CN203545924U - Equipment for preparing fluorine-containing polymer in microemulsion state - Google Patents
Equipment for preparing fluorine-containing polymer in microemulsion state Download PDFInfo
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- CN203545924U CN203545924U CN201320649117.3U CN201320649117U CN203545924U CN 203545924 U CN203545924 U CN 203545924U CN 201320649117 U CN201320649117 U CN 201320649117U CN 203545924 U CN203545924 U CN 203545924U
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Abstract
The utility model discloses equipment for preparing a fluorine-containing polymer in a microemulsion state. The equipment comprises a microchannel reaction device, an ultraviolet lamp, a gas-liquid separation device and a pipeline for connecting the microchannel reaction device and the gas-liquid separation device together to convey reaction materials, wherein a reaction heat cooler is arranged in the microchannel reaction device; the gas-liquid separation device is provided with a microemulsion discharge hole and a monomer gas discharge hole; and the ultraviolet lamp is arranged above the microchannel reaction device. The equipment provided by the utility model has the advantages that the polymerization speed is high, polymerization can be aroused at a low temperature, the safety of the polymerization reaction is high, the reaction equipment is simple, the investment is low and the production cost is low.
Description
Technical field
The utility model relates to chemical field, particularly under microemulsion form, prepares the equipment 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.
Utility model content
In order to address the above problem, the utility model provides a kind of equipment of preparing fluoropolymer under microemulsion form.The technical problems to be solved in the utility model is: prior art polymerization velocity is slow, and initiated polymerization temperature is high, and polyreaction is dangerous large, and conversion unit is responsible for, invest high, production cost is high.In order to realize above-mentioned technical purpose, the technical solution of the utility model is: 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;
In such scheme, 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 is 0.1 μ m～100 μ m.
In such scheme, described UV-lamp is that main crest is the UV-lamp of 480nm～300nm.
The method of using the utility model to prepare fluoropolymer under microemulsion form is: the liquid fluorinated monomer of pure water, tensio-active agent, cosurfactant, required polymerization and light trigger are entered in the microchannel reaction device that nitrogen has fully cleaned, at mixing section, fully mix, form the o/w microemulsion that monomer and water form; Microemulsion enters polymeric segment, and under the irradiation of UV-lamp, initiated polymerization, becomes microemulsion fluoropolymer, and meanwhile, reaction heat makes liquid monomer be converted into gaseous monomer; Then fluoropolymer microemulsion is separated in gas-liquid separation equipment with unpolymerized liquid monomer, fluoropolymer microemulsion is discharged from microemulsion relief outlet, and unpolymerized gaseous monomer reclaims from monomer gas relief outlet.
The utility model provides the equipment of preparing fluoropolymer under microemulsion form, and advantage of the present utility model and beneficial effect are: polymerization velocity is fast, can low temperature initiated polymerization, and polyreaction is safe, and conversion unit is simple, less investment, production cost is low.
Accompanying drawing explanation
In order to be illustrated more clearly in the utility model embodiment 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 embodiment more of the present utility model, 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 the utility model equipment.
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, embodiment of the present utility model is further described.Following examples are only for the technical solution of the utility model is more clearly described, and can not limit protection domain of the present utility model with this.
As shown in Figure 1, equipment of the present utility model 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 utility model; not in order to limit the utility model; all within spirit of the present utility model and principle, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection domain of the present utility model.
Claims (6)
1. 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.
2. the equipment of preparing fluoropolymer under microemulsion form according to claim 1, 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.
3. the equipment of preparing fluoropolymer under microemulsion form according to claim 2, it is characterized in that, described micro passage reaction comprises mixing section and polymeric segment, and described UV-lamp is arranged at the top of polymeric segment, and described polymeric segment is glass or quartzy material.
4. according to the arbitrary described equipment of fluoropolymer of preparing under microemulsion form of claim 2 or 3, it is characterized in that, the degree of depth of described micro passage reaction and width are 0.1 μ m～100 μ m.
5. according to the arbitrary described equipment of fluoropolymer of preparing of claim 1～3, it is characterized in that the UV-lamp that the main crest that described UV-lamp is emission of light is 480nm～300nm under microemulsion form.
6. the equipment of preparing fluoropolymer under microemulsion form according to claim 4, is characterized in that, the UV-lamp that the main crest that described UV-lamp is emission of light is 480nm～300nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320649117.3U CN203545924U (en) | 2013-10-21 | 2013-10-21 | Equipment for preparing fluorine-containing polymer in microemulsion state |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201320649117.3U CN203545924U (en) | 2013-10-21 | 2013-10-21 | Equipment for preparing fluorine-containing polymer in microemulsion state |
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| Publication Number | Publication Date |
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| CN203545924U true CN203545924U (en) | 2014-04-16 |
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| CN201320649117.3U Expired - Fee Related CN203545924U (en) | 2013-10-21 | 2013-10-21 | Equipment for preparing fluorine-containing polymer in microemulsion state |
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| CN (1) | CN203545924U (en) |
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- 2013-10-21 CN CN201320649117.3U patent/CN203545924U/en not_active Expired - Fee Related
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140416 Termination date: 20181021 |