CN103497086A - Preparation method of perfluoropropane - Google Patents
Preparation method of perfluoropropane Download PDFInfo
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- CN103497086A CN103497086A CN201310431026.7A CN201310431026A CN103497086A CN 103497086 A CN103497086 A CN 103497086A CN 201310431026 A CN201310431026 A CN 201310431026A CN 103497086 A CN103497086 A CN 103497086A
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Abstract
The invention discloses a preparation method of perfluoropropane. The preparation method sequentially comprises the following steps: (1) electrolyzing potassium bifluoride to obtain a mixed fluorine gas, and sequentially carrying out dust extraction, condensation and adsorption treatments on the mixed fluorine gas to purify the mixed fluorine gas to raw material fluoride; (2) pressurizing the raw material fluoride and uniformly mixing the raw material fluoride with an inert gas to obtain a mixed gas; (3) introducing the mixed gas into a reactor filled with cobaltous fluoride to react to obtain cobaltic oxide; (4) carrying out purging and vacuumizing replacement treatments on the reactor and related pipelines and pipe fittings after the reaction; (5) introducing hexafluoropropylene into the reactor to react with the cobaltic oxide to obtain perfluoropropane containing impurities; (6) cooling and adsorbing the perfluoropropane; and (7) introducing the perfluoropropane into a rectifying column through a compressor to be rectified. By adopting the preparation method disclosed by the invention, the corrosion of impurities on the reactor can be reduced, such unfavorable side reactions as hexafluoropropylene pyrolysis, self polymerization, addition, and the like, are inhibited, and perfluoropropane with high purity is prepared.
Description
Technical field
The present invention relates to chemical field, relate in particular to a kind of preparation method of octafluoropropane.
Background technology
Octafluoropropane, be commonly used for the etching or the purge gas that prepare in semiconductor device technology.Existing have multiple about the method for using R 1216 directly to prepare octafluoropropane as raw material:
Japanese Patent JP-B-62-61572 points out, carries out direct fluoridation and prepare octafluoropropane between R 1216 and fluorine gas; Japanese Patent JP-B-1-45455 points out, under catalyzer exists, makes R 1216 react and prepare octafluoropropane with fluorine; Japanese Patent JP-B-62-54777 points out, R 1216 is reacted and prepares octafluoropropane with senior (high-order) metal fluoride; Japanese Patent JP-B-62-61682 points out, in the situation that use rare gas element and reaction product gas dilution, makes R 1216 react and prepare octafluoropropane with fluorine gas; Japanese Patent JP-B-62-61115 points out, in hydrogen fluoride, makes the R 1216 electrofluorination to prepare octafluoropropane.
Yet, in aforesaid method, because R 1216 cracking in reaction process produces tetrafluoromethane (CF
4) and hexafluoroethane (C
2f
6), and addition produces C
4f
8and C
6f
12, and cycloaddition produces the by products such as 4 annulus, simultaneously, also fluorizating agent (senior metal fluoride) do not done to advanced treatment, makes the selectivity of purpose product and the productive rate of octafluoropropane reduce.In addition, some compound in impurity is difficult to fall by rectifying separation, therefore almost can not get high-purity octafluoropropane.Particularly, in the implementation process of aforesaid method, be all the feasibility that experimental has been proved method, not mentioned industrialized manufacturing technique.And these methods are to carry out under higher temperatures, and the thinner hydrogen fluoride (HF) that in reaction process, reactant adds is very serious to the corrosion of equipment, therefore, material to equipment requires also just very high, increase the weight of the equipment cost of this product industrialization, seriously restricted the suitability for industrialized production of octafluoropropane.
