CN115584020A - Production method for preparing perfluoropolyether with peroxide by photo-oxidative polymerization - Google Patents
Production method for preparing perfluoropolyether with peroxide by photo-oxidative polymerization Download PDFInfo
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- 239000010702 perfluoropolyether Substances 0.000 title claims abstract description 92
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 69
- 150000002978 peroxides Chemical class 0.000 title claims abstract description 66
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 54
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 74
- 150000001336 alkenes Chemical class 0.000 claims abstract description 74
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 74
- 239000011737 fluorine Substances 0.000 claims abstract description 74
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000000047 product Substances 0.000 claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- 239000007806 chemical reaction intermediate Substances 0.000 claims abstract description 42
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000001301 oxygen Substances 0.000 claims abstract description 34
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 34
- 238000002360 preparation method Methods 0.000 claims abstract description 26
- 239000007791 liquid phase Substances 0.000 claims abstract description 19
- 230000001590 oxidative effect Effects 0.000 claims abstract description 18
- 238000001704 evaporation Methods 0.000 claims abstract description 4
- 238000005336 cracking Methods 0.000 claims description 44
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 33
- 238000007872 degassing Methods 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 27
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 25
- 239000007795 chemical reaction product Substances 0.000 claims description 25
- 238000010574 gas phase reaction Methods 0.000 claims description 25
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- 238000000034 method Methods 0.000 claims description 21
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- 239000012467 final product Substances 0.000 claims description 10
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 6
- 230000009471 action Effects 0.000 claims description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 6
- 239000006227 byproduct Substances 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 6
- 238000000199 molecular distillation Methods 0.000 claims description 6
- 239000012074 organic phase Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 6
- 230000011218 segmentation Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000006555 catalytic reaction Methods 0.000 claims description 5
- 238000004590 computer program Methods 0.000 claims description 5
- 238000007539 photo-oxidation reaction Methods 0.000 claims description 4
- LGPPATCNSOSOQH-UHFFFAOYSA-N 1,1,2,3,4,4-hexafluorobuta-1,3-diene Chemical compound FC(F)=C(F)C(F)=C(F)F LGPPATCNSOSOQH-UHFFFAOYSA-N 0.000 claims description 3
- MIZLGWKEZAPEFJ-UHFFFAOYSA-N 1,1,2-trifluoroethene Chemical group FC=C(F)F MIZLGWKEZAPEFJ-UHFFFAOYSA-N 0.000 claims description 3
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 claims description 3
- FDMFUZHCIRHGRG-UHFFFAOYSA-N 3,3,3-trifluoroprop-1-ene Chemical compound FC(F)(F)C=C FDMFUZHCIRHGRG-UHFFFAOYSA-N 0.000 claims description 3
- 239000005711 Benzoic acid Substances 0.000 claims description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- 235000010233 benzoic acid Nutrition 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 3
- NDMMKOCNFSTXRU-UHFFFAOYSA-N 1,1,2,3,3-pentafluoroprop-1-ene Chemical compound FC(F)C(F)=C(F)F NDMMKOCNFSTXRU-UHFFFAOYSA-N 0.000 claims description 2
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 claims description 2
- 125000002081 peroxide group Chemical group 0.000 claims 7
- 238000003776 cleavage reaction Methods 0.000 claims 1
- 239000007858 starting material Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 8
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- 238000004886 process control Methods 0.000 abstract description 3
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- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- 238000003491 array Methods 0.000 description 2
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- 230000005494 condensation Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
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- 238000011112 process operation Methods 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 pentafluoropropylene, hexafluoropropylene Chemical group 0.000 description 1
- 229920005548 perfluoropolymer Polymers 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/002—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds
- C08G65/005—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens
- C08G65/007—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from unsaturated compounds containing halogens containing fluorine
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/123—Ultra-violet light
Abstract
The invention belongs to the technical field of organic chemistry, and discloses a production method for preparing perfluoropolyether with peroxide by photo-oxidative polymerization, wherein fluorine-containing olefin is fed into a photopolymerization kettle from a liquid-phase feed inlet, and oxygen is continuously fed into the photopolymerization kettle from an oxygen channel; carrying out oxidative polymerization reaction under the irradiation of an ultraviolet generator to obtain a reaction intermediate product; and then evaporating and recovering to prepare the peroxide-containing perfluoropolyether product. According to the production method for preparing the perfluoropolyether with peroxide through photo-oxidative polymerization, the production preparation process of the perfluoropolyether with peroxide is realized through ultraviolet catalytic oxidative polymerization, and under the coordination of specific reaction equipment and process control thereof, the production is simple and obvious in effect, the operation efficiency can be greatly increased, and the cost is reduced; meanwhile, the fluorine-containing olefin with high purity can be obtained, and the yield and the product purity are high; the reaction intermediate product is obtained, so that the discharge of three wastes is reduced, the environment is protected, the economic benefit is obvious, and the large-scale industrial production is facilitated.
