CN117384005A - Preparation method of hexafluoroethane - Google Patents
Preparation method of hexafluoroethane Download PDFInfo
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- CN117384005A CN117384005A CN202311169395.3A CN202311169395A CN117384005A CN 117384005 A CN117384005 A CN 117384005A CN 202311169395 A CN202311169395 A CN 202311169395A CN 117384005 A CN117384005 A CN 117384005A
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- hexafluoroethane
- preparation
- activated carbon
- cobalt
- cobalt chloride
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- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 69
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 34
- 238000003682 fluorination reaction Methods 0.000 claims abstract description 34
- 239000003054 catalyst Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 25
- GTLACDSXYULKMZ-UHFFFAOYSA-N pentafluoroethane Chemical compound FC(F)C(F)(F)F GTLACDSXYULKMZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 51
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 35
- 229910052731 fluorine Inorganic materials 0.000 claims description 35
- 239000011737 fluorine Substances 0.000 claims description 35
- 238000001035 drying Methods 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 25
- 229910021583 Cobalt(III) fluoride Inorganic materials 0.000 claims description 22
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 18
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 17
- YCYBZKSMUPTWEE-UHFFFAOYSA-L cobalt(ii) fluoride Chemical compound F[Co]F YCYBZKSMUPTWEE-UHFFFAOYSA-L 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- WZJQNLGQTOCWDS-UHFFFAOYSA-K cobalt(iii) fluoride Chemical compound F[Co](F)F WZJQNLGQTOCWDS-UHFFFAOYSA-K 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 9
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 9
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 9
- 238000002791 soaking Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 229910021582 Cobalt(II) fluoride Inorganic materials 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 231100000719 pollutant Toxicity 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 13
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 239000010949 copper Substances 0.000 abstract 1
- 229910052759 nickel Inorganic materials 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- HXELGNKCCDGMMN-UHFFFAOYSA-N [F].[Cl] Chemical group [F].[Cl] HXELGNKCCDGMMN-UHFFFAOYSA-N 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- YUYSUBJFEIVPHT-UHFFFAOYSA-H [Co](F)(F)(F)(F)(F)F Chemical compound [Co](F)(F)(F)(F)(F)F YUYSUBJFEIVPHT-UHFFFAOYSA-H 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention relates to a preparation method of hexafluoroethane, which comprises a fluorination process of cobalt chloride loaded on active carbon and doped with metal elements such as nickel, copper and the like, so that the contact area of a catalyst is greatly increased, and pentafluoroethane is introduced at 200-700 ℃ to generate hexafluoroethane under the action of the catalyst. The catalyst after the reaction can be repeatedly fluorinated and utilized, and the method has the advantages of easily available raw materials, simple process, high selectivity, high conversion rate, repeated utilization of the catalyst and the like.
Description
Technical Field
The invention relates to a preparation method of hexafluoroethane.
Background
Hexafluoroethane is widely used in semiconductor manufacturing processes, such as: etching gas used as a wafer, cavity cleaning after chemical vapor deposition, and the like. With the development of semiconductor devices, the precision requirements of integrated circuits are higher and higher, and hexafluoroethane as dry etching has the advantages of extremely small edge erosion phenomenon, high etching rate and high accuracy.
At present, the industry generally adopts a fluorine-chlorine exchange method to prepare hexafluoroethane. The pentafluoroethane which is a raw material in the method belongs to dangerous goods with stronger toxicity, and the container burst danger easily occurs due to the fact that the pentafluoroethane is easily subjected to heat pressure rise during transportation, so the pentafluoroethane belongs to a management and control product, and the raw material is not easy to purchase or even cannot purchase.
In the industry, a method for preparing hexafluoroethane by taking pentafluoroethane as a raw material has the advantages of easily available raw materials and low cost. However, the existing catalyst for preparing hexafluoroethane by taking pentafluoroethane as a raw material is cobalt fluoride, and the cobalt fluoride is generated after hydrogen fluoride and/or fluorine gas are/is fluorinated in the reaction process. And then cobalt trifluoride and pentafluoroethane are reacted to generate hexafluoroethane, and the unreacted completely middle pentafluoroethane can be reused through procedures such as rectification and the like. However, cobalt fluoride used as a catalyst in the method has the problems of amorphous and easy pulverization, which can cause a series of problems of greatly influencing the yield due to the reduction of catalytic performance in production, causing safety problems due to pipeline blockage and the like. Cobalt trifluoride is very unstable in nature, and oxidation and reduction are very easy to occur in air at room temperature to form cobalt fluoride, so that cobalt trifluoride is not directly adopted in the process for preparing hexafluoroethane from pentafluoroethane.
