CN114426258A - Process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride - Google Patents
Process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride Download PDFInfo
- Publication number
- CN114426258A CN114426258A CN202210127471.3A CN202210127471A CN114426258A CN 114426258 A CN114426258 A CN 114426258A CN 202210127471 A CN202210127471 A CN 202210127471A CN 114426258 A CN114426258 A CN 114426258A
- Authority
- CN
- China
- Prior art keywords
- purity
- iodine pentafluoride
- carbon tetrafluoride
- reactor
- nitrogen trifluoride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/24—Inter-halogen compounds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/10—Carbon fluorides, e.g. [CF]nor [C2F]n
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride, which comprises the following steps: adding carbon tetraiodide into a reactor, preheating and diluting nitrogen trifluoride gas, introducing the nitrogen trifluoride gas into the reactor for reaction, and condensing and collecting iodine pentafluoride in a product by using a cold trap after the reaction is finished; and sequentially carrying out alkali washing, freeze drying, adsorption and rectification on the residual product to obtain high-purity carbon tetrafluoride, and rectifying the iodine pentafluoride collected by cold trap condensation to obtain high-purity iodine pentafluoride. The method can realize the co-production of high-purity iodine pentafluoride and carbon tetrafluoride, also avoids the safety risk of using fluorine gas as a fluorinating agent, reduces the introduction of impurities which are difficult to remove by using high-purity raw materials, is more favorable for preparing the high-purity iodine pentafluoride, ensures the purity of iodine pentafluoride and carbon tetrafluoride products, reduces the comprehensive cost, improves the economic benefit, and meets the production requirements of chemical enterprises on safety, environmental protection, high efficiency and circular economy.
Description
Technical Field
The invention belongs to the technical field of fluorine chemical industry, and particularly relates to a process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride.
Background
Iodine pentafluoride is a general fluorinating agent and a strong oxidizing agent, has important function in organic synthesis, and is mainly used for preparing a telomerization agent for synthesizing perfluoroiodonium iodide. The most important application is the synthesis of fluorine-containing surfactant and perfluoroiodoalkane used as raw material of fluorine-containing fabric finishing agent. In addition, iodine pentafluoride has specific bioactivity and biocompatibility, and can be used as a catalyst, a fluorinating agent, a halogen exchanger, an etching agent for semiconductor production and the like.
At present, the production of iodine pentafluoride at home and abroad mainly comprises the following four methods:
1. the method is characterized in that iodine reacts with a fluorine-nitrogen mixed gas to generate iodine pentafluoride, and the fluorine gas or the fluorine-nitrogen mixed gas reacts with iodine vapor, solution or solid to generate the iodine pentafluoride. The method adopts fluorine gas as a fluorinating agent, and the fluorine gas is a highly toxic product and has strong corrosivity and strong oxidizing property, so the method has higher safety risk;
2. the method comprises the steps of dissolving iodine in iodine pentafluoride, and then introducing iodine pentafluoride to react with iodine to prepare iodine pentafluoride, wherein the method is low in reaction efficiency, and the obtained iodine pentafluoride is low in purity;
3. the chlorine trifluoride and solid iodine reaction method can react at room temperature, but chlorine trifluoride serving as an oxidant has strong corrosivity and strong oxidizing property, and a small amount of leakage can cause fire, damage equipment and be not beneficial to industrial production.
4. The silver fluoride and iodine reaction method is characterized in that silver fluoride and iodine are mixed and then react under proper conditions to prepare iodine pentafluoride, but due to the cost factor of the raw materials of the silver fluoride, the method is difficult to realize industrial production.
And industrial grade iodine pentafluoride contains impurities such as iodine heptafluoride, free iodine, free fluorine gas and the like, so that the high-purity iodine pentafluoride is difficult to produce by purifying raw materials, wherein the fluorine gas is difficult to remove.
Thereby providing a process method for coproducing high-purity iodine pentafluoride and carbon tetrafluoride.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a process for co-producing high-purity iodine pentafluoride and carbon tetrafluoride, which is directed to the above deficiencies of the prior art, so as to solve the above problems in the background art.
In order to solve the technical problems, the invention adopts the technical scheme that: a process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride comprises the following steps:
s1, adding carbon tetraiodide into a reactor, preheating and diluting nitrogen trifluoride gas, and introducing the nitrogen trifluoride gas into the reactor for reaction, wherein the preheating temperature of the nitrogen trifluoride is controlled to be 200-350 ℃, the reaction temperature is controlled to be 100-200 ℃, and the reaction pressure is 0.1-3 MPa;
s2, after the reaction is finished, condensing and collecting iodine pentafluoride in the product by using a cold trap;
s3, sequentially carrying out alkali washing, freeze drying, adsorption and rectification on the residual product to obtain high-purity carbon tetrafluoride;
s4, rectifying and rectifying the iodine pentafluoride collected by cold trap condensation to obtain the high-purity iodine pentafluoride.
