CN102432633A - Alcoholysis process of chloropropyltriethoxysilane - Google Patents
Alcoholysis process of chloropropyltriethoxysilane Download PDFInfo
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- CN102432633A CN102432633A CN2011104034662A CN201110403466A CN102432633A CN 102432633 A CN102432633 A CN 102432633A CN 2011104034662 A CN2011104034662 A CN 2011104034662A CN 201110403466 A CN201110403466 A CN 201110403466A CN 102432633 A CN102432633 A CN 102432633A
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Abstract
The invention relates to an alcoholysis process of chloropropyltriethoxysilane, comprising the following steps: controlling the pressure of an ethanol evaporating pot within 0.1MPa, the liquid level of ethanol below 1/2 liquid level, the transfer pressure of the ethanol within 0.1MPa and the pressure of nitrogen gas input through a pneumatic film valve at 0.2-0.25MPa; opening an ethanol vapor inlet valve of an ethanol heating buffer tank and a conduction oil inlet valve, and controlling the oil temperature of a jacket at 165 DEG C and the temperature in the pot at 135 DEG C; starting up a falling film absorber recirculating cooling water hydrochloric acid storage pump, enabling the negative pressure to reach minus 0.03MPa and a system to keep a constant negative pressure state, opening a chloropropyltrichlorosilane storage and transfer valve, and adjusting and keeping the pressure of the nitrogen gas in the pot at 0.2-0.25MPa; opening an air inlet valve of an intake tower, and controlling the flow of an initial rotor flowmeter of an ethanol gas heating pot at 70m<3>/h, and the temperature on the top of the tower at 50 DEG C; opening a valve of a chloropropyltrichlorosilane feeding rotor flowmeter, adjusting the feed rate and the flow of gas ethanol and keeping the temperature on the top of the tower at 50 DEG C; opening the oil inlet valve in the reaction process, closing the oil inlet valve when the temperature of material is up to 175 DEG C, sampling from a sample connection for analysis, sucking the material into a product collecting pot at negative pressure after products are qualified, and cooling. The conversion rate of products is increased, the content of the products is increased, the production cost is reduced and the economic benefit is increased.
Description
Technical field
The present invention relates to a kind of alcoholysis esterification technique of chloropropyl triethoxysilane alcoholysis process, particularly a kind of γ-chloropropyl triethoxysilane.
Background technology
γ-chloropropyl triethoxysilane is a kind of important silane coupling agent and other kind silane coupling agent synthetic key intermediates; Be used for coupling organic polymer and mineral filler; Strengthen its cohesiveness, improve the machinery of product, performance such as electric, water-fast and anti-aging.Be usually used in industries such as glass, casting, yarn fabric auxiliary agent, insulating material and glue paste, vast market prospect is arranged.
The alcoholysis esterification technique of existing traditional γ-chloropropyl triethoxysilane mainly contains: the alcoholysis esterification takes place in (1) γ-chloropropyl trichloro-silane and absolute ethyl alcohol in common esterifying kettle, the bullion that obtains in sodium ethylate and after the entering distillation system obtain product.This method has following deficiency: reaction process is simple, but reaction conditions is difficult to control, and the processing condition such as constant of temperature and vacuum tightness are had relatively high expectations; Reaction time is long simultaneously; React problems such as incomplete and energy consumption height, and the feedstock conversion utilization ratio is low, it is high to make the bullion foreign matter content.(2) the alcoholysis esterification takes place in γ-chloropropyl trichloro-silane and absolute ethyl alcohol under catalyst actions such as lithium chloride in esterifying kettle, after neutralization, rectifying, obtains product.Though this method has shortened the esterification cycle and improved feed stock conversion, still has difficult control of reaction conditions, γ-chloropropyl trichloro-silane and absolute ethyl alcohol obtain bullion behind the esterifying kettle internal reaction need neutralization, distillation system just can obtain product.
Summary of the invention
Its purpose of the present invention just is to provide a kind of chloropropyl triethoxysilane alcoholysis process, has improved the transformation efficiency of product, has improved product content, has reduced production cost and has increased economic benefit.
