CN109942614A - A kind of preparation method of the based polysiloxane containing hexamethylene - Google Patents
A kind of preparation method of the based polysiloxane containing hexamethylene Download PDFInfo
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- CN109942614A CN109942614A CN201910161956.2A CN201910161956A CN109942614A CN 109942614 A CN109942614 A CN 109942614A CN 201910161956 A CN201910161956 A CN 201910161956A CN 109942614 A CN109942614 A CN 109942614A
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Abstract
The invention discloses a kind of preparation methods of based polysiloxane containing hexamethylene, belong to organosilicon synthesis technical field.The present invention can obtain the RR of base silane containing hexamethylene of higher yields through one-step technology1(C6H11)Si‑R4, and by R2R3Si(R4)2、RR1(C6H11)Si‑R4, organic acid and catalyst A 1:(1-1.25 in molar ratio): (1-1.8): (0.001-0.004) is added in reaction flask, stirring is warming up to 85 DEG C -95 DEG C, and after being stirred to react 40-60 minutes at this temperature, be added dehydrating agent, continue 85 DEG C -95 DEG C of reactions 3-6 hours；It is down to room temperature after reaction, non-polar organic solvent dilution is added, is washed with deionized water to neutrality, collects organic phase, drying, filtering, concentration, concentrate vacuum distillation collects relevant pressure fraction at a temperature of, obtains the based polysiloxane containing hexamethylene.The present invention synthesizes the based polysiloxane containing hexamethylene of high quality by optimization reaction condition, and product purity and yield are higher, is suitable for industrialized production.
Description
Technical field
The present invention relates to organosilicon synthesis technical fields, and in particular to a kind of preparation method of the based polysiloxane containing hexamethylene.
Background technique
It is important in high refractive index organosilicon product it is well known that being " noble " in silicone oil product containing phenyl silicone oil
Support element contains unstable unsaturated bond in phenyl structure, so seeking to increase the stability of product, it has to by benzene
Base is replaced with the cyclohexyl of more rock-steady structure.Basic around this principle, a series of silicone product containing cyclohexyl is exhaled
Be intended to out.Especially in recent years, with the development of LED organosilicon material for packaging, silicon can be improved containing hexamethylene based polysiloxane
Glue refractive index reduces product viscosity, has wide practical use.However, being difficult to obtain silane monomer containing cyclohexyl, market at present
The mixture of upper only cyclohexyl silane monomer, stability is poor, so as to cause the hexamethylene based polysiloxane of hydrolytic condensation
Structure can not be stablized, thus prepare the expanding production method of the based polysiloxane containing hexamethylene currently not yet.
Summary of the invention
It is an object of the invention to provide a kind of system of based polysiloxane containing hexamethylene in place of overcome the deficiencies in the prior art
Preparation Method.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of the based polysiloxane containing hexamethylene, the structural formula of the based polysiloxane containing hexamethylene such as formula (I) institute
Show:
R2R3Si(R4)2And RR1(C6H11)Si-R4, wherein n >=1, R, R1、R2And R3It is identical or not identical, independently
Selected from alkoxy, halogen, alkyl, cyclohexyl, aryl, the alkyl replaced by one or more halogens, acryloyl group and epoxy group
Monovalent hydrocarbon；
The preparation method of the based polysiloxane containing hexamethylene, includes the following steps:
(1) by R2R3Si(R4)2、RR1(C6H11)Si-R4, organic acid and catalyst A 1:(1-1.25 in molar ratio): (1-
1.8): (0.001-0.004) is added in reaction flask, and stirring is warming up to 85 DEG C -95 DEG C, and is stirred to react 40- at this temperature
After sixty minutes, be added dehydrating agent, continue 85 DEG C -95 DEG C of reactions 3-6 hours,