Further, in S1, the purity of nitrogen trifluoride is 99.99% or more; the purity of the carbon tetraiodide is more than 99%.
Further, in S1, the volume ratio of nitrogen trifluoride to diluent gas when the nitrogen trifluoride gas is diluted by preheating is 1: 1-10.
Further, the diluent gas is any one of nitrogen, helium and argon.
Further, in S1, nitrogen trifluoride is introduced into the upper gas phase space in the reactor or into carbon tetraiodide solid/liquid.
Further, in S1, the preheater for nitrogen trifluoride and the reactor are made of monel or stainless steel.
Further, in S2, the product includes iodine pentafluoride, carbon tetrafluoride, and nitrogen.
Further, in S4, the rectification is specifically vacuum rectification.
Further, the reactor is a tubular reactor or a coil type reaction kettle.
Compared with the prior art, the invention has the following advantages:
the process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride not only can realize co-production of high-purity iodine pentafluoride and carbon tetrafluoride, but also avoids the safety risk of producing iodine pentafluoride by using fluorine gas as a fluorinating agent, reduces the introduction of impurities difficult to remove by using high-purity raw materials, reduces the difficulty of purifying iodine pentafluoride, is more favorable for preparing high-purity iodine pentafluoride, ensures the purity of iodine pentafluoride and carbon tetrafluoride products, only discharges nitrogen, reduces the comprehensive cost, improves the economic benefit, and meets the production requirements of chemical enterprises on safety, environmental protection, high efficiency and circular economy.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1, the present invention provides a technical solution: a process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride comprises the following steps:
s1, adding carbon tetraiodide into a tubular reactor, wherein the reactor is made of stainless steel, the reaction temperature is set to be 100 ℃, the reaction pressure is 0.1MPa, high-purity nitrogen trifluoride gas is preheated at 200 ℃, diluted by nitrogen in a ratio of 1:1 and introduced into a gas phase space above the reactor for reaction;
s2, after the reaction is finished, condensing and collecting iodine pentafluoride in the product by using a cold trap;
s3, sequentially carrying out alkali washing, freeze drying, adsorption and rectification on the residual crude product to obtain a high-purity carbon tetrafluoride product, wherein the purity of the product is 99.997%;
s4, rectifying and rectifying the iodine pentafluoride collected by cold trap condensation to obtain high-purity iodine pentafluoride with the purity of 99.994%.
Embodiment 2, the present invention provides a technical solution: a process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride comprises the following steps:
s1, adding carbon tetraiodide into a coil type reaction kettle, wherein the material of the reaction kettle is Monel, the reaction temperature is set to be 125 ℃, the reaction pressure is 0.5MPa, high-purity nitrogen trifluoride gas is preheated at 240 ℃, diluted by helium 2:1 and introduced into a gas phase space above the reaction kettle for reaction;
s2, after the reaction is finished, condensing and collecting iodine pentafluoride in the product by using a cold trap;
s3, sequentially carrying out alkali washing, freeze drying, adsorption and rectification on the residual crude product to obtain a high-purity carbon tetrafluoride product, wherein the purity of the product is 99.999%;
s4, rectifying and rectifying the iodine pentafluoride collected by cold trap condensation to obtain high-purity iodine pentafluoride, and carrying out reduced pressure rectification on the crude iodine pentafluoride to obtain a high-purity iodine pentafluoride product with the purity of 99.996%.
Embodiment 3, the present invention provides a technical solution: a process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride comprises the following steps:
s1, adding carbon tetraiodide into a tubular reactor, wherein the reactor is made of stainless steel, the reaction temperature is set to be 150 ℃, the reaction pressure is 1.0MPa, high-purity nitrogen trifluoride gas is preheated at 280 ℃, diluted by argon gas 3:1 and introduced into a gas phase space above the reactor for reaction;
s2, after the reaction is finished, condensing and collecting iodine pentafluoride in the product by using a cold trap;
s3, sequentially carrying out alkali washing, freeze drying, adsorption and rectification on the residual crude product to obtain a high-purity carbon tetrafluoride product, wherein the purity of the product is 99.998%;
s4, rectifying and rectifying the iodine pentafluoride collected by cold trap condensation to obtain high-purity iodine pentafluoride, and carrying out reduced pressure rectification on the crude iodine pentafluoride to obtain a high-purity iodine pentafluoride product with the purity of 99.998%.