The technical scheme that realizes above-mentioned purpose and take, process step of the present invention comprises
(1) the ethanol evaporation pressure tank is controlled in the 0.1MPa, and the ethanol liquid level is controlled at below 1/2nd the liquid level, and the ethanol transfer pressure is controlled within the 0.1MPa, and air bladder valve input nitrogen control pressure is at 0.2-0.25MPa;
(2) open ethanol heating surge tank alcohol vapour intake valve, open the thermal oil fuel charging valve, at 165 ℃, temperature reaches 135 ℃ in the controlling tank with the temperature control of chuck oil;
(3) open falling-film absorber recirculated cooling water hydrochloric acid tank pump, negative pressure is reached-0.03MPa, make system keep the constant negative pressure state, open chloropropyl trichloro-silane storage tank transfer valve, regulate nitrogen pressure 0.2-0.25Mpa in the maintenance jar;
(4) opening the tower intake valve, is 70m with alcohol gas heating tank initial stage spinner-type flowmeter dominant discharge
3/ h, tower top temperature is controlled at 50 ℃;
(5) open chloropropyl trichloro-silane charging spinner-type flowmeter valve, the adjustment inlet amount, adjustment gas alcohol flow keeps tower top temperature at 50 ℃;
(6) in the reaction process, open fuel charging valve, when the material temperature reaches 175 ℃, close fuel charging valve,, with negative pressure material suction product holding tank is cooled off after the qualified products from the thief hole sampling analysis.
Compared with prior art the present invention has the following advantages.
1. the present invention is a gas phase alcoholysis esterification technique, and the gas contact area is big, reacts more abundant, and feed stock conversion can reach 99.8%;
2. the product that goes out through explained hereafter of the present invention, content reach more than 98%, and pH value is 5-6, can satisfy the production needs of derived product, and the present invention has simultaneously save neutralization, rectification process, save production cost, save energy;
3. the present invention adopts Sequential Production, once carries out the reacted pattern of an esterifying kettle with traditional technology and compares, and can improve the production production capacity, practices thrift human cost, enhances productivity.
Description of drawings
Below in conjunction with accompanying drawing the present invention is made further detailed description.
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
Shown in accompanying drawing, process step of the present invention comprises
(1) the ethanol evaporation pressure tank is controlled in the 0.1MPa, and the ethanol liquid level is controlled at below 1/2nd the liquid level, and the ethanol transfer pressure is controlled within the 0.1MPa, and air bladder valve input nitrogen control pressure is at 0.2-0.25MPa;
(2) open ethanol heating surge tank alcohol vapour intake valve, open the thermal oil fuel charging valve, at 165 ℃, temperature reaches 135 ℃ in the controlling tank with the temperature control of chuck oil;
(3) open falling-film absorber recirculated cooling water hydrochloric acid tank pump, negative pressure is reached-0.03MPa, make system keep the constant negative pressure state, open chloropropyl trichloro-silane storage tank transfer valve, regulate nitrogen pressure 0.2-0.25Mpa in the maintenance jar;
(4) opening the tower intake valve, is 70m with alcohol gas heating tank initial stage spinner-type flowmeter dominant discharge
3/ h, tower top temperature is controlled at 50 ℃;
(5) open chloropropyl trichloro-silane charging spinner-type flowmeter valve, the adjustment inlet amount, adjustment gas alcohol flow keeps tower top temperature at 50 ℃;
(6) in the reaction process, open fuel charging valve, when the material temperature reaches 175 ℃, close fuel charging valve,, with negative pressure material suction product holding tank is cooled off after the qualified products from the thief hole sampling analysis.
Embodiment
(1) the ethanol evaporation pressure tank is controlled in the 0.1MPa, the ethanol liquid level is controlled at below 1/2nd the liquid level, and the ethanol transfer pressure is controlled within the 0.1MPa, and air bladder valve input nitrogen control pressure is at 0.2-0.25MPa;
(2) open ethanol heating surge tank alcohol vapour intake valve, open the thermal oil fuel charging valve, at 165 ℃, temperature reaches 135 ℃ in the controlling tank with the temperature control of chuck oil;
(3) open falling-film absorber recirculated cooling water hydrochloric acid tank pump, negative pressure is reached-0.03MPa, make system keep the constant negative pressure state, open chloropropyl trichloro-silane storage tank transfer valve, regulate nitrogen pressure 0.2-0.25Mpa in the maintenance jar;
(4) open the tower intake valve, with alcohol gas heating tank initial stage spinner-type flowmeter, dominant discharge is 70m
3/ h, observing tower serve as a fill-in the temperature display degree and are controlled at 50 ℃.
