CN115975167B - Method for synthesizing perfluoropolyether by gas phase method - Google Patents
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Abstract
本发明提供了一种气相法合成全氟聚醚的方法，涉及化工领域。本发明气相法合成全氟聚醚的方法包括如下步骤：(1)全氟烯烃、三氟氯乙烯和氧气以气相形式混合；(2)进行光氧化反应，即得。本发明解决了现有制备全氟聚醚工艺中工艺复杂、反应控制难、而且具有较大危险性、安全风险大，生产率低、成本高、装置维修与维护困难的问题，实现了装置的连续运行。该方法以六氟丙烯或者四氟乙烯为原料，与氧一起紫外光照，氧化聚合得到结构略有不同的聚醚。经过脱过氧、水解、水洗、精馏、后处理、调配等工序得到均匀稳定的全氟聚醚表面活性剂。本发明具有高效、连续、安全的优点。
The present invention provides a method for synthesizing perfluoropolyether by a gas phase method, and relates to the field of chemical industry. The method for synthesizing perfluoropolyether by a gas phase method of the present invention comprises the following steps: (1) mixing perfluoroolefin, chlorotrifluoroethylene and oxygen in a gas phase; (2) performing a photooxidation reaction to obtain. The present invention solves the problems of the existing process for preparing perfluoropolyether, such as complex process, difficult reaction control, great danger, high safety risk, low productivity, high cost, and difficulty in repairing and maintaining the device, and realizes the continuous operation of the device. The method uses hexafluoropropylene or tetrafluoroethylene as raw materials, irradiates with ultraviolet light together with oxygen, and oxidatively polymerizes to obtain polyethers with slightly different structures. After deoxygenation, hydrolysis, washing, distillation, post-treatment, blending and other processes, a uniform and stable perfluoropolyether surfactant is obtained. The present invention has the advantages of high efficiency, continuity and safety.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a method for synthesizing perfluoropolyether by a gas phase method.
Background
The perfluoro polyether (PFPE) is a high-molecular polymer, is colorless, odorless and transparent liquid at normal temperature, and is only dissolved in perfluoro organic solvent. The PFPE has the characteristics of heat resistance, oxidation resistance, radiation resistance, corrosion resistance, low volatility, incombustibility and the like, and has good comprehensive properties of being compatible with plastics, elastomers, metal materials and the like, thereby becoming a very reliable lubricant in severe environments and being widely applied to the fields of chemical industry, electronics, electricity, machinery, magnetic media, nuclear industry, aerospace and the like.
At present, the preparation methods of the perfluoropolyether mainly comprise 2 methods, namely a direct photooxidation method of perfluoroolefin and an anion polymerization method of perfluoroepoxide. In the anionic polymerization of perfluoroepoxides to obtain perfluoropolyethers, hexafluoropropylene oxide is generally used as the starting material. For example, chinese patent application publication CN103030800 describes a process for the preparation of high molecular weight perfluoropolyethers by polymerizing hexafluoropropylene oxide in the presence of a fluorine-containing solvent and a metal fluoride catalyst. Chinese patent application publication CN103788363 describes the completion of a polymerization of hexafluoropropylene oxide in an aprotic solvent with a phase transfer agent and an anhydrous alkali metal fluoride as catalysts. The above patents all use hexafluoropropylene oxide as a starting material, but this process is not an economical process for the preparation of perfluoropolyethers due to the relatively high cost of hexafluoropropylene oxide.