Description
Technical Field
The invention belongs to the technical field of organic chemistry, and particularly relates to a production method for preparing perfluoropolyether with peroxide by photo-oxidative polymerization.
Background
Currently, perfluoropolyether (PFPE) is a synthetic polymer that is liquid at room temperature, and was studied in the first 60 th century, and is a relatively special perfluoropolymer compound that has characteristics of heat resistance, oxidation resistance, radiation resistance, corrosion resistance, non-flammability, and the like, and has been used for very reliable lubrication and sealing in advanced fields such as military, aerospace, nuclear industry, and the like for decades. Perfluoropolyethers are now widely used in many fields, such as chemical, electronic, electrical, mechanical, nuclear, and aerospace industries.
Although the microchannel reactor has very high mass transfer and heat transfer effects, the microchannel reactor is easily blocked by possible coking, solid particles, solid impurities and the like, so that the industrial production cannot be continuously carried out, and meanwhile, the microchannel reactor is very high in design and manufacturing cost as a novel reaction device, so that the difficulty in detecting and controlling equipment is increased and the process operation cost is greatly increased when the microchannel reactor is popularized and applied in the high-energy industrial production process.
Through the above analysis, the problems and defects of the prior art are as follows:
(1) The existing microchannel reactor for preparing perfluoropolyether is easy to be blocked by possible coking, solid particles, solid impurities and the like, so that the industrial production cannot be continuously carried out.
(2) The existing microchannel reactor for preparing perfluoropolyether has high design and manufacturing cost, not only increases the difficulty of equipment detection and control, but also greatly improves the process operation cost.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a production method for preparing peroxide-bearing perfluoropolyether by photo-oxidative polymerization.
The present invention is achieved by a production method for producing a peroxide-carrying perfluoropolyether by photooxidative polymerization, comprising:
feeding fluorine-containing olefin into the photopolymerization kettle from a liquid-phase feed inlet, and continuously feeding oxygen into the photopolymerization kettle from an oxygen channel; carrying out oxidative polymerization reaction under the irradiation of an ultraviolet generator to obtain a reaction intermediate product; and then evaporating and recovering to prepare the peroxide-containing perfluoropolyether product.
Further, the production method for preparing the peroxide-bearing perfluoropolyether by photo-oxidative polymerization comprises the following steps:
step one, carrying out pretreatment operation on raw materials for producing perfluoropolyether: obtaining a fluorine-containing olefin crude product and carrying out cracking reaction to obtain a cracking product; carrying out catalytic reaction on the cracking product to obtain a gas-phase reaction product; carrying out gas-liquid separation on the gas-phase reaction product, and then sending the gas-phase reaction product into a fluorine-containing olefin production system to obtain high-purity fluorine-containing olefin;
step two, preparing an intermediate product of the photo-oxidative polymerization reaction: feeding high-purity fluorine-containing olefin into a photopolymerization kettle, and carrying out oxidative polymerization reaction with oxygen under the irradiation of an ultraviolet light generator to obtain an intermediate product; feeding the reaction intermediate product into a degassing tower for degassing treatment to obtain a final reaction intermediate product;
step three, preparing the final product of perfluoropolyether with peroxide: placing the final reaction intermediate product in a three-neck flask, introducing nitrogen for reaction, cooling to normal temperature, and adding methanol; the polymer is precipitated and the unreacted raw material is washed out, the solvent is removed by distillation under reduced pressure, and the fraction is cut to obtain the perfluoropolyether with peroxide.
Further, the method for pretreating raw materials for producing perfluoropolyether in the first step comprises the following steps:
(1) Obtaining a fluorine-containing olefin crude product, wherein the fluorine-containing olefin crude product is any one of vinylidene fluoride, trifluoroethylene, trifluoropropene, tetrafluoroethylene, pentafluoropropene, hexafluoropropylene or hexafluorobutadiene;
(2) Putting the fluorine-containing olefin crude product into a cracking device for cracking reaction, and reacting hydrogen chloride and glycerol in the cracking gas under the action of a catalyst to obtain a gas-phase reaction product;
(3) And (3) condensing the gas-phase reaction product in a condensing device, then carrying out gas-liquid separation to obtain a gas phase and a liquid phase, and sending the gas phase into a fluorine-containing olefin production system to prepare the high-purity fluorine-containing olefin.
