirement of partial working conditions cannot be met, and the production cost is higher. On the other hand, the special molecular structure of polysiloxane causes poor solubility to additives such as high-temperature antioxidant, and homogeneous transparent silicone oil products are difficult to obtain after the additives are added. Therefore, how to provide a polysiloxane product with excellent high temperature resistance, good low temperature resistance and low cost for the market becomes a technical problem to be solved urgently by the technical personnel in the field at present.
Disclosure of Invention
In view of the above, the present invention provides a titanium polysiloxane and a preparation method thereof, and the titanium polysiloxane provided by the present invention has excellent high temperature resistance and low temperature resistance, and is low in cost.
The invention provides a titanium polysiloxane, which has a structure shown in a formula (I):
wherein m + n is 50-400.
The invention also provides a preparation method of the titanium polysiloxane, which comprises the following steps:
a) dropwise adding tetrabutyl titanate into the hydrolysate of the reaction raw material, and performing hydrolysis reaction to obtain an oligomer; the reaction raw material is dimethyl diethoxy silane and/or dimethyl dichlorosilane;
b) and c) carrying out polymerization reaction on the oligomer obtained in the step a), a dimethyl cyclosiloxane mixture and a methyl silicone oil distillation light component under the action of a catalyst to obtain the titanium polysiloxane.
Preferably, the hydrolysate of the reaction raw materials in the step a) is obtained by hydrolyzing the reaction raw materials at 30-80 ℃.
Preferably, the mass ratio of the reaction raw materials in the hydrolysate of the reaction raw materials in the step a) to the tetrabutyl titanate is 1: (0.1-0.2).
Preferably, the speed of dropwise adding tetrabutyl titanate in the step a) is 2mL/min to 5 mL/min.
Preferably, the temperature of the hydrolysis reaction in step a) is 30 ℃ to 80 ℃.
Preferably, the mass ratio of the oligomer, the dimethyl cyclosiloxane mixture and the methyl silicone oil distillation light component in the step b) is 1: (1-10): (0.01-0.04).
Preferably, the catalyst in the step b) is concentrated sulfuric acid with the mass fraction of 70-98%.
Preferably, the temperature of the polymerization reaction in the step b) is 20-30 ℃ and the time is 8-10 h.
Preferably, after the polymerization reaction in step b), the method further comprises:
standing to remove the catalyst, washing the polymer to be neutral, distilling, and removing light fractions to obtain the titanium polysiloxane;
the distillation temperature is 300-310 ℃, the pressure is-0.1 MPa to-0.095 MPa, and the time is 1.5h to 2.5 h.
The invention provides a titanium polysiloxane and a preparation method thereof, wherein the preparation method comprises the following steps: a) dropwise adding tetrabutyl titanate into the hydrolysate of the reaction raw material, and performing hydrolysis reaction to obtain an oligomer; the reaction raw material is dimethyl diethoxy silane and/or dimethyl dichlorosilane; b) and c) carrying out polymerization reaction on the oligomer obtained in the step a), a dimethyl cyclosiloxane mixture and a methyl silicone oil distillation light component under the action of a catalyst to obtain the titanium polysiloxane. Compared with the prior art, the titanium-containing polysiloxane provided by the invention is prepared by taking dimethyl diethoxy silane and/or dimethyl dichlorosilane as raw materials, is low in cost and adopting a specific preparation method, has a structure shown in a formula (I), is a colorless transparent liquid, and has excellent high-temperature resistance and low-temperature performance. Experimental results show that the poly-titanium siloxane provided by the invention is colorless transparent liquid, the initial oxidation temperature is above 312 ℃, the condensation point is below-52 ℃, and the poly-titanium siloxane has good industrial application prospect.
In addition, the preparation method provided by the invention has the advantages of simple process, mild conditions and easiness in operation, and is suitable for large-scale industrial production.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The invention provides a titanium polysiloxane, which has a structure shown in a formula (I):
wherein m + n is 50 to 400, preferably 100 to 300, and more preferably 150 to 200.
The poly titanium siloxane provided by the invention has a structure shown in a formula (I), is colorless transparent liquid, and has excellent high temperature resistance and low temperature resistance; compared with common silicone oil, the silicone oil has more excellent high-temperature resistance, the maximum use temperature can be increased by 50 ℃, and the low-temperature performance is equivalent to that of polydimethylsiloxane; the silicone oil can be used in the traditional fields of heat conduction, viscous transmission, demoulding and the like with higher requirements on the thermal stability, the service life and the like of silicone oil and the emerging development fields of solar photo-thermal power generation and the like.
The invention also provides a preparation method of the titanium polysiloxane, which comprises the following steps:
a) dropwise adding tetrabutyl titanate into the hydrolysate of the reaction raw material, and performing hydrolysis reaction to obtain an oligomer; the reaction raw material is dimethyl diethoxy silane and/or dimethyl dichlorosilane;
b) and c) carrying out polymerization reaction on the oligomer obtained in the step a), a dimethyl cyclosiloxane mixture and a methyl silicone oil distillation light component under the action of a catalyst to obtain the titanium polysiloxane.