Summary of the invention
Technical problem to be solved by this invention is, a kind of preparation method of octafluoropropane is provided, and can reduce the corrosion to equipment, improves productive rate, the purity of octafluoropropane, realizes industrialization.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of octafluoropropane, step comprises successively: (1) potassium bifluoride obtains the fluorine gas gas mixture after electrolytic tank electrolysis is processed, and described fluorine gas gas mixture is carried out to dedusting, condensation, adsorption treatment successively, and purifying is raw material fluorine gas; (2) the compressed machine pressurization of described raw material fluorine gas is rear and rare gas element evenly is mixed to get gas mixture; (3) described gas mixture is passed in the reactor that cohalt difluoride is housed, described gas mixture reacts with cohalt difluoride and obtains three cobalt oxides; (4), after having reacted, described reactor and associated pipe pipe fitting are carried out by inert gas purge and vacuumize inert gas replacement processing successively; (5) R 1216 is passed in vacuumizing the reactor after inert gas replacement is processed, described R 1216 reacts and obtains the octafluoropropane that contains impurity with described cobaltic fluoride; (6) to described reactor, octafluoropropane out carries out cooling process, and adopts sorbent material to carry out adsorption treatment to remove micro-hydrogen fluoride and moisture content; (7) described octafluoropropane after cooling, adsorption treatment is entered to rectifying tower by compressor and carry out rectification process.
As the improvement of aforesaid method, described by the process of the compressed machine pressurization of raw material fluorine gas, the pressure of described compressor is 0.01 ~ 0.9MPa; In described gas mixture, concentration of fluorine is 20% ~ 80%.
As the improvement of aforesaid method, in the process that described gas mixture reacts with cohalt difluoride, temperature of reaction is controlled at the first preset temperature range, and described the first preset temperature range is 250 ~ 350 ℃.
As the improvement of aforesaid method, described reactor temperature passes into described gas mixture after reaching described the first preset temperature range, and described gas mixture is reacted with cohalt difluoride.
As the improvement of aforesaid method, in the process that described R 1216 reacts with cobaltic fluoride, temperature of reaction is controlled at the second preset temperature range, and described preset temperature range is 200-500 ℃.
As the improvement of aforesaid method, described reactor temperature passes into described R 1216 after reaching described the second preset temperature range, and described R 1216 is reacted with cobaltic fluoride.
As the improvement of aforesaid method, in described reactor adopts, type of heating is heated.
As the improvement of aforesaid method, described sorbent material is any one in gac, silica gel, aluminum oxide, Calcium Fluoride (Fluorspan), Sodium Fluoride, molecular sieve.
As the improvement of aforesaid method, described octafluoropropane enters rectifying tower by compressor to carry out in the process of rectification process, and the pressure of rectifying tower is 0.01 ~ 0.9MPa.
As the improvement of aforesaid method, described rectifying tower comprises light constituent rectifying tower and heavy constituent rectifying tower; Described light constituent rectifying tower is for removing the light constituent impurity of the octafluoropropane after cooling, adsorption treatment; Described heavy constituent rectifying tower is for removing the heavy constituent impurity of the octafluoropropane after cooling, adsorption treatment.
Implement the present invention, there is following beneficial effect:
After the fluorine gas gas mixture carries out dedusting, condensation, adsorption treatment successively, the impurity such as hydrogen fluoride, potassium bifluoride in the fluorine gas gas mixture have been removed, purifying is raw material fluorine gas, effectively reduce the corrosion of hydrogen fluoride to reactor, the life-span of extension reactor, the material that has also reduced equipment requires, tooling cost, realizes the industrialization production of octafluoropropane simultaneously.By after the pressurization of the compressed machine of raw material fluorine gas with after rare gas element evenly mixes, then will be reacted with cohalt difluoride, can reduce the severe degree of reaction, reaction process is carried out to Effective Regulation, the corrosion of reduction fluorine gas to equipment.After having reacted, described reactor and associated pipe pipe fitting are carried out by inert gas purge and vacuumize inert gas replacement processing successively, can remove free fluorine gas residual in reactor and associated pipe pipe fitting, effectively suppress the generation of the bad side reactions such as R 1216 cracking, autohemagglutination, addition.To described reactor, octafluoropropane out carries out preparing highly purified octafluoropropane after cooling, absorption, rectification process.
The accompanying drawing explanation
Fig. 1 is the preparation method's of octafluoropropane of the present invention schema.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, the present invention is described in further detail.
Fig. 1 is the preparation method's of octafluoropropane of the present invention schema.
As shown in Figure 1, the preparation method's of described octafluoropropane step comprises successively: electrolysis, dedusting, condensation, absorption; Mix; Gas mixture reacts with cohalt difluoride; Purge, vacuumize inert gas replacement; R 1216 reacts with cobaltic fluoride; Cooling, absorption; Rectifying.
