CN115259989A - Preparation method of electronic-grade acetylene - Google Patents
Preparation method of electronic-grade acetylene Download PDFInfo
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- CN115259989A CN115259989A CN202211041416.9A CN202211041416A CN115259989A CN 115259989 A CN115259989 A CN 115259989A CN 202211041416 A CN202211041416 A CN 202211041416A CN 115259989 A CN115259989 A CN 115259989A
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- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
- C07C7/14858—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound with inorganic compounds not provided for before
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- C—CHEMISTRY; METALLURGY
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- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
- C07C7/13—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers by molecular-sieve technique
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Abstract
The invention provides a preparation method of electronic-grade acetylene, which comprises the following steps: the method comprises the steps of introducing acetylene raw material gas into a dehydration tank to remove part of water to obtain an acetylene raw material crude product, introducing into a first-stage adsorption tower with a molecular sieve as a filler to remove impurities for the first time to obtain a first-stage acetylene crude product, introducing into a second-stage adsorption tower with a coal activated carbon adsorbent to remove impurities for the second time to obtain a second-stage acetylene crude product, introducing into a third-stage adsorption tower with an alumina adsorbent to remove impurities for the third time to obtain an acetylene fine product, filtering particles through a filter, introducing into a buffer tank, pressurizing through a compressor, and filling to obtain electronic-grade acetylene. The method can improve the purity of acetylene products, shorten the purification route and realize the preparation and purification of high-purity acetylene electronic gas in industrial scale production.
Description
Technical Field
The invention belongs to the technical field of electronic-grade acetylene, and particularly relates to a preparation method of electronic-grade acetylene.
Background
Acetylene is an important industrial product, along with the rapid development of the semiconductor industry, the application of high-purity acetylene in the semiconductor industry is more and more emphasized, and the acetylene with higher purity can be used for preparing a carbon mask in the photoetching technology in the manufacturing of large-scale integrated circuits. In addition, by the plasma enhanced chemical vapor deposition process, high-purity acetylene can form a stable carbon layer structure on the surface of a silicon material, and a carbon mask for a photoetching process can be constructed, wherein the carbon mask is an important raw material for producing logic devices, memory devices, panel devices and photoetching devices.
Acetylene is generally prepared by cracking calcium carbide or natural gas in industry, impurities in acetylene raw gas generally comprise phosphine, arsine, hydrogen sulfide, water, part of higher alkynes (propadiene, propyne, butadiene, vinyl acetylene) and the like, and a traditional method generally adopts a concentrated sulfuric acid absorption method, so that the method is strong in corrosivity, high in operation cost and serious in environmental pollution.
Therefore, the improvement of the purity of acetylene products, the shortening of purification routes and the industrial scale production are problems to be solved in the research of the preparation and purification of high-purity acetylene electronic gases.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for preparing electronic-grade acetylene, aiming at the defects of the prior art, the method can improve the purity of acetylene products, shorten a purification route, and realize industrial scale production, namely preparation and purification of high-purity acetylene electronic gas.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a method for preparing electronic-grade acetylene, which comprises the following steps:
s1, introducing acetylene raw material gas from a steel cylinder into a dehydration tank, and removing partial water under the conditions that the temperature is 15-25 ℃ and the pressure is 0.1-0.15 MPa to obtain an acetylene raw material crude product;
s2, introducing the crude acetylene raw material obtained in the S1 into a primary adsorption tower, and performing primary impurity removal under the conditions that the temperature is 15-25 ℃ and the pressure is 0.1-0.15 MPa to obtain a primary crude acetylene product; the filler of the first-stage adsorption tower is a molecular sieve;
s3, introducing the primary acetylene crude product obtained in the S2 into a secondary adsorption tower, and performing secondary impurity removal under the conditions that the temperature is 15-25 ℃ and the pressure is 0.1-0.15 MPa to obtain a secondary acetylene crude product; the filler of the secondary adsorption tower is a coal activated carbon adsorbent;
s4, introducing the secondary acetylene crude product obtained in the step S3 into a three-stage adsorption tower, and performing third impurity removal under the conditions that the temperature is 15-25 ℃ and the pressure is 0.1-0.15 MPa to obtain an acetylene fine product; the filler of the three-stage adsorption tower is an alumina adsorbent;
and S5, filtering particles of the fine acetylene product obtained in the S4 through a filter, introducing the fine acetylene product into a buffer tank with the pressure of 0.1-0.15 MPa, pressurizing the fine acetylene product to 2.0-3.0 MPa through a compressor, and filling the fine acetylene product to obtain the electronic-grade acetylene.
