CN113149803A - High-efficiency removing process for high-grade alkyne in acetylene-containing cracking gas - Google Patents
High-efficiency removing process for high-grade alkyne in acetylene-containing cracking gas Download PDFInfo
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Abstract
The invention discloses a high-efficiency removing process of high-grade alkyne in acetylene-containing pyrolysis gas, belonging to the technical field of acetylene preparation. The invention relates to a high-efficiency removing process of high-grade alkyne in acetylene-containing pyrolysis gas, which comprises the steps of compressing and cooling the pyrolysis gas, then feeding the pyrolysis gas into a pre-heavy removal tower, removing part of high-grade alkyne by using a first solvent, then compressing and cooling the pyrolysis gas, feeding the pyrolysis gas into a main heavy removal tower, and removing all high-grade alkyne by using a second solvent. The invention has scientific design and ingenious conception, improves the pressure of the cracking gas through sectional compression, avoids the safety risk caused by overhigh gas temperature in the compression process of the cracking gas, efficiently and completely removes the diacetylene in the heavy component removal section, avoids the diacetylene from entering an acetylene product working section, and effectively improves the purity of the acetylene product.
Description
Technical Field
The invention belongs to the technical field of acetylene preparation, and particularly relates to a high-efficiency removing process of high-grade alkyne in acetylene-containing pyrolysis gas.
Background
Acetylene is an important raw material in organic chemistry industry and is widely applied to the production of chemicals such as 1, 4-butanediol, chloroethylene, acetylene black, chloroprene rubber, butanediol, butynediol, tetrahydrofuran, cyclooctatetraene and the like. The acetylene production process includes calcium carbide process, natural gas partial oxidation process, electric arc process and plasma cracking process.
The calcium carbide method is the earliest method for synthesizing acetylene and is also the method with the highest technical maturity. The method needs to build a huge calcium carbide furnace, has high energy consumption, high water consumption and high pollution, 30-60 t of water is consumed for producing 1t of acetylene, 2.6t of calcium carbide waste residues are generated, and the calcium carbide waste residues are difficult to treat, so that huge environmental protection pressure is caused to the environment of the location of an enterprise. At present, the acetylene production technology by the calcium carbide method in developed countries is replaced by the technology for producing acetylene by partial oxidation of natural gas. But over 95 percent of acetylene production capacity in China still comes from a calcium carbide method, and only a small amount of acetylene is produced by a natural gas oxidation method.
The natural gas partial oxidation method is superior to the calcium carbide method in environmental protection, but has own disadvantages. The partial oxidation method of natural gas has oxygen to participate in the reaction, and the generated cracked gas contains a large amount of CO and H2And a methanol synthesis device needs to be constructed in a matched manner, so that the process flow is increased. Due to the existence of oxygen, explosion-proof equipment is required to be added, the cost of separation and purification is increased, and the cost is increased.
The method for preparing acetylene by cracking natural gas with plasma has the characteristics of low investment, low production cost, high utilization rate of raw materials, easy separation of cracked gas, simple process flow, safe and reliable production, no environmental pollution and the like, and is superior to the existing calcium carbide method, natural gas arc cracking method and partial oxidation method in technical and economic aspects. The natural gas partial oxidation method needs to consume 6000m for producing 1t of acetylene3Natural gas, whereas the plasma cracking process requires only about 2000m3The utilization rate of the raw materials of the natural gas is higher. In ChinaIn addition, research on preparing acetylene by plasma cracking has been carried out in the United states and Germany, and a 3000t/a industrial device for preparing acetylene by natural gas plasma is built by the German ISP company. The research work of the device and the process for preparing acetylene by plasma cracking has been carried out by the national institute of Chinese institute of Oken, Sichuan university, Qinghua university and the national institute of metals, but no device which can realize industrialization in the whole process exists in China.