Wherein, R, R1、R2And R3It is identical or not identical, it is respectively and independently selected from alkoxy, halogen, alkyl, allyl, virtue
Base, the alkyl replaced by one or more halogens, acryloyl group and epoxy group monovalent hydrocarbon；R4For halogen or alkoxy；
(2) it is down to room temperature after reaction, non-polar organic solvent dilution is added, is washed with deionized water to neutrality, collects
Relevant pressure fraction at a temperature of is collected in organic phase, drying, filtering, concentration, concentrate vacuum distillation, is obtained described containing hexamethylene
Based polysiloxane；
The RR1(C6H11)Si-R4The preparation method comprises the following steps:
S1, R is weighed in proportion1R2R3SiR4, magnesium chips and catalyst B, under nitrogen atmosphere, by R1R2R3SiR4, magnesium chips and urge
Agent B mixing, is heated to 90 DEG C -150 DEG C, wherein R1、R2、R3It is identical or different, and R1、R2And R3It is respectively and independently selected from alcoxyl
Base, halogen, alkyl, unsaturated alkyl or aryl, R4For alkoxy or halogen；
S2, a certain amount of cyclohexane halide reaction is first added in the mixed solution of S1；
Reactant in S2 is reacted 2-3h by S3, heat preservation at a reflux temperature；
S4, remaining cyclohexane halide is added, the reaction was continued, and keeps the temperature 45-50min；
R1R2R3SiR4, the molar ratio of total amount and magnesium chips is added is 1:(1-2.2 to cyclohexane halide): (1-2.1), wherein S2
The additional amount of middle cyclohexane halide accounts for the 30%-40% that total amount is added in cyclohexane halide；The catalyst B dosage is
R1R2R3SiR4The 0.7%-1% of quality, the catalyst B are the mixture of stannous chloride and magnesium nitrate.
The present invention, which is reacted using cyclohexane halide with magnesium, generates cyclohexyl Grignard Reagent, R1R2R3SiR4With cyclohexyl grignard
Reagent is in the presence of catalyst, by heating, stir, carries out the nucleophilic substitution of SN1, thus stablized, purity compared with
High, tool hydrolysing activity base silane containing hexamethylene, and contain hexamethylene base silane using this, by optimizing reaction condition, reaction synthesizes
The based polysiloxane containing hexamethylene of high quality.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, the organic acid are
Formic acid, acetic acid or propionic acid.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, the catalyst A
For SO4 2-/TiO2Strong solid acid catalyst.Catalyst of the invention selects SO4 2-/TiO2Strong solid acid catalyst has good
Catalytic activity is conducive to the yield and purity that improve hexamethylene based polysiloxane.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, the dehydrating agent are
N, N '-dicyclohexylcarbodiimide.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, the dehydrating agent with
R2R3Si(R4)2Molar ratio be 2-2.5:1.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, the step (1)
In, R2R3Si(R4)2、RR1(C6H11)Si-R4, organic acid and catalyst A molar ratio be 1:1.15:1.6:0.002.Test table
Bright, the proportion of above-mentioned raw materials is closely related with the yield of the based polysiloxane containing hexamethylene, works as R2R3Si(R4)2、RR1(C6H11)Si-R4、
When the control of the molar ratio of organic acid and catalyst A is 1:1.15:1.6:0.002, the purity and yield of the based polysiloxane containing hexamethylene
It is higher, it is conducive to improve product quality.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, the nonpolarity have
Solvent is at least one of benzene,toluene,xylene, n-hexane, hexamethylene, normal heptane.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, the RR1
(C6H11)Si-R4For dicyclohexylmethyl methoxy silane.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, in the step S1
The dosage of catalyst is R1R2R3SiR4The 0.9% of quality, the mass ratio of stannous chloride and magnesium nitrate is 0.1- in the catalyst
0.4:1, it is preferable that the mass ratio of stannous chloride and magnesium nitrate is 0.25:1 in the catalyst, and it is higher can to obtain purity
Dicyclohexylmethyl methoxy silane.
