CN111153792A - Preparation device and use method of perfluoropentyl diacyl fluoride - Google Patents
Preparation device and use method of perfluoropentyl diacyl fluoride Download PDFInfo
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- CN111153792A CN111153792A CN201911399605.1A CN201911399605A CN111153792A CN 111153792 A CN111153792 A CN 111153792A CN 201911399605 A CN201911399605 A CN 201911399605A CN 111153792 A CN111153792 A CN 111153792A
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Abstract
The invention belongs to the field of fluorine chemical industry, and particularly relates to a preparation device and a use method of perfluoropentyl diacyl fluoride, wherein the preparation device comprises an ozone generation chamber, an activation chamber, a gasification chamber, a cracking chamber and a product treatment unit which are sequentially communicated; a material storage tank is arranged in the activation chamber; the storage tank is filled with metal oxide and is provided with a raw material inlet and an active substance outlet connected with the gasification chamber; the cracking chamber is provided with an oxygen inlet; a cracking catalyst is arranged in the cracking chamber; the product treatment unit comprises a 30 ℃ cold trap and a-20 ℃ cold trap which are connected by a conduit in sequence; wherein a 30 ℃ cold trap is connected with a rectification unit to obtain a high-purity product. The device of this application at first carries out the ozone activation with raw materials per fluoro cyclopentene, and the raw materials after the activation gets into and cracks with oxygen reaction in the cracking chamber to obtain the product, the collection of product, the recovery of raw materials and the separation of low boiling point accessory substance can be realized through the regulation and control of the temperature of different cold traps to the product processing unit.
Description
Technical Field
The invention belongs to the field of fluorine chemical industry, and particularly relates to a preparation device and a use method of perfluoropentyl diacyl fluoride.
Background
Perfluoroalkyl diacyl fluoride (with the general formula FOC (CF2) nCOF) is an important compound for synthesizing perfluorovinyl ether, bifunctional perfluoropolyether and bifunctional fluorinated polyurethane/polyamide monomer, and the synthesis of high-performance functional fluorinated polymer material by using the perfluoroalkyl diacyl fluoride as a raw material is one of the scientific research subjects of the current fluorinated materials. The perfluoroalkyl diacyl fluoride can be used for preparing amorphous optical transparent polymers, perfluorocarboxylic acid type ion exchange resins, perfluoroether rubber and the like by copolymerizing perfluorovinyl ether monomer Cytop and tetrafluoroethylene. These polymers have unique chemical stability, corrosion resistance, fire resistance, hydrophobic and oleophobic properties, antifouling properties, etc. The application of the high-voltage optical fiber has been deeply applied to various social production and living fields of communication, war industry, electronics, aerospace, corrosion prevention, chemical engineering, surface protection and the like, and is widely applied to industrial and commercial activities of optical fiber, high-grade buildings, aircraft manufacturing, precision machining, cultural relic protection, high-voltage insulation, ocean development, coating paint and the like.
The research and development of a new synthesis method of perfluoroalkyl diacyl fluoride is always an important direction for fluorine chemists at home and abroad, and the application provides a preparation method of perfluoropentyl diacyl fluoride and matches with an applicable preparation device of perfluoropentyl diacyl fluoride.
Disclosure of Invention
The invention aims to provide a preparation device and a using method of perfluoropentyl diacyl fluoride.
In order to achieve the purpose, the invention adopts the following technical scheme:
a perfluoropentyl diacyl fluoride preparation device comprises an ozone generation chamber, an activation chamber, a gasification chamber, a cracking chamber and a product treatment unit which are sequentially communicated; a material storage tank is arranged in the activation chamber; the storage tank is filled with metal oxide and is provided with a raw material inlet and an activator outlet connected with the gasification chamber; the cracking chamber is provided with an oxygen inlet; a cracking catalyst is arranged in the cracking chamber; the product processing unit comprises a cold trap at 30 ℃ and a cold trap at-20 ℃ which are connected by a conduit in sequence; wherein the 30 ℃ cold trap is connected with a rectification unit to obtain a high-purity product.
A 10 ℃ cold trap is arranged between the 30 ℃ cold trap and the-20 ℃ cold trap; the outlet of the 10 ℃ cold trap is communicated with the raw material inlet of the storage tank through a pressure pump.
A gas flowmeter is arranged between the gasification chamber and the cracking chamber;
wherein, the metal oxide in the material storage tank is one of TiO2, Fe2O3, Fe3O4, CoO, Co3O4, Ag2O and Pd 2O. The temperature of the storage tank is-10 ℃ to 20 ℃, and the activation reaction is carried out under the condition of light irradiation; the light irradiation time was: 10-90 min.
