CN102070785A - Preparation method of hydroxyl-terminated polymethylphenyl sioxane - Google Patents

Preparation method of hydroxyl-terminated polymethylphenyl sioxane Download PDF

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CN102070785A
CN102070785A CN2010105672261A CN201010567226A CN102070785A CN 102070785 A CN102070785 A CN 102070785A CN 2010105672261 A CN2010105672261 A CN 2010105672261A CN 201010567226 A CN201010567226 A CN 201010567226A CN 102070785 A CN102070785 A CN 102070785A
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hydroxy
end capped
preparation
hydrolyzate
capped psi
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陈雪忠
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HANGZHOU SAIMO SCIENCE AND TECHNOLOGY Co Ltd
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HANGZHOU SAIMO SCIENCE AND TECHNOLOGY Co Ltd
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Abstract

The invention relates to a preparation method of hydroxyl-terminated polymethylphenyl sioxane. The preparation method is characterized by comprising the following steps: (a) weighting methylphenyldichlorosilane hydrolyzate, dimethyldichlorosilane hydrolyzate, methylphenylcyclosiloxane and alkali metal silicon alkoxide according to a certain ratio to add in a reaction tank provided with a mixer, a thermometer and a reflux condenser; (b) vacuumizing the reaction tank at 60-80 DEG C to 0.02-0.095MPa, removing a small amount of water in the reactants; (c) increasing the reaction temperature to 130-170 DEG C to perform polymerization reaction for 2-8h; (d) adding phosphoric acid-alkyl alcohol solution to adjust the pH value of the solution in the reaction tank to 6-7, mixing 0.5-1h; and (e) increasing the reaction temperature to 160-190 DEG C, starting a vacuum pump for 0.5-2h to ensure that the pressure is 0.095-0.1MPa and removing low molecular-weight substances to obtain hydroxyl-terminated polymethylphenyl sioxane. The preparation method of the invention has the advantages of mild and controllable polymerization process and easy operation process.

