CN113896893A - Preparation method of high-conversion low-cycle-content simethicone - Google Patents
Preparation method of high-conversion low-cycle-content simethicone Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 48
- 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 title claims description 18
- 229940083037 simethicone Drugs 0.000 title claims description 18
- 238000002360 preparation method Methods 0.000 title description 4
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- UXJHQBVRZUANLK-UHFFFAOYSA-N azanylidyne(dichloro)-$l^{5}-phosphane Chemical compound ClP(Cl)#N UXJHQBVRZUANLK-UHFFFAOYSA-N 0.000 claims abstract description 29
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 17
- 229920002545 silicone oil Polymers 0.000 claims abstract description 17
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 12
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 10
- 239000000413 hydrolysate Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 claims description 8
- 108010009736 Protein Hydrolysates Proteins 0.000 claims description 4
- 239000002981 blocking agent Substances 0.000 claims description 3
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 3
- 238000010189 synthetic method Methods 0.000 claims description 3
- YFCGDEUVHLPRCZ-UHFFFAOYSA-N [dimethyl(trimethylsilyloxy)silyl]oxy-dimethyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C YFCGDEUVHLPRCZ-UHFFFAOYSA-N 0.000 claims description 2
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- -1 polysiloxane Polymers 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 229920001296 polysiloxane Polymers 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C08G77/08—Preparatory processes characterised by the catalysts used
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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 relates to the technical field of polysiloxane synthesis, and provides a method for synthesizing dimethyl silicone oil with high conversion rate and low cyclic body content, which adopts the following technical scheme: taking a high linear siloxane hydrolysate as a raw material, adding an end-capping agent and a linear phosphonitrile chloride catalyst, reacting for 1-4 hours at the temperature of 70-150 ℃ under a negative pressure condition, adding hexamethyldisilazane to neutralize the catalyst after the reaction is finished, and removing low content of the product to obtain the dimethyl silicone oil. The catalytic system used in the invention has high activity, the primary conversion rate can reach more than 99%, the utilization rate of raw materials is extremely high, no obvious cyclosiloxane is generated in the reaction process, the energy consumption for removing is greatly reduced, and the final product has excellent performance.
Description
Technical Field
The invention relates to a synthetic method of dimethyl silicone oil with high conversion rate and low cyclic body content, belonging to the technical field of polysiloxane synthesis.
Background
The simethicone is colorless, tasteless and non-volatile transparent liquid, and has the advantages of stable chemical property, high boiling point, low freezing point and wide temperature range existing as liquid. Has excellent heat resistance, weather resistance, physiological inertia, electric insulation, smaller surface tension, low viscosity-temperature coefficient and higher compression resistance. The polymer is widely applied to various departments of national economy such as machinery, electricity, textile, coating, medicine and the like, and is a high molecular polymer with large development scale and early industrialization. With the development of industries such as medical treatment, food, electronic information and the like, higher requirements are put on the performance of the methyl silicone oil, particularly, the low-volatile methyl silicone oil is a trend developed at present, and volatile siloxane ring bodies contained in the methyl silicone oil can be slowly released in the environment, so that the application of the methyl silicone oil in high-end fields is greatly limited.
At present, in domestic methyl silicone oil preparation, dimethyl siloxane mixed ring bodies (DMC) or octamethylcyclotetrasiloxane (D4) are mostly used as raw materials, tetramethyl ammonium hydroxide, potassium hydroxide, acidic resin, sulfuric acid and other acidic or basic catalysts are used for ring-opening balancing reaction, the molecular weight distribution of products is wide, 10-15% of volatile cyclosiloxane oligomers are generally contained, the volatile cyclosiloxane oligomers need to be removed through high-temperature removal, and the energy consumption in the process is large. Moreover, a small amount of residual ring bodies in the product are difficult to remove, and the expansion of downstream high-end products is influenced.
Linear body is used as raw material, linear phosphonitrile chloride is used as catalyst, methyl silicone oil is prepared by the polycondensation of silanol group, no obvious cyclosiloxane is generated in the reaction process, and the method is one of the main approaches for synthesizing low-volatility methyl silicone oil.
Disclosure of Invention
Aiming at the technical difficulties of low primary conversion rate of raw materials, generation of a large amount of volatile cyclosiloxane oligomers in the process of equilibration reaction, wide molecular weight distribution, difficulty in removing a small amount of residual rings and the like in the prior art, the invention provides a method for synthesizing simethicone with high conversion rate and low ring content.