Further, the temperature of the cracking reaction in the step (2) is 90-160 ℃, the pressure of the reaction is 0.2-0.5 MPa, and the reaction time is 8-36 h; the molar ratio of hydrogen chloride to glycerin in the fluorine-containing olefin cracking gas is 3-8: 1, the dosage of the catalyst is 5-30% of the molar weight of glycerol;
the catalyst in the step (2) is selected from any one or more of acetic acid, propionic acid, succinic acid, adipic acid, sebacic acid, suberic acid, benzoic acid or terephthalic acid;
and (3) after gas-liquid separation, layering the liquid phase to obtain an inorganic phase and an organic phase, and returning the organic phase to the cracking device for continuous cracking reaction.
Further, the preparation method of the photo-oxidative polymerization intermediate product in the second step comprises:
(1) Feeding the high-purity fluorine-containing olefin prepared in the step one into a photopolymerization kettle through a liquid-phase feed inlet, and continuously feeding oxygen into the photopolymerization kettle through an oxygen channel;
(2) Uniformly mixing high-purity fluorine-containing olefin and oxygen in a photopolymerization reaction kettle, and then carrying out oxidative polymerization reaction under the irradiation of an ultraviolet generator to obtain a reaction intermediate product;
(3) And (3) feeding the reaction intermediate product into a degassing tower, degassing for 1-3 h at the temperature of 30-35 ℃, and removing the by-product and unreacted oxygen to obtain the final reaction intermediate product.
Further, the preparation method of the final product perfluoropolyether with peroxide in the third step comprises the following steps:
(1) Placing the final reaction intermediate product obtained in the step two into a three-neck flask, introducing nitrogen, stirring at normal temperature for 20-40 min, heating to 55-75 ℃, and stirring again for reaction for 1-3 h;
(2) After the reaction is finished, cooling to normal temperature, adding methanol, precipitating the polymer, washing out unreacted raw materials, and removing the solvent by reduced pressure distillation to obtain perfluoropolyether with peroxide;
(3) And (3) performing fraction segmentation on the perfluoropolyether with peroxide of the final product obtained in the step (2) by adopting molecular distillation to obtain perfluoropolyethers with peroxide of different average molecular weights.
Another object of the present invention is to provide a production system for producing a peroxide-bearing perfluoropolyether by photo-oxidative polymerization, which employs the production method for producing a peroxide-bearing perfluoropolyether by photo-oxidative polymerization, the production system for producing a peroxide-bearing perfluoropolyether by photo-oxidative polymerization comprising:
a photopolymerization reaction kettle provided with an ultraviolet generator and a stirrer;
the upper part of the photopolymerization reaction kettle is provided with a liquid phase feed inlet, a gas phase feed inlet and a gas phase outlet, a gas distributor is communicated with the gas phase feed inlet to form an oxygen channel, and a stirrer is positioned below the outlet of the gas distributor;
the production system for preparing the peroxide-bearing perfluoropolyether through photo-oxidation polymerization also comprises a central processing module; the central processing module is sequentially connected with the fluorine-containing olefin crude product pretreatment module, the high-purity fluorine-containing olefin preparation module, the intermediate product degassing module and the perfluoropolyether preparation module, and is used for coordinating and controlling the normal operation of each module of the production system of the perfluoropolyether with peroxide through the central processing unit;
the pretreatment module of the fluorine-containing olefin crude product is used for placing the fluorine-containing olefin crude product into a cracking device for cracking reaction, and reacting the cracking product under the action of a catalyst to obtain a gas-phase reaction product;
the high-purity fluorine-containing olefin preparation module is used for condensing the gas-phase reaction product in a condensing device, then carrying out gas-liquid separation, and sending the gas phase into a fluorine-containing olefin production system to prepare high-purity fluorine-containing olefin;
the intermediate product preparation module is used for feeding high-purity fluorine-containing olefin into the photopolymerization reaction kettle through the liquid phase feed port and carrying out oxidative polymerization reaction on the high-purity fluorine-containing olefin and oxygen under the irradiation of the ultraviolet generator to obtain an intermediate product;
the intermediate product degassing module is used for sending the reaction intermediate product into a degassing tower, degassing for 1-3 h at the temperature of 30-35 ℃, and removing the by-products and unreacted oxygen to obtain a final reaction intermediate product;
the perfluoropolyether preparation module is used for placing the final reaction intermediate product into a three-neck flask, introducing nitrogen gas for reaction, cooling to normal temperature, and adding methanol; and precipitating the polymer, washing out unreacted raw materials, removing the solvent by reduced pressure distillation, and performing fraction segmentation by molecular distillation to obtain the perfluoropolyether with peroxide.
It is another object of the present invention to provide a computer program product stored on a computer readable medium, comprising a computer readable program for providing a user input interface for applying the steps of the method for producing a peroxide-containing perfluoropolyether by photo-oxidative polymerization described herein when the computer program product is executed on an electronic device.