Description

A kind of preparation method of hydroxy-end capped PSI
Technical field
The present invention relates to chemical technology field, particularly a kind of preparation method of hydroxy-end capped PSI.
Background technology
Methyl polysiloxane has advantages such as good thermostability, electrical insulating property, weathering resistance, ozone resistance, ventilation property, very high transparency, good thermal diffusivity and excellent cementability, flowability, and the polysiloxane that contains phenyl more is better than polydimethylsiloxane at aspects such as resistance to elevated temperatures, damping capacity, radiation resistances, has more wide application prospect.
The production technique of traditional hydroxy-end capped polysiloxane is to be the polymerization system of raw material with annular siloxane or alkoxyl silicone functional silicone, under acid or base catalysis, carry out the high temperature ring-opening polymerization and produce full-bodied polymkeric substance, hydrolysis telomerizes then, obtains low viscous product.As people such as gold-tinted speed at " China Synthetic Rubber Industry " (2004) 27,10-12 has reported that with aminomethyl phenyl diethoxy silane and octamethylcyclotetrasiloxane be raw material, ring opening copolymer under base catalysis, feed the water vapor degraded at last, prepared the hydroxy-end capped PSI oligopolymer of high phenyl content.Want the water content in the strict control raw material in reaction process, and the used moisture content of degraded superpolymer viscosity after the polymerization, not miscible with polysiloxane because water is inorganics, simultaneously, what of water content directly have influence on product degree of polymerization and viscosity.So this technology exists reaction process medium viscosity and process to be difficult to regulation and control, the unsettled defective of product batches.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of more convenient, the preparation method of the hydroxy-end capped PSI that is easy to control.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of hydroxy-end capped PSI, described hydroxy-end capped PSI can be used general formula
Expression, wherein x, y are the polymerization degree, x=1-100, y=1-50 is characterized in that adopting following steps:
(a) according to proportioning be: dichloromethyl phenylsilane hydrolyzate 20%-80%
Dimethyldichlorosilane(DMCS) hydrolyzate 0%-50%
Methyl phenyl ring siloxane 0%-30%
The 0.01-0.1% of the above-mentioned three kinds of component gross weights of basic metal silicon alkoxide
Taking by weighing dichloromethyl phenylsilane hydrolyzate, dimethyldichlorosilane(DMCS) hydrolyzate, methyl phenyl ring siloxane, basic metal silicon alkoxide joins in the reactor that agitator, thermometer and reflux exchanger are housed;
(b) under 60-80 ℃ reactor is vacuumized, pressure is reduced to 0.02MPa～0.095Mpa, removes the minor amount of water in the reactant;
(c) temperature of reaction is risen to 130-170 ℃, polyreaction 2-8h;
(d) add the alkyl acid phosphate alcoholic solution, it is 6～7 that solution in the reactor is neutralized to pH, stirs 0.5-1h;
(e) temperature of reaction is risen to 160-190 ℃, start vacuum pump, under 0.095～0.1MPa pressure, keep 0.5-2h, remove lower-molecular substance and obtain hydroxy-end capped PSI.
As preferably, described dichloromethyl phenylsilane hydrolyzate is methyl phenyl ring siloxane and hydroxy-end capped polydimethyl phenyl siloxane, and its general formula is HO (SiMePhO) nH, wherein n=2-20.
Described dimethyldichlorosilane(DMCS) hydrolyzate is methyl cyclosiloxane and hydroxy-end capped polydimethylsiloxane, and its general formula is HO (SiMe 2O) nH, wherein n=2-20.
Described methyl phenyl ring siloxane is 1,3,5-trimethylammonium-1,3,5-triphenyl cyclotrisiloxane, 1,3,5,7-tetramethyl--1,3,5, any one in 7-tetraphenyl cyclotetrasiloxane, the aminomethyl phenyl D5.
Temperature of reaction is preferably 140～150 ℃ described in the step (c), and polymerization time is preferably 4～6 hours.
Described basic metal silicon alkoxide is preferably the siloxanes potassium alcoholate.The basic metal silicon alkoxide can also be silica alkanol caesium or silica alkanol rubidium or siloxanes sodium alkoxide or siloxanes lithium alkoxide.
The KOH mass concentration of described siloxanes potassium alcoholate is 1%～5%.
Described alkyl acid phosphate alcoholic solution is preferably alkyl acid phosphate methanol solution or alkyl acid phosphate ethanolic soln.
The mass concentration of phosphoric acid is 10%～50% in described alkyl acid phosphate methanol solution or the alkyl acid phosphate ethanolic soln.
The present invention is a raw material with dichloromethyl phenylsilane hydrolyzate, dimethyldichlorosilane(DMCS) hydrolyzate and methyl phenyl ring siloxane directly, with the basic metal silicon alkoxide is catalyzer, with the alkyl acid phosphate alcoholic solution is neutralizing agent, have following advantage: the polymerization process gentleness is controlled, easy handling, after finishing, polyreaction do not need to add the water degraded, and the catalytic amount that consumes in synthetic is few, also few in the corresponding consumption with dosage, the salt particle that produces is little and few, the hydroxy-end capped PSI transparency that makes is good, even molecular weight distribution, yield height.
Embodiment
The invention will be further described below in conjunction with embodiment, but be not limited thereto.
Embodiment 1:
Adding 1000g dichloromethyl phenylsilane hydrolyzate, 1000g dimethyldichlorosilane(DMCS) hydrolyzate, 2gKOH mass concentration are 1% siloxanes potassium alcoholate in the reactor of 5000mL, stir, temperature is controlled at 70 ℃, pressure-controlling is at 0.05MPa, remove the moisture content in the reactant, the low-boiling point material that carries in the moisture content of deviating from returns reactor after being cooled off by equilibration tube.The dichloromethyl phenylsilane hydrolyzate adopts methyl phenyl ring siloxane and hydroxy-end capped polydimethyl phenyl siloxane, and its chemical formula is HO (SiMePhO) 2H, the dimethyldichlorosilane(DMCS) hydrolyzate adopts methyl cyclosiloxane and hydroxy-end capped polydimethylsiloxane, and its chemical formula is HO (SiMe 2O) 2H.