The natural gas partial oxidation method is to crack natural gas at 1500 deg.c in oxygen to produce cracked gas containing acetylene. The technology for preparing acetylene by cracking methane-rich gas with plasma is to utilize methane to form plasma in a high-voltage reactor, and then to chill to form cracking gas containing acetylene. The cracked gas formed by the two process technologies is subjected to the processes of carbon black removal, washing and the like to remove substances such as carbon black, tar and the like in the cracked gas, the cracked gas mainly contains acetylene, methane, hydrogen, nitrogen, diacetylene and the like, and the cracked gas obtained by the natural gas partial oxidation method also contains a large amount of carbon monoxide. The purified cracking gas is pressurized by a compressor and enters an acetylene concentration process, and the high-grade alkyne and the non-condensable gas, namely methane, hydrogen, carbon monoxide, nitrogen and acetylene, are sequentially removed by utilizing the different solubility in a solvent, so that the high-purity acetylene product gas is finally obtained.
Diacetylene belongs to gas with very active properties, is easy to polymerize and is easy to decompose and explode at high temperature and high pressure, in industry, the partial pressure of diacetylene is limited to be not more than 20kPa due to safety considerations, the compression process of cracking gas is not more than 1.2MPa, and because the pressure is low, higher alkynes such as diacetylene cannot be completely removed in the de-heavy process, the higher alkynes can enter the following process along with acetylene, the separation difficulty of the later section is increased, so that a small amount of higher alkynes can be generated in acetylene products, the quality of acetylene is influenced, and more byproducts are brought to the production process of acetylene downstream products. Therefore, the method is provided, which improves the compression pressure of the cracking gas under the condition that the safe partial pressure of the diacetylene is not exceeded, increases the removal efficiency of the higher alkynes such as diacetylene in the process of removing heavy components, prevents the higher alkynes such as diacetylene from entering a later stage process, and improves the purity of the acetylene product, and the method becomes a problem to be solved by technical personnel in the field.
Disclosure of Invention
The invention aims to provide a process for efficiently removing high-grade alkyne in acetylene-containing cracking gas, which can efficiently and completely remove diacetylene in a heavy removal section on the premise of ensuring the process safety, prevent diacetylene from entering an acetylene product working section and effectively improve the purity of acetylene product.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention relates to a high-efficiency removing process of high-grade alkyne in acetylene-containing pyrolysis gas, wherein the pyrolysis gas enters a pre-heavy removal tower after being compressed and cooled, a part of high-grade alkyne is removed by a first solvent, then the pyrolysis gas enters a main heavy removal tower after being compressed and cooled, and all high-grade alkyne is removed by a second solvent.
In some embodiments of the present invention, the cracked gas is decompressed and cooled after carbon black and tar are removed, and then enters a pre-de-weighting tower.
In some embodiments of the invention, the cracked gas is compressed and cooled at least twice before entering the pre-de-weighting column.
In some embodiments of the present invention, the cracked gas from which some of the higher acetylenes are removed in the pre-de-heaving column is compressed and cooled at least twice before entering the main de-heaving column.
The pyrolysis gas contains part of water vapor even after being purified, and the invention compresses and cools the pyrolysis gas at least twice before entering the pre-de-weighting tower and at least twice before entering the main de-weighting tower so as to gradually condense and separate the water vapor in the pyrolysis gas, thereby avoiding a large amount of water vapor from entering the absorption solvent of the main de-weighting tower to influence the absorption effect. In addition, the cracked gas is divided into at least four sections of compression processes, so that the over-high temperature of the cracked gas in the compression process can be avoided. Because the cracking gas contains a large amount of acetylene and a small amount of higher alkyne such as diacetylene, the alkyne is active in property, particularly the higher alkyne is easy to decompose and explode at high temperature and high pressure, and the gas temperature in the compression process needs to be limited to be lower than 110 ℃. Therefore, the invention cools the cracked gas after each compression and then enters the next stage of compression process. The cracked gas after at least two times of compression and cooling enters a pre-de-weighting tower, and a part of higher alkyne such as butyne and the like is absorbed by utilizing a first solvent so as to reduce the content of the higher alkyne in the cracked gas, so that the condition that the content of the higher alkyne in the cracked gas is close to or exceeds the safe partial pressure limit of 20kPa after subsequent compression is avoided, and the risk is reduced. After at least four times of compression, the pressure of the cracking gas reaches about 2.0 MPa. Under the pressure, the solvent has good absorption effect on the high-grade alkyne, the high-grade alkyne such as diacetylene, vinyl acetylene and propyne with high risk can be completely removed, the separation difficulty of the rear section is reduced, the high-grade alkyne is prevented from entering an acetylene product, the purity of the acetylene product is improved, and the use effect of the acetylene downstream product is enhanced.
