CN103131010A - Silicone oil preparation method by means of simultaneous hydrolysis of high-boiling residues and low-boiling residues of organic silicon - Google Patents
Silicone oil preparation method by means of simultaneous hydrolysis of high-boiling residues and low-boiling residues of organic silicon Download PDFInfo
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Abstract
The invention belongs to the technical field of organic silicon production, and particularly relates to a silicone oil preparation method by means of simultaneous hydrolysis of high-boiling residues and low-boiling residues of organic silicon. The steps of the method includes that the high-boiling residues and the low-boiling residues are added to a monomer mixing kettle to be uniformly mixed, and inorganic salt and water are uniformly mixed; mixed monomer is slowly dripped into a hydrolysis kettle, the reaction temperature is controlled to be at 10 DEG C-80 DEG C, the dripping speed of the monomer is adjusted according to the reaction temperature of the hydrolysis kettle, dripping of the monomer is finished in three hours, the reaction temperature is raised, backflow is carried out for 1 hour, complete hydrolysis is further promoted, meanwhile hydrogen chloride gas produced in the reaction is sent to a water spraying tower through an air draft device to be absorbed; and reaction liquid is transferred into an acid accumulator trap to be layered in a standing mode, acid-stage silicone oil and diluted hydrochloric acid are obtained, the acid-stage silicone oil carries out a neutral reaction, and products after neutralization are obtained to obtain silicone oil product. Reaction conditions are easy to control, the oil yield rate reaches 80%, viscosity of the product is adjustable and controllable, the prepared silicone oil can form membranes through crosslinking and solidity, and the utilization value is high.
Description
Technical field
The invention belongs to the organosilicon production technical field, is a kind of method of utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil specifically.
Background technology
Along with the fast development of organosilicon industry, the output of methyl chlorosilane monomer constantly enlarges, and by-product organosilicon high-boiling product, low-boiling-point substance are also more and more simultaneously, in the industry of direct synthesis methyl chlorosilane, often synthetic one ton of crude monomer, approximately produce 5 ~ 10% high boiling material, produces 1 ~ 3% low-boiling-point substance.Yet these high boiling material, low-boiling-point substance be due to its complicated component, separation difficulty, and utility value is lower, and has strong corrodibility, stores and utilizes all more difficultly, becomes the difficult problem that impact and the industry of restriction organosilicon further develop.
At present, for the research of organosilicon high-boiling product low-boiling-point substance comprehensive utilization, be mainly cracking process and prepare methyl chlorosilane monomer both at home and abroad, cracking process prepares single silane and has complex process, severe reaction conditions, catalyzer are easily poisoning, and the problems such as the single silane productive rate that is worth is low of utilizing are arranged.
Summary of the invention
The object of the present invention is to provide a kind of technological process of production short, productive capacity is easy to control, constant product quality, and in production process, utilize organosilicon high-boiling product, the low-boiling-point substance cohydrolysis of three-waste free discharge prepares the production method of silicone oil.
The present invention adopts following technical scheme:
A kind of method of utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil adopts following steps to carry out: to add in proportion the monomer mixing kettle to mix high boiling material, low-boiling-point substance, inorganic salt and water are added in hydrolysis kettle in proportion mix; High boiling material is the by product of direct synthesis methyl chlorosilane, be main chain with Si-Si, Si-O-Si, Si-C-Si are main multiple silane mixture, its density is 1. 13 g/ cm
3
, boiling range is 80 ℃～215 ℃;
The organosilicon low-boiling-point substance is the by product of direct synthesis methyl chlorosilane, is boiling point lower than the multiple silane mixture of 40 ℃, and main component is (CH
3
)
4
Si, (CH
3
)
2
HSiCl, CH
3
HSiCl
2
The weight ratio of high boiling material and low-boiling-point substance is 1:0.1 ~ 3;
Slowly splash into mix monomer in hydrolysis kettle, controlling temperature of reaction is 10 ℃ ~ 80 ℃, adjust monomer dropping speed according to the hydrolysis kettle temperature of reaction, be controlled in 2～3 hours monomer is dripped off, then the temperature of reaction that raises refluxed 1 hour, further facilitation of hydrolysis is complete, and the hydrogen chloride gas that will react simultaneously generation is sent into the water spray column by extractor fan and absorbed;
Reaction solution is moved into standing demix in acid trap, obtain acid silicone oil and dilute hydrochloric acid, acid Silicone oil injection neutralization reaction still is carried out neutralization reaction, the reactant after neutralization obtains the silicone oil product after filtration.