The reaction process in the cracking chamber is that oxygen and activated cyclic olefin are used as raw materials and react under the action of a catalyst to prepare the catalyst; wherein the molar ratio of oxygen to the cyclic olefin is 20:1-1: 10; the contact reaction time is 0.1s to 200 s; the reaction pressure is 0-1 MPa; the reaction temperature is 200-700 ℃. The catalyst is a supported catalyst, and the active component is one or a mixture of more of AgO, Al2O3, CuO, AgF, NaF, KF, RbF and CsF.
The product obtained after cracking firstly enters a cold trap at 30 ℃, the gas guide tube needs to go deep into the bottom of the cold trap at the moment for collecting the diacyl fluoride generated by cracking, and the obtained diacyl fluoride is rectified and purified by a rectifying unit to obtain a high-purity diacyl fluoride product. The gas-guide tube is led out from the upper part of the cold trap at 30 ℃ and enters the bottom of the cold trap at 10 ℃ for collecting the uncracked perfluorocyclopentene, and the gas-guide tube is led out from the upper part of the cold trap at 10 ℃ and enters the bottom of the cold trap at-20 ℃ for collecting low-boiling-point byproducts possibly generated in the cracking process. The liquid discharging valve at the bottom of the 10 ℃ cold trap is connected with a raw material inlet of the storage tank, uncracked perfluorocyclopentene can be circularly placed into the storage tank for activation and cracking, and a pressure pump is connected to a pipeline between the liquid discharging valve and the raw material inlet of the storage tank and used for assisting liquid to enter the storage tank under certain pressure.
Compared with the prior art, the invention has the beneficial effects that:
the device is utilized to firstly carry out ozone activation on raw material perfluorocyclopentene, the activated raw material enters a cracking chamber to react with oxygen for cracking so as to obtain a product, and a product processing unit can realize the collection of the product, the recovery of the raw material and the separation of low-boiling-point byproducts through the regulation and control of the temperatures of different cold traps; the device is reasonable in design, and can realize separation of products and cyclic utilization of raw materials.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the following preferred embodiments.
FIG. 1 shows a perfluoropentyl diacyl fluoride manufacturing apparatus, comprising an ozone generation chamber 1, an activation chamber 2, a gasification chamber 4, a cracking chamber 5, and a product treatment unit, which are connected in series; a material storage tank 3 is arranged in the activation chamber; the storage tank is filled with metal oxide and is provided with a raw material inlet and an activator outlet connected with the gasification chamber 4; the cracking chamber 5 is provided with an oxygen inlet; a cracking catalyst is arranged in the cracking chamber; the product processing unit comprises a cold trap 6 at 30 ℃ and a cold trap 8 at-20 ℃ which are connected in sequence by using a conduit; wherein the 30 ℃ cold trap is connected with a rectification unit 9 to obtain a high-purity product. A 10 ℃ cold trap 7 is arranged between the 30 ℃ cold trap and the-20 ℃ cold trap; the outlet of the 10 ℃ cold trap is communicated with the raw material inlet of the storage tank 3 through a pressure pump. A gas flowmeter is arranged between the gasification chamber and the cracking chamber;
the application method of the device comprises the following steps: ozone is led into an activation chamber with an ozone irradiation lamp arranged at the upper part, a temperature-controllable material storage tank is arranged in the activation chamber, a vertical irradiation mode is adopted during irradiation, namely the direction of a particle beam is vertical to the surface of liquid, metal oxide is arranged in the material storage tank, the raw material perfluorocyclopentene is added, the reaction temperature is controlled to be-10-20 ℃, the irradiation time is 10-90min, a liquid discharge valve at the bottom of the material storage tank is opened after irradiation is finished, the activated perfluorocyclopentene is placed into a vaporization chamber for slow vaporization, and the temperature rise process of the vaporization chamber adopts the programmed temperature rise: keeping the temperature at 20 ℃ for 5-10min, and then increasing the temperature to 30-40 ℃ at the speed of 0.5-1 ℃/min. The gasified raw material enters a cracking chamber, and is heated and cracked in the presence of oxygen, and a cracking catalyst is arranged in the cracking chamber; the feeding molar ratio of the gasified raw material to the oxygen is controlled to be 20:1-1:10 by a gas flow meter in the cracking process. The contact reaction time is 0.1s to 200 s; the reaction pressure is 0-1 MPa; the reaction temperature is 200-700 ℃. Wherein, the metal oxide in the material storage tank is one of TiO2, Fe2O3, Fe3O4, CoO, Co3O4, Ag2O and Pd 2O. The cracking catalyst is a supported catalyst, and the active component is one or a mixture of more of AgO, Al2O3, CuO, AgF, NaF, KF, RbF and CsF.