Disclosure of Invention
The invention aims to overcome the defects that pentafluoroethane is adopted as a raw material in the prior art, and provides a preparation method for preparing hexafluoroethane by adopting pentafluoroethane as the raw material, which comprises a preparation method of a catalyst, wherein the prepared catalyst has the advantages of high specific surface area and high dispersibility, can avoid the problems of amorphous cobalt fluoride and easy pulverization of the catalyst in the prior art, and can also greatly improve the conversion rate and selectivity of hexafluoroethane; and the catalyst can be repeatedly fluorinated and utilized after the reaction is completed by adopting the process.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
a preparation method of hexafluoroethane comprises the following preparation steps:
s1, pretreatment of activated carbon: placing the activated carbon in a muffle furnace, calcining for 1-2h at 200-300 ℃ under nitrogen atmosphere to remove pollutants attached to the activated carbon, and reserving the calcined activated carbon;
s2, preparing cobalt chloride into a cobalt chloride solution by using a proper solvent (the cobalt chloride is not required to be quantified and dissolved), soaking the activated carbon into the cobalt chloride solution, wherein the cobalt chloride accounts for 10-30% of the mass ratio of the cobalt chloride to the activated carbon, soaking for 8 hours at normal temperature (25-30 ℃), and then evaporating, drying and calcining the cobalt chloride solution soaked with the activated carbon;
s3, putting the substance calcined in the S2, namely the activated carbon loaded with cobalt chloride, into a reactor, introducing fluorine gas and hydrogen fluoride gas, and carrying out fluorination to prepare a corresponding catalyst cobalt trifluoride, wherein the flow rate of the fluorine gas and the hydrogen fluoride gas is 50-150ml/min, the reaction temperature is 100-500 ℃, and the volume ratio of the fluorine gas to the hydrogen fluoride gas is 1:1-5:1, a step of;
s4, after the fluorination is finished, introducing pentafluoroethane gas, generating hexafluoroethane by pentafluoroethane under the action of cobalt trifluoride catalyst, setting the flow rate of pentafluoroethane gas to be 20-200ml/min, setting the reaction temperature to be 200-700 ℃, and sampling and detecting after the reaction is finished (the process continuously reacts and samples in real time).
Further, the activated carbon selected in step s1 of the present invention is an activated carbon having a high specific surface area (high specific surface area activated carbon means a specific surface area exceeding 2500m 2 Activated carbon per g).
Further, the cobalt chloride used in step s2 of the present invention may be contaminated with a small amount (1% -5%) of a metal such as copper chloride and nickel chloride.
Further, the solvent for preparing the cobalt chloride solution in the step s2 of the invention adopts one or a mixture of more solvents of deionized water, ethanol and acetone.
Further, in the step s2 of the invention, the evaporating treatment is to heat the cobalt chloride solution soaked with the active carbon, and heat the solution to 100-110 ℃ until the solution is completely evaporated; after the drying treatment, the temperature of the drying treatment is 70-85 ℃ and the drying time is 6-8 hours; the calcination treatment adopts a horse boiling furnace, nitrogen protection is selected, the temperature is 450-1100 ℃, and the calcination time is 8-10h.
Further, the cobalt chloride in step s2 of the present invention is dissolved in deionized water or ethanol solution or a mixed solution of deionized water and ethanol solution, and the drying temperature is 70-85 ℃.
Further, in the step s2 of the invention, a muffle furnace is adopted for calcination treatment, nitrogen protection is adopted, the temperature is 450-1100 ℃, and the calcination and calcination time is 8-10h.
Further, the temperature of the calcination treatment according to the present invention is preferably 800 to 900 ℃.
Further, the fluorination is performed in the step s3, and the volume ratio of fluorine gas to hydrogen fluoride gas is 1:1-3:1; the fluorination temperature is 100-200 ℃.
