CN105985459B - A method of it is continuously washed for fluoropolymer - Google Patents
A method of it is continuously washed for fluoropolymer Download PDFInfo
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- CN105985459B CN105985459B CN201510089639.6A CN201510089639A CN105985459B CN 105985459 B CN105985459 B CN 105985459B CN 201510089639 A CN201510089639 A CN 201510089639A CN 105985459 B CN105985459 B CN 105985459B
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Abstract
The present invention relates to a kind of methods continuously washed for fluoropolymer, include the following steps：The fluoropolymer emulsion obtained using emulsion polymerization is raw material, polymer suspension is obtained after machinery is demulsified, continuously it is passed through scrubbing tower lower part, it is continuously passed through deionized water from scrubbing tower top, the fluoropolymer suspension is washed with deionized water counter current contacting, it washes rear fluoropolymer to be discharged from the position higher than the deionized water entrance and obtain qualified products through centrifugal drying, washes is discharged from the position less than the fluoropolymer emulsion entrance.The device for fluoropolymer continuous washing method is utilized the present invention also provides a kind of.This method can continuously wash fluoropolymer under the conditions of totally-enclosed, have many advantages, such as applied widely, and detersive efficiency is high, water consumption is few, while will not introduce other impurities, helps to promote product quality.
Description
Technical field
The present invention relates to a kind of methods continuously washed for fluoropolymer.
Background technology
Fluoropolymer has excellent weatherability, electrical insulating property, chemical-resistant, corrosion resistance and resistant of high or low temperature
Can, it is widely used in fields such as aviation, automobile, oil and chemical industry.Emulsion polymerization is the important of fluoropolymer preparation
One of technique, including polytetrafluoroethylene (PTFE), Kynoar, perfluoroethylene-propylene, tetrafluoraoethylene-hexafluoropropylene copolymer, inclined fluorine
The method that emulsion polymerization can be used in ethylene-hexafluoropropylene copolymer, ethylene-chlorotrifluoro-ethylene copolymer etc..And emulsion polymerization
It is most important the disadvantage is that aftertreatment technology is complex, need by processes such as filtering, demulsification, washing, drying, granulations.It is domestic
Numerous studies are carried out to emulsion after-treatment technology outside, it is intended to improve production efficiency, reduce production cost.
In the prior art, there is described below washing process after being demulsified for fluoropolymer：
（1）After washing process is resin demulsification after traditional fluoropolymer demulsification, deionized water is added, stirring is opened
Promote the ion exchange of resin and water, then water layer is removed by modes such as stratification or centrifugations, it is repeated multiple times until resin
Middle impurity residual quantity is less than index.This method frequent operation, and detersive efficiency is low, and water consumption is big, generally requires 6 times or more
Washing is just up to standard.
（2）Chinese patent CN102875711A elaborate polyvinylidene fluoride emulsion cohesion prepared by a kind of emulsion polymerization and
The new method of resin washing.Toner grain size is smaller after the patent thinks the cohesion that traditional handicraft obtains, and the resin of cohesion is in
Paste is unfavorable for washing in next step.The patented invention is by using freezing demulsification and the united method of mechanical agitation Shearing demulsification
It is 200 μm or so of toner to be demulsified to lotion and obtain grain size, and studies and obtained washing pure water preferable temperature, excellent
Select number and single wash preferred time.It, be first although this method reduces washing times and wash time to a certain extent
By freezing demulsification, reusable heat water washing, energy consumption is larger.