In order to achieve the purpose, the invention adopts the following technical scheme:
a synthetic method of dimethyl silicone oil with high conversion rate and low cyclic body content comprises the following steps:
(1) adding the raw materials into a reaction kettle, and heating to 70-150 ℃;
(2) adding a blocking agent, uniformly stirring, adding a catalyst, and stirring and reacting for 1-4 hours at 70-150 ℃ under the negative pressure condition;
(3) recovering the system pressure to be normal pressure, adding hexamethyldisilazane and stirring for 0.5-4 h to neutralize the catalyst;
(4) heating to 180-240 ℃ for removing the low part, and cooling to obtain the product.
The raw material in the step (1) is dimethyl dichlorosilane hydrolysate, cyclosiloxane is removed to obtain high linear siloxane hydrolysate, the linear siloxane content is more than 90%, and the cyclosiloxane content is less than 10%.
The end-capping agent in the step (2) is one or a mixture of hexamethyldisiloxane (MM), octamethyltrisiloxane (MDM), decamethyltetrasiloxane (MDDM) and dimethyl silicone oil with the viscosity of 2-50 cSt.
The catalyst in the step (2) is linear phosphonitrile chloride or a linear phosphonitrile chloride solution (the solvent is ethyl acetate, toluene, tetrachloroethane or dimethyl silicone oil with the viscosity of 50-200 cSt), and the structural formula is as follows:
linear phosphonitrile chloride structures
And (3) in the step (2), the adding amount of the catalyst is 5-50 ppm calculated by linear phosphonitrile chloride.
And (3) in the step (2), the negative pressure is 0.02-0.1 MPa lower than the atmospheric pressure.
And (3) adding the hexamethyldisilazane in the step (3) by 1-10 times of the adding mass of the linear phosphonitrile chloride.
The low vacuum degree in the step (4) is minus 0.095 to minus 0.1 MPa.
In the step (4), the viscosity of the product is 50-200000 cp, the content of the ring body is less than 0.5%, and the preferable content of the ring body is less than 0.1%.
Compared with the prior art, the invention has the following beneficial effects:
(1) the raw material used in the invention is high-content linear siloxane hydrolysate obtained by removing cyclosiloxane from dimethyldichlorosilane hydrolysate, and compared with the raw material DMC or D4 used in the traditional process, the method has certain cost advantage.
(2) The raw materials of the invention do not contain free water, and a dehydration link is not needed, thereby saving equipment investment, simplifying production process and improving production efficiency.
(3) The method has the advantages of high utilization rate of raw materials, high primary conversion rate of over 99 percent, no obvious cyclosiloxane generated in the reaction process, low removal demand, reduction of material consumption and energy consumption and great cost advantage.
(4) The linear phosphonitrile chloride catalyst can promote the redistribution of polysiloxane without obvious cyclosiloxane generation, and has low content of low-molecular volatile cyclosiloxane and excellent product performance.
Drawings
FIG. 1 is a nuclear magnetic spectrum of a linear phosphonitrile chloride prepared in example 1.
Detailed Description
Example 1
Preparation method of linear phosphonitrile chloride catalyst
Adding 20.5g of phosphorus pentachloride, 2.6g of ammonium chloride and 100mL of tetrachloroethane into a 250mL three-neck flask, carrying out reflux reaction at 150 ℃ for 6h, cooling to room temperature after the reaction is finished, injecting the reaction solution into 100mL of petroleum ether, precipitating a precipitate, washing the precipitate for multiple times by using the petroleum ether, and removing residual petroleum ether under a reduced pressure condition to obtain the linear phosphonitrile chloride catalyst, wherein the structural formula is shown in the specification, and a nuclear magnetic spectrum is shown in figure 1.
Linear phosphonitrile chloride structures.
Example 2
Adding 300g of high linear siloxane hydrolysate into a three-neck flask, stirring and heating to 70 ℃, adding 40g of simethicone with the viscosity of 10cSt, stirring uniformly, and adding 0.7g of simethicone solution with the linear phosphonitrile chloride content of 2 wt%. (2 wt% means that the amount of linear phosphonitrile chloride in the catalyst solution is 2wt%, and examples 3-12 mean that only different amounts are added) is reacted for 3 hours under the negative pressure condition of 0.08MPa lower than the atmospheric pressure, the system pressure is recovered to the normal pressure after the reaction is finished, 0.1g of hexamethyldisilazane is added and stirred for 0.5 hour to neutralize the catalyst, the temperature is raised to 200 ℃ for removing the catalyst, and the finished product is obtained after cooling. The conversion rate was 98.21%, the viscosity was 14040cp, and the volatile matter was 0.21%.
