CN105597462A - Treatment process for dust-containing tail gas in synthesis and emptying of methyl chlorosilane - Google Patents

Treatment process for dust-containing tail gas in synthesis and emptying of methyl chlorosilane Download PDF

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Publication number
CN105597462A
CN105597462A CN201610148267.4A CN201610148267A CN105597462A CN 105597462 A CN105597462 A CN 105597462A CN 201610148267 A CN201610148267 A CN 201610148267A CN 105597462 A CN105597462 A CN 105597462A
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China
Prior art keywords
dust
emptying
tail gas
sink
treatment process
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Pending
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CN201610148267.4A
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Chinese (zh)
Inventor
王英明
伊港
刘青海
周玲
张旭
朱永和
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SHANDONG DONGYUE SILICON MATERIAL CO Ltd
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SHANDONG DONGYUE SILICON MATERIAL CO Ltd
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Priority to CN201610148267.4A priority Critical patent/CN105597462A/en
Publication of CN105597462A publication Critical patent/CN105597462A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D47/00Separating dispersed particles from gases, air or vapours by liquid as separating agent
    • B01D47/02Separating dispersed particles from gases, air or vapours by liquid as separating agent by passing the gas or air or vapour over or through a liquid bath
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2247/00Details relating to the separation of dispersed particles from gases, air or vapours by liquid as separating agent
    • B01D2247/10Means for removing the washing fluid dispersed in the gas or vapours

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)

Abstract

The invention belongs to the technical field of tail-gas treatment and particularly relates to a treatment process for dust-containing tail gas in synthesis and emptying of methyl chlorosilane. The treatment process is characterized in that the dust-containing tail gas passing through a discharging hopper enters a washing groove by a bottom inserting pipe, and chlorosilane is filled into the washing groove; a stirring device is added in the washing groove to carry out treatment, and dust-containing chlorosilane is treated by using an N2 pulp-residue pressing-in device periodically; the tail gas dust-removed by the washing groove enters an emptying condenser, a condensate enters an emptying and condensate collecting groove, and noncondensable gas enters a water washing system for treatment; and nitrogen gas for liquid phase, which is collected in the emptying and condensate collecting groove is stamped and is periodically recovered into the system for use. The treatment process has the advantages that the emptying amount of dust and the chlorosilane and the like can be obviously reduced, the chlorosilane in the tail gas is recovered, the material consumption is reduced and the environmental-friendly effect and obvious economic benefit are achieved.