Specifically introduce the preparation method's of octafluoropropane detailed step below in conjunction with Fig. 1:
S101, potassium bifluoride obtains the fluorine gas gas mixture after electrolytic tank electrolysis is processed, and described fluorine gas gas mixture is carried out to dedusting, condensation, adsorption treatment successively, and purifying is raw material fluorine gas.
Electrolytic reaction formula: 2KHF
2→ 2KF+H
2+ F
2
Originally it should be noted that, potassium bifluoride obtains the fluorine gas gas mixture after electrolytic tank electrolysis is processed, and in wherein said fluorine gas gas mixture, containing having an appointment 90% fluorine gas, all the other are other impurity such as hydrogen fluoride and potassium bifluoride.After electrolysis, described fluorine gas gas mixture is carried out to dust removal process through fly-ash separator and remove the part potassium bifluoride, entering condensation separator carries out condensation process and removes most of hydrogen fluoride and potassium bifluoride again, finally, carry out adsorption treatment through the Sodium Fluoride adsorber again and further remove the hydrogen fluoride in the fluorine gas gas mixture, purifying is that content of fluorine is more than the 99% and basic raw material fluorine gas of fluorinated hydrogen not, effectively reduces the corrosion of hydrogen fluoride to reactor, the life-span of extension reactor.Therefore, in production process, can also reduce the material requirement of reactor equipment component and pipeline pipe fitting, thereby reduce the tooling cost of equipment Pipe-Line pipe fitting.
S102, pressurize the compressed machine of described raw material fluorine gas afterwards and rare gas element evenly is mixed to get gas mixture.
More preferably, described by the process of the compressed machine pressurization of raw material fluorine gas, the pressure of described compressor is 0.01 ~ 0.9MPa.Preferably, in described gas mixture, concentration of fluorine is 20% ~ 80%.
It should be noted that, raw material fluorine gas after compression is with after rare gas element mixes by a certain percentage, then enters reactor and cohalt difluoride prepares cobaltic fluoride, can reduce the severe degree of reaction process, reaction process is carried out effectively regulating and controlling, reduce the corrosion of fluorine gas to equipment.
Preferably, described compressor is freon compressor, and in addition, described compressor also can be used for the pressure of electrolyzer and/or reactor to be regulated.
S103, pass into described gas mixture in the reactor that cohalt difluoride is housed, and described gas mixture reacts with cohalt difluoride and obtains three cobalt oxides.
Reaction formula: 2CoF
2+ F
2→ 2CoF
3
More preferably, in the process that the fluorine gas in described gas mixture reacts with cohalt difluoride, temperature of reaction is controlled at the first preset temperature range, and described the first preset temperature range is 250 ~ 350 ℃.Described the first preset temperature range, for generating the optimum temperature range of cobaltic fluoride, can effectively improve the transformation efficiency that cohalt difluoride is converted into cobaltic fluoride.
More preferably, after described reactor temperature reaches described the first preset temperature range, then pass into described gas mixture, can make described gas mixture react more abundant with cohalt difluoride, can effectively improve the transformation efficiency that cohalt difluoride is converted into cobaltic fluoride.
Preferably, when gas mixture passes into the reactor that cohalt difluoride is housed, flow velocity is 12.5Nm
3/ h.Reactor pressure is 0.1 ~ 0.3 MPa, makes reaction more abundant, correspondingly, can regulate pressure by compressor.
S104, after having reacted, carry out by inert gas purge and vacuumize inert gas replacement processing to described reactor and associated pipe pipe fitting successively.
After having prepared cobaltic fluoride, stop to the logical gas mixture of reactor, and with rare gas element, reactor and associated pipe pipe fitting are purged, the fluorine gas remained in reactor is purged into to exhaust gas processing device, then, again reactor and associated pipe pipe fitting are vacuumized to the inert gas replacement processing, can be removed free fluorine gas residual in reactor and associated pipe pipe fitting as far as possible, effectively prevented and suppress the generation of the bad negative side reactions such as R 1216 cracking, autohemagglutination, addition.
Preferably, described rare gas element is nitrogen.