Further, after the step s4, namely after the reaction is completed, fluorine gas is introduced again, cobalt difluoride reacts again under the fluorination of the fluorine gas to generate cobalt trifluoride for synthesizing hexafluoroethane again, so that the repeated fluorination utilization of the catalyst is realized, and the fluorine gas flow rate is 100-200ml/min; the temperature of fluorine gas selected for this fluorination is 100-500 ℃.
Further, according to the invention, fluorine gas is introduced again, cobalt difluoride reacts again under the fluorination of the fluorine gas to generate cobalt trifluoride, and the fluorine gas flow rate is preferably 100-150ml/min; the temperature of the fluorine gas is preferably 100-200 ℃.
The beneficial effects of the invention are as follows: the traditional hexafluoroethane preparation adopts a fluorine-chlorine exchange method. The raw material pentafluoroethane can not be purchased because of the control requirement. The invention adopts pentafluoroethane as the raw material to prepare hexafluoroethane, and has the advantages of easily available raw material and low cost. In the prior art, the catalyst adopted in the preparation of hexafluoroethane by taking pentafluoroethane as a raw material is cobalt fluoride, and the cobalt fluoride as solid powder has the problems of amorphous and very easy pulverization, which can cause a series of problems of greatly influencing the yield due to the reduction of the catalytic performance in the production, causing the safety hazard caused by the blockage of a pipeline, and the like. The invention adopts a novel method to prepare the catalyst, and completely solves the problems. According to the invention, cobalt fluoride is loaded in a void structure on the activated carbon, and powdered cobalt fluoride is impregnated and loaded on the activated carbon, so that pulverization can be completely avoided, the specific surface area of the cobalt fluoride is greatly increased by utilizing the property of the activated carbon, the larger the specific surface area is, the more the conversion rate is obviously improved by multiplying the contact surface of the compound, and the selectivity of cobalt hexafluoride can be improved.
Detailed Description
Example 1
100g of activated carbon is weighed, placed in a muffle furnace and subjected to high-temperature treatment for 2 hours in a nitrogen atmosphere.
30g of cobalt chloride and 5g of copper chloride are weighed, dissolved in 100ml of deionized water, stirred, and after all the cobalt chloride and copper chloride are dissolved, the dried activated carbon is soaked in cobalt chloride and copper chloride aqueous solution for 4 hours.
After the soaking is completed, the beaker is heated, the temperature is raised to 110 ℃, and the water solution is completely evaporated to dryness.
And after the completion of the drying, placing the beaker into a drying box at 75 ℃ for drying for 8 hours.
And after the drying is finished, placing the dried substance into a muffle furnace, purging with nitrogen, and calcining at 800 ℃ for 8 hours. And (3) putting the calcined substance into a reactor, and introducing fluorine gas and hydrogen fluoride gas, wherein the flow rate of the fluorine gas is 100ml/min. The flow rate of hydrogen fluoride was 100ml/min, and fluorination was carried out at 200℃for 3 hours.
After the fluorination, pentafluoroethane (flow rate 20 ml/min) was introduced, and the fluorination reaction was carried out at 400 ℃. And (5) sampling and detecting.
Example 2
100g of activated carbon is weighed, placed in a muffle furnace and subjected to high-temperature treatment for 2 hours in a nitrogen atmosphere.
30g of cobalt chloride and 5g of nickel chloride are weighed, dissolved in 100ml of deionized water, stirred, and after all the cobalt chloride and the nickel chloride are dissolved, the dried active carbon is soaked in cobalt chloride and nickel chloride aqueous solution for 4 hours.
After the soaking is completed, the beaker is heated, the temperature is raised to 110 ℃, and the water solution is completely evaporated to dryness.
And after the completion of the drying, placing the beaker into a drying box at 75 ℃ for drying for 8 hours.
And after the drying is finished, placing the dried substance into a muffle furnace, purging with nitrogen, and calcining at 800 ℃ for 8 hours. And (3) putting the calcined substance into a reactor, and introducing fluorine gas and hydrogen fluoride gas, wherein the flow rate of the fluorine gas is 100ml/min. The flow rate of hydrogen fluoride was 100ml/min, and fluorination was carried out at 200℃for 3 hours.
After the fluorination, pentafluoroethane (flow rate 20 ml/min) was introduced, and the fluorination reaction was carried out at 400 ℃. And (5) sampling and detecting.
Example 3
100g of activated carbon is weighed, placed in a muffle furnace and subjected to high-temperature treatment for 2 hours in a nitrogen atmosphere.
