CN103665381B - Synthesis method of hydroxyl capped polydimethylsiloxane - Google Patents
Synthesis method of hydroxyl capped polydimethylsiloxane Download PDFInfo
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- CN103665381B CN103665381B CN201310734257.5A CN201310734257A CN103665381B CN 103665381 B CN103665381 B CN 103665381B CN 201310734257 A CN201310734257 A CN 201310734257A CN 103665381 B CN103665381 B CN 103665381B
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- hydroxyl endblocked
- endblocked polydimethylsiloxane
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Abstract
The invention relates to a synthesis method of hydroxyl capped polydimethylsiloxane. The method comprises the steps of taking dimethyl hydrolysate with the viscosity of 30-50CS and toroidal content of 20-30% as an end capping reagent, taking dimethyl cyclosiloxane (DMC) as a raw material, taking silanol potassium as a catalyst, and synthesizing hydroxyl capped polydimethylsiloxane with the viscosity of 10000-600000CS at 120-170 DEG C, wherein the use amount of the catalyst is 10-50ppm. Hydroxyl capped polydimethylsiloxane can be used for preparing adhesives, potting compounds, sealants and the like for electric and electronic devices. According to the method, the preparation process is simple, the viscosity is accurate to control, the polymerization time is short, the production efficiency is high, and the molecular weight distribution of a product is narrow.
Description
Technical field
The present invention relates to a kind of synthetic method of compound, more particularly, to a kind of conjunction of hydroxyl endblocked polydimethylsiloxane
One-tenth method.
Background technology
Hydroxyl endblocked polydimethylsiloxane (107 silicone rubber) is with hydroxy-end capped straight chain type reactive polysiloxanes, energy
Enough make line style or the cross-linking type polysiloxanes of high molecular weight.It is the basic material preparing room temperature vulcanized silicone rubber etc..In electricity
Being bonded and sealed of sub- components and parts and Macintosh, moistureproof shockproof and insulant aspect have been widely used, with skyscraper
Substantial increase, 107 silicone rubber also greatly increase as the raw materials requirement amount of building sealant.
Introducing the conventional hydroxyl endblocked polydimethylsiloxane method of preparation in document has: typically with dimethyl siloxane ring
Add water based on degraded after the polymerization of body base catalysis, but product has that molecular weight distribution is wider so that dihydroxy gathers
The following process of dimethyl siloxane and serviceability be such as: hardness, toughness, tensile strength, tear resistance, cohesive force, during sulfuration
Between wait and not fully up to expectations.Also useful viscosity is the hydroxyl endblocked polydimethylsiloxane linear body of 50～150cs in linear chlorine
Change polycondensation under phosphazene catalyst to be obtained.
A kind of cn200510068144.1 catalyzed synthesizing alpha of offer, the method for alpha, omega-dihydroxy polydimethyl siloxane,
Under normal pressure, with methyl cyclosiloxane as raw material, catalyst is made using potassium hydroxide, gathered with steam method synthesis α, alpha, omega-dihydroxy
Dimethyl siloxane, with silicon substrate phosphate ester as nertralizer in and polymerizate, then remove low molecule in neutralized reaction product and not anti-
The ring body answered, the α of prepared viscosity 5～80pa s, alpha, omega-dihydroxy polydimethyl siloxane, but viscosity control is inaccurate.
Cn101210074a provides a kind of production α, the method for alpha, omega-dihydroxy polydimethyl siloxane, and described method is: diformazan
Cyclosiloxane is copolymerized with base catalyst, reaches after 500～550 pa s after viscosity, atomized water is sprayed on poly-
Close its surface to be allowed to degradation reaction, de- low-boiling-point substance 2～3h.This kind of biodegrading process has the α making production, ω-dihydroxy
The features such as base polydimethylsiloxane even molecular weight distribution, high income, but viscosity control is inaccurate.
Content of the invention
The present invention is directed to the deficiencies in the prior art it is proposed that a kind of reaction condition is gentle, reaction process is simple, viscosity controls
The accurately synthetic method of hydroxyl endblocked polydimethylsiloxane.
The present invention is achieved through the following technical solutions:
A kind of synthetic method of hydroxyl endblocked polydimethylsiloxane, concrete steps include: by following weight proportion: will
4000 parts of dmc(dimethicone) and 40～400 parts of viscosity be 30～50cs, ring body content be 20～30% diformazan water
Solution thing (Dimethyldichlorosilane hydrolysate) adds in the reaction vessels equipped with agitator, thermometer and condensing reflux pipe, opens
Stirring, is warming up to addition silanol potassium catalyst when 90～150 DEG C, and balancing response 2 hours at 120～170 DEG C, is directly added into
It is neutralized with the phosphoric acid of the same quality of catalyst or its silanol hydrochloric acid glue, continue stirring 1 hour, de- at 1kpa/180 DEG C
To no distillation, obtain final product hydroxyl endblocked polydimethylsiloxane.
