CN103554318A - Method and device for preparing fluorine-containing polymer under micro-emulsion form - Google Patents
Method and device for preparing fluorine-containing polymer under micro-emulsion form Download PDFInfo
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- CN103554318A CN103554318A CN201310495146.3A CN201310495146A CN103554318A CN 103554318 A CN103554318 A CN 103554318A CN 201310495146 A CN201310495146 A CN 201310495146A CN 103554318 A CN103554318 A CN 103554318A
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- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 17
- 229920000642 polymer Polymers 0.000 title abstract description 7
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title abstract 11
- 229910052731 fluorine Inorganic materials 0.000 title abstract 11
- 239000011737 fluorine Substances 0.000 title abstract 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 80
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 37
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000000178 monomer Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004064 cosurfactant Substances 0.000 claims abstract description 6
- 238000004064 recycling Methods 0.000 claims abstract description 4
- 230000000694 effects Effects 0.000 claims abstract description 3
- 239000004094 surface-active agent Substances 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims description 30
- 229920002313 fluoropolymer Polymers 0.000 claims description 20
- 239000004811 fluoropolymer Substances 0.000 claims description 20
- -1 perfluoroalkyl vinyl ether Chemical compound 0.000 claims description 17
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 8
- FDMFUZHCIRHGRG-UHFFFAOYSA-N 3,3,3-trifluoroprop-1-ene Chemical compound FC(F)(F)C=C FDMFUZHCIRHGRG-UHFFFAOYSA-N 0.000 claims description 5
- 239000013543 active substance Substances 0.000 claims description 5
- PKBXXIJDESMGDN-UHFFFAOYSA-N 1-fluorobuta-1,2,3-triene Chemical compound FC=C=C=C PKBXXIJDESMGDN-UHFFFAOYSA-N 0.000 claims description 4
- QMIWYOZFFSLIAK-UHFFFAOYSA-N 3,3,3-trifluoro-2-(trifluoromethyl)prop-1-ene Chemical compound FC(F)(F)C(=C)C(F)(F)F QMIWYOZFFSLIAK-UHFFFAOYSA-N 0.000 claims description 4
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 claims description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 4
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical group FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- JDPDLMITLVAWKZ-UHFFFAOYSA-N 1,3-dioxolan-4-yl(phenyl)methanone Chemical class C=1C=CC=CC=1C(=O)C1COCO1 JDPDLMITLVAWKZ-UHFFFAOYSA-N 0.000 claims description 2
- HEQOJEGTZCTHCF-UHFFFAOYSA-N 2-amino-1-phenylethanone Chemical compound NCC(=O)C1=CC=CC=C1 HEQOJEGTZCTHCF-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 2
- ISAOCJYIOMOJEB-UHFFFAOYSA-N benzoin Chemical class C=1C=CC=CC=1C(O)C(=O)C1=CC=CC=C1 ISAOCJYIOMOJEB-UHFFFAOYSA-N 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 239000003999 initiator Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000008213 purified water Substances 0.000 abstract 1
- 230000001960 triggered effect Effects 0.000 abstract 1
- 239000000376 reactant Substances 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 7
- 229910052753 mercury Inorganic materials 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 6
- 238000012703 microemulsion polymerization Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 230000002269 spontaneous effect Effects 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 230000007928 solubilization Effects 0.000 description 2
- 238000005063 solubilization Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000003019 stabilising effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000012725 vapour phase polymerization Methods 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a method for preparing a fluorine-containing polymer under a micro-emulsion form, comprises the following steps: A, sufficiently mixing purified water, a surfactant, a cosurfactant, a liquid state fluorine-containing monomer and a photo-initiator in a reactor to form an O/W micro-emulsion composed of a fluorine-containing monomer and water; B, placing the O/W micro-emulsion formed in the step A under an ultraviolet lamp to irradiate to trigger poly reaction, forming a fluorine-containing polymer in a micro-emulsion form, wherein the unpolymerized liquid state fluorine-containing monomer is transferred into a gaseous fluorine-containing monomer under the effect of reaction heat; C, separating the fluorine-containing polymer forming the micro-emulsion form from the gaseous fluorine-containing monomer in the step B, and recycling the gaseous fluorine-containing monomer. The invention further discloses a device for preparing the fluorine-containing polymer using the above method. The method and device have the beneficial effect that the polymerization speed is fast, the polymerization can be triggered at a low temperature, the poly reaction is high in security, the reaction device is simple, the investment is less, the production cost is low, and the product quality is excellent.
