CN113816826B - Purification method of electronic grade monofluoromethane - Google Patents
Purification method of electronic grade monofluoromethane Download PDFInfo
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- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
Abstract
The invention discloses a purification method of electronic grade monofluoromethane, which comprises the following steps: washing the crude monofluoromethane gas in an absorption tower by using sodium ethoxide-absolute ethanol solution, removing acidic impurities in the crude monofluoromethane gas, and reducing the water content in the crude monofluoromethane gas to obtain pre-purified monofluoromethane; removing residual ethanol and water from the pre-purified monofluoromethane in a low-temperature flash tank to obtain the low-temperature flash-evaporated monofluoromethane; introducing the low-temperature flash-evaporated monofluoromethane into a light component removal tower for low-temperature rectification to remove light component impurities and obtain light component-removed gas; and finally, introducing the light component removed gas into a heavy component removal tower for secondary low-temperature rectification to remove heavy component impurities and obtain the electronic grade monofluoromethane. The method can effectively remove water, hydrogen chloride and hydrocarbon substances in the crude product gas of the monofluoromethane to ppm level, so that the monofluoromethane of a target product meets the electronic level requirement.
Description
Technical Field
The invention belongs to the technical field of gas purification, and particularly relates to a purification method of electronic grade monofluoromethane.
Background
Monofluoromethane, code HFC-41 or R41, formula CH 3 F is a catalyst having a boiling point of-78.2 ℃ and a density of 1.44gcm at normal temperature and normal pressure -2 Is a nontoxic, liquefiable gas. The application of the monofluoromethane is very wide, and the monofluoromethane can be used as an organic molecule selective fluoromethylation reagent in organic synthesis and drug synthesis, and also can be used as a raw material in the preparation of an important pesticide fluorobromomethane. At the same time, the greenhouse effect of the monofluoromethane itselfThe low-potential value, zero value and ozone depletion potential value can also be used as low-temperature heat pump materials. Today, where integrated circuit processes are being developed at high speed, high purity monofluoromethane is widely recognized as one of the core gases of the current chip fabrication process due to its high selectivity to silicon nitride films.
According to the national standard GB/T40418-2021 electronic Special gas fluoromethane, the technical requirements of the fluoromethane are met: the content of monofluoromethane is more than or equal to 99.999 weight percent, the water content is less than or equal to 2ppm, the nitrogen content is less than or equal to 4ppm, the oxygen content is less than or equal to 2ppm, and the total content of hydrocarbon substances is less than or equal to 5ppm.
The synthesis method of the fluoromethane mainly comprises two methods:
(1) Methanol reacts with hydrogen fluoride:
reaction of methanol with Hydrogen fluoride in chromium fluoride (chromium fluoride particles or supported on Al) 2 O 3 On a carrier) in the gas phase, the reaction equation is:
CH 3 OH+HF→CH 3 F+H 2 O
in the reaction process, there is also a side reaction that the methanol is dehydrated to generate dimethyl ether:
2CH 3 OH→CH 3 OCH 3 +H 2 O
(2) Halogen exchange reaction of chloromethane with hydrogen fluoride:
methyl chloride and hydrogen fluoride are introduced into a fixed bed reactor, and react to generate methyl fluoride under the action of a metal chromium catalyst loaded on carbon-doped alumina, wherein the reaction equation is as follows:
CH 3 Cl+HF→CH 3 F+HCl
both the above methods complete the reaction process under the action of a catalyst, and produce byproducts such as water, carbon dioxide, hydrogen chloride, and hydrocarbon substances such as methane, ethylene, ethane, propylene, etc., and the above impurities are important points of attention in the purification process of monofluoromethane. Therefore, it is important to develop an electronic grade monofluoromethane purification process that can remove the above impurities.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a purification method of electronic grade monofluoromethane aiming at the defects of the prior art. The method removes impurity components such as water, carbon dioxide, hydrogen chloride and the like which are difficult to remove through gas washing and low-temperature flash evaporation in an absorption tower, and then the target product, namely the monofluoromethane, meets the electronic grade requirement through the subsequent secondary low-temperature rectification process.