Reactor temperature rises to 145 ℃, catalysis shrink polymerization 5h, adding phosphoric acid quality concentration and be 10% phosphoric acid ethanol solution, to be neutralized to the pH value be 6, stirred 0.7 hour, continue to be warming up to 180 ℃, the control reacting kettle inner pressure is 0.095MPa, keeps 1h, and removing and obtaining viscosity behind the lower-molecular substance is 5000～120000mm 2The hydroxy-end capped PSI of/s.The hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 88.51%, and fugitive constituent is 1.47%.
Embodiment 2:
Adding 1600g dichloromethyl phenylsilane hydrolyzate, 400g dimethyldichlorosilane(DMCS) hydrolyzate, 0.2gKOH mass concentration are 5% siloxanes potassium alcoholate in the reactor of 5000mL, stir, temperature is controlled at 60 ℃, pressure-controlling is at 0.02MPa, remove the moisture content in the reactant, the low-boiling point material that carries in the moisture content of deviating from returns reactor after being cooled off by equilibration tube.The dichloromethyl phenylsilane hydrolyzate adopts methyl phenyl ring siloxane and hydroxy-end capped polydimethyl phenyl siloxane, and its chemical formula is HO (SiMePhO) 20H, the dimethyldichlorosilane(DMCS) hydrolyzate adopts methyl cyclosiloxane and hydroxy-end capped polydimethylsiloxane, and its chemical formula is HO (SiMe 2O) 20H.
Reactor temperature rises to 130 ℃, catalysis shrink polymerization 8h, adding phosphoric acid quality concentration and be 50% phosphoric acid methanol solution, to be neutralized to the pH value be 7, stirred 0.5 hour, continue to be warming up to 160 ℃, the control reacting kettle inner pressure is 0.095MPa, keeps 2h, and removing and obtaining viscosity behind the lower-molecular substance is 5000～120000mm 2The hydroxy-end capped PSI of/s.The hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 89.87%, and fugitive constituent is 1.21%.
Embodiment 3:
Adding 400g dichloromethyl phenylsilane hydrolyzate, 1000g dimethyldichlorosilane(DMCS) hydrolyzate, 600 gram methyl phenyl ring siloxanes, 2gKOH mass concentration are 3% siloxanes potassium alcoholate in the reactor of 5000mL, stir, temperature is controlled at 80 ℃, pressure-controlling is at 0.095MPa, remove the moisture content in the reactant, the low-boiling point material that carries in the moisture content of deviating from returns reactor after being cooled off by equilibration tube.The dichloromethyl phenylsilane hydrolyzate adopts methyl phenyl ring siloxane and hydroxy-end capped polydimethyl phenyl siloxane, and its chemical formula is HO (SiMePhO) 10H, the dimethyldichlorosilane(DMCS) hydrolyzate adopts methyl cyclosiloxane and hydroxy-end capped polydimethylsiloxane, and its chemical formula is HO (SiMe 2O) 10H, methyl phenyl ring siloxane adopts 1,3,5-trimethylammonium-1,3,5-triphenyl cyclotrisiloxane.
Reactor temperature rises to 170 ℃, catalysis shrink polymerization 2h, adding phosphoric acid quality concentration and be 10% phosphoric acid methanol solution, to be neutralized to the pH value be 7, stirred 1 hour, continue to be warming up to 190 ℃, the control reacting kettle inner pressure is 0.1MPa, keeps 0.5h, and removing and obtaining viscosity behind the lower-molecular substance is 5000～120000mm 2The hydroxy-end capped PSI of/s.The hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 90%, and fugitive constituent is 0.87%.
Embodiment 4:
In the reactor of 5000mL, add 1500g dichloromethyl phenylsilane hydrolyzate, 1500 gram methyl phenyl ring siloxanes, 2.5gKOH mass concentration are 1% siloxanes potassium alcoholate, stir, temperature is controlled at 80 ℃, pressure-controlling is at 0.095MPa, remove the moisture content in the reactant, the low-boiling point material that carries in the moisture content of deviating from returns reactor after being cooled off by equilibration tube.The dichloromethyl phenylsilane hydrolyzate adopts methyl phenyl ring siloxane and hydroxy-end capped polydimethyl phenyl siloxane, and its chemical formula is HO (SiMePhO) 8H, methyl phenyl ring siloxane adopts 1,3,5,7-tetramethyl--1,3,5,7-tetraphenyl cyclotetrasiloxane.
Reactor temperature rises to 150 ℃, catalysis shrink polymerization 4h, adding phosphoric acid quality concentration and be 50% phosphoric acid ethanol solution, to be neutralized to the pH value be 6, stirred 1 hour, continue to be warming up to 190 ℃, the control reacting kettle inner pressure is 0.1MPa, keeps 0.5h, and removing and obtaining viscosity behind the lower-molecular substance is 5000～120000mm 2The hydroxy-end capped PSI of/s.The hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 92%, and fugitive constituent is 0.87%.
Embodiment 5:
In the reactor of 5000mL, add 1400g dichloromethyl phenylsilane hydrolyzate, 600 gram methyl phenyl ring siloxanes, 1.8gKOH mass concentration are 1% siloxanes potassium alcoholate, stir, temperature is controlled at 80 ℃, pressure-controlling is at 0.095MPa, remove the moisture content in the reactant, the low-boiling point material that carries in the moisture content of deviating from returns reactor after being cooled off by equilibration tube.The dichloromethyl phenylsilane hydrolyzate adopts methyl phenyl ring siloxane and hydroxy-end capped polydimethyl phenyl siloxane, and its chemical formula is HO (SiMePhO) 8H, methyl phenyl ring siloxane adopts the aminomethyl phenyl D5.
Reactor temperature rises to 140 ℃, catalysis shrink polymerization 6h, adding phosphoric acid quality concentration and be 30% phosphoric acid ethanol solution, to be neutralized to the pH value be 7, stirred 1 hour, continue to be warming up to 190 ℃, the control reacting kettle inner pressure is 0.1MPa, keeps 2h, and removing and obtaining viscosity behind the lower-molecular substance is 5000～120000mm 2The hydroxy-end capped PSI of/s.The hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 92%, and fugitive constituent is 0.87%.
Embodiment 6:
Catalyzer employing CsOH concentration is 1% silica alkanol caesium, other conditions such as embodiment 1, and the hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 88.32%, and fugitive constituent is 0.97%.
Embodiment 7:
Catalyzer employing RbOH concentration is 1% silica alkanol rubidium, other conditions such as embodiment 1, and the hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 89.32%, and fugitive constituent is 0.96%.
Embodiment 8:
Catalyzer employing NaOH concentration is 1% siloxanes sodium alkoxide, other conditions such as embodiment 1, and the hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 86.79%, and fugitive constituent is 1.21%.
Embodiment 9:
Catalyzer employing LiOH concentration is 1% siloxanes lithium alkoxide, other conditions such as embodiment 1, and the hydroxy-end capped PSI transparency of gained is good, and per pass conversion is 82.59%, and fugitive constituent is 1.42%.

