CN1037158A - Preparation techlonogy for polydipheny dimethyl linear siloxane - Google Patents
Preparation techlonogy for polydipheny dimethyl linear siloxane Download PDFInfo
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- CN1037158A CN1037158A CN 88105182 CN88105182A CN1037158A CN 1037158 A CN1037158 A CN 1037158A CN 88105182 CN88105182 CN 88105182 CN 88105182 A CN88105182 A CN 88105182A CN 1037158 A CN1037158 A CN 1037158A
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Abstract
Preparation techlonogy for polydipheny dimethyl linear siloxane is with dimethyldichlorosilane(DMCS).Diphenyl dichlorosilane, hexamethyldisiloxane and corresponding catalyst are raw material, are made of hydrolysis, separation, cracking, polymerization, washing and distillation six procedures.Poly-phenylbenzene dimethyl linear siloxane can be used for the aspects such as lubricated, demoulding, insulation high and low temperature and normal temperature condition under, is processed into demoulding that silicone oil can be used for aspects such as chemical fibre SPINNERETS FOR MELT SPINNING face treatment agent and rubber, pottery, food, lubricates.
Description
The present invention relates to the silicone resin synthesis technical field.Be mainly used in and do that chemical fibre is molten to spin that spinning plate surface is handled and revise the lubrication sdemoulding agent.
At present, be used for the molten silicone oil that spins the spinning plate surface processing and revise lubrication sdemoulding of chemical fibre both at home and abroad, all belong to the product of organo-siloxane series.As: the polymethylphenyl siloxane fluid of methyl-silicone oil and low phenyl.The shortcoming of these silicone oil is that ageing resistance and volatile performance are poor.
The objective of the invention is, provide a kind of anti-aging, the technology of preparing of the silicone oil of high temperature resistant difference-poly-phenylbenzene dimethyl linear siloxane.
The molecular formula of poly-phenylbenzene dimethyl linear siloxane is:
（CH
3）
3SiO
（CH
3）
2SiO
（CH）
nSiO]-Si（CH
3）
3
m∶n＝9-0.25
Molecular weight: 2000-10000
Raw material and prescription thereof that the present invention uses are:
1. raw material
Dimethyldichlorosilane(DMCS) (CH
3)
eSiCl
2
Diphenyl dichlorosilane (C
6H
5)
2SiCl
2
Hexamethyldisiloxane (CH
3)
3Si-O-Si(CH
3)
3
Hexamethyldisiloxane is a closure agent.
2. composition of raw materials (weight ratio)
Dimethyldichlorosilane(DMCS) 0.16-9
Diphenyl dichlorosilane 1
Hexamethyldisiloxane is an amount of
Its optimum feed stock prescription (weight ratio) is:
Dimethyldichlorosilane(DMCS) 1.5-2
Diphenyl dichlorosilane 1
Hexamethyldisiloxane is an amount of
Preparation technology of the present invention as shown in the figure, by hydrolysis. separate. cracking. polymerization. washing. distill six procedures and constitute.
Now preparation technology is described below step by step:
1. hydrolysis
To add dimethyldichlorosilane(DMCS) by prescription, diphenyl dichlorosilane is thrown in the hydrolytic decomposition pot under 70 degree-80 degree temperature and is hydrolyzed.Drip while stirring, added in 2 hours, continue to stir 20-30 minute, after hydrolysis is finished material is delivered in the oleic acid separator of separation circuit.
The chemical reaction of hydrolysis is:
In the formula:
m+n＝3-9
2. separate
Acid told behind oleic acid separator standing demix from the material of hydrolyzing process and to discard, material is delivered in the cracking still of cracking operation.
3. cracking
With Sodium Fluoride, potassium hydroxide aqueous solution is a catalyzer during cracking, carries out cracking under (180-360 degree) decompression (700mmHg) condition of heating.
Sodium Fluoride adds with solid form in the catalyzer, and add-on is 0.15% of a weight of material; The weight of potassium hydroxide is 0.2% of material, and it is made into content is that 50% aqueous solution adds in the material.
The cracked chemical reaction is:
In the formula:
M and n are 6-9
P+q＝3-5
Material after the cracking is delivered in the polymeric kettle of polymerization process.
4. polymerization
Material after the cracking is a catalyzer with the vitriol oil in polymeric kettle, carries out polymerization under (75 degree) stirring condition of heating.The add-on of the catalyzer vitriol oil is that material gets 1.5%, adds suitable closure agent (hexamethyldisiloxane) simultaneously.
Chemical reaction during polymerization is:
Material after the polymerization is delivered in the water washing tank of washing step.
5. washing
At first remove the catalyzer in the polymer material, clean residual acid with 80-90 degree hot water then.
6. distillation
Material in the still kettle distills under the condition of vacuum tightness 〉=650mmHg at the 250-300 degree, and the above fraction of 250 degree is a finished product, and the following fraction of 250 degree returns the cracking again of cracking operation, polymerization.