It is another object of the present invention to provide a computer-readable storage medium storing instructions that, when executed on a computer, cause the computer to apply the steps of the method for producing a peroxide-bearing perfluoropolyether by photo-oxidative polymerization.
Another object of the present invention is to provide an information data processing terminal, which is used for implementing the production system for preparing peroxide-containing perfluoropolyether by photo-oxidative polymerization.
In combination with the technical solutions and the technical problems to be solved, please analyze the advantages and positive effects of the technical solutions to be protected in the present invention from the following aspects:
first, aiming at the technical problems existing in the prior art and the difficulty in solving the problems, the technical problems to be solved by the technical scheme of the present invention are closely combined with results, data and the like in the research and development process, and some creative technical effects are brought after the problems are solved. The specific description is as follows:
in the production method for preparing the perfluoropolyether with peroxide by photo-oxidative polymerization, the cracking product is obtained by carrying out cracking reaction on the obtained fluorine-containing olefin crude product; carrying out catalytic reaction on the cracking product to obtain a gas-phase reaction product; the gas-phase reaction product is subjected to gas-liquid separation and then is sent to a fluorine-containing olefin production system, so that the fluorine-containing olefin with high purity can be obtained, the yield and the product purity are high, and the economic benefit is good. Sending high-purity fluorine-containing olefin into a photopolymerization kettle, and carrying out oxidative polymerization reaction with oxygen under the irradiation of an ultraviolet light generator to obtain an intermediate product; the reaction intermediate product is sent into a degassing tower for degassing treatment, so that the final reaction intermediate product can be obtained, the discharge of three wastes is reduced, and the method is green and environment-friendly. Placing the final reaction intermediate product into a three-neck flask, introducing nitrogen for reaction, cooling to normal temperature, and adding methanol; the polymer is precipitated and unreacted raw materials are washed out, the solvent is removed by reduced pressure distillation, and the fraction is cut, so that the final perfluoropolyether with peroxide can be obtained, the economic benefit is remarkable, and the large-scale industrial production is facilitated.
Secondly, considering the technical scheme as a whole or from the perspective of products, the technical effect and advantages of the technical scheme to be protected by the invention are specifically described as follows:
the method for preparing the perfluorinated polyether with peroxide by photo-oxidative polymerization realizes the production and preparation process of the perfluorinated polyether with peroxide by adopting ultraviolet light catalytic oxidative polymerization, has simple manufacture and obvious effect under the coordination of specific reaction equipment and process control thereof, and can greatly increase the operation efficiency and reduce the cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of a process for producing a perfluoropolyether with peroxide by photo-oxidative polymerization according to the embodiment of the present invention;
FIG. 2 is a flow chart of a method for pretreating a raw material for producing perfluoropolyether according to an embodiment of the present invention;
FIG. 3 is a flow chart of a method for preparing an intermediate product of a photo-oxidative polymerization reaction according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
In view of the problems of the prior art, the present invention provides a production method for preparing peroxide-containing perfluoropolyether by photo-oxidative polymerization, and the present invention is described in detail below with reference to the accompanying drawings.
1. Illustrative embodiments are explained. This section is an explanatory embodiment expanding on the claims so as to fully understand how the present invention is embodied by those skilled in the art.
The production method for preparing the peroxide-containing perfluoropolyether by photo-oxidative polymerization, provided by the embodiment of the invention, comprises the following steps: feeding fluorine-containing olefin into the photopolymerization kettle from a liquid-phase feed inlet, and continuously feeding oxygen into the photopolymerization kettle from an oxygen channel; carrying out oxidative polymerization reaction under the irradiation of an ultraviolet generator to obtain a reaction intermediate product; and then evaporating and recovering to prepare the peroxide-containing perfluoropolyether product.
According to the method for preparing the peroxide-containing perfluoropolyether through photo-oxidative polymerization, provided by the embodiment of the invention, the production and preparation of the peroxide-containing perfluoropolyether are realized through ultraviolet light catalytic oxidative polymerization, and under the coordination of specific reaction equipment and process control, the preparation is simple and obvious in effect, the operation efficiency can be greatly increased, and the cost is reduced.
As shown in FIG. 1, the production method for preparing perfluoropolyether with peroxide by photo-oxidative polymerization provided by the embodiment of the invention comprises the following steps:
s101, carrying out pretreatment operation on raw materials for producing perfluoropolyether: obtaining a fluorine-containing olefin crude product and carrying out cracking reaction to obtain a cracking product; carrying out catalytic reaction on the cracking product to obtain a gas-phase reaction product; gas-liquid separation is carried out on the gas-phase reaction product, and then the gas-phase reaction product is sent into a fluorine-containing olefin production system to obtain high-purity fluorine-containing olefin;
s102, preparing an intermediate product of the photo-oxidative polymerization reaction: feeding high-purity fluorine-containing olefin into a photopolymerization kettle, and carrying out oxidative polymerization reaction with oxygen under the irradiation of an ultraviolet light generator to obtain an intermediate product; feeding the reaction intermediate product into a degassing tower for degassing treatment to obtain a final reaction intermediate product;
s103, preparing the final product, namely the perfluoropolyether with peroxide: placing the final reaction intermediate product into a three-neck flask, introducing nitrogen for reaction, cooling to normal temperature, and adding methanol; the polymer is precipitated and the unreacted raw material is washed out, the solvent is removed by distillation under reduced pressure, and the fraction is cut to obtain the perfluoropolyether with peroxide.
