CN110229337A - The production method of phenyl methyl silicone oil - Google Patents
The production method of phenyl methyl silicone oil Download PDFInfo
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- CN110229337A CN110229337A CN201910625627.9A CN201910625627A CN110229337A CN 110229337 A CN110229337 A CN 110229337A CN 201910625627 A CN201910625627 A CN 201910625627A CN 110229337 A CN110229337 A CN 110229337A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
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Abstract
The invention discloses a kind of production methods of phenyl methyl silicone oil, it is dehydrated after 40-70 parts by weight phenyl methyl cyclotetrasiloxane and 10 parts by weight hexamethyl cyclotrisiloxanes are stirred and evenly mixed, is then stirred 0.5~1 hour under conditions of 60~70 DEG C, -0.10~-0.12MPa；Reacting liquid temperature is warming up to 80~90 DEG C, tetramethylammonium hydroxide, dimethyl sulfoxide and butanone is added, is stirred to react 0.5~1 hour；Then it is added at 95-105 DEG C of hexamethyldisiloxane and is stirred to react 0.5-1.5 hours；150 DEG C or more broken matchmakers are then heated to, are taken off under the conditions of 180~200 DEG C, -0.09~-0.12MPa small molecule 1~2 hour；After removing small molecule, it is continuously passed through dry gas, decompression stirring, then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl silicone oil.The present invention avoids to be generated sour water using chlorosilane, only being generated a small amount of ammonia, and acid solution absorption can be used and be made into nitrogenous fertilizer, environmental pollution is small, and products obtained therefrom viscosity is up to 925mPas, and yield is up to 91.2%, and transmitance is up to 96.2%.
Description
Technical field
The invention belongs to field of organic silicon, are related to a kind of production method of phenyl methyl silicone oil.
Background technique
Phenyl methyl silicone oil is the product after the part methyl in methyl-silicone oil is substituted by phenyl, resistance to due to phenyl silicone oil
Low temperature, high temperature resistant, lubricity, intermiscibility, radiation resistance are superior to methyl-silicone oil, in aerospace, ship automobile, electronics electricity
The various fields such as gas, petrochemical industry, health care have a extensive future.
The phenyl methyl silicone oil of different phenyl contents, performance and purposes are different, and phenyl content can pass through refractive power
Rate is measured, and phenyl content is higher, and the index of refraction of phenyl methyl silicone oil is higher.In traditional industry production, it is often used chlorosilane
Hydrolyze method prepares phenyl methyl silicone oil, and this method causes serious pollution to the environment, and the sour water processing cost after reaction is high.
Summary of the invention
In view of the deficiencies in the prior art, the present invention provides a kind of production method of phenyl methyl silicone oil, to solve
Existing phenyl methyl silicone oil production method pollutes problem big, at high cost.Another object of the present invention is production index of refraction
In 1.460 or more high viscosity phenyl methyl silicone oil.
To achieve the above objectives, the technical solution adopted by the present invention is that:
A kind of production method of phenyl methyl silicone oil, comprising the following steps:
Bottom band logical is added in 40-70 parts by weight phenyl methyl cyclotetrasiloxane and 10 parts by weight hexamethyl cyclotrisiloxanes
In the decompression stirring jacket canister of air valve, dehydration is stirred after stirring and evenly mixing under conditions of 40~50 DEG C, -0.10~-0.12MPa
It 0.5~1 hour, is then stirred 0.5~1 hour under conditions of 60~70 DEG C, -0.10~-0.12MPa；
Reacting liquid temperature is warming up to 80~90 DEG C, 0.8~1 parts by weight tetramethylammonium hydroxide, 0.5~1.5 weight is added
The butanone for measuring part dimethyl sulfoxide and 2-3 parts by weight, is stirred to react 0.5~1.5 hour under the conditions of -0.09~-0.12MPa；So
15~25 parts by weight hexamethyldisiloxane are added afterwards, are stirred to react 0.5-1.5 hours at 95-105 DEG C；
150 DEG C or more heat preservations 0.5-1 hours are then heated to, under the conditions of 180~200 DEG C, -0.09~-0.12MPa
Removing small molecule 1~2 hour；
After removing small molecule, decompression stirring jacket canister bottom valve is opened, dry gas is continuously passed through, and is vacuumized to protect
Negative pressure is 0.09-0.1Mpa in pressure of keeping reducing stirring jacket canister, and continuously stirs 1-3 hours, then Temperature fall to 50 DEG C hereinafter,
Obtain phenyl methyl silicone oil.
Based on the above technical solution, the additional amount of the tetramethylammonium hydroxide is phenyl methyl cyclotetrasiloxane
With the 1wt% of hexamethyl cyclotrisiloxane total weight.
Based on the above technical solution, the dry gas is dehydrated air or drying nitrogen.
Based on the above technical solution, the de- low boiling point small molecule is condensed after removed under reduced pressure, reenters
Lower secondary response.
Based on the above technical solution, phenyl methyl cyclotetrasiloxane is diphenyl hexamethyl cyclotetrasiloxane.
Based on the above technical solution, it is 1 hour that the time reacted after tetramethylammonium hydroxide, which is added,.
Compared with the prior art, the advantages of the present invention are as follows:
(1) present invention avoids to be generated sour water using chlorosilane, only being generated a small amount of ammonia, and acid solution absorption can be used and do
At nitrogenous fertilizer, environmental pollution is small.
(2) present invention production products obtained therefrom viscosity is up to 925mPas, and yield is up to 91.2%, and transmitance is up to
96.2%.