The direct photooxidation method of perfluoroolefin is to copolymerize hexafluoropropylene or tetrafluoroethylene with oxygen, so that the technology for synthesizing the perfluoropolyether is more reasonable and the application is wider. The direct photooxygenation process of perfluoro olefine uses hexafluoropropylene or tetrafluoroethylene as material, and makes them undergo the process of ultraviolet irradiation together with oxygen at low temperature, and oxidation polymerization so as to obtain polyether with slightly different structure. The production process flow mainly comprises tetrafluoroethylene or hexafluoropropylene, photo-oxidative polymerization, crude ether distillation, alkali washing or fluoridation refining, fractionation, post-treatment, blending and PFPE. The patent application publication US3704214 describes a process for obtaining perfluoropolyethers from hexafluoropropylene and oxygen, liquid phase, at a temperature of-100 to 80 ℃, at a pressure of 0.1 to 40bar, ultraviolet radiation. The patent application publication US5149842 describes a process for obtaining perfluoroalkyl derivatives from fluoroolefins and oxygen, provided that the liquid phase, the temperature is not higher than 50 ℃, contains one or more F-X groups, where x=f, cl, O, or ultraviolet radiation is an initiator. The preparation process described in the patent application with the publication number of CN103073410A comprises the steps of generating fluoroether acyl chloride and fluoroether acyl fluoride through ultraviolet light-induced photochemical reaction at the temperature of minus 40 to minus 80 ℃ by using fluoroolefin monomers, oxygen and a molecular weight regulator, generating fluoroether carboxylic acid through hydrolysis of the fluoroether acyl chloride and the fluoroether acyl fluoride under the irradiation of ultraviolet light, and obtaining a fluoroether carboxylic acid finished product through washing and purification. The preparation method is described in the patent application with the publication number of CN107501538A, hexafluoropropylene liquid is concentrated in a reactor in the synthesis stage, oxygen and an initiator are introduced, and low-temperature oxidative polymerization is carried out at-75 to-40 ℃. The patent application with publication number CN114031762A discloses a preparation process of perfluoropolyether, which comprises the steps of placing liquid-phase hexafluoropropylene and chlorotrifluoroethylene in a photochemical reaction kettle, introducing oxygen to perform photooxidation reaction, keeping the pressure in the photochemical reaction kettle at 0-0.05 MPa, keeping the ultraviolet wavelength at 200-400 nm, the power of a light source at 200-600 w and the temperature at-30 to-70 ℃ for 4-10 hours, and removing the peroxidation, rectifying, hydrolyzing, washing and neutralizing the crude product after the reaction to obtain a finished product. The preparation process of perfluoro-olefine direct photooxidation method disclosed by the prior art has the defects of (1) reaction at low temperature, high requirement on a refrigerating system by a reaction device, high cost, low temperature and pressure controllability of the reaction, threat to process safety and high risk, and (thirdly) low selectivity of target products, high by-products and high difficulty in subsequent treatment of the by-products due to the fact that the temperature is increased along with the progress of the reaction in a reaction system, and (IV) intermittent reaction of discharging reaction materials after the completion of the reaction by the liquid phase, and long time consumption of the whole process is a low-productivity process.
Thus, there is a need to develop a safe, efficient, low cost method of synthesizing perfluoropolyethers.
Disclosure of Invention
The invention aims to provide a method for synthesizing perfluoropolyether by a gas phase method, which aims to solve the problems of difficult reaction control, high safety risk, single variety, low production rate, high cost and incapability of continuous production in the existing preparation process of the perfluoropolyether.
The above object of the present invention is achieved by the following technical solutions:
The invention provides a method for synthesizing perfluoropolyether by a gas phase method, which comprises the following steps:
(1) Mixing perfluoroolefin, chlorotrifluoroethylene and oxygen in a gas phase;
(2) And (3) performing photooxidation reaction to obtain the light-emitting diode.
Further, in step (1), the perfluoroolefin is hexafluoropropylene or tetrafluoroethylene.
Further, in step (1), the molar ratio of perfluoroolefin, chlorotrifluoroethylene and oxygen is determined by the target perfluoropolyether molecular weight;
preferably, the target perfluoropolyether has a molecular weight of 450-800.
In the step (1), the molar ratio of the perfluoroolefin to the chlorotrifluoroethylene to the oxygen is (1-20): 1 (1-10).
Further, in the step (1), the molar ratio of the perfluoroolefin to the chlorotrifluoroethylene to the oxygen is (6-15): 1 (3-7);
preferably, in the step (1), the molar ratio of the perfluoroolefin, the chlorotrifluoroethylene and the oxygen is 6:1:7.
Further, in the step (2), the reaction temperature of the photo-oxidation reaction is-15-40 ℃;
and/or in the step (2), the reaction pressure of the photo-oxidation reaction is 0-0.05 MPa;
and/or, in the step (2), ultraviolet light is adopted in the photo-oxidation reaction.
The reaction product of the photooxidation reaction of the present invention is a liquid phase, and the reaction system is a reaction with a reduced volume, so that the progress of the reaction is controlled by controlling the reaction pressure.
Further, in the step (2), the reaction temperature of the photo-oxidation reaction is-15 ℃;
And/or in the step (2), the wavelength of the ultraviolet light is 200-500 nm, and the intensity is 10-30 Kw;
Preferably, in the step (2), the ultraviolet light has a wavelength of 350nm and an intensity of 15Kw.
Further, in the step (2), the photooxidation reaction is a continuous photooxidation reaction performed in a photooxidation reactor.
Further, in the photooxidation reactor, unreacted perfluoroolefin, chlorotrifluoroethylene and oxygen can be recycled into the photooxidation reactor for continuous reaction.