Description

The treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane
Technical field
The invention belongs to vent gas treatment technical field, be specifically related to the treatment process of the synthetic emptying dust-containing tail gas of a kind of methylchlorosilane.
Background technology
In methylchlorosilane synthesis procedure, chlorosilane reacts under catalyst action with silica flour in fluid bed, synthesizesMethylchlorosilane after dedusting rectifying, obtain the dimethyldichlorosilane that purity is higher, in order to improve the utilization rate of raw material, each factoryThe unreacted that business often collects part dust arrester contact pressurization is completely sent into fluid bed and is re-started reaction, after conveying,The pressure release of hopper device is again carried out collection preparation pressure release gas and (is comprised N2, chlorosilane gas etc.) to carry a small amount of high-temperature dust secretly (thinSilica flour and waste catalyst etc.) form and synthesize dust-containing tail gas.
High-temperature dust is first collected by resistant to elevated temperatures sack cleaner by it by most domestic manufacturer, then removes acid chlorine through water scrubberEmptying after silane gas and the dust do not collected by sack cleaner. In this technique, because tail gas emptying amount is large, short temperature of timeSpend highly, and carry dust secretly, (dust forms flocculent deposit in water, easily causes washing circulation easily to cause washing effect extreme differencePump breaks down), do not caused serious environmental pollution by the chlorosilane monomer emptying meeting of water absorption reaction, most manufacturers is letter justSingle increases water scrubber, strengthen, although obtain certain effect, reaches far away the degree of radical cure, and indivedual manufacturers are by dwindlingDeduster gathering-device volume or reduce the temporal frequency of fluid bed of pressurizeing back, reduces such tail gas emptying amount as far as possible, therebyReduce and administer pressure, but effect improved not very desirable.
Summary of the invention
The object of this invention is to provide the treatment process of the synthetic emptying dust-containing tail gas of a kind of methylchlorosilane, can obviously reduce dust,The emptying amount of chlorosilane etc., reclaims chlorosilane in tail gas, reduces supplies consumption, and environmental protection, economic benefit are obvious.
The treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane of the present invention, step is as follows:
(1) enter sink through the dust-containing tail gas of hopper by bottom insert canal, in sink, be filled with chlorosilane; In sink, addDress stirs and processes, and the chlorosilane that contains dust is regularly used to N2Be pressed into the processing of screenings system;
(2) enter blowdown condenser through the tail gas of sink dedusting, condensate liquid enters emptying condensate storage, and fixed gas entersEnter water wash system processing;
(3) the liquid phase nitrogen punching press of collecting in emptying condensate storage is regularly recovered in system and uses.
In sink described in step (1), washing liquid phase is the chlorosilane that boiling point is greater than 70 DEG C.
Sink liquid level control 40-60% described in step (1).
In sink described in step (1), be provided with bottom insert canal.
Described bottom insert canal, apart from sink bottom 20-30cm, is cleared up bottom insert canal when easy access timely.
Speed of agitator described in step (1) is 60r/min, stirs and adopts three oblique leaf turbine impellers.
Sink described in step (1), by opening up valve control in two formulas, is regularly pressed into the processing of screenings system by nitrogen.
In step (1), in sink, be preferably filled with 50% left and right chlorosilane.
Blowdown condenser described in step (2) is vertical structure; For preventing that high gas speed is to pipe wear, import department is provided with gearPlate.
Blowdown condenser described in step (2) carries out condensation with recirculated water, and its blanking temperature control is not higher than 45 DEG C.
The treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane of the present invention, concrete steps are as follows:
(1) tail gas enters sink by bottom insert canal, in sink, through the washing of liquid phase higher boiling chlorosilane, removes gasIn the dust carried secretly, washed lower dust and enter into sink and mix with higher boiling chlorosilane, sink increases stirring and prevents powderDirt precipitation, knot wall, sink top is provided with radar level gauge, for the accumulation that reduces dust will contain according to level condition in grooveThe chlorosilane of dust is regularly drained in screenings system and goes by opening up valve on root;
(2) be washed dropping a hint of dedusting and enter into blowdown condenser, blowdown condenser is cooled with circulating water, and controls its blankingTemperature is not higher than 45 DEG C, and the liquid phase under condensation enters emptying condensate storage, and fixed gas enters water system system;
(3) liquid phase under condensation enters emptying condensate storage, controls the liquid level of emptying condensate storage, according to on-the-spot liquidPosition meter shows emptying condensate storage level condition, and the liquid phase of collection regularly reclaims by retrieval system in nitrogen ramming system.
