CN101798388A - Method for preparing poly-methyl siloxane through catalytic synthesis by using active bentonite - Google Patents
Method for preparing poly-methyl siloxane through catalytic synthesis by using active bentonite Download PDFInfo
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Abstract
The invention relates to a method for preparing poly-methyl siloxane through catalytic synthesis by using active bentonite, in particular to a method for preparing a series of poly-methyl siloxane products, such as methyl silicone oil, phenyl silicone oil, vinyl silicone oil, addition silicone rubber base and other products, from polymeric monomers including Dn, DnH, DnPh and DnVi and blocking agent in the presence of activated bentonite as a catalyst. The poly-methyl siloxane products prepared by the invention have the advantages of high single-pass conversion, wide viscosity range and good quality, and the method of the invention has the advantages of low cost, mild reaction conditions, simple process, convenient operation, pollution-free application, easy industrialization and the like. Therefore, the invention is particularly suitable to use as silicone oil, additives and silicone rubber products in the fields of automobile, electronics, aerospace, food, medicine and the like.
Description
Technical field
The present invention relates to a kind of preparation method of polymethyl siloxane, specifically be meant the preparation method who uses active bentonite to make the synthetic polymethyl siloxane of catalyst.
Technical background
Polymethyl siloxane is to have a most important series products in the organopolysiloxane of many special performances, and the polymethyl siloxane product comprises the basic glue of methyl-silicone oil, phenyl silicone oil, containing hydrogen silicone oil, vinyl silicone oil or addition-type silicon rubber.Normally by an acidic catalysts such as basic catalysts such as potassium hydroxide, Tetramethylammonium hydroxide and tetrabutylammonium hydroxide phosphorus and silicon alkoxide thereof or the vitriol oil, sulfonic fluoropolymer, phosphoric acid, catalytic polymerization is prepared from.
Adopt above-mentioned catalyst to synthesize polymethyl siloxane, catalyzer need be neutralized or the inactivation processing, technology is loaded down with trivial details on the one hand, cost is high, can make Pt catalyst poisoning in the add-on type sulphurated siliastic such as meeting owing to the catalyzer that contains element impurity such as S, N, P, Cl of remnants or the quality that neutralizing agent influences the polymethyl siloxane product on the other hand.In addition, because crosslinking reaction can take place in silicon hydrogen group and alkaline matter, vinyl group is met the strongly-acid material can generate ethene, and other side reaction, makes these catalyzer be restricted when producing the isostructural polymethyl siloxane product of siliceous hydrogen, vinyl group.
Summary of the invention
The present invention is directed to the deficiency in the polymethyl siloxane product technologies such as the synthetic silicone oil of existing strong basicity or strongly acidic catalyst catalysis, silicon rubber, a kind of method with the active bentonite preparing poly-methyl siloxane through catalytic synthesis is provided.
Terminological interpretation:
1、D
n、D
n H、D
n Ph、D
n Vi
D
n: the dimethyl cyclosiloxane write a Chinese character in simplified form D
n H: the methyl hydrogen cyclosiloxane write a Chinese character in simplified form D
n Ph: methyl phenyl ring siloxane write a Chinese character in simplified form D
n Vi: the writing a Chinese character in simplified form of methyl ethylene cyclosiloxane, but market is bought.
2, DMC is the abbreviation of dimethyl siloxane ring body.
3. active bentonite catalyzer, main component is SiO
2XAl
2O
3NH
2O.But market is bought.
Many particular performances such as that described wilkinite has is strong as swelling, thixotroping shape, adsorptivity, cation exchange capacity (CEC), catalytic activity height are called as " omnipotent soil ".Particularly active bentonite has excellent catalytic capability.Active bentonite is very sophisticated product, can buy the back by market and directly use.
4. polymethyl siloxane product comprises the basic glue of methyl-silicone oil, phenyl silicone oil, containing hydrogen silicone oil, vinyl silicone oil or addition-type silicon rubber.
The present invention is achieved by following technical proposals:
A kind of preparation method of polymethyl siloxane is with dimethyl cyclosiloxane (D
n), methyl hydrogen cyclosiloxane (D
n H), methyl phenyl ring siloxane (D
n Ph), methyl ethylene cyclosiloxane (D
n Vi) in one or more be the monomer of polyreaction, D
n, D
n H, D
n Ph, D
n ViChemical structural formula respectively as follows:
Above-mentioned D
n, D
n H, D
n Ph, D
n ViN in the chemical structural formula is 3～8 integer;
With material with following formula I structure end-capping reagent as polyreaction,
R wherein is H, methyl, vinyl, chloropropyl, trifluoro propyl, chain alkyl, fluorine replacement chain alkyl, phenyl, cyclohexyl methoxy or ethoxy group.Preferred R is H, methyl, vinyl or methoxyl group.