（3）Chinese patent CN102838820A describes a kind of aftertreatment technology of fluoropolymer.The patent is by fluorine-containing tree
The units such as emulsion breaking, washing, dehydration, the exhaust of fat are integrated into a set of extruder with different operation region.It is squeezing out
The different zones of machine realize different functions.It was demulsified before this to lotion with high steam, and fluoropolymer after demulsification
Enter washing dehydration region together in molten condition and water, multiple washing dehydration is carried out to molten fluoropolymer, until surface
Activating agent residual is less than 10ppm.Fluoropolymer enters vacuum area and is exhausted after washing is qualified, and moisture content is down to 0.1%
Hereinafter, entering back into comminutor granulation.The method is will again to be washed after fluoropolymer melt, is not suitable for thermosetting polymer, and
It is unable to get powder product.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of method continuously washed for fluoropolymer, including with
Lower step：The fluoropolymer emulsion obtained using emulsion polymerization obtains polymer suspension as raw material after machinery is demulsified,
It is characterized in that, fluoropolymer emulsion is continuously passed through scrubbing tower lower part, is continuously passed through from scrubbing tower top after machinery is demulsified
Ionized water, the fluoropolymer suspension wash with deionized water counter current contacting, wash rear fluoropolymer and gone from higher than described
The position of ion water inlet is discharged and obtains qualified products through centrifugal drying, and washes is from less than the fluoropolymer emulsion
The position of entrance is discharged.
Further, the fluoropolymer is polytetrafluoroethylene (PTFE), Kynoar, perfluoroethylene-propylene, ethylene-trifluoro
Vinyl chloride copolymer, tetrafluoraoethylene-hexafluoropropylene copolymer, vinylidene fluoride-hexafluoropropylene copolymer and tetrafluoroethylene-perfluoro
One kind in alkyl alkene ether copolymer.
Further, the solid holdup of the fluoropolymer emulsion raw material is 5% ~ 30% g/g.
Further, fluoropolymer apparent density is 0.2 g/cm after demulsification3~0.8g/cm3。
Further, the matter of deionized water described in washing process and the charging of fluoropolymer suspension after the demulsification
It is 1 to measure the ratio between flow:1~10:1, preferably 1:1~5:1.
Further, deionized water temperature described in washing process is 10 DEG C ~ 80 DEG C, preferably 25 DEG C ~ 70 DEG C.
Further, in washing process, the fluoropolymer that gas reduces washes is passed through in the lower part of the scrubbing tower
Object entrainment, the gas are preferably nitrogen.
Further, in washing process, enhanced to containing in tower by the way that the multiphase flow pump in the tower body of scrubbing tower is arranged
The suspension of fluoropolymer and the mixing of both deionized waters；The multiphase flow pump is symmetrically staggered installation of in the scrubbing tower
Tower body both sides；For the same multiphase flow pump, the height of entrance is higher than the height of its outlet；And entrance is located at the same gear
In the separate space that plate is formed；The ratio between the multiphase flow pump and the mass flow of deionized water of the washing are 2 ~ 50 times, preferably
It is 4 ~ 10 times.
The device for fluoropolymer continuous washing method, including demulsification are utilized the present invention also provides a kind of
Kettle, medial launder and scrubbing tower, the medial launder are arranged between demulsification kettle and the scrubbing tower, and the scrubbing tower includes buffering
Kettle, tower body and standing tank, the accumulator still are connected to the lower part of the tower body, and the standing tank is connected to the upper of the tower body
Portion is provided with distributor in the accumulator still, and for being passed through being uniformly distributed for gas, the accumulator still lower part is set the distributor
It is equipped with the outlet of washes, the tower body lower part is provided with the entrance of fluoropolymer suspension after demulsification, in the tower body
Portion is provided with baffle, and the baffle is for extending washings and fluoropolymer suspension in the residence time of tower body, the tower
It is provided with multiple multiphase flow pumps in the middle part of body, the multiphase flow pump is symmetrically staggered installation of in the tower body both sides of the scrubbing tower, right
In the same multiphase flow pump, the height of entrance is higher than the height of its outlet, and entrance be located at that the same baffle formed every
Intracavitary, the tower body top are provided with the entrance of deionized water, the standing tank top be provided with wash it is rear it is fluoropolymer-containing go out
Mouthful.The layering for standing tank and being used for resin and water, reduces the moisture content for washing rear resin；The scrubbing tower tower body is resin and water
The main place of countercurrent washing occurs；The accumulator still is for reducing resin clip band in washes；The multiphase flow pump is used for
Enhance the local dip inside scrubbing tower tower body, the mixed effect of reinforced resin and deionized water；The distributor is used for nitrogen
Gas forms uniform minute bubbles in water.