S105, pass into R 1216 in vacuumizing the reactor after inert gas replacement is processed, and described R 1216 reacts and obtains the octafluoropropane that contains impurity with described cobaltic fluoride.
Reaction formula: C
3f
6+ 2CoF
3→ C
3f
8+ 2CoF
2
More preferably, in the process that described R 1216 reacts with cobaltic fluoride, temperature of reaction is controlled at the second preset temperature range, and described preset temperature range is 200-500 ℃.Described the second preset temperature range, for generating the optimum temperature range of octafluoropropane, can effectively improve the transformation efficiency that R 1216 is converted into octafluoropropane.
More preferably, after described reactor temperature reaches described the second preset temperature range, then pass into described R 1216, make described R 1216 react more abundant with cobaltic fluoride, can effectively improve the transformation efficiency that R 1216 is converted into octafluoropropane.
More preferably, described reactor adopts interior type of heating to be heated.
Preferably, when R 1216 is passed into to reactor, flow velocity is 5.6Nm
3/ h.
S106, to described reactor, octafluoropropane out carries out cooling process, and adopts sorbent material to carry out adsorption treatment to remove micro-hydrogen fluoride and moisture content.
More preferably, described sorbent material is any one in gac, silica gel, aluminum oxide, Calcium Fluoride (Fluorspan), Sodium Fluoride, molecular sieve.
S107, enter rectifying tower by described octafluoropropane after cooling, adsorption treatment by compressor and carry out rectification process.
It should be noted that, will be from reactor octafluoropropane out can prepare highly purified octafluoropropane successively after overcooling, absorption, rectifying, thereby realize its industrialization purpose.
More preferably, described octafluoropropane compresses into by compressor the process that rectifying tower carries out rectification process, and the pressure of rectifying tower is 0.01 ~ 0.9MPa.
More preferably, described rectifying tower comprises light constituent rectifying tower and heavy constituent rectifying tower.Wherein, described light constituent rectifying tower is for removing the light constituent impurity of the octafluoropropane after cooling, adsorption treatment; Described heavy constituent rectifying tower is for removing the heavy constituent impurity of the octafluoropropane after cooling, adsorption treatment.
Preferably, but after rectifying the Returning reactor such as isolated rare gas element and a small amount of heavy constituent Perfluorocyclobutane as purging, replacement Treatment.
Below by embodiment, the present invention is described in more detail.
Embodiment 1
Reactor is fixed-bed reactor, adopts interior type of heating and establishes 8 temperature control points.In gas mixture, concentration of fluorine is 20%, and its production method is:
A, unlatching electrolyzer, controlling cell pressure is micro-negative pressure, and potassium bifluoride obtains the fluorine gas gas mixture after electrolytic tank electrolysis is processed, and the fluorine gas gas mixture is passed through to dedusting, condensation, adsorption treatment successively, and purifying is raw material fluorine gas.
B, by after the pressurization of the compressed machine of raw material fluorine gas and rare gas element evenly be mixed to get gas mixture, and, in gas mixture, concentration of fluorine is 20%.
C, temperature of reactor is risen to 300 ℃ in advance, with 12.5Nm
3the flow velocity of/h passes into reactor by gas mixture, and reactor pressure is controlled at 0.1 ~ 0.3MPa, gas mixture is reacted with cohalt difluoride and generate cobaltic fluoride.
D, then reactor and associated pipe pipe fitting are carried out by inert gas purge and vacuumize inert gas replacement processing successively.
E, maintenance reactor are in the time of 300 ℃, with 5.6Nm
3the flow velocity of/h passes into R 1216 in reactor, R 1216 is reacted with cobaltic fluoride and generate the octafluoropropane that contains impurity.
F, to described reactor, octafluoropropane out carries out cooling process, and adopts sorbent material to carry out adsorption treatment to remove micro-hydrogen fluoride and moisture content.
G, described octafluoropropane after cooling, adsorption treatment is entered to rectifying tower by compressor, rectifying separation under 0.01 ~ 0.9MPa pressure, isolated rare gas element and a small amount of heavy constituent Perfluorocyclobutane etc. Returning reactor are used as purging, replacement Treatment.