Described Dimethyldichlorosilane hydrolysate by Zhejiang Province become civilized synthetic material company limited provide.
In a kind of described synthetic method of hydroxyl endblocked polydimethylsiloxane, catalyst is silanol potassium, and consumption is total
10～50ppm of inventory, preferably 10～20ppm.
In a kind of described synthetic method of hydroxyl endblocked polydimethylsiloxane, hydroxyl endblocked polydimethylsiloxane
Viscosity can be controlled in 10000～600000cs.
This method is by adding quantitative hydrolysate to be used as end-capping reagent so that the response time shortens so that viscosity controls
Accurately, laboratory is reproducible.
Advantages of the present invention is as follows:
1) it is used hydrolysate as end-capping reagent, shorten the response time；
2) it is used hydrolysate as end-capping reagent so that viscosity precise control, product viscosity scope control is within 2%；
3) reaction once can complete, simple production process.
Specific embodiment
Below by embodiment, technical scheme is described in further detail.The invention is not restricted to following
Embodiment, can also have the combination of many operations.Those skilled in the art directly can derive from present disclosure or
The all scenario associated, is all considered to be protection scope of the present invention.
Embodiment 1: a kind of synthetic method of hydroxyl endblocked polydimethylsiloxane, concrete steps include: by following weight
Proportioning: by 4000 parts of dmc(dimethicone) and 40 parts of viscosity be 30cs, ring body content be 30% diformazan hydrolysate (two
Dimethyl dichlorosilane (DMCS) hydrolysate) add in reaction vessels equipped with agitator, thermometer and condensing reflux pipe, open stirring, rise
Temperature adds silanol potassium catalyst to when 90 DEG C, and balancing response 2 hours at 120 DEG C, is directly added into the same quality with catalyst
Phosphoric acid or its silanol hydrochloric acid glue be neutralized, continue stirring 1 hour, take off at 1kpa/180 DEG C to no distillation, that is,
Obtain hydroxyl endblocked polydimethylsiloxane.Viscosity during 25 DEG C of hydroxyl endblocked polydimethylsiloxane of record, yield, viscosity are inclined
Difference, response time and molecular weight distribution value.
Described Dimethyldichlorosilane hydrolysate by Zhejiang Province become civilized synthetic material company limited provide.
In a kind of described synthetic method of hydroxyl endblocked polydimethylsiloxane, catalyst is silanol potassium, and consumption is total
The 10ppm of inventory.
Embodiment 2: a kind of synthetic method of hydroxyl endblocked polydimethylsiloxane, concrete steps include: by following weight
Proportioning: by 4000 parts of dmc(dimethicone) and 400 parts of viscosity be 50cs, ring body content be 20% diformazan hydrolysate
(Dimethyldichlorosilane hydrolysate) adds in the reaction vessels equipped with agitator, thermometer and condensing reflux pipe, opens stirring,
It is warming up to addition silanol potassium catalyst when 150 DEG C, and balancing response 2 hours at 170 DEG C, it is directly added into the same matter with catalyst
The phosphoric acid of amount or its silanol hydrochloric acid glue are neutralized, and continue stirring 1 hour, take off at 1kpa/180 DEG C to no distillation,
Obtain final product hydroxyl endblocked polydimethylsiloxane.Viscosity during 25 DEG C of hydroxyl endblocked polydimethylsiloxane of record, yield, viscosity are inclined
Difference, response time and molecular weight distribution value.
In a kind of described synthetic method of hydroxyl endblocked polydimethylsiloxane, catalyst is silanol potassium, and consumption is total
The 50ppm of inventory.
Remaining is with embodiment 1.
Embodiment 3: a kind of synthetic method of hydroxyl endblocked polydimethylsiloxane, concrete steps include: by following weight
Proportioning: by 4000 parts of dmc(dimethicone) and 240 parts of viscosity be 40cs, ring body content be 25% diformazan hydrolysate
(Dimethyldichlorosilane hydrolysate) adds in the reaction vessels equipped with agitator, thermometer and condensing reflux pipe, opens stirring,
It is warming up to addition silanol potassium catalyst when 120 DEG C, and balancing response 2 hours at 150 DEG C, it is directly added into the same matter with catalyst
The phosphoric acid of amount or its silanol hydrochloric acid glue are neutralized, and continue stirring 1 hour, take off at 1kpa/180 DEG C to no distillation,
Obtain final product hydroxyl endblocked polydimethylsiloxane.Viscosity during 25 DEG C of hydroxyl endblocked polydimethylsiloxane of record, yield, viscosity are inclined
Difference, response time and molecular weight distribution value.