In the step (2), after the photooxidation reaction, the product is purified, wherein the purification method comprises the steps of deoxidizing, hydrolyzing, washing with water, distilling, post-treating and blending the reaction solution to obtain the perfluoropolyether.
Compared with the prior art, the invention has the beneficial effects that:
(1) The reaction efficiency is high, the reaction is controllable, and the gas phase method is adopted to synthesize the perfluoropolyether, so that the mass transfer and heat transfer efficiency is high, the temperature and pressure control of the polymerization reaction are stable, and the efficient, controllable and safe production is realized.
(2) The selectivity of the target product is high, byproducts are reduced, unreacted materials can be recycled into the reaction system to continue the reaction, and the consumption of raw materials is reduced.
(3) The raw materials of the synthesis method are in a gaseous state, and continuous production can be realized by regulating and controlling the flow rate of the gas and continuously introducing the gas into the reactor, so that the productivity is greatly improved.
(4) The synthesis method has low requirement on the refrigerating capacity of the refrigerating system, and greatly reduces the equipment cost.
(5) The addition amount of each raw material gas in the reaction process can be regulated and controlled to synthesize the perfluoropolyether with various molecular weights, so that the reaction varieties are various.
In conclusion, the gas phase synthesis method of the perfluoropolyether is provided, and the synthesis method uses gaseous raw materials, has strong controllability and good safety in the reaction process, and meanwhile, the synthesis method is simple in process operation, mild in reaction condition, high in mass and heat transfer efficiency of the gaseous raw materials, high in selectivity of target products, few in byproducts and capable of realizing continuous production, so that the production efficiency of the synthesis method is very high. In addition, by regulating and controlling the addition amount of raw materials in the reaction process, various molecular weight perfluoropolyethers can be synthesized, and the product variety is increased. Therefore, the synthesis method ensures the safety of equipment and technology, can synthesize perfluoropolyethers with various molecular weights, realizes continuous production, greatly improves the productivity, changes the state that the prior perfluoropolyether product has single variety and extremely low production capacity and can not meet the actual requirements, and has good application prospect.
Furthermore, the invention solves the problems of complex process, difficult reaction control, high risk, high safety risk, low productivity, high cost and difficult device maintenance in the existing perfluoropolyether preparation process, and realizes the continuous operation of the device. The method uses hexafluoropropylene or tetrafluoroethylene as raw material, and ultraviolet light irradiates with oxygen, and oxidation polymerization is carried out to obtain polyether with slightly different structures. The uniform and stable perfluoropolyether surfactant is obtained through the working procedures of peroxidation, hydrolysis, water washing, rectification, post-treatment, blending and the like. The invention has the advantages of high efficiency, continuity and safety.
It should be apparent that, in light of the foregoing, various modifications, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
The above-described aspects of the present invention will be described in further detail below with reference to specific embodiments in the form of examples. It should not be understood that the scope of the above subject matter of the present invention is limited to the following examples only. All techniques implemented based on the above description of the invention are within the scope of the invention.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
Unless otherwise indicated, all materials and equipment used in the detailed description are conventional and well known to those skilled in the art and are commercially available from the open market.
The process flow diagram of the invention is shown in figure 1.
EXAMPLE 1 Synthesis of perfluoropolyether by gas phase method
Continuously introducing a mixed gas with the mol ratio of hexafluoropropylene/chlorotrifluoroethylene/oxygen=6/1/7 into a photooxidation reactor in a continuous reaction mode, starting an ultraviolet lamp, adjusting the frequency to 350nm, controlling the intensity to 15Kw, controlling the reaction temperature to-15 ℃, controlling the reaction pressure to 0-0.05 Mpa, starting the reaction, discharging while feeding in the reaction process, discharging the liquid phase of the photooxidation reactor to a crude product collecting tank, then entering a peroxidation device to remove the peroxy, and finally obtaining the qualified perfluoropolyether through the procedures of hydrolysis, water washing, rectification, post-treatment, blending and the like according to a conventional method. And condensing unreacted hexafluoropropylene, chlorotrifluoroethylene and oxygen in the photooxidation reactor through a condenser, and then feeding the condensed hexafluoropropylene, chlorotrifluoroethylene and oxygen into a mixer for recycling.