Embodiment 4, the present invention provides a technical solution: a process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride comprises the following steps:
s1, adding carbon tetraiodide into a coil pipe type reaction kettle, wherein the reaction kettle is made of stainless steel, the reaction temperature is set to be 175 ℃, the reaction pressure is 2.0MPa, high-purity nitrogen trifluoride gas is preheated at 320 ℃, diluted by using nitrogen gas 5:1 and introduced into a liquid phase below the reaction kettle for reaction;
s2, after the reaction is finished, condensing and collecting iodine pentafluoride in the product by using a cold trap;
s3, sequentially carrying out alkali washing, freeze drying, adsorption and rectification on the residual crude product to obtain a high-purity carbon tetrafluoride product, wherein the purity of the product is 99.996%;
s4, rectifying and rectifying the iodine pentafluoride collected by cold trap condensation to obtain high-purity iodine pentafluoride, and carrying out reduced pressure rectification on the crude iodine pentafluoride to obtain a high-purity iodine pentafluoride product with the purity of 99.996%.
Embodiment 5, the present invention provides a technical solution: a process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride comprises the following steps:
s1, adding carbon tetraiodide into a tubular reactor, wherein the material of the reactor is Monel, the reaction temperature is set to be 200 ℃, the reaction pressure is 5.0MPa, high-purity nitrogen trifluoride gas is preheated at 350 ℃, diluted by helium gas 10:1 and introduced into a liquid phase below the reactor for reaction;
s2, after the reaction is finished, condensing and collecting iodine pentafluoride in the product by using a cold trap;
s3, sequentially carrying out alkali washing, freeze drying, adsorption and rectification on the residual crude product to obtain a high-purity carbon tetrafluoride product, wherein the purity of the product is 99.999%;
s4, rectifying and rectifying the iodine pentafluoride collected by cold trap condensation to obtain high-purity iodine pentafluoride, and carrying out reduced pressure rectification on the crude iodine pentafluoride to obtain a high-purity iodine pentafluoride product with the purity of 99.999%.
It should be noted that, in this document, relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride is characterized by comprising the following steps:
s1, adding carbon tetraiodide into a reactor, preheating and diluting nitrogen trifluoride gas, and introducing the nitrogen trifluoride gas into the reactor for reaction, wherein the preheating temperature of the nitrogen trifluoride is controlled to be 200-350 ℃, the reaction temperature is controlled to be 100-200 ℃, and the reaction pressure is 0.1-3 MPa;
s2, after the reaction is finished, condensing and collecting iodine pentafluoride in the product by using a cold trap;
s3, sequentially carrying out alkali washing, freeze drying, adsorption and rectification on the residual product to obtain high-purity carbon tetrafluoride;
s4, rectifying and rectifying the iodine pentafluoride collected by cold trap condensation to obtain the high-purity iodine pentafluoride.
2. The process for co-producing high-purity iodine pentafluoride and carbon tetrafluoride according to claim 1, wherein in S1, the purity of nitrogen trifluoride is above 99.99%; the purity of the carbon tetraiodide is more than 99%.
3. The process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride according to claim 1, wherein in S1, the volume ratio of nitrogen trifluoride to diluent gas when nitrogen trifluoride gas is preheated for dilution is 1: 1-10.
4. The process method for co-producing high-purity iodine pentafluoride and carbon tetrafluoride according to claim 3, wherein the diluent gas is any one of nitrogen, helium and argon.
5. The process of claim 1, wherein in S1, nitrogen trifluoride is introduced into the upper gas phase space of the reactor or into the carbon tetraiodide solid/liquid.
6. The process of claim 1, wherein in S1, the preheater and the reactor of nitrogen trifluoride are made of Monel or stainless steel.
7. The process of claim 1, wherein in S2, the product comprises iodine pentafluoride, carbon tetrafluoride and nitrogen.
8. The process for co-producing high-purity iodine pentafluoride and carbon tetrafluoride according to claim 1, wherein in S4, the rectification is vacuum rectification.