Preferably, the filler of the dehydration tank in S1 is calcium carbide or silicon tetrachloride.
Preferably, the impurities removed in the first impurity removal in S2 include water and carbon dioxide.
Preferably, the packing of the first-stage adsorption tower in S2 is a 4A molecular sieve or a 5A molecular sieve.
Preferably, the impurities removed in the second impurity removal in S3 comprise arsine, phosphine and hydrogen sulfide.
Preferably, the impurities of said third impurity removal in S4 comprise olefinic impurities.
Preferably, the olefinic impurities include propadiene, propyne, butadiene, vinylacetylene.
Preferably, the pore size of the filter in S5 is 0.1 μm.
Preferably, the purity of the acetylene raw material gas in S1 is more than or equal to 99.5%.
Preferably, the purity of the electronic-grade acetylene in S5 is more than or equal to 99.98%.
Compared with the prior art, the invention has the following advantages:
the method can improve the purity of acetylene products, shorten the purification route and realize the preparation and purification of high-purity acetylene electronic gas in industrial scale production.
The present invention will be described in further detail with reference to examples.
Detailed Description
Example 1
The preparation method of the electronic-grade acetylene of the embodiment comprises the following steps:
s1, introducing acetylene raw material gas from a steel cylinder into a dehydration tank, and removing partial water under the conditions that the temperature is 20 ℃ and the pressure is 0.12MPa to obtain an acetylene raw material crude product; the filler of the dehydration tank is silicon tetrachloride;
the purity of the acetylene feed gas in this example was 95%;
s2, introducing the acetylene raw material crude product obtained in the S1 into a primary adsorption tower, and performing primary impurity removal under the conditions that the temperature is 20 ℃ and the pressure is 0.12MPa to obtain a primary acetylene crude product; the filler of the first-stage adsorption tower is a 4A molecular sieve; the impurities removed by the first impurity removal comprise water and carbon dioxide;
s3, introducing the primary acetylene crude product obtained in the S2 into a secondary adsorption tower, and performing secondary impurity removal under the conditions that the temperature is 20 ℃ and the pressure is 0.12MPa to obtain a secondary acetylene crude product; the filler of the secondary adsorption tower is a coal activated carbon adsorbent; the impurities removed by the second impurity removal comprise arsine, phosphine and hydrogen sulfide;
s4, introducing the secondary acetylene crude product obtained in the S3 into a three-stage adsorption tower, and performing third impurity removal under the conditions that the temperature is 20 ℃ and the pressure is 0.12MPa to obtain an acetylene fine product; the filler of the three-stage adsorption tower is an alumina adsorbent; the impurities removed by the third impurity removal comprise olefin impurities; the olefin impurities comprise propadiene, propine, butadiene and vinyl acetylene;
and S5, filtering particles of the refined acetylene product obtained in the S4 through a filter with the pore diameter of 0.1 mu m, introducing the filtered acetylene product into a buffer tank with the pressure of 0.12MPa, pressurizing the acetylene product to 2.5MPa through a compressor, and filling the acetylene product to obtain the electronic-grade acetylene with the purity of 99.985 percent.
H in electronic grade acetylene 2 The content is less than 2ppm 2 The content is less than 1ppm 2 Content < 5ppm 4 Content (c) of<5ppm of CO content<2ppm,CO 2 Content (wt.)<1ppm，H 2 Content of O<5ppm, other CH and Compounds<10ppm (including propadiene, propyne, butadiene, vinyl acetylene).