In some embodiments of the present invention, the cracked gas from which the carbon black and tar are removed mainly contains acetylene, hydrogen, nitrogen, carbon monoxide, methane, diacetylene, ethylene, propyne, propadiene, vinylacetylene, butadiene, and the like.
In some embodiments of the invention, the method comprises the following steps:
s1, after being compressed by a first-stage compressor, pyrolysis gas from which carbon black and tar are removed enters a first cooler for cooling, water vapor carried in the pyrolysis gas is condensed into liquid water to be discharged, the pyrolysis gas cooled by the first cooler enters a second-stage compressor for secondary compression and then enters a second cooler for cooling, the condensed liquid is discharged, and the pyrolysis gas cooled by the second cooler enters a pre-de-weighting tower from the lower end of the tower;
s2, the cracking gas entering the pre-heavy-component removal tower is sprayed downwards from bottom to top, the first solvent is sprayed downwards from the top of the pre-heavy-component removal tower, and the high-grade alkyne in the cracking gas can be partially absorbed by the first solvent; the first solvent absorbing the gas is removed to the later stage process, and the pyrolysis gas with part of the higher alkyne removed is discharged from the top of the pre-de-weighting tower;
s3, sequentially compressing the cracked gas discharged from the top of the pre-de-weighting tower by a three-stage compressor, cooling by a third cooler, compressing by a four-stage compressor, cooling by a fourth cooler, and then entering a main de-weighting tower from the lower end of the tower;
s4, the cracking gas entering the main de-weighting tower is sprayed downwards from bottom to top, the second solvent is sprayed downwards from the top of the main de-weighting tower, and all high-grade alkyne in the cracking gas is absorbed by the second solvent; the second solvent absorbing the gas is sent to the subsequent process, and the gas without the high-grade alkyne is discharged from the top of the main de-heavy tower.
In some embodiments of the present invention, the following gases are present in the pyrolysis gas in a volume ratio of: 3 to 11% of acetylene, 0.03 to 1.2% of diacetylene, 0.05 to 0.8% of propyne, 0.01 to 0.2% of vinyl acetylene and 0.001 to 0.02% of butadiene.
In some embodiments of the invention, the gas pressure after being compressed by the first-stage compressor is 0.20-0.28 MPa;
or/and the pressure of the gas compressed by the two-stage compressor is 0.40-0.56 MPa;
or/and the gas pressure after being compressed by the three-stage compressor is 0.80-1.12 MPa;
or/and the pressure of the gas compressed by the four-stage compressor is 1.60-2.24 MPa;
or/and the temperature of the pyrolysis gas cooled by the first cooler, the second cooler, the third cooler and the fourth cooler is 5-25 ℃.
In some embodiments of the present invention, the first solvent and the second solvent each comprise at least one of N-methylpyrrolidone, kerosene, nitroformamide, and ammonia.
In some embodiments of the invention, the solvent absorption temperature of the pre-de-heavy tower and the main de-heavy tower is 10-25 ℃.
In some embodiments of the invention, the pre-de-heaving column and the main de-heaving column are plate columns or packed columns.
Compared with the prior art, the invention has the following beneficial effects:
the invention has scientific design and ingenious conception, improves the pressure of the cracking gas through sectional compression, avoids the safety risk caused by overhigh gas temperature in the compression process of the cracking gas, simultaneously absorbs the high-grade alkyne part in the gas through the pre-de-weighting tower under lower pressure, reduces the content of the high-grade alkyne in the gas, avoids the decomposition and explosion risk caused by the partial pressure of the high-grade alkyne approaching or exceeding 20kPa when the three-section and the four-section are compressed to high pressure, and achieves more efficient absorption of the high-grade alkyne by the solvent under high pressure. In the technical scheme of the invention, under the condition of 1.60-2.24 MPa, the absorption rate of the solvent to higher acetylene hydrocarbon diacetylene, propyne and vinyl acetylene can reach 100%, the difficulty in the separation process of the acetylene at the later stage is reduced, and the purity of the acetylene product is improved.
