CN105080172A - Desulfurating rectifying tower for manufacturing carbon disulfide by virtue of high pressure non-catalytic natural gas method - Google Patents

Desulfurating rectifying tower for manufacturing carbon disulfide by virtue of high pressure non-catalytic natural gas method Download PDF

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Publication number
CN105080172A
CN105080172A CN201510371803.2A CN201510371803A CN105080172A CN 105080172 A CN105080172 A CN 105080172A CN 201510371803 A CN201510371803 A CN 201510371803A CN 105080172 A CN105080172 A CN 105080172A
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China
Prior art keywords
carbon disulfide
tower
sulphur
rectifying column
natural gas
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CN201510371803.2A
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Chinese (zh)
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李刚
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LIAONING RUIXING CHEMICAL GROUP CO Ltd
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LIAONING RUIXING CHEMICAL GROUP CO Ltd
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a desulfurating rectifying tower for manufacturing carbon disulfide by virtue of a high pressure non-catalytic natural gas method and belongs to the field of inorganic chemical product production. The rectifying tower is composed of parts such as a barrel, an ADV type float valve tray, scatter piled pricking, a grating, a liquid distributor and the like. In a carbon disulfide production process, a gas-liquid component comprising carbon disulfide, methane, hydrogen sulfide and sulfur enters into the desulfurating rectifying tower through a feed inlet for gas-liquid contact and transfer in the tower; volatile components methane, hydrogen sulfide and carbon disulfide are separated in form of gaseous phase from the tower top and is cooled by a tower top condenser; in addition to a part for reflux, the rest part is transferred to the next step for re-separation; nonvolatile sulfur is accumulated to the tower bottom and is discharged to the next step to be treated, so that the purpose of removing sulfur is achieved.