Compared with the prior art, the advantages of the present invention are as follows：
（1）A kind of method continuously washed for fluoropolymer is provided, while substantially increasing detersive efficiency
Reduce water consumption；
（2）Traditional stirring is substituted with pump circulation stream, to enhance the ion exchange process in washing process, is not only more held
It easily realizes industrialization, and new impurity will not be introduced；
（3）Nitrogen is introduced in wash tower bottoms and generates bubble, it is therefore intended that is reduced fluoropolymer in washes and is pressed from both sides
Ribbon amount, while fluoropolymer apparent density after demulsification is also reduced, advantageously reduce slurry amount.
Description of the drawings
Fig. 1 is the flow of the present invention and the schematic diagram of device.
In figure：1 is demulsification kettle；2 be medial launder；3-1 is accumulator still；3-2 is tower body；3-3 is to stand tank；3-11 is distribution
Device；3-21 is baffle；3-22 is multiphase flow pump.
Specific implementation mode
It is next in the following with reference to the drawings and specific embodiments that invention is further explained.
Embodiment 1
The polyvinylidene fluoride emulsion that solid holdup is 25% is passed through demulsification kettle, it is complete to open stirring demulsification.It again will be after demulsification
Polyvinylidene fluoride resin pumps the lower part for being delivered to scrubbing tower；Resin feeding flow is 500kg/h after demulsification；Washing deionized water
Dosage is 1000kg/h, and water temperature is 25 DEG C；All multiphase flow pumps are opened, it is small to wash rear resin conductivity by pump discharge 5000kg/h
In 5 μ s/cm, solid holdup 12%；Washes conductivity is 120 ~ 160 μ s/cm, and solid holdup is less than 0.05%.
Embodiment 2
The perfluoroethylene-propylene emulsion that solid holdup is 15% is passed through demulsification kettle, it is complete to open stirring demulsification.After being demulsified again
Exhaustive fluorinated ethylene propylene is pumped to the lower part of scrubbing tower；Resin feeding flow is 400kg/h after demulsification；Washing is used with deionized water
Amount is 1500kg/h, and water temperature is 65 DEG C；All multiphase flow pumps are opened, pump discharge is that 15000kg/h is not open close toward tower reactor distributor
Enter nitrogen, nitrogen use level 4m3/h；It washes rear exhaustive fluorinated ethylene propylene conductivity and is less than 2 μ s/cm, solid holdup 10%；Washing
Conductivity of waste water is 50 ~ 60 μ s/cm, and solid holdup is less than 0.05%.
Embodiment 3
The polyvinylidene fluoride emulsion that solid holdup is 8% is passed through demulsification kettle, it is complete to open stirring demulsification.It will gather after demulsification again
Fluorinated ethylene propylene resin is pumped to the lower part of scrubbing tower；Resin feeding flow is 800kg/h after demulsification；Washing deionized water dosage
For 1000kg/h, water temperature is 45 DEG C；Open all multiphase flow pumps, pump discharge 2000kg/h；It is constantly passed through toward tower reactor distributor
Nitrogen, nitrogen use level 2m3/h；It washes rear exhaustive fluorinated ethylene propylene conductivity and is less than 3 μ s/cm, solid holdup 12%；Washing is useless
Water conductivity is 50 ~ 60 μ s/cm, and solid holdup is less than 0.05%.
Embodiment 4
The device for fluoropolymer continuous washing method, including demulsification kettle are utilized the present invention also provides a kind of
1, medial launder 2 and scrubbing tower, the medial launder 2 are arranged between the demulsification kettle 1 and scrubbing tower, and the scrubbing tower includes buffering
Kettle 3-1, tower body 3-2 and standing tank 3-3, the accumulator still 3-1 are connected to the lower part of the tower body 3-2, and the standing tank 3-3 connects
It is connected on the top of the tower body 3-2, distributor 