CN103896281A - Method for rectifying and purifying silicon tetrachloride by complete thermal coupling - Google Patents
Method for rectifying and purifying silicon tetrachloride by complete thermal coupling Download PDFInfo
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- CN103896281A CN103896281A CN201410155447.6A CN201410155447A CN103896281A CN 103896281 A CN103896281 A CN 103896281A CN 201410155447 A CN201410155447 A CN 201410155447A CN 103896281 A CN103896281 A CN 103896281A
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Abstract
The invention discloses a method for rectifying and purifying silicon tetrachloride by complete thermal coupling, which comprises the following steps: (1) crude silicon tetrachloride enters a light component removal tower, a produced gas phase enters a condenser, the condensed liquid phase partially flows back and is partially produced, the produced liquid is light component impurities, the crude silicon tetrachloride in the light component removal tower kettle partially enters a condensation reboiler of the light component removal tower kettle and is partially used as a discharged material, and the discharged material enters a heavy component removal tower; and (2) an overhead gas phase of the heavy component removal tower is produced as a heat source and enters the condensation reboiler of the light component removal tower kettle, the backflow is regulated so that the condensation heat is equal to heat required by the light component removal tower kettle, the gas phase subjected to heat exchange is completely condensed into a liquid phase, and the liquid phase is partially discharged as the silicon tetrachloride product and partially flows back to the heavy component removal tower. The method adopts continuous operation, and is suitable for large-scale industrial production; after the light component impurities are removed by the light component removal tower and the heavy component impurities are removed by the heavy component removal tower, the purity of the product silicon tetrachloride can reach 99.9999%; and the process is convenient to operate and easy to implement.
Description
Technical field
The invention belongs to distillation technology field, be specifically related to a kind of method of complete thermal coupling rectification and purification silicon tetrachloride.
Background technology
Silicon tetrachloride is a kind of important industrial chemicals, be mainly used in synthesizing organo-silicon compound, inorganic silicon compound and produce pure silicon etc. for the preparation of silicoorganic compound and war smoke screen, produce organosilicon, silicic acid acid esters, organic silicone oil, high-temperature insulation, silicone resin, silicon rubber etc. and synthesizing organo-silicon compound, silicon monomer, silicone oil, silicon rubber and silicone resin.Thick silicon tetrachloride mainly by ferrosilicon with chlorine reaction through distillation and or polysilicon by-product separate and obtain.Therefore, in thick silicon tetrachloride, contain trichlorosilane, high boiling point metal chloride and nonmetal muriate.Because the silicon tetrachloride of low-purity limits its application at industry-by-industry.So the separating-purifying of thick silicon tetrachloride has great significance.
Existing silicon tetrachloride method of purification has absorption method, reaction method and rectification method.
Absorption method is to utilize in mixture the different processes that make each component separation of bonding force between each component and sorbent material, absorption method is general only effective to one or a class impurity removal, but bad to other impurity removal effects, this has limited the application of absorption method in silicon tetrachloride is purified.
Reaction method is to utilize to add some component reaction in a kind of component and mixture, after reaction, each component is easy to separate and reaches the method for separating effect, general and the additive method coupling energy of reaction method is to the separating effect having added, but cost is higher, and this has limited the application of reaction method.
Rectification method is the difference of utilizing each component volatilization degree by the part method that partial condensation separates each component of vaporizing, and conventional rectifying thermodynamic(al) efficiency is low, energy consumption is large, is unfavorable for reducing production costs.
The energy consumption of purification process directly affects its application in silicon tetrachloride purification field, therefore, finds a kind of purifying technique of energy-efficient silicon tetrachloride to have great significance to silicon tetrachloride production industry; Provide more wide use range to byproduct in polysilicon production process simultaneously, be conducive to reduce production of polysilicon cost.
Summary of the invention
In order to solve the problems of the prior art, the invention provides a kind of method of complete thermal coupling rectification and purification silicon tetrachloride, in solution prior art, rectifying thermodynamic(al) efficiency is low, energy consumption is large, the problem that production cost is high.
