CN101434510A - Method and apparatus for recovering methyl chloride in organosilicon monomer synthesis - Google Patents

Method and apparatus for recovering methyl chloride in organosilicon monomer synthesis Download PDF

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Publication number
CN101434510A
CN101434510A CNA200810238480XA CN200810238480A CN101434510A CN 101434510 A CN101434510 A CN 101434510A CN A200810238480X A CNA200810238480X A CN A200810238480XA CN 200810238480 A CN200810238480 A CN 200810238480A CN 101434510 A CN101434510 A CN 101434510A
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methyl chloride
tower
crude monomer
monomer
crude
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CN101434510B (en
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王维东
伊港
赵玉芳
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Shandong Dongyue organosilicon material Limited by Share Ltd
Beijing Petrochemical Engineering Co Ltd
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SHANDONG DONGYUE SILICON MATERIAL CO Ltd
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Abstract

The invention relates to a recycling method of methyl chloride in the synthesis and production of an organic silicon monomer, and equipment thereof. The synthesis gas sent out from a fluidized bed reactor is transmitted into a crude monomer-methyl chloride tower after the processes of washing, dedusting and condensating; the gas can directly separate noncondensable gas, methyl chloride and crude monomer. The methyl chloride is extracted from the sidetrack of the crude monomer-methyl chloride tower, and is transmitted into a methyl chloride recovery drum after being condensated by a methyl chloride condenser. The method changes rear-system prior three-tower process flow into two-tower process flow, and controls temperature and pressure, therefore, the methyl chloride in the crude product of the monomer and the hydrocarbonaceous component and impurity in the methyl chloride are eliminated simultaneously so as to reach the technique requirement of the crude monomer product and the recycling of the methyl chloride. The method simplifies the process of recycling the methyl chloride so that one-off equipment investment and the energy consumption in the producing process can be reduced.

