CN108147411A - A kind of method that carbon disulfide is prepared using hydrocarbon as raw material - Google Patents
A kind of method that carbon disulfide is prepared using hydrocarbon as raw material Download PDFInfo
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- CN108147411A CN108147411A CN201710242796.5A CN201710242796A CN108147411A CN 108147411 A CN108147411 A CN 108147411A CN 201710242796 A CN201710242796 A CN 201710242796A CN 108147411 A CN108147411 A CN 108147411A
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- carbon disulfide
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- carbonyl sulfur
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Abstract
The present invention relates to one kind using hydrocarbon as raw material, CS is simply prepared2Method.The present invention one is by adjusting raw material, and more efficient land productivity industrial waste gas hydrogen sulfide and CO gas significantly improve the yield of COS, CO made to reach complete conversion, improves CS at a lower temperature2Yield；Second is that the first reaction tower output is contained into COS, H2、CO2And CS2Gaseous mixture is further catalytically decomposed by condensing to detach with rectifying and then the isolated pure gas of COS is entered carbonyl sulfur disproportionation tower, improves CS2Yield;Third, employ compression rectification means separation CO2, COS and CS2, contain CO so as to significantly improve2, COS and CS2Converted product separative efficiency and operability.The technological process realizes the continuous cycle of entire production process, substantially increases the conversion ratio of carbonyl sulfur, hence it is evident that increase CS2Yield, whole process is without side reaction waste discharge.
Description
Technical field
The present invention relates to one kind using hydrocarbon as raw material, CS is simply prepared2Method.
Background technology
Carbon disulfide is a kind of important Inorganic Chemicals, widely used, presently mainly as solvent and as one
The raw material of a little fine chemical product synthesis.As solvent, it is mainly used for viscose rayon, the synthesis of glassine paper and insoluble sulfur
Huang, grease, wax, resin, rubber production.As industrial chemicals, for synthesizing dimethyl thioether, carbon tetrachloride, dimethyl sulfoxide (DMSO),
Dimethyl sulfone, rubber vulcanization accelerator M, D, xanthates mineral flotation agent etc., it is also possible to make the sulphur of como shift catalyst etc.
Agent.Carbon disulfide may further be used to manufacture pesticide, be used as insecticide and cereal fumigant.
The world is widely used sulphur and charcoal, natural gas, propylene etc. and produces carbon disulfide for raw material at present, by reactiveness
Two major class of gas-solid phase reaction and gas phase reaction can be divided into.Gas-solid phase reaction uses charcoal sulphur steam to be made to pass through red heat for raw material
The outer thermal response of charcoal fixed bed is quivered or electric furnace, product is condensed, it is refined just carbon disulfide.Though gas-solid phase reaction is simple easily
Row, but it is apparent the shortcomings that be that small scale, working condition difference intensity are big, energy consumption is big, low production efficiency, of high cost, and disappears
A large amount of forest reserves are consumed, the three wastes environmental pollution generated in production process is serious etc..
Gas phase reaction refers to sulphur and carbon raw material, be it is gaseous under the conditions of reacted, such as methane and sulfur vapor
Reaction, propane, propylene belong to such with reacting for sulfur vapor.Natural gas act is extensive by the production production man of domestic and international CS2 at present
Using.Compared with charcoal process, natural gas act not only have flow it is compact, structurally and operationally it is simple, can continuously automatic control produce it is excellent
Point, but it has strict requirements to raw material, it is necessary to raw material is handled, not so can analyse carbon, coking and blocking catalyst bed, is dropped
Low catalyst activity.Therefore, low temperature and environmentally friendly carbon disulphide production technique are developed, is had great importance.
The reaction of carbon disulfide is prepared using carbon monoxide, has more research, patent US4078045 both at home and abroad
In metal sulfide is used at high temperature as catalyst preparation CS to carbon monoxide and sulfur vapor2Detailed report has been carried out,
But it is not high there are conversion rate of products in preparation process, and conversion ratio can with the growth of catalyst usage time asking for reducing
Topic.The present invention reports a kind of use carbon monoxide and hydrogen sulfide synthesis COS, then is disproportionated by COS and prepares CS2New method.Sulphur
It is a kind of relatively cheap material to change hydrogen, can be obtained from the desulphurization reaction of fossil fuel and natural gas deposit in large quantity,
It can also be produced in the chemical plant installations such as carbon disulfide and obtained by natural gas act.Carbonyl sulfur disproportionation generation carbon disulphide and titanium dioxide
The reaction of carbon is reversible, under normal operation more difficult positive progress.It is therefore, it is necessary to expensive around this using novel method
With inefficient limitation.Therefore take it is a kind of it is novel catalyst include silicon, titanium oxide, aluminium oxide, silica-zirconia
Aluminium, zirconium oxide, silicon carbide, boron, various phosphate etc. have high surface area（>50 MZ/g）Gama-alumina and titanium dioxide
The first choice of silicon-aluminium oxide.The new catalyst can effectively facilitate the positive of reaction and carry out at a lower temperature, so as to substantially carry
The yield of high carbon disulfide provides the synthesis of sulfur dioxide a kind of efficiently convenient production ways.
