CN108440592B - Preparation method of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane - Google Patents
Preparation method of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane Download PDFInfo
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- MFWYAJVOUCTAQI-UHFFFAOYSA-N bis[[ethenyl(dimethyl)silyl]oxy]-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C=C MFWYAJVOUCTAQI-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 27
- FSIJKGMIQTVTNP-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C=C)C=C FSIJKGMIQTVTNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- UBHZUDXTHNMNLD-UHFFFAOYSA-N dimethylsilane Chemical compound C[SiH2]C UBHZUDXTHNMNLD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical group CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims description 5
- YYLGKUPAFFKGRQ-UHFFFAOYSA-N dimethyldiethoxysilane Chemical compound CCO[Si](C)(C)OCC YYLGKUPAFFKGRQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- DMZWVCJEOLBQCZ-UHFFFAOYSA-N chloro(ethenyl)silane Chemical compound Cl[SiH2]C=C DMZWVCJEOLBQCZ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000007809 chemical reaction catalyst Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 17
- 239000000203 mixture Substances 0.000 description 13
- XSDCTSITJJJDPY-UHFFFAOYSA-N chloro-ethenyl-dimethylsilane Chemical compound C[Si](C)(Cl)C=C XSDCTSITJJJDPY-UHFFFAOYSA-N 0.000 description 6
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 6
- -1 polysiloxane Polymers 0.000 description 6
- 229920002545 silicone oil Polymers 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 150000003377 silicon compounds Chemical class 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000005227 gel permeation chromatography Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
- C07F7/0872—Preparation and treatment thereof
- C07F7/0874—Reactions involving a bond of the Si-O-Si linkage
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- Chemical Kinetics & Catalysis (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a preparation method of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane. The method comprises the steps of taking divinyl tetramethyl disiloxane and dialkoxy dimethyl silane as reaction raw materials, taking anhydrous ferric trichloride as a reaction catalyst, carrying out a kettle type reaction at 70-80 ℃, filtering to remove the catalyst after the reaction is finished, and rectifying to obtain the product. The method has the advantages of simple process, mild reaction conditions, high catalytic efficiency, high safety, high yield, environmental friendliness and the like, and abandons the use of the vinyl chlorosilane which is not environment-friendly.
Description
Technical Field
The invention belongs to the field of synthesis of organic silicon compounds, and particularly relates to a preparation method of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane.
Background
1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane belongs to the category of vinyl silicone oil, has the lowest polymerization degree, and is an important organosilicon intermediate. Because the molecular chain segment is short, the main chain structure is only three silica chain segments, and simultaneously two ends of the main chain structure contain active ethylene groups, the organic silicon compound has a plurality of unique functions, can be used for synthesizing short-chain organic silicon compounds with various properties by utilizing the hydrosilylation reaction of the ethylene groups and other hydrosilanes, and can also be used as an end sealing agent for synthesizing organic silicon polymers such as silicone oil, silicone resin, silicone rubber and the like. However, the existing synthesis process also has the defects of low yield, complex by-product and the like generally, so the invention of the synthesis method which is environment-friendly, harmless, reasonable in process and high in yield has important significance.
The structural formula of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane is as follows:
in the prior art, a preparation method of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane mainly adopts a mode of cohydrolysis of vinyl dimethylchlorosilane and dimethyldichlorosilane in an ice-water bath. Under the low temperature state, vinyl dimethylchlorosilane and dimethyldichlorosilane are synchronously dripped into the water inlet phase for cohydrolysis, the acid water layer is separated after the hydrolysis is finished, the organic phase is washed to be neutral, and then products are separated. In the reaction system, the hydrolysis rates of the vinyl dimethylchlorosilane and the dimethyldichlorosilane are greatly different, the self-hydrolysis condensation reaction of the vinyl dimethylchlorosilane and the dimethyldichlorosilane is inevitably generated to generate polysiloxane mixtures with different components and different polymerization degrees, and the reaction selectivity of the target product 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane is poor. In addition, the raw materials of the method, namely the vinyl dimethylchlorosilane and the dimethyldichlorosilane, have poor stability, hydrochloric acid vapor is easily generated in the operation process, and the health and the environmental safety are seriously harmed.