Emptying gas of the present invention enters sink by bottom insert canal, and sink tapering is connected with flash tank, further reclaims; TopGas vent is connected with blowdown condenser by pipeline, and blowdown condenser inner tip is provided with protective baffle plate, blowdown condenser taperingBe connected with emptying condensate storage by pipeline, feeder overhead line is connected with water wash system, and top is provided with pressurising dress in additionPut, feeder bottom and the height liquid bath that boils is connected, regularly reclaims collection liquid.
The present invention compared with prior art, has following beneficial effect:
Existing technique is that water wash system is directly removed in hopper emptying after bag-type dust, and it is bad that one side is washed effect, the opposing partyFace has caused chlorosilane emptying, causes the waste of material, has increased the burden of water wash system. Dust of the present invention can be by washingGroove is effectively removed, and the chlorosilane that sink contains dust can turn back to recovery again in system, reclaims through condenserChlorosilane is regularly collected retrieval system, has saved production cost, and water wash system chlorosilane content reduces greatly simultaneously, environmental benefitObviously.
Brief description of the drawings
Fig. 1 is the structural representation of present device;
In figure: 1, sink; 2, blowdown condenser; 3, emptying condensate storage; 4, sink nitrogen air inlet; 5,The import of sink gas phase; 6, sink gas outlet; 7, sink material receiving port; 8, on sink, open up valve; 9, bottom insert canal; 10,Agitating device; 11, blowdown condenser gas phase import; 12, blowdown condenser liquid-phase outlet; 13, emptying condensate storage nitrogenGas air inlet; 14, fixed gas outlet; 15, emptying condensate storage liquid-phase outlet; 16, liquid level gauge; 17, emptying is cut offValve; 18, baffle plate.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Drop a hint by the import of sink gas phase by bottom insert canal from the dust-laden of hopper, control bottom insert canal and enter apart from bottom 20cmEntering sink, is higher boiling chlorosilane (boiling point is greater than 70 DEG C) control sink liquid level 40%, powder after washing in sinkDirt enters in higher boiling chlorine silicon solution, and sink is installed and stirred, control mixing speed and be 60r/min device prevent dust accumulation,Knot wall is opened and on sink, is opened up valve and be pressed into screenings system to 0.6mpa to sink punching press in the time that liquid level is greater than 65% in sinkProcess. Dust-containing tail gas through washing enters into blowdown condenser by sink gas outlet, and condenser carries out cold with recirculated waterBut, control 40 DEG C of condensate temperatures, the liquid phase under condensation enters into emptying condensate storage by blowdown condenser liquid-phase outletIn, the liquid phase of collection by liquid level gauge observe reach more than 50% by after the punching press of 0.6mpa nitrogen by emptying condensed fluid collection tank liquorExport in ramming system and reclaim mutually, fixed gas is exported and is entered into water scrubber and further process by fixed gas.
Embodiment 2
Drop a hint by the import of sink gas phase by bottom insert canal from the dust-laden of hopper, control bottom insert canal and enter apart from bottom 30cmEntering sink, is higher boiling chlorosilane (boiling point is greater than 70 DEG C) control sink liquid level 50%, powder after washing in sinkDirt enters in higher boiling chlorine silicon solution, and sink is installed and stirred, control mixing speed and be 60r/min device prevent dust accumulation,Knot wall is opened and on sink, is opened up valve and be pressed into screenings system to 0.6mpa to sink punching press in the time that liquid level is greater than 65% in sinkProcess. Dust-containing tail gas through washing enters into blowdown condenser by sink gas outlet, and condenser carries out cold with recirculated waterBut, control 45 DEG C of condensate temperatures, the liquid phase under condensation enters into emptying condensate storage by blowdown condenser liquid-phase outletIn, the liquid phase of collection by liquid level gauge observe reach more than 60% by after the punching press of 0.6mpa nitrogen by emptying condensed fluid collection tank liquorExport in ramming system and reclaim mutually, fixed gas is exported and is entered into water scrubber and further process by fixed gas.
Embodiment 3
Drop a hint by the import of sink gas phase by bottom insert canal from the dust-laden of hopper, control bottom insert canal and enter apart from bottom 25cmEntering sink, is higher boiling chlorosilane (boiling point is greater than 70 DEG C) control sink liquid level 60%, powder after washing in sinkDirt enters in higher boiling chlorine silicon solution, and sink is installed and stirred, control mixing speed and be 60r/min device prevent dust accumulation,Knot wall is opened and on sink, is opened up valve and be pressed into screenings system to 0.6mpa to sink punching press in the time that liquid level is greater than 65% in sinkProcess. Dust-containing tail gas through washing enters into blowdown condenser by sink gas outlet, and condenser carries out cold with recirculated waterBut, control 42 DEG C of condensate temperatures, the liquid phase under condensation enters into emptying condensate storage by blowdown condenser liquid-phase outletIn, the liquid phase of collection by liquid level gauge observe reach more than 55% by after the punching press of 0.6mpa nitrogen by emptying condensed fluid collection tank liquorExport in ramming system and reclaim mutually, fixed gas is exported and is entered into water scrubber and further process by fixed gas.