Example 3
Adding 300g of high linear siloxane hydrolysate into a three-neck flask, stirring and heating to 70 ℃, adding 41g of dimethyl silicone oil with the viscosity of 2cSt, uniformly stirring, adding 0.84g of dimethyl silicone oil solution with the linear phosphonitrile chloride content of 2wt%, adjusting the system pressure to be 0.02Mpa lower than the atmospheric pressure for reaction for 2h, recovering the system pressure to the normal pressure after the reaction is finished, adding 0.134g of hexamethyldisilazane, stirring for 0.5h to neutralize the catalyst, heating to 200 ℃, removing the catalyst, cooling and filtering to obtain the finished product. The finished product has transparent appearance, 98.46 percent of conversion rate, 88cSt of viscosity and 0.14 percent of volatile component.
Example 4
Adding 300g of high linear siloxane hydrolysate into a three-neck flask, stirring and heating to 100 ℃, adding 45g of dimethyl silicone oil with the viscosity of 5cSt, uniformly stirring, adding 0.69g of dimethyl silicone oil solution with the linear phosphonitrile chloride content of 2wt%, reacting for 4h under the negative pressure condition of 0.09Mpa lower than the atmospheric pressure, recovering the system pressure to the normal pressure after the reaction is finished, adding 0.09g of hexamethyldisilazane, stirring for 1h to neutralize the catalyst, heating to 220 ℃, removing the catalyst, cooling and filtering to obtain the finished product. The finished product has transparent appearance, the conversion rate is 97.65 percent, the viscosity is 105cSt, and the volatile component is 0.09 percent.
Example 5
Adding 700g of high linear siloxane hydrolysate into a three-neck flask, stirring and heating to 110 ℃, adding 62g of dimethyl silicone oil with the viscosity of 5cSt, uniformly stirring, adding 0.28g of dimethyl silicone oil solution with the linear phosphonitrile chloride content of 5w%, reacting for 1h under the negative pressure condition of 0.095Mpa lower than the atmospheric pressure, adjusting the system temperature to 150 ℃, keeping the pressure at the normal pressure, continuing to react for 2h, recovering the system pressure to the normal pressure after the reaction is finished, adding 0.054g of hexamethyldisilazane, stirring for 1h to neutralize the catalyst, heating to 240 ℃, removing the catalyst, cooling and filtering to obtain the finished product. The finished product has transparent appearance, 99.02 percent of conversion rate, 263cSt of viscosity and 0.07 percent of volatile component.
Example 6
Adding 700g of high linear siloxane hydrolysate into a three-neck flask, stirring and heating to 85 ℃, adding 50g of dimethyl silicone oil with the viscosity of 5cSt, uniformly stirring, adding 0.89g of dimethyl silicone oil solution with the linear phosphonitrile chloride content of 2.1wt%, reacting for 4h under the negative pressure condition of 0.095Mpa lower than the atmospheric pressure, adding 0.16g of hexamethyldisilazane after the reaction is finished, stirring for 1h to neutralize the catalyst, heating to 230 ℃, removing the catalyst, cooling and filtering to obtain the finished product. The finished product has transparent appearance, 98.42 percent of conversion rate, 346cSt of viscosity and 0.072 percent of volatile component.
Example 7
Adding 3.5kg of high linear siloxane hydrolysate into a three-neck flask, stirring and heating to 100 ℃, adding 240g of dimethyl silicone oil with the viscosity of 5cSt, uniformly stirring, adding 0.0748g of linear phosphonitrile chloride, reacting for 2 hours under the negative pressure condition of 0.09Mpa lower than the atmospheric pressure, recovering the system pressure to the normal pressure after the reaction is finished, adding 0.45g of hexamethyldisilazane, stirring for 4 hours to neutralize the catalyst, heating to 230 ℃, removing the catalyst, cooling and filtering to obtain the finished product. The finished product has transparent appearance, 99.21 percent of conversion rate, 382cSt of viscosity and 0.11 percent of volatile component.
Example 8
Adding 300g of high linear siloxane hydrolysate into a three-neck flask, stirring and heating to 70 ℃, adding 17.3g of hexamethyldisiloxane (MM), stirring uniformly, adding 0.32g of dimethyl silicone oil solution with 2wt% of linear phosphonitrile chloride, adjusting the system pressure to be lower than the atmospheric pressure by 0.02Mpa, reacting for 2 hours, recovering the system pressure to the normal pressure after the reaction is finished, adding 0.058g of hexamethyldisilazane, stirring for 0.5 hour to neutralize the catalyst, heating to 200 ℃, removing the catalyst, and cooling to obtain the finished product. Viscosity 13760cp, volatile 0.34%.
Example 9
The procedure and procedure were as in example 6 except that the catalyst was 0.89g of an ethyl acetate solution containing 2.1wt% of linear phosphonitrile chloride, giving a transparent finished product with 98.44% conversion, 362cSt viscosity and 0.084% volatiles.
Example 10
The procedure and procedure were as in example 6 except that the catalyst was 0.89g of a toluene solution containing 2.1wt% of linear phosphonitrile chloride, giving a transparent finished product with a conversion of 97.68%, a viscosity of 359cSt and a volatile content of 0.088%.