The preferred embodiment of preparation method as the based polysiloxane of the present invention containing hexamethylene, in the step S2
The additional amount of cyclohexane halide accounts for total amount is added in cyclohexane halide 30%.The cyclohexyl Grignard Reagent generated due to reaction process
Compare vivaciously, the additional amount of cyclohexane halide is excessive in the step S2, is easy to react production by-product with cyclohexane halide, lead
Product yield is caused to reduce.
Compared with prior art, the invention has the benefit that
The present invention, which is reacted using cyclohexane halide with magnesium, generates cyclohexyl Grignard Reagent, R1R2R3SiR4With cyclohexyl grignard
Reagent is in the presence of catalyst, by heating, stir, carries out the nucleophilic substitution of SN1, thus stablized, purity compared with
High, tool hydrolysing activity base silane containing hexamethylene, and contain hexamethylene base silane using this, by optimizing reaction condition, reaction synthesizes
The based polysiloxane containing hexamethylene of high quality.Reaction condition of the present invention is mild, and product purity and yield are higher, is suitable for industrial metaplasia
It produces.
Specific embodiment
Purposes, technical schemes and advantages in order to better illustrate the present invention, below in conjunction with specific embodiment to the present invention
It further illustrates.It will be appreciated by those skilled in the art that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
In embodiment, used experimental method is conventional method unless otherwise specified, material used, reagent etc.,
It is commercially available unless otherwise specified.
The magnesium chips that dilute HCl solution that it is 5% that magnesium chips described in following embodiment, which is by mass fraction, is washed and is dried for standby,
Removing magnesium chips surface, there are oxidation films.
Embodiment 1
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method, including walk as follows
It is rapid:
(1) methyldicyclohexyl methoxy silane is prepared
S1, methyltrimethoxysilane, magnesium chips and catalyst are weighed in proportion；
S2, justify in tetra- mouthfuls of glass of 250mL with reflux condensing tube, thermometer, blender, heater and balance charging device
In flask, under nitrogen protection, tetramethoxy-silicane, magnesium chips and catalyst is added, is heated to 135 DEG C；
S3, a certain amount of chlorocyclohexane reaction, the charging rate of chlorocyclohexane are first added in the mixed solution of S1
For 0.3g/min；
Reactant in S3 is reacted 3h by S4, heat preservation at a reflux temperature；
S5, remaining chlorocyclohexane is added, the reaction was continued, and keeps the temperature 50min, and reaction was completed；
It is 1:2.2:2.1 that total amount and the molar ratio of magnesium chips, which is added, in methyltrimethoxysilane, chlorocyclohexane, wherein S3
The additional amount of middle chlorocyclohexane accounts for total amount is added in chlorocyclohexane 35%；The catalyst amount is methyl trimethoxy oxygroup silicon
The 0.9% of alkane quality, the catalyst are the mixture of stannous chloride and magnesium nitrate, and the mass ratio of stannous chloride and magnesium nitrate is
0.25:1.Analysis the result shows that, the methyldicyclohexyl methoxy silane yield of the present embodiment is 86.36%, and purity is
99.52%.