30g of cobalt chloride, 5g of copper chloride and 5g of nickel chloride are weighed, dissolved in 100ml of deionized water, stirred, and after all the solutions are dissolved, the dried activated carbon is soaked in aqueous solutions of cobalt chloride, copper chloride and nickel chloride for 4 hours.
After the soaking is completed, the beaker is heated, the temperature is raised to 110 ℃, and the water solution is completely evaporated to dryness.
And after the completion of the drying, placing the beaker into a drying box at 75 ℃ for drying for 8 hours.
And after the drying is finished, placing the dried substance into a muffle furnace, purging with nitrogen, and calcining at 800 ℃ for 8 hours. And (3) putting the calcined substance into a reactor, and introducing fluorine gas and hydrogen fluoride gas, wherein the flow rate of the fluorine gas is 100ml/min. The flow rate of hydrogen fluoride was 100ml/min, and fluorination was carried out at 200℃for 3 hours.
After the fluorination, pentafluoroethane (flow rate 20 ml/min) was introduced, and the fluorination reaction was carried out at 400 ℃. And (5) sampling and detecting.
Example 4
100g of activated carbon is weighed, placed in a muffle furnace and subjected to high-temperature treatment for 2 hours in a nitrogen atmosphere.
30g of cobalt chloride, 5g of copper chloride and 5g of nickel chloride are weighed, dissolved in 100ml of deionized water, stirred, and after all the solutions are dissolved, the dried activated carbon is soaked in aqueous solutions of cobalt chloride, copper chloride and nickel chloride for 4 hours.
After the soaking is completed, the beaker is heated, the temperature is raised to 110 ℃, and the water solution is completely evaporated to dryness.
And after the completion of the drying, placing the beaker into a drying box at 75 ℃ for drying for 8 hours.
And after the drying is finished, placing the dried substance into a muffle furnace, purging with nitrogen, and calcining at 800 ℃ for 8 hours. And (3) putting the calcined substance into a reactor, and introducing fluorine gas and hydrogen fluoride gas, wherein the flow rate of the fluorine gas is 200ml/min. The flow rate of hydrogen fluoride was 100ml/min, and fluorination was carried out at 200℃for 3 hours.
After the fluorination, pentafluoroethane (flow rate 20 ml/min) was introduced, and the fluorination reaction was carried out at 400 ℃. And (5) sampling and detecting.
And when the catalytic rate of the catalyst is reduced, introducing fluorine gas, wherein the flow rate of the fluorine gas is 100ml/min. And (3) carrying out secondary catalyst fluorination, wherein the fluorination temperature is 300 ℃ and the fluorination time is 3 hours. After the fluorination is completed, the method can be used for preparing hexafluoroethane continuously.
The following are the data results obtained from the sample testing of examples 1-3 of the present invention using Agilent-7820 gas chromatography.
Wherein, table 1: catalyst status and catalytic experimental data summary
Table 2: summary of catalytic yields for the double fluorination recycle catalyst of example 4
From the above detection data we can conclude that: the catalyst prepared by the method can improve the selectivity of hexafluoroethane to more than 88 percent in the whole catalytic reaction experimental process, the conversion rate can be more than 95 percent, and the reactivating and regenerating the catalyst can improve the reaction yield. The characteristics of the secondary reviving complete catalyst are still uniformly distributed, and the secondary reviving complete catalyst is not pulverized, so that the method of the invention not only avoids the problems of amorphous cobalt fluoride and easy pulverization of the catalyst in the prior art, but also greatly improves the general yield and selectivity, and solves the problems of low yield and selectivity in the prior art.
The method has the advantages that the selectivity and the yield can reach higher level, meanwhile, the price of the raw materials is superior, the problems of amorphous cobalt fluoride and easy pulverization of the catalyst in the prior art are avoided, the catalyst can be reused after the secondary fluorination is finished, and the yield is improved after the catalyst is reused.
