CN108409775A - A kind of preparation method of 1- vinyl -1,1,3,3,3- pentamethyl disiloxanes - Google Patents
A kind of preparation method of 1- vinyl -1,1,3,3,3- pentamethyl disiloxanes Download PDFInfo
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- CN108409775A CN108409775A CN201810246857.XA CN201810246857A CN108409775A CN 108409775 A CN108409775 A CN 108409775A CN 201810246857 A CN201810246857 A CN 201810246857A CN 108409775 A CN108409775 A CN 108409775A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- MRRXLWNSVYPSRB-UHFFFAOYSA-N ethenyl-dimethyl-trimethylsilyloxysilane Chemical class C[Si](C)(C)O[Si](C)(C)C=C MRRXLWNSVYPSRB-UHFFFAOYSA-N 0.000 title description 11
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 19
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-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 16
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 12
- 239000000706 filtrate Substances 0.000 claims abstract description 8
- 238000006462 rearrangement reaction Methods 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 19
- 239000000047 product Substances 0.000 abstract description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 150000001923 cyclic compounds Chemical class 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 2
- XEZNGIUYQVAUSS-UHFFFAOYSA-N 18-crown-6 Chemical compound C1COCCOCCOCCOCCOCCO1 XEZNGIUYQVAUSS-UHFFFAOYSA-N 0.000 abstract 1
- 150000003983 crown ethers Chemical class 0.000 abstract 1
- AOJHDNSYXUZCCE-UHFFFAOYSA-N dimethylsilyloxy(trimethyl)silane Chemical class C[SiH](C)O[Si](C)(C)C AOJHDNSYXUZCCE-UHFFFAOYSA-N 0.000 abstract 1
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000011541 reaction mixture Substances 0.000 description 5
- 230000008707 rearrangement Effects 0.000 description 5
- 239000005046 Chlorosilane Substances 0.000 description 4
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 2
- XSDCTSITJJJDPY-UHFFFAOYSA-N chloro-ethenyl-dimethylsilane Chemical compound C[Si](C)(Cl)C=C XSDCTSITJJJDPY-UHFFFAOYSA-N 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 2
- 229920005560 fluorosilicone rubber Polymers 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 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 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000000739 chaotic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- 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
- C07F7/20—Purification, separation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The present invention relates to a kind of 1 vinyl 1,1,3,3, the preparation method of 3 pentamethyl disiloxanes, with 1,3 divinyl 1,1,3,3, tetramethyl disiloxane and 1,1,1,3,3,3 hexamethyldisiloxane are raw material, and rearrangement reaction is carried out under the catalytic action of complex catalyst KOH/18 crown ethers 6, then product is made in catalyst neutralisation, filtering, rectifying filtrate.The present invention forms a kind of complex catalyst using 18 crown ether 6 of macromolecular cyclic compound and KOH, by complex reaction, improves the activity of catalyst, can efficient catalytic rearrangement reaction.Meanwhile preparation method of the invention is simple, rapid reaction is stablized, and also has many advantages, such as that high income, safety are good, environmentally friendly.
Description
Technical field
The invention belongs to the synthesis fields of organosilicon chemistry, and in particular to a kind of 1- vinyl -1,1,3,3,3- pentamethyls
The preparation method of disiloxane.
Background technology
1- vinyl -1,1,3,3,3- pentamethyl disiloxanes are a kind of important silicone intermediates, and feature is
Functional group on two silicon is asymmetric, and there are one active vinyl groups, the structure, and it to be made to can be used as synthesis for tool in molecular structure
The monomer of organo-silicon compound carries out hydrosilylation with other hydrogen-containing compounds, prepares the product of different performance, is having
Machine chemistry of silicones and organic synthesis field play an important roll.Meanwhile 1- vinyl -1,1,3,3,3- pentamethyl disiloxanes may be used also
As closure agent, the synthesis for organosilicon polymers such as fluorosilicon oil, fluorine silicon raw rubbers uses, with the high molecular polymer of its preparation
One end is inert methyl, one end is active vinyl, in sulfidation medium vinyl and the other raw rubbers of fluorine silicone rubber
Molecule forms bridge crosslinking structure, and methyl end molecule is then free on except system, forms a kind of Semi-IPN winding arrangement, advantageously
The intrusion of external small molecule is resisted in fluorine silicone rubber, improves the oil resistance of rubber.It can be seen that 1- vinyl -1,1,3,3,
3- pentamethyl disiloxanes have important industrial utility value, there is good application prospect, invent a kind of efficient preparation side
Method is of great significance.