(2) by dimethyldimethoxysil,ne, methyldicyclohexyl methoxy silane, formic acid and SO4 2-/TiO2Solid is strong
1:1.15:1.6:0.002 is added in reaction flask acid catalyst in molar ratio, and stirring is warming up to 95 DEG C, and stirs at this temperature
After mixing reaction 55 minutes, N, N '-dicyclohexylcarbodiimide, the N, N '-dicyclohexylcarbodiimide and dimethyl two is added
The molar ratio of methoxy silane is 2.4:1, continues to react 5 hours at 95 DEG C；
(3) it is down to room temperature after reaction, dilution with toluene is added, is washed with deionized water to neutrality, collects toluene layer, be added
Anhydrous calcium chloride is dry.Desiccant is filtered off, removes toluene after filtrate concentration.The purity of concentrate is 99.28%, and yield is
66.82%, nmr analysis result is (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 2
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, dimethyldimethoxysil,ne in step (2), methyldicyclohexyl methoxy silane, formic acid and
SO4 2-/TiO2Strong solid acid catalyst 1:1.15:1.6:0.001 in molar ratio.The purity of concentrate is 93.64%, and yield is
58.55%, nmr analysis result is (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 3
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, dimethyldimethoxysil,ne in step (2), methyldicyclohexyl methoxy silane, formic acid and
SO4 2-/TiO2Strong solid acid catalyst 1:1.15:1.6:0.004 in molar ratio.The purity of concentrate is 97.35%, and yield is
65.20%, nmr analysis result is (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 4
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, dimethyldimethoxysil,ne in step (2), methyldicyclohexyl methoxy silane, formic acid and
SO4 2-/TiO2Strong solid acid catalyst 1:1.15:1.6:0.005 in molar ratio.The purity of concentrate is 97.42%, and yield is
64.57%, nmr analysis result is (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 5
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, dimethyldimethoxysil,ne, methyldicyclohexyl methoxy silane, organic acid in step (2)
And SO4 2-/TiO2Strong solid acid catalyst 1:1.1:2.0:0.002 in molar ratio.The purity of concentrate is 98.38%, and yield is
59.17%, nmr analysis result is (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 6
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, dimethyldimethoxysil,ne in step (2), methyldicyclohexyl methoxy silane, formic acid and
SO4 2-/TiO2Strong solid acid catalyst 1:1.25:1.8:0.002 in molar ratio.The purity of concentrate is 96.73%, and yield is
61.57%, nmr analysis result is (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 7
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, the present embodiment is by SO4 2-/TiO2Strong solid acid catalyst replaces with acetic anhydride.Concentrate it is pure
Degree is 89.08%, yield 62.85%, and nmr analysis result is (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2
(CH3)。
Embodiment 8
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, the molar ratio of the present embodiment N, N '-dicyclohexylcarbodiimide and dimethyldimethoxysil,ne
For 2:1.The purity of concentrate is 86.36%, yield 58.45%, and nmr analysis result is (CH3)(C6H11)2Si-O-
(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 9
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, the molar ratio of the present embodiment N, N '-dicyclohexylcarbodiimide and dimethyldimethoxysil,ne
For 2.5:1.The purity of concentrate is 96.42%, yield 66.28%, and nmr analysis result is (CH3)(C6H11)2Si-O-
(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 10
The present embodiment (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) preparation method and 1 base of embodiment
This is identical, the difference is that, the molar ratio of the present embodiment N, N '-dicyclohexylcarbodiimide and dimethyldimethoxysil,ne
For 3:1.The purity of concentrate is 96.59%, yield 66.45%, and nmr analysis result is (CH3)(C6H11)2Si-O-
(CH3)2Si-O-Si(C6H11)2(CH3)。
Embodiment 11
The present embodiment (CH3)2(C6H11)Si-O-(CH3)2Si-O-Si(C6H11)(CH3)2Preparation method, including walk as follows
It is rapid:
(1) cyclohexyldimethyl methoxy silane is prepared
S1, dimethyldimethoxysil,ne, magnesium chips and catalyst are weighed in proportion；
S2, justify in tetra- mouthfuls of glass of 250mL with reflux condensing tube, thermometer, blender, heater and balance charging device
In flask, under nitrogen protection, dimethyldimethoxysil,ne, magnesium chips and catalyst is added, is heated to 140 DEG C；
S3, a certain amount of chlorocyclohexane reaction, the charging rate of chlorocyclohexane are first added in the mixed solution of S1
For 0.33g/min；
Reactant in S3 is reacted 3.5h by S4, heat preservation at a reflux temperature；
S5, remaining chlorocyclohexane is added, the reaction was continued, and keeps the temperature 50min, and reaction was completed；
It is 1:2.2:2.1 that total amount and the molar ratio of magnesium chips, which is added, in dimethyldimethoxysil,ne, chlorocyclohexane, wherein
The additional amount of chlorocyclohexane accounts for total amount is added in chlorocyclohexane 35% in S3；The catalyst amount is dimethylformamide dimethyl oxygen
The 0.9% of base silane quality, the catalyst are the mixture of stannous chloride and magnesium nitrate, the quality of stannous chloride and magnesium nitrate
Than for 0.25:1.Reaction solution is evaporated under reduced pressure, 68-78 DEG C/35mmHg fraction is collected, the analysis result of gained fraction is dimethyl
Cyclohexyl methoxy silane yield is 84.34%, purity 98.59%.