As shown in fig. 2, the method for pretreating a raw material for producing perfluoropolyether in step S101 according to the embodiment of the present invention includes:
s201, obtaining a fluorine-containing olefin crude product;
s202, placing the fluorine-containing olefin crude product into a cracking device for cracking reaction, and reacting hydrogen chloride and glycerol in cracking gas under the action of a catalyst to obtain a gas-phase reaction product;
s203, placing the gas-phase reaction product in a condensing device for condensation, then carrying out gas-liquid separation to obtain a gas phase and a liquid phase, and sending the gas phase into a fluorine-containing olefin production system to prepare the high-purity fluorine-containing olefin.
In the step S201 provided in the embodiment of the present invention, the fluorine-containing olefin crude product is selected from any one of vinylidene fluoride, trifluoroethylene, trifluoropropene, tetrafluoroethylene, pentafluoropropylene, hexafluoropropylene, or hexafluorobutadiene;
the temperature of the cracking reaction in the step S202 provided by the embodiment of the invention is 90-160 ℃, the pressure of the reaction is 0.2-0.5 MPa, and the reaction time is 8-36 h; the mol ratio of the hydrogen chloride to the glycerin in the fluorine-containing olefin cracking gas is 3-8: 1, the dosage of the catalyst is 5 to 30 percent of the molar weight of the glycerol.
The catalyst in step S202 provided in the embodiment of the present invention is selected from any one or more of acetic acid, propionic acid, succinic acid, adipic acid, sebacic acid, suberic acid, benzoic acid, and terephthalic acid.
In step S203 provided in the embodiment of the present invention, after performing gas-liquid separation, the liquid phase is layered to obtain an inorganic phase and an organic phase, and the organic phase is returned to the cracking apparatus to continue the cracking reaction.
In the production method for preparing perfluoropolyether with peroxide by photo-oxidative polymerization provided by the embodiment of the invention, a cracking product is obtained by carrying out cracking reaction on the obtained fluorine-containing olefin crude product; carrying out catalytic reaction on the cracking product to obtain a gas-phase reaction product; the gas-phase reaction product is subjected to gas-liquid separation and then is sent to a fluorine-containing olefin production system, so that the fluorine-containing olefin with high purity can be obtained, the yield and the product purity are high, and the economic benefit is good.
As shown in fig. 3, the method for preparing the photo-oxidative polymerization intermediate product in step S102 according to the embodiment of the present invention includes:
s301, feeding the high-purity fluorine-containing olefin prepared in the step S101 into a photopolymerization kettle through a liquid-phase feed inlet, and continuously feeding oxygen into the photopolymerization kettle through an oxygen channel;
s302, uniformly mixing high-purity fluorine-containing olefin and oxygen in a photopolymerization kettle, and then carrying out oxidative polymerization reaction under the irradiation of an ultraviolet generator to obtain a reaction intermediate product;
and S303, feeding the reaction intermediate product into a degassing tower, degassing for 1-3 h at the temperature of 30-35 ℃, and removing the by-product and unreacted oxygen to obtain the final reaction intermediate product.
In the preparation method of the photo-oxidative polymerization intermediate product provided by the embodiment of the invention, high-purity fluorine-containing olefin is fed into a photo-polymerization kettle and undergoes an oxidative polymerization reaction with oxygen under the irradiation of an ultraviolet light generator to obtain the intermediate product; the reaction intermediate product is sent into a degassing tower for degassing treatment, so that the final reaction intermediate product can be obtained, the discharge of three wastes is reduced, and the method is green and environment-friendly.
The preparation method of the final product perfluoropolyether with peroxide in step S103 provided by the embodiment of the present invention includes:
(1) Placing the final reaction intermediate product obtained in the step S102 into a three-neck flask, introducing nitrogen, stirring at normal temperature for 20-40 min, heating to 55-75 ℃, and stirring again for reaction for 1-3 h;
(2) After the reaction is finished, cooling to normal temperature, adding methanol, precipitating the polymer, washing out unreacted raw materials, and removing the solvent by reduced pressure distillation to obtain perfluoropolyether with peroxide;
(3) And (3) performing fraction segmentation on the perfluoropolyether with peroxide of the final product obtained in the step (2) by adopting molecular distillation to obtain perfluoropolyethers with peroxide of different average molecular weights.
