CN112778077A - Micro-reactor based electronic stage C2F6Preparation method - Google Patents
Micro-reactor based electronic stage C2F6Preparation method Download PDFInfo
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- CN112778077A CN112778077A CN202110063579.6A CN202110063579A CN112778077A CN 112778077 A CN112778077 A CN 112778077A CN 202110063579 A CN202110063579 A CN 202110063579A CN 112778077 A CN112778077 A CN 112778077A
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- Prior art keywords
- fluorine
- gas
- microreactor
- based electronic
- pentafluoroethane
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- 238000000034 method Methods 0.000 title description 7
- 239000007789 gas Substances 0.000 claims abstract description 54
- 238000006243 chemical reaction Methods 0.000 claims abstract description 40
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 35
- 239000011737 fluorine Substances 0.000 claims abstract description 35
- YPDSOAPSWYHANB-UHFFFAOYSA-N [N].[F] Chemical compound [N].[F] YPDSOAPSWYHANB-UHFFFAOYSA-N 0.000 claims abstract description 21
- GTLACDSXYULKMZ-UHFFFAOYSA-N pentafluoroethane Chemical compound FC(F)C(F)(F)F GTLACDSXYULKMZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 8
- 230000014759 maintenance of location Effects 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000003513 alkali Substances 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 3
- 239000011552 falling film Substances 0.000 claims description 3
- 238000005194 fractionation Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 4
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 238000003682 fluorination reaction Methods 0.000 description 13
- 229910001512 metal fluoride Inorganic materials 0.000 description 4
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 3
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- KWVVTSALYXIJSS-UHFFFAOYSA-L silver(ii) fluoride Chemical compound [F-].[F-].[Ag+2] KWVVTSALYXIJSS-UHFFFAOYSA-L 0.000 description 2
- 229910021571 Manganese(III) fluoride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012025 fluorinating agent Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 description 1
- SRVINXWCFNHIQZ-UHFFFAOYSA-K manganese(iii) fluoride Chemical compound [F-].[F-].[F-].[Mn+3] SRVINXWCFNHIQZ-UHFFFAOYSA-K 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- -1 perhalogenated ethane compound Chemical class 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention provides an electronic grade C based on a microreactor2F6The preparation method comprises the following steps: s1, introducing a mixture of fluorine gas and nitrogen gas into a mixing tank to mix to form a fluorine-nitrogen mixed gas, wherein the fluorine gas volume content in the fluorine-nitrogen mixed gas is 40-50%; s2, introducing the fluorine-nitrogen mixed gas and the gasified pentafluoroethane into a microchannel reactor for reaction, controlling the volume ratio of the fluorine gas to the pentafluoroethane to be 1.05-1.2: 1, controlling the reaction temperature to be 65-70 ℃, the reaction pressure to be 100 Pa-5 kPa, and controlling the retention time to be 60-100S.
Description
Technical Field
The invention relates to an electronic grade C based on a micro-reactor2F6A preparation method.
Background
At present, various process routes for preparing hexafluoroethane are available, and mainly comprise the following steps: electrochemical fluorination, pyrolysis, metal fluoride fluorination, hydrogen fluoride catalytic fluorination, direct fluorination.
Electrochemical fluorination: acetylene, ethylene or ethane are fluorinated under electrolytic conditions. The manufacturers have: dupont, Macro, U.S.A.
Pyrolysis method: by tetrafluoroethylene and CO2The thermal decomposition reaction between the two. The manufacturers have: kanto electric Co., Ltd., Beijing Yuji.
Metal fluoride fluorination: such as acetylene, ethylene and ethane with metal fluorides (CoF)3，MnF3，AgF2) The reaction is carried out. The manufacturers have: asahi glass gall, Henan Huaneng.
Hydrogen fluoride catalytic fluorination: fluorination of perhalogenated ethane compound (C) in the presence of catalyst2FxCly). The manufacturers have: kanto electric Co., Ltd., south China specialty gas Co., Ltd.
Direct fluorination: gases such as activated carbon, acetylene, ethane and pentafluoroethane react directly with fluorine gas.
Electrochemical fluorination has many side reactions, and because electrochemical fluorination occurs on the surface of the electrode, the yield is low due to the limitation of the length of the electrode. Pyrolysis methods require high decomposition temperatures, higher than 700 ℃, produce large amounts of CF4, and have low yields. The fluorination of metal fluorides has problems of regeneration of the metal fluorinating agent and large amount of fluorine gas. Hydrogen fluoride catalyzes fluorination, and chlorine atoms are difficult to replace by fluorine atoms due to the influence of adjacent fluorine atoms, often resulting in low conversion, often requiring high temperature and pressure to increase conversion, and producing a large amount of HCl by-product.
At present, a preparation method for performing direct fluorine reaction by utilizing pentafluoroethane and fluorine gas has not been reported.
Disclosure of Invention
The invention provides an electronic grade C based on a microreactor2F6The preparation method can effectively solve the problemsAnd (5) problems are solved.
The invention is realized by the following steps:
electronic grade C based on microreactor2F6The preparation method comprises the following steps:
s1, introducing a mixture of fluorine gas and nitrogen gas into a mixing tank to mix to form a fluorine-nitrogen mixed gas, wherein the fluorine gas volume content in the fluorine-nitrogen mixed gas is 40-50%;
s2, introducing the fluorine-nitrogen mixed gas and the gasified pentafluoroethane into a microchannel reactor for reaction, controlling the volume ratio of the fluorine gas to the pentafluoroethane to be 1.05-1.2: 1, the reaction temperature to be 65-70 ℃, the reaction pressure to be 100 Pa-5 kPa, and the retention time to be 60-100S
The invention has the beneficial effects that: the method provided by the invention can solve the problem of C in the prior art2F6The preparation method has the technical problem of low conversion rate, and the conversion rate can reach more than 90 percent; in addition, the invention can greatly prevent C through the optimized control of the reaction conditions in the microchannel reactor2F6The breakage of the C-C bond further improves the conversion rate and the yield of the reaction.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIGS. 1 and 2 show an electronic stage C based on a microreactor according to an embodiment of the present invention2F6The preparation method is a flow chart.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Referring to fig. 1 and 2, an embodiment of the invention is an electronic stage C based on a microreactor2F6The preparation method comprises the following steps:
s1, introducing a mixture of fluorine gas and nitrogen gas into a mixing tank to mix to form a fluorine-nitrogen mixed gas, wherein the fluorine gas volume content in the fluorine-nitrogen mixed gas is 40-50%;
s2, introducing the fluorine-nitrogen mixed gas and the gasified pentafluoroethane into a microchannel reactor 10 for reaction, controlling the volume ratio of the fluorine gas to the pentafluoroethane to be 1.05-1.2: 1, controlling the reaction temperature to be 65-70 ℃, the reaction pressure to be 100 Pa-5 kPa, and controlling the retention time to be 60-100S.
It can be understood that the fluorine-nitrogen mixed gas is formed by introducing the mixture of fluorine gas and nitrogen gas into the mixing tank and mixing, so that the activity of the fluorine gas can be reduced, and C can be prevented from reacting too violently2F6The C-C bond is cleaved. When the fluorine gas content is too low, the contact is insufficient in the reaction process, and the conversion is easily reducedThe rate and yield. Therefore, in step S1, the fluorine gas content in the mixed fluorine-nitrogen gas is preferably 40% to 45% by volume. In one embodiment, the fluorine-nitrogen mixed gas contains about 42% fluorine by volume.
As a further improvement, in step S2, the microchannel reactor 10 is of the type WH-INDHJ160, and has a diameter D of 10 microns or more and 100 microns or less. It can be understood that, since the microchannel reactor 10 has an extremely large specific surface area which can be several hundred times or even thousands times the specific surface area of the stirred tank, it has excellent heat and mass transfer capabilities, and can realize instantaneous uniform mixing and efficient heat transfer of fluorine gas and pentafluoroethane, thereby improving the reaction efficiency. As a further improvement, in order to further improve the conversion rate and the yield, it is necessary to control the volume ratio of the fluorine gas to the pentafluoroethane. When the fluorine gas content is too high, not only the fluorine gas is wasted but also C is generated2F6The C-C bond is cleaved. Preferably, in step S2, the volume ratio of the fluorine gas to the pentafluoroethane is 1.1: 1.
