CN101003585A - Agglomeration washing method of fluorinated ethylene propylene - Google Patents
Agglomeration washing method of fluorinated ethylene propylene Download PDFInfo
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- CN101003585A CN101003585A CN 200610170939 CN200610170939A CN101003585A CN 101003585 A CN101003585 A CN 101003585A CN 200610170939 CN200610170939 CN 200610170939 CN 200610170939 A CN200610170939 A CN 200610170939A CN 101003585 A CN101003585 A CN 101003585A
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Abstract
This invention discloses a method for condensing and washing perfluoroethylene-perfluoropropylene copolymer prepared by emulsion polymerization. The method comprises: (1) adding 1-10 deg.C deionized water to perfluoroethylene-perfluoropropylene copolymer emulsion, stirring, demulsifying, and washing the precipitate with 40-80 deg.C deionized water for 2-6 times (1-5 min for each time). The method can largely increase the equipment productivity, lower the consumption of pure water, save the raw materials, and shorten the treatment period.
Description
Technical field
The present invention relates to agglomeration washing method of fluorinated ethylene propylene, belong to technical field of macromolecules.
Background technology
Perfluoroethylene-propylene is the multipolymer of tetrafluoroethylene and R 1216, has the premium properties of similar tetrafluoroethylene, and the characteristics of thermoplastic shaping are arranged again, and with glass metal etc. good cohesive force is arranged, and therefore is widely used.It is the most important modification kind of tetrafluoroethylene, is its topmost purposes as the fire resistant electric wire cable insulation material.
Perfluoroethylene-propylene is at first succeeded in developing in nineteen forty-six by the SAUER of du pont company, prepares machinable FEP film at 25～65Mpa, 55～64 ℃ of nearly 10h of following reaction.Through various countries scientist's effort, nowadays it can be by mass polymerization, solution polymerization, suspension polymerization and emulsion polymerization prepared on this basis.Because the whole bag of tricks exists different advantages and shortcoming, thereby is not that above-mentioned all technologies all are fit to suitability for industrialized production.Begin so far research through six the seventies, now industrialized polymerization process mainly contains three kinds: letex polymerization, suspension polymerization and supercritical polymerization.
Emulsion polymerization technique generally adopts aqueous medium, operation easily, thereby preparation FEP.In this heterogeneous technology, adopt perfluorinated surfactant such as Perfluorocaprylic Acid and gentle stirring can obtain the particle of spheroid shape.Because perfluorinated surfactant has splendid aqueous solution dispersion stabilization, and can reduce the chain transfer reaction that surfactant molecule is carried out, thereby widespread use in the preparation perfluoroethylene-propylene.
The formed emulsion of letex polymerization must be through just can further processing after the cohesion.Agglomeration process is a breakdown of emulsion process just, breakdown of emulsion is mainly by physics breakdown of emulsion and two kinds of methods of chemical demulsification, the physics breakdown of emulsion is for example freezing, electrolysis, stirring etc., and chemical demulsification for example adds the effect that chemical substances such as inorganic salt, methyl alcohol, acetate reach breakdown of emulsion in emulsion.The breakdown of emulsion mode that present perfluoroethylene-propylene is adopted mostly is mechanical breakdown of emulsion, and emulsion by certain whipped form, is made the mutual bump of molecule be combined into the bigger particle of volume by high speed shear and separates out from emulsion, thereby reach demulsification.Can have influence on the outward appearance of product owing to acid group particle residual in the polymerization process, metal ion etc., so separating out later material at breakdown of emulsion will further wash, further process after the washing of residual acid ion and metal ion removed, but the cycle of breakdown of emulsion washing at present is oversize, and the throughput of oneself need improve by increase equipment in manufacturer.
Summary of the invention
At the deficiencies in the prior art, provide a kind of improved agglomeration washing method of fluorinated ethylene propylene.Present method is the improved technical scheme that proposes at the cohesion washing of the formed perfluoroethylene-propylene emulsion of letex polymerization.
Agglomeration washing method of fluorinated ethylene propylene of the present invention, step is as follows:
(1) freezing breakdown of emulsion
Add 1～10 ℃ of deionized water of temperature in the perfluoroethylene-propylene emulsion, open then and stir, the breakdown of emulsion time is 5～30min.
(2) hot wash
Material after breakdown of emulsion separated out washs with 40～80 ℃ of deionized waters of temperature, and washing time is 1～5min, repetitive scrubbing 2～6 times, and measure washing back electrical conductivity of water, specific conductivity be lower than 4 μ s/cm be qualified.