In order to solve the technical problems, the invention adopts the following technical scheme: a method for purifying electronic grade monofluoromethane, comprising the steps of:
introducing the crude monofluoromethane gas into an absorption tower filled with sodium ethoxide-absolute ethyl alcohol solution for gas washing, removing acidic impurities in the crude monofluoromethane gas, reducing the water content in the crude monofluoromethane gas, and obtaining pre-purified monofluoromethane after gas washing; introducing the pre-purified monofluoromethane into a low-temperature flash tank to remove residual ethanol and water, thereby obtaining the low-temperature flash-evaporated monofluoromethane; and sequentially introducing the low-temperature flash-evaporated monofluoromethane into a secondary rectification system consisting of a light component removal tower and a heavy component removal tower to sequentially remove light component impurities and heavy component impurities, thereby obtaining electronic-grade monofluoromethane.
Preferably, the sodium ethoxide-absolute ethyl alcohol solution is formed by mixing sodium ethoxide and an absolute ethyl alcohol solution, wherein the concentration of sodium ethoxide in the sodium ethoxide-absolute ethyl alcohol solution is 2-25 wt%, and the mass fraction of ethanol in the absolute ethyl alcohol solution is 99.5%.
Preferably, the operating temperature of the absorption tower is 0-50 ℃ and the operating pressure is 0.7-1.3 MPa.
Preferably, the theoretical plate number of the light component removal tower is 40-80, the reflux ratio is 30-70, the operating temperature is-44 ℃ to-15 ℃, and the operating pressure is 0.4MPa to 1.1MPa.
Preferably, the theoretical plate number of the heavy-removal tower is 30-50, the reflux ratio is 1-10, the operating temperature is-37 ℃ to-10 ℃, and the operating pressure is 0.9MPa to 1.4MPa.
Preferably, the acidic impurities include hydrogen chloride and carbon dioxide, and the light component impurities include nitrogen, carbon monoxide, methane and ethylene; the heavy component impurities include propylene and hydrogen fluoride.
Compared with the prior art, the invention has the following advantages:
1. in the invention, in the gas washing process in the absorption tower, an absolute ethanol solution of sodium ethoxide is adopted to remove acid gases such as hydrogen chloride, carbon dioxide and the like in the crude product gas of the monofluoromethane, meanwhile, the moisture in the crude product gas of the monofluoromethane is absorbed by the absolute ethanol solution, and a trace of water is replaced by ethanol to form an ethanol aqueous solution.
2. According to the invention, ethanol and water are removed in the low-temperature flash evaporation tank, and the freezing point of the ethanol aqueous solution is lower than that of water because the ethanol and the water form azeotropy, so that the ethanol aqueous solution can not be frozen at low temperature, and ethanol and water can be better removed by the low-temperature flash evaporation technology, so that impurities in a subsequent light component removal tower and a subsequent heavy component removal tower are easier to remove.
3. The invention has simple whole flow and easily obtained raw materials, can realize continuous operation and effectively reduce the production cost; the invention can obtain the electronic grade monofluoromethane with the mass fraction of more than 99.999 percent, the water content of less than or equal to 2ppm, the nitrogen content of less than or equal to 4ppm, the oxygen content of less than or equal to 1.5ppm and the total content of hydrocarbon substances of less than or equal to 5 ppm; meets the technical requirements of national standard GB/T40418-2021 electronic Special gas fluoromethane: the content of monofluoromethane is more than or equal to 99.999 weight percent, the water content is less than or equal to 2ppm, the nitrogen content is less than or equal to 4ppm, the oxygen content is less than or equal to 2ppm, and the total content of hydrocarbon substances is less than or equal to 5ppm.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a schematic flow chart of the purification method of electronic grade monofluoromethane.
Reference numerals illustrate:
t101-an absorption tower; FLASH-low temperature FLASH tank; t102-a light component removing tower; t103-heavy-duty removal tower.
Detailed Description
The crude gas specification of monofluoromethane used in examples 1-3 was: the crude monofluoromethane has a mass purity of 99.82%, and the impurities include 0.01% hydrogen chloride, 0.01% carbon dioxide, 0.01% nitrogen, 0.01% oxygen, 0.01% carbon monoxide, 0.05% hydrogen fluoride, 0.01% propylene, 0.01% methane, 0.01% ethylene and 0.05% water.