(2) by dimethyldimethoxysil,ne, dimethyleyelohexane methoxylsilane, formic acid and SO4 2-/TiO2Solid is strong
1:1.15:1.6:0.002 is added in reaction flask acid catalyst in molar ratio, and stirring is warming up to 95 DEG C, and stirs at this temperature
It mixes reaction after forty minutes, N, N '-dicyclohexylcarbodiimide, the N, N '-dicyclohexylcarbodiimide and dimethyl two is added
The molar ratio of methoxy silane is 2.4:1, continues to react 6 hours at 95 DEG C；
(3) it is down to room temperature after reaction, dilution with toluene is added, is washed with deionized water to neutrality, collects toluene layer, be added
Anhydrous calcium chloride is dry.Desiccant is filtered off, removes toluene after filtrate concentration.The yield of concentrate is 60.75%, and purity is
95.27%, nmr analysis result is (CH3)2(C6H11)Si-O-(CH3)2Si-O-Si(C6H11)(CH3)2。
Embodiment 1-4,7 the result shows that, the dosage and type of catalyst will affect the yield of the based polysiloxane containing hexamethylene,
Using SO4 2-/TiO2Strong solid acid catalyst, the purity and yield for the based polysiloxane containing hexamethylene being prepared are higher.
By embodiment 1, the result of embodiment 5-6 it is found that by adjusting dimethyldimethoxysil,ne, methyldicyclohexyl
Methoxy silane, organic acid and SO4 2-/TiO2The proper ratio of strong solid acid catalyst can effectively improve (CH3)(C6H11)2Si-
O-(CH3)2Si-O-Si(C6H11)2(CH3) purity and yield.
Embodiment 1, embodiment 8-10's the result shows that, N, N '-dicyclohexylcarbodiimide and dimethylformamide dimethyl oxygroup silicon
When the molar ratio of alkane is 2.4:1, (CH3)(C6H11)2Si-O-(CH3)2Si-O-Si(C6H11)2(CH3) purity be up to
99.28%.
