CN109095468A - A method of carbon disulfide is prepared by raw material of hydrogen sulfide - Google Patents
A method of carbon disulfide is prepared by raw material of hydrogen sulfide Download PDFInfo
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- CN109095468A CN109095468A CN201711443962.4A CN201711443962A CN109095468A CN 109095468 A CN109095468 A CN 109095468A CN 201711443962 A CN201711443962 A CN 201711443962A CN 109095468 A CN109095468 A CN 109095468A
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- hydrogen sulfide
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Abstract
The invention discloses a kind of methods for preparing carbon disulfide as raw material using hydrogen sulfide, and the mixed gas of natural gas and hydrogen sulfide is reacted under the action of new catalyst, generate carbon disulfide and hydrogen；By the mix products containing a small amount of hydrogen sulfide based on carbon disulfide, hydrogen and natural gas of generation by rectifying column I, carbon disulfide is condensed and separated；The isolated mix products boosting based on hydrogen, natural gas and hydrogen sulfide is entered into II compression rectification of rectifying column, hydrogen goes out from rectifying tower top part in gaseous form；Unreacted natural gas and the complete hydrogen sulfide of minute quantity unreacted are returned through delivery pump makees raw material use, realize circulation production process, raw material sources in the preparation method are wide, it is cheap, and reaction efficiency is high, low in the pollution of the environment, no industrial waste gas discharge, low energy consumption, good in economic efficiency, can continuous safe production.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a method of carbon disulfide is prepared by raw material of hydrogen sulfide.
Background technique
Carbon disulfide is a kind of important Inorganic Chemicals, widely used, is presently mainly used as solvent and as one
The raw material of a little fine chemical products synthesis is used for synthesizing dimethyl thioether as industrial chemicals, carbon tetrachloride, dimethyl sulfoxide,
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；As solvent, it is mainly used for viscose rayon, the synthesis of glassine paper and insoluble sulfuy, grease, wax, resin, rubber life
It produces；Carbon disulfide may further be used to manufacture pesticide, be used as insecticide and cereal fumigant.
With the rapid development of the industry such as China's chemistry, metallurgy, the purposes of carbon disulfide is more and more extensive, in order to adapt to this
Kind needs, and the carbon disulphide production in China is also evolving.Sulphur and charcoal, natural gas, propylene is widely used in the world at present
Carbon disulfide is produced Deng for raw material, gas-solid phase reaction and gas phase reaction two major classes can be divided by reactiveness.Gas-solid phase reaction is adopted
It is raw material with charcoal, makes that sulphur steam is quivered by the outer thermal response of fervid charcoal fixed bed or electric furnace, product are condensed, refined
Just carbon disulfide is obtained, though gas-solid phase reaction is simple and easy, significantly the disadvantage is that small scale, working condition difference intensity are big, the energy
Consumption is big, and production efficiency is low, at high cost, and consumes a large amount of forest reserves, and the three wastes environmental pollution generated in production process is tight
Again etc., belong to the production line being eliminated；Gas phase reaction refers to sulphur and carbon raw material, carries out under the conditions of being gaseous
Reaction, such as reacting for methane and sulfur vapor, propane, propylene belong to such with reacting for sulfur vapor.Natural gas act is domestic at present
Outer CS2Production produce family be widely used and state encourage process route.Compared with charcoal process, natural gas and Containing Sulfur are used
It closes object and prepares the reaction of carbon disulfide, have more research both at home and abroad, to natural gas and sulphur in patent US4078045
Use metal sulfide as catalyst preparation CS at high temperature2Detailed report has been carried out, but has been existed during the preparation process
The problem of conversion rate of products is not high, and conversion ratio can be reduced with catalyst using the growth of time, while carbonyl sulfur disproportionation life
It is reversible at the reaction of carbon disulfide and carbon dioxide, under normal operation more difficult positive progress.Therefore, it is necessary to using novel
Method around this expensive and inefficient limitation.
It is well known that hydrogen sulfide is the toxic gas discharged in natural gas and petroleum industry, therefore at desulfurization and hydrogen sulfide
Reason becomes technical process important in oil and natural gas industry.Current most common method is to use Crouse's recovery process,
Hydrogen sulfide partial oxidation is sulfur dioxide and reacts Recovered sulphur by catalysis, hydrogen is then oxidized to water and is wasted.Cause
A kind of low pressure of the reasonable exploitation of hydrogen sulfide waste gas and environmentally friendly carbon disulphide production technique are also a kind of reasons by this
The method for the recycling hydrogen sulfide thought, has great importance.