The method comprises the steps of firstly, dropwise adding tetrabutyl titanate into hydrolysate of reaction raw materials, and carrying out hydrolysis reaction to obtain the oligomer. In the present invention, the reaction raw material is dimethyldiethoxysilane and/or dimethyldichlorosilane, and dimethyldiethoxysilane is preferred. The present invention is not particularly limited in terms of the source of the reaction raw materials, and commercially available products of the above-mentioned dimethyldiethoxysilane and dimethyldichlorosilane known to those skilled in the art may be used.
In the present invention, the hydrolysate of the reaction raw materials is preferably obtained by hydrolyzing the reaction raw materials at 30 to 80 ℃, and more preferably obtained by hydrolyzing the reaction raw materials at 50 ℃.
In the present invention, the mass ratio of the reaction raw material to tetrabutyl titanate in the hydrolysate of the reaction raw material is preferably 1: (0.1 to 0.2), more preferably 1: (0.13-0.18). The source of the tetrabutyl titanate is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the present invention, the dropping rate of tetrabutyl titanate is preferably 2mL/min to 5mL/min, and more preferably 3mL/min to 4 mL/min.
In the present invention, the temperature of the hydrolysis reaction is preferably 30 to 80 ℃, and more preferably 50 to 60 ℃.
After the oligomer is obtained, the obtained oligomer, a dimethyl cyclosiloxane mixture and a methyl silicone oil distillation light component are subjected to polymerization reaction under the action of a catalyst to obtain the polytitanium siloxane. In the present invention, the mass ratio of the oligomer, the dimethylcyclosiloxane mixture and the simethicone distillation light component is preferably 1: (1-10): (0.01 to 0.04), more preferably 1: (5-8): (0.02-0.03).
In the invention, the catalyst is preferably concentrated sulfuric acid with the mass fraction of 70-98%, and more preferably concentrated sulfuric acid with the mass fraction of 90-98%. In the present invention, the amount of the catalyst added is preferably 1 wt% to 10 wt%, more preferably 5 wt% to 6 wt% of the charged amount.
In the present invention, the temperature of the polymerization reaction is preferably 20 to 30 ℃, more preferably 25 ℃; the time for the polymerization reaction is preferably 8 to 10 hours, more preferably 9 hours.
In the present invention, after the polymerization reaction, it is preferable to further include:
standing to remove the catalyst, washing the polymer to be neutral, distilling, and removing light fractions to obtain the titanium polysiloxane. In the present invention, the temperature of the distillation is preferably 300 ℃ to 310 ℃; the distillation pressure is preferably-0.1 MPa to-0.095 MPa, and more preferably-0.098 MPa; the distillation time is preferably 1.5h to 2.5h, more preferably 2 h.
The titanium-containing polysiloxane provided by the invention takes dimethyl diethoxysilane and/or dimethyl dichlorosilane as raw materials, has low cost, simple process, mild condition and easy operation, and is suitable for large-scale industrial production; the product prepared by the preparation method has the structure shown in the formula (I), is colorless transparent liquid, and has excellent high-temperature resistance and low-temperature resistance.
The invention provides a titanium polysiloxane and a preparation method thereof, wherein the preparation method comprises the following steps: a) dropwise adding tetrabutyl titanate into the hydrolysate of the reaction raw material, and performing hydrolysis reaction to obtain an oligomer; the reaction raw material is dimethyl diethoxy silane and/or dimethyl dichlorosilane; b) and c) carrying out polymerization reaction on the oligomer obtained in the step a), a dimethyl cyclosiloxane mixture and a methyl silicone oil distillation light component under the action of a catalyst to obtain the titanium polysiloxane. Compared with the prior art, the titanium-containing polysiloxane provided by the invention is prepared by taking dimethyl diethoxy silane and/or dimethyl dichlorosilane as raw materials, is low in cost and adopting a specific preparation method, has a structure shown in a formula (I), is a colorless transparent liquid, and has excellent high-temperature resistance and low-temperature performance. Experimental results show that the poly-titanium siloxane provided by the invention is colorless transparent liquid, the initial oxidation temperature is above 312 ℃, the condensation point is below-52 ℃, and the poly-titanium siloxane has good industrial application prospect.
In addition, the preparation method provided by the invention has the advantages of simple process, mild conditions and easiness in operation, and is suitable for large-scale industrial production.
To further illustrate the present invention, the following examples are provided for illustration.
Examples
Raw materials: dimethyl diethoxy silane or dimethyl dichlorosilane, tetrabutyl titanate, dimethyl cyclosiloxane mixture (DMC), and methyl silicone oil distillation light component (polymethyl siloxane mixture with molecular weight of 162 g/mol-1000 g/mol).
