CN104524904A - Method for filtering tail gas impurities in polycrystalline silicon production process - Google Patents

Method for filtering tail gas impurities in polycrystalline silicon production process Download PDF

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Publication number
CN104524904A
CN104524904A CN201410856902.5A CN201410856902A CN104524904A CN 104524904 A CN104524904 A CN 104524904A CN 201410856902 A CN201410856902 A CN 201410856902A CN 104524904 A CN104524904 A CN 104524904A
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CN
China
Prior art keywords
tail gas
membrane separator
tower
membrane
filter
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410856902.5A
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Chinese (zh)
Inventor
石程亮
姜海明
李辉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
INNER MONGOLIA SHENZHOU SILICON INDUSTRY Co Ltd
Original Assignee
INNER MONGOLIA SHENZHOU SILICON INDUSTRY Co Ltd
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Application filed by INNER MONGOLIA SHENZHOU SILICON INDUSTRY Co Ltd filed Critical INNER MONGOLIA SHENZHOU SILICON INDUSTRY Co Ltd
Priority to CN201410856902.5A priority Critical patent/CN104524904A/en
Publication of CN104524904A publication Critical patent/CN104524904A/en
Pending legal-status Critical Current

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/229—Integrated processes (Diffusion and at least one other process, e.g. adsorption, absorption)
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/40—Processes or apparatus using other separation and/or other processing means using hybrid system, i.e. combining cryogenic and non-cryogenic separation techniques
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/50—Processes or apparatus using other separation and/or other processing means using absorption, i.e. with selective solvents or lean oil, heavier CnHm and including generally a regeneration step for the solvent or lean oil
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

The invention discloses a method for filtering tail gas impurities in the polycrystalline silicon production process. A copious cooling process is used for optimizing and adjusting and mainly comprises the steps that low-temperature liquid form chlorosilane is in reverse contact with tail gas and safe discharge gas which are mixed from bottom to top at the bottom of a tower in a bubbling spraying mode, chlorosilane materials in the tail gas are liquefied and recovered, and uncondensed non-condensable gases come out from the top of the bubbling spraying tower to enter in a downstream procedure to be processed. The application of a membrane separation technology mainly relates to the filtering through a built-in filter element of a membrane separator, clear liquid comes out from a top outlet of the membrane separator through the filter element to enter in a downstream rectification process, and solid particles larger than 1 micron are filtered by the filter element. The method has the advantages that the structure is simple, the performance is stable, and the performance for impurity filtering and removing is good.