Claims (8)

1. a treatment process for the synthetic emptying dust-containing tail gas of methylchlorosilane, is characterized in that step is as follows:
(1) enter sink through the dust-containing tail gas of hopper by bottom insert canal, in sink, be filled with chlorosilane; In sink, addDress stirs and processes, and the chlorosilane that contains dust is regularly used to N2Be pressed into the processing of screenings system;
(2) enter blowdown condenser through the tail gas of sink dedusting, condensate liquid enters emptying condensate storage, and fixed gas entersEnter water wash system processing;
(3) the liquid phase nitrogen punching press of collecting in emptying condensate storage is regularly recovered in system and uses.
2. the treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane according to claim 1, is characterized in that step (1)Described in sink in washing liquid phase be the chlorosilane that boiling point is greater than 70 DEG C.
3. the treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane according to claim 1, is characterized in that step (1)Described in sink liquid level control 40-60%.
4. the treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane according to claim 1, is characterized in that step (1)Described in sink in be provided with bottom insert canal.
5. the treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane according to claim 4, described in it is characterized in thatBottom insert canal is apart from sink bottom 20-30cm.
6. the treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane according to claim 1, is characterized in that step (1)Described in speed of agitator be 60r/min, stir adopt three oblique leaf turbine impellers.
7. the treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane according to claim 1, is characterized in that step (2)Described in blowdown condenser be vertical structure, import department is provided with baffle plate.
8. the treatment process of the synthetic emptying dust-containing tail gas of methylchlorosilane according to claim 1, is characterized in that step (2)Described in blowdown condenser carry out condensation with recirculated water, its blanking temperature control is not higher than 45 DEG C.
CN201610148267.4A 2016-03-16 2016-03-16 Treatment process for dust-containing tail gas in synthesis and emptying of methyl chlorosilane Pending CN105597462A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105999891A (en) * 2016-07-05 2016-10-12 湖北兴发化工集团股份有限公司 Process and equipment for recycling organic silicone monomers and dust in vented tail gas
CN109107325A (en) * 2018-09-06 2019-01-01 合盛硅业股份有限公司 Methylchlorosilane emptying end gas recovery method and recyclable device
CN110215804A (en) * 2019-06-18 2019-09-10 南京宏匡硅材料有限公司 A kind of device for absorbing tail gas producing trim,ethylchlorosilane
CN111632469A (en) * 2020-05-09 2020-09-08 山东东岳有机硅材料股份有限公司 Dust-containing waste gas interception process and device in organic silicon monomer production
CN114247265A (en) * 2021-11-29 2022-03-29 鲁西化工集团股份有限公司硅化工分公司 System and method for purifying and recycling organic silicon emptying tail gas
CN114949905A (en) * 2022-06-17 2022-08-30 贵州天福化工有限责任公司 Device and method for recovering methanol in methanol rectification non-condensable gas

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105999891A (en) * 2016-07-05 2016-10-12 湖北兴发化工集团股份有限公司 Process and equipment for recycling organic silicone monomers and dust in vented tail gas
CN105999891B (en) * 2016-07-05 2018-06-26 湖北兴发化工集团股份有限公司 A kind of Processes and apparatus for recycling organic silicon monomer and the dust in emptying end gas
CN109107325A (en) * 2018-09-06 2019-01-01 合盛硅业股份有限公司 Methylchlorosilane emptying end gas recovery method and recyclable device
CN109107325B (en) * 2018-09-06 2021-08-27 合盛硅业股份有限公司 Methyl chlorosilane emptying tail gas recovery method and recovery device
CN110215804A (en) * 2019-06-18 2019-09-10 南京宏匡硅材料有限公司 A kind of device for absorbing tail gas producing trim,ethylchlorosilane
CN110215804B (en) * 2019-06-18 2024-06-18 南京宏匡硅材料有限公司 Tail gas absorbing device for producing trimethylchlorosilane
CN111632469A (en) * 2020-05-09 2020-09-08 山东东岳有机硅材料股份有限公司 Dust-containing waste gas interception process and device in organic silicon monomer production
CN114247265A (en) * 2021-11-29 2022-03-29 鲁西化工集团股份有限公司硅化工分公司 System and method for purifying and recycling organic silicon emptying tail gas
CN114247265B (en) * 2021-11-29 2024-05-24 鲁西化工集团股份有限公司硅化工分公司 Organic silicon emptying tail gas purifying and recycling treatment system and method
CN114949905A (en) * 2022-06-17 2022-08-30 贵州天福化工有限责任公司 Device and method for recovering methanol in methanol rectification non-condensable gas
CN114949905B (en) * 2022-06-17 2024-04-09 贵州天福化工有限责任公司 Device and method for recycling methanol in methanol rectification non-condensable gas

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