(5) open chloropropyl trichloro-silane charging spinner-type flowmeter valve, the adjustment inlet amount, adjustment gas alcohol flow keeps tower top temperature at 50 ℃;
(6) observe material reaction situation in the esterifying kettle through visor in the reaction process, open fuel charging valve, when the material temperature reaches 175 ℃, close fuel charging valve,, with negative pressure material suction product holding tank is cooled off after the qualified products from the thief hole sampling analysis;
(7) quality index of the γ-chloropropyl triethoxysilane of above-mentioned prepared is following:
| Sequence number | Detect index | Analytical procedure | Detected result |
| 1 | Outward appearance | Range estimation | Colourless transparent liquid |
| 2 | Purity (GC) % | Vapor-phase chromatography | 98.5% |
| 3 | Density (20 ℃), g/cm 3 | G B /T4472 | 1.01 |
| 4 | A flash-point! ℉) | G B /T1671 | 99℉ |
| 5 | Refractive index (25 ℃) | G B /6488 | 1.418 |
| 6 | ? | ? | ? |
Claims (1)
1. a chloropropyl triethoxysilane alcoholysis process is characterized in that process step comprises
(1) the ethanol evaporation pressure tank is controlled in the 0.1MPa, and the ethanol liquid level is controlled at below 1/2nd the liquid level, and the ethanol transfer pressure is controlled within the 0.1MPa, and air bladder valve input nitrogen control pressure is at 0.2-0.25Mpa;
(2) open ethanol heating surge tank alcohol vapour intake valve, open the thermal oil fuel charging valve, at 165 ℃, temperature reaches 135 ℃ in the controlling tank with the temperature control of chuck oil;
(3) open falling-film absorber recirculated cooling water hydrochloric acid tank pump, negative pressure is reached-0.03MPa, make system keep the constant negative pressure state, open chloropropyl trichloro-silane storage tank transfer valve, regulate nitrogen pressure 0.2-0.25Mpa in the maintenance jar;
(4) opening the tower intake valve, is 70m with alcohol gas heating tank initial stage spinner-type flowmeter dominant discharge
3/ h, tower top temperature is controlled at 50 ℃;
(5) open chloropropyl trichloro-silane charging spinner-type flowmeter valve, the adjustment inlet amount, adjustment gas alcohol flow keeps tower top temperature at 50 ℃;
(6) in the reaction process, open fuel charging valve, when the material temperature reaches 175 ℃, close fuel charging valve,, with negative pressure material suction product holding tank is cooled off after the qualified products from the thief hole sampling analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201110403466.2A CN102432633B (en) | 2011-12-07 | 2011-12-07 | Alcoholysis process of chloropropyltriethoxysilane |
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| CN201110403466.2A CN102432633B (en) | 2011-12-07 | 2011-12-07 | Alcoholysis process of chloropropyltriethoxysilane |
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| CN102432633A true CN102432633A (en) | 2012-05-02 |
| CN102432633B CN102432633B (en) | 2014-05-07 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718791A (en) * | 2012-06-08 | 2012-10-10 | 新亚强硅化学江苏有限公司 | Preparation process of trimethylethoxysilane |
| CN102718792A (en) * | 2012-06-08 | 2012-10-10 | 新亚强硅化学江苏有限公司 | Preparation method of dimethylethoxysilane |
| CN102924504A (en) * | 2012-11-20 | 2013-02-13 | 江西晨光新材料有限公司 | Preparation method of propyl trimethoxy silane |
| CN105542168A (en) * | 2015-12-21 | 2016-05-04 | 浙江衢州正邦有机硅有限公司 | Polymethyl triethoxysilane double-tower continuous production process |
| CN103396432B (en) * | 2013-08-16 | 2016-08-31 | 唐山三友硅业有限责任公司 | Chloromethanes is utilized to produce the device of methylchlorosilane |
| CN111804267A (en) * | 2020-07-10 | 2020-10-23 | 凯莱英医药化学（阜新）技术有限公司 | Continuous reaction equipment and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102718791A (en) * | 2012-06-08 | 2012-10-10 | 新亚强硅化学江苏有限公司 | Preparation process of trimethylethoxysilane |
| CN102718792A (en) * | 2012-06-08 | 2012-10-10 | 新亚强硅化学江苏有限公司 | Preparation method of dimethylethoxysilane |
| CN102924504A (en) * | 2012-11-20 | 2013-02-13 | 江西晨光新材料有限公司 | Preparation method of propyl trimethoxy silane |
| CN103396432B (en) * | 2013-08-16 | 2016-08-31 | 唐山三友硅业有限责任公司 | Chloromethanes is utilized to produce the device of methylchlorosilane |
| CN105542168A (en) * | 2015-12-21 | 2016-05-04 | 浙江衢州正邦有机硅有限公司 | Polymethyl triethoxysilane double-tower continuous production process |
| CN105542168B (en) * | 2015-12-21 | 2019-04-09 | 浙江衢州正邦有机硅有限公司 | A kind of poly- methyltriethoxysilane double tower continuous production technology |
| CN111804267A (en) * | 2020-07-10 | 2020-10-23 | 凯莱英医药化学（阜新）技术有限公司 | Continuous reaction equipment and application thereof |
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