EXAMPLE 2 Synthesis of perfluoropolyether by gas phase method
Continuously introducing a mixed gas with the mol ratio of hexafluoropropylene/chlorotrifluoroethylene/oxygen=9/1/7 into a photooxidation reactor in a continuous reaction mode, starting an ultraviolet lamp, adjusting the frequency to 350nm, controlling the intensity to 15Kw, controlling the reaction temperature to-15 ℃, controlling the reaction pressure to 0-0.05 Mpa, starting the reaction, discharging while feeding in the reaction process, discharging the liquid phase of the photooxidation reactor to a crude product collecting tank, then entering a peroxidation device to remove the peroxy, and finally obtaining the qualified perfluoropolyether through the procedures of hydrolysis, water washing, distillation, post-treatment, blending and the like according to a conventional method. And condensing unreacted hexafluoropropylene, chlorotrifluoroethylene and oxygen in the photooxidation reactor through a condenser, and then feeding the condensed hexafluoropropylene, chlorotrifluoroethylene and oxygen into a mixer for recycling.
EXAMPLE 3 Synthesis of perfluoropolyether by gas phase method
Continuously introducing a mixed gas with the mol ratio of hexafluoropropylene/chlorotrifluoroethylene/oxygen=6/1/5 into a photooxidation reactor in a continuous reaction mode, starting an ultraviolet lamp, adjusting the frequency to 350nm, controlling the intensity to 15Kw, controlling the reaction temperature to-5 ℃, controlling the reaction pressure to 0-0.05 Mpa, starting the reaction, discharging while feeding in the reaction process, discharging the liquid phase of the photooxidation reactor to a crude product collecting tank, then entering a peroxidation device to remove the peroxy, and finally obtaining the qualified perfluoropolyether through the procedures of hydrolysis, water washing, distillation, post-treatment, blending and the like according to a conventional method. And condensing unreacted hexafluoropropylene, chlorotrifluoroethylene and oxygen in the photooxidation reactor through a condenser, and then feeding the condensed hexafluoropropylene, chlorotrifluoroethylene and oxygen into a mixer for recycling.
EXAMPLE 4 Synthesis of perfluoropolyether by gas phase method
Continuously introducing a mixed gas with the mol ratio of hexafluoropropylene/chlorotrifluoroethylene/oxygen=9/1/5 into a photooxidation reactor in a continuous reaction mode, starting an ultraviolet lamp, adjusting the frequency to 350nm, controlling the intensity to 15Kw, controlling the reaction temperature to-5 ℃, controlling the reaction pressure to 0-0.05 Mpa, starting the reaction, discharging while feeding in the reaction process, discharging the liquid phase of the photooxidation reactor to a crude product collecting tank, then entering a peroxidation device to remove the peroxy, and finally obtaining the qualified perfluoropolyether through the procedures of hydrolysis, water washing, distillation, post-treatment, blending and the like according to a conventional method. And condensing unreacted hexafluoropropylene, chlorotrifluoroethylene and oxygen in the photooxidation reactor through a condenser, and then feeding the condensed hexafluoropropylene, chlorotrifluoroethylene and oxygen into a mixer for recycling.
EXAMPLE 5 Synthesis of perfluoropolyether by gas phase method
Continuously introducing a mixed gas with the mol ratio of hexafluoropropylene/chlorotrifluoroethylene/oxygen=9/1/3 into a photooxidation reactor in a continuous reaction mode, starting an ultraviolet lamp, adjusting the frequency to 350nm, controlling the intensity to 15Kw, controlling the reaction temperature to 15 ℃, controlling the reaction pressure to 0-0.05 Mpa, starting the reaction, discharging while feeding in the reaction process, discharging the liquid phase of the photooxidation reactor to a crude product collecting tank, then entering a deoiling device to remove peroxy, and finally obtaining qualified perfluoropolyether through the procedures of hydrolysis, water washing, distillation, post-treatment, blending and the like according to a conventional method. And condensing unreacted hexafluoropropylene, chlorotrifluoroethylene and oxygen in the photooxidation reactor through a condenser, and then feeding the condensed hexafluoropropylene, chlorotrifluoroethylene and oxygen into a mixer for recycling.
EXAMPLE 6 Synthesis of perfluoropolyether by gas phase method
Continuously introducing a mixed gas with the mol ratio of hexafluoropropylene/chlorotrifluoroethylene/oxygen=15/1/3 into a photooxidation reactor in a continuous reaction mode, starting an ultraviolet lamp, adjusting the frequency to 350nm, controlling the intensity to 15Kw, controlling the reaction temperature to 15 ℃, controlling the reaction pressure to 0-0.05 Mpa, starting the reaction, discharging while feeding in the reaction process, discharging the liquid phase of the photooxidation reactor to a crude product collecting tank, then entering a deoxidiser to remove peroxy, and finally obtaining qualified perfluoropolyether through the procedures of hydrolysis, water washing, distillation, post-treatment, blending and the like according to a conventional method. And condensing unreacted hexafluoropropylene, chlorotrifluoroethylene and oxygen in the photooxidation reactor through a condenser, and then feeding the condensed hexafluoropropylene, chlorotrifluoroethylene and oxygen into a mixer for recycling.