Example 11
The procedure is as in example 6 except that the catalyst is 0.89g of tetrachloroethane solution containing 2.1wt% of linear phosphonitrile chloride, the product has transparent appearance, 99.08% conversion, 354cSt viscosity and 0.12% volatile component.
Example 12
The procedure is as in example 6 except that the catalyst is 10.1g of a 2wt% solution of simethicone in which linear phosphonitrile chloride is present, the product is transparent, has a conversion of 93.2%, a viscosity of 270cSt and a volatile content of 0.094%.
The above-described embodiments are merely preferred embodiments of the present invention, and should not be construed as limiting the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (10)
1. A synthetic method of dimethyl silicone oil with high conversion rate and low cyclic body content is characterized by comprising the following steps:
(1) adding the raw materials into a reaction kettle, and heating to 70-150 ℃;
(2) adding a blocking agent, uniformly stirring, adding a catalyst, and stirring and reacting for 1-4 hours at 70-150 ℃ under the negative pressure condition;
(3) recovering the system pressure to be normal pressure, adding hexamethyldisilazane and stirring for 0.5-4 h to neutralize the catalyst;
(4) heating to 180-240 ℃ for removing the low part, and cooling to obtain the product.
2. The method for synthesizing simethicone with high conversion rate and low cyclic body content as claimed in claim 1, wherein the raw material in step (1) is dimethyldichlorosilane hydrolysate which is subjected to cyclosiloxane removal to obtain high linear body siloxane hydrolysate, the linear body siloxane content is more than 90%, and the cyclosiloxane content is less than 10%.
3. The method for synthesizing simethicone with high conversion rate and low cycle content as claimed in claim 1, wherein the blocking agent in step (2) is one or more of hexamethyldisiloxane (MM), octamethyltrisiloxane (MDM), decamethyltetrasiloxane (MDDM), and simethicone with viscosity of 2-50 cSt.
4. The method for synthesizing simethicone with high conversion rate and low cycle content as claimed in claim 1, wherein the catalyst in step (2) is linear phosphonitrile chloride or a linear phosphonitrile chloride solution, and the structural formula is as follows:
5. the method for synthesizing simethicone with high conversion rate and low cyclic body content as claimed in claim 4, wherein the solvent used in the linear phosphonitrile chloride solution comprises any one of ethyl acetate, toluene, tetrachloroethane or simethicone with viscosity of 50-200 cSt.
6. The method for synthesizing simethicone with high conversion rate and low cyclic body content as claimed in claim 1, wherein the amount of the catalyst added in the step (2) is 5-50 ppm calculated by linear phosphonitrile chloride.
7. The method for synthesizing simethicone with high conversion rate and low ring body content as claimed in claim 1, wherein the negative pressure in step (2) is 0.02-0.1 MPa lower than atmospheric pressure.
8. The method for synthesizing simethicone with high conversion rate and low ring body content as claimed in claim 1, wherein the amount of hexamethyldisilazane added in step (3) is 1-10 times of the amount of linear phosphonitrile chloride.
9. The method for synthesizing simethicone with high conversion rate and low ring body content as claimed in claim 1, wherein the vacuum degree of the step (4) is-0.095 to-0.1 MPa.
10. The method for synthesizing simethicone with high conversion rate and low cyclic body content as claimed in claim 1, wherein the viscosity of the product in the step (4) is 50-200000 cp, the cyclic body content is less than 0.5%, and the preferred cyclic body content is less than 0.1%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115651201A (en) * | 2022-10-31 | 2023-01-31 | 湖北兴瑞硅材料有限公司 | Method for reducing content of silicon hydroxyl in dimethyl silicone oil |
| CN115850705A (en) * | 2022-12-12 | 2023-03-28 | 东莞市贝特利新材料有限公司 | Preparation method of methyl phenyl silicone oil |
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| 黄文润: ""线形氯化磷腈催化端羟基二甲基硅氧烷低聚物的缩聚反应"", 《有机硅材料》 * |
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| CN115651201A (en) * | 2022-10-31 | 2023-01-31 | 湖北兴瑞硅材料有限公司 | Method for reducing content of silicon hydroxyl in dimethyl silicone oil |
| CN115651201B (en) * | 2022-10-31 | 2024-08-09 | 湖北兴瑞硅材料有限公司 | Method for reducing silicon hydroxyl content in simethicone |
| CN115850705A (en) * | 2022-12-12 | 2023-03-28 | 东莞市贝特利新材料有限公司 | Preparation method of methyl phenyl silicone oil |
| CN115850705B (en) * | 2022-12-12 | 2024-08-13 | 东莞市贝特利新材料有限公司 | Preparation method of methylphenyl silicone oil |
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