In a kind of described synthetic method of hydroxyl endblocked polydimethylsiloxane, catalyst is silanol potassium, and consumption is total
The 20ppm of inventory.
Remaining is with embodiment 1.
Embodiment 4: a kind of synthetic method of hydroxyl endblocked polydimethylsiloxane, concrete steps include: by following weight
Proportioning: by 4000 parts of dmc(dimethicone) and 30 parts of viscosity be 20cs, ring body content be 40% diformazan hydrolysate (two
Dimethyl dichlorosilane (DMCS) hydrolysate) add in reaction vessels equipped with agitator, thermometer and condensing reflux pipe, open stirring, rise
Temperature adds silanol potassium catalyst to when 80 DEG C, and balancing response 2 hours at 110 DEG C, is directly added into the same quality with catalyst
Phosphoric acid or its silanol hydrochloric acid glue be neutralized, continue stirring 1 hour, take off at 1kpa/180 DEG C to no distillation, that is,
Obtain hydroxyl endblocked polydimethylsiloxane.Viscosity during 25 DEG C of hydroxyl endblocked polydimethylsiloxane of record, yield, viscosity are inclined
Difference, response time and molecular weight distribution value.
In a kind of described synthetic method of hydroxyl endblocked polydimethylsiloxane, catalyst is silanol potassium, and consumption is total
The 8ppm of inventory.
Remaining is with embodiment 1.
Embodiment 5: a kind of synthetic method of hydroxyl endblocked polydimethylsiloxane, concrete steps include: by following weight
Proportioning: by 4000 parts of dmc(dimethicone) and 420 parts of viscosity be 60cs, ring body content be 15% diformazan hydrolysate
(Dimethyldichlorosilane hydrolysate) adds in the reaction vessels equipped with agitator, thermometer and condensing reflux pipe, opens stirring,
It is warming up to addition silanol potassium catalyst when 160 DEG C, and balancing response 2 hours at 180 DEG C, it is directly added into the same matter with catalyst
The phosphoric acid of amount or its silanol hydrochloric acid glue are neutralized, and continue stirring 1 hour, take off at 1kpa/180 DEG C to no distillation,
Obtain final product hydroxyl endblocked polydimethylsiloxane.Viscosity during 25 DEG C of hydroxyl endblocked polydimethylsiloxane of record, yield, viscosity are inclined
Difference, response time and molecular weight distribution value.
In a kind of described synthetic method of hydroxyl endblocked polydimethylsiloxane, catalyst is silanol potassium, and consumption is total
The 60ppm of inventory.
Remaining is with embodiment 1.
Embodiment 6: a kind of synthetic method of hydroxyl endblocked polydimethylsiloxane, concrete steps include: by following weight
Proportioning: by 4000 parts of dmc(dimethicone) and 120 parts of viscosity be 20cs, ring body content be 40% diformazan hydrolysate
(Dimethyldichlorosilane hydrolysate) adds in the reaction vessels equipped with agitator, thermometer and condensing reflux pipe, opens stirring,
It is warming up to addition silanol potassium catalyst when 80 DEG C, and balancing response 2 hours at 180 DEG C, it is directly added into the same matter with catalyst
The phosphoric acid of amount or its silanol hydrochloric acid glue are neutralized, and continue stirring 1 hour, take off at 1kpa/180 DEG C to no distillation,
Obtain final product hydroxyl endblocked polydimethylsiloxane.Viscosity during 25 DEG C of hydroxyl endblocked polydimethylsiloxane of record, yield, viscosity are inclined
Difference, response time and molecular weight distribution value.
In a kind of described synthetic method of hydroxyl endblocked polydimethylsiloxane, catalyst is silanol potassium, and consumption is total
The 20ppm of inventory.
Remaining is with embodiment 1.
Comparative example 1:
The Chinese patent of cn 102558563 discloses a kind of preparation method of high viscosity 107 silicone rubber, by following weight
Proportioning: 300 parts of dmc are added in the reaction vessels equipped with agitator, thermometer and condensing reflux pipe, opens stirring, at 60 DEG C,
It is dehydrated 20min under 2kpa, eliminates vacuum, be warming up to when 110 DEG C and add the catalysis of 25ppm tetrabutylammonium hydroxide phosphorus silanol saline and alkaline glue
Agent, reacts 2.5 hours at this temperature, plus 0.07 part of water degraded, heats up and decomposes base catalyst, then in 1kpa after 3 hours
Take off to no distillation at/180 DEG C, obtain viscosity (25 DEG C) 460,000 cs, high-viscosity 107 silicone rubber of water white transparency, yield
63.7%, viscosity deviation is 10%, and total reaction time is 5.5 hours, and molecular weight distribution value is 2.24.