Embodiment 2
In the present embodiment, in gas mixture, concentration of fluorine is 40%, and all the other are identical with the method for implementing 1.
Embodiment 3
In the present embodiment, in gas mixture, concentration of fluorine is 60%.All the other are identical with the method for implementing 1.
The index contrast that table one is above-mentioned three embodiment:
It should be noted that, described content refers to the content of each reaction product after the rectifying tower rectifying separation.
As shown in Table 1, after adopting present method, in reaction product, the content of octafluoropropane > 99%, by product (air, tetrafluoro-methane, R 1216 etc.) content is few, and the purity of the octafluoropropane generated > 99.999%, the Zhuan Huan of R 1216 Shuais>=and 90%, make R 1216 prepare the octafluoropropane industrialization and become a reality.
As from the foregoing, after the fluorine gas gas mixture carries out dedusting, condensation, adsorption treatment successively, the impurity such as hydrogen fluoride, potassium bifluoride in the fluorine gas gas mixture have been removed, purifying is raw material fluorine gas, effectively reduce the corrosion of hydrogen fluoride to reactor, in the life-span of extension reactor, the material that has also reduced equipment simultaneously requires, tooling cost, realizes the industrialization production of octafluoropropane.
By after the pressurization of the compressed machine of raw material fluorine gas with after rare gas element evenly mixes, then will be reacted with cohalt difluoride, can reduce the severe degree of reaction, reaction process is carried out to Effective Regulation, the corrosion of reduction fluorine gas to equipment.
After having reacted, described reactor and associated pipe pipe fitting are carried out by inert gas purge and vacuumize inert gas replacement processing successively, can remove free fluorine gas residual in reactor and associated pipe pipe fitting, effectively suppress the generation of the bad side reactions such as R 1216 cracking, autohemagglutination, addition.
To described reactor, octafluoropropane out carries out preparing highly purified octafluoropropane after cooling, absorption, rectification process.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also are considered as protection scope of the present invention.
Claims (10)
1. the preparation method of an octafluoropropane, is characterized in that, described preparation method's step comprises successively:
(1) potassium bifluoride obtains the fluorine gas gas mixture after electrolytic tank electrolysis is processed, and described fluorine gas gas mixture is carried out to dedusting, condensation, adsorption treatment successively, and purifying is raw material fluorine gas;
(2) the compressed machine pressurization of described raw material fluorine gas is rear and rare gas element evenly is mixed to get gas mixture;
(3) described gas mixture is passed in the reactor that cohalt difluoride is housed, described gas mixture reacts with cohalt difluoride and obtains three cobalt oxides;
(4), after having reacted, described reactor and associated pipe pipe fitting are carried out by inert gas purge and vacuumize inert gas replacement processing successively;
(5) R 1216 is passed in vacuumizing the reactor after inert gas replacement is processed, described R 1216 reacts and obtains the octafluoropropane that contains impurity with described cobaltic fluoride;
(6) to described reactor, octafluoropropane out carries out cooling process, and adopts sorbent material to carry out adsorption treatment to remove micro-hydrogen fluoride and moisture content;
(7) described octafluoropropane after cooling, adsorption treatment is entered to rectifying tower by compressor and carry out rectification process.
2. the preparation method of octafluoropropane as claimed in claim 1, is characterized in that, described by the process of the compressed machine pressurization of raw material fluorine gas, the pressure of described compressor is 0.01 ~ 0.9MPa;
In described gas mixture, concentration of fluorine is 20% ~ 80%.
3. the preparation method of octafluoropropane as claimed in claim 1, is characterized in that, in the process that described gas mixture reacts with cohalt difluoride, temperature of reaction is controlled at the first preset temperature range, and described the first preset temperature range is 250 ~ 350 ℃.
4. the preparation method of octafluoropropane as claimed in claim 3, is characterized in that, described reactor temperature passes into described gas mixture after reaching described the first preset temperature range, and described gas mixture is reacted with cohalt difluoride.
5. the preparation method of octafluoropropane as claimed in claim 1, is characterized in that, in the process that described R 1216 reacts with cobaltic fluoride, temperature of reaction is controlled at the second preset temperature range, and described preset temperature range is 200-500 ℃.