Summary of the invention
In order to overcome the deficiencies of the prior art, the present invention provides one kind and prepares carbon disulfide using hydrogen sulfide and natural gas as raw material
Method, the raw material sources in the preparation method are wide, cheap, and reaction efficiency is high, low in the pollution of the environment, no industrial waste gas
Discharge, low energy consumption, good in economic efficiency, can continuous safe production.
The purpose of the present invention is what is be achieved through the following technical solutions:
A method of carbon disulfide is prepared by raw material of hydrogen sulfide, which is characterized in that specifically includes the following steps:
A: by raw material natural gas and hydrogen sulfide gas after the pressurization of first gas compressor, the equal of natural gas and hydrogen sulfide is obtained
Even gaseous mixture, then introduce equipped with catalyst carbon disulfide synthetic tower in reacted, generate containing carbon disulfide, hydrogen,
The mix products of natural gas and a small amount of hydrogen sulfide, in unstripped gas natural gas to the molar ratio control of hydrogen sulfide gas in 2:1 or more,
Catalysis reaction is carried out at 0.01-1.8MPa, 400-1600 DEG C, and the catalyst is N0.1-2N* 0.01-1N** 0.01-2OXSY, N is extremely
It is that molybdenum, tungsten, iron are one such less, N*At least ruthenium, rhodium, silver, platinum, palladium, gold, rhenium, osmium, iridium are one such, N**At least
Vanadium, chromium, titanium, cobalt, nickel, copper are one such；The catalyst is the corresponding metal oxide of above-mentioned metallic element and vulcanization
Agent is reacted and is made, carrier A1203, Si02, Ti02, Zr02In any one or a few with arbitrary proportion mixing and
At；
B: the mix products of the carbon disulfide that generation is reacted in step a, hydrogen, natural gas and a small amount of hydrogen sulfide are passed through into rectifying column
I condenses and separates carbon disulfide, is discharged by rectifying column I tower bottom, pure CS can be obtained2Liquid product, tower top discharge gas phase then with
Based on hydrogen and natural gas, contain minimal amount of hydrogen sulfide；The condensing pressure of rectifying column I is controlled in 0.1-2.5 MPa in this step,
Condensation temperature controls the dew point in carbon disulfide hereinafter, carbon disulfide is promoted to be condensed into liquid.
C: by the mix products of the hydrogen, natural gas, hydrogen sulfide of the discharge of rectifying column I tower top in step b through second gas pressure
After the pressurization of contracting machine, into II compression rectification of rectifying column, pure hydrogen is discharged from tower top with gas phase, and the hydrogen of discharge burns
As institute's calorific requirement in carbon disulfide synthetic tower, natural gas is sent with the complete hydrogen sulfide of minute quantity unreacted through delivery pump again
Enter first gas compressor and make raw material use, continue to carry out reaction and rectifying again according to above-mentioned steps, to realize circulation production
Process.The operating pressure of rectifying column II is 1.0-3.5 MPa in above-mentioned steps c, and feeding manner can be gas phase, liquid phase or gas-liquid
Any one in mixed phase, the purpose that rectifying column II is added is separating degree in order to improve hydrogen and natural gas, hydrogen sulfide,
Obtain pure hydrogen.
Natural gas in the step a in unstripped gas is to choose the mixing that the molar content of methane and ethane is 90% or more
Gas, hydrogen sulfide are the industrial waste gases discharged in industrial production.
The present invention provides a kind of process flow by natural gas and hydrogen sulfide production carbon disulfide, innovation performances
: first is that industrial waste gas hydrogen sulfide is relatively efficiently utilized, and gas source is extensive by adjusting raw material and preparation method,
Carbon disulfide is directly prepared in lower pressure；Second is that rectifying column II is isolated with natural gas and pole by condensation and rectifying
A small amount of complete hydrogen sulfide of unreacted is returned through delivery pump makees raw material use, is reacted again according to above-mentioned steps, realizes former
Expect the circulation production process of gas；Third is that compression rectification means separating natural gas, hydrogen and carbon disulfide are used, carbon disulfide
Normal boiling point is 46.2 DEG C, and the boiling point of natural gas and hydrogen is then respectively -161.5~-88.6 DEG C and -257.8 DEG C, pressurization
The boiling point of fraction can be reduced, to significantly improve containing natural gas, the separative efficiency of the converted product of hydrogen and carbon disulfide
And operability；Fourth is that carbon disulfide synthetic tower can be carried out by using byproduct hydrogen gas full combustion obtained in production process
Energy supply, hydrogen not only realizes the Collaboration of technology room as a kind of clean new energy, the method, and realizes energy
It is reasonable using and environmental protection unification.