The product obtained after cracking firstly enters a cold trap at 30 ℃, the gas guide tube needs to go deep into the bottom of the cold trap at the moment for collecting the diacyl fluoride generated by cracking, and the obtained diacyl fluoride is rectified and purified by a rectifying unit to obtain a high-purity diacyl fluoride product. The gas-guide tube is led out from the upper part of the cold trap at 30 ℃ and enters the bottom of the cold trap at 10 ℃ for collecting the uncracked perfluorocyclopentene, and the gas-guide tube is led out from the upper part of the cold trap at 10 ℃ and enters the bottom of the cold trap at-20 ℃ for collecting low-boiling-point byproducts possibly generated in the cracking process. The liquid discharging valve at the bottom of the 10 ℃ cold trap is connected with a raw material inlet of the storage tank, uncracked perfluorocyclopentene can be circularly placed into the storage tank for activation and cracking, and a pressure pump is connected to a pipeline between the liquid discharging valve and the raw material inlet of the storage tank and used for assisting liquid to enter the storage tank under certain pressure.
Wherein the parameters of the various examples are varied and the yields are shown in table 1. Comparative example 1: the comparative example differs from example 1 only in that perfluorocyclopentene was added directly to the cracking chamber without pre-activation to react with oxygen.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | |
| Metal oxides | TiO2 | Ag2O | TiO2 | Ag2O | / |
| Catalyst and process for preparing same | NaF | NaF | KF | KF | NaF |
| Perfluoro cyclopentene: oxygen gas | 20:1 | 1:1 | 1:1 | 1:10 | 1:1 |
| Reaction temperature/. degree.C | 200 | 350 | 350 | 700 | 350 |
| End time/s | 30 | 60 | 100 | 200 | 100 |
| Yield of | 76.2％ | 85.1％ | 86.9％ | 92.3％ | 62.3％ |
The device for preparing perfluoropentyl diacyl fluoride comprises a raw material perfluorocyclopentene, a product processing unit, a reaction chamber and a cooling chamber, wherein the raw material perfluorocyclopentene is subjected to ozone activation, the activated raw material enters the cracking chamber to react with oxygen to crack so as to obtain a product, and the product processing unit can realize the collection of the product, the recovery of the raw material and the separation of low-boiling-point byproducts through the regulation and control of the temperatures of different cold traps; the device is reasonable in design, and can realize separation of products and cyclic utilization of raw materials.
The above description is only a preferred embodiment of the present invention, and for those skilled in the art, the present invention should not be limited by the description of the present invention, which should be interpreted as a limitation.
Claims (7)
1. The device for preparing perfluoropentyl diacyl fluoride is characterized by comprising an ozone generation chamber, an activation chamber, a gasification chamber, a cracking chamber and a product treatment unit which are sequentially communicated; a material storage tank is arranged in the activation chamber; the storage tank is filled with metal oxide and is provided with a raw material inlet and an activator outlet connected with the gasification chamber; the cracking chamber is provided with an oxygen inlet; a cracking catalyst is arranged in the cracking chamber; the product processing unit comprises a cold trap at 30 ℃ and a cold trap at-20 ℃ which are connected by a conduit in sequence; wherein the 30 ℃ cold trap is connected with a rectification unit to obtain a high-purity product.
2. The apparatus according to claim 1, wherein a 10 ℃ cold trap is provided between said 30 ℃ cold trap and said-20 ℃ cold trap; the outlet of the 10 ℃ cold trap is communicated with the raw material inlet of the storage tank through a pressure pump.
3. The apparatus for producing perfluoropentyl diacyl fluoride as claimed in claim 1, wherein a gas flow meter is disposed between said vaporizing chamber and said cracking chamber.
