CN109502587A - A method of carbon disulfide is purified using next door tower - Google Patents
A method of carbon disulfide is purified using next door tower Download PDFInfo
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- CN109502587A CN109502587A CN201811650769.2A CN201811650769A CN109502587A CN 109502587 A CN109502587 A CN 109502587A CN 201811650769 A CN201811650769 A CN 201811650769A CN 109502587 A CN109502587 A CN 109502587A
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- tower
- carbon disulfide
- next door
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- separation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/70—Compounds containing carbon and sulfur, e.g. thiophosgene
- C01B32/72—Carbon disulfide
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- Organic Chemistry (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention provides a kind of method using next door tower purification carbon disulfide, the method, including into separating in raw material, next door tower.The next door tower, including public rectifying section, compartmented, public stripping section；The separation is disconnected, including pre-separation area, demarcation plate, sterling area；The demarcation plate is between pre-separation area and sterling area；The cross-sectional area ratio in pre-separation area and sterling area is 0.5-2:1.The present invention uses a tower, and a reboiler and condenser complete the purification of carbon disulfide.Equipment investment and energy consumption are effectively reduced, occupied area is reduced；Using the method for this patent, the carbon disulfide product close to 100% is obtained.Using the method for this patent, plant energy consumption reduces by 45.6%.
Description
Technical field
The invention belongs to chemical intermediate separation fields, are related to a kind of process for separating and purifying of carbon disulfide, and in particular to
To a kind of method using next door rectifying column purification carbon disulfide.
Background technique
Carbon disulfide participates in sulfonating reaction and side reaction, purity of the production technology to carbon disulfide as key reaction substance
It is required that very high.With the hydrogen sulfide and sulphur dissolved on a small quantity in carbon disulfide, since hydrogen sulfide is dissolved in carbon disulfide,
Pure carbon disulfide cannot be obtained using simple evaporation and distillating method, it is necessary to carry out rectifying.Rectifying is by two sulphur of crude product
Change carbon distillation, carbon disulfide and hydrogen sulfide steam generated phase in rectifying column with the liquid carbon disulphide to flow back after condensation
Interaction, and hydrogen sulfide and sulphur are isolated, obtain high-purity carbon disulfide fine work.
Process for preparation of CS 2 disclosed in US2492719A, reaction product gaseous mixture after-condenser carry out sulphur content from rear,
Gas phase enters condenser and so that carbon disulfide is liquefied and enter stripper separation carbon disulfide and hydrogen sulfide, the hydrogen sulfide separated
It is absorbed into hydrogen sulfide scrubber tower using diethanol amine, methane is recycled from the recovered overhead of scrubbing tower, is finally passed through
Analytic Tower, which parses hydrogen sulfide from tower top, to flow out.
CN101912718B provides a kind of device and method with carbon disulfide in solvent absorption hydrogen sulfide gas.By molten
Agent and mass transfer dynamics control process are absorbed, are isolated hydrogen sulfide and carbon disulfide product.
CN105129799A provides a kind of method of carbon bisulfide refining purification, takes and first gasifies, then rectifying, finally passes through
Three-level condensation, micro hydrogen sulfide of going out finally obtain the new process of carbon bisulfide refining product.It needs through hydrogen persulfide destilling tower
With two equipment of carbon bisulfide refining tower.
CN102153053B provides a kind of method of purification of the by-product hydrogen sulfide in carbon disulphide production technique, the present invention
Be related to a kind of method that the by-product hydrogen sulfide by methane method carbon disulphide production technique purifies and to by-product into
The method of row comprehensive utilization, after the product mixtures after desulfurization are passed through the initial gross separation of hydrogen sulfide destilling tower, further to gas phase
Product is purified: being first passed through primary condenser and ultimate condenser for the gas phase distillate of hydrogen sulfide overhead and is carried out two
Grade condensation, then further purified via purification feedstock vessel and hydrogen sulfide treating column, finally obtain high-pure hydrogen sulfide.The present invention uses
Constant pressure B-grade condensation not only can achieve lower condensation temperature, is separated off, also reduces conducive to inert gas in acid gas
Equipment number of packages enhances safety, while reducing equipment investment；The present invention realizes purification overall process exhaust gas and waste liquid simultaneously
Minimum discharge, clean and environmental protection.
CN100447079C provides the rectifying device and method of a kind of coarse carbon bisulfide.It will include sulphur, methane, sulphur
The gas-liquid mixture for changing hydrogen and carbon disulfide passes through rough removing tower respectively, and fine removing tower and finishing column carry out three-tower type continuous rectification, adopt
Obtain the hydrogen sulfide that concentration reaches 99%-99.95% with three-tower type continuous rectification, and better than national standard carbon disulfide at
Product.Three rectifying columns are used in scheme, energy consumption is larger.