In the preparation method of the final product of the perfluoropolyether with peroxide, provided by the embodiment of the invention, the final reaction intermediate product is placed in a three-neck flask, nitrogen is introduced for reaction, and methanol is added after the final reaction intermediate product is cooled to normal temperature; the polymer is precipitated and unreacted raw materials are washed out, the solvent is removed by reduced pressure distillation, and the fraction is cut, so that the final perfluoropolyether with peroxide can be obtained, the economic benefit is remarkable, and the large-scale industrial production is facilitated.
The production system for preparing the peroxide-bearing perfluoropolyether by photo-oxidative polymerization, provided by the embodiment of the invention, comprises:
a photopolymerization reaction kettle provided with an ultraviolet generator and a stirrer;
the upper part of the photopolymerization reaction kettle is provided with a liquid phase feed inlet, a gas phase feed inlet and a gas phase outlet, a gas distributor is communicated with the gas phase feed inlet to form an oxygen channel, and a stirrer is positioned below the outlet of the gas distributor;
the production system for preparing the peroxide-bearing perfluoropolyether through photo-oxidation polymerization also comprises a central processing module; the central processing module is sequentially connected with the fluorine-containing olefin crude product pretreatment module, the high-purity fluorine-containing olefin preparation module, the intermediate product degassing module and the perfluoropolyether preparation module and is used for coordinating and controlling the normal operation of each module of the production system of the perfluoropolyether with peroxide through the central processing unit;
the pretreatment module of the fluorine-containing olefin crude product is used for placing the fluorine-containing olefin crude product into a cracking device for cracking reaction, and reacting the cracking product under the action of a catalyst to obtain a gas-phase reaction product;
the high-purity fluorine-containing olefin preparation module is used for placing the gas-phase reaction product into a condensing device for condensation, then carrying out gas-liquid separation, and sending the gas phase into a fluorine-containing olefin production system to prepare high-purity fluorine-containing olefin;
the intermediate product preparation module is used for sending high-purity fluorine-containing olefin into the photopolymerization kettle through the liquid-phase feed inlet to perform oxidative polymerization with oxygen under the irradiation of the ultraviolet generator to obtain an intermediate product;
the intermediate product degassing module is used for sending the reaction intermediate product into a degassing tower, degassing for 1-3 h at the temperature of 30-35 ℃, and removing the by-products and unreacted oxygen to obtain a final reaction intermediate product;
the perfluoropolyether preparation module is used for placing the final reaction intermediate product into a three-neck flask, introducing nitrogen gas for reaction, cooling to normal temperature, and adding methanol; and precipitating the polymer, washing out unreacted raw materials, removing the solvent by reduced pressure distillation, and performing fraction segmentation by molecular distillation to obtain the perfluoropolyether with peroxide.
2. Application examples. In order to prove the creativity and the technical value of the technical scheme of the invention, the part is an application example of the technical scheme of the claims to a specific product or related technology.
An application embodiment of the present invention provides a computer program product stored on a computer readable medium, comprising a computer readable program for providing a user input interface to apply the steps of the method for producing perfluoropolyether with peroxide by photo-oxidative polymerization described herein when the computer program product is executed on an electronic device.
An application embodiment of the present invention provides a computer-readable storage medium storing instructions that, when executed on a computer, cause the computer to apply the steps of the method for producing a peroxide-containing perfluoropolyether by photo-oxidative polymerization.
The application embodiment of the invention provides an information data processing terminal, which is used for realizing the production system for preparing the perfluoropolyether with peroxide by photo-oxidation polymerization.
It should be noted that embodiments of the present invention can be realized in hardware, software, or a combination of software and hardware. The hardware portion may be implemented using dedicated logic; the software portions may be stored in a memory and executed by a suitable instruction execution system, such as a microprocessor or specially designed hardware. Those skilled in the art will appreciate that the apparatus and methods described above may be implemented using computer executable instructions and/or embodied in processor control code, such code being provided on a carrier medium such as a disk, CD-or DVD-ROM, programmable memory such as read only memory (firmware), or a data carrier such as an optical or electronic signal carrier, for example. The apparatus and its modules of the present invention may be implemented by hardware circuits such as very large scale integrated circuits or gate arrays, semiconductors such as logic chips, transistors, or programmable hardware devices such as field programmable gate arrays, programmable logic devices, etc., or by software executed by various types of processors, or by a combination of hardware circuits and software, e.g., firmware.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A production method for preparing perfluoropolyether with peroxide by photo-oxidative polymerization, which is characterized in that the production method for preparing the perfluoropolyether with peroxide by photo-oxidative polymerization comprises the following steps:
feeding fluorine-containing olefin into the photopolymerization kettle from a liquid-phase feed inlet, and continuously feeding oxygen into the photopolymerization kettle from an oxygen channel; carrying out oxidative polymerization reaction under the irradiation of an ultraviolet generator to obtain a reaction intermediate product; and then evaporating and recovering to prepare the peroxide-containing perfluoropolyether product.