Example 1
The purification method of the electronic grade monofluoromethane of the present embodiment comprises the following steps:
introducing the crude monofluoromethane gas into an absorption tower T101 filled with sodium ethoxide-absolute ethanol solution for gas washing, removing acidic impurities in the crude monofluoromethane gas, and reducing the water content in the crude monofluoromethane gas to obtain pre-purified monofluoromethane, wherein the operation temperature of the absorption tower T101 is 25 ℃, and the operation pressure is 0.7MPa; the sodium ethoxide-absolute ethyl alcohol solution is formed by mixing sodium ethoxide and absolute ethyl alcohol solution, wherein the concentration of sodium ethoxide in the sodium ethoxide-absolute ethyl alcohol solution is 2wt%, and the mass fraction of ethanol in the absolute ethyl alcohol solution is 99.5%; the acidic impurities include hydrogen chloride and carbon dioxide;
introducing the pre-purified monofluoromethane into a low-temperature FLASH tank FLASH to remove residual ethanol and water to obtain the low-temperature FLASH-evaporated monofluoromethane, wherein the operating temperature of the low-temperature FLASH tank FLASH is-22 ℃ and the operating pressure is 0.2MPa; the content of the monofluoromethane in the monofluoromethane subjected to low-temperature flash evaporation is 99.80wt%, the water content is 1.9ppm, the nitrogen content is 100ppm, the oxygen content is 100ppm, and the total content of hydrocarbon substances is 0.18wt%;
introducing the low-temperature flash-evaporated monofluoromethane into a light component removal tower T102 for low-temperature rectification to remove light component impurities to obtain light component-removed gas, wherein the operating temperature of the light component removal tower T102 is-15 ℃, the operating pressure is 0.4MPa, the theoretical plate number of the light component removal tower T102 is 80, and the reflux ratio is 30; the content of monofluoromethane in the light-removed gas is 99.990wt%, the water content is 2.0ppm, the nitrogen content is 1.0ppm, the oxygen content is 1.5ppm, and the total content of hydrocarbon substances is 100.0ppm; the light component impurities include nitrogen, carbon monoxide, methane and ethylene;
and (3) introducing the light component removed gas into a heavy component removal tower T103 for secondary low-temperature rectification to remove heavy component impurities, so as to obtain the electronic grade monofluoromethane, wherein the operating temperature of the heavy component removal tower T103 is-10 ℃, the operating pressure is 0.9MPa, the theoretical plate number of the heavy component removal tower T103 is 50, the reflux ratio is 1, and the heavy component impurities comprise propylene and hydrogen fluoride.
And (3) detecting: the electronic grade monofluoromethane obtained by the purification method of this example had a monofluoromethane content of 99.999% by weight, a water content of 2.0ppm, a nitrogen content of 1.4ppm, an oxygen content of 1.6ppm and a total hydrocarbon content of 5.0ppm. Meets the national standard GB/T40418-2021 (electronic Special gas fluoromethane), and meets the technical requirements of the monofluoromethane: the content of monofluoromethane is more than or equal to 99.999 weight percent, the water content is less than or equal to 2ppm, the nitrogen content is less than or equal to 4ppm, the oxygen content is less than or equal to 2ppm, and the total content of hydrocarbon substances is less than or equal to 5ppm.