Description
Technical field
The present invention relates to chemical field, particularly under microemulsion form, prepare the method and apparatus of fluoropolymer.
Background technology
If two or more immiscible liquid is after mixing and emulsifying, the diameter of dispersant liquid drop is between 5nm～100nm, and this system is called microemulsion.Microemulsion is transparent dispersion system, and its formation is relevant with the solubilization of micella, is called again " by the micellar solution of swelling " or " micella emulsion ".Conventionally the transparent or semitransparent aqueous stabilising system being formed by oil, water, tensio-active agent, cosurfactant and ionogen etc.The particle of disperse phase is less than 0.1 μ m, even little of tens of dusts.Be characterized in that disperse phase particle size is between 0.01～0.1 μ m, evenly, microscope is invisible for particle size; It is spherical that particle is; Microemulsion is translucent to transparent, Thermodynamically stable, if system is transparent, and good fluidity, and can think microemulsion with separated five minutes of the centrifugal acceleration of whizzer 100g is not stratified; With oil, water is miscible within the specific limits.The system that disperse phase is water for oil, dispersion medium is called O/W type microemulsion, otherwise is called w/o type microemulsion.The feature of O/W type micro-emulsion polymerization is that the place of polyreaction is not solubilization micelle, but emulsified monomer drop is planted the generation of core and the growth of particle, all in monomer droplet, occurs; The diameter of the median size of polymer particle and initial monomer drop is basic identical.From reported first such as stoffer in 1980, take microemulsion since polymerisation medium, micro-emulsion polymerization has caused people's great attention as an important branch of letex polymerization.Micro-emulsion polymerization reacting balance, quick, reaction process need not stir, so equipment is simple, safe and reliable; Polymerisate is the polymer microemulsion that particle diameter is minimum, monodispersity is better, stability is high, can obtain after treatment that relative molecular weight is high, the polymkeric substance of narrowly distributing; For the properties that improves polymkeric substance, there is very important realistic meaning; The application prospect of micro-emulsion polymerization is boundless.
In prior art, also there is micro-emulsion polymerization perfluoroethylene-propylene and by the method for R 1216, tetrafluoroethylene, trifluoro propene binary polymerization microemulsion, but, there is following problem: 1, gas phase monomer is directly passed in polymeric kettle, or the material after vapour phase polymerization " is sneaked into " in established microemulsion, or gaseous phase materials is dissolved in the polyreaction in microemulsion, but it is not micro-emulsion polymerization truly; And, in polymeric kettle, due to the gathering of gas phase monomer, there is the danger of implode; 2, use radical initiator initiated polymerization, its polymerization temperature is higher; 3, in polymerization process, need constantly to add monomer and initiator.
Summary of the invention
In order to address the above problem, the invention provides a kind of method of preparing fluoropolymer under microemulsion form.The technical problem to be solved in the present invention is: prior art polymerization velocity is slow, and initiated polymerization temperature is high, and polyreaction is dangerous large, and conversion unit is complicated, invest high, production cost is high.In order to realize above-mentioned technical purpose, technical scheme of the present invention is: under microemulsion form, prepare the method for fluoropolymer, it is characterized in that: comprise the following steps:
A. pure water, tensio-active agent, cosurfactant, liquid fluorinated monomer and light trigger are fully mixed in reaction vessel, form the o/w microemulsion that fluorochemical monomer and water form;
B. o/w microemulsion steps A being formed is placed under UV-lamp and irradiates, initiated polymerization, and the fluoropolymer of generation microemulsion form, unpolymerized liquid fluorinated monomer is converted into gaseous state fluorochemical monomer under the effect of reaction heat;
C. the fluoropolymer that generates microemulsion form in step B is separated with gaseous state fluorochemical monomer, by the recycling use of described gaseous state fluorochemical monomer.
In such scheme, described fluorochemical monomer is one or more the mixture in tetrafluoroethylene, R 1216, trifluoro propene, trifluorochloroethylene, vinylidene, vinyl fluoride, hexafluoro-isobutene, perfluoroalkyl vinyl ether, or is at least one the mixture in ethene or propylene and tetrafluoroethylene, R 1216, trifluoro propene, trifluorochloroethylene, vinylidene, vinyl fluoride, hexafluoro-isobutene, perfluoroalkyl vinyl ether.