Adopt the present invention of technique scheme compared with prior art, owing to adopting high boiling material and low-boiling-point substance cohydrolysis technique, make production technique easily control, product is with active reactive group, under certain condition can crosslinked film forming, enlarged the use range of silicone oil.Adopt simultaneously the inorganic salt solution hydrolysis process, effectively improved the easy emulsification of hydrolysis silicone oil, the layering difficulty waits technical barrier.
It is low that the present invention has a production cost, easy control of reaction conditions, and oil yield is high, and it is controlled that product viscosity is adjustable, and the silicone oil of preparation has certain reactive behavior, and by-product dilute hydrochloric acid is outer selling directly, produces without advantages such as three wastes generations.
The technical target of the product that technique scheme obtains is as follows:
Outward appearance: faint yellow to colourless transparent oil liquid, machinery-free impurity; Viscosity (25 ℃, mm
2
/ s): 10～100; Refractive index (25 ℃): 1.43～1.47; PH value: 6.0～8.0; Density (g/cm
3
): 0.95～1.10.
Preferred version of the present invention is:
Inorganic salt are one or more in sodium carbonate, sodium bicarbonate, sodium sulfate, salt of wormwood, vitriolate of tartar, Repone K, sodium-chlor, calcium chloride; The concentration of inorganic salt is 1% to saturated.
The neutralizing agent that adds in the neutralization reaction still is one or more in sodium carbonate, sodium bicarbonate, bicarbonate of ammonia, ammoniacal liquor.
The weight ratio of high boiling material and low-boiling-point substance is 1:1 or 1:2 or 1:0.2.
The concentration of inorganic salt is 2% or 5% or 10%.
Inorganic salt are sodium carbonate or sodium-chlor or vitriolate of tartar.
Neutralizing agent is sodium carbonate or bicarbonate of ammonia or ammoniacal liquor.
The present invention also is applicable to high boiling material, low-boiling-point substance, the independent hydrolysis process of azeotrope, and wherein both or three's cohydrolysis prepare the silicone oil process.
Embodiment
Embodiment 1:
A kind of method for preparing silicone oil with organosilicon high-boiling product, low-boiling-point substance cohydrolysis, its processing step is as follows:
Add the monomer mixing kettle to mix by weight 1:0.2 high boiling material, low-boiling-point substance, 10 weight part sodium carbonate and 90 weight parts waters are added in hydrolysis kettle in proportion mix, be made into 10% concentration salt brine solution.
Slowly splash into 100 weight part mix monomers in hydrolysis kettle, controlling temperature of reaction is 10 ℃～80 ℃, adjust monomer dropping speed according to the hydrolysis kettle temperature of reaction, be controlled in 2～3 hours monomer is dripped off, then the temperature of reaction to 80 that raises ℃ backflow 1 hour, further facilitation of hydrolysis is complete, and the hydrogen chloride gas that will react simultaneously generation is sent into the water spray column by extractor fan and absorbed;
Reaction solution is moved into standing demix in acid trap, obtain acid silicone oil and dilute hydrochloric acid, acid Silicone oil injection neutralization reaction still is carried out neutralization reaction, add in the sodium carbonate of 10 weight parts and 2～3 hours, pH value is neutrality, completes N-process; Reactant after neutralization obtains the silicone oil product after filtration.
Embodiment 2:
A kind of method for preparing silicone oil with organosilicon high-boiling product low-boiling-point substance cohydrolysis, its processing step is as follows:
Add the monomer mixing kettle to mix by weight 1:1 high boiling material, low-boiling-point substance, 5 weight part sodium-chlor and 95 weight parts waters are added in hydrolysis kettle in proportion mix, be made into 5% concentration salt brine solution.
Slowly splash into 100 weight part mix monomers in hydrolysis kettle, controlling temperature of reaction is 10 ℃～80 ℃, adjust monomer dropping speed according to the hydrolysis kettle temperature of reaction, be controlled in 2～3 hours monomer is dripped off, then the temperature of reaction to 80 that raises ℃, refluxed 1 hour, further facilitation of hydrolysis is complete, and the hydrogen chloride gas that will react simultaneously generation is sent into the water spray column by extractor fan and absorbed.
Reaction solution is moved into standing demix in acid trap, obtain acid silicone oil and dilute hydrochloric acid, acid Silicone oil injection neutralization reaction still is carried out neutralization reaction, add in the bicarbonate of ammonia of 15 weight parts and 2～3 hours, pH value is neutrality, completes N-process; Reactant after neutralization obtains the silicone oil product after filtration.