As a further improvement, in step S2, the reaction temperature is 68 ℃; the reaction pressure is 500 Pa-1 kPa; the retention time is 75-80 s.
As a further improvement, after step S2, the method may further comprise the steps of separation, falling film, water washing, alkali washing, compression, fractionation and rectification. The steps of separation, falling film, water washing, alkali washing, compression, fractionation and rectification can be selected from the existing steps, and are not described herein again.
Example 1
Introducing a mixture of fluorine gas and nitrogen gas into a mixing tank to mix to form a fluorine-nitrogen mixed gas, wherein the fluorine gas content in the fluorine-nitrogen mixed gas is respectively 35%, 40%, 42%, 50% and 55%; the fluorine-nitrogen mixed gas and the gasified pentafluoroethane are introduced into a microchannel reactor 10 to react, the volume ratios of the fluorine gas to the pentafluoroethane are respectively controlled to be 1:1, 1.05:1, 1.1:1, 1.2:1 and 1.3:1, the reaction temperature is respectively 68 ℃, the reaction pressure is 1kPa, the retention time is 70s, and the test data (conversion rate%) are shown in the following table 1.
Table 1 shows the conversion at a reaction temperature of 68 ℃
Example 2:
introducing a mixture of fluorine gas and nitrogen gas into a mixing tank to mix to form a fluorine-nitrogen mixed gas, wherein the volume content of the fluorine gas in the fluorine-nitrogen mixed gas is 42%; the fluorine-nitrogen mixed gas and the gasified pentafluoroethane are introduced into a microchannel reactor 10 to react, the volume ratio of the fluorine gas to the pentafluoroethane is controlled to be 1.1:1, the reaction temperature is controlled to be 60 ℃, 65 ℃, 68 ℃, 70 ℃ and 75 ℃, the reaction pressure is 1kPa, the retention time is controlled to be 70s, and a control test is carried out, wherein the test data (conversion rate%) are shown in the following table 2.
Table 2 shows the conversion at different reaction temperatures.
| Temperature of | 60℃ | 65℃ | 68℃ | 70℃ | 75℃ |
| Conversion rate | 83.4％ | 93.5％ | 95.6％ | 94.0％ | 81.8％ |
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. Electronic grade C based on microreactor2F6The preparation method is characterized by comprising the following steps:
s1, introducing a mixture of fluorine gas and nitrogen gas into a mixing tank to mix to form a fluorine-nitrogen mixed gas, wherein the fluorine gas volume content in the fluorine-nitrogen mixed gas is 40-50%;
s2, introducing the fluorine-nitrogen mixed gas and the gasified pentafluoroethane into a microchannel reactor for reaction, controlling the volume ratio of the fluorine gas to the pentafluoroethane to be 1.05-1.2: 1, controlling the reaction temperature to be 65-70 ℃, the reaction pressure to be 100 Pa-5 kPa, and controlling the retention time to be 60-100S.
2. The microreactor-based electronic stage C of claim 12F6The production method is characterized in that, in step S1, the volume content of fluorine gas in the mixed gas of fluorine and nitrogen is 40% to 45%.
3. The microreactor-based electronic stage C of claim 12F6The preparation method is characterized in that in step S2, the model of the microchannel reactor is WH-IND HJ 160.
4. The microreactor-based electronic stage C of claim 12F6The production method is characterized in that, in step S2, the volume ratio of the fluorine gas to the pentafluoroethane is 1.1: 1.
5. The microreactor-based electronic stage C of claim 12F6A production method characterized in that, in step S2, the reaction temperature is 68 ℃.
6. The microreactor-based electronic stage C of claim 12F6The production method is characterized in that, in step S2, the reaction pressure is 500Pa to 1 kPa.
7. The microreactor-based electronic stage C of claim 12F6The preparation method is characterized in that in step S2, the retention time is 75-80S.
8. The microreactor-based electronic stage C of claim 12F6The preparation method is characterized by further comprising the steps of separation, falling film washing, water washing, alkali washing, compression, fractionation and rectification after the step S2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114573417A (en) * | 2021-12-23 | 2022-06-03 | 西安近代化学研究所 | Preparation method of tetrafluoromethane and tetrafluoromethane mixed gas |
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|---|---|---|---|---|
| JPH09241186A (en) * | 1996-03-07 | 1997-09-16 | Showa Denko Kk | Production of hexafluoroethane |
| CN1161952A (en) * | 1996-03-26 | 1997-10-15 | 昭和电工株式会社 | Method for production of perfluorocarbon |
| CN1457332A (en) * | 2001-02-23 | 2003-11-19 | 昭和电工株式会社 | Process for producing perfluorocarbons and use thereof |
| TWI320035B (en) * | 2001-02-23 | 2010-02-01 | Process for producing perfluorocarbons and use thereof | |
| CN103288587A (en) * | 2013-05-23 | 2013-09-11 | 上海华捷视医疗设备有限公司 | Preparation method of perfluoroalkane |
| CN105461507A (en) * | 2015-11-19 | 2016-04-06 | 中国船舶重工集团公司第七一八研究所 | A method of preparing hexafluoroethane at high temperature |
| CN107602338A (en) * | 2017-09-15 | 2018-01-19 | 巨化集团技术中心 | A kind of synthetic method of low carbon chain perfluoroalkyl iodides |
| CN109867586A (en) * | 2017-12-04 | 2019-06-11 | 浙江省化工研究院有限公司 | A kind of method of fluoroform resourcable transformation production carbon tetrafluoride |
| CN111484389A (en) * | 2020-04-16 | 2020-08-04 | 山东重山光电材料股份有限公司 | Production process for co-producing high-purity electronic grade hydrogen fluoride and carbon fluoride |
-
2021
- 2021-01-18 CN CN202110063579.6A patent/CN112778077A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09241186A (en) * | 1996-03-07 | 1997-09-16 | Showa Denko Kk | Production of hexafluoroethane |
| CN1161952A (en) * | 1996-03-26 | 1997-10-15 | 昭和电工株式会社 | Method for production of perfluorocarbon |
| CN1457332A (en) * | 2001-02-23 | 2003-11-19 | 昭和电工株式会社 | Process for producing perfluorocarbons and use thereof |
| TWI320035B (en) * | 2001-02-23 | 2010-02-01 | Process for producing perfluorocarbons and use thereof | |
| CN103288587A (en) * | 2013-05-23 | 2013-09-11 | 上海华捷视医疗设备有限公司 | Preparation method of perfluoroalkane |
| CN105461507A (en) * | 2015-11-19 | 2016-04-06 | 中国船舶重工集团公司第七一八研究所 | A method of preparing hexafluoroethane at high temperature |
| CN107602338A (en) * | 2017-09-15 | 2018-01-19 | 巨化集团技术中心 | A kind of synthetic method of low carbon chain perfluoroalkyl iodides |
| CN109867586A (en) * | 2017-12-04 | 2019-06-11 | 浙江省化工研究院有限公司 | A kind of method of fluoroform resourcable transformation production carbon tetrafluoride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114573417A (en) * | 2021-12-23 | 2022-06-03 | 西安近代化学研究所 | Preparation method of tetrafluoromethane and tetrafluoromethane mixed gas |
| CN114573417B (en) * | 2021-12-23 | 2023-12-12 | 西安近代化学研究所 | Preparation method of tetrafluoromethane and tetrafluoromethane mixed gas |
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Inventor after: Li Jiming Inventor after: Zhang Kui Inventor after: Huang Yudi Inventor after: Zhu Junwei Inventor after: Huang Rongbao Inventor after: Que Xiangyu Inventor before: Zhang Kui Inventor before: Li Jiming Inventor before: Huang Yudi Inventor before: Zhu Junwei Inventor before: Huang Rongbao Inventor before: Que Xiangyu |
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Address after: No. 6, Gongye Road, Jiaoyang industrial concentration zone, Jiaoyang Town, Shanghang County, Longyan City, Fujian Province, 364204 Applicant after: Fujian del Technology Co.,Ltd. Address before: No. 6, Gongye Road, Jiaoyang industrial concentration zone, Jiaoyang Town, Shanghang County, Longyan City, Fujian Province, 364000 Applicant before: FUJIAN DEER TECHNOLOGY CO.,LTD. |
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Application publication date: 20210511 |