The preparation method comprises the following steps:
(1) hydrolyzing 200g of dimethyl diethoxysilane at 50 ℃ to obtain hydrolysate;
(2) and (2) dropwise adding tetrabutyl titanate into the hydrolysate obtained in the step (1), and continuously hydrolyzing at 50 ℃ to obtain the oligomer.
(3) Polymerizing the oligomer obtained in the step (2), a dimethyl cyclosiloxane mixture (DMC) and a methyl silicone oil distillation light component for 9 hours at 25 ℃ under the catalysis of concentrated sulfuric acid with the mass fraction of 98% (the dosage is 5 wt%) and standing to remove the concentrated sulfuric acid after polymerization, washing the polymer to be neutral, distilling and removing the light fraction to obtain the titanium polysiloxane.
According to the preparation method, the reaction conditions are changed, and products of different examples and comparative examples are prepared, and the specific table is shown in table 1.
TABLE 1 data for different reaction conditions
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Hydrolysis temperature of | 50 | 50 | 50 | — | 50 | 50 |
| The amount of tetrabutyl titanate used% | 13 | 18 | 13 | — | 30 | 13 |
| Dropping speed, mL/min | 3 | 3 | 4 | — | 3 | 10 |
| Polymerization charge ratio | 1:5:0.03 | 1:5:0.03 | 1:5:0.03 | 0:6:0.03 | 1:5:0.03 | 1:5:0.03 |
| Distillation temperature, C | 300～310 | 300～310 | 300～310 | 300～310 | 300～310 | 300～310 |
| Distillation pressure, MPa | -0.098 | -0.098 | -0.098 | -0.098 | -0.098 | -0.098 |
| Distillation time h | 2 | 2 | 2 | 2 | 2 | 2 |
In table 1, the amount (%) of tetrabutyl titanate used is the ratio of the mass of tetrabutyl titanate to the mass of dimethyldiethoxysilane; the polymer charge ratio refers to the mass ratio of the oligomer, the Dimethylcyclosiloxane Mixture (DMC) and the methyl silicone oil distillation light component.
The products obtained in examples 1 to 3 and comparative examples 1 to 3 were tested for their respective properties, and the results are shown in table 2.
TABLE 2 Performance data of the products obtained in examples 1 to 3 and comparative examples 1 to 3
As can be seen from Table 2, the polytitanium siloxane provided by the invention has good high temperature resistance as a liquid material, and has low condensation point and good industrial application prospect.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A polytitanium siloxane having the structure of formula (I):
wherein m + n is 50-400.
2. A method for preparing the polytitanium siloxane of claim 1, comprising the steps of:
a) dropwise adding tetrabutyl titanate into the hydrolysate of the reaction raw material, and performing hydrolysis reaction to obtain an oligomer; the reaction raw material is dimethyl diethoxy silane and/or dimethyl dichlorosilane;
b) and c) carrying out polymerization reaction on the oligomer obtained in the step a), a dimethyl cyclosiloxane mixture and a methyl silicone oil distillation light component under the action of a catalyst to obtain the titanium polysiloxane.
3. The method according to claim 2, wherein the hydrolysate of the reaction raw material in the step a) is obtained by hydrolyzing the reaction raw material at 30 to 80 ℃.
4. The preparation method according to claim 2, wherein the mass ratio of the reaction raw materials to tetrabutyl titanate in the hydrolysate of the reaction raw materials in the step a) is 1: (0.1-0.2).
5. The method according to claim 2, wherein the dropping of tetrabutyl titanate in step a) is at a rate of 2 to 5 mL/min.
6. The method according to claim 2, wherein the temperature of the hydrolysis reaction in step a) is 30 to 80 ℃.
7. The method according to claim 2, wherein the mass ratio of the oligomer, the dimethylcyclosiloxane mixture and the simethicone distillation light component in step b) is 1: (1-10): (0.01-0.04).
8. The preparation method according to claim 2, wherein the catalyst in step b) is concentrated sulfuric acid with a mass fraction of 70-98%.
9. The method according to claim 2, wherein the polymerization in step b) is carried out at a temperature of 20 ℃ to 30 ℃ for a time of 8h to 10 h.
10. The method according to any one of claims 2 to 9, further comprising, after the polymerization reaction in step b):
standing to remove the catalyst, washing the polymer to be neutral, distilling, and removing light fractions to obtain the titanium polysiloxane;
the distillation temperature is 300-310 ℃, the pressure is-0.1 MPa to-0.095 MPa, and the time is 1.5h to 2.5 h.
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| CN109988308A (en) * | 2019-04-26 | 2019-07-09 | 中国石油化工股份有限公司 | A kind of modified silicon oil and preparation method thereof |
| CN112143240A (en) * | 2020-08-31 | 2020-12-29 | 三联泵业股份有限公司 | Preparation method of lining material of slurry pump |
| CN114957671A (en) * | 2022-04-26 | 2022-08-30 | 中国石油化工股份有限公司 | High-temperature methyl silicone oil and preparation method and application thereof |
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Application publication date: 20200623 |