CN101829484B - Tail gas recovery method of carbon bisulfide refining system - Google Patents

Tail gas recovery method of carbon bisulfide refining system Download PDF

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Publication number
CN101829484B
CN101829484B CN 201010184438 CN201010184438A CN101829484B CN 101829484 B CN101829484 B CN 101829484B CN 201010184438 CN201010184438 CN 201010184438 CN 201010184438 A CN201010184438 A CN 201010184438A CN 101829484 B CN101829484 B CN 101829484B
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tail gas
sulfur
sulphur
molten sulfur
carbon
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CN101829484A (en
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郑道敏
余焮
冯海兵
刘希望
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NINGXIA ZIGUANG TIANHUA METHIONINE CO., LTD.
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Chongqing Unisplendour Chemical Co Ltd
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Abstract

The invention relates to a tail gas recovery method of a carbon bisulfide refining system, comprising the following steps of: regulating the pressure of tail gas in the carbon bisulfide refining system by an automatic-control pressure regulating valve; loading the tail gas into a Crouse system to recover sulfur, wherein the tail gas pressure is 0.027-0.045MPa (manometer pressure). With the tail gas recovery method, tail gas is sufficiently recovered and converted into sulfur, and environment pollution caused by discharging sulfur tail gas into air after the sulfur tail gas is burnt is avoided; meanwhile, the carbon bisulfide refining system adopts a sulfur separator with 7-8 column plates and a sulfur sealing height in a specific sulfur seal device, increases the separation effect of carbon bisulfide and molten sulfur, ensures that the molten sulfur recovered to a molten sulfur storage tank by the sulfur seal device almost contains no carbon bisulfide, and increases the technical safety.