Description

A kind of method of tail gas contaminant filter in polysilicon production process
Technical field
The present invention relates to production of polysilicon technology, refer in particular to the method for tail gas contaminant filter in a kind of polysilicon production process.
Background technology
In polysilicon production process, according to the different physicochemical characteristics of each material, in specific equipment, control certain temperature, pressure, realizing the purifying of various material, recovery, be separated, recycle being indispensable important step, is also the guarantee of polysilicon product quality and production cost, scale, due to its successful technology, adopted by internationally famous polysilicon producer, and be confirmed.
In recent years, the tail gas impurity faced below along with expansion scale gradually in polysilicon industry, needed to strengthen removing tail gas contaminant filter, to guarantee the stable operation such as subsequent handling and dynamic equipment.Based on above background, design tail gas contaminant filter minimizing technology in a kind of polysilicon production process, in polysilicon industry, the tail gas impurity that expansion scale is faced below adds strong filter removal dynamics and plant running stability has important function.
Summary of the invention
The technical problem to be solved in the present invention is to provide the method for tail gas contaminant filter in a kind of polysilicon production process, this method is optimized and revised and application of membrane separation technology by cryogenic technology, strengthen and tail gas contaminant filter is removed, guarantee the stable operation such as subsequent handling and dynamic equipment.
For solving the problems of the technologies described above, the present invention proposes following scheme: the method designed by the present invention is optimized and revised by cryogenic technology and formed with application of membrane separation technology two parts.1. cryogenic technology is optimized and revised, and tail gas is through low temperature chlorosilane bubbling spray, and wherein most of chlorosilane is got off by cold pouring.Then gaseous mixture is by after compressor compresses to certain pressure, then carries out cryogenic condensation; 2. application of membrane separation technology take micropore filter element as filter element, and stainless steel is the closed precise filtering device that filter shell (particular application can select titanium shell or inner liner rubber, lining tetrafluoro etc.) combines.Thus by solid-liquid separation method, can by disposable for the particle of more than 1 μm filtering, and stability is high, without adsorbing loss problem, original composition of not modified filter medium.
Specific embodiment is as follows: in a kind of polysilicon production process tail gas contaminant filter method, optimized and revised and application of membrane separation technology by cryogenic technology, to tail gas contaminant filter remove, guarantee the stable operation such as subsequent handling and dynamic equipment.Enter bottom bubbling spray tower after the mixing of the tail gas discharged in polysilicon production process, safety relief gas, in tower, temperature is≤-40--33 DEG C, pressure is under the environment of 50-80KPaG, from the low temperature liquid chlorosilane under top spray, mixed tail gas, safety relief gas carry out reverse contact from below to up with tower bottom, chlorosilane material liquefaction in tail gas is reclaimed, the on-condensible gas (H be not condensed 2, nitrogen etc.) out enter lower procedure process from bubbling spray tower top, liquid chlorosilane at the bottom of tower divides two-way to carry by reflux pump, and a road supplies bubbling spray tower spray-absorption tail gas after delivering to freon cooler cooling again, another route delivery pump enters the membrane separator in downstream, by the filtration of the built-in filter core of membrane separator, clear liquid out enters downstream rectification working process by filter core from the top exit of membrane separator, the solid particle being greater than 1 μm is got off by described filter element filtering, when membrane separator inlet and outlet pressure difference is greater than the regulation process parameter value of 100KPaG, backwash is carried out in stopper film filter operation, first the solid particle being deposited on membrane separator bottom is drained into raffinate treating column alkali lye by outlet at bottom to process, then nitrogen or clear liquid is used to enter membrane separator from UF membrane top material mouth, the solid particle be attached on UF membrane wall is rinsed well, counter-flushing liquid enters raffinate storage tank, the filter operation of condensate liquid is carried out again after backwash is qualified.
Advantage of the present invention is: this method and apparatus structure are simple, stable performance, that contaminant filter removes performance is good.By solid-liquid separation method, can by disposable for the particle of more than 1 μm filtering, and stability is high, and without absorption loss problem, original composition of not modified filter medium.There is good effect in actual use.
Accompanying drawing explanation
Fig. 1 is flow process simplified schematic diagram of the present invention.
Fig. 2 is the schematic diagram that cryogenic technology optimizes bubbling spray.
Fig. 3 is the schematic diagram of application of membrane separation technology.
Detailed description of the invention
The following detailed description of the invention illustrating tail gas contaminant filter minimizing technology in the present invention and a kind of polysilicon production process according to example, but any restriction is not produced to the present invention.
Schematic flow sheet as shown in Figure 1, is optimized and revised and application of membrane separation technology by cryogenic technology, removes, guarantee the stable operation such as subsequent handling and dynamic equipment to tail gas contaminant filter.
As shown in Figure 2, enter bottom bubbling spray tower after the mixing of the tail gas discharged in polysilicon production process, safety relief gas, in tower, temperature is-33 DEG C, pressure is under the environment of 50KPaG, from the low temperature liquid chlorosilane under top spray, mixed tail gas, safety relief gas carry out reverse contact from below to up with tower bottom, chlorosilane material liquefaction in tail gas is reclaimed, the on-condensible gas (H be not condensed 2, nitrogen etc.) out enter lower procedure process from bubbling spray tower top, liquid chlorosilane at the bottom of tower divides two-way to carry by reflux pump, and a road supplies bubbling spray tower spray-absorption tail gas after delivering to freon cooler cooling again; Another route delivery pump enters the membrane separator in downstream.
As shown in Figure 3, by the filtration of the built-in filter core of membrane separator, clear liquid out enters downstream rectification working process by filter core from the top exit of membrane separator, the solid particle being greater than 1 μm is got off by described filter element filtering, when membrane separator inlet and outlet pressure difference is greater than the regulation process parameter value of 100KPaG, backwash is carried out in stopper film filter operation, first the solid particle being deposited on membrane separator bottom is drained into raffinate treating column alkali lye by outlet at bottom to process, then nitrogen or clear liquid is used to enter membrane separator from UF membrane top material mouth, the solid particle be attached on UF membrane wall is rinsed well, counter-flushing liquid enters raffinate storage tank, the filter operation of condensate liquid is carried out again after backwash is qualified.