Example 2
The preparation method of the electronic-grade acetylene of the embodiment comprises the following steps:
s1, introducing acetylene raw material gas from a steel cylinder into a dehydration tank, and removing partial water under the conditions that the temperature is 15 ℃ and the pressure is 0.15MPa to obtain an acetylene raw material crude product; the filler of the dehydration tank is calcium carbide or silicon tetrachloride;
the purity of the acetylene feed gas in this example was 96%;
s2, introducing the acetylene raw material crude product obtained in the S1 into a primary adsorption tower, and performing primary impurity removal under the conditions that the temperature is 15 ℃ and the pressure is 0.15MPa to obtain a primary acetylene crude product; the filler of the first-stage adsorption tower is a 4A molecular sieve; the impurities removed by the first impurity removal comprise water and carbon dioxide;
s3, introducing the primary acetylene crude product obtained in the S2 into a secondary adsorption tower, and performing secondary impurity removal under the conditions that the temperature is 15 ℃ and the pressure is 0.15MPa to obtain a secondary acetylene crude product; the filler of the secondary adsorption tower is a coal active carbon adsorbent; the impurities removed by the second impurity removal comprise arsine, phosphine and hydrogen sulfide;
s4, introducing the secondary acetylene crude product obtained in the step S3 into a three-stage adsorption tower, and performing third impurity removal under the conditions that the temperature is 15 ℃ and the pressure is 0.15MPa to obtain an acetylene fine product; the filler of the three-stage adsorption tower is an alumina adsorbent; the impurities removed by the third impurity removal comprise olefin impurities; the olefin impurities comprise propadiene, propine, butadiene and vinyl acetylene;
and S5, filtering particles of the fine acetylene product obtained in the S4 by a filter with the pore diameter of 0.1 mu m, introducing the fine acetylene product into a buffer tank with the pressure of 0.15MPa, pressurizing the fine acetylene product to 3.0MPa by a compressor, and filling the mixture to obtain the electronic-grade acetylene with the purity of 99.980%.
H in electronic grade acetylene 2 The content is less than 2ppm 2 The content is less than 1ppm 2 Content < 5ppm 4 Content (wt.)<5ppm of CO content<2ppm,CO 2 Content (wt.)<1ppm，H 2 O content<5ppm, other CH and Compounds<10ppm (including propadiene, propyne, butadiene, vinyl acetylene).
Example 3
The preparation method of electronic-grade acetylene in the embodiment comprises the following steps:
s1, introducing acetylene raw material gas from a steel cylinder into a dehydration tank, and removing partial water under the conditions that the temperature is 25 ℃ and the pressure is 0.1MPa to obtain an acetylene raw material crude product; the filler of the dehydration tank is silicon tetrachloride;
the purity of the acetylene feed gas in this example was 95%;
s2, introducing the acetylene raw material crude product obtained in the S1 into a primary adsorption tower, and performing primary impurity removal under the conditions that the temperature is 25 ℃ and the pressure is 0.1MPa to obtain a primary acetylene crude product; the filler of the first-stage adsorption tower is a 5A molecular sieve; the impurities removed by the first impurity removal comprise water and carbon dioxide;
s3, introducing the primary acetylene crude product obtained in the S2 into a secondary adsorption tower, and performing secondary impurity removal under the conditions that the temperature is 25 ℃ and the pressure is 0.1MPa to obtain a secondary acetylene crude product; the filler of the secondary adsorption tower is a coal active carbon adsorbent; the impurities removed by the second impurity removal comprise arsine, phosphine and hydrogen sulfide;
s4, introducing the secondary acetylene crude product obtained in the step S3 into a three-stage adsorption tower, and performing third impurity removal under the conditions that the temperature is 25 ℃ and the pressure is 0.1MPa to obtain an acetylene fine product; the filler of the three-stage adsorption tower is an alumina adsorbent; the impurities removed by the third impurity removal comprise olefin impurities; the olefin impurities comprise propadiene, propine, butadiene and vinyl acetylene;
and S5, filtering the fine acetylene product obtained in the step S4 by a filter with the pore diameter of 0.1m to filter particles, introducing the fine acetylene product into a buffer tank with the pressure of 0.1MPa, pressurizing the fine acetylene product to 2.0MPa by a compressor, and filling to obtain the electronic-grade acetylene with the purity of 99.981 percent.
H in electronic grade acetylene 2 The content is less than 2ppm 2 The content is less than 1ppm 2 Content < 5ppm 4 Content (wt.)<5ppm of CO content<2ppm,CO 2 Content (c) of<1ppm，H 2 Content of O<5ppm, other CH and Compounds<10ppm (including propadiene, propyne, butadiene, vinyl acetylene).