The process flow realizes the continuous circulation of entire production process, hence it is evident that the yield of carbon disulfide is improved, and
Reaction and separation process simply and readily operate, and the natural gas and a small amount of hydrogen sulfide after separation can be recycled, whole process
Without side reaction waste discharge, raw material availability is high；Industrial waste gas hydrogen sulfide can be efficiently used, avoids handling sulphur in claus oven
Change hydrogen exhaust gas and waste a large amount of manpower, material resources and financial resources, environment is effectively protected, embodies energy conservation and environment-friendly advantage.
Detailed description of the invention
Fig. 1 is the easy device of synthesis technology of the present invention.
In figure: 1- first gas compressor；2- carbon disulfide synthetic tower；3- catalyst；4- rectifying column I, 5- second gas
Compressor；6- rectifying column II；7- delivery pump.
Specific embodiment
Technical solutions according to the invention are clearly and completely described below in conjunction with embodiment, it is clear that described
Embodiment be only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, originally
Field those of ordinary skill every other embodiment obtained without creative efforts, belongs to the present invention
The range of protection.
A method of carbon disulfide being prepared by raw material of hydrogen sulfide, specifically includes the following steps:
A: the molar content of methane and ethane is chosen as 90% or more natural gas, collects the Industry Waste discharged in industrial production
Gas hydrogen sulfide obtains natural gas and hydrogen sulfide by raw material natural gas and hydrogen sulfide gas after the pressurization of first gas compressor 1
Homogeneous mixture, then introduce equipped with catalyst 3 carbon disulfide synthetic tower 2 in reacted, generate containing carbon disulfide,
The mix products of hydrogen, natural gas and a small amount of hydrogen sulfide, natural gas controls in 2:1 the molar ratio of hydrogen sulfide gas in unstripped gas
More than, catalysis reaction is carried out at 0.01-1.8MPa, 400-1600 DEG C, and the catalyst is N0.1-2N* 0.01-1N** 0.01- 2OXSY, it is one such that N is at least molybdenum, tungsten, iron, N*At least ruthenium, rhodium, silver, platinum, palladium, gold, rhenium, osmium, iridium are one such,
N**At least vanadium, chromium, titanium, cobalt, nickel, copper are one such；The catalyst is the corresponding metal oxidation of above-mentioned metallic element
Object is reacted with vulcanizing agent and is made, carrier A1203, Si02, Ti02, Zr02In any one or a few arbitrarily to compare
Example mixes；In the specific implementation, metallic element N is iron, N*For silver, N**For copper, the oxide and sulphur of these metallic elements
Agent, which is reacted, is made catalyst Fe2AgCuO7S, in addition carrier is Si02, catalyst is Fe2AgCuO7S/Si02。
B: the mix products of the carbon disulfide that generation is reacted in step a, hydrogen, natural gas and a small amount of hydrogen sulfide are passed through into essence
Tower I4 is evaporated, carbon disulfide is condensed and separated, is discharged by rectifying column I4 tower bottom, pure CS can be obtained2Liquid product, the gas of tower top discharge
Phase then based on hydrogen and natural gas, contains minimal amount of hydrogen sulfide；The condensing pressure of rectifying column I is controlled in 0.1- in this step
2.5 MPa, condensation temperature control the dew point in carbon disulfide hereinafter, carbon disulfide is promoted to be condensed into liquid.
C: by the mix products of the hydrogen, natural gas, hydrogen sulfide of the discharge of rectifying column I tower top in step b through second gas pressure
After contracting machine 5 pressurizes, into II 6 compression rectification of rectifying column, pure hydrogen is discharged from tower top with gas phase, and the hydrogen of discharge is fired
Burning can be used as institute's calorific requirement in carbon disulfide synthetic tower, at this time by natural gas with the complete hydrogen sulfide of minute quantity unreacted through conveying
Pump 7 is re-fed into first gas compressor and makees raw material use, continues to carry out reaction and rectifying again according to above-mentioned steps, to realize
Recycle production process.The operating pressure of rectifying column II is 1.0-3.5 MPa in above-mentioned steps c, and feeding manner can be gas phase, liquid
Mutually or gas-liquid mixed phase in any one, be added rectifying column II purpose be to improve hydrogen and natural gas, hydrogen sulfide
Separating degree, obtain pure hydrogen.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Content of the invention can be understood and implemented accordingly, it is not intended to limit the scope of the present invention, all according to this hair
Equivalent change or modification made by bright Spirit Essence, is all included within the scope of the present invention.