9. The process of claim 1, wherein in S1, the reactor is a tubular reactor or a coil reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210127471.3A CN114426258B (en) | 2022-02-11 | 2022-02-11 | Process method for co-production of high-purity iodine pentafluoride and carbon tetrafluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210127471.3A CN114426258B (en) | 2022-02-11 | 2022-02-11 | Process method for co-production of high-purity iodine pentafluoride and carbon tetrafluoride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114426258A true CN114426258A (en) | 2022-05-03 |
| CN114426258B CN114426258B (en) | 2023-04-25 |
Family
ID=81313557
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210127471.3A Active CN114426258B (en) | 2022-02-11 | 2022-02-11 | Process method for co-production of high-purity iodine pentafluoride and carbon tetrafluoride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114426258B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE666456A (en) * | 1964-07-07 | 1965-11-03 | ||
| TW523491B (en) * | 1999-03-12 | 2003-03-11 | Showa Denko Kk | Treating method, treating agent and treating devices for exhausted gas with fluorided halogen |
| JP2010155742A (en) * | 2008-12-26 | 2010-07-15 | Daikin Ind Ltd | Method for producing iodine pentafluoride |
| CN104326443A (en) * | 2014-07-18 | 2015-02-04 | 多氟多化工股份有限公司 | Preparation method and production device of iodine pentafluoride |
| WO2017013916A1 (en) * | 2015-07-23 | 2017-01-26 | セントラル硝子株式会社 | Method for producing iodine pentafluoride |
| CN110061139A (en) * | 2013-12-17 | 2019-07-26 | 牛津大学科技创新有限公司 | Photovoltaic devices comprising metal halide perovskite and passivator |
-
2022
- 2022-02-11 CN CN202210127471.3A patent/CN114426258B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE666456A (en) * | 1964-07-07 | 1965-11-03 | ||
| TW523491B (en) * | 1999-03-12 | 2003-03-11 | Showa Denko Kk | Treating method, treating agent and treating devices for exhausted gas with fluorided halogen |
| JP2010155742A (en) * | 2008-12-26 | 2010-07-15 | Daikin Ind Ltd | Method for producing iodine pentafluoride |
| CN110061139A (en) * | 2013-12-17 | 2019-07-26 | 牛津大学科技创新有限公司 | Photovoltaic devices comprising metal halide perovskite and passivator |
| CN104326443A (en) * | 2014-07-18 | 2015-02-04 | 多氟多化工股份有限公司 | Preparation method and production device of iodine pentafluoride |
| WO2017013916A1 (en) * | 2015-07-23 | 2017-01-26 | セントラル硝子株式会社 | Method for producing iodine pentafluoride |
Non-Patent Citations (1)
| Title |
|---|
| 李梅;魏磊;酒坤;汪建春;: "五氟化碘的合成方法研究" * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114426258B (en) | 2023-04-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112723313A (en) | Method for preparing chlorine trifluoride | |
| CN107188778B (en) | Preparation method of octafluorocyclopentene | |
| CN113562700A (en) | Preparation method of chlorine trifluoride | |
| CN111484389A (en) | Production process for co-producing high-purity electronic grade hydrogen fluoride and carbon fluoride | |
| CN113735683A (en) | Purification device and purification method for electronic-grade difluoromethane | |
| CN114426258B (en) | Process method for co-production of high-purity iodine pentafluoride and carbon tetrafluoride | |
| CN216946810U (en) | A facility for industrial preparation high-purity hexafluoroethane | |
| CN112979607A (en) | Method for continuously preparing chlorinated ethylene carbonate | |
| CN112125773A (en) | Preparation method of 1,2,3, 4-tetrachlorohexafluorobutane | |
| CN107540514A (en) | A kind of preparation method of perfluoroethane | |
| CN110204414A (en) | A kind of preparation method of a fluoromethane | |
| WO2020137825A1 (en) | Method for producing cyclobutene | |
| CN102603461A (en) | Method for preparing 1,2-dibromotetrafluoroethane from tail gas in production of tetrafluoroethylene | |
| CN106629604A (en) | Method for preparing gas-phase hydrogen chloride by utilizing chlorosilane residue | |
| CN218392293U (en) | System for preparing trichloroethylene and tetrachloroethylene by azeotropic separation | |
| CN115583631A (en) | Method and device for preparing chlorine trifluoride | |
| CN105461507B (en) | A kind of method that perfluoroethane is prepared under high temperature | |
| CN110092704B (en) | Preparation method of 1, 1, 1-trichlorotrifluoroethane | |
| CN111116304B (en) | Method for synthesizing 1, 2-difluoroethane and 1,1, 2-trifluoroethane | |
| CN105218296A (en) | A kind of vapor-phase synthesis 1,1, Isosorbide-5-Nitrae, the method for the chloro-2-butylene of 4,4-hexafluoro-2- | |
| CN114436761B (en) | Method and system for preparing chlorine by catalyzing fluorine-containing hydrogen chloride and adding methane chloride and methane chloride into coproduction | |
| WO2020145088A1 (en) | Method for producing cyclobutane | |
| CN114314513B (en) | Method for fluoridation of low-valence fluoride by using chlorine trifluoride | |
| CN216890735U (en) | Device for industrial production of trifluoromethyl hypofluorite | |
| CN117285028A (en) | Process method for co-production of tungsten halide and carbon tetrafluoride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |