CN113816826A - Purification method of electronic-grade monofluoromethane - Google Patents
Purification method of electronic-grade monofluoromethane Download PDFInfo
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Abstract
The invention discloses a method for purifying electronic grade monofluoromethane, which comprises the following steps: firstly, washing crude monofluoromethane gas in an absorption tower by using a sodium ethoxide-absolute ethyl alcohol solution to remove acidic impurities in the crude monofluoromethane gas and reduce the water content in the crude monofluoromethane gas to obtain pre-purified monofluoromethane; then removing residual ethanol and water from the pre-purified monofluoromethane in a low-temperature flash tank to obtain the monofluoromethane after low-temperature flash evaporation; introducing the low-temperature flash evaporated monofluoromethane into a light component removal tower for low-temperature rectification to remove light component impurities, and obtaining light component removal gas; and finally, introducing the light component removed gas into a heavy component removing 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 the ppm level, so that the target product monofluoromethane meets the requirement of electronic grade.
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 CH3F, is a compound with a boiling point of-78.2 ℃ and a density of 1.44gcm at normal temperature and pressure-2Is a non-toxic, liquefiable gas. The monofluoromethane has wide application, can be used as an organic molecule selective fluoromethylation reagent in organic synthesis and drug synthesis, and can also be used as a raw material in the preparation of an important pesticide, namely the fluorobromomethane. Meanwhile, the monofluoromethane has low greenhouse effect potential, zero value and ozone loss potential, and can be used as a low-temperature heat pump material. Today, high purity fluoromethane is widely recognized as one of the core gases in the advanced 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 should meet the following requirements: the content of monofluoromethane is more than or equal to 99.999 wt%, 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 5 ppm.
The synthesis method of monofluoromethane mainly has two methods:
(1) reaction of methanol with hydrogen fluoride:
reaction of methanol with hydrogen fluoride on chromium fluoride (chromium fluoride particles or supported on Al)2O3Supported) in the gas phase, the reaction equation is:
CH3OH+HF→CH3F+H2O
in the reaction process, the side reaction of generating dimethyl ether by dehydrating methanol is also carried out:
2CH3OH→CH3OCH3+H2O
(2) halogen exchange reaction of methyl chloride with hydrogen fluoride:
introducing methane chloride and hydrogen fluoride into a fixed bed reactor, and reacting to generate fluoromethane under the action of a metal chromium catalyst loaded on carbon-doped alumina, wherein the reaction equation is as follows:
CH3Cl+HF→CH3F+HCl
in both methods, the reaction process is completed under the action of a catalyst, and by-products of water, carbon dioxide, hydrogen chloride and hydrocarbons such as methane, ethylene, ethane and propylene are generated, and the impurities are important 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 present invention is to provide a method for purifying electronic grade monofluoromethane, which is aimed at overcoming the shortcomings of the prior art. According to the method, impurity components such as water, carbon dioxide, hydrogen chloride and the like which are difficult to remove are removed in the processes of gas washing and low-temperature flash evaporation in an absorption tower, and then the target product monofluoromethane meets the requirements of electronic grade through the subsequent two-stage low-temperature rectification process.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for purifying electronic grade monofluoromethane, comprising the steps of:
introducing the crude monofluoromethane gas into an absorption tower filled with a sodium ethoxide-absolute ethyl alcohol solution for gas washing, removing acidic impurities in the crude monofluoromethane gas and 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, and removing residual ethanol and water to obtain the monofluoromethane subjected to low-temperature flash evaporation; and sequentially introducing the monofluoromethane subjected to low-temperature flash evaporation 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 the electronic grade monofluoromethane.
Preferably, the sodium ethoxide-anhydrous ethanol solution is formed by mixing sodium ethoxide and an anhydrous ethanol solution, the concentration of the sodium ethoxide in the sodium ethoxide-anhydrous ethanol solution is 2 wt% -25 wt%, and the mass fraction of ethanol in the anhydrous ethanol 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 1.1 MPa.
Preferably, the theoretical plate number of the heavy component 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 1.4 MPa.
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 process of scrubbing in the absorption tower, the anhydrous ethanol solution of sodium ethoxide is used for removing acid gases such as hydrogen chloride, carbon dioxide and the like in the crude monofluoromethane gas, meanwhile, water in the crude monofluoromethane gas is absorbed by the anhydrous ethanol solution, and trace water is replaced by ethanol to form ethanol water solution.
2. According to the invention, ethanol and water are removed in the low-temperature flash tank, because the ethanol and the water form azeotropy, the freezing point of the ethanol aqueous solution is lower than that of the water, so that the ethanol aqueous solution cannot be frozen at low temperature, the ethanol and the water can be removed better by the low-temperature flash technology, and the subsequent removal of impurities in the light component removal tower and the heavy component removal tower is easier.
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 99.999wt 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 wt%, 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 5 ppm.
The technical solution of the present invention is further described in detail by the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic flow diagram of the process for the purification of electronic grade monofluoromethane according to the present invention.
Description of reference numerals:
t101-absorption tower; FLASH-low temperature FLASH tank; t102-lightness-removing tower; t103-heavy component removal tower.
Detailed Description
The crude monofluoromethane gas specifications used in examples 1-3 were: the mass purity was 99.82% crude monofluoromethane, and the impurities included 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 method for purifying electronic grade monofluoromethane of the present embodiment comprises the following steps:
introducing the crude monofluoromethane gas into an absorption tower T101 filled with a sodium ethoxide-absolute ethyl alcohol 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 0.7 MPa; the sodium ethoxide-absolute ethyl alcohol solution is formed by mixing sodium ethoxide and an absolute ethyl alcohol solution, the concentration of the sodium ethoxide in the sodium ethoxide-absolute ethyl alcohol solution is 2 wt%, and the mass fraction of the ethyl alcohol 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, so as to obtain the monofluoromethane subjected to low-temperature FLASH evaporation, wherein the operating temperature of the low-temperature FLASH tank FLASH is-22 ℃, and the operating pressure is 0.2 MPa; the content of monofluoromethane in the monofluoromethane after low-temperature flash evaporation is 99.80 wt%, the content of water is 1.9ppm, the content of nitrogen is 100ppm, the content of oxygen is 100ppm, and the total content of hydrocarbon substances is 0.18 wt%;
introducing the fluoromethane subjected to low-temperature flash evaporation 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 lightness-removed gas is 99.990 wt%, the content of water is 2.0ppm, the content of nitrogen is 1.0ppm, the content of oxygen is 1.5ppm, and the total content of hydrocarbon substances is 100.0 ppm; the light component impurities include nitrogen, carbon monoxide, methane and ethylene;
and 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 prepare 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.
Through detection: the electronic grade monofluoromethane prepared by the purification method of the embodiment has a monofluoromethane content of 99.999 wt%, a water content of 2.0ppm, a nitrogen content of 1.4ppm, an oxygen content of 1.6ppm, and a total hydrocarbon content of 5.0 ppm. Meets the national standard GB/T40418-2021 electronic special gas fluoromethane, and the technical requirement of the fluoromethane is as follows: the content of monofluoromethane is more than or equal to 99.999 wt%, 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 5 ppm.
Example 2
The method for purifying electronic grade monofluoromethane of the present embodiment comprises the following steps:
introducing the crude monofluoromethane gas into an absorption tower T101 filled with a sodium ethoxide-absolute ethyl alcohol 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 1.0 MPa; the sodium ethoxide-absolute ethyl alcohol solution is formed by mixing sodium ethoxide and an absolute ethyl alcohol solution, the concentration of the sodium ethoxide in the sodium ethoxide-absolute ethyl alcohol solution is 15 wt%, and the mass fraction of the ethyl alcohol 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, so as to obtain the monofluoromethane subjected to low-temperature FLASH evaporation, wherein the operating temperature of the low-temperature FLASH tank FLASH is-30 ℃, and the operating pressure is 0.8 MPa; the content of monofluoromethane in the monofluoromethane after low-temperature flash evaporation is 99.85 wt%, the content of water is 2.0ppm, the content of nitrogen is 100.0ppm, the content of oxygen is 100.0ppm, and the total content of hydrocarbon substances is 0.13 wt%;
introducing the fluoromethane subjected to low-temperature flash evaporation 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 lightness-removed gas is 99.987 wt%, 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 125.0 ppm; the light component impurities include nitrogen, carbon monoxide, methane and ethylene;
and 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 prepare 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.
Through detection: the electronic grade monofluoromethane prepared by the purification method of the embodiment has a monofluoromethane content of 99.999 wt%, a water content of 2.0ppm, a nitrogen content of 1.5ppm, an oxygen content of 1.7ppm, and a total hydrocarbon content of 4.8 ppm. Meets the national standard GB/T40418-2021 electronic special gas fluoromethane, and the technical requirement of the fluoromethane is as follows: the content of monofluoromethane is more than or equal to 99.999 wt%, 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 5 ppm.