Claims (3)
1. a kind of method for preparing carbon disulfide as raw material using hydrogen sulfide, which is characterized in that specifically includes the following steps:
A: by raw material natural gas and hydrogen sulfide gas after the pressurization of first gas compressor, the equal of natural gas and hydrogen sulfide is obtained
Then even gaseous mixture is introduced in the carbon disulfide synthetic tower equipped with catalyst and is reacted, which reacts in 0.01-
It is carried out at 1.8MPa, 400-1600 DEG C, generates the mix products containing carbon disulfide, hydrogen, natural gas and a small amount of hydrogen sulfide, it is former
Expect that natural gas controls in 2:1 or more the molar ratio of hydrogen sulfide gas in gas；
B: the mix products of the carbon disulfide that generation is reacted in step a, hydrogen, natural gas and a small amount of hydrogen sulfide are passed through into rectifying column
I condenses and separates carbon disulfide, is discharged by rectifying column I tower bottom, pure CS can be obtained2Liquid product, tower top discharge gas phase then with
Based on hydrogen and natural gas, contain minimal amount of hydrogen sulfide；The condensing pressure of rectifying column I is controlled in 0.1-2.5 MPa in this step,
Condensation temperature controls the dew point in carbon disulfide hereinafter, carbon disulfide is promoted to be condensed into liquid；
C: by the mix products of the hydrogen, natural gas, hydrogen sulfide of the discharge of rectifying column I tower top in step b through second gas compressor
After pressurization, into II compression rectification of rectifying column, pure hydrogen is discharged from tower top with gas phase, and the hydrogen of discharge carries out burning conduct
Natural gas and the complete hydrogen sulfide of minute quantity unreacted are re-fed into the through delivery pump by institute's calorific requirement in carbon disulfide synthetic tower
One gas compressor makees raw material use, continues to carry out reaction and rectifying again according to above-mentioned steps, to realize circulation production process,
The operating pressure of rectifying column II is 1.0-3.5 MPa in this step c, and feeding manner is in gas phase, liquid phase or gas-liquid mixed phase
Any one.
2. a kind of method for preparing carbon disulfide as raw material using hydrogen sulfide according to claim 1, which is characterized in that described
Catalyst in step a is N0.1-2N* 0.01-1N** 0.01-2OXSY, it is one such that N is at least molybdenum, tungsten, iron, N*At least ruthenium, rhodium,
Silver, platinum, palladium, gold, rhenium, osmium, iridium are one such, N**At least vanadium, chromium, titanium, cobalt, nickel, copper are one such；The catalyst
It reacts and is made with vulcanizing agent for the corresponding metal oxide of above-mentioned metallic element, carrier A1203, Si02, Ti02, Zr02
In any one or a few be mixed in any proportion.
3. a kind of method for preparing carbon disulfide as raw material using hydrogen sulfide according to claim 1, which is characterized in that described
Natural gas in step a in unstripped gas is to choose the gaseous mixture that the molar content of methane and ethane is 90% or more, and hydrogen sulfide is work
The industrial waste gas discharged in industry production.
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Cited By (3)
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| CN111265969A (en) * | 2020-03-20 | 2020-06-12 | 鹤壁市恒力橡塑股份有限公司 | Method for efficiently recovering carbon disulfide from tail gas |
| CN113428861A (en) * | 2021-07-19 | 2021-09-24 | 华东理工大学 | Methane and hydrogen sulfide reforming hydrogen production process |
| EP4101815A1 (en) * | 2021-06-10 | 2022-12-14 | Evonik Operations GmbH | Hydrogen sulfide reforming of hydrocarbons |
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| CN111265969A (en) * | 2020-03-20 | 2020-06-12 | 鹤壁市恒力橡塑股份有限公司 | Method for efficiently recovering carbon disulfide from tail gas |
| EP4101815A1 (en) * | 2021-06-10 | 2022-12-14 | Evonik Operations GmbH | Hydrogen sulfide reforming of hydrocarbons |
| CN113428861A (en) * | 2021-07-19 | 2021-09-24 | 华东理工大学 | Methane and hydrogen sulfide reforming hydrogen production process |
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Application publication date: 20181228 |