Poly-phenylbenzene dimethyl linear siloxane product with the technology of the present invention preparation can reach following standard:
Fugitive constituent≤15%(290 degree in loft drier were deposited 24 hours)
The 90 hours anti-aging time (in 290 degree loft drier)
Phenyl content 20-30%(is with learning outer absorption spectrometry)
Poly-phenylbenzene dimethyl linear siloxane can be used for height, lubricates demoulding, aspects such as insulation low temperature and normal temperature condition under; As be processed into atomizing silicone oil and then can be used for chemical fibre SPINNERETS FOR MELT SPINNING face treatment agent and rubber, pottery, the demoulding of aspects such as food, lubricated.
Advantage of the present invention is, technology is simple, and flow process is short, makes the silicone oil that atomizes with poly-phenylbenzene dimethyl linear siloxane and can make chemical fibre SPINNERETS FOR MELT SPINNING treatment agent.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention
Claims (7)
1, preparation techlonogy for polydipheny dimethyl linear siloxane is characterized in that by hydrolysis. separates. and cracking. polymerization. wash and distill six procedures and constitute.
2, the preparation technology who narrates according to claim 1, the weight ratio of dimethyldichlorosilane(DMCS) and diphenyl dichlorosilane is 0.16-9 when it is characterized in that hydrolysis: 1, its optimum weight ratio is 1.5-2: 1, hydrolysis temperature is the 70-80 degree.
3, the preparation technology who narrates according to claim 1, the hydrochloric acid that produces when it is characterized in that in separator hydrolysis is separated.
4, the preparation technology who narrates according to claim 1 is characterized in that cracking temperature is the 180-360 degree, and vacuum tightness 700mmHg is a catalyzer with Sodium Fluoride and potassium hydroxide aqueous solution, and Sodium Fluoride adds with solid form.Add-on is 0.15% of a weight of material, and the add-on of potassium hydroxide is 0.2% of a weight of material, is that 50% aqueous solution form adds and holds withg both hands with content
5, the preparation technology who narrates according to claim 1 is characterized in that polymerization temperature is 75 degree, and the vitriol oil is a catalyzer, and its add-on is 1.5% of a material, and closure agent is a hexamethyldisiloxane.Its add-on suitably gets final product.
6, the preparation technology who narrates according to claim 1 at first removes the catalyzer in the polymkeric substance when it is characterized in that washing.Wash residual acid off with 80-90 hot water then.
7, the preparation technology who narrates according to claim 1 is characterized in that distillation temperature is the 250-300 degree, and vacuum tightness is 650mmHg, and the above fraction of 250 degree is a finished product.The following fraction of 250 degree returns the cracking again of cracking operation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105182 CN1037158A (en) | 1988-12-12 | 1988-12-12 | Preparation techlonogy for polydipheny dimethyl linear siloxane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105182 CN1037158A (en) | 1988-12-12 | 1988-12-12 | Preparation techlonogy for polydipheny dimethyl linear siloxane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1037158A true CN1037158A (en) | 1989-11-15 |
Family
ID=4833409
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88105182 Pending CN1037158A (en) | 1988-12-12 | 1988-12-12 | Preparation techlonogy for polydipheny dimethyl linear siloxane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1037158A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037505B (en) * | 2007-01-30 | 2011-05-04 | 姜景勋 | Production method of dimethyl hydroxyl silicon oil |
| CN103304818A (en) * | 2013-06-26 | 2013-09-18 | 江苏大学 | Preparation method of methyl phenyl silicone oil |
| CN106637440A (en) * | 2016-11-15 | 2017-05-10 | 东华大学 | Low-damping polymer efficient dry-wet spinning method |
| CN106757410A (en) * | 2016-11-15 | 2017-05-31 | 东华大学 | A kind of spinneret orifice and its processing method |
| CN110180467A (en) * | 2019-06-12 | 2019-08-30 | 湖北兴瑞硅材料有限公司 | A kind of Dimethyldichlorosilane hydrolysate cracker and technique |
-
1988
- 1988-12-12 CN CN 88105182 patent/CN1037158A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037505B (en) * | 2007-01-30 | 2011-05-04 | 姜景勋 | Production method of dimethyl hydroxyl silicon oil |
| CN103304818A (en) * | 2013-06-26 | 2013-09-18 | 江苏大学 | Preparation method of methyl phenyl silicone oil |
| CN106637440A (en) * | 2016-11-15 | 2017-05-10 | 东华大学 | Low-damping polymer efficient dry-wet spinning method |
| CN106757410A (en) * | 2016-11-15 | 2017-05-31 | 东华大学 | A kind of spinneret orifice and its processing method |
| CN106637440B (en) * | 2016-11-15 | 2018-08-21 | 东华大学 | A kind of low resistance polymer high efficiency dry-wet spinning method |
| CN110180467A (en) * | 2019-06-12 | 2019-08-30 | 湖北兴瑞硅材料有限公司 | A kind of Dimethyldichlorosilane hydrolysate cracker and technique |
| CN110180467B (en) * | 2019-06-12 | 2021-10-12 | 湖北兴瑞硅材料有限公司 | Dimethyl dichlorosilane hydrolysate cracking device and process |
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