Invention content
The conversion ratio of sulphur is relatively low when the present invention is in order to solve existing preparation carbonyl sulfur, generates industrial waste gas hydrogen sulfide more
Seriously, the problems such as dismutation conversion ratio of carbonyl sulfur is low, and the separative efficiency of carbonyl sulfur and carbon dioxide is relatively low, provides
A kind of method that carbon disulfide is prepared using hydrocarbon as raw material.
The present invention adopts the following technical scheme that realization：Carbon disulfide is prepared by raw material of hydrocarbon（CS2）'s
Method, this method include the following steps：
A. the mixed gas of carbon monoxide and hydrogen sulfide is passed through in new catalyst in 0.5-2.8 MPa, 200-400 DEG C
Under the action of the method reacted, generate carbonyl sulfur and hydrogen；
B. generation is contained into a small amount of carbon disulfide based on carbonyl sulfur and hydrogen<The mix products of 5 % and carbon dioxide lead to
Condensation separator is crossed, by carbon disulfide condensation separation；
C. the isolated mix products boosting based on carbonyl sulfur and carbon dioxide of b step is entered first rectifying column to pressurize
Rectifying, hydrogen go out with carbon dioxide from rectifying tower top part in gaseous form；
D. first rectifying column kettle base solution decompression after, with step b condensation and separation of carbon disulfide condensate liquid mix, into second
Rectifying column rectifying, bottom of towe obtain carbon disulfide crude product, and carbonyl sulfur goes out in gaseous form from rectifying tower top part；
E. step d rectifying is obtained gaseous state carbonyl sulfur to be passed through, in the carbonyl sulfur disproportionation tower equipped with acidic metal oxide catalyst
Disproportionation decomposition is carried out, carbon disulfide, carbon dioxide, the mixture of carbonyl sulfur and step a that disproportionation obtains are obtained with carbonyl sulfur
Based on the mix products containing a small amount of carbon disulfide and carbon dioxide merge after, in the condensation separator for entering step b, according to
Above-mentioned steps carry out subsequent separation process again, realize cycle production process.
The raw material of carbon monoxide described above is in the industrial waste gas discharged with factories and miness such as nitrogen fertilizer plant, Yellow Phosphorous Plant, coke-oven plants
Main component CO；The wherein described hydrogen sulfide is by the industrial waste gas that is discharged in industrial production.
Should be kept in admixture of gas in above-mentioned steps a carbon monoxide to the molar ratio of hydrogen sulfide about 1 with this novel
Catalyst include M0.1-2M* 0.01-1M** 0.01-2OxSy, M is at least molybdenum, tungsten, iron one kind therein, M*At least ruthenium, rhodium, silver,
Platinum, palladium, gold, rhenium, osmium, iridium one kind therein；M**At least vanadium, chromium, titanium, cobalt, nickel, copper one kind therein；Reaction temperature is
200―400℃。
In 0.1-2.5MPa, condensation temperature is controlled in curing for the condensing pressure control of condensation separator in above-mentioned steps b
The dew point of carbon is hereinafter, promote most of carbon disulfide to be condensed into liquid.
In above-mentioned steps c the operating pressure of first rectifying column be 1.0-3.5MPa, feeding manner can be gas phase, liquid phase or
Arbitrary in gas-liquid mixed phase, the purpose for adding in rectifying column is to improve COS and CO2Separating degree.
The operating pressure of Second distillation column is 0.1-2.0MPa in above-mentioned steps d, and feeding manner is liquid phase feeding.
The disproportionated reaction temperature of carbonyl sulfur is 100-450 DEG C in above-mentioned steps e, and the acidic metal oxide catalyst is
A1203, Si02, Ti02, Zr02, any one or a few in molecular sieve, diatomite are mixed with arbitrary proportion.