Technical scheme of the present invention is:
A method for complete thermal coupling rectification and purification silicon tetrachloride, comprises the following steps:
(1) the thick silicon tetrachloride of FEOL enters lightness-removing column, described lightness-removing column overhead extraction gas phase enters lightness-removing column overhead condenser, described lightness-removing column overhead condenser is complete condenser, the liquid phase part obtaining through complete condenser condensation refluxes, part extraction, extraction liquid phase is light constituent impurity, the thick silicon tetrachloride part in lightness-removing column tower reactor enters lightness-removing column tower reactor condensation reboiler, part is as discharging, and discharging enters weight-removing column;
(2) extraction of weight-removing column top gaseous phase is as thermal source, enter lightness-removing column tower reactor condensation reboiler, refluxed and made its condenser heat equal lightness-removing column tower reactor institute heat requirement by adjustment, the gas phase after heat exchange is all condensed into liquid phase, part is with product silicon tetrachloride product discharge, and part refluxes as weight-removing column; Weight-removing column tower reactor material part enters weight-removing column reboiler, part extraction, the extraction composition impurity of attaching most importance to.
Described lightness-removing column tower top pressure is normal pressure.
Described weight-removing column tower top pressure is 300～500kPa.
Described lightness-removing column tower reactor temperature is lower than weight-removing column top gaseous phase drop temperature more than 15 ℃; As preferably, lightness-removing column tower reactor temperature is lower than 20 ℃ of weight-removing column top gaseous phase drop temperatures.
The invention has the beneficial effects as follows: adopt operate continuously, be applicable to large-scale commercial production; Remove light constituent impurity by lightness-removing column, remove heavy constituent impurity by weight-removing column after product silicon tetrachloride purity can arrive 99.9999%, flow operations is convenient, be easy to realize; By the reboiler of weight-removing column top gaseous phase heating lightness-removing column, realize the second stage employ of energy, can energy efficient 40% to 50%, also save the consumption of recirculated water simultaneously.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the method for complete thermal coupling rectification and purification silicon tetrachloride.
Embodiment
Below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described further:
The method of of the present invention complete thermal coupling rectification and purification silicon tetrachloride as shown in Figure 1, it comprises the following steps: the thick silicon tetrachloride of (1) FEOL enters lightness-removing column 1, described lightness-removing column 1 overhead extraction gas phase enters lightness-removing column overhead condenser 3, described lightness-removing column overhead condenser 3 is complete condenser, the liquid phase part obtaining through complete condenser condensation refluxes, part extraction, extraction liquid phase is light constituent impurity, thick silicon tetrachloride part in lightness-removing column 1 tower reactor enters lightness-removing column tower reactor condensation reboiler 4, part is as discharging, and discharging enters weight-removing column 2; (2) weight-removing column 2 top gaseous phase extraction are as thermal source, enter lightness-removing column tower reactor condensation reboiler 4, reflux and make its condenser heat equal lightness-removing column tower reactor institute heat requirement by adjustment, gas phase after heat exchange is all condensed into liquid phase, part is with product silicon tetrachloride product discharge, and part refluxes as weight-removing column 2; Weight-removing column 2 tower reactor material parts enter weight-removing column reboiler 5, part extraction, the extraction composition impurity of attaching most importance to.
Preferred described lightness-removing column tower top pressure is normal pressure;
Preferred described weight-removing column tower top pressure is 300～500kPa;
Preferred described lightness-removing column tower reactor temperature more than 15 ℃, take 20 ℃ as good, is beneficial to conduct heat lower than weight-removing column top gaseous phase drop temperature.
Embodiment 1
(1) the thick silicon tetrachloride of FEOL enters lightness-removing column, described lightness-removing column overhead extraction gas phase enters lightness-removing column overhead condenser, described lightness-removing column overhead condenser is complete condenser, the liquid phase part obtaining through complete condenser condensation refluxes, part extraction, extraction liquid phase is light constituent impurity, the thick silicon tetrachloride part in lightness-removing column tower reactor enters lightness-removing column tower reactor condensation reboiler, part is as discharging, and discharging enters weight-removing column; Lightness-removing column tower top pressure is normal pressure; (2) extraction of weight-removing column top gaseous phase is as thermal source, enter lightness-removing column tower reactor condensation reboiler, refluxed and made its condenser heat equal lightness-removing column tower reactor institute heat requirement by adjustment, the gas phase after heat exchange is all condensed into liquid phase, part is with product silicon tetrachloride product discharge, and part refluxes as weight-removing column; Weight-removing column tower reactor material part enters weight-removing column reboiler, part extraction, the extraction composition impurity of attaching most importance to; Weight-removing column tower top pressure 300kPa.
Described lightness-removing column tower reactor temperature is lower than 15 ℃ of weight-removing column top gaseous phase drop temperatures.