Claims (9)

1. the preparation method of a hydroxy-end capped PSI, described hydroxy-end capped PSI can be used general formula
Figure FSA00000367890400011
Expression, wherein x, y are the polymerization degree, x=1-100, y=1-50 is characterized in that adopting following steps:
(a) according to proportioning be: dichloromethyl phenylsilane hydrolyzate 20%-80%
Dimethyldichlorosilane(DMCS) hydrolyzate 0%-50%
Methyl phenyl ring siloxane 0%-30%
The 0.01-0.1% of the above-mentioned three kinds of component gross weights of basic metal silicon alkoxide
Taking by weighing dichloromethyl phenylsilane hydrolyzate, dimethyldichlorosilane(DMCS) hydrolyzate, methyl phenyl ring siloxane, basic metal silicon alkoxide joins in the reactor that agitator, thermometer and reflux exchanger are housed;
(b) under 60-80 ℃ reactor is vacuumized, pressure is reduced to 0.02MPa～0.095Mpa, removes the minor amount of water in the reactant;
(c) temperature of reaction is risen to 130-170 ℃, polyreaction 2-8h;
(d) add the alkyl acid phosphate alcoholic solution, it is 6～7 that solution in the reactor is neutralized to pH, stirs 0.5-1h;
(e) temperature of reaction is risen to 160-190 ℃, start vacuum pump, under 0.095～0.1MPa pressure, keep 0.5-2h, remove lower-molecular substance and obtain hydroxy-end capped PSI.
2. the preparation method of hydroxy-end capped PSI according to claim 1, it is characterized in that: described dichloromethyl phenylsilane hydrolyzate is methyl phenyl ring siloxane and hydroxy-end capped polydimethyl phenyl siloxane, and its general formula is HO (SiMePhO) nH, wherein n=2-20.
3. the preparation method of hydroxy-end capped PSI according to claim 1, it is characterized in that: described dimethyldichlorosilane(DMCS) hydrolyzate is methyl cyclosiloxane and hydroxy-end capped polydimethylsiloxane, and its general formula is HO (SiMe 2O) nH, wherein n=2-20.
4. the preparation method of hydroxy-end capped PSI according to claim 1, it is characterized in that: described methyl phenyl ring siloxane is 1,3,5-trimethylammonium-1,3,5-triphenyl cyclotrisiloxane, 1,3,5,7-tetramethyl--1,3,5, any one in 7-tetraphenyl cyclotetrasiloxane, the aminomethyl phenyl D5.
5. the preparation method of hydroxy-end capped PSI according to claim 1, it is characterized in that: temperature of reaction is preferably 140～150 ℃ described in the step (c), and polymerization time is preferably 4～6 hours.
6. the preparation method of hydroxy-end capped PSI according to claim 1, it is characterized in that: described basic metal silicon alkoxide is preferably the siloxanes potassium alcoholate.
7. the preparation method of hydroxy-end capped PSI according to claim 6, it is characterized in that: the KOH mass concentration of described siloxanes potassium alcoholate is 1%～5%.
8. the preparation method of hydroxy-end capped PSI according to claim 1, it is characterized in that: described alkyl acid phosphate alcoholic solution is preferably alkyl acid phosphate methanol solution or alkyl acid phosphate ethanolic soln.
9. the preparation method of hydroxy-end capped PSI according to claim 8, it is characterized in that: the mass concentration of phosphoric acid is 10%～50% in described alkyl acid phosphate methanol solution or the alkyl acid phosphate ethanolic soln.
CN2010105672261A 2010-11-26 2010-11-26 Preparation method of hydroxyl-terminated polymethylphenyl sioxane Pending CN102070785A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103073723A (en) * 2013-01-31 2013-05-01 株洲时代新材料科技股份有限公司 High-viscosity organosilicon elastic glue mud for buffers and preparation method of high-viscosity organosilicon elastic glue mud
CN110358089A (en) * 2018-04-11 2019-10-22 苏州润特新材料科技有限公司 A kind of preparation method of alkylaryl modified silicon oil
CN113117434A (en) * 2019-12-30 2021-07-16 西安工程大学 Preparation method of flexible reticular vein structure ceramic nanofiber ultrahigh-temperature filtering membrane
CN115197425A (en) * 2022-08-17 2022-10-18 国元新能源科技发展(武汉)有限公司 Process for separating siloxane linear body and ring body and application thereof
CN117430782A (en) * 2023-12-21 2024-01-23 山东一诺威聚氨酯股份有限公司 Resin for high-brightness pore-free polyurethane sole, and preparation method and application thereof