Example 3
The method for purifying electronic grade monofluoromethane of the present embodiment comprises the following steps:
introducing the crude monofluoromethane gas into an absorption tower T101 filled with a sodium ethoxide-absolute ethyl alcohol 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 1.3 MPa; the sodium ethoxide-absolute ethyl alcohol solution is formed by mixing sodium ethoxide and an absolute ethyl alcohol solution, the concentration of the sodium ethoxide in the sodium ethoxide-absolute ethyl alcohol solution is 25 wt%, and the mass fraction of the ethyl alcohol 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, so as to obtain the monofluoromethane subjected to low-temperature FLASH evaporation, wherein the operating temperature of the low-temperature FLASH tank FLASH is-10 ℃, and the operating pressure is 0.5 MPa; the content of monofluoromethane in the monofluoromethane after low-temperature flash evaporation is 99.86 wt%, the content of water is 2.0ppm, the content of nitrogen is 100.0ppm, the content of oxygen is 100.0ppm, and the total content of hydrocarbon substances is 0.12 wt%;
introducing the fluoromethane subjected to low-temperature flash evaporation 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 lightness-removed gas is 99.985 wt%, 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 145.0 ppm; the light component impurities include nitrogen, carbon monoxide, methane and ethylene;
and 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 prepare 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.
Through detection: the electronic grade monofluoromethane prepared by the purification method of the embodiment has a monofluoromethane content of 99.999 wt%, a water content of 2.0ppm, a nitrogen content of 1.4ppm, an oxygen content of 1.7ppm, and a total hydrocarbon content of 4.9 ppm. Meets the national standard GB/T40418-2021 electronic special gas fluoromethane, and the technical requirement of the fluoromethane is as follows: the content of monofluoromethane is more than or equal to 99.999 wt%, 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 5 ppm.
In examples 1-3, the apparatus used in the electronic grade monofluoromethane purification process consisted of an absorber column T101, a low temperature FLASH tank FLASH, a light ends removal column T102 and a heavy ends removal column T103 connected in series, as shown in fig. 1.
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 (6)
1. A method for purifying electronic grade monofluoromethane, which is characterized by comprising the following steps:
introducing the crude monofluoromethane gas into an absorption tower filled with a sodium ethoxide-absolute ethyl alcohol solution for gas washing, removing acidic impurities in the crude monofluoromethane gas and 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, and removing residual ethanol and water to obtain the monofluoromethane subjected to low-temperature flash evaporation; and sequentially introducing the monofluoromethane subjected to low-temperature flash evaporation 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 the electronic grade monofluoromethane.
2. The method for purifying electronic grade monofluoromethane according to claim 1, wherein the sodium ethoxide-anhydrous ethanol solution is formed by mixing sodium ethoxide and anhydrous ethanol solution, the concentration of sodium ethoxide in the sodium ethoxide-anhydrous ethanol solution is 2 wt% to 25 wt%, and the mass fraction of ethanol in the anhydrous ethanol solution is 99.5%.
3. The method for purifying electronic grade monofluoromethane according to claim 1, wherein the operating temperature of the absorption column is from 0 ℃ to 50 ℃ and the operating pressure is from 0.7MPa to 1.3 MPa.
4. The method for purifying electronic grade monofluoromethane according to claim 1, wherein the number of theoretical plates of the lightness-removing column is 40-80, the reflux ratio is 30-70, the operating temperature is-44 ℃ to-15 ℃, and the operating pressure is 0.4MPa to 1.1 MPa.
5. The method for purifying electronic grade monofluoromethane according to claim 1, wherein the number of theoretical plates of the de-weighting 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 1.4 MPa.
6. The method of claim 1, wherein the acidic impurities comprise hydrogen chloride and carbon dioxide, and the light component impurities comprise nitrogen, carbon monoxide, methane, and ethylene; the heavy component impurities include propylene and hydrogen fluoride.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114413572A (en) * | 2021-12-28 | 2022-04-29 | 苏州金宏气体股份有限公司 | Device and method for removing fluoromethane impurities by low-temperature freezing method |
| WO2023206914A1 (en) * | 2022-04-28 | 2023-11-02 | 福建德尔科技股份有限公司 | Rectification control system and rectification control method for preparing electronic-grade methyl fluoride |
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| WO2006030677A1 (en) * | 2004-09-16 | 2006-03-23 | Showa Denko K.K. | Fluoromethane production process and product |
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