Description

The desulfurization rectifying column of manufacturing carbon disulfide using high pressure non catalytic natural gas method
Technical field
The invention belongs to inorganic chemical product production field.Relate to a kind of chemical products separation equipment, be specifically related to a kind of rectifying column that can be separated micro-sulphur in carbon disulfide.
Background technology
Carbon disulfide is a kind of important chemical raw material, is widely used in the industries such as staple fibre, agricultural chemicals, rubber, technics of metallurgy mineral dressing.The method of current domestic production carbon disulfide, according to raw materials used difference, is divided into natural gas act, coke method two kinds, and wherein most widely used production method is natural gas act, and concrete reaction equation is as follows:
CH 4+4S→CS 2+2H 2S
Methane and sulphur at high temperature react and generate carbon disulfide and accessory substance hydrogen sulfide.Also containing unreacted methane, sulphur in product, according to the difference of each component boiling point, high boiling sulphur is wherein separated by the general mode of rectifying that adopts.The form that current carbon disulphide production desulfurization rectifying column adopts has valve tower, packed tower, wherein at the bottom of simple, the cost of packed tower structure, is applicable to carbon disulphide production on a small scale; Valve tower has that treating capacity is large, operational load fluctuation range is large, structure is simple, easily manufactured, cost is low, the perforated area of column plate blocks greatly, not easily, plate efficiency high, is widely used in serialization, carbon disulphide production in enormous quantities.
The carbon disulphide production raw material sulphur overwhelming majority derives from petrochemical industry and coal chemical industry, and due to production technology and the raw material sources difference of sulphur, in product, organism kinds is many, and content is generally between 0.3-0.8%.The quality requirement of valve tower to raw material sulphur is high, once sulphur abnormal quality, then cause carbon disulfide output and quality defective, exceed state quality standard, products application is restricted.
Summary of the invention
An object of the present invention is to provide the equipment-desulfurization rectifying column being separated sulphur in a kind of carbon disulphide production process.Based on the raw material components of carbon disulfide, hydrogen sulfide, sulphur and methane, pressure reduction is utilized to enter into desulfurization rectifying column from charging aperture, gas-liquid contact, mass transfer is carried out in tower, volatile components methane, hydrogen sulfide, carbon disulfide are separated from tower top, cool through overhead condenser, except a part is for except refluxing, remainder is then transferred to subsequent processing and is separated; Not volatile sulphur is then accumulated at the bottom of tower, reaches the object removing sulphur.
Another object of the present invention is the irregular filler by increasing certain altitude at former ADV valve tower stripping section, improve rectifying column feed separation effect not changing on existing equipment agent structure basis, reduce entrainment, reduce non-volatile content content in carbon disulfide finished product, improve carbon disulfide product quality; Expand raw material sulfur source, sulphur quality expands to certified products by the top grade product in GB/T2449-2006 " industrial sulphur ", facilitates materials procurement.
Accompanying drawing explanation
Fig. 1 is the equipment drawing of the desulfurization rectifying column of manufacturing carbon disulfide using high pressure non catalytic natural gas method of the present invention
Wherein, mouth of pipe 1-charging aperture; Liquid-phase outlet at the bottom of mouth of pipe 2-tower; Mouth of pipe 3-overhead reflux mouth; Mouth of pipe 4-top gaseous phase exports; 5-packing layer; 6-column plate.
Fig. 2 is the process chart involved by desulfurization rectifying column of manufacturing carbon disulfide using high pressure non catalytic natural gas method of the present invention
Wherein, A-402-desulfurization rectifying column: H-202-overhead condenser; H-403 tower bottom reboiler; A-209-carbon disulfide condensate liquid receiving tank; P-201-desulfurizing tower reflux pump.
Technical scheme
As shown in Figure 2 with the raw material that carbon disulfide, hydrogen sulfide, sulphur and methane are principal component, utilize pressure reduction to enter into desulfurization rectifying column A-402 from charging aperture, carry out gas with the steam that boils again at the bottom of overhead reflux condensate liquid and tower
Liquid contact, mass transfer, volatile components methane, hydrogen sulfide, carbon disulfide are separated from desulfurization rectifying column tower top A-402, cool through overhead condenser H-202, enter carbon disulfide condensate liquid receiving tank A-209, part liquid carbon disulphide returns desulfurization rectifying column A-402 for backflow through desulfurizing tower reflux pump P-201, and remainder carbon disulfide and solidifying hydrogen sulfide and methane are then transferred to subsequent processing and is separated; Not volatile sulphur and carbon disulfide liquid then flow at the bottom of desulfurization rectifying tower, and through reboiler H-403 heat cycles, vaporized away by carbon disulfide contained in molten sulfur, sulphur is then accumulated at the bottom of tower, reach the object removing sulphur, isolated sulphur can return and be used further to produce.
Desulfurization rectifying column A-402 adopts plate column structure, adopts ADV formula float valve tray, can reduce entrainment, improve gas-liquid mass transfer efficiency; Stripping section filler adopts irregular filler as Raschig ring, Pall ring, and its specification is Ф 16-Ф 50, packed height 0.5-3 rice.
In course of normal operation, desulfurization rectifying column A-402 pressure maintains between 0.6-1.3Mpa (gauge pressure), and column bottom temperature remains on 130-160 DEG C, and tower top temperature remains on 90-110 DEG C, reflux ratio R is 0.5-1, and at the bottom of tower, liquid level remains on 30-50%.
Relative to existing production technology, the present invention mainly has following advantage:
1, desulfurization rectifying column A-402 adopts with valve tower main body and sets up the random packing of certain altitude at rectifying section, have that treating capacity is large, operational load fluctuation range is wide, the perforated area of column plate greatly, the not easily feature such as blocking, to be applicable on a large scale, continuous prodution.
2, adopt desulfurizer material mass transfer provided by the invention, good separating effect, can effectively reduce non-volatile content in carbon disulfide, improve the quality of products, meet the needs of different users.Raw material sulfur product quality can expand to certified products by the top grade product in former GB/T2449-2006 " industrial sulphur ", facilitates materials procurement.
3, adopt that desulfurizer structure provided by the invention is simple, cost is low, can transform on original plate column basis, tower agent structure and each technique mouth of pipe do not change, and only increase one section of tower joint, and load certain altitude filler, and transformation is convenient, it is little to invest.
Detailed description of the invention
Methane and sulphur at high temperature react and generate carbon disulfide, methane, sulphur and methane mixed gas fluid component, and wherein gas flow is 519m 3/ h, fluid flow is 3.86m 3/ h, utilizes pressure reduction to enter into desulfurization rectifying column A-402 from charging aperture, carries out gas-liquid contact, mass transfer with the steam that boils again at the bottom of overhead reflux condensate liquid and tower, and tower top pressure is 1.0Mpa (gauge pressure), tower top temperature 108 DEG C; Volatile components methane, hydrogen sulfide and carbon disulfide are separated from tower top, cool through overhead condenser H-202, part liquid carbon disulphide returns desulfurization rectifying column A-402 for backflow through desulfurizing tower reflux pump P-201, reflux ratio R is 0.7, and remainder carbon disulfide and solidifying hydrogen sulfide and methane are then transferred to subsequent processing and is separated; Not volatile sulphur and carbon disulfide liquid then flow at the bottom of tower, and through tower bottom reboiler H-403 heat cycles, carbon disulfide contained in molten sulfur is vaporized away, tower bottom pressure is 1.1Mpa (gauge pressure), column bottom temperature is 146 DEG C, liquid level 47% at the bottom of tower, and sulphur is then accumulated at the bottom of tower, reach the object removing sulphur, isolated sulphur can return sulphur recovery unit for regenerative ratio.Desulfurization rectifying column A-402 is plate column, and adopt ADV float valve tray, open ratio of plate is 18.5%; For reducing the non-volatile content of carbon disulfide, more than stripping section setting up 2.5 meters high irregular fillers, adopting Ф 30 stainless steel Pall ring.
Produce and adopt certified products, wherein sulfur content 99.3% with raw material sulphur; In finished product carbon disulfide, non-volatile content is 0.006%.