In addition, a catalytic equilibrium synthesis process of short-chain vinyl silicone oil is reported in documents, and the short-chain vinyl silicone oil is mainly prepared by taking dimethyl siloxane mixed ring bodies (DMC) and a vinyl-terminated end capping agent as reaction raw materials and carrying out processes of raw material dehydration, catalytic equilibrium, catalyst decomposition and low-boiling-point substance removal under the action of a temporary catalyst (tetramethylammonium hydroxide). The product of the reaction process is mainly vinyl-terminated silicone oil with the average polymerization degree of 6-20, and 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane with the polymerization degree of 1 is difficult to obtain.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the preparation method of the 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane, which has the advantages of simple process, high catalytic efficiency and mild reaction conditions. The method abandons the use of the vinyl chlorosilane which is not environment-friendly, and has the advantages of good safety, high yield, environment friendliness and the like.
The technical scheme of the invention is as follows:
a preparation method of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane comprises the following steps:
the method comprises the steps of uniformly mixing divinyl tetramethyl disiloxane and dialkoxy dimethyl silane, adding catalyst anhydrous ferric trichloride, stirring to form a suspension, heating to 70-80 ℃ until materials react completely, cooling the system, filtering to remove the catalyst, collecting filtrate, and rectifying to obtain 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane.
According to the present invention, preferably, the dialkoxydimethylsilane is dimethoxydimethylsilane or diethoxydimethylsilane.
According to the invention, preferably, the divinyl tetramethyl disiloxane and the dialkoxy dimethylsilane are uniformly mixed according to a molar ratio of 1 (1.0-1.2).
According to the invention, the feeding amount of the anhydrous ferric trichloride is preferably 0.5-5% of the total mass of the divinyltetramethyldisiloxane and the dialkoxydimethylsilane, and more preferably 1-3%.
According to the invention, the reaction time of the divinyltetramethyldisiloxane and the dialkoxydimethylsilane is preferably 2-6 h.
According to the invention, preferably, after the reaction is finished, the temperature of the system is reduced to room temperature (20-25 ℃).
According to the present invention, preferably, the rectification conditions of the product are as follows: the pressure is-0.098 MPa, and the temperature is 82-84 ℃; namely, intercepting the fraction at 82-84 ℃ and 0.098MPa in the rectification process to obtain the product 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane;
preferably, the reflux ratio is controlled to be 10:1 in the rectification process.
The present invention has not been described in detail, but is in accordance with conventional techniques in the art.
Compared with the prior art, the invention has the following technical characteristics and beneficial effects:
1. the invention adopts anhydrous ferric trichloride as a catalyst, can efficiently catalyze the reaction of divinyl tetramethyl disiloxane and dialkoxy dimethyl silane at lower temperature, and has the characteristics of simple process, high catalysis efficiency and the like.
2. The invention does not use chlorosilane raw materials, and solves the problems of a large amount of acid water and environmental pollution caused by adopting a chlorosilane process in the prior art.
3. The invention adopts an anhydrous reaction system, avoids respective hydrolysis of reaction raw materials to generate a polysiloxane mixture, and has the advantages of mild reaction conditions and high product selectivity.
4. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane has high yield which far exceeds a reaction system with DMC catalysis equilibrium.
Drawings
FIG. 1 is a gas chromatogram of the product obtained by distillation in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
The starting materials described in the examples are conventional and are commercially available or prepared according to the prior art.
Example 1
Adding 558g (3mol) of divinyl tetramethyl disiloxane and 396g (3.3mol) of dimethoxy dimethyl silane into a 2L three-neck flask provided with a stirrer, a thermometer and a condenser, uniformly mixing, then adding 9.54g of anhydrous ferric trichloride into the mixture, stirring to form a suspension, starting to heat, slowly heating to 70-80 ℃, maintaining the reaction for 4 hours, then cooling the system to room temperature, filtering to remove the ferric trichloride, collecting filtrate, carrying out rectification and purification by adopting a reflux ratio of 10:1, and intercepting a fraction at 82-84 ℃ to 0.098MPa to obtain a product 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane with the purity of 99.48% and the yield of 92.8%.