With the active bentonite is catalyzer;
Add monomer, catalyzer and the end-capping reagent of the polyreaction of certain mass in reaction unit, temperature of reaction is stabilized in 50 ℃-160 ℃, the reaction times is 1-16h; After reaction finished, catalyzer was removed in pressure filtration, and low-boiling-point substance is taken out in decompression, got the polymethyl siloxane target product.
As preferably, the polymerization reaction monomer D described in the above-mentioned preparation method
n, D
n H, D
n Ph, D
n ViN be 3,4,5 or 6.
As preferably, the end-capping reagent of the polyreaction described in the above-mentioned preparation method is selected from 1,1,3,3-tetramethyl--1,3-dihydro sily oxide (HM), hexamethyldisiloxane (MM) or 1,1,3,3-tetramethyl--1,3-divinyl disiloxane (VM).The consumption of end-capping reagent is the 0.2%-50% of polymerization single polymerization monomer quality, and preferable amount is 0.3%-20%.
As preferably, the main component of the active bentonite catalyzer described in the above-mentioned preparation method is SiO
2XAl
2O
3NH
2O.As preferably, the consumption of the active bentonite among the above-mentioned preparation method is the 1-50% of polymerization single polymerization monomer quality.Further preferred, the consumption of the active bentonite among the above-mentioned preparation method is the 4-16% of polymerization single polymerization monomer quality.
As preferably, the temperature of reaction among the above-mentioned preparation method is 85 ℃-105 ℃, and polymerization reaction time is 2-10h.Further preferred temperature of reaction is 90-100 ℃, and the reaction times is 3-6h.As a kind of optimal selection, temperature of reaction is 95 ℃, and the reaction times is 4h.
As preferably, the pressure filtration described in the above-mentioned preparation method removes catalyzer, and pressure is 0.1-0.3MPa.
For the purity that makes target product is higher, after low-boiling-point substance is taken out in the decompression in above-mentioned preparation method, be warming up to 180 ℃, in the polymethyl siloxane product, add gac and stir, pressure filtration gets water white polymethyl siloxane then.
Preferably, the gac of above-mentioned adding is the 1-10wt% powder food product level gac of polymethyl siloxane product, can obtain effect preferably.
Technical characterstic of the present invention and beneficial effect are as follows:
1, to adopt active bentonite be solid catalyst in the present invention, can save in the prior art in the catalyzer and Processes and apparatus, and the active bentonite catalyzer can be fixed in the reactor, and be suitable for continuous production processes.
2, to adopt active bentonite be catalyzer in the present invention, because of it has greater activity, can be under lower temperature product such as catalysis silicone oil synthetic, its preferred temperature of reaction is 90-100 ℃, and the reaction times is shorter.110-150 ℃ temperature range with respect to the continuous processing of catalyzer such as industrial potassium hydroxide, Tetramethylammonium hydroxide and silicon alkoxide thereof is produced silicone oil or silicon rubber has higher power savings advantages.
3, adopt the technology of active bentonite Preparation of Catalyst polymethyl siloxane product of the present invention, because the catalytic activity height, and can not cause silicon hydrogen group generation side reaction, be particularly suitable for the preparation of hydrogenous polymethyl siloxane product such as containing hydrogen silicone oil.In addition, because the composition of catalyzer is single relatively, need not to use the toluene equal solvent in the reaction process, sorption by high quality active carbon again after reaction finishes, the quality height of prepared containing hydrogen silicone oil product, residual impurity is few, helps improving the quality of products such as add-on type sulphurated siliastic, modified silicon oil.
4, adopt active bentonite catalyst of the present invention to prepare polymethyl siloxane products such as silicone oil, silicon rubber, it is low to have a cost, mild condition, technology is simple, and is easy and simple to handle, pollution-free, be convenient to advantages such as industrialization, the impurity that especially has products obtained therefrom is few, the quality advantages of higher.
5, adopt the method for the invention can prepare high-quality polymethyl siloxane product, as the basic glue of methyl-silicone oil, phenyl silicone oil, containing hydrogen silicone oil, vinyl silicone oil or addition-type silicon rubber.Adopt present method to prepare the per pass conversion height of polymethyl siloxane product, the product viscosity haves a wide reach, have advantages such as colourless, tasteless, transparent, heat-resisting, resistance to acids and bases, be particularly suitable for silicone oil, additive and silastic product etc. in automobile, electronic apparatus, aerospace, the food medicine and other fields.