2. The process for producing a peroxide-bearing perfluoropolyether by photooxidative polymerization as claimed in claim 1, wherein said process for producing a peroxide-bearing perfluoropolyether by photooxidative polymerization comprises the steps of:
step one, carrying out pretreatment operation on raw materials for producing perfluoropolyether: obtaining a fluorine-containing olefin crude product and carrying out cracking reaction to obtain a cracking product; carrying out catalytic reaction on the cracking product to obtain a gas-phase reaction product; gas-liquid separation is carried out on the gas-phase reaction product, and then the gas-phase reaction product is sent into a fluorine-containing olefin production system to obtain high-purity fluorine-containing olefin;
step two, preparing an intermediate product of the photo-oxidative polymerization reaction: feeding high-purity fluorine-containing olefin into a photopolymerization kettle, and carrying out oxidative polymerization reaction with oxygen under the irradiation of an ultraviolet light generator to obtain an intermediate product; feeding the reaction intermediate product into a degassing tower for degassing treatment to obtain a final reaction intermediate product;
step three, preparing the final product of perfluoropolyether with peroxide: placing the final reaction intermediate product into a three-neck flask, introducing nitrogen for reaction, cooling to normal temperature, and adding methanol; the polymer is precipitated and the unreacted raw material is washed out, the solvent is removed by distillation under reduced pressure, and the fraction is cut to obtain the perfluoropolyether with peroxide.
3. The process for producing perfluoropolyether with peroxide by photooxidative polymerization as set forth in claim 2, wherein the pretreatment of the starting material for producing perfluoropolyether in said first step comprises:
(1) Obtaining a fluorine-containing olefin crude product, wherein the fluorine-containing olefin crude product is selected from any one of vinylidene fluoride, trifluoroethylene, trifluoropropene, tetrafluoroethylene, pentafluoropropene, hexafluoropropylene or hexafluorobutadiene;
(2) Putting the fluorine-containing olefin crude product into a cracking device for cracking reaction, and reacting hydrogen chloride and glycerol in the cracking gas under the action of a catalyst to obtain a gas-phase reaction product;
(3) And (3) condensing the gas-phase reaction product in a condensing device, then carrying out gas-liquid separation to obtain a gas phase and a liquid phase, and sending the gas phase into a fluorine-containing olefin production system to prepare the high-purity fluorine-containing olefin.
4. The process for producing perfluoropolyether with peroxide by photooxidative polymerization as claimed in claim 3, wherein the temperature of the cleavage reaction in the step (2) is 90 to 160 ℃, the pressure of the reaction is 0.2 to 0.5MPa, and the reaction time is 8 to 36 hours; the mol ratio of the hydrogen chloride to the glycerol in the fluorine-containing olefin cracking gas is 3-8: 1, the dosage of the catalyst is 5-30% of the molar weight of glycerol;
the catalyst in the step (2) is selected from one or more of acetic acid, propionic acid, succinic acid, adipic acid, sebacic acid, suberic acid, benzoic acid or terephthalic acid;
and (4) in the step (3), after gas-liquid separation, layering the liquid phase to obtain an inorganic phase and an organic phase, and returning the organic phase to the cracking device to continue cracking reaction.
5. The process for producing a peroxide-carrying perfluoropolyether by photo-oxidative polymerization as claimed in claim 2, wherein the intermediate product of the photo-oxidative polymerization in the second step is produced by a process comprising:
(1) Feeding the high-purity fluorine-containing olefin prepared in the step one into a photopolymerization kettle through a liquid-phase feed inlet, and continuously feeding oxygen into the photopolymerization kettle through an oxygen channel;
(2) Uniformly mixing high-purity fluorine-containing olefin and oxygen in a photopolymerization reaction kettle, and then carrying out oxidative polymerization reaction under the irradiation of an ultraviolet generator to obtain a reaction intermediate product;
(3) And (3) feeding the reaction intermediate product into a degassing tower, degassing for 1-3 h at the temperature of 30-35 ℃, and removing the by-product and unreacted oxygen to obtain the final reaction intermediate product.