6. the preparation method of octafluoropropane as claimed in claim 5, is characterized in that, described reactor temperature passes into described R 1216 after reaching described the second preset temperature range, and described R 1216 is reacted with cobaltic fluoride.
7. as the preparation method of claim 4 or 6 described octafluoropropanes, it is characterized in that, in described reactor adopts, type of heating is heated.
8. the preparation method of octafluoropropane as claimed in claim 1, is characterized in that, described sorbent material is any one in gac, silica gel, aluminum oxide, Calcium Fluoride (Fluorspan), Sodium Fluoride, molecular sieve.
9. the preparation method of octafluoropropane as claimed in claim 1, is characterized in that, described octafluoropropane enters rectifying tower by compressor to carry out in the process of rectification process, and the pressure of rectifying tower is 0.01 ~ 0.9MPa.
10. the preparation method of octafluoropropane as claimed in claim 1, is characterized in that, described rectifying tower comprises light constituent rectifying tower and heavy constituent rectifying tower;
Described light constituent rectifying tower is for removing the light constituent impurity of the octafluoropropane after cooling, adsorption treatment;
Described heavy constituent rectifying tower is for removing the heavy constituent impurity of the octafluoropropane after cooling, adsorption treatment.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980087A (en) * | 2014-05-20 | 2014-08-13 | 佛山市华特气体有限公司 | Method for preparing fluorating agent |
| CN106380372A (en) * | 2016-08-31 | 2017-02-08 | 中国船舶重工集团公司第七八研究所 | Octafluoropropane purifying method and purifying apparatus thereof |
| CN107540514A (en) * | 2016-06-27 | 2018-01-05 | 和立气体（上海）有限公司 | A kind of preparation method of perfluoroethane |
| CN111039749A (en) * | 2019-12-26 | 2020-04-21 | 福建德尔科技有限公司 | Preparation system and method of electronic-grade carbon tetrafluoride |
| CN112079757A (en) * | 2020-10-20 | 2020-12-15 | 山东重山光电材料股份有限公司 | Preparation and purification method of trifluoromethyl sulfur pentafluoride |
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| CN1455764A (en) * | 2001-01-15 | 2003-11-12 | 昭和电工株式会社 | Process for purifying octafluoropropane, process for preparing same and use thereof |
| CN102963870A (en) * | 2012-12-11 | 2013-03-13 | 中昊晨光化工研究院有限公司 | Method for purifying fluorine gas |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980087A (en) * | 2014-05-20 | 2014-08-13 | 佛山市华特气体有限公司 | Method for preparing fluorating agent |
| CN103980087B (en) * | 2014-05-20 | 2015-11-25 | 广东华特气体股份有限公司 | A kind of preparation method of fluorizating agent |
| CN107540514A (en) * | 2016-06-27 | 2018-01-05 | 和立气体（上海）有限公司 | A kind of preparation method of perfluoroethane |
| CN106380372A (en) * | 2016-08-31 | 2017-02-08 | 中国船舶重工集团公司第七八研究所 | Octafluoropropane purifying method and purifying apparatus thereof |
| CN106380372B (en) * | 2016-08-31 | 2019-05-21 | 中国船舶重工集团公司第七一八研究所 | A kind of purification process and purification devices of octafluoropropane |
| CN111039749A (en) * | 2019-12-26 | 2020-04-21 | 福建德尔科技有限公司 | Preparation system and method of electronic-grade carbon tetrafluoride |
| CN112079757A (en) * | 2020-10-20 | 2020-12-15 | 山东重山光电材料股份有限公司 | Preparation and purification method of trifluoromethyl sulfur pentafluoride |
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Address after: 528244 Nanhai District, Guangdong City, Foshan Province town of water and water in the west side of the head of the foot of the ridge Applicant after: GUANGDONG HUATE GASES CO., LTD. Applicant after: Suining County associating chemical industry limited liability company Address before: 528244 Nanhai District, Guangdong City, Foshan Province town of water and water in the west side of the head of the foot of the ridge Applicant before: Foshan Huate Gases Co., Ltd. Applicant before: Suining County associating chemical industry limited liability company |
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Application publication date: 20140108 |
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| RJ01 | Rejection of invention patent application after publication |