Drawings
FIG. 1 is a schematic diagram of a process flow for removing high-grade alkyne from acetylene-containing pyrolysis gas.
Wherein, the names corresponding to the reference numbers are:
1-first-stage compressor, 2-first cooler, 3-second-stage compressor, 4-second cooler, 5-pre-heavy-removing tower, 6-third-stage compressor, 7-third cooler, 8-fourth-stage compressor, 9-fourth cooler and 10-main heavy-removing tower.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The process flow of this embodiment is shown in fig. 1, and the volume contents of the following gases in the cracked gas purified in this embodiment are: acetylene 3%, diacetylene 0.5%, propyne 0.3%, vinylacetylene 0.2%, butadiene 0.001%, hydrogen 60%, carbon monoxide 30%, nitrogen 5%, ethylene 0.7%, propadiene 0.1%.
Cracked gas enters a first-stage compressor 1 to be compressed to 0.2MPa, the compressed gas is cooled to 5 ℃ through a first cooler 2, condensate obtained by cooling is discharged to a wastewater treatment system, the cooled gas enters a second-stage compressor 3 to be compressed to 0.4MPa, and then enters a second cooler 4 to be cooled to 5 ℃. The condensate obtained by cooling through the second cooler 4 enters a wastewater treatment system, and the gas cooled through the second cooler 4 enters the pre-heavy-component removal tower 5 from the lower end of the tower.
The tower top of the pre-heavy removal tower 5 is sprayed and absorbed by N-methylpyrrolidone (NMP) at the temperature of 10 ℃, the content of the high-grade alkyne in the absorbed gas is reduced by 31 percent, and the pre-heavy removal tower 5 is a plate tower. A latter step of removing NMP having absorbed the gas; the cracking gas without part of high alkyne is discharged from the top of the pre-de-heavy tower.
The gas from the top of the pre-de-heavy tower 5 enters a three-stage compressor 6 to be compressed to 0.8MPa, and the compressed gas is cooled to 5 ℃ through a third cooler 7. The condensate obtained by cooling through the third cooler 7 enters a wastewater treatment system, and the gas cooled through the third cooler 7 enters a four-section compressor 8 to be compressed to 1.6 MPa. The compressed gas is cooled to 5 c by a fourth cooler 9. The condensate obtained by cooling through the third cooler 9 enters a wastewater treatment system, and the gas cooled through the third cooler 9 enters the main de-weighting tower 10 from the lower end thereof.
Spraying and absorbing NMP at 10 ℃ at the top of the main de-heavy tower 10, and removing NMP absorbing gas in the later stage; the content of higher alkynes such as diacetylene, vinyl acetylene, propyne, allene and the like in the gas from the top of the main de-heavy tower 10 is reduced to 0.00 percent, and the higher alkynes in the cracked gas are all absorbed by the solvent. Acetylene-containing gas from the top of the main de-heavy tower passes through the acetylene absorption and desorption process of the later section, and the obtained acetylene product contains a small amount of ethylene and does not contain higher alkynes such as diacetylene, vinyl acetylene, propyne, allene and the like.
Example 2
The process flow of this embodiment is shown in fig. 1, and the volume contents of the following gases in the cracked gas purified in this embodiment are: 11% of acetylene, 0.5% of diacetylene, 0.8% of propyne, 0.2% of vinylacetylene, 0.02% of butadiene content, 80% of hydrogen, 2% of carbon monoxide, 5% of nitrogen, 0.3% of ethylene and 0.18% of propadiene.