Example 2
Adding 558g (3mol) of divinyl tetramethyl disiloxane and 396g (3.3mol) of dimethoxy dimethyl silane into a 2L three-neck flask provided with a stirrer, a thermometer and a condenser, uniformly mixing, then adding 19.08g of anhydrous ferric trichloride into the mixture, stirring to form a suspension, starting to heat, slowly heating to 70-80 ℃, maintaining the reaction for 4 hours, then cooling the system to room temperature, filtering to remove the ferric trichloride, collecting filtrate, carrying out rectification and purification by adopting a reflux ratio of 10:1, and intercepting a fraction at 82-84 ℃ to 0.098MPa to obtain a product 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane with the purity of 99.25% and the yield of 94.2%.
Example 3
558g (3mol) of divinyl tetramethyl disiloxane and 488.4g (3.3mol) of diethoxydimethylsilane are added into a 2L three-neck flask provided with a stirrer, a thermometer and a condenser and mixed uniformly, 10.46g of anhydrous ferric trichloride is added into the mixture and stirred to form suspension, the mixture is heated to 70-80 ℃ slowly, the reaction is maintained for 4 hours, the system is cooled to room temperature, ferric trichloride is removed by filtration, filtrate is collected and is rectified and purified by adopting the reflux ratio of 10:1, and the fraction with the temperature of 82-84 ℃ to 0.098MPa is intercepted, namely the product 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane with the purity of 99.06 percent and the yield of 91.3 percent.
Example 4
558g (3mol) of divinyl tetramethyl disiloxane and 488.4g (3.3mol) of diethoxydimethylsilane are added into a 2L three-neck flask provided with a stirrer, a thermometer and a condenser and mixed uniformly, 20.93g of anhydrous ferric trichloride is added into the mixture and stirred to form suspension, the mixture is heated to 70-80 ℃ slowly, the reaction is maintained for 4 hours, the system is cooled to room temperature, ferric trichloride is removed by filtration, filtrate is collected and rectified and purified by adopting the reflux ratio of 10:1, and the fraction of 82-84 ℃ to 0.098MPa is intercepted, namely the product 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane with the purity of 99.32 percent and the yield of 93.4 percent.
Comparative example 1
1000g of distilled water was charged into a 2L three-necked flask equipped with a stirrer, a thermometer and a condenser, vigorously stirred, and then 241g (2mol) of vinyldimethylchlorosilane and 129g (1mol) of dimethyldichlorosilane were simultaneously dropped into the flask using two constant-pressure dropping funnels at a dropping rate of 2:1, to conduct a cohydrolysis reaction. Maintaining the temperature of cohydrolysis at 0-10 deg.C, stirring for 1 hr, standing for layering, washing the upper organic phase to neutrality, and drying to obtain cohydrolysate.
The cohydrolysate is analyzed by gas chromatography, the product contains different cyclosiloxanes and polysiloxane with different chain numbers, the components are multiple and disordered, and the target product 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane has poor selectivity and low yield.
Comparative example 2
Adding 370g of dimethyl siloxane mixed ring body (DMC), 930g of divinyl tetramethyl disiloxane and 6.5g of tetramethyl ammonium hydroxide alkali gum (purity of 1%) into a 2L three-neck flask provided with a stirrer, a thermometer and a condensation pipe, starting stirring to uniformly mix the system, dehydrating for 2 hours at 40-50 ℃ and-0.05 MPa, recovering negative pressure by adopting dry nitrogen after dehydration is finished, heating to 90-100 ℃ for equilibrium reaction for 5 hours, quickly heating to 160 ℃ after the reaction is finished, maintaining for 1 hour, decomposing and deactivating a catalyst, heating to 200 ℃ under the condition of ultimate vacuum, removing unreacted ring body and micromolecules, and cooling to obtain the product.
The product prepared by the method is analyzed by gel permeation chromatography to be the vinyl-terminated silicone oil with the average polymerization degree of 6-20, and almost no 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane exists.