Claims (10)
1. A preparation method of hexafluoroethane is characterized in that: the preparation method comprises the following steps of
S1, pretreatment of activated carbon: placing the activated carbon in a muffle furnace, calcining for 1-2h at 200-300 ℃ under nitrogen atmosphere to remove pollutants attached to the activated carbon, and reserving the calcined activated carbon;
s2, preparing cobalt chloride into a cobalt chloride solution by using a proper solvent, then soaking the active carbon prepared in the S1 into the cobalt chloride solution, wherein the mass ratio of the cobalt chloride to the active carbon is 10-30%, soaking the cobalt chloride solution for 7-8 hours at the temperature of 25-30 ℃, and then evaporating, drying and calcining the cobalt chloride solution soaked with the active carbon;
s3, putting the substance calcined in the step S2, namely the activated carbon loaded with cobalt chloride, into a reactor, introducing fluorine gas and hydrogen fluoride gas, and carrying out fluorination to prepare a corresponding catalyst cobalt trifluoride, wherein the flow rate of the fluorine gas and the hydrogen fluoride gas is 50-150ml/min, the reaction temperature is 100-500 ℃, and the volume ratio of the fluorine gas to the hydrogen fluoride gas is 1:1-5:1;
s4, after the fluorination is finished, introducing pentafluoroethane gas, generating hexafluoroethane by pentafluoroethane under the action of cobalt trifluoride serving as a catalyst, wherein the flow rate of the pentafluoroethane gas is 20-200ml/min, the reaction temperature is 200-700 ℃, and sampling and detecting are carried out after the reaction is finished.
2. A process for the preparation of hexafluoroethane as claimed in claim 1, wherein: the activated carbon in the step s1 is selected from high specific surface area activated carbon, wherein the high specific surface area activated carbon refers to the specific surface area exceeding 2500m 2 Activated carbon per gram.
3. A process for the preparation of hexafluoroethane as claimed in claim 1, wherein: the cobalt chloride adopted in the step s2 is doped with 1% -5% of copper chloride and/or nickel chloride.
4. A process for the preparation of hexafluoroethane as claimed in claim 1, wherein: the solvent for preparing the cobalt chloride solution in the step s2 adopts one or a mixture of more solvents of deionized water, ethanol and acetone.
5. A process for the preparation of hexafluoroethane as claimed in claim 1, wherein: the cobalt chloride in the step s2 is dissolved in deionized water or ethanol solution or a mixed solution of deionized water and ethanol solution.
6. A process for the preparation of hexafluoroethane as claimed in claim 1, wherein: in the step s2, the evaporating treatment is to heat the cobalt chloride solution soaked with the active carbon, and heat the solution to 100-110 ℃ until the solution is completely evaporated; after the drying treatment, the temperature of the drying treatment is 70-85 ℃ and the drying time is 6-8 hours; the calcination treatment adopts a horse boiling furnace, nitrogen protection is selected, the temperature is 450-1100 ℃, and the calcination time is 8-10h.
7. The method for producing hexafluoroethane as claimed in claim 6, wherein: the temperature of the calcination treatment in the step s2 is selected to be 800-900 ℃.
8. A process for the preparation of hexafluoroethane as claimed in claim 1, wherein: and (3) carrying out fluorination in the step (s 3), wherein the fluorination temperature is 100-200 ℃, the flow rate of fluorine gas and hydrogen fluoride gas is 100-150ml/min, and the volume ratio of the fluorine gas to the hydrogen fluoride gas is 1:1-3:1.
9. A process for the preparation of hexafluoroethane as claimed in claim 1, wherein: after step s4, namely after the reaction is completed, introducing fluorine again, and reacting cobalt difluoride again under the fluorination of fluorine gas to generate cobalt trifluoride for synthesizing hexafluoroethane again, so that the repeated fluorination utilization of the catalyst is realized, the fluorine gas flow rate is 100-200ml/min, and the fluorine gas temperature selected by the fluorination is 100-500 ℃.
10. A process for the preparation of hexafluoroethane as claimed in claim 9, wherein: and introducing fluorine again, wherein the fluorine gas flow rate is 100-150ml/min, and the fluorine gas temperature is 100-200 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311169395.3A CN117384005A (en) | 2023-09-12 | 2023-09-12 | Preparation method of hexafluoroethane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202311169395.3A CN117384005A (en) | 2023-09-12 | 2023-09-12 | Preparation method of hexafluoroethane |
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| CN117384005A true CN117384005A (en) | 2024-01-12 |
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| CN202311169395.3A Pending CN117384005A (en) | 2023-09-12 | 2023-09-12 | Preparation method of hexafluoroethane |
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- 2023-09-12 CN CN202311169395.3A patent/CN117384005A/en active Pending
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