Cracked gas enters a first-stage compressor 1 to be compressed to 0.28MPa, the compressed gas is cooled to 25 ℃ through a first cooler 2, condensate obtained by cooling is discharged to a wastewater treatment system, the cooled gas enters a second-stage compressor 3 to be compressed to 0.56MPa, and then enters a second cooler 4 to be cooled to 25 ℃. The condensate obtained by cooling through the second cooler 4 enters a wastewater treatment system, and the gas cooled through the second cooler 4 enters the pre-heavy-component removal tower 5 from the lower end of the tower.
The tower top of the pre-heavy removal tower 5 is sprayed and absorbed by kerosene with the temperature of 25 ℃, the content of the high-grade alkyne in the absorbed gas is reduced by 35 percent, and the pre-heavy removal tower 5 is a plate tower. The kerosene absorbed with gas goes to the back-end process; the cracking gas without part of high alkyne is discharged from the top of the pre-de-heavy tower.
The gas from the top of the pre-de-heavy tower 5 enters a three-stage compressor 6 to be compressed to 1.12MPa, and the compressed gas is cooled to 25 ℃ through a third cooler 7. The condensate obtained by cooling through the third cooler 7 enters a wastewater treatment system, and the gas cooled through the third cooler 7 enters a four-section compressor 8 to be compressed to 2.24 MPa. The compressed gas is cooled to 25 c by a fourth cooler 9. The condensate obtained by cooling through the third cooler 9 enters a wastewater treatment system, and the gas cooled through the third cooler 9 enters the main de-weighting tower 10 from the lower end thereof.
Spraying and absorbing kerosene at 25 ℃ at the top of a main de-weighting tower 10, and removing the kerosene absorbing gas to a later stage process; the content of higher alkynes such as diacetylene, vinyl acetylene, propyne, allene and the like in the gas from the top of the main de-heavy tower 10 is reduced to 0.00 percent, and the higher alkynes in the cracked gas are all absorbed by the solvent. Acetylene-containing gas from the top of the main de-heavy tower passes through the acetylene absorption and desorption process of the later section, and the obtained acetylene product contains a small amount of ethylene and does not contain higher alkynes such as diacetylene, vinyl acetylene, propyne, allene and the like.
Comparative example 1
Compared with the embodiment 1, the gas cooled by the second cooler 4 directly enters the three-stage compressor 6 to be compressed to 0.8MPa, and does not enter the pre-de-weighting tower 5 and is sprayed and absorbed by NMP, and the rest conditions are the same.
In this comparative example, the content of higher alkynes such as diacetylene, vinyl acetylene, propyne, propadiene in the gas from the top of the main de-weighting column 10 was reduced to 0.3%, and the acetylene-containing gas from the top of the main de-weighting column was subjected to the acetylene absorption and desorption processes at the subsequent stage to obtain an acetylene product containing a small amount of ethylene and higher alkynes such as diacetylene, vinyl acetylene, propyne, propadiene. Wherein the volume content of the propadiene in the acetylene product exceeds 0.5%. Because part of the higher alkyne is not removed in advance through the pre-de-heavy tower 5, when the gas is compressed to 1.6MPa, the partial pressure of the higher alkyne in the compressed gas reaches 17.6kpa, which is very close to the safe partial pressure of the higher alkyne of 20kpa, and the safety risk is increased.
Finally, it should be noted that: the above embodiments are only preferred embodiments of the present invention to illustrate the technical solutions of the present invention, but not to limit the technical solutions, and certainly not to limit the patent scope of the present invention; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention; that is, the technical problems to be solved by the present invention, which are not substantially changed or supplemented by the spirit and the concept of the main body of the present invention, are still consistent with the present invention and shall be included in the scope of the present invention; in addition, the technical scheme of the invention is directly or indirectly applied to other related technical fields, and the technical scheme is included in the patent protection scope of the invention.
Claims (10)
1. A process for efficiently removing high-grade alkyne from acetylene-containing cracked gas is characterized in that the cracked gas enters a pre-heavy removal tower after being compressed and cooled, a part of high-grade alkyne is removed by a first solvent, then the cracked gas enters a main heavy removal tower after being compressed and cooled, and all high-grade alkyne is removed by a second solvent.