Preferably, used perfluoroethylene-propylene emulsion and deionized water volume ratio 1/4～1/2 during step (1) breakdown of emulsion.
Preferably, step (2) washing time adds perfluoroethylene-propylene emulsion and deionized water volume ratio 1/4～1/2.
Preferably, step (2) washing is 4 times.
Evidence method of the present invention is that mechanical breakdown of emulsion and freezing breakdown of emulsion are combined, thereby has beat all demulsification, and in addition, electrolytical solubleness in the water has been quickened in hot wash, thereby has strengthened the washing dynamics.Test method and result are compared as follows:
Test is carried out in identical equipment, will be relatively with cold water and hot water condense respectively and the method for washing and former useful normal-temperature water are condensed washing method, employed cold water temperature is 1～10 ℃ of deionized water, employed hot water temperature is 40～80 ℃ of deionized waters, used emulsion volume is 140ml during breakdown of emulsion, and deionized water that breakdown of emulsion adds is 350ml, adds deionized water during washing and is 300mml, washing time all is 1min at every turn, and its experiment data statistics is as follows:
| The complete breakdown of emulsion time (min) | Specific conductivity (μ s/cm) | ||||||
| Wash 1 time | Wash 2 times | Wash 3 times | Wash 4 times | Wash 5 times | Wash 6 times | ||
| Cold water breakdown of emulsion, hot wash | 8 | Greater than sensing range | Greater than sensing range | 4.55 | 2.4 | 1.88 | / |
| Normal-temperature water breakdown of emulsion, washing | 13 | Greater than sensing range | Greater than sensing range | Greater than sensing range | Greater than sensing range | 19.6 | 10.9 |
Interpretation is compared:
This experiment is that breakdown of emulsion and washing process method and the original technology normal-temperature water with cold water and hot water compared, analyze relatively and can obviously find out from The above results, with breakdown of emulsion time of cold water than shortened for 40% time with normal-temperature water.During washing, just qualified with hot wash 4 times, and compare with normal-temperature water to wash all do not have for 6 times qualified, as seen washing time and bath water amount have all reduced to original over half, thereby the processing power of starting material and equipment is significantly improved, and everything changes, and only need set up once cover and can respectively the device of deionized water cooling and heating can be realized.Thereby improved the throughput of equipment greatly, reduced the usage quantity of pure water, and shortened the processing cycle.
Embodiment
The invention will be further described below in conjunction with embodiment, but be not limited thereto.
Embodiment 1: agglomeration washing method of fluorinated ethylene propylene, and step is as follows:
(1) add 1～10 ℃ of deionized water 350ml of temperature in 140ml perfluoroethylene-propylene emulsion, open then and stir, the breakdown of emulsion time is 8min.
(2) subsequently water is poured out, the deionized water that powder is added about 65 ℃ of 300ml washs, and is qualified behind the repetitive scrubbing 4 times.Measure washing back electrical conductivity of water 2.4 μ s/cm, for the purpose of validate result, specific conductivity becomes 1.9 μ s/cm after washing the 5th, illustrates that the result is accurate.
Embodiment 2: agglomeration washing method of fluorinated ethylene propylene, and step is as follows:
(1) to 1m
3Add 200L perfluoroethylene-propylene emulsion in the cohesion bucket, add 450L deionized water (1～10 ℃) then, open and stir, mixing speed is that 1000r/min condenses, and observes the changing conditions of material in the agglomeration process.
(2) powder after will condensing adds 65 ℃ of left and right sides 400L deionized waters and washs, and from the back of opening entry washing for the third time electrical conductivity of water, it is 2.8 μ s/cm that washing back electrical conductivity of water is measured in the 4th washing back.
Conclusion: it is 30min that step (1) is condensed the used time with cold water, has reduced 1/3 than the normal-temperature water pool time, and it is promptly qualified to wash the 4th in the step (2), and normal-temperature water washing six times is also defective.
Claims (4)
1, agglomeration washing method of fluorinated ethylene propylene, step is as follows:
(1) freezing breakdown of emulsion
Add 1～10 ℃ of deionized water of temperature in the perfluoroethylene-propylene emulsion, open then and stir, the breakdown of emulsion time is 5～30min,
(2) hot wash
Material after breakdown of emulsion separated out washs with a temperature 40-80 ℃ deionized water, and washing time is 1～5min, and repetitive scrubbing gets final product for 2～6 times.