In such scheme, described tensio-active agent is nonionic surface active agent; Described cosurfactant is low carbon chain alcohol; Described light trigger is selected from methylol st-yrax, Benzoin derivative, 4-benzoyl-1,3-dioxolane derivatives, dibenzoyl ketone acetal, α, α-dialkoxy methyl phenyl ketone, alpha-aminoacetophenone, 2,4, any in 6-Three methyl Benzene formyl phenylbenzene phosphatization oxyhydroxide.
In such scheme, in described step B, polymerization temperature is 32 ℃～23 ℃.
In such scheme, in described step B, polymerization pressure is 3.92MPa～4.42MPa.
In such scheme, in described step B, polymerization time is 1～60 minute.
In such scheme, the main crest of described UV-lamp emission of light is 480nm～300nm.
The invention also discloses the equipment of preparing fluoropolymer under microemulsion form: comprise microchannel reaction device, UV-lamp, gas-liquid separation device and described microchannel reaction device and gas-liquid separation device are coupled together and carry the pipeline of reaction mass, in described microchannel reaction device, be provided with reaction heat water cooler, described gas-liquid separation device is provided with microemulsion relief outlet and monomer gas relief outlet, and described UV-lamp is arranged at reaction device top, microchannel.
In such scheme, described microchannel reaction device is single micro passage reaction, or two micro passage reaction groups that above micro passage reaction consists of serial or parallel connection; Described micro passage reaction comprises mixing section and polymeric segment, and described UV-lamp is arranged at the top of polymeric segment; Described polymeric segment is glass or quartzy material.
In such scheme, the degree of depth of described micro passage reaction and width are 0.1 μ m～100 μ m.
The invention provides the method and apparatus of preparing fluoropolymer under microemulsion form, advantage of the present invention and beneficial effect are: polymerization velocity is fast, can low temperature initiated polymerization, polyreaction is safe, and conversion unit is simple, less investment, production cost is low, and product performance are superior.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skills, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structural representation of present device.
In figure: 1, the mixing section 12 of micro passage reaction 11, micro passage reaction is, the microemulsion relief outlet 22 of the polymeric segment 2 of micro passage reaction, gas-liquid separation device 21, gas-liquid separation device, the monomer gas relief outlet 3 of gas-liquid separation device, UV-lamp
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is further described.Following examples are only for technical scheme of the present invention is more clearly described, and can not limit the scope of the invention with this.
As shown in Figure 1, equipment of the present invention comprises: comprise micro passage reaction 1, UV-lamp 3, gas-liquid separation device 2 and described micro passage reaction 1 and gas-liquid separation device 2 are coupled together and carry the pipeline of reaction mass; Micro passage reaction 1 comprises mixing section 11 and polymeric segment 12, UV-lamp 2 is arranged at the top of micro passage reaction polymeric segment 12, the discharge port of the polymeric segment 12 of micro passage reaction 1 is connected with the opening for feed of gas/liquid separator device 2 by pipeline, and gas-liquid separation device 2 is provided with microemulsion relief outlet 21 and monomer gas relief outlet 22.The UV-lamp of using in embodiment is kapillary extra-high-pressure mercury vapour lamp, and the main crest of its isolychn is 300nm～480nm.
Embodiment 1
The kind of reactant, title and weight are as following table:
The micro passage reaction fully cleaning with nitrogen, by the mixing section of above-mentioned reactant input micro passage reaction, after above-mentioned reactant fully mixes, spontaneous formation microemulsion; Open kapillary extra-high-pressure mercury vapour lamp, microemulsion enters the polymeric segment of micro passage reaction, and polymerization temperature is controlled at 25 ℃～28 ℃; Polymerization pressure is controlled at 3.95MPa～4.05MPa; Polymerization time is 25min; Then the reaction system in micro passage reaction polymeric segment is conveyed into gas-liquid separation device, in gas-liquid separation device, reaction system separation obtains tetrafluoroethylene microemulsion 5575g, unpolymerized tetrafluoroethylene gas recovery recycling.
The kind of reactant, title and weight are as following table:
The micro passage reaction fully cleaning with nitrogen, by the mixing section of above-mentioned reactant input micro passage reaction, after above-mentioned reactant fully mixes, spontaneous formation microemulsion; Open kapillary extra-high-pressure mercury vapour lamp, microemulsion enters the polymeric segment of micro passage reaction, and polymerization temperature is controlled at 27 ℃～30 ℃; Polymerization pressure is controlled at 3.95MPa～4.05MPa; Polymerization time is 35min; Then the reaction system in micro passage reaction polymeric segment is conveyed into gas-liquid separation device, in gas-liquid separation device, reaction system separation obtains tetrafluoroethylene microemulsion; The tetrafluoroethylene microemulsion breakdown of emulsion of heating is processed, filtered and clean material, 130 ℃ of oven dry, obtain fine polytetrafluoroethylpowder powder 465g; Reclaim tetrafluoroethylene 33g.
The kind of reactant, title and weight are as following table:
The micro passage reaction fully cleaning with nitrogen, by the mixing section of above-mentioned reactant input micro passage reaction, after above-mentioned reactant fully mixes, spontaneous formation microemulsion; Open kapillary extra-high-pressure mercury vapour lamp, microemulsion is inputted to the polymeric segment of micro passage reaction, polymerization temperature is controlled at 26 ℃～28 ℃; Polymerization pressure is controlled at 3.95MPa～4.05MPa; Polymerization time is 40min; Then the reaction system in micro passage reaction polymeric segment is conveyed into gas-liquid separation device, in gas-liquid separation device, reaction system separation obtains perfluoroethylene-propylene microemulsion; The perfluoroethylene-propylene microemulsion breakdown of emulsion of heating is processed, filtered and clean material, 130 ℃ of constant temperature are dried for 2 hours, are then warming up to 190 ℃, and constant temperature 4 hours, obtains the perfluoroethylene-propylene fine powder 503g without caking.
Embodiment 4
The kind of reactant, title and weight are as following table:
The micro passage reaction fully cleaning with nitrogen, by the mixing section of above-mentioned reactant input micro passage reaction, after above-mentioned reactant fully mixes, spontaneous formation microemulsion; Open kapillary extra-high-pressure mercury vapour lamp, microemulsion is inputted to the polymeric segment of micro passage reaction, polymerization temperature is controlled at 30 ℃～32 ℃; Polymerization pressure is controlled at 3.95MPa～4.05MPa; Polymerization time is 60min; Then the reaction system in micro passage reaction polymeric segment is conveyed into gas-liquid separation device, in gas-liquid separation device, reaction system separation obtains multipolymer microemulsion 5576g.
Embodiment 5
The kind of reactant, title and weight are as following table:
The micro passage reaction fully cleaning with nitrogen, by the mixing section of above-mentioned reactant input micro passage reaction, after above-mentioned reactant fully mixes, spontaneous formation microemulsion; Open kapillary extra-high-pressure mercury vapour lamp, microemulsion is inputted to the polymeric segment of micro passage reaction, polymerization temperature is controlled at 29 ℃～30 ℃; Polymerization pressure is controlled at 3.92MPa～4.05MPa; Polymerization time is 25min; Then the reaction system in micro passage reaction polymeric segment is conveyed into gas-liquid separation device, in gas-liquid separation device, reaction system separation obtains tetrafluoroethylene microemulsion; The tetrafluoroethylene microemulsion breakdown of emulsion of heating is processed, filtered and clean material, 130 ℃ of constant temperature dryings, obtain fine polytetrafluoroethylpowder powder 463g; Reclaim tetrafluoroethylene 35g.
Embodiment 6
The kind of reactant, title and weight are as following table:
The micro passage reaction fully cleaning with nitrogen, by the mixing section of above-mentioned reactant input micro passage reaction, after above-mentioned reactant fully mixes, spontaneous formation microemulsion; Open kapillary extra-high-pressure mercury vapour lamp, microemulsion is inputted to the polymeric segment of micro passage reaction, polymerization temperature is controlled at 27 ℃～28 ℃; Polymerization pressure is controlled at 3.95MPa～4.42MPa; Polymerization time is 20min; Then the reaction system in micro passage reaction polymeric segment is conveyed into gas-liquid separation device, in gas-liquid separation device, reaction system separation obtains perfluoroethylene-propylene microemulsion; The perfluoroethylene-propylene microemulsion breakdown of emulsion of heating is processed, filtered and clean material, 130 ℃ of constant temperature are dried for 2 hours, are then warming up to 190 ℃, and constant temperature 3 hours, obtains the perfluoroethylene-propylene fine powder 501g without caking.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. under microemulsion form, prepare the method for fluoropolymer, it is characterized in that: comprise the following steps:
A. pure water, tensio-active agent, cosurfactant, liquid fluorinated monomer and light trigger are fully mixed in reaction vessel, form the o/w microemulsion that fluorochemical monomer and water form;
B. o/w microemulsion steps A being formed is placed under UV-lamp and irradiates, initiated polymerization, and the fluoropolymer of generation microemulsion form, unpolymerized liquid fluorinated monomer is converted into gaseous state fluorochemical monomer under the effect of reaction heat;
C. the fluoropolymer that generates microemulsion form in step B is separated with gaseous state fluorochemical monomer, by the recycling use of described gaseous state fluorochemical monomer.