In conclusion general at present, there are two types of methods to obtain carbon disulfide sterling, using organic solvent or using essence
Means are evaporated, organic solvent has remaining possibility, and distillation process energy consumption is larger, is mainly shown as that reboiler input heat uses effect
Rate it is low, the energy of reboiler input is largely transferred to the condensing agent of overhead condenser, and it is effective to be really supplied to logistics
The part of energy is seldom.The distillation process of carbon disulfide is needed by three towers, absorption tower, Analytic Tower, treating column, by three at present
A tower, most of the heat that public work provides are condensed agent consumption, and final energy consumption cost is attached on target product, to enterprise
For be worthless.
Summary of the invention
Led to the problem of in existing industrialized production, the present invention provide it is a kind of using the rectifying of next door tower removing sulphur and
Hydrogen sulfide, the method for purifying carbon disulfide realize following goal of the invention:
(1) a tower is used only and purifies carbon disulfide, reduce equipment investment and energy consumption, reduce occupied area；
(2) purification obtains the carbon disulfide product that content is greater than 99.9%.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A method of carbon disulfide is purified using next door tower, including into separating in raw material, next door tower；
It is described into raw material, carbon disulfide crude product 1 enters next door tower pre-separation area A by feed inlet E on the left of the tower of next door；
Separation, trechmannite component 2 are steamed by next door column overhead in the next door tower, and return tank is entered after overhead condenser, is not coagulated
Gas is sent directly into claus oven and burns recycling sulphur, and liquid phase component a part passes back into tower, and a part is plucked out of into trechmannite storage tank.
Weight sulphur component 4 is discharged by next door tower tower bottom, into weight sulphur storage tank.Carbon disulfide finished product 3 is produced by the finished product in the king-tower area of right side
Mouth F extraction, is sent into finished pot.
It is provided with feed inlet E on the next door tower, finished product produces mouth F, overhead condenser, demarcation plate H, tower bottom reboiler,
Tower top return pump, tower reactor discharging pump.
The next door tower, including public rectifying section C, compartmented, public stripping section D；
The separation is disconnected, is located at midsection；The separation is disconnected, including pre-separation area A, demarcation plate H, sterling area B；The demarcation plate
H is located between pre-separation area A and sterling area B；
The demarcation plate H, can control and move in parallel, and the cross-sectional area ratio of pre-separation area A and sterling area B are 0.5-2:
1。
The next door tower, king-tower number of theoretical plate >=20；
The pre-separation area A and sterling area B, theoretical cam curve >=6；It is preferred that 6 ~ 12；
The public rectifying section C is region of the upper end demarcation plate H apart from tower top, theoretical cam curve >=8；It is preferred that 8 ~ 16；
The public stripping section D is region of the lower end demarcation plate H apart from tower bottom, theoretical cam curve >=6；It is preferred that 6 ~ 12；
Reflux ratio, which refers to, flows back into amount of the amount of tower than upper extraction.
The feed inlet E is pre-separation area A from top to bottom at 2/3 column plate；
Finished product extraction mouth F is sterling area B from top to bottom at 1/3 column plate；
The carbon disulfide crude product 1 includes hydrogen sulfide 30-50%, sulphur 1%-3%, remaining is carbon disulfide in terms of weight content.
The feeding temperature is 30-180 DEG C, pressure 6-10bar；
Separation in the next door tower, tower top temperature are 10-60 DEG C, pressure 4-9bar；Overhead reflux ratio >=3；It is preferred that 3 ~ 6；
Column bottom temperature is 100-140 DEG C, pressure 4-10bar.
The mass content of carbon disulfide finished product 3 is 99.92-99.997%, close to 100%；
The quality group of tower top discharging trechmannite component 2 becomes H2S 99.97-99.98%, CS2< 10ppm；
Tower bottom discharging attach most importance to sulphur component 4 quality group become CS20.02-0.11%, S 99.73-99.98%.
The invention has the advantages that:
(1) tower is used, a reboiler and condenser complete the purification of carbon disulfide.Effectively reduce equipment investment and energy
Consumption, reduces occupied area.
(2) method for using this patent, mass content 99.92-99.997%, close to 100% carbon disulfide product.
(3) method for using this patent, plant energy consumption reduce by 45.6%.
Detailed description of the invention
Process flow of the invention and equipment are further described below in conjunction with attached drawing and implementation method.