Embodiment 3:
A kind of method for preparing silicone oil with organosilicon high-boiling product low-boiling-point substance cohydrolysis, its processing step is as follows:
Add the monomer mixing kettle to mix by weight 1:2 high boiling material, low-boiling-point substance, 2 weight part vitriolate of tartar and 98 weight parts waters are added in hydrolysis kettle in proportion mix, be made into 2% concentration salt brine solution.
Slowly splash into 100 weight part mix monomers in hydrolysis kettle, controlling temperature of reaction is 10 ℃～80 ℃, adjust monomer dropping speed according to the hydrolysis kettle temperature of reaction, be controlled in 2～3 hours monomer is dripped off, then the temperature of reaction to 80 that raises ℃, refluxed 1 hour, further facilitation of hydrolysis is complete, and the hydrogen chloride gas that will react simultaneously generation is sent into the water spray column by extractor fan and absorbed.
Reaction solution is moved into standing demix in acid trap, obtain acid silicone oil and dilute hydrochloric acid, acid Silicone oil injection neutralization reaction still is carried out neutralization reaction, add the ammonia neutralization 2～3 hours of 5 weight parts, the pH value is neutral, completes N-process; Reactant after neutralization obtains the silicone oil product after filtration.
Embodiment 4:
A kind of method for preparing silicone oil with organosilicon high-boiling product low-boiling-point substance cohydrolysis, its processing step is as follows:
Add the monomer mixing kettle to mix by weight 1:2 high boiling material, low-boiling-point substance, 2 weight part vitriolate of tartar and 98 weight parts waters are added in hydrolysis kettle in proportion mix, be made into 2% concentration salt brine solution.
Slowly splash into 100 weight part mix monomers in hydrolysis kettle, controlling temperature of reaction is 60 ℃, adjust monomer dropping speed according to the hydrolysis kettle temperature of reaction, be controlled in 3 hours monomer is dripped off, then the temperature of reaction to 80 that raises ℃, refluxed 1 hour, further facilitation of hydrolysis is complete, and the hydrogen chloride gas that will react simultaneously generation is sent into the water spray column by extractor fan and absorbed.
Reaction solution is moved into standing demix in acid trap, obtain acid silicone oil and dilute hydrochloric acid, acid Silicone oil injection neutralization reaction still is carried out neutralization reaction, add the ammonia neutralization 3 hours of 5 weight parts, the pH value is neutral, completes N-process; Reactant after neutralization obtains the silicone oil product after filtration.
Embodiment 5:
A kind of method for preparing silicone oil with organosilicon high-boiling product low-boiling-point substance cohydrolysis, its processing step is as follows:
Add the monomer mixing kettle to mix by weight 1:1 high boiling material, low-boiling-point substance, 5 weight part sodium-chlor and 95 weight parts waters are added in hydrolysis kettle in proportion mix, be made into 5% concentration salt brine solution.
Slowly splash into 100 weight part mix monomers in hydrolysis kettle, controlling temperature of reaction is 70 ℃, adjust monomer dropping speed according to the hydrolysis kettle temperature of reaction, be controlled in 2 hours monomer is dripped off, then the temperature of reaction to 80 that raises ℃, refluxed 1 hour, further facilitation of hydrolysis is complete, and the hydrogen chloride gas that will react simultaneously generation is sent into the water spray column by extractor fan and absorbed.
Reaction solution is moved into standing demix in acid trap, obtain acid silicone oil and dilute hydrochloric acid, acid Silicone oil injection neutralization reaction still is carried out neutralization reaction, add in the bicarbonate of ammonia of 15 weight parts and 2 hours, pH value is neutrality, completes N-process; Reactant after neutralization obtains the silicone oil product after filtration.
Embodiment 6:
A kind of method for preparing silicone oil with organosilicon high-boiling product, low-boiling-point substance cohydrolysis, its processing step is as follows:
Add the monomer mixing kettle to mix by weight 1:0.2 high boiling material, low-boiling-point substance, 10 weight part sodium carbonate and 90 weight parts waters are added in hydrolysis kettle in proportion mix, be made into 10% concentration salt brine solution.