2. the method for preparing fluoropolymer under microemulsion form according to claim 1, it is characterized in that, described fluorochemical monomer is one or more the mixture in tetrafluoroethylene, R 1216, trifluoro propene, trifluorochloroethylene, vinylidene, vinyl fluoride, hexafluoro-isobutene, perfluoroalkyl vinyl ether, or is at least one the mixture in ethene or propylene and tetrafluoroethylene, R 1216, trifluoro propene, trifluorochloroethylene, vinylidene, vinyl fluoride, hexafluoro-isobutene, perfluoroalkyl vinyl ether.
3. the method for preparing fluoropolymer under microemulsion form according to claim 1, is characterized in that, described tensio-active agent is nonionic surface active agent; Described cosurfactant is low carbon chain alcohol; Described light trigger is selected from methylol st-yrax, Benzoin derivative, 4-benzoyl-1,3-dioxolane derivatives, dibenzoyl ketone acetal, α, α-dialkoxy methyl phenyl ketone, alpha-aminoacetophenone, 2,4, any in 6-Three methyl Benzene formyl phenylbenzene phosphatization oxyhydroxide.
4. the method for preparing fluoropolymer under microemulsion form according to claim 1, is characterized in that, in described step B, polymerization temperature is 32 ℃～23 ℃.
5. the method for preparing fluoropolymer under microemulsion form according to claim 1, is characterized in that, in described step B, polymerization pressure is 3.92MPa～4.42MPa.
6. the method for preparing fluoropolymer under microemulsion form according to claim 1, is characterized in that, in described step B, polymerization time is 1～60 minute.
7. according to the arbitrary described method of fluoropolymer of preparing under microemulsion form of claim 1～6, it is characterized in that, the main crest of described UV-lamp emission of light is 480nm～300nm.
8. under microemulsion form, prepare the equipment of fluoropolymer, it is characterized in that, comprise microchannel reaction device, UV-lamp, gas-liquid separation device and described microchannel reaction device and gas-liquid separation device are coupled together and carry the pipeline of reaction mass, in described microchannel reaction device, be provided with reaction heat water cooler, described gas-liquid separation device is provided with microemulsion relief outlet and monomer gas relief outlet, and described UV-lamp is arranged at reaction device top, microchannel.
9. the equipment of preparing fluoropolymer under microemulsion form according to claim 8, it is characterized in that, described microchannel reaction device is single micro passage reaction, or two micro passage reaction groups that above micro passage reaction consists of serial or parallel connection; Described micro passage reaction comprises mixing section and polymeric segment, and described UV-lamp is arranged at the top of polymeric segment; Described polymeric segment is glass or quartzy material.
10. the equipment of preparing fluoropolymer under microemulsion form according to claim 9, is characterized in that, the degree of depth of described micro passage reaction and width are 0.1 μ m～100 μ m.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104098730A (en) * | 2014-07-10 | 2014-10-15 | 中昊晨光化工研究院有限公司 | Low-Mooney and high-fluoride fluororubber and preparation method thereof |
| CN109651539A (en) * | 2018-11-23 | 2019-04-19 | 宜宾天原集团股份有限公司 | For producing micro- reaction system of polyvinyl chloride and the Production of PVC method based on the system |
| CN113880978A (en) * | 2021-08-31 | 2022-01-04 | 泰兴梅兰新材料有限公司 | Method and device for preparing microchannel of fluoropolyether carboxylic acid for fluorinated ethylene propylene |
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| CN104098730A (en) * | 2014-07-10 | 2014-10-15 | 中昊晨光化工研究院有限公司 | Low-Mooney and high-fluoride fluororubber and preparation method thereof |
| CN109651539A (en) * | 2018-11-23 | 2019-04-19 | 宜宾天原集团股份有限公司 | For producing micro- reaction system of polyvinyl chloride and the Production of PVC method based on the system |
| CN109651539B (en) * | 2018-11-23 | 2023-11-17 | 宜宾天原集团股份有限公司 | Micro-reaction system for producing polyvinyl chloride and polyvinyl chloride production method based on micro-reaction system |
| CN113880978A (en) * | 2021-08-31 | 2022-01-04 | 泰兴梅兰新材料有限公司 | Method and device for preparing microchannel of fluoropolyether carboxylic acid for fluorinated ethylene propylene |
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