6. The process for the preparation of peroxide-bearing perfluoropolyether by photooxidative polymerization as claimed in claim 2, wherein the process for the preparation of peroxide-bearing perfluoropolyether as the final product in step three comprises:
(1) Placing the final reaction intermediate product obtained in the step two into a three-neck flask, introducing nitrogen, stirring at normal temperature for 20-40 min, heating to 55-75 ℃, and stirring again for reaction for 1-3 h;
(2) After the reaction is finished, cooling to normal temperature, adding methanol, precipitating the polymer, washing out unreacted raw materials, and removing the solvent by reduced pressure distillation to obtain perfluoropolyether with peroxide;
(3) And (3) performing fraction segmentation on the perfluoropolyether with peroxide of the final product obtained in the step (2) by adopting molecular distillation to obtain perfluoropolyethers with peroxide of different average molecular weights.
7. A production system for producing a peroxide-containing perfluoropolyether by photooxidative polymerization using the production process for producing a peroxide-containing perfluoropolyether by photooxidative polymerization as described in any one of claims 1 to 6, characterized by comprising:
a photopolymerization reaction kettle provided with an ultraviolet generator and a stirrer;
the upper part of the photopolymerization reaction kettle is provided with a liquid-phase feed inlet, a gas-phase feed inlet and a gas-phase outlet, a gas distributor is communicated with the gas-phase feed inlet to form an oxygen channel, and a stirrer is positioned below the outlet of the gas distributor;
the production system for preparing the peroxide-bearing perfluoropolyether through photo-oxidation polymerization also comprises a central processing module; the central processing module is sequentially connected with the fluorine-containing olefin crude product pretreatment module, the high-purity fluorine-containing olefin preparation module, the intermediate product degassing module and the perfluoropolyether preparation module, and is used for coordinating and controlling the normal operation of each module of the production system of the perfluoropolyether with peroxide through the central processing unit;
the pretreatment module of the fluorine-containing olefin crude product is used for placing the fluorine-containing olefin crude product into a cracking device for cracking reaction, and reacting the cracking product under the action of a catalyst to obtain a gas-phase reaction product;
the high-purity fluorine-containing olefin preparation module is used for condensing the gas-phase reaction product in a condensing device, then carrying out gas-liquid separation, and sending the gas phase into a fluorine-containing olefin production system to prepare high-purity fluorine-containing olefin;
the intermediate product preparation module is used for sending high-purity fluorine-containing olefin into the photopolymerization kettle through the liquid-phase feed inlet and carrying out oxidative polymerization reaction with oxygen under the irradiation of the ultraviolet light generator to obtain an intermediate product;
the intermediate product degassing module is used for sending the reaction intermediate product into a degassing tower, degassing for 1-3 h at the temperature of 30-35 ℃, and removing the by-products and unreacted oxygen to obtain a final reaction intermediate product;
the perfluoropolyether preparation module is used for placing the final reaction intermediate product into a three-neck flask, introducing nitrogen gas for reaction, cooling to normal temperature, and adding methanol; and precipitating the polymer, washing out unreacted raw materials, removing the solvent by reduced pressure distillation, and performing fraction segmentation by molecular distillation to obtain the perfluoropolyether with peroxide.
8. A computer program product stored on a computer readable medium, comprising a computer readable program for providing a user input interface for applying the steps of the method of any one of claims 1-6 for the production of a peroxide-bearing perfluoropolyether by photooxidative polymerization when executed on an electronic device.
9. A computer-readable storage medium storing instructions that, when executed on a computer, cause the computer to apply the steps of the method for producing a peroxide-bearing perfluoropolyether by photo-oxidative polymerization according to any one of claims 1 to 6.
10. An information data processing terminal characterized by being used for realizing the production system for producing the peroxide-carrying perfluoropolyether by photo-oxidative polymerization according to claim 7.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110071263A1 (en) * | 2008-06-03 | 2011-03-24 | Solvay (Societe Anonyme) | Process for the manufacture of at least one ethylene derivative compound |
| CN111138384A (en) * | 2019-12-27 | 2020-05-12 | 浙江巨化技术中心有限公司 | Treatment method for byproduct hydrogen chloride in fluorine-containing olefin production process |
| CN114621427A (en) * | 2020-12-11 | 2022-06-14 | 成都晨光博达新材料股份有限公司 | Production process for preparing perfluoropolyether with peroxide by photo-oxidative polymerization |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110071263A1 (en) * | 2008-06-03 | 2011-03-24 | Solvay (Societe Anonyme) | Process for the manufacture of at least one ethylene derivative compound |
| CN111138384A (en) * | 2019-12-27 | 2020-05-12 | 浙江巨化技术中心有限公司 | Treatment method for byproduct hydrogen chloride in fluorine-containing olefin production process |
| CN114621427A (en) * | 2020-12-11 | 2022-06-14 | 成都晨光博达新材料股份有限公司 | Production process for preparing perfluoropolyether with peroxide by photo-oxidative polymerization |
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