Specific embodiment
Clear, complete description is carried out to the technical solution of embodiment each in the present invention below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiment of the present invention, this field is common
Technical staff's obtained all other embodiment without making creative work belongs to the present invention and is protected
Range.
Embodiment 1
Bottom belt ventilation is added in 60 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes
It in the decompression stirring jacket canister of valve, stirs and evenly mixs, then stirring dehydration 0.5 hour under the conditions of 40 DEG C, -0.10MPa, then exists
65 DEG C, stirring heat preservation 1 hour under conditions of -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 2
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 3
40 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40~
50 DEG C, be dehydrated 0.5~1 hour under conditions of -0.10~-0.12MPa, then in 60~70 DEG C, the item of -0.10~-0.12MPa
1 hour is kept the temperature under part；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 4
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 0.5 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 5
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1.5 hours under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 6
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 2 hours under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 7
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 3 hours under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 8
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 4 hours under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 9
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 0.5 hour；Then 15 parts by weight hexamethyl, two silicon is added
Oxygen alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 10
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1.5 hours；Then 15 parts by weight hexamethyl, two silicon is added
Oxygen alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 11
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 2 hours；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 12
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 3 hours；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 13
50 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 4 hours；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 14
30 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 15
70 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 16
80 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
Embodiment 17
90 parts by weight phenyl methyl cyclotetrasiloxanes and 10 parts by weight hexamethyl cyclotrisiloxanes are mixed, then 40
DEG C, be dehydrated 0.5 hour under conditions of -0.10MPa, then keep the temperature 1 hour under conditions of 65 DEG C, -0.12MPa；
Reacting liquid temperature is warming up to 80 DEG C, 0.5 parts by weight tetramethylammonium hydroxide, 0.5 parts by weight dimethyl sulfoxide is added
With the butanone of 2 parts by weight, it is stirred to react under conditions of -0.09MPa 1 hour；Then 15 parts by weight hexamethyl, two silicon oxygen is added
Alkane is stirred to react 0.5 hour at 95 DEG C；
150 DEG C of heat preservation 30min are then heated to, are taken off under the conditions of 180 DEG C, -0.09Mpa small molecule 1 hour；
After removing small molecule, jacket canister bottom valve is stirred in crack decompression, is continuously passed through drying nitrogen, and decompression is kept to stir
Mixing negative pressure in jacket canister is 0.09-0.1Mpa, and is continuously stirred 3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining phenyl methyl
Silicone oil.
The product parameters of 1 various embodiments of the present invention of table
Table 1 illustrates product parameters made from each embodiment, wherein raw material ratio refer to phenyl methyl cyclotetrasiloxane with
The weight ratio of hexamethyl cyclotrisiloxane, soaking time a refer to dehydration after, be added tetramethylammonium hydroxide and dimethyl sulfoxide it
The preceding time, polymerization reaction time b refer to being added tetramethylammonium hydroxide and dimethyl sulfoxide into reaction solution after, pregnancy is added
Polymerization reaction time before base disiloxane.
The present invention is not limited to the above-described embodiments, for those skilled in the art, is not departing from
Under the premise of the principle of the invention, several improvements and modifications can also be made, these improvements and modifications are also considered as protection of the invention
Within the scope of.The content being not described in detail in this specification belongs to the prior art well known to professional and technical personnel in the field.
Claims (6)
1. a kind of production method of phenyl methyl silicone oil, which comprises the following steps:
Bottom belt breather valve is added in 40-70 parts by weight phenyl methyl cyclotetrasiloxane and 10 parts by weight hexamethyl cyclotrisiloxanes
Decompression stirring jacket canister in, after stirring and evenly mixing under conditions of 40~50 DEG C, -0.10~-0.12MPa stirring dehydration 0.5~1
Hour, then stirred 0.5~1 hour under conditions of 60~70 DEG C, -0.10~-0.12MPa；
Reacting liquid temperature is warming up to 80~90 DEG C, 0.8~1 parts by weight tetramethylammonium hydroxide, 0.5~1.5 parts by weight is added
The butanone of dimethyl sulfoxide and 2-3 parts by weight is stirred to react 0.5~1.5 hour under the conditions of -0.09~-0.12MPa；Then plus
Enter 15~25 parts by weight hexamethyldisiloxane, is stirred to react at 95-105 DEG C 0.5-1.5 hours；
150 DEG C or more heat preservations 0.5-1 hours are then heated to, are removed under the conditions of 180~200 DEG C, -0.09~-0.12MPa
Small molecule 1~2 hour；
After removing small molecule, decompression stirring jacket canister bottom valve is opened, dry gas is continuously passed through, and vacuumized to keep subtracting
Negative pressure is 0.09-0.1Mpa in pressure stirring jacket canister, and is continuously stirred 1-3 hours, and then Temperature fall is to 50 DEG C hereinafter, obtaining benzene
Ylmethyl silicone oil.
2. production method according to claim 1, it is characterised in that: the additional amount of the tetramethylammonium hydroxide is phenyl
The 1wt% of methyl cyclotetrasiloxane and hexamethyl cyclotrisiloxane total weight.
3. production method according to claim 1, it is characterised in that: the dry gas is dehydrated air or dry nitrogen
Gas.
4. production method according to claim 1, it is characterised in that: de- low boiling point small molecule quilt after removed under reduced pressure
Condensation, reenters lower secondary response.
5. production method according to claim 1, it is characterised in that: phenyl methyl cyclotetrasiloxane is diphenyl hexamethyl
Cyclotetrasiloxane.
6. production method according to claim 1, it is characterised in that: time for reacting is after tetramethylammonium hydroxide is added
1 hour.
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