Preparation method in the prior art in relation to vinyl pentamethyl disiloxane, mainly by equimolar vinyl two
Methylchlorosilane and trim,ethylchlorosilane carry out cohydrolysis and then are condensed to yield under low-temperature condition.Preparation method reaction is multiple
It is miscellaneous, it is difficult to it controls, it is main during cohydrolysis because of the vinyldimethylchlorosilane hydrolysis rate different with trim,ethylchlorosilane
Based on itself hydrolytic condensation, the product that causes is mostly divinyl tetramethyl disiloxane and hexamethyldisiloxane,
The selectivity and yield of vinyl pentamethyl disiloxane are very low.Moreover, this method uses chlorosilane as reaction raw materials, it is steady
It is qualitative very poor, it is easy to generate hydrochloric acid steam fog in operating process, seriously endangers health and Environmental security, it is raw after the completion of hydrolysis
At a large amount of sour waters further generate environmental protection pressure.
Invention content
In view of the deficienciess of the prior art, the present invention provides, a kind of preparation method is simple, and stable reaction is efficient, when reaction
Between shorter 1- vinyl -1,1,3,3,3- pentamethyl disiloxanes preparation method.This method solve make in the prior art
The problems such as environmental protection brought with chlorosilane and poor selectivity, have many advantages, such as that high income, safety are good, environmentally friendly.
Technical scheme is as follows：
A kind of 1- vinyl -1,1, the preparation method of 3,3,3- pentamethyl disiloxanes include the following steps：
By divinyl -1,1,3,3 1,3-,-tetramethyl disiloxane and 1,1,1,3,3,3- hexamethyldisiloxane are mixed
It closes uniformly, complex catalyst KOH/18- crown ethers -6 are then added and stir, be heated to 70~90 DEG C of progress rearrangement reactions,
Then neutralizer neutralization reaction is added into system, cooling, filtering collect filtrate rectifying, obtain 1- vinyl -1,1, and 3,3,3-
Pentamethyl disiloxane.
, according to the invention it is preferred to, 1, the 3- divinyl -1,1,3,3,-tetramethyl disiloxane and 1,1,1,
3,3,3- hexamethyldisiloxane is according to molar ratio 1：(1.1~1.5) it is uniformly mixed.
, according to the invention it is preferred to, the complex catalyst KOH/18- crown ethers -6 are that 18- crown ethers -6 and KOH complexings are anti-
It should be formed；
Preferably, in the complex catalyst KOH/18- crown ethers -6, the inventory of KOH is 1,3- divinyl -1,1,
3,3, the 0.1%~1% of-tetramethyl disiloxane and 1,1,1,3,3,3- hexamethyldisiloxane gross mass of feeding intake；
Preferably, in the complex catalyst KOH/18- crown ethers -6, the inventory of 18- crown ethers -6 is KOH inventorys
20%~80%.
, according to the invention it is preferred to, the rearrangement reaction time is 0.5~2h.
, according to the invention it is preferred to, the neutralizer is anhydrous acetic acid, and neutralization reaction to system is in neutrality.
, according to the invention it is preferred to, room temperature (20~25 DEG C) is cooled to after neutralization reaction.
, according to the invention it is preferred to, the rectifying condition is pressure -0.082MPa extremely -0.096MPa, kettle temperature 50~80
℃；
Preferably, the reflux ratio of the rectifying is preferably 8~10:1.
What the present invention did not elaborate, press this field routine techniques.