Claims (1)

1. in a polysilicon production process tail gas contaminant filter method, optimized and revised and application of membrane separation technology by cryogenic technology, tail gas contaminant filter is removed, guarantee the stable operation such as subsequent handling and dynamic equipment, it is characterized in that: the tail gas discharged in polysilicon production process, enter bottom bubbling spray tower after the mixing of safety relief gas, in tower, temperature is≤-40--33 DEG C, pressure is under the environment of 50-80KPaG, from the low temperature liquid chlorosilane under top spray and tower bottom mixed tail gas from below to up, safety relief gas carries out reverse contact, chlorosilane material liquefaction in tail gas is reclaimed, on-condensible gas (the H be not condensed 2, nitrogen etc.) out enter lower procedure process from bubbling spray tower top, liquid chlorosilane at the bottom of tower divides two-way to carry by reflux pump, and a road supplies bubbling spray tower spray-absorption tail gas after delivering to freon cooler cooling again, another route delivery pump enters the membrane separator in downstream, by the filtration of the built-in filter core of membrane separator, clear liquid out enters downstream rectification working process by filter core from the top exit of membrane separator, the solid particle being greater than 1 μm is got off by described filter element filtering, when membrane separator inlet and outlet pressure difference is greater than the regulation process parameter value of 100KPaG, backwash is carried out in stopper film filter operation, first the solid particle being deposited on membrane separator bottom is drained into raffinate treating column alkali lye by outlet at bottom to process, then nitrogen or clear liquid is used to enter membrane separator from UF membrane top material mouth, the solid particle be attached on UF membrane wall is rinsed well, counter-flushing liquid enters raffinate storage tank, the filter operation of condensate liquid is carried out again after backwash is qualified.
CN201410856902.5A 2014-12-31 2014-12-31 Method for filtering tail gas impurities in polycrystalline silicon production process Pending CN104524904A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410856902.5A CN104524904A (en) 2014-12-31 2014-12-31 Method for filtering tail gas impurities in polycrystalline silicon production process

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Application Number Priority Date Filing Date Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107758673A (en) * 2017-11-03 2018-03-06 洛阳中硅高科技有限公司 Chlorosilane Recovery Purifying device and method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010184831A (en) * 2009-02-12 2010-08-26 Osaka Titanium Technologies Co Ltd Method for producing high purity polycrystalline silicon
CN202297154U (en) * 2011-10-14 2012-07-04 唐山三孚硅业股份有限公司 Wet process dust removal device in trichlorosilane production
CN202924720U (en) * 2012-08-10 2013-05-08 中国恩菲工程技术有限公司 Dry-process recovery system for reduction exhaust produced in polycrystalline silicone production technology
CN103331057A (en) * 2013-07-19 2013-10-02 新特能源股份有限公司 Filtering device for silica powder in liquid chlorosilane

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2010184831A (en) * 2009-02-12 2010-08-26 Osaka Titanium Technologies Co Ltd Method for producing high purity polycrystalline silicon
CN202297154U (en) * 2011-10-14 2012-07-04 唐山三孚硅业股份有限公司 Wet process dust removal device in trichlorosilane production
CN202924720U (en) * 2012-08-10 2013-05-08 中国恩菲工程技术有限公司 Dry-process recovery system for reduction exhaust produced in polycrystalline silicone production technology
CN103331057A (en) * 2013-07-19 2013-10-02 新特能源股份有限公司 Filtering device for silica powder in liquid chlorosilane

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张雪华: "多晶硅生产尾气的回收再利用工艺概述", 《科技经济市场》, no. 10, 31 October 2012 (2012-10-31), pages 18 - 19 *
杨涛: "改良西门子法生产多晶硅工艺涉及探讨", 《贵州化工》, vol. 34, no. 3, 30 June 2009 (2009-06-30), pages 7 - 11 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107758673A (en) * 2017-11-03 2018-03-06 洛阳中硅高科技有限公司 Chlorosilane Recovery Purifying device and method
CN107758673B (en) * 2017-11-03 2024-01-12 洛阳中硅高科技有限公司 Chlorosilane purifying and recycling equipment and method

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Application publication date: 20150422