Specific implementation method
The present invention can be described further by following embodiment, but embodiment is not a limiting the scope of the invention.The catalyst activity wilkinite that uses among the embodiment is available from Suisawa Chemical Industry Co., Ltd..
Embodiment 1, methyl-silicone oil
In the reaction unit that mechanical stirring, thermometer, serpentine condenser are installed, add 100 parts of polymerization reaction monomer octamethylcyclotetrasiloxane (D
4), add 10 parts of catalyst activity wilkinites then, 2.5 parts of hexamethyldisiloxane of disposable adding (MM) end-capping reagent at the charging opening place.Behind the sealed reaction device, the temperature of reaction system is risen to 100 ℃, stop behind the constant 4h stirring and leave standstill.
To be cooled to the reaction mixture of room temperature, be transferred in the strainer, be forced into 0.15MPa and filter, reclaim the active bentonite catalyzer, obtaining polydimethylsiloxane simultaneously is methyl-silicone oil filtrate.
Be decompressed to-0.098MPa, be warming up to 180 ℃ gradually and remove lower-molecular substance, cooling obtains water white methyl-silicone oil.Food grade gac add silicone oil quality 5% in methyl-silicone oil stirs 2h, and pressure filtration obtains as clear as crystal methyl-silicone oil product.As calculated, the per pass conversion of this reaction is 88.1%.
The about 100mPas of the rotary viscosity of gained methyl-silicone oil product (25 ℃, down with), volatile content (150 ℃, 1h, down with) be 0.2%, pH value (mixes with acetone, water stir 2h after, with the pH meter survey, under together) be 6.5, refractive index n
D 25Be 1.4025, it is 6.1 * 10 that GPC records number-average molecular weight (Mn)
3, molecular weight distribution width (MWD) is 2.1.
Embodiment 2,
Adopt the method identical, with 100 parts of D with embodiment 1
4Be polymerization single polymerization monomer, 10 parts of active bentonite catalyzer, 0.3 part of MM is an end-capping reagent, after polyreaction and aftertreatment finish, obtains water white methyl-silicone oil.As calculated, the per pass conversion of this reaction is 87.6%.
The about 5100mPas of rotary viscosity of gained methyl-silicone oil product, volatile content is 0.1%, the pH value is 6.7, refractive index n
D 25Be 1.4040, it is 4.9 * 10 that GPC records number-average molecular weight (Mn)
4, molecular weight distribution width (MWD) is 2.5.
Embodiment 3
Adopt the method identical, with 100 parts of D with embodiment 1
4Be polymerization single polymerization monomer, 10 parts of active bentonite catalyzer, 2.5 parts MM are end-capping reagent, after 80 ℃ of reactions 8h and aftertreatments finish, obtain water white methyl-silicone oil.As calculated, the per pass conversion of this reaction is 85.5%.
The about 95mPas of rotary viscosity of gained methyl-silicone oil product, volatile content is 0.3%, the pH value is 6.7, refractive index n
D 25Be 1.4025, it is 6.0 * 10 that GPC records number-average molecular weight (Mn)
3, molecular weight distribution width (MWD) is 2.5.
Embodiment 4
Adopt the method identical, with 100 parts of D with embodiment 1
4Be polymerization single polymerization monomer, 10 parts of active bentonite catalyzer, 2.5 parts MM are end-capping reagent, after 110 ℃ of reactions 3h and aftertreatments finish, obtain water white methyl-silicone oil.As calculated, the per pass conversion of this reaction is 88.1%.
The about 110mPas of rotary viscosity of gained methyl-silicone oil product, volatile content is 0.2%, the pH value is 6.7, refractive index n
D 25Be 1.4025, it is 6.1 * 10 that GPC records number-average molecular weight (Mn)
3, molecular weight distribution width (MWD) is 2.1.
Embodiment 5
Adopt the method identical, with 100 parts of D with embodiment 1
4Be polymerization single polymerization monomer, 6 parts of active bentonite catalyzer, 2.5 parts MM are end-capping reagent, after 100 ℃ of reactions 4h and aftertreatments finish, obtain water white methyl-silicone oil.As calculated, the per pass conversion of this reaction is 85.3%.
The about 95mPas of rotary viscosity of gained methyl-silicone oil product, volatile content is 0.1%, the pH value is 6.7, refractive index n
D 25Be 1.4025, it is 6.0 * 10 that GPC records number-average molecular weight (Mn)
3, molecular weight distribution width (MWD) is 2.3.