Fig. 1 is the flow diagram that carbon disulfide is purified using next door tower
In figure:
A-pre-separation area；B-sterling area；The public rectifying section of C-；The public stripping section of D-
E-feed inlet；F-finished product produces mouth；H-demarcation plate；
1-carbon disulfide crude product；2-trechmannite components；3-carbon disulfide finished products；4-weight sulphur components.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be appreciated that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1
The following steps are included:
(1) into raw material
The discharging of carbon disulfide synthesizer includes CS247%, S 3%, H2S 50%(mass ratio) carbon disulfide crude product 1, with
The charging rate of 6250kg/h is sent into next door tower；Raw material is sent by feed inlet E, and feed inlet E is opened in the 6th tower of pre-separation area A
On plate, 30 DEG C of feeding temperature, pressure 6bar.
The next door tower, king-tower have 30 blocks of column plates, and public rectifying section C has 10 blocks of column plates, and public stripping section D has 12 pieces of towers
Plate, midsection have 8 blocks of column plates, and midsection is divided into pre-separation area A and sterling area B by demarcation plate H, pre-separation area A and sterling area B's
Cross-sectional area ratio is 0.5:1.
(2) separation in the tower of next door
Tower bottom is passed through steam, and 100 DEG C of column bottom temperature, pressure 4bar, tower bottom discharging is attached most importance to sulphur component 4, and flow is 188kg/h(packet
Include CS20.11%, S 99.73%), it 10 DEG C of tower top temperature, 4 bar of pressure, discharges and flows back for trechmannite component 2 by condenser
Than being 6, the flow of tower top discharging trechmannite component 2 is 3120kg/h(wherein H2S 99.98%, CS2< 10ppm), finished product produces mouth
F is opened on the 3rd block of column plate of sterling area B, and extraction material is carbon disulfide finished product 3, and flow 2942kg/h contains CS2
99.92%。
Embodiment 2
(1) into raw material
The discharging of carbon disulfide synthesizer includes CS269%, S 1%, H2S 30%(mass ratio) carbon disulfide crude product 1, with
The speed of 6250kg/h is sent into next door tower；Raw material is sent by feed inlet E, and feed inlet E is opened on the 8th column plate of pre-separation area A,
180 DEG C of feeding temperature, pressure 10bar；
The next door tower, king-tower have 40 blocks of column plates, and public rectifying section C has 16 blocks of column plates, and public stripping section D has 12 blocks of column plates, tower
There are 12 blocks of column plates in middle section, and midsection is divided into pre-separation area A and sterling area B by demarcation plate H, and pre-separation area A and sterling area B's is transversal
Area ratio is 1.5:1.
(2) separation in the tower of next door
Tower bottom is passed through steam, and 140 DEG C of column bottom temperature, pressure 10bar, tower bottom discharging is attached most importance to sulphur component 4, and flow is 63kg/h(packet
Include S 99.98%, CS20.02%), 60 DEG C of tower top temperature, 9 bar of pressure discharge and flow back for trechmannite component 2 by condenser
Than being 5, it includes H that the flow of tower top discharging trechmannite component 2, which is 1874kg/h(,2S 99.97%,CS2< 10ppm), finished product produces mouth F
It is opened on the 4th block of column plate of sterling area B, extraction material is carbon disulfide finished product 3, and flow 4313kg/h contains CS2
99.997%。
Embodiment 3
(1) into raw material
The discharging of carbon disulfide synthesizer includes CS258%, S 2%, H2S 40%(mass ratio) carbon disulfide crude product 1, with
The speed of 6250kg/h is sent into next door tower；Raw material is sent by feed inlet E, and feed inlet E is opened on the 4th column plate of pre-separation area A,
100 DEG C of feeding temperature, pressure 8bar；
The next door tower, king-tower have 20 blocks of column plates, and public rectifying section C has 8 blocks of column plates, and public stripping section D has 6 blocks of column plates, in tower
Section has 6 blocks of column plates, and midsection is divided into pre-separation area A and sterling area B, the cross section of pre-separation area A and sterling area B by demarcation plate H
Product ratio is 2:1.
(2) separation in the tower of next door
Tower bottom is passed through steam, and 120 DEG C of column bottom temperature, pressure 8bar, tower bottom discharging is attached most importance to sulphur component 4, and flow is 125kg/h(packet
Include S 99.91%, CS2 0.09%), 30 DEG C of tower top temperature, 7 bar of pressure discharge as trechmannite component 2, by condenser, reflux ratio
It is 6, it includes H that the flow of tower top discharging trechmannite component 2, which is 2497kg/h(,2S 99.98%, CS2< 10ppm), finished product extraction mouth F is opened
On the 2nd block of column plate of sterling area B, extraction material is carbon disulfide finished product 3, and flow 3628kg/h contains CS2 99.94%。
Unless specifically indicated, ratio of the present invention is mass ratio, and the percentage is mass percent.