The present invention provides a kind of by CO and hydrogen sulfide production CS on the basis of patent US38569252It is different and
More rational new technological flow, innovation are shown：When by adjusting raw material and preparation method, it is relatively efficiently sharp
With industrial waste gas hydrogen sulfide and CO gas, the yield of COS is significantly improved at a lower temperature, is reached CO and is turned completely
Change, improve CS2Yield；Second is that the first reaction tower output is contained into COS, H2、 CO2And CS2Gaseous mixture, by condensation and essence
Fraction enters carbonyl sulfur disproportionation tower from and then by the isolated pure gas of COS and is further catalytically decomposed, and significantly improves
CS2Yield;Third, employ compression rectification means separation CO2, COS and CS2, CS2Normal boiling point for 46.2 DEG C, and COS
And CO2Boiling point be respectively then -50.3 DEG C and -78.5 DEG C, pressurization can improve the boiling point of fraction, contain so as to significantly improve
CO2, COS and CS2Converted product separative efficiency and operability.The technological process realizes the continuous of entire production process
Cycle substantially increases the conversion ratio of carbonyl sulfur, hence it is evident that increase CS2Yield, and react with separation process simply and readily
Operation;COS and CO after separation2It can recycle, whole process is an atom economy and section without side reaction waste discharge
Energy environment-friendly type clean manufacturing process, if being CO and H with some by-products2The chemical production device of S, which is combined, founds the factory and can embody
The energy saving and environment-friendly advantage of bigger.
Description of the drawings
Fig. 1 is the process flow chart of the present invention；
In figure：1- metal sulfide COS low temperature synthetic catalysts；2- carbonyl sulfur synthetic towers；3- condensation separators；The first rectifying of 4-
Tower;5- Second distillation columns;6- acidic metal oxide catalyst;7- carbonyl sulfurs are disproportionated tower;8- carbon monoxide producers;9- gases
Compressor;10- delivery pumps.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawings and detailed description, but not limited to the examples.
One kind prepares CS by raw material of hydrocarbon2Method, using coke to be former first in the carbon monoxide producer 8
Material, oxygen and carbon dioxide prepare unstripped gas carbon monoxide for gasifying agent, and the carbon dioxide is what is isolated in above-mentioned steps c
Then carbon dioxide includes the following steps:A. carbon monoxide obtained and hydrogen sulfide are obtained after gas compressor 9 pressurizes
Then the homogeneous mixture of CO and hydrogen sulfide introduce the carbonyl sulfur synthetic tower equipped with metal sulfide COS low temperature synthetic catalysts,
Carbonyl sulfur is generated, and part carbonyl sulfur disproportionation is made to be decomposed into carbon disulfide and carbon dioxide;It should be protected in step a admixture of gas
Hold carbon monoxide to the molar ratio of hydrogen sulfide about 1 with this novel catalyst includes M0.1-2M* 0.01-1M** 0.01-2OxSy,M
At least molybdenum, tungsten, iron one kind therein, M*At least ruthenium, rhodium, silver, platinum, palladium, gold, rhenium, osmium, iridium one kind therein；M**At least
It is vanadium, chromium, titanium, cobalt, nickel, copper one kind therein；Reaction temperature is 200-400 DEG C, and it is corresponding to pass through selected metallic element
Metal oxide react and be made with vulcanizing agent, carrier A1203, Si02, Ti02, Zr02In any one or it is several
Kind is mixed with arbitrary proportion.B. by generation based on carbonyl sulfur and the mixing containing a small amount of carbon disulfide and carbon dioxide produce
By condensation separator 3, condensing pressure is controlled in 0.1-2.5MPa values object (may contain a small amount of carbon monoxide for reaction)
Can be 0.1MPa or 2.5MPa or 1MPa or 1.5MPa or 2MPa), condensation temperature controls the dew point in carbon disulfide hereinafter, making two
Nitric sulfid and hydrogen are condensed separation, are discharged by condenser bottom;In obtained condensate liquid based on carbon disulfide, Ke Nengrong
There are a certain amount of COS and minimal amount of CO2, the gas phase separated is then based on COS, containing a certain amount of CO2 and minimal amount of CS2;
C. by the isolated gas phase mixtures based on carbonyl sulfur and carbon dioxide of step b after gas compressor 6 boosts, enter