Description

A kind of method of carbon bisulfide refining system tail gas recycle
Technical field
The present invention relates to a kind of method of tail gas recycle, be specifically related to a kind of method of carbon bisulfide refining system tail gas recycle.
Background technology
When being raw material production carbon disulfide with rudimentary hydro carbons such as molten sulfur and methane or the oil gas that contains saturated and/or unsaturated lower carbon number hydrocarbons, the gaseous state carbon disulfide that comes from heated reaction system is through condenser cooling becoming bullion CS 2Liquid gets into desulfurizing tower, rectifying column is made with extra care it then.Carbon disulfide is the good solvent of a kind of solubility property, such as patent CN02128149.1 description, the liquid CS that comes out from condenser 2, can be catching the small amount of sulfur that the carbon device comes and wash from catching sulphur, carbon disulfide also is dissolved with a small amount of hydrogen sulfide in addition, thus the liquid carbon disulphide that contains sulphur and hydrogen sulfide gets into rough system.Rough carbon disulfide liquid gets into the desulfurizing tower desulfuration purification that filler is housed; Carry out gas-liquid mass transfer with gas carbon disulfide from the tower still; Purer gas carbon disulfide gets into condenser condenses with the form of light component; Get into rectifying column rectifying then, the carbon disulfide product is by the into condenser cooling back discharging of coming out of tower still bottom; Lower from system's tail gas that condenser comes out owing to pressure, get into the incinerator calcination and handle the back emptying.
The characteristics that existing carbon bisulfide refining system and method for recovering tail gas show are: molten sulfur separates with carbon disulfide not exclusively; Be entrained with carbon disulfide in the molten sulfur that reclaims; Because the aerial self-ignition point of carbon disulfide is 90 ℃; Under chance high temperature and conditions of air, be easy to catch fire, thereby bring more serious potential safety hazard; Refining system tail gas pressure is not high; Getting into incinerator calcination processing emptying meeting pollutes; With 10,000 tons of/year carbon disulfide is example, if sulfide hydrogen that desulfurizing tower and distillation column condenser give off and carbon disulfide tail gas are 40kg/h, gets into incinerator burning back emptying; The then annual oxysulfide that enters atmosphere has 300t~400t (the annual production time continuously is in 8000h); No matter be,, all can not allow still from enterprise self economic benefit from more and more stricter at present environmental regulation.
Summary of the invention
The object of the present invention is to provide a kind of method of carbon bisulfide refining system tail gas recycle.
A kind of method of carbon bisulfide refining system tail gas recycle is characterized in that: the tail gas of carbon bisulfide refining system is sent into the Crouse system reclaim, said tail gas pressure is 0.027~0.045MPa (gauge pressure).
Main sulfide hydrogen of the tail gas of above-mentioned refining system and carbon disulfide, its pressure is regulated through the automatic control pressure-regulating valve.
The tail gas pressure of above-mentioned carbon bisulfide refining system is the pressure greater than combustion furnace burner in the Crouse system, and combustion furnace burner pressure is 0.015~0.027Mpa (gauge pressure).
Reclaim in order to make tail gas send into the Crouse system better, above-mentioned tail gas pressure is preferably 0.030~0.040MPa (gauge pressure).
After tail gas pressure raises; In order to make the carbon disulfide in the refining system desulfurizing tower effectively separate the eliminating potential safety hazard with molten sulfur; Molten sulfur in the carbon bisulfide refining system desulfurization Tata still behind the washing carbon disulfide gets into the sulphur separator; Molten sulfur is further separated with carbon disulfide, and the carbon disulfide of separating is back to desulfurizing tower; The number of plates of said sulphur separator is 5~10, is preferably 7~8.
The refining system and the sulphur separator pressure that bring for the rising of balance tail gas pressure raise, and the separating effect that improves the sulphur separator, and the molten sulfur that above-mentioned sulphur separator separates gets into the Sulphur sealer that fluid-tight is arranged, and height liquid seal is 2200~2500mm.
In order not contain carbon disulfide in the molten sulfur that more effectively improves separating effect and assurance recovery, the height liquid seal in the above-mentioned Sulphur sealer is preferably 2400mm, and its fluid-tight medium is a molten sulfur; The molten sulfur that reclaims in the Sulphur sealer is delivered to the molten sulfur storage tank and is utilized again.
Specifically; A kind of method for recovering tail gas of carbon bisulfide refining system: it is 0.027~0.045MPa (gauge pressure) that carbon bisulfide refining system tail gas (main sulfide hydrogen and carbon disulfide) is regulated pressure through the automatic control pressure-regulating valve; Be preferably 0.030~0.040MPa (gauge pressure), send into again and carry out imperfect combustion in the combustion furnace of Crouse system and reclaim sulphur; Said carbon bisulfide refining system comprises desulfurizing tower, sulphur separator, Sulphur sealer, condenser and rectifying column etc.; Carbon disulfide washs the molten sulfur that gets off and gets into the sulphur separator in the desulfurization Tata still; Molten sulfur is further separated with carbon disulfide, and the carbon disulfide of separating is back to desulfurizing tower, and molten sulfur gets into Sulphur sealer; The number of plates of said sulphur separator is 5~10, is preferably 7~8; The height liquid seal of said Sulphur sealer is 2200~2500mm, is preferably 2400mm, and the fluid-tight medium is a molten sulfur; The molten sulfur that reclaims in the Sulphur sealer is delivered to the molten sulfur storage tank and is utilized again.
The present invention has following beneficial effect:
The inventive method has adopted the automatic control pressure-regulating valve to regulate the tail gas pressure of carbon bisulfide refining system; Make it can successfully get into the Crouse system and reclaim sulphur; Make full use of tail gas and made it be converted into sulphur, and avoided the environmental pollution that emptying brought after the calcination of sulfur-bearing tail gas; Simultaneously; It is 7~8 sulphur separator and the specific interior sulphur envelope of Sulphur sealer height that carbon bisulfide refining system of the present invention adopts the number of plates; Improved the separating effect of carbon disulfide and molten sulfur, guaranteed that the molten sulfur that Sulphur sealer is recycled to the molten sulfur storage tank contains carbon disulfide hardly, has improved process safety.
The specific embodiment
Through embodiment the present invention is carried out concrete description below; Be necessary to be pointed out that at this following examples only are used for the present invention is further specified; Can not be interpreted as the restriction to protection domain of the present invention, the technical staff in this field can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment 1:
Coarse carbon bisulfide is introduced desulfurization in the desulfurizing tower; Molten sulfur is accumulated entering sulphur separator and further molten sulfur is separated with carbon disulfide in the tower still; The separation tray number of sulphur separator is 8 blocks of column plates, and the molten sulfur of recovery gets into Sulphur sealer by the sulphur separator, and the sulphur envelope in the Sulphur sealer highly is 2400mm; Carbon disulfide entering rectifying column by overflowing in the desulfurizing tower top is made with extra care; Pressure is improved to 0.033MPa from system's tail gas (being mainly hydrogen sulfide and carbon disulfide) that condenser comes out through the automatic control pressure-regulating valve in the back, and the combustion furnace of sending into the Crouse system reclaims sulphur.
With 10,000 tons of/year carbon disulphide production devices is example; Carbon bisulfide refining system tail gas (hydrogen sulfide: 15~25kg/h; Carbon disulfide: send into the Crouse system behind 12~22kg/h) the raising pressure and reclaim sulphur, then the sulphur of annual (in 8000h) recovery is 310t.
Embodiment 2:
Coarse carbon bisulfide is introduced desulfurization in the desulfurizing tower; Molten sulfur is accumulated entering sulphur separator and further molten sulfur is separated with carbon disulfide in the tower still; The separation tray number of sulphur separator is 5 blocks of column plates, and the molten sulfur of recovery gets into Sulphur sealer by the sulphur separator, and the sulphur envelope in the Sulphur sealer highly is 2500mm; Carbon disulfide entering rectifying column by overflowing in the desulfurizing tower top is made with extra care; Pressure is improved to 0.045MPa from system's tail gas (being mainly hydrogen sulfide and carbon disulfide) that condenser comes out through the automatic control pressure-regulating valve in the back, and the combustion furnace of sending into the Crouse system reclaims sulphur.
With 10,000 tons of/year carbon disulphide production devices is example; Carbon bisulfide refining system tail gas (hydrogen sulfide: 15~25kg/h; Carbon disulfide: send into the Crouse system behind 12~22kg/h) the raising pressure and reclaim sulphur, then the sulphur of annual (in 8000h) recovery is 290t.
Embodiment 3:
Coarse carbon bisulfide is introduced desulfurization in the desulfurizing tower; Molten sulfur is accumulated entering sulphur separator and further molten sulfur is separated with carbon disulfide in the tower still; The separation tray number of sulphur separator is 10 blocks of column plates, and the molten sulfur of recovery gets into Sulphur sealer by the sulphur separator, and the sulphur envelope in the Sulphur sealer highly is 2200mm; Carbon disulfide entering rectifying column by overflowing in the desulfurizing tower top is made with extra care; Pressure is improved to 0.027MPa from system's tail gas (being mainly hydrogen sulfide and carbon disulfide) that condenser comes out through the automatic control pressure-regulating valve in the back, and the combustion furnace of sending into the Crouse system reclaims sulphur.
With 10,000 tons of/year carbon disulphide production devices is example; Carbon bisulfide refining system tail gas (hydrogen sulfide: 15~25kg/h; Carbon disulfide: send into the Crouse system behind 12~22kg/h) the raising pressure and reclaim sulphur, then the sulphur of annual (in 8000h) recovery is 280t.
The comparative example 1:
Coarse carbon bisulfide is introduced desulfurization in the desulfurizing tower, and molten sulfur is accumulated in the tower still and is got into the sulphur separator, further molten sulfur is separated with carbon disulfide; Carbon disulfide gets into destilling tower by the top effusion and makes with extra care.After carbon disulfide is made with extra care in rectifying column, low from system's tail gas (being mainly hydrogen sulfide and carbon disulfide) that condenser comes out owing to pressure, get into the incinerator calcination and handle the back emptying.
With 10,000 tons of/year carbon disulphide production devices is example; Carbon bisulfide refining system tail gas (hydrogen sulfide: 12~29kg/h; Carbon disulfide: 15~27kg/h) get into the incinerator calcination handles the back emptying; The oxysulfide that then annual (in 8000h) enters atmosphere and separates the sulphur that obtains and contains carbon disulfide and also have big potential safety hazard more than 350t.