Can reach energy-conservation 45% by complete thermal coupling.
(1) the thick silicon tetrachloride of FEOL enters lightness-removing column, described lightness-removing column overhead extraction gas phase enters lightness-removing column overhead condenser, described lightness-removing column overhead condenser is complete condenser, the liquid phase part obtaining through complete condenser condensation refluxes, part extraction, extraction liquid phase is light constituent impurity, the thick silicon tetrachloride part in lightness-removing column tower reactor enters lightness-removing column tower reactor condensation reboiler, part is as discharging, and discharging enters weight-removing column; Lightness-removing column tower top pressure is normal pressure; (2) extraction of weight-removing column top gaseous phase is as thermal source, enter lightness-removing column tower reactor condensation reboiler, refluxed and made its condenser heat equal lightness-removing column tower reactor institute heat requirement by adjustment, the gas phase after heat exchange is all condensed into liquid phase, part is with product silicon tetrachloride product discharge, and part refluxes as weight-removing column; Weight-removing column tower reactor material part enters weight-removing column reboiler, part extraction, the extraction composition impurity of attaching most importance to; Weight-removing column tower top pressure 400kPa.
Described lightness-removing column tower reactor temperature is lower than 17 ℃ of weight-removing column top gaseous phase drop temperatures.
Can reach energy-conservation 44.5% by complete thermal coupling.
(1) the thick silicon tetrachloride of FEOL enters lightness-removing column, described lightness-removing column overhead extraction gas phase enters lightness-removing column overhead condenser, described lightness-removing column overhead condenser is complete condenser, the liquid phase part obtaining through complete condenser condensation refluxes, part extraction, extraction liquid phase is light constituent impurity, the thick silicon tetrachloride part in lightness-removing column tower reactor enters lightness-removing column tower reactor condensation reboiler, part is as discharging, and discharging enters weight-removing column; Lightness-removing column tower top pressure is normal pressure; (2) extraction of weight-removing column top gaseous phase is as thermal source, enter lightness-removing column tower reactor condensation reboiler, refluxed and made its condenser heat equal lightness-removing column tower reactor institute heat requirement by adjustment, the gas phase after heat exchange is all condensed into liquid phase, part is with product silicon tetrachloride product discharge, and part refluxes as weight-removing column; Weight-removing column tower reactor material part enters weight-removing column reboiler, part extraction, the extraction composition impurity of attaching most importance to; Weight-removing column tower top pressure 500kPa.
Described lightness-removing column tower reactor temperature is lower than 20 ℃ of weight-removing column top gaseous phase drop temperatures.
Can reach energy-conservation 44.2% by complete thermal coupling.
Claims (5)
1. a method for complete thermal coupling rectification and purification silicon tetrachloride, is characterized in that, comprises the following steps:
(1) the thick silicon tetrachloride of FEOL enters lightness-removing column, described lightness-removing column overhead extraction gas phase enters lightness-removing column overhead condenser, described lightness-removing column overhead condenser is complete condenser, the liquid phase part obtaining through complete condenser condensation refluxes, part extraction, extraction liquid phase is light constituent impurity, the thick silicon tetrachloride part in lightness-removing column tower reactor enters lightness-removing column tower reactor condensation reboiler, part is as discharging, and discharging enters weight-removing column;
(2) extraction of weight-removing column top gaseous phase is as thermal source, enter lightness-removing column tower reactor condensation reboiler, refluxed and made its condenser heat equal lightness-removing column tower reactor institute heat requirement by adjustment, the gas phase after heat exchange is all condensed into liquid phase, part is with product silicon tetrachloride product discharge, and part refluxes as weight-removing column; Weight-removing column tower reactor material part enters weight-removing column reboiler, part extraction, the extraction composition impurity of attaching most importance to.
2. the complete method of thermal coupling rectification and purification silicon tetrachloride according to claim 1, is characterized in that, described lightness-removing column tower top pressure is normal pressure.
3. the complete method of thermal coupling rectification and purification silicon tetrachloride according to claim 1, is characterized in that, described weight-removing column tower top pressure is 300～500kPa.
4. the complete method of thermal coupling rectification and purification silicon tetrachloride according to claim 1, is characterized in that, described lightness-removing column tower reactor temperature is lower than weight-removing column top gaseous phase drop temperature more than 15 ℃.