4. The use method of the preparation device according to any one of claims 1 to 3, characterized by comprising the following steps of introducing ozone into an activation chamber with an ozone irradiation lamp at the upper part, arranging a temperature-controllable material storage tank in the activation chamber, adding the raw material perfluorocyclopentene into the material storage tank, controlling the reaction temperature to be-10-20 ℃ and the irradiation time to be 10-90min, opening a liquid discharge valve at the bottom of the material storage tank after the irradiation is finished, and putting the activated perfluorocyclopentene into a vaporization chamber for vaporization;
the gasified raw material enters a cracking chamber, and is heated and cracked in the presence of oxygen, and a cracking catalyst is arranged in the cracking chamber; controlling the feeding molar ratio of the gasified raw material to the oxygen to be 20:1-1:10 by a gas flowmeter in the cracking process; the contact reaction time is 0.1s to 200 s; the reaction pressure is 0-1 MPa; the reaction temperature is 200-700 ℃;
the product obtained after cracking firstly enters a cold trap at 30 ℃ for collecting the diacyl fluoride generated by cracking, and the obtained diacyl fluoride is rectified and purified by a rectifying unit to obtain a high-purity diacyl fluoride product; then enters the bottom of a cold trap at 10 ℃ for collecting the uncracked perfluorocyclopentene, and finally enters the bottom of a cold trap at-20 ℃ for collecting low-boiling point byproducts possibly generated in the cracking process.
5. The use of claim 4, wherein the vaporizer warming process employs a programmed temperature: keeping the temperature at 20 ℃ for 5-10min, and then increasing the temperature to 30-40 ℃ at the speed of 0.5-1 ℃/min.
6. The use method of claim 4, wherein the metal oxide in the storage tank is one of TiO2, Fe2O3, Fe3O4, CoO, Co3O4, Ag2O and Pd 2O.
7. The use method of claim 4, wherein the cracking catalyst is a supported catalyst, and the active component is one or a mixture of more of AgO, Al2O3, CuO, AgF, NaF, KF, RbF and CsF.
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| CN201911399605.1A CN111153792B (en) | 2019-12-30 | 2019-12-30 | Preparation device and application method of perfluoro amyl diacid fluoride |
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| CN201911399605.1A CN111153792B (en) | 2019-12-30 | 2019-12-30 | Preparation device and application method of perfluoro amyl diacid fluoride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112811978A (en) * | 2021-04-22 | 2021-05-18 | 北京宇极科技发展有限公司 | Preparation method of Z-1,3,3, 3-tetrafluoropropene |
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| JPS5159818A (en) * | 1974-11-15 | 1976-05-25 | Asahi Chemical Ind | |
| US4151200A (en) * | 1977-10-25 | 1979-04-24 | Asahi Glass Company Ltd. | Process for producing polyfluorodiacyl fluoride |
| US4316986A (en) * | 1980-09-23 | 1982-02-23 | E. I. Dupont De Nemours & Company | Preparation of difluoromalonyl fluoride |
| JPH01149749A (en) * | 1988-01-13 | 1989-06-12 | Tokuyama Soda Co Ltd | Production of perfluoromalonyl fluoride |
| CN109503366A (en) * | 2018-11-30 | 2019-03-22 | 天津市长芦化工新材料有限公司 | Hexafluoropropylene dimmer prepares the method and perfluor isobutyl ether and application of perfluor isobutyl ether |
| CN109750314A (en) * | 2018-12-29 | 2019-05-14 | 中船重工（邯郸）派瑞特种气体有限公司 | A kind of preparation method of the double acyl fluorides of perfluoroalkyl |
| CN211814212U (en) * | 2019-12-30 | 2020-10-30 | 天津市长芦化工新材料有限公司 | Preparation facilities of perfluor pentyl diacyl fluorine |
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2019
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5159818A (en) * | 1974-11-15 | 1976-05-25 | Asahi Chemical Ind | |
| US4151200A (en) * | 1977-10-25 | 1979-04-24 | Asahi Glass Company Ltd. | Process for producing polyfluorodiacyl fluoride |
| US4316986A (en) * | 1980-09-23 | 1982-02-23 | E. I. Dupont De Nemours & Company | Preparation of difluoromalonyl fluoride |
| JPH01149749A (en) * | 1988-01-13 | 1989-06-12 | Tokuyama Soda Co Ltd | Production of perfluoromalonyl fluoride |
| CN109503366A (en) * | 2018-11-30 | 2019-03-22 | 天津市长芦化工新材料有限公司 | Hexafluoropropylene dimmer prepares the method and perfluor isobutyl ether and application of perfluor isobutyl ether |
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| CN211814212U (en) * | 2019-12-30 | 2020-10-30 | 天津市长芦化工新材料有限公司 | Preparation facilities of perfluor pentyl diacyl fluorine |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112811978A (en) * | 2021-04-22 | 2021-05-18 | 北京宇极科技发展有限公司 | Preparation method of Z-1,3,3, 3-tetrafluoropropene |
| CN112811978B (en) * | 2021-04-22 | 2021-07-16 | 泉州宇极新材料科技有限公司 | Preparation method of Z-1,3,3, 3-tetrafluoropropene |
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