Description

The recovery method and the equipment of methyl chloride in the synthetic production of a kind of organosilane monomer
Technical field
The present invention relates to the recovery method and the equipment of methyl chloride in the synthetic production of a kind of organosilane monomer, belong to the organosilicon technical field.
Background technology
In the methyl chlorosilane monomer synthesis and production process, because raw material methyl chloride per pass conversion is lower, generally between 20%-40%, the methyl chloride internal circulating load is big, causes energy dissipation also very big.
Existing methyl chloride reclaims technical process: a part enters the methyl chloride tower from the thick methyl chloride of crude monomer overhead distillate through condensation; A part is sent into the methyl chloride tower from the thick methyl chloride gas from washing tower tail cooler behind methane compression system compression condensation.The methyl chloride column overhead is given vent to anger behind cooling condensation, the liquid phase total reflux, and non-condensable gas send the methyl chloride compression system; The crude monomer tower is returned in the discharging of tower still; Reclaim methyl chloride and extract out, after condensation, send the methyl chloride withdrawing can, recycle with new methyl chloride from tower side line gas phase.As publication number is the Chinese patent of CN1438226, discloses a kind of using inorganic chlorosilane gas wet dedusting technology.It will be from the synthetic gas of secondary cyclone, and in wash tower bottoms entered tower, the feed liquid that the tower still is discharged entered flash tank, gas after the flash distillation enters flash condenser and carries out condensation, noncondensable gas is by water wash column washing back emptying, and phlegma enters and reclaims the liquid groove, and residue enters the waste residue groove.Overhead gas enters the scrubber overhead pre-cooler, gas phase behind washing tower overhead condenser deep cooling, non-condensable gas dechlorination methane surge tank, phlegma enters the crude monomer tundish, partial reflux is in tower, the part discharging send the crude monomer tower to handle.This methyl chloride recovery system technical process shortcoming is: it is excessive to reclaim in the methyl chloride process energy consumption, causes producing the crude monomer cost and rises.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, the method and the specific equipment thereof that reclaim methyl chloride in the synthetic production of a kind of organosilane monomer are provided.
Summary of the invention
The present invention relates to a kind of organosilane monomer and synthesize the method and apparatus that reclaims methyl chloride in the production, it reclaims technical process by optimizing methyl chloride: system's three tower process flow scheme improvements were two tower process flow processs after existing organosilane monomer was synthesized.Utilize methyl chloride different with the crude monomer boiling point, realization crude monomer tower and methyl chloride tower are merged into a crude monomer-methyl chloride tower, the tower still produces crude monomer, cat head takes the total reflux mode to remove than the low-boiling non-condensable gas of methyl chloride, the unconverted methyl chloride of tower middle and upper part side line gas phase extraction, after condensation, deliver to the methyl chloride accumulator tank again, enter fluidized-bed reactor with the new raw material methyl chloride.
Crude monomer of the present invention, methyl chloride separation and purification process are carried out in a tower of optimization design simultaneously, control certain service temperature and working pressure, make the methyl chloride in the crude monomer product, the hydrocarbon components impurity in the methyl chloride remove simultaneously, the technical requirements that reaches the crude monomer product and reclaim methyl chloride.Present method has been simplified the existing crude monomer that separates earlier, re-refines and reclaims the complicated flow process of methyl chloride, thereby greatly reduce disposable apparatus investment and production process energy consumption, remarkable in economical benefits is installed.
Detailed Description Of The Invention
Technical scheme of the present invention is as follows:
The recovery method of methyl chloride in the synthetic production of a kind of organosilane monomer, it is characterized in that, from the synthetic gas of fluidized-bed reactor output after scrubbing dust collection and condensation, enter crude monomer-methyl chloride tower, directly non-condensable gas, methyl chloride and crude monomer are separated, methyl chloride enters the methyl chloride withdrawing can by crude monomer-methyl chloride tower top side line extraction after the methyl chloride condenser condenses.
The methyl chloride of above-mentioned recovery can enter fluidized-bed reactor and participate in reaction after the new raw material methyl chloride mixes.
In the recovery method of above-mentioned methyl chloride, separate the gas part that obtains in described crude monomer-methyl chloride tower and discharge, after condensation, be back in the tower by cat head.A small amount of uncooled gas is discharged by the condenser exhaust pipe.
In the recovery method of above-mentioned methyl chloride, separating the liquid phase part that obtains in described crude monomer-methyl chloride tower is the crude monomer product, by crude monomer-methyl chloride tower bottom extraction.
Preferably, described crude monomer-methyl chloride Tata internal pressure is 0.45-0.85mpa.
Preferably, the heat-eliminating medium of described crude monomer-methyl chloride overhead condenser is-30~-37 ℃ a refrigerating fulid.
Preferably, described crude monomer-methyl chloride overhead gas temperature is 38~42 ℃.
Preferably, described crude monomer-methyl chloride overhead condensation liquid temp is 35~45 ℃.
Preferably, the methyl chloride condenser heat-eliminating medium of described crude monomer-methyl chloride tower side line is 20~40 ℃ of recirculated waters.
A kind of specific equipment of above-mentioned recovery method, comprise washing tower, crude monomer-methyl chloride tower, methyl chloride withdrawing can, crude monomer reboiler, the opening for feed of crude monomer-methyl chloride tower links to each other with the washing tower outlet, crude monomer-methyl chloride tower upper portion side wall is established the methyl chloride outlet and is linked to each other with the methyl chloride withdrawing can, the bottom of crude monomer-methyl chloride tower is linked to each other with the crude monomer reboiler by liquid exit (crude monomer exports extraction by this), the overhead gas outlet of crude monomer-methyl chloride tower is connected with the phlegma return tank, and return tank is communicated with crude monomer-methyl chloride tower again.