The conditions and results of examples 1 to 6 are shown in Table 1.
TABLE 1 conditions and results for examples 1-6
In conclusion, the gas phase synthesis method of the perfluoropolyether is provided, and the synthesis method uses gaseous raw materials, has strong controllability and good safety in the reaction process, and meanwhile, the synthesis method is simple in process operation, mild in reaction condition, high in mass and heat transfer efficiency of the gaseous raw materials, high in selectivity of target products, few in byproducts and capable of realizing continuous production, so that the production efficiency of the synthesis method is very high. In addition, by regulating and controlling the addition amount of raw materials in the reaction process, various molecular weight perfluoropolyethers can be synthesized, and the product variety is increased. Therefore, the synthesis method ensures the safety of equipment and technology, can synthesize perfluoropolyethers with various molecular weights, realizes continuous production, greatly improves the productivity, changes the state that the prior perfluoropolyether product has single variety and extremely low production capacity and can not meet the actual requirements, and has good application prospect.
Claims (6)
1. A method for synthesizing perfluoropolyether by a gas phase method is characterized by comprising the following steps:
(1) The perfluoroolefin, the chlorotrifluoroethylene and the oxygen are mixed in a gas phase form, wherein the perfluoroolefin is hexafluoropropylene or tetrafluoroethylene, and the molar ratio of the perfluoroolefin to the chlorotrifluoroethylene to the oxygen is (6-15) 1 (3-7);
(2) Performing photooxidation reaction, wherein the reaction temperature of the photooxidation reaction is-15 ℃;
the reaction pressure of the photo-oxidation reaction is 0-0.05 MPa, ultraviolet light is adopted in the photo-oxidation reaction, the wavelength of the ultraviolet light is 350nm, and the intensity of the ultraviolet light is 15Kw.
2. The method of claim 1, wherein the perfluoropolyether has a molecular weight of 450-800.
3. The method according to claim 1, wherein in the step (1), the molar ratio of the perfluoroolefin, chlorotrifluoroethylene and oxygen is 6:1:7.
4. The method according to claim 1, wherein in the step (2), the photooxidation reaction is a continuous photooxidation reaction performed in a photooxidation reactor.
5. The method according to claim 4, wherein in the photooxidation reactor, unreacted perfluoroolefin, chlorotrifluoroethylene and oxygen are recycled to the photooxidation reactor for continuous reaction.
6. The method of claim 1, wherein in the step (2), after the photooxidation reaction, the product is purified by deoxidizing, hydrolyzing, washing with water, distilling, post-treating and blending the reaction solution to obtain the perfluoropolyether.
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| CN114031762A (en) * | 2021-09-30 | 2022-02-11 | 四川弘氟新材料有限公司 | Preparation process of perfluoropolyether surfactant and perfluoropolyether surfactant |
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| IT1229845B (en) * | 1989-04-20 | 1991-09-13 | Ausimont Srl | PROCEDURE FOR THE PREPARATION OF PEROXIDE PERFLUOROPOLYETERS. |
| ITMI20050383A1 (en) * | 2005-03-10 | 2006-09-11 | Solvay Solexis Spa | PROCESS FOR PREPARING PEROXIDE PERFLUOROPOLIETERS |
| CN103724559B (en) * | 2013-12-17 | 2016-08-17 | 中昊晨光化工研究院有限公司 | A kind of by the method for PFPE peroxide synthesis PFPE |
| CN107501538A (en) * | 2017-08-01 | 2017-12-22 | 巨化集团技术中心 | A kind of PFPE and preparation method thereof |
| 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 |
| CN114015033B (en) * | 2021-09-30 | 2024-06-18 | 四川弘氟新材料有限公司 | Fluorine-containing polyether carboxylic acid type surfactant and preparation method thereof |
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| RU2397181C2 (en) * | 2008-10-23 | 2010-08-20 | Закрытое акционерное общество "Завод оргсинтез Ока" | Polytetrafluoroethylene oxide synthesis method |
| CN114031762A (en) * | 2021-09-30 | 2022-02-11 | 四川弘氟新材料有限公司 | Preparation process of perfluoropolyether surfactant and perfluoropolyether surfactant |
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