The present invention can also be according to R2R3Si(R4)2And RR1(C6H11)Si-R4Different structure, a variety of differences can be synthesized
The based polysiloxane containing hexamethylene of structure.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of preparation method of based polysiloxane containing hexamethylene, which is characterized in that the structural formula of the based polysiloxane containing hexamethylene
As shown in formula (I):
R2R3Si(R4)2And RR1(C6H11)Si-R4, wherein n >=1, R, R1、R2And R3It is identical or not identical, it is respectively and independently selected from
Alkoxy, halogen, alkyl, cyclohexyl, aryl, the alkyl replaced by one or more halogens, acryloyl group and epoxy group one
Valency alkyl；
The preparation method of the based polysiloxane containing hexamethylene, includes the following steps:
(1) by R2R3Si(R4)2、RR1(C6H11)Si-R4, organic acid and catalyst A 1:(1-1.25 in molar ratio): (1-1.8):
(0.001-0.004) is added in reaction flask, and stirring is warming up to 85 DEG C -95 DEG C, and is stirred to react at this temperature 40-60 minutes
Afterwards, be added dehydrating agent, continue 85 DEG C -95 DEG C of reactions 3-6 hours,
Wherein, R, R1、R2And R3It is identical or not identical, it is respectively and independently selected from alkoxy, halogen, alkyl, allyl, aryl, quilt
The monovalent hydrocarbon of alkyl, acryloyl group and epoxy group that one or more halogens replace；R4For halogen or alkoxy；
(2) it is down to room temperature after reaction, non-polar organic solvent dilution is added, is washed with deionized water to neutrality, collects organic
Relevant pressure fraction at a temperature of is collected in phase, drying, filtering, concentration, concentrate vacuum distillation, is obtained described poly- containing cyclohexyl
Siloxanes；
The RR1(C6H11)Si-R4The preparation method comprises the following steps:
S1, R is weighed in proportion1R2R3SiR4, magnesium chips and catalyst B, under nitrogen atmosphere, by R1R2R3SiR4, magnesium chips and catalyst
B mixing, is heated to 90 DEG C -150 DEG C, wherein R1、R2、R3It is identical or different, and R1、R2And R3It is respectively and independently selected from alkoxy, halogen
Element, alkyl, unsaturated alkyl or aryl, R4For alkoxy or halogen；
S2, a certain amount of cyclohexane halide reaction is first added in the mixed solution of S1；
Reactant in S2 is reacted 2-3h by S3, heat preservation at a reflux temperature；
S4, remaining cyclohexane halide is added, the reaction was continued, and keeps the temperature 45-50min；
R1R2R3SiR4, the molar ratio of total amount and magnesium chips is added is 1:(1-2.2 to cyclohexane halide): (1-2.1), wherein halogen in S2
The 30%-40% of cyclohexane halide addition total amount is accounted for for the additional amount of hexamethylene；The catalyst B dosage is R1R2R3SiR4Matter
The 0.7%-1% of amount, the catalyst B are the mixture of stannous chloride and magnesium nitrate.
2. the preparation method of the based polysiloxane according to claim 1 containing hexamethylene, which is characterized in that the organic acid is first
Acid, acetic acid or propionic acid.
3. the preparation method of the based polysiloxane according to claim 1 containing hexamethylene, which is characterized in that the catalyst A is
SO4 2-/TiO2Strong solid acid catalyst.
4. the preparation method of the based polysiloxane according to claim 1 containing hexamethylene, which is characterized in that the dehydrating agent is N,
N '-dicyclohexylcarbodiimide.
5. the preparation method of the based polysiloxane according to claim 4 containing hexamethylene, which is characterized in that the dehydrating agent with
R2R3Si(R4)2Molar ratio be 2-2.5:1.
6. the preparation method of the based polysiloxane according to claim 1 containing hexamethylene, which is characterized in that in the step (1),
R2R3Si(R4)2、RR1(C6H11)Si-R4, organic acid and catalyst A molar ratio be 1:1.15:1.6:0.002.
7. the preparation method of the based polysiloxane according to claim 1 containing hexamethylene, which is characterized in that the nonpolarity is organic
Solvent is at least one of benzene,toluene,xylene, n-hexane, hexamethylene, normal heptane.
8. the preparation method of the based polysiloxane according to claim 1 containing hexamethylene, which is characterized in that the RR1(C6H11)
Si-R4For dicyclohexylmethyl methoxy silane.
9. the preparation method of the based polysiloxane according to claim 8 containing hexamethylene, which is characterized in that urged in the step S1
The dosage of agent is R1R2R3SiR4The 0.9% of quality, the mass ratio of stannous chloride and magnesium nitrate is 0.1- in the catalyst
0.4:1, it is preferable that the mass ratio of stannous chloride and magnesium nitrate is 0.25:1 in the catalyst.
10. the preparation method of the based polysiloxane containing hexamethylene according to claim 8 or claim 9, which is characterized in that the step S2
The additional amount of middle cyclohexane halide accounts for total amount is added in cyclohexane halide 30%.
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