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (10)
1. A method for preparing electronic-grade acetylene, which is characterized by comprising the following steps:
s1, introducing acetylene raw material gas from a steel cylinder into a dehydration tank, and removing partial water under the conditions that the temperature is 15-25 ℃ and the pressure is 0.1-0.15 MPa to obtain an acetylene raw material crude product;
s2, introducing the acetylene raw material crude product obtained in the S1 into a primary adsorption tower, and performing primary impurity removal under the conditions that the temperature is 15-25 ℃ and the pressure is 0.1-0.15 MPa to obtain a primary acetylene crude product; the filler of the first-stage adsorption tower is a molecular sieve;
s3, introducing the primary acetylene crude product obtained in the S2 into a secondary adsorption tower, and performing secondary impurity removal under the conditions that the temperature is 15-25 ℃ and the pressure is 0.1-0.15 MPa to obtain a secondary acetylene crude product; the filler of the secondary adsorption tower is a coal active carbon adsorbent;
s4, introducing the secondary acetylene crude product obtained in the S3 into a three-stage adsorption tower, and performing third impurity removal under the conditions that the temperature is 15-25 ℃ and the pressure is 0.1-0.15 MPa to obtain an acetylene fine product; the filler of the three-stage adsorption tower is an alumina adsorbent;
and S5, filtering the fine acetylene product obtained in the step S4 by using a filter to filter particles, introducing the fine acetylene product into a buffer tank with the pressure of 0.1-0.15 MPa, pressurizing the fine acetylene product to 2.0-3.0 MPa by using a compressor, and filling to obtain the electronic-grade acetylene.
2. The method for preparing electronic grade acetylene according to claim 1, wherein the filler of the dehydration tank in S1 is calcium carbide or silicon tetrachloride.
3. The method for preparing electronic grade acetylene according to claim 1, wherein the impurities removed in the first impurity removal in S2 comprise water and carbon dioxide.
4. The method for preparing electronic grade acetylene according to claim 1, wherein the packing of the first-stage adsorption tower in S2 is 4A molecular sieve or 5A molecular sieve.
5. The method of claim 1, wherein the impurities removed in the second removal of impurities in S3 comprise arsine, phosphine, and hydrogen sulfide.
6. The method of claim 1, wherein the impurities removed in the third impurity removal in S4 comprise olefinic impurities.
7. The method of claim 6, wherein the olefinic impurities comprise propadiene, propyne, butadiene, and vinyl acetylene.
8. The method according to claim 1, wherein the pore size of the filter in S5 is 0.1 μm.
9. The method for preparing electronic grade acetylene according to claim 1, wherein the purity of the acetylene raw material gas in S1 is not less than 99.5%.
10. The method for preparing electronic-grade acetylene according to claim 1, wherein the purity of the electronic-grade acetylene in S5 is not less than 99.98%.
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| CN202211041416.9A CN115259989A (en) | 2022-08-29 | 2022-08-29 | Preparation method of electronic-grade acetylene |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH148755A (en) * | 1930-08-15 | 1931-08-15 | Lonza Ag | Process for purifying acetylene. |
| JPH09110739A (en) * | 1995-10-24 | 1997-04-28 | Tokuyama Corp | Dehydration of hydrocarbons |
| JP2004148257A (en) * | 2002-10-31 | 2004-05-27 | Nichigo Acetylene Kk | Portable supply apparatus for ultra-high purity acetylene |
| CN104496740A (en) * | 2014-12-15 | 2015-04-08 | 苏州金宏气体股份有限公司 | Device and method for purifying industrial acetylene into high-purity acetylene |
| US20200368670A1 (en) * | 2019-05-20 | 2020-11-26 | Transform Materials Llc | Systems and methods for acetylene purification |
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- 2022-08-29 CN CN202211041416.9A patent/CN115259989A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH148755A (en) * | 1930-08-15 | 1931-08-15 | Lonza Ag | Process for purifying acetylene. |
| JPH09110739A (en) * | 1995-10-24 | 1997-04-28 | Tokuyama Corp | Dehydration of hydrocarbons |
| JP2004148257A (en) * | 2002-10-31 | 2004-05-27 | Nichigo Acetylene Kk | Portable supply apparatus for ultra-high purity acetylene |
| CN104496740A (en) * | 2014-12-15 | 2015-04-08 | 苏州金宏气体股份有限公司 | Device and method for purifying industrial acetylene into high-purity acetylene |
| US20200368670A1 (en) * | 2019-05-20 | 2020-11-26 | Transform Materials Llc | Systems and methods for acetylene purification |
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