Claims (9)
1. a kind of method using next door tower purification carbon disulfide, it is characterised in that: the method, including into raw material, next door tower
Interior separation.
2. a kind of method using next door tower purification carbon disulfide according to claim 1, it is characterised in that:
The next door tower, including public rectifying section, compartmented, public stripping section；
The separation is disconnected, including pre-separation area, demarcation plate, sterling area；The demarcation plate is between pre-separation area and sterling area；
The cross-sectional area ratio in pre-separation area and sterling area is 0.5-2:1.
3. a kind of method using next door tower purification carbon disulfide according to claim 1, it is characterised in that: the next door
Tower, king-tower number of theoretical plate >=20；The pre-separation area and sterling area, theoretical cam curve >=6；The public rectifying section, theoretical tower
Plate number >=8；The public stripping section, theoretical cam curve >=6.
4. a kind of method using next door tower purification carbon disulfide according to claim 1, it is characterised in that: described into original
Material, feed inlet are pre-separation area from top to bottom at 2/3 column plate.
5. a kind of method using next door tower purification carbon disulfide according to claim 1, it is characterised in that: described into original
Material, feeding temperature are 30 DEG C -180 DEG C, feed pressure 6-10 bar.
6. a kind of method using next door tower purification carbon disulfide according to claim 1, it is characterised in that: described into original
Material, raw material are carbon disulfide crude product；The carbon disulfide crude product, in terms of weight content, including hydrogen sulfide 30-50%, sulphur 1%-
3%, remaining is carbon disulfide.
7. a kind of method using next door tower purification carbon disulfide according to claim 1, it is characterised in that: the next door
Separation in tower, carbon disulfide crude product enter next door tower pre-separation area, and carbon disulfide finished product is produced by the finished product extraction mouth in sterling area.
8. a kind of method using next door tower purification carbon disulfide according to claim 1, it is characterised in that: the next door
Separation in tower, tower top temperature are 10-60 DEG C, tower top pressure 4-9bar；Column bottom temperature is 100-140 DEG C, tower bottom pressure 4-
10bar；Overhead reflux ratio >=3.
9. a kind of method using next door tower purification carbon disulfide according to claim 7, it is characterised in that: the finished product
Mouth is produced, at sterling area from top to bottom 1/3 column plate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811650769.2A CN109502587B (en) | 2018-12-31 | 2018-12-31 | Method for purifying carbon disulfide by using dividing wall tower |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811650769.2A CN109502587B (en) | 2018-12-31 | 2018-12-31 | Method for purifying carbon disulfide by using dividing wall tower |
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| CN109502587B CN109502587B (en) | 2020-07-28 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19541339A1 (en) * | 1995-11-06 | 1997-05-07 | Linde Ag | Recovering carbon mon:oxide from carbon mon:oxide-rich gas |
| CN103657352A (en) * | 2013-12-16 | 2014-03-26 | 华陆工程科技有限责任公司 | High-purity hydrogen sulfide recovery device and recovery method |
| CN107082427A (en) * | 2017-04-19 | 2017-08-22 | 苏州市兴鲁空分设备科技发展有限公司 | Carbon disulfide retracting device |
| CN108601988A (en) * | 2016-01-22 | 2018-09-28 | 阿科玛股份有限公司 | Utilize dividing wall column distillation purifying mercaptan or thiophene |
-
2018
- 2018-12-31 CN CN201811650769.2A patent/CN109502587B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19541339A1 (en) * | 1995-11-06 | 1997-05-07 | Linde Ag | Recovering carbon mon:oxide from carbon mon:oxide-rich gas |
| CN103657352A (en) * | 2013-12-16 | 2014-03-26 | 华陆工程科技有限责任公司 | High-purity hydrogen sulfide recovery device and recovery method |
| CN108601988A (en) * | 2016-01-22 | 2018-09-28 | 阿科玛股份有限公司 | Utilize dividing wall column distillation purifying mercaptan or thiophene |
| CN107082427A (en) * | 2017-04-19 | 2017-08-22 | 苏州市兴鲁空分设备科技发展有限公司 | Carbon disulfide retracting device |
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| CN109502587B (en) | 2020-07-28 |
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