Comparative example 3
558g (3mol) of divinyl tetramethyl disiloxane and 396g (3.3mol) of dimethoxy dimethyl silane are added into a 2L three-neck flask provided with a stirrer, a thermometer and a condenser tube and are uniformly mixed, then 9.54g of concentrated sulfuric acid with the mass concentration of 98% is added into the mixture, the mixture is vigorously stirred, the mixture is heated to 70-80 ℃ slowly, the reaction is maintained for 4 hours, then the system is cooled to the room temperature, 19.08g of sodium carbonate is added into the mixture for neutralization, vacuum filtration is carried out, filtrate is collected and rectified, and 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane with the extremely small amount is obtained, and the yield is 5.2%.
Comparative example 3 simulates the material ratio and the reaction process of example 1, but the catalyst is changed from anhydrous ferric chloride to concentrated sulfuric acid with the mass concentration of 98%, the reaction effect is very poor, the product rearrangement is serious, the components are very complex, the reaction selectivity of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane is very poor, the yield is very low, only 5.2%, and the product cannot be efficiently synthesized.
Claims (9)
1. A preparation method of 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane comprises the following steps:
the method comprises the steps of uniformly mixing divinyl tetramethyl disiloxane and dialkoxy dimethyl silane, adding catalyst anhydrous ferric trichloride, stirring to form a suspension, heating to 70-80 ℃ until materials react completely, cooling the system, filtering to remove the catalyst, collecting filtrate, and rectifying to obtain 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane.
2. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane as claimed in claim 1, wherein said dialkoxydimethylsilane is dimethoxydimethylsilane or diethoxydimethylsilane.
3. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane according to claim 1, wherein divinyl tetramethyl disiloxane and dialkoxy dimethylsilane are uniformly mixed according to a molar ratio of 1 (1.0-1.2).
4. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane as claimed in claim 1, wherein the feeding amount of anhydrous ferric trichloride is 0.5-5% of the total mass of divinyl tetramethyl disiloxane and dialkoxy dimethyl silane.
5. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyl trisiloxane as claimed in claim 4, wherein the feeding amount of anhydrous ferric trichloride is 1-3% of the total mass of divinyl tetramethyl disiloxane and dialkoxy dimethyl silane.
6. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane as claimed in claim 1, wherein the reaction time of divinyl tetramethyldisiloxane and dialkoxydimethylsilane is 2-6 h.
7. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane as claimed in claim 1, characterized in that the temperature of the system is reduced to room temperature after the reaction is completed.
8. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane as claimed in claim 1, characterized in that the rectification conditions for rectification to obtain 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane are as follows: the pressure is-0.098 MPa, and the temperature is 82-84 ℃.
9. The method for preparing 1, 5-divinyl-1, 1,3,3,5, 5-hexamethyltrisiloxane as claimed in claim 1, characterized in that the reflux ratio is controlled to be 10:1 during rectification.
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| CN107021976A (en) * | 2017-02-27 | 2017-08-08 | 广东省稀有金属研究所 | A kind of preparation method of the hydrogen-based diphenyl trisiloxanes of tetramethyl two |
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| WO2013191955A1 (en) * | 2012-06-20 | 2013-12-27 | Dow Corning Corporation | Monofunctional organopolysiloxanes for compatabilzing polyheterosiloxanes |
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|---|---|---|---|---|
| CN1989178A (en) * | 2004-05-20 | 2007-06-27 | 通用电气公司 | Silicone condensation reaction |
| CN103387586A (en) * | 2013-07-24 | 2013-11-13 | 山东省科学院新材料研究所 | Preparation method of vinyl-terminated siloxane |
| CN105218575A (en) * | 2015-11-04 | 2016-01-06 | 威海新元化工有限公司 | A kind of preparation method of 1-vinyl-3-hydroxyl-1,1,3,3-tetramethyl disiloxane |
| CN107021976A (en) * | 2017-02-27 | 2017-08-08 | 广东省稀有金属研究所 | A kind of preparation method of the hydrogen-based diphenyl trisiloxanes of tetramethyl two |
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