Be provided with condenser between described methyl chloride outlet and the methyl chloride withdrawing can, be provided with crude monomer-methyl chloride overhead gas condenser between overhead gas outlet and the phlegma return tank.
Described crude monomer-methyl chloride tower is a tray column, and valve tray is arranged in the tower.
The discharge port of described crude monomer reboiler is provided with the crude monomer reactor product cooler.
The overhead gas condenser of described crude monomer-methyl chloride tower is provided with exhaust pipe, is used to discharge a small amount of uncooled gas.
Aforesaid method step and equipment unit all can adopt state of the art if no special instructions.
Beneficial effect of the present invention is as follows:
1. crude monomer-methyl chloride overhead condenser heat-eliminating medium is adopted as-30~-37 ℃ of refrigerating fulids, replaces the crude monomer overhead condenser in the former technical process, methyl chloride overhead condenser, methyl chloride tower tail gas condenser.
2. crude monomer-methyl chloride overhead gas carries out total reflux operation through the condensed lime set of overhead condenser that heat-eliminating medium is adopted as-30~-37 ℃ of refrigerating fulids.Noncondensable gas enters exhaust pipe.Reduce the methyl chloride content in the process tail gas gas that removes incinerator, improve the methyl chloride cyclic utilization rate.
3. crude monomer-methyl chloride tower side line extraction methyl chloride gas, the phlegma that obtains through the side line condenser condenses enters the methyl chloride withdrawing can, reclaims pump through methyl chloride and squeezes into methyl chloride and reclaim storage tank.The side line condenser adopts recirculated water as heat-eliminating medium, and other alkanes gas of the trace that only contains in the material realizes that a tower directly reclaims methyl chloride purity and reaches more than 99%.
4. crude monomer-methyl chloride Tata still liquid phase extraction methyl chloride content is less than 0.1% qualified crude monomer product, and depended on pressure enters in the crude monomer basin after the cooling of product water cooler.
5. this reclaims the facility investment of methyl chloride process flow saves, saves the energy consumption in the production process.Obvious economic.
Description of drawings
Fig. 1 is a production process equipment synoptic diagram of the present invention; Wherein, 1, washing tower; 2, crude monomer-methyl chloride tower; 3, crude monomer-methyl chloride overhead gas condenser; 4, gas-condensate liquid return tank; 5, exhaust pipe; 6, reflux pump; 7, the methyl chloride condenser of side line; 8, methyl chloride withdrawing can; 9, methyl chloride reclaims pump; The methyl chloride outlet of 10, reclaiming; 11, crude monomer reboiler; 12, crude monomer reactor product cooler; 13, crude monomer products export.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing and embodiment.
Embodiment 1:
The recovery method of methyl chloride utilizes methyl chloride different with the crude monomer boiling point in the synthetic production of a kind of organosilane monomer, directly non-condensable gas, methyl chloride and crude monomer is separated at crude monomer-methyl chloride tower, specifically can adopt following steps to realize:
1) from the synthetic gas of fluidized-bed reactor output after scrubbing dust collection and condensation, through condenser condenses, phlegma enters crude monomer-methyl chloride tower by crude monomer-methyl chloride tower opening for feed by cat head, the tower internal pressure keeps 0.6~0.85Mpa;
2) phlegma is through behind crude monomer-methyl chloride tower, the overhead gas temperature keeps 39~41 ℃, overhead gas is by the crude monomer-methyl chloride overhead condenser condensation of cat head process, heat-eliminating medium is-35 ℃ a refrigerating fulid, gained overhead condensation liquid temp is 37~40 ℃, overhead condensation liquid enters crude monomer-methyl chloride tower return tank, and non-condensable gas is discharged by exhaust pipe;
3) phlegma is through behind crude monomer-methyl chloride tower, and methyl chloride gas is by crude monomer-methyl chloride tower side line extraction, and through crude monomer-methyl chloride tower side line condenser condenses, the methyl chloride phlegma enters the methyl chloride withdrawing can;
4) phlegma is through behind crude monomer-methyl chloride tower, and still liquid is qualified crude monomer product at the bottom of crude monomer-methyl chloride Tata, and extraction gets final product.
A kind of specific equipment of above-mentioned recovery method, comprise washing tower 1, crude monomer-methyl chloride tower 2, methyl chloride withdrawing can 8, crude monomer reboiler 11, the opening for feed of crude monomer-methyl chloride tower 2 links to each other with washing tower 1 outlet, crude monomer-methyl chloride tower 2 upper portion side wall are established the methyl chloride outlet and are linked to each other with methyl chloride withdrawing can 8 by condenser 7, the bottom of crude monomer-methyl chloride tower 2 is linked to each other with crude monomer reboiler 11 by liquid exit (crude monomer exports extraction by this), and the discharge port of crude monomer reboiler 11 is provided with crude monomer reactor product cooler 12.The overhead gas outlet of crude monomer-methyl chloride tower 2 is connected with phlegma return tank 4 by crude monomer-methyl chloride overhead gas condenser 3, and the phlegma return tank is communicated with crude monomer-methyl chloride tower 2 again.Crude monomer-methyl chloride overhead gas condenser 3 is provided with exhaust pipe 5, is used to discharge a small amount of uncooled gas; Crude monomer-methyl chloride tower 2 is tray columns, and valve tray is arranged in the tower.
Present method production method is more in the past produced crude monomer product energy consumption per ton aspect and can be saved 500 yuan; The methyl chloride utilization ratio can improve 2%; Existing production method is owing to reduce equipment such as tower and condenser, and every covering device equipment investment cost descends about 5%.
Embodiment 2:
A kind of embodiment 1 described recovery method, its difference are that the heat-eliminating medium of crude monomer-methyl chloride overhead condenser is-32 ℃ a refrigerating fulid, and crude monomer-methyl chloride Tata internal pressure is 0.45~0.6mpa; Equipment is with embodiment 1.
Produce crude monomer product energy consumption per ton aspect by this method and can save 450 yuan; The methyl chloride utilization ratio can improve 1.5%.
Embodiment 3:
A kind of embodiment 1 described recovery method, its difference are that the heat-eliminating medium of crude monomer-methyl chloride overhead condenser is-37 ℃ a refrigerating fulid, and crude monomer-methyl chloride Tata internal pressure is 0.5~0.7mpa; Equipment is with embodiment 1.
Produce crude monomer product energy consumption per ton aspect by this method and can save 400 yuan; The methyl chloride utilization ratio can improve 1.7%.