Embodiment 6
Adopt the method identical, with 100 parts of D with embodiment 1
4Be polymerization single polymerization monomer, 6 parts of active bentonite catalyzer, 14.6 parts MM are end-capping reagent, after 100 ℃ of reactions 4h and aftertreatments finish, obtain water white methyl-silicone oil.As calculated, the per pass conversion of this reaction is 70.5%.
The about 11mPas of rotary viscosity of gained methyl-silicone oil product, volatile content is 0.2%, the pH value is 6.7, refractive index n
D 25Be 1.4005, it is 1.5 * 10 that GPC records number-average molecular weight (Mn)
3, molecular weight distribution width (MWD) is 2.1.
Embodiment 7
Adopt the method identical, with 100 parts of D with embodiment 1
4Be polymerization single polymerization monomer, 6 parts of active bentonite catalyzer, 0.32 part MM are end-capping reagent, after 100 ℃ of reactions 4h and aftertreatments finish, obtain water white methyl-silicone oil.As calculated, the per pass conversion of this reaction is 85.6%.
The about 5160mPas of rotary viscosity of gained methyl-silicone oil product, volatile content is 0.2%, the pH value is 6.7, refractive index n
D 25Be 1.4025, it is 5.3 * 10 that GPC records number-average molecular weight (Mn)
4, molecular weight distribution width (MWD) is 2.4.
Embodiment 8, vinyl silicone oil
Adopt the method identical, with 100 parts of D with embodiment 1
4Be polymerization single polymerization monomer, 10 parts of active bentonite catalyzer, 0.9 part 1,1,3,3-tetramethyl--1,3-divinyl disiloxane VM is an end-capping reagent, after the 100 ℃ of reaction polyreactions of 4h and aftertreatment finish, obtains water white vinyl silicone oil.As calculated, the per pass conversion of this reaction is 87.5%.
The about 1060mPas of rotary viscosity of gained vinyl silicone oil product, contents of ethylene is 0.65%.Volatile content is 0.3%, and the pH value is 6.7, refractive index n
D 25Be 1.4040, it is 2.2 * 10 that GPC records number-average molecular weight (Mn)
4, molecular weight distribution width (MWD) is 2.4.
Embodiment 9
Adopt the method identical, with 96 parts of D with embodiment 1
4, 4 parts of D
4 ViBe polymerization single polymerization monomer, 10 parts of active bentonite catalyzer, 0.9 part 1,1,3,3-tetramethyl--1,3-divinyl disiloxane VM is an end-capping reagent, after the 100 ℃ of reaction polyreactions of 4h and aftertreatment finish, obtains water white vinyl silicone oil.As calculated, the per pass conversion of this reaction is 87.5%.
The about 1030mPas of rotary viscosity of gained vinyl silicone oil product, contents of ethylene is 4.1%.Volatile content is 0.3%, and the pH value is 6.7, refractive index n
D 25Be 1.4040, it is 2.3 * 10 that GPC records number-average molecular weight (Mn)
4, molecular weight distribution width (MWD) is 2.6.
Embodiment 10, containing hydrogen silicone oil
Adopt the method identical with embodiment 1, with 100 parts of D4 is polymerization single polymerization monomer, 10 parts of active bentonite catalyzer, 3.8 1,1,3 of part, 3-tetramethyl--1,3-dihydro sily oxide (HM) is an end-capping reagent, after the polyreaction of reaction 4h and aftertreatment finish under 90 ℃ the temperature, obtains water white containing hydrogen silicone oil.As calculated, the per pass conversion of this reaction is 87.0%.
The about 55mPas of rotary viscosity of gained containing hydrogen silicone oil product, hydrogen richness is 0.05%, and volatile content is 0.1%, and the pH value is 6.5, refractive index n
D 25Be 1.4010, it is 3.6 * 10 that GPC records number-average molecular weight (Mn)
3, molecular weight distribution width (MWD) is 1.9.
Embodiment 11, containing hydrogen silicone oil
Adopt the method identical with embodiment 1, with 100 parts of D4 is polymerization single polymerization monomer, 10 parts of active bentonite catalyzer, 3.8 1,1,3 of part, 3-tetramethyl--1,3-dihydro sily oxide (HM) is an end-capping reagent, after the polyreaction of reaction 4h and aftertreatment finish under 90 ℃ the temperature, obtains water white containing hydrogen silicone oil.As calculated, the per pass conversion of this reaction is 87.0%.
The about 55mPas of rotary viscosity of gained containing hydrogen silicone oil product, hydrogen richness is 0.36%, and volatile content is 0.1%, and the pH value is 6.5, refractive index n
D 25Be 1.4010, it is 4.1 * 10 that GPC records number-average molecular weight (Mn)
3, molecular weight distribution width (MWD) is 2.1.