Slowly splash into 100 weight part mix monomers in hydrolysis kettle, controlling temperature of reaction is 50 ℃, adjust monomer dropping speed according to the hydrolysis kettle temperature of reaction, be controlled in 3 hours monomer is dripped off, then the temperature of reaction to 80 that raises ℃ backflow 1 hour, further facilitation of hydrolysis is complete, and the hydrogen chloride gas that will react simultaneously generation is sent into the water spray column by extractor fan and absorbed;
Reaction solution is moved into standing demix in acid trap, obtain acid silicone oil and dilute hydrochloric acid, acid Silicone oil injection neutralization reaction still is carried out neutralization reaction, add in the sodium carbonate of 10 weight parts and 3 hours, pH value is neutrality, completes N-process; Reactant after neutralization obtains the silicone oil product after filtration.
The present invention adopts organosilicon high-boiling product low-boiling-point substance normal temperature cohydrolysis technique to prepare silicone oil, easy control of reaction conditions, and oil yield is up to 80%, it is controlled that product viscosity is adjustable, the silicone oil of preparation has certain reactive behavior, under certain condition can the crosslinking curing film forming, and utility value is higher.Adopt simultaneously the inorganic salt solution hydrolysis process, effectively improved the easy emulsification of hydrolysis silicone oil, the layering difficulty waits technical barrier.
The present invention effectively solved present domestic in high boiling material low-boiling-point substance comprehensive utilization product and the comparatively single problem of route.
Claims (10)
1. method of utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil, adopt following steps to carry out:
Add in proportion the monomer mixing kettle to mix high boiling material, low-boiling-point substance, inorganic salt and water are added in hydrolysis kettle in proportion mix; High boiling material is the by product of direct synthesis methyl chlorosilane, be main chain with Si-Si, Si-O-Si, Si-C-Si are main multiple silane mixture, its density is 1. 13 g/ cm
3, boiling range is 80 ℃～215 ℃;
The organosilicon low-boiling-point substance is the by product of direct synthesis methyl chlorosilane, is boiling point lower than the multiple silane mixture of 40 ℃, and main component is (CH
3)
4Si, (CH
3)
2HSiCl, CH
3HSiCl
2The weight ratio of high boiling material and low-boiling-point substance is 1:0.1 ~ 3;
Slowly splash into mix monomer in hydrolysis kettle, controlling temperature of reaction is 10 ℃ ~ 80 ℃, adjust monomer dropping speed according to the hydrolysis kettle temperature of reaction, be controlled in 2～3 hours monomer is dripped off, then the temperature of reaction that raises refluxed 1 hour, further facilitation of hydrolysis is complete, and the hydrogen chloride gas that will react simultaneously generation is sent into the water spray column by extractor fan and absorbed;
Reaction solution is moved into standing demix in acid trap, obtain acid silicone oil and dilute hydrochloric acid, acid Silicone oil injection neutralization reaction still is carried out neutralization reaction, the reactant after neutralization obtains the silicone oil product after filtration.
2. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 1, it is characterized in that: described inorganic salt are one or more in sodium carbonate, sodium bicarbonate, sodium sulfate, salt of wormwood, vitriolate of tartar, Repone K, sodium-chlor, calcium chloride; The concentration of inorganic salt is 1% to saturated.
3. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 1, it is characterized in that: the neutralizing agent that adds in the neutralization reaction still is one or more in sodium carbonate, sodium bicarbonate, bicarbonate of ammonia, ammoniacal liquor.
4. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 1, it is characterized in that: the weight ratio of high boiling material and low-boiling-point substance is 1:1 or 1:2 or 1:0.2.
5. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 1 and 2, it is characterized in that: the concentration of inorganic salt is 2% or 5% or 10%.
6. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 1 and 2, it is characterized in that: described inorganic salt are sodium carbonate.
7. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 1 and 2, it is characterized in that: described inorganic salt are sodium-chlor.
8. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 3, it is characterized in that: neutralizing agent is sodium carbonate.
9. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 3, it is characterized in that: neutralizing agent is bicarbonate of ammonia.
10. the method for utilizing organosilicon high-boiling product, low-boiling-point substance cohydrolysis to prepare silicone oil according to claim 3, it is characterized in that: neutralizing agent is ammoniacal liquor.