Claims (10)

1. an organosilane monomer is synthetic produce in the recovery method of methyl chloride, it is characterized in that, from the synthetic gas of fluidized-bed reactor output after scrubbing dust collection and condensation, enter crude monomer-methyl chloride tower, directly non-condensable gas, methyl chloride and crude monomer are separated, methyl chloride enters the methyl chloride withdrawing can by crude monomer-methyl chloride tower top side line extraction after the methyl chloride condenser condenses.
2. the recovery method of methyl chloride as claimed in claim 1 is characterized in that, the methyl chloride of above-mentioned recovery can enter fluidized-bed reactor and participate in reaction after the new raw material methyl chloride mixes.
3. the recovery method of methyl chloride as claimed in claim 1 is characterized in that, separates the gas part that obtains in described crude monomer-methyl chloride tower and is discharged by cat head, is back to after condensation in the tower, and a small amount of uncooled gas is discharged by the condenser exhaust pipe.
4. the recovery method of methyl chloride as claimed in claim 1 is characterized in that, separating the liquid phase part that obtains in described crude monomer-methyl chloride tower is the crude monomer product, by crude monomer-methyl chloride tower bottom extraction.
5. the recovery method of methyl chloride as claimed in claim 1 is characterized in that, described crude monomer-methyl chloride Tata internal pressure is 0.45-0.85Mpa.
6. the recovery method of methyl chloride as claimed in claim 1 is characterized in that, the heat-eliminating medium of described crude monomer-methyl chloride overhead condenser is-30~-37 ℃ a refrigerating fulid.
7. the recovery method of methyl chloride as claimed in claim 1 is characterized in that, described crude monomer-methyl chloride overhead gas temperature is 38~42 ℃.
8. the recovery method of methyl chloride as claimed in claim 1 is characterized in that, described crude monomer-methyl chloride overhead condensation liquid temp is 35~45 ℃.
9. the recovery method of methyl chloride as claimed in claim 1 is characterized in that, the methyl chloride condenser heat-eliminating medium of described crude monomer-methyl chloride tower side line is 20~40 ℃ of recirculated waters.
10. the specific equipment of the described methyl chloride recovery method of claim 1, comprise washing tower, crude monomer-methyl chloride tower, methyl chloride withdrawing can, crude monomer reboiler, the opening for feed of crude monomer-methyl chloride tower links to each other with the washing tower outlet, crude monomer-methyl chloride tower upper portion side wall is established the methyl chloride outlet and is linked to each other with the methyl chloride withdrawing can, the bottom of crude monomer-methyl chloride tower is linked to each other with the crude monomer reboiler by liquid exit, the overhead gas outlet of crude monomer-methyl chloride tower is connected with the phlegma return tank, and return tank is communicated with crude monomer-methyl chloride tower again.
CN200810238480XA 2008-12-19 2008-12-19 Method and apparatus for recovering methyl chloride in organosilicon monomer synthesis Active CN101434510B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101870709A (en) * 2010-06-25 2010-10-27 天津大学 Method for refining and reclaiming chloromethane from organic silicon production process
CN103055614A (en) * 2012-12-25 2013-04-24 蓝星化工新材料股份有限公司江西星火有机硅厂 Process for reclaimed chloromethane purification and device thereof
CN105503935A (en) * 2015-11-24 2016-04-20 湖北兴瑞化工有限公司 Method for recovery and utilization of vented tail gas of organosilicon crude monomer synthesis
CN108689798A (en) * 2018-06-28 2018-10-23 湖北兴瑞硅材料有限公司 A method of improving organic silicon monomer synthesis recycling chloromethanes quality
CN110590828A (en) * 2019-09-26 2019-12-20 合盛硅业股份有限公司 Methyl chlorosilane synthesis equipment and parking method
CN113861232A (en) * 2021-10-08 2021-12-31 华陆工程科技有限责任公司 Improved method and device for energy conservation and quality improvement of organic silicon production system