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US4551515A (en) * 1984-02-27 1985-11-05 General Electric Company Process for the continuous manufacture of silicone gums
CN101074284A (en) * 2007-05-22 2007-11-21 杭州师范大学 Production of polymethylphenylsilixane containing trifunctional phenyl-silox-chain
CN101074283A (en) * 2007-05-22 2007-11-21 杭州师范大学 Method for producing hydroxy-end capped polymethylphenylsilixane

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4551515A (en) * 1984-02-27 1985-11-05 General Electric Company Process for the continuous manufacture of silicone gums
CN101074284A (en) * 2007-05-22 2007-11-21 杭州师范大学 Production of polymethylphenylsilixane containing trifunctional phenyl-silox-chain
CN101074283A (en) * 2007-05-22 2007-11-21 杭州师范大学 Method for producing hydroxy-end capped polymethylphenylsilixane

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103073723A (en) * 2013-01-31 2013-05-01 株洲时代新材料科技股份有限公司 High-viscosity organosilicon elastic glue mud for buffers and preparation method of high-viscosity organosilicon elastic glue mud
CN110358089A (en) * 2018-04-11 2019-10-22 苏州润特新材料科技有限公司 A kind of preparation method of alkylaryl modified silicon oil
CN113117434A (en) * 2019-12-30 2021-07-16 西安工程大学 Preparation method of flexible reticular vein structure ceramic nanofiber ultrahigh-temperature filtering membrane
CN115197425A (en) * 2022-08-17 2022-10-18 国元新能源科技发展(武汉)有限公司 Process for separating siloxane linear body and ring body and application thereof
CN117430782A (en) * 2023-12-21 2024-01-23 山东一诺威聚氨酯股份有限公司 Resin for high-brightness pore-free polyurethane sole, and preparation method and application thereof
CN117430782B (en) * 2023-12-21 2024-04-19 山东一诺威聚氨酯股份有限公司 Resin for high-brightness pore-free polyurethane sole, and preparation method and application thereof

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