2. The process for efficiently removing high-grade alkyne in acetylene-containing pyrolysis gas as claimed in claim 1, wherein the pyrolysis gas is subjected to carbon black and tar removal, then is compressed and cooled, and enters a pre-de-weighting tower.
3. The process for efficiently removing high-grade alkynes in acetylene-containing pyrolysis gas as claimed in claim 1, wherein the pyrolysis gas is compressed and cooled at least twice before entering the pre-de-weighting tower.
4. The process for efficiently removing higher alkynes from acetylene-containing cracked gas according to claim 1, characterized in that the cracked gas from which part of the higher alkynes are removed by the pre-de-heaving tower is compressed and cooled at least twice before entering the main de-heaving tower.
5. The process for efficiently removing high-grade alkyne in acetylene-containing pyrolysis gas according to any one of claims 1 to 4, characterized by comprising the following steps:
s1, after being compressed by a first-stage compressor, pyrolysis gas from which carbon black and tar are removed enters a first cooler for cooling, water vapor carried in the pyrolysis gas is condensed into liquid water to be discharged, the pyrolysis gas cooled by the first cooler enters a second-stage compressor for secondary compression and then enters a second cooler for cooling, the condensed liquid is discharged, and the pyrolysis gas cooled by the second cooler enters a pre-de-weighting tower from the lower end of the tower;
s2, the cracking gas entering the pre-heavy-component removal tower is sprayed downwards from bottom to top, the first solvent is sprayed downwards from the top of the pre-heavy-component removal tower, and the high-grade alkyne in the cracking gas can be partially absorbed by the first solvent; the first solvent absorbing the gas is removed to the later stage process, and the pyrolysis gas with part of the higher alkyne removed is discharged from the top of the pre-de-weighting tower;
s3, sequentially compressing the cracked gas discharged from the top of the pre-de-weighting tower by a three-stage compressor, cooling by a third cooler, compressing by a four-stage compressor, cooling by a fourth cooler, and then entering a main de-weighting tower from the lower end of the tower;
s4, the cracking gas entering the main de-weighting tower is sprayed downwards from bottom to top, the second solvent is sprayed downwards from the top of the main de-weighting tower, and all high-grade alkyne in the cracking gas is absorbed by the second solvent; the second solvent absorbing the gas is sent to the subsequent process, and the gas without the high-grade alkyne is discharged from the top of the main de-heavy tower.
6. The process for efficiently removing high-grade alkyne in acetylene-containing pyrolysis gas according to claim 5, wherein the pyrolysis gas contains the following gases by volume: 3 to 11% of acetylene, 0.03 to 1.2% of diacetylene, 0.05 to 0.8% of propyne, 0.01 to 0.2% of vinyl acetylene and 0.001 to 0.02% of butadiene.
7. The process for efficiently removing high-grade alkyne in acetylene-containing cracking gas according to claim 5, wherein the gas pressure after being compressed by a section of compressor is 0.20-0.28 MPa;
or/and the pressure of the gas compressed by the two-stage compressor is 0.40-0.56 MPa;
or/and the gas pressure after being compressed by the three-stage compressor is 0.80-1.12 MPa;
or/and the pressure of the gas compressed by the four-stage compressor is 1.60-2.24 MPa;
or/and the temperature of the pyrolysis gas cooled by the first cooler, the second cooler, the third cooler and the fourth cooler is 5-25 ℃.
8. The process for efficiently removing high-grade alkynes in acetylene-containing cracking gas according to claim 5, wherein the first solvent and the second solvent respectively comprise at least one of N-methylpyrrolidone, kerosene, nitroformamide and ammonia water.
9. The process for efficiently removing high-grade alkyne in acetylene-containing pyrolysis gas as claimed in claim 5, wherein the solvent absorption temperature of the pre-de-heavy tower and the main de-heavy tower is 10-25 ℃.
10. The process for efficiently removing high-grade alkynes in acetylene-containing cracking gas according to claim 1, wherein the pre-heavy removal tower and the main heavy removal tower are plate towers or packed towers.
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