Compared with prior art, it technical characterstic of the invention and has the beneficial effect that：
1, the present invention forms a kind of complex catalyst using macromolecular cyclic compound 18- crown ethers -6 and KOH, the catalyst
With potassium ion complex reaction occurs for middle 18- crown ethers -6, and potassium ion is complexed into space in ring, is dissolved in the form of ion pair anti-
System is answered, the activity of catalyst is improved, can efficiently be catalyzed 1,3- divinyl -1,1 at a lower temperature, 3,3, -
Tetramethyl disiloxane and 1,1,1,3,3,3- hexamethyldisiloxane carry out rearrangement reaction, catalysis effect fast with reaction speed
The features such as rate is high.
2, the present invention uses anhydrous rearrangement reaction system, avoids lacking for the chaotic complexity of product that hydrolysis reaction system is brought
It falls into, has the advantages that reaction condition is mild, product selectivity is high.
3, the present invention do not use chlorosilane raw material, solve in the prior art using chlorosilane process bands come a large amount of sour waters
And problem of environmental pollution, alleviate environmental protection pressure.
4, preparation method of the invention is simple, is easy to control, and high income, the purity of product are high.
Description of the drawings
Fig. 1 is product 1- vinyl -1,1,3,3,3- pentamethyl disiloxanes prepared by the embodiment of the present invention 11H-NMR
Spectrogram.
Specific implementation mode
With reference to following embodiment, the present invention is further illustrated, can not limit present disclosure.
Raw material described in embodiment is convenient source, can market buy or obtained according to prior art preparation.
Embodiment 1
To equipped with blender, thermometer, condenser pipe 2L three-necked flasks in 744g 1,3- divinyl -1,1,3 are added,
3,1,1,1,3,3,3- hexamethyldisiloxane of-tetramethyl disiloxane and 712.8g is uniformly mixed, is then added into bottle
The mixture of 4.37g KOH and 2.19g 18- crown ethers -6, is vigorously stirred, open heating be to slowly warm up to 80 DEG C it is anti-into rearrangement
It answers, maintains reaction 1h, 4.96g anhydrous acetic acid neutralization reactions are then added into system, and reaction mixture is down to room temperature, mistake
Filtrate, rectifying are collected in filter, and rectifying condition is pressure -0.082MPa extremely -0.096MPa, 50~80 DEG C of kettle temperature, and the rectifying is returned
Stream is than being 10:1；1- vinyl -1,1,3,3,3- pentamethyl disiloxanes, purity 99.32%, yield 95.7% is made.
Embodiment 2
To equipped with blender, thermometer, condenser pipe 2L three-necked flasks in 744g 1,3- divinyl -1,1,3 are added,
3,1,1,1,3,3,3- hexamethyldisiloxane of-tetramethyl disiloxane and 712.8g is uniformly mixed, is then added into bottle
The mixture of 7.28g KOH and 2.19g 18- crown ethers -6, is vigorously stirred, open heating be to slowly warm up to 80 DEG C it is anti-into rearrangement
It answers, maintains reaction 1h, 8.08g anhydrous acetic acid neutralization reactions are then added into system, and reaction mixture is down to room temperature, mistake
Filtrate, rectifying are collected in filter, and rectifying condition is pressure -0.082MPa extremely -0.096MPa, 50~80 DEG C of kettle temperature, and the rectifying is returned
Stream is than being 10:1；1- vinyl -1,1,3,3,3- pentamethyl disiloxanes, purity 99.25%, yield 95.2% is made.
Embodiment 3
To equipped with blender, thermometer, condenser pipe 2L three-necked flasks in 744g 1,3- divinyl -1,1,3 are added,
3,1,1,1,3,3,3- hexamethyldisiloxane of-tetramethyl disiloxane and 712.8g is uniformly mixed, is then added into bottle
The mixture of 7.28g KOH and 3.64g 18- crown ethers -6, is vigorously stirred, open heating be to slowly warm up to 80 DEG C it is anti-into rearrangement
It answers, maintains reaction 1h, 8.08g anhydrous acetic acid neutralization reactions are then added into system, and reaction mixture is down to room temperature, mistake
Filtrate, rectifying are collected in filter, and rectifying condition is pressure -0.082MPa extremely -0.096MPa, 50~80 DEG C of kettle temperature, and the rectifying is returned
Stream is than being 9:1；1- vinyl -1,1,3,3,3- pentamethyl disiloxanes, purity 99.58%, yield 96.2% is made.