2, perfluoroethylene-propylene condensing method as claimed in claim 1 is characterized in that, used deionized water temperature is 1～10 ℃ during step (1) cohesion, and perfluoroethylene-propylene emulsion and deionized water volume ratio are 1/4～1/2.
3, perfluoroethylene-propylene washing methods as claimed in claim 1 is characterized in that, used deionized water temperature is 40～80 ℃ during step (2) washing, perfluoroethylene-propylene emulsion and deionized water volume ratio 1/4～1/2.
4, agglomeration washing method of fluorinated ethylene propylene as claimed in claim 1 is characterized in that, the washing of step (2) gets final product for 4 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006101709398A CN100488989C (en) | 2006-12-30 | 2006-12-30 | Agglomeration washing method of fluorinated ethylene propylene |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101709398A CN100488989C (en) | 2006-12-30 | 2006-12-30 | Agglomeration washing method of fluorinated ethylene propylene |
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| CN101003585A true CN101003585A (en) | 2007-07-25 |
| CN100488989C CN100488989C (en) | 2009-05-20 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102443091A (en) * | 2011-10-25 | 2012-05-09 | 中昊晨光化工研究院 | Condensation washing method for fluorinated ethylene-propylene resin |
| CN104292369A (en) * | 2014-11-03 | 2015-01-21 | 上海三爱富新材料股份有限公司 | Continuous condensation method of perfluorinated ethylene propylene emulsion |
| CN104530265A (en) * | 2014-12-18 | 2015-04-22 | 中昊晨光化工研究院有限公司 | Fluorine-containing polymer powder and preparation method thereof |
| CN109762081A (en) * | 2018-12-29 | 2019-05-17 | 山东华夏神舟新材料有限公司 | The continuous condensing method and duct type mulser of fluoropolymer emulsion |
| CN110016098A (en) * | 2019-02-25 | 2019-07-16 | 聊城氟尔新材料科技有限公司 | A kind of perfluoroethylene-propylene production cohesion wash mill |
| CN113831429A (en) * | 2020-06-24 | 2021-12-24 | 中昊晨光化工研究院有限公司 | Coagulation washing method of peroxide vulcanized fluororubber emulsion for extrusion |
| CN113861312A (en) * | 2021-11-23 | 2021-12-31 | 常熟三爱富中昊化工新材料有限公司 | Preparation method of powdered fluororubber |
-
2006
- 2006-12-30 CN CNB2006101709398A patent/CN100488989C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102443091A (en) * | 2011-10-25 | 2012-05-09 | 中昊晨光化工研究院 | Condensation washing method for fluorinated ethylene-propylene resin |
| CN102443091B (en) * | 2011-10-25 | 2013-07-24 | 中昊晨光化工研究院 | Condensation washing method for fluorinated ethylene-propylene resin |
| CN104292369A (en) * | 2014-11-03 | 2015-01-21 | 上海三爱富新材料股份有限公司 | Continuous condensation method of perfluorinated ethylene propylene emulsion |
| CN104530265A (en) * | 2014-12-18 | 2015-04-22 | 中昊晨光化工研究院有限公司 | Fluorine-containing polymer powder and preparation method thereof |
| CN104530265B (en) * | 2014-12-18 | 2017-07-11 | 中昊晨光化工研究院有限公司 | A kind of fluoropolymer powder and preparation method thereof |
| CN109762081A (en) * | 2018-12-29 | 2019-05-17 | 山东华夏神舟新材料有限公司 | The continuous condensing method and duct type mulser of fluoropolymer emulsion |
| CN109762081B (en) * | 2018-12-29 | 2021-06-29 | 山东华夏神舟新材料有限公司 | Continuous coagulation method of fluorine-containing polymer emulsion and pipeline type emulsifying machine |
| CN110016098A (en) * | 2019-02-25 | 2019-07-16 | 聊城氟尔新材料科技有限公司 | A kind of perfluoroethylene-propylene production cohesion wash mill |
| CN113831429A (en) * | 2020-06-24 | 2021-12-24 | 中昊晨光化工研究院有限公司 | Coagulation washing method of peroxide vulcanized fluororubber emulsion for extrusion |
| CN113861312A (en) * | 2021-11-23 | 2021-12-31 | 常熟三爱富中昊化工新材料有限公司 | Preparation method of powdered fluororubber |
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| Publication number | Publication date |
|---|---|
| CN100488989C (en) | 2009-05-20 |
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