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3610706A1 (en) * 1986-03-29 1987-10-08 Bayer Ag Purification of methyl chloride during continuous methylchlorosilane synthesis
CN100434431C (en) * 2003-01-07 2008-11-19 蓝星化工新材料股份有限公司江西星火有机硅厂 Wet-dusting and high-boiling-point separation technology for organic silane chloride synthesized gas
CN101148394B (en) * 2006-09-21 2011-03-16 蓝星化工新材料股份有限公司 Method for separating methyl chlorosilane and methyl chloride by technique of increasing and reducing pressure
CN101148453B (en) * 2006-09-21 2010-05-12 蓝星化工新材料股份有限公司 Dry dust removing method by using inorganic chlorosilane gas and device thereof

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101870709A (en) * 2010-06-25 2010-10-27 天津大学 Method for refining and reclaiming chloromethane from organic silicon production process
CN101870709B (en) * 2010-06-25 2012-08-08 天津大学 Method for refining and reclaiming chloromethane from organic silicon production process
CN103055614A (en) * 2012-12-25 2013-04-24 蓝星化工新材料股份有限公司江西星火有机硅厂 Process for reclaimed chloromethane purification and device thereof
CN103055614B (en) * 2012-12-25 2014-08-27 蓝星化工新材料股份有限公司江西星火有机硅厂 Process for reclaimed chloromethane purification and device thereof
CN105503935A (en) * 2015-11-24 2016-04-20 湖北兴瑞化工有限公司 Method for recovery and utilization of vented tail gas of organosilicon crude monomer synthesis
CN105503935B (en) * 2015-11-24 2018-05-29 湖北兴瑞化工有限公司 A kind of method for the emptying end gas for recycling and being synthesized using organosilicon crude monomer
CN108689798A (en) * 2018-06-28 2018-10-23 湖北兴瑞硅材料有限公司 A method of improving organic silicon monomer synthesis recycling chloromethanes quality
CN108689798B (en) * 2018-06-28 2021-10-12 湖北兴瑞硅材料有限公司 Method for improving quality of methyl chloride recovered by synthesizing organic silicon monomer
CN110590828A (en) * 2019-09-26 2019-12-20 合盛硅业股份有限公司 Methyl chlorosilane synthesis equipment and parking method
CN113861232A (en) * 2021-10-08 2021-12-31 华陆工程科技有限责任公司 Improved method and device for energy conservation and quality improvement of organic silicon production system
CN113861232B (en) * 2021-10-08 2024-05-28 华陆工程科技有限责任公司 Improved method and device for energy conservation and quality improvement of organosilicon production system

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