Example 2
The purification method of the electronic grade monofluoromethane of the present embodiment comprises the following steps:
introducing the crude monofluoromethane gas into an absorption tower T101 filled with sodium ethoxide-absolute ethanol solution for gas washing, removing acidic impurities in the crude monofluoromethane gas, and reducing the water content in the crude monofluoromethane gas to obtain pre-purified monofluoromethane, wherein the operation temperature of the absorption tower T101 is 50 ℃, and the operation pressure is 1.0MPa; the sodium ethoxide-absolute ethyl alcohol solution is formed by mixing sodium ethoxide and absolute ethyl alcohol solution, wherein the concentration of sodium ethoxide in the sodium ethoxide-absolute ethyl alcohol solution is 15wt%, and the mass fraction of ethanol in the absolute ethyl alcohol solution is 99.5%; the acidic impurities include hydrogen chloride and carbon dioxide;
introducing the pre-purified monofluoromethane into a low-temperature FLASH tank FLASH to remove residual ethanol and water to obtain the low-temperature FLASH-evaporated monofluoromethane, wherein the operating temperature of the low-temperature FLASH tank FLASH is minus 30 ℃ and the operating pressure is 0.8MPa; the content of the monofluoromethane in the monofluoromethane subjected to low-temperature flash evaporation is 99.85wt%, the water content is 2.0ppm, the nitrogen content is 100.0ppm, the oxygen content is 100.0ppm, and the total content of hydrocarbon substances is 0.13wt%;
introducing the low-temperature flash-evaporated monofluoromethane into a light component removal tower T102 for low-temperature rectification to remove light component impurities to obtain light component-removed gas, wherein the operating temperature of the light component removal tower T102 is-31 ℃, the operating pressure is 0.8MPa, the theoretical plate number of the light component removal tower T102 is 40, and the reflux ratio is 70; the content of monofluoromethane in the light-removed gas is 99.987wt%, the water content is 2.0ppm, the nitrogen content is 1.5ppm, the oxygen content is 1.5ppm, and the total content of hydrocarbon substances is 125.0ppm; the light component impurities include nitrogen, carbon monoxide, methane and ethylene;
and (3) introducing the light component removed gas into a heavy component removal tower T103 for secondary low-temperature rectification to remove heavy component impurities, so as to obtain the electronic grade monofluoromethane, wherein the operating temperature of the heavy component removal tower T103 is-20 ℃, the operating pressure is 1.1MPa, the theoretical plate number of the heavy component removal tower T103 is 30, the reflux ratio is 10, and the heavy component impurities comprise propylene and hydrogen fluoride.
And (3) detecting: the electronic grade monofluoromethane obtained by the purification method of this example had a monofluoromethane content of 99.999% by weight, a water content of 2.0ppm, a nitrogen content of 1.5ppm, an oxygen content of 1.7ppm and a total hydrocarbon content of 4.8ppm. Meets the national standard GB/T40418-2021 (electronic Special gas fluoromethane), and meets the technical requirements of the monofluoromethane: the content of monofluoromethane is more than or equal to 99.999 weight percent, the water content is less than or equal to 2ppm, the nitrogen content is less than or equal to 4ppm, the oxygen content is less than or equal to 2ppm, and the total content of hydrocarbon substances is less than or equal to 5ppm.
Example 3
The purification method of the electronic grade monofluoromethane of the present embodiment comprises the following steps:
introducing the crude monofluoromethane gas into an absorption tower T101 filled with sodium ethoxide-absolute ethanol solution for gas washing, removing acidic impurities in the crude monofluoromethane gas, and reducing the water content in the crude monofluoromethane gas to obtain pre-purified monofluoromethane, wherein the operation temperature of the absorption tower T101 is 0 ℃, and the operation pressure is 1.3MPa; the sodium ethoxide-absolute ethyl alcohol solution is formed by mixing sodium ethoxide and absolute ethyl alcohol solution, wherein the concentration of sodium ethoxide in the sodium ethoxide-absolute ethyl alcohol solution is 25wt%, and the mass fraction of ethanol in the absolute ethyl alcohol solution is 99.5%; the acidic impurities include hydrogen chloride and carbon dioxide;
introducing the pre-purified monofluoromethane into a low-temperature FLASH tank FLASH to remove residual ethanol and water to obtain the low-temperature FLASH-evaporated monofluoromethane, wherein the operating temperature of the low-temperature FLASH tank FLASH is-10 ℃ and the operating pressure is 0.5MPa; the content of the monofluoromethane in the monofluoromethane subjected to low-temperature flash evaporation is 99.86wt%, the water content is 2.0ppm, the nitrogen content is 100.0ppm, the oxygen content is 100.0ppm, and the total content of hydrocarbon substances is 0.12wt%;
introducing the low-temperature flash-evaporated monofluoromethane into a light component removal tower T102 for low-temperature rectification to remove light component impurities to obtain light component-removed gas, wherein the operating temperature of the light component removal tower T102 is-44 ℃, the operating pressure is 1.1MPa, the theoretical plate number of the light component removal tower T102 is 60, and the reflux ratio is 65; the content of monofluoromethane in the light-removed gas is 99.985wt%, the water content is 2.0ppm, the nitrogen content is 1.5ppm, the oxygen content is 1.5ppm, and the total content of hydrocarbon substances is 145.0ppm; the light component impurities include nitrogen, carbon monoxide, methane and ethylene;
and (3) introducing the light component removed gas into a heavy component removal tower T103 for secondary low-temperature rectification to remove heavy component impurities, so as to obtain the electronic grade monofluoromethane, wherein the operating temperature of the heavy component removal tower T103 is-37 ℃, the operating pressure is 1.4MPa, the theoretical plate number of the heavy component removal tower T103 is 40, the reflux ratio is 6, and the heavy component impurities comprise propylene and hydrogen fluoride.