Embodiment 4
To equipped with blender, thermometer, condenser pipe 2L three-necked flasks in 744g 1,3- divinyl -1,1,3 are added,
3,1,1,1,3,3,3- hexamethyldisiloxane of-tetramethyl disiloxane and 712.8g is uniformly mixed, is then added into bottle
The mixture of 7.28g KOH and 5.09g 18- crown ethers -6, is vigorously stirred, open heating be to slowly warm up to 80 DEG C it is anti-into rearrangement
It answers, maintains reaction 1h, 8.08g anhydrous acetic acid neutralization reactions are then added into system, and reaction mixture is down to room temperature, mistake
Filtrate, rectifying are collected in filter, and rectifying condition is pressure -0.082MPa extremely -0.096MPa, 50~80 DEG C of kettle temperature, and the rectifying is returned
Stream is than being 10:1；1- vinyl -1,1,3,3,3- pentamethyl disiloxanes, purity 99.45%, yield 94.8% is made.
Embodiment 5
To equipped with blender, thermometer, condenser pipe 2L three-necked flasks in 744g 1,3- divinyl -1,1,3 are added,
3,1,1,1,3,3,3- hexamethyldisiloxane of-tetramethyl disiloxane and 712.8g is uniformly mixed, is then added into bottle
The mixture of 11.66g KOH and 5.83g 18- crown ethers -6, is vigorously stirred, open heating be to slowly warm up to 80 DEG C it is anti-into rearrangement
It answers, maintains reaction 1h, 12.77g anhydrous acetic acid neutralization reactions are then added into system, and reaction mixture is down to room temperature,
Filtrate, rectifying are collected in filtering, and rectifying condition is pressure -0.082MPa extremely -0.096MPa, 50~80 DEG C of kettle temperature, the rectifying
Reflux ratio is 8:1；1- vinyl -1,1,3,3,3- pentamethyl disiloxanes, purity 99.08%, yield 94.6% is made.
Comparative example 1
To equipped with blender, thermometer, condenser pipe 2L three-necked flasks in 744g 1,3- divinyl -1,1,3 are added,
3,1,1,1,3,3,3- hexamethyldisiloxane of-tetramethyl disiloxane and 712.8g is uniformly mixed, and is then only added into bottle
Enter 4.37g KOH, be vigorously stirred, open heating and be to slowly warm up to 80 DEG C and reacted, maintain reaction 1h, by gas-chromatography into
Row analysis has no 1- vinyl -1,1, and 3,3,3- pentamethyl disiloxanes generate, and continues to extend the reaction time to 5h, no product
It generates, then extends the reaction time to 12h, still generated without product；The reaction system is kept, increases KOH into bottle to 11.66g, and
Reaction 5h is maintained, by gas chromatographic analysis, still without 1- vinyl -1,1 in system, 3,3,3- pentamethyl disiloxanes generate.
Comparative example 1 repeats the reaction process of embodiment, but catalyst only selects KOH, by gas-chromatography to react into
Cheng Jinhang is analyzed, and is generated without 1- vinyl -1,1,3,3,3- pentamethyl disiloxanes in discovery system, even if extend reaction
Between, increase KOH inventory, still without product generate.
Comparative example 2
To equipped with blender, thermometer, condenser pipe 2L four-hole boiling flasks in be added 1000g distilled water, pass through two constant pressures
Dropping funel, which synchronizes, is added dropwise 108.5g trim,ethylchlorosilanes and 120.5g vinyldimethylchlorosilanes progress cohydrolysis reaction, to the greatest extent
Amount keeps drop rate consistent, and system is cooled down using ice-water bath, maintains 0~10 DEG C of dropping temperature, continues after being added dropwise to complete
2h is stirred, layering is then allowed to stand, upper organic phase is washed to neutrality, cohydrolysis object is obtained after dry.
Cohydrolysis object is subjected to gas chromatographic analysis, component is sufficiently complex in product, and primary product is divinyl tetramethyl
The yield of base disiloxane and hexamethyldisiloxane, 1- vinyl -1,1,3,3,3- pentamethyl disiloxanes is very low.