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Cited By (9)
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|---|---|---|---|---|
| CN103539810A (en) * | 2013-10-23 | 2014-01-29 | 泸州北方化学工业有限公司 | Treatment method of organic silicon low-boiling-point substance |
| CN105061766A (en) * | 2015-09-16 | 2015-11-18 | 浙江新安化工集团股份有限公司 | Treatment device and method for organic silicon waste liquor |
| CN106397474A (en) * | 2016-08-29 | 2017-02-15 | 山东东岳有机硅材料有限公司 | Method for reducing acid content of dimethyldichlorosilane hydrolysate |
| CN106589376A (en) * | 2016-11-30 | 2017-04-26 | 江西蓝星星火有机硅有限公司 | High-quality high-boiling silicone oil and preparation method thereof |
| CN107075119A (en) * | 2014-09-30 | 2017-08-18 | 株式会社钟化 | The manufacture method of silicone resin |
| CN107603230A (en) * | 2017-08-25 | 2018-01-19 | 山东东岳有机硅材料有限公司 | Silicon rubber prepared using organosilicon low boiling hydrolysate and preparation method thereof |
| CN108726484A (en) * | 2018-08-03 | 2018-11-02 | 山东东岳有机硅材料股份有限公司 | The method of organic silicon low-boiling-point substance reforming catalyst recycling |
| CN109569489A (en) * | 2018-12-05 | 2019-04-05 | 江西华昊化工有限公司 | A kind of process units and its preparation process of high boiling point silicon oil |
| CN115197424A (en) * | 2022-08-05 | 2022-10-18 | 鲁西化工集团股份有限公司硅化工分公司 | Method for preparing polymethylsiloxane through alcoholysis of organic silicon azeotrope and high-boiling-point substance |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539810B (en) * | 2013-10-23 | 2016-06-15 | 泸州北方化学工业有限公司 | The processing method of organic silicon low-boiling-point substance |
| CN103539810A (en) * | 2013-10-23 | 2014-01-29 | 泸州北方化学工业有限公司 | Treatment method of organic silicon low-boiling-point substance |
| CN107075119A (en) * | 2014-09-30 | 2017-08-18 | 株式会社钟化 | The manufacture method of silicone resin |
| CN105061766A (en) * | 2015-09-16 | 2015-11-18 | 浙江新安化工集团股份有限公司 | Treatment device and method for organic silicon waste liquor |
| CN105061766B (en) * | 2015-09-16 | 2017-08-25 | 浙江新安化工集团股份有限公司 | The processing unit and method of a kind of organic silicon waste liquid |
| CN106397474A (en) * | 2016-08-29 | 2017-02-15 | 山东东岳有机硅材料有限公司 | Method for reducing acid content of dimethyldichlorosilane hydrolysate |
| CN106397474B (en) * | 2016-08-29 | 2018-11-09 | 山东东岳有机硅材料股份有限公司 | A kind of method of acid content in reduction Dimethyldichlorosilane hydrolysate |
| CN106589376B (en) * | 2016-11-30 | 2019-05-03 | 江西蓝星星火有机硅有限公司 | A kind of high-quality high boiling point silicon oil and preparation method thereof |
| CN106589376A (en) * | 2016-11-30 | 2017-04-26 | 江西蓝星星火有机硅有限公司 | High-quality high-boiling silicone oil and preparation method thereof |
| CN107603230A (en) * | 2017-08-25 | 2018-01-19 | 山东东岳有机硅材料有限公司 | Silicon rubber prepared using organosilicon low boiling hydrolysate and preparation method thereof |
| CN108726484A (en) * | 2018-08-03 | 2018-11-02 | 山东东岳有机硅材料股份有限公司 | The method of organic silicon low-boiling-point substance reforming catalyst recycling |
| CN108726484B (en) * | 2018-08-03 | 2021-10-22 | 山东东岳有机硅材料股份有限公司 | Method for recycling organosilicon low-boiling-point substance conversion catalyst |
| CN109569489A (en) * | 2018-12-05 | 2019-04-05 | 江西华昊化工有限公司 | A kind of process units and its preparation process of high boiling point silicon oil |
| CN109569489B (en) * | 2018-12-05 | 2021-07-30 | 江西华昊化工有限公司 | Production device and preparation process of high-boiling silicone oil |
| CN115197424A (en) * | 2022-08-05 | 2022-10-18 | 鲁西化工集团股份有限公司硅化工分公司 | Method for preparing polymethylsiloxane through alcoholysis of organic silicon azeotrope and high-boiling-point substance |
| CN115197424B (en) * | 2022-08-05 | 2023-08-22 | 鲁西化工集团股份有限公司硅化工分公司 | Method for preparing polymethyl siloxane by alcoholysis of organosilicon azeotrope and high-boiling-point substance |
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Application publication date: 20130605 |