Claims (1)

1. the method for recovering tail gas of a carbon bisulfide refining system is characterized in that: utilize the automatic control pressure-regulating valve that the tail gas gauge pressure of carbon bisulfide refining system is adjusted to 0.030 ~ 0.040MPa and send into the Crouse system and reclaim; The molten sulfur that comes out in the desulfurizing tower of said carbon bisulfide refining system gets into the sulphur separator to be separated with carbon disulfide molten sulfur; The number of plates of sulphur separator is 7~8; Adopting with the molten sulfur is that fluid-tight medium, height liquid seal are that the Sulphur sealer of 2400mm further separates with carbon disulfide molten sulfur again, and the molten sulfur that reclaims is at last delivered to the molten sulfur storage tank.
CN 201010184438 2010-05-27 2010-05-27 Tail gas recovery method of carbon bisulfide refining system Active CN101829484B (en)

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CN102153053B (en) * 2010-11-20 2013-04-10 辽宁瑞兴化工集团有限公司 Methods for purifying and comprehensively utilizing hydrogen sulfide byproduct during production of carbon disulfide by methane method
CN107158890A (en) * 2017-05-05 2017-09-15 安徽宣城金宏化工有限公司 It is a kind of to be used for the processing equipment of volatile organic matter in carbon disulphide production
CN108298539B (en) * 2018-04-10 2024-02-27 上海东庚化工技术有限公司 Sulfur high-temperature condensation separator used in carbon disulfide production process
CN112408392B (en) * 2020-12-09 2023-04-25 吉林三源化工有限公司 Carbon disulfide warehousing and transportation system

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CN1919733A (en) * 2006-09-18 2007-02-28 孔庆然 Apparatus and method for recovering carbon disulfide in hydrogen sulfide gas during preparing process of carbon disulfide
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CN1935646A (en) * 2006-09-18 2007-03-28 孔庆然 Equipment and method for treating exhaust gas for carbon bisulfide preparing process

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