5. the complete method of thermal coupling rectification and purification silicon tetrachloride according to claim 4, is characterized in that, described lightness-removing column tower reactor temperature is lower than 20 ℃ of weight-removing column top gaseous phase drop temperatures.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693754A (en) * | 2016-04-08 | 2016-06-22 | 天津市华瑞奕博化工科技有限公司 | Organosilicone high-boiling-component removing and low-boiling-component removing tower pressure-variable thermal coupling distillation method and equipment |
| WO2018006695A1 (en) * | 2016-07-06 | 2018-01-11 | 成都蜀菱科技发展有限公司 | High purity silicon tetrachloride purification method |
| CN107648976A (en) * | 2017-09-22 | 2018-02-02 | 杭州杭氧股份有限公司 | A kind of cryogenic separation produces the method and cryogenic separation system of ultra-pure gases |
| CN108434766A (en) * | 2018-04-03 | 2018-08-24 | 烟台国邦化工机械科技有限公司 | A kind of high-melting-point object system's recovery system and process |
| CN109704345A (en) * | 2019-02-21 | 2019-05-03 | 浙江中宁硅业有限公司 | A kind of ocratation rectifier unit and its production method |
| CN114681942A (en) * | 2020-12-28 | 2022-07-01 | 天津市华瑞奕博化工科技有限公司 | Tert-butyl alcohol recovery complete variable-voltage coupling rectification device and rectification method |
| CN114906852A (en) * | 2022-06-15 | 2022-08-16 | 北京化工大学 | Method for producing high-purity silicon tetrachloride by combination of adsorption, rectification and photoreaction |
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| CN101920964A (en) * | 2010-09-11 | 2010-12-22 | 天津大学 | Method for purifying silicon tetrachloride by double-effect distillation |
| CN102807222A (en) * | 2012-08-17 | 2012-12-05 | 中国天辰工程有限公司 | Purification method of silicon tetrachloride |
| CN102923714A (en) * | 2012-11-05 | 2013-02-13 | 天津大学 | Next-door thermal coupling distillation method and equipment for producing polycrystalline silicon |
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Patent Citations (3)
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| CN101920964A (en) * | 2010-09-11 | 2010-12-22 | 天津大学 | Method for purifying silicon tetrachloride by double-effect distillation |
| CN102807222A (en) * | 2012-08-17 | 2012-12-05 | 中国天辰工程有限公司 | Purification method of silicon tetrachloride |
| CN102923714A (en) * | 2012-11-05 | 2013-02-13 | 天津大学 | Next-door thermal coupling distillation method and equipment for producing polycrystalline silicon |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105693754A (en) * | 2016-04-08 | 2016-06-22 | 天津市华瑞奕博化工科技有限公司 | Organosilicone high-boiling-component removing and low-boiling-component removing tower pressure-variable thermal coupling distillation method and equipment |
| WO2018006695A1 (en) * | 2016-07-06 | 2018-01-11 | 成都蜀菱科技发展有限公司 | High purity silicon tetrachloride purification method |
| CN107648976A (en) * | 2017-09-22 | 2018-02-02 | 杭州杭氧股份有限公司 | A kind of cryogenic separation produces the method and cryogenic separation system of ultra-pure gases |
| CN107648976B (en) * | 2017-09-22 | 2020-10-09 | 衢州杭氧气体有限公司 | Method for preparing ultra-high-purity gas through low-temperature separation and low-temperature separation system |
| CN108434766A (en) * | 2018-04-03 | 2018-08-24 | 烟台国邦化工机械科技有限公司 | A kind of high-melting-point object system's recovery system and process |
| CN109704345A (en) * | 2019-02-21 | 2019-05-03 | 浙江中宁硅业有限公司 | A kind of ocratation rectifier unit and its production method |
| CN114681942A (en) * | 2020-12-28 | 2022-07-01 | 天津市华瑞奕博化工科技有限公司 | Tert-butyl alcohol recovery complete variable-voltage coupling rectification device and rectification method |
| CN114681942B (en) * | 2020-12-28 | 2023-07-07 | 天津市华瑞奕博化工科技有限公司 | Complete pressure swing coupling rectification device and rectification method for tertiary butanol recovery |
| CN114906852A (en) * | 2022-06-15 | 2022-08-16 | 北京化工大学 | Method for producing high-purity silicon tetrachloride by combination of adsorption, rectification and photoreaction |
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Application publication date: 20140702 |