Claims (9)
1. a kind of 1- vinyl -1,1, the preparation method of 3,3,3- pentamethyl disiloxanes include the following steps：
By divinyl -1,1,3,3 1,3-,-tetramethyl disiloxane and the mixing of 1,1,1,3,3,3- hexamethyldisiloxane are equal
It is even, complex catalyst KOH/18- crown ethers -6 are then added and stir, are heated to 70~90 DEG C of progress rearrangement reactions, then
Neutralizer neutralization reaction is added into system, cooling, filtering collect filtrate rectifying, obtain 1- vinyl -1,1,3,3,3- five first
Base disiloxane.
2. 1- vinyl -1,1 according to claim 1, the preparation method of 3,3,3- pentamethyl disiloxanes, feature exist
In, 1, the 3- divinyl -1,1,3,3,-tetramethyl disiloxane and 1,1,1,3,3,3- hexamethyldisiloxane according to
Molar ratio 1：(1.1~1.5) it is uniformly mixed.
3. 1- vinyl -1,1 according to claim 1, the preparation method of 3,3,3- pentamethyl disiloxanes, feature exist
In, in the complex catalyst KOH/18- crown ethers -6, the inventory of KOH is 1,3- divinyl -1,1,3,3,-tetramethyl
The 0.1%~1% of disiloxane and 1,1,1,3,3,3- hexamethyldisiloxane gross mass of feeding intake.
4. 1- vinyl -1,1 according to claim 3, the preparation method of 3,3,3- pentamethyl disiloxanes, feature exist
In in the complex catalyst KOH/18- crown ethers -6, the inventory of 18- crown ethers -6 is the 20%~80% of KOH inventorys.
5. 1- vinyl -1,1 according to claim 1, the preparation method of 3,3,3- pentamethyl disiloxanes, feature exist
In the rearrangement reaction time is 0.5~2h.
6. 1- vinyl -1,1 according to claim 1, the preparation method of 3,3,3- pentamethyl disiloxanes, feature exist
In the neutralizer is anhydrous acetic acid, and neutralization reaction to system is in neutrality.
7. 1- vinyl -1,1 according to claim 1, the preparation method of 3,3,3- pentamethyl disiloxanes, feature exist
In being cooled to room temperature after neutralization reaction.
8. 1- vinyl -1,1 according to claim 1, the preparation method of 3,3,3- pentamethyl disiloxanes, feature exist
In the rectifying condition is pressure -0.082MPa extremely -0.096MPa, 50~80 DEG C of kettle temperature.
9. 1- vinyl -1,1 according to claim 1, the preparation method of 3,3,3- pentamethyl disiloxanes, feature exist
In the reflux ratio of the rectifying is 8~10:1.
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| CN109776593A (en) * | 2017-11-14 | 2019-05-21 | 石家庄圣泰化工有限公司 | The preparation method of four ethylene disiloxane of 1,3- dimethyl -1,1,3,3- |
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| CN107235996A (en) * | 2017-06-16 | 2017-10-10 | 壮铭新材料科技江苏有限公司 | A kind of preparation method and application of trimethyl silicane alkoxide |
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|---|---|---|---|---|
| CN106986890A (en) * | 2017-06-07 | 2017-07-28 | 威海新元化工有限公司 | A kind of environment-friendly preparation method of the pentamethyl cyclotrisiloxane of 2 vinyl 2,4,4,6,6 |
| CN107235996A (en) * | 2017-06-16 | 2017-10-10 | 壮铭新材料科技江苏有限公司 | A kind of preparation method and application of trimethyl silicane alkoxide |
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| CN109776593A (en) * | 2017-11-14 | 2019-05-21 | 石家庄圣泰化工有限公司 | The preparation method of four ethylene disiloxane of 1,3- dimethyl -1,1,3,3- |
| CN109776593B (en) * | 2017-11-14 | 2023-05-09 | 河北圣泰材料股份有限公司 | Preparation method of 1, 3-dimethyl-1, 3-tetraethylenedisiloxane |
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