Comparative example 2:
A kind of preparation method of 107 silicone rubber, by following weight proportion: 300 parts of dmc are added equipped with agitator, temperature
In the reaction vessels of meter and condensing reflux pipe, open stirring, at 60 DEG C, under 2kpa, be dehydrated 20min, eliminate vacuum, be warming up to 120
DEG C when add 15ppm potassium hydroxide catalyst, and react 1 hour at 150 DEG C, add the degraded of 0.09 part of water, after 5 hours plus
15ppm phosphoric acid is neutralized, and then takes off to no distillation at 1kpa/180 DEG C, obtains viscosity (25 DEG C) 100,000 cs, no
107 transparent silicone rubber of color, yield 73.7%, viscosity deviation is 25%, and total reaction time is 6 hours, and molecular weight distribution value is
2.18.Blending can obtain 107 silicone rubber that viscosity is 80,000 cs by adding 107 glue that viscosity is 10,000 cs.
The various products parameter of the hydroxyl endblocked polydimethylsiloxane that embodiment 1-6 and comparative example 1-2 are obtained by we
Compare, the results are shown in Table 1.
The various products parameter of table 1 hydroxyl endblocked polydimethylsiloxane
Note: it is more accurate that viscosity deviation less explanation viscosity controls.
As it can be seen from table 1 embodiment 1-3(items technical parameter all in technical scheme) be obtained hydroxyl
End-blocking polydimethylsiloxane yield, viscosity deviation, molecular weight distribution value, response time are superior to other embodiments and contrast
Example, illustrates that the hydroxyl endblocked polydimethylsiloxane that the present invention is obtained has even molecular weight distribution, high income, viscosity control standard
Really, response time short advantage.
Claims (2)
1. a kind of synthetic method of hydroxyl endblocked polydimethylsiloxane it is characterised in that: concrete steps include: by following weight
Proportioning: by 4000 parts of dmc and 40～400 part of viscosity be 30～50cs, ring body content be 20～30% diformazan hydrolysate add dress
Have in the reaction vessels of agitator, thermometer and condensing reflux pipe, open stirring, be warming up to addition silanol potassium when 90～150 DEG C
Catalyst, and balancing response 2 hours at 120～170 DEG C, are directly added into the phosphoric acid with the same quality of catalyst or its silicon alkoxide
Sour glue is neutralized, and continues stirring 1 hour, takes off to no distillation, obtain final product hydroxy-end capped poly- diformazan at 1kpa/180 DEG C
Radical siloxane；Described catalyst is silanol potassium, and consumption is 10～50ppm of total amount of feeding.
2. as claimed in claim 1 a kind of synthetic method of hydroxyl endblocked polydimethylsiloxane it is characterised in that: a kind of hydroxyl
Base blocks the synthetic method of polydimethylsiloxane, and concrete steps include: by following weight proportion: by 4000 parts dmc and 240 part
The diformazan hydrolysate that viscosity is 40cs, ring body content is 25% adds the reactor equipped with agitator, thermometer and condensing reflux pipe
In ware, open stirring, be warming up to addition silanol potassium catalyst when 120 DEG C, and balancing response 2 hours at 150 DEG C, it is directly added into
It is neutralized with the phosphoric acid of the same quality of catalyst or its silanol hydrochloric acid glue, continue stirring 1 hour, de- at 1kpa/180 DEG C
To no distillation, obtain final product hydroxyl endblocked polydimethylsiloxane.
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| CN111072969A (en) * | 2019-12-31 | 2020-04-28 | 浙江新安化工集团股份有限公司 | Preparation method of viscosity-controllable hydroxyl-terminated polymethylphenylsiloxane |
| CN112831049A (en) * | 2021-03-09 | 2021-05-25 | 浙江新安化工集团股份有限公司 | Preparation method of alpha, omega-dihydroxy polydimethylsiloxane |
| CN113985701A (en) * | 2021-12-06 | 2022-01-28 | 潍坊星泰克微电子材料有限公司 | Negative photoresist composition, preparation method and method for forming photoresist pattern |
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Effective date of registration: 20170111 Address after: 330319 Jiangxi province Jiujiang Yongxiu County Yangjialing Patentee after: JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE CO., LTD. Address before: 330319 Jiangxi province Jiujiang Yongxiu County Yangjialing Patentee before: Jiangxi Xinghuo Organo-Silicon Plant, Lanxing Chemical New Material Co., Ltd. |