First rectifying column 4 (de- CO2 towers) compression rectification, feeding manner can be any one in gas phase, liquid phase or gas-liquid mixed phase,
Operating pressure is that 1.0-3.5MPa values can be 1.OMPa or 3.5MPa or 2MPa or 3.OMPa), carbon dioxide is from tower top with gas
It mutually separates, returns CO Gas-making Furnaces after depressurizing throttle expansion valve 10 and make raw material use, and recycle cold, the liquid phase that bottom of towe separates is
COS (may contain minute quantity CS2);D. the kettle base solution of first rectifying column 4 obtains after delivery pump, the decompression of liquid pressure-reducing valve with step b
After the carbon disulfide condensate liquid mixing arrived, into Second distillation column 5 (de- COS towers) rectifying, operating pressure takes for 0.1-2.OMPa
Value can be 0.1MPa or 1.5MPa or 2.OMPa), feeding manner is liquid phase feeding, and gas phase carbonyl sulfur is separated from tower top, and bottom of towe obtains
To liquid carbon disulphide crude product, CS2 crude products finally can obtain pure CS2 fluid products after further rectifying processing;E. from step
After the gas phase carbonyl sulfur decompression that d is obtained, into the carbonyl sulfur disproportionation tower 7 equipped with acidic metal oxide catalyst 6, (COS is disproportionated
Tower) carry out disproportionation decomposition, disproportionated reaction temperature be 100-450 DEG C (value can be 100 DEG C or 450 DEG C or 200 DEG C or 250 DEG C or
350 DEG C or 300 DEG C or 400 DEG C), the acidic metal oxide catalyst 6 is A1203,Si02, Ti02, Zr02, molecule
Any one or a few in sieve, diatomite is mixed with arbitrary proportion, can be to be individually for A1 in the specific implementation203Or
Si02Or Ti02Or Zr02Or molecular sieve or diatomite or A 1203-5 iO2 or A 1203-TiO2Or Si02Diatomite or
SiO2-TiO2-Zr02Etc. a variety of;It obtained cos-containing, the mixture of carbon dioxide and carbon disulfide and is obtained from step b
Merge based on carbonyl sulfur and containing the mix products of a small amount of carbon disulfide and carbon dioxide after, enter step the condensation separation of b
Device 3 and subsequent rectifying separation, carry out subsequent separation process according to above-mentioned steps (step b, c, d, e), realize cycle again
Production process not only greatly improves the yield of carbon disulfide, but also without any waste discharge.
Claims (7)
1. a kind of method that carbon disulfide is prepared using hydrocarbon as raw material, it is characterized in that this method includes the following steps：
The side that the mixed gas of carbon monoxide and hydrogen sulfide is reacted under the action of new catalyst is passed through at 200-400 DEG C
Method generates carbonyl sulfur and hydrogen；
The mix products containing a small amount of carbon disulfide and carbon dioxide based on carbonyl sulfur and hydrogen of generation are passed through into condensation
Separator, by carbon disulfide and hydrogen condensation separation；
The isolated mix products boosting based on carbonyl sulfur, hydrogen and carbon dioxide of b step is entered into first rectifying column
Compression rectification, hydrogen go out with carbon dioxide from rectifying tower top part in gaseous form；
After the kettle base solution decompression of first rectifying column, with step b condensation and separation of carbon disulfide condensate liquid mix, it is smart into second
Tower rectifying is evaporated, bottom of towe obtains carbon disulfide crude product, and carbonyl sulfur goes out in gaseous form from rectifying tower top part；
Step d rectifying is obtained gaseous state carbonyl sulfur to be passed through, in carbonyl sulfur equipped with acidic metal oxide catalyst disproportionation tower into
Row disproportionation is decomposed, will be disproportionated obtained carbon disulfide, carbon dioxide, the mixture of carbonyl sulfur and step a obtain using carbonyl sulfur as
After the main mix products containing a small amount of carbon disulfide and carbon dioxide merge, in the condensation separator for entering step b, according to upper
It states step and carries out subsequent separation process again, realize cycle production process.
2. the method according to claim 1 that carbon disulfide is prepared using hydrocarbon as raw material, it is characterized in that with industry
Exhaust gas（Nitrogen fertilizer plant, Yellow Phosphorous Plant, coke-oven plant）In main component CO.
3. hydrogen sulfide described in is obtained from the desulphurization reaction of fossil fuel and natural gas deposit, can also be by using Crouse
The plant processes that technique carries out removing hydrogen sulfide gas provide.