Claims (10)
1. the preparation method of a polymethyl siloxane is with dimethyl cyclosiloxane (D
n), methyl hydrogen cyclosiloxane (D
n H), methyl phenyl ring siloxane (D
n Ph), methyl ethylene cyclosiloxane (D
n Vi) in one or more be the monomer of polyreaction, D
n, D
n H, D
n Ph, D
n ViChemical structural formula respectively as follows:
Above-mentioned D
n, D
n H, D
n Ph, D
n ViN in the chemical structural formula is 3～8 integer;
With material with following formula I structure end-capping reagent as polyreaction,
R wherein is H, methyl, vinyl, chloropropyl, trifluoro propyl, chain alkyl, fluorine replacement chain alkyl, phenyl, cyclohexyl methoxy or ethoxy group; Preferred R is H, methyl, vinyl or methoxyl group;
With the active bentonite is catalyzer;
Add monomer, catalyzer and the end-capping reagent of the polyreaction of certain mass in reaction unit, polymeric reaction temperature is stabilized in 50 ℃-160 ℃, the reaction times is 1-16h; After reaction finished, catalyzer was removed in pressure filtration, and low-boiling-point substance is taken out in decompression, got the polymethyl siloxane target product.
2. preparation method as claimed in claim 1 is characterized in that described polymerization reaction monomer D
n, D
n H, D
n Ph, D
n ViN be 3,4,5 or 6.
3. preparation method as claimed in claim 1 is characterized in that the end-capping reagent of described polyreaction is selected from 1,1,3,3-tetramethyl--1,3-dihydro sily oxide, hexamethyldisiloxane or 1,1,3,3-tetramethyl--1,3-divinyl disiloxane.
4. as claim 1 or 3 described preparation methods, the consumption that it is characterized in that active bentonite is the 1-50% of polymerization single polymerization monomer quality; Wherein the consumption of preferred active bentonite is the 4-16% of polymerization single polymerization monomer quality.
5. as claim 1 or 3 described preparation methods, the consumption that it is characterized in that end-capping reagent is the 0.2%-50% of polymerization single polymerization monomer quality, and preferable amount is 0.3%-20%.
6. preparation method as claimed in claim 1 is characterized in that polymeric reaction temperature is 85 ℃-105 ℃, and polymerization reaction time is 2-10h.
7. preparation method as claimed in claim 1 is characterized in that polymeric reaction temperature is 90-100 ℃, and the reaction times is 3-6h; Wherein most preferably temperature of reaction is 95 ℃, and the reaction times is 4h.
8. preparation method as claimed in claim 1 is characterized in that described pressure filtration removes catalyzer, and pressure is 0.1-0.3MPa.
9. preparation method as claimed in claim 1, it is characterized in that low-boiling-point substance is taken out in decompression after, be warming up to 180 ℃, in the polymethyl siloxane product, add gac and stir, pressure filtration gets water white polymethyl siloxane then.
10. preparation method as claimed in claim 9 is characterized in that the gac that adds is the 1-10wt% powder food product level gac of polymethyl siloxane product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709407A (en) * | 2013-11-29 | 2014-04-09 | 山东东岳有机硅材料有限公司 | Preparation method of phenyl silicone oil |
| CN115322378A (en) * | 2022-07-25 | 2022-11-11 | 佳化化学科技发展（上海）有限公司 | Hydrogen-terminated silicone oil, terminal polyether silicone oil, and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709407A (en) * | 2013-11-29 | 2014-04-09 | 山东东岳有机硅材料有限公司 | Preparation method of phenyl silicone oil |
| CN103709407B (en) * | 2013-11-29 | 2016-03-09 | 山东东岳有机硅材料有限公司 | A kind of preparation method of phenyl silicone oil |
| CN115322378A (en) * | 2022-07-25 | 2022-11-11 | 佳化化学科技发展（上海）有限公司 | Hydrogen-terminated silicone oil, terminal polyether silicone oil, and preparation method and application thereof |
| CN115322378B (en) * | 2022-07-25 | 2023-09-15 | 佳化化学科技发展（上海）有限公司 | Hydrogen-terminated silicone oil, polyether-terminated silicone oil, and preparation methods and applications thereof |
| WO2024021968A1 (en) * | 2022-07-25 | 2024-02-01 | 佳化化学科技发展（上海）有限公司 | Hydrogen-terminated silicone oil, terminated polyether modified silicone oil, preparation methods therefor, and uses thereof |
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Open date: 20100811 |