And (3) detecting: the electronic grade monofluoromethane obtained by the purification method of this example had a monofluoromethane content of 99.999% by weight, a water content of 2.0ppm, a nitrogen content of 1.4ppm, an oxygen content of 1.7ppm and a total hydrocarbon content of 4.9ppm. Meets the national standard GB/T40418-2021 (electronic Special gas fluoromethane), and meets the technical requirements of the monofluoromethane: the content of monofluoromethane is more than or equal to 99.999 weight percent, the water content is less than or equal to 2ppm, the nitrogen content is less than or equal to 4ppm, the oxygen content is less than or equal to 2ppm, and the total content of hydrocarbon substances is less than or equal to 5ppm.
In examples 1-3, the apparatus used in the electronic grade monofluoromethane purification process consisted of an absorber T101, a low temperature FLASH tank FLASH, a light ends column T102 and a heavy ends column T103 connected in series, as shown in FIG. 1.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (5)
1. A method for purifying electronic grade monofluoromethane, comprising the steps of:
introducing the crude monofluoromethane gas into an absorption tower filled with sodium ethoxide-absolute ethyl alcohol solution for gas washing, removing acidic impurities in the crude monofluoromethane gas, reducing the water content in the crude monofluoromethane gas, and obtaining pre-purified monofluoromethane after gas washing; introducing the pre-purified monofluoromethane into a low-temperature flash tank to remove residual ethanol and water, thereby obtaining the low-temperature flash-evaporated monofluoromethane; sequentially introducing the low-temperature flash-evaporated monofluoromethane into a secondary rectification system consisting of a light component removal tower and a heavy component removal tower to sequentially remove light component impurities and heavy component impurities, thereby obtaining electronic-grade monofluoromethane; the acidic impurities include hydrogen chloride and carbon dioxide, and the light component impurities include nitrogen, carbon monoxide, methane and ethylene; the heavy component impurities include propylene and hydrogen fluoride.
2. The method for purifying electronic grade monofluoromethane of claim 1, wherein the sodium ethoxide-absolute ethyl alcohol solution is formed by mixing sodium ethoxide and absolute ethyl alcohol solution, the concentration of sodium ethoxide in the sodium ethoxide-absolute ethyl alcohol solution is 2wt% to 25wt%, and the mass fraction of ethanol in the absolute ethyl alcohol solution is 99.5%.
3. The method for purifying electronic grade monofluoromethane of claim 1, wherein the operating temperature of the absorption tower is 0 ℃ to 50 ℃ and the operating pressure is 0.7mpa to 1.3mpa.
4. The purification method of electronic grade monofluoromethane according to claim 1, wherein the theoretical plate number of the light component removal tower is 40-80, the reflux ratio is 30-70, the operation temperature is-44 ℃ to-15 ℃, and the operation pressure is 0.4 mpa-1.1 mpa.
5. The purification method of electronic grade monofluoromethane according to claim 1, wherein the theoretical plate number of the de-weighting tower is 30-50, the reflux ratio is 1-10, the operation temperature is-37 ℃ to-10 ℃, and the operation pressure is 0.9 mpa-1.4 mpa.
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| CN114870416B (en) * | 2022-04-28 | 2023-01-24 | 福建德尔科技股份有限公司 | Rectification control system and rectification control method for preparing electronic-grade monofluoromethane |
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| JP2010248104A (en) * | 2009-04-14 | 2010-11-04 | Tokuyama Corp | Manufacturing method for 1,1,1,2,3-pentachloropropane |
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| WO2006030677A1 (en) * | 2004-09-16 | 2006-03-23 | Showa Denko K.K. | Fluoromethane production process and product |
| JP2010248104A (en) * | 2009-04-14 | 2010-11-04 | Tokuyama Corp | Manufacturing method for 1,1,1,2,3-pentachloropropane |
| CN109251124A (en) * | 2018-11-01 | 2019-01-22 | 广东华特气体股份有限公司 | An a kind of fluoromethane purifying technique |
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