4. the method according to claim 1 that carbon disulfide is prepared using hydrocarbon as raw material, it is characterized in that step a gas
Should be kept in body mixture carbon monoxide to the molar ratio of hydrogen sulfide about 1 with this novel catalyst includes M0.1- 2M* 0.01-1M** 0.01-2OxSy, M is at least molybdenum, tungsten, iron one kind therein, M*At least ruthenium, rhodium, silver, platinum, palladium, gold, rhenium, osmium, iridium
One kind therein；M**At least vanadium, chromium, titanium, cobalt, nickel, copper one kind therein；Reaction temperature is 200-400 DEG C.
5. the method according to claim 1 or 2 that carbon disulfide is prepared using hydrocarbon as raw material, it is characterized in that above-mentioned
The condensing pressure control of condensation separator (3) is in 0.1-2.5MPa in step b, condensation temperature control the dew point in carbon disulfide with
Under.
6. the method according to claim 1 or 2 that carbon disulfide is prepared using hydrocarbon as raw material, it is characterized in that above-mentioned
The operating pressure of first rectifying column (4) is 1.0-3.5MPa in step c, and feeding manner can be gas phase, liquid phase or gas-liquid mixed
It is arbitrary in phase
The method according to claim 1 or 2 that carbon disulfide is prepared using hydrocarbon as raw material, it is characterized in that above-mentioned step
The operating pressure of Second distillation column (5) is 0.1-2.0MPa in rapid d, and feeding manner is liquid phase feeding.
7. the method according to claim 1 or 2 that carbon disulfide is prepared using hydrocarbon as raw material, it is characterized in that above-mentioned
In step e the disproportionated reaction temperature of carbonyl sulfur be 100-450 DEG C, the acidic metal oxide catalyst be A1203, Si02,
Ti02, Zr02, any one or a few in molecular sieve, diatomite are mixed with arbitrary proportion.
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| CN201710242796.5A CN108147411A (en) | 2017-04-14 | 2017-04-14 | A kind of method that carbon disulfide is prepared using hydrocarbon as raw material |
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| CN201710242796.5A CN108147411A (en) | 2017-04-14 | 2017-04-14 | A kind of method that carbon disulfide is prepared using hydrocarbon as raw material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110862087A (en) * | 2019-12-20 | 2020-03-06 | 顺毅南通化工有限公司 | Method and device for preparing high-purity carbonyl sulfide |
| CN113811510A (en) * | 2019-06-27 | 2021-12-17 | 日本瑞翁株式会社 | Process for producing carbonyl sulfide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5609845A (en) * | 1995-02-08 | 1997-03-11 | Mobil Oil Corporation | Catalytic production of hydrogen from hydrogen sulfide and carbon monoxide |
| CA2341069A1 (en) * | 2000-03-22 | 2001-09-22 | Lehigh University | Improved production of hydrogen from hydrogen sulfide |
| CN101811698A (en) * | 2009-12-24 | 2010-08-25 | 上海百金化工集团有限公司 | Method for producing carbon disulfide |
-
2017
- 2017-04-14 CN CN201710242796.5A patent/CN108147411A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5609845A (en) * | 1995-02-08 | 1997-03-11 | Mobil Oil Corporation | Catalytic production of hydrogen from hydrogen sulfide and carbon monoxide |
| CA2341069A1 (en) * | 2000-03-22 | 2001-09-22 | Lehigh University | Improved production of hydrogen from hydrogen sulfide |
| CN101811698A (en) * | 2009-12-24 | 2010-08-25 | 上海百金化工集团有限公司 | Method for producing carbon disulfide |
Non-Patent Citations (2)
| Title |
|---|
| FARAJI, F ET AL.: "CO-Catalyzed conversion of H2S to H-2+S .1. Reaction between CO and H2S", 《INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH》 * |
| 陈兆辉等: "金属氧化物吸附剂脱硫过程中羰基硫的生成", 《现代化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113811510A (en) * | 2019-06-27 | 2021-12-17 | 日本瑞翁株式会社 | Process for producing carbonyl sulfide |
| CN110862087A (en) * | 2019-12-20 | 2020-03-06 | 顺毅南通化工有限公司 | Method and device for preparing high-purity carbonyl sulfide |
| CN110862087B (en) * | 2019-12-20 | 2024-02-13 | 顺毅南通化工有限公司 | Method and device for preparing high-purity carbonyl sulfide |
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Application publication date: 20180612 |