Claims (5)

1. a desulfurization rectifying column for manufacturing carbon disulfide using high pressure non catalytic natural gas method, described rectifying column includes the parts such as cylindrical shell, ADV type float valve tray, random packing, grid, liquid distribution trough.In carbon disulphide production process, include carbon disulfide, methane, hydrogen sulfide, sulfury fluid component enter into desulfurization rectifying column through charging aperture, gas-liquid contact, mass transfer is carried out with the steam that boils again at the bottom of overhead condensation liquid and tower, volatile components methane, hydrogen sulfide, carbon disulfide to be separated with gas phase from tower top and are cooled through overhead condenser, except a part is for except refluxing, remainder is then transferred to subsequent processing and is separated; Not volatile sulphur is then accumulated at the bottom of tower, reaches the object removing sulphur.
2. the method for claim 1, is characterized in that: the present invention is applicable to sulphur and natural gas being separated for sulphur in material in raw material carbon disulphide production process.
3. the method for claim 1, is characterized in that: desulfurization rectifying column main body adopts plate column form, and sets up one section of irregular filler at rectifying section.
4. method as claimed in claim 3, is characterized in that: desulfurization rectifying column adopts ADV type float valve tray, and irregular filler can adopt Raschig ring or Pall ring form, and its specification is Φ 16-Φ 50, prioritizing selection Φ 30 Pall ring.
5. method as claimed in claim 2, is characterized in that: carbon disulphide production raw material sulphur quality requirement is in GB/T2449-2006 " industrial sulphur " more than certified products, prioritizing selection Grade A.
CN201510371803.2A 2015-06-25 2015-06-25 Desulfurating rectifying tower for manufacturing carbon disulfide by virtue of high pressure non-catalytic natural gas method Pending CN105080172A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107551591A (en) * 2017-08-19 2018-01-09 安徽泛亚环保科技有限公司 A kind of float valve plate distillation column for reducing mist
CN109173310A (en) * 2018-08-29 2019-01-11 张家港市科华化工装备制造有限公司 Dimethoxym ethane rectifying column
CN112239208A (en) * 2020-12-09 2021-01-19 吉林三源化工有限公司 Carbon disulfide production system

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CN1935645A (en) * 2006-09-18 2007-03-28 孔庆然 Coarse carbon bisulfide rectifying equipment and method
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CN1272389A (en) * 2000-04-19 2000-11-08 天津市新天进科技开发有限公司 Double-flow injection float valve tray
CN1422804A (en) * 2002-12-31 2003-06-11 王起超 Method for collecting and treating excess sulphur and elemental carbon from process gas of carbon bisulfide production
CN1919732A (en) * 2006-09-18 2007-02-28 孔庆然 Primary separation tower for carbon disulphide preparation process
CN1935645A (en) * 2006-09-18 2007-03-28 孔庆然 Coarse carbon bisulfide rectifying equipment and method
CN202876409U (en) * 2012-09-29 2013-04-17 山东金岭化学有限公司 Combined coarse monomer rectification device

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107551591A (en) * 2017-08-19 2018-01-09 安徽泛亚环保科技有限公司 A kind of float valve plate distillation column for reducing mist
CN109173310A (en) * 2018-08-29 2019-01-11 张家港市科华化工装备制造有限公司 Dimethoxym ethane rectifying column
CN112239208A (en) * 2020-12-09 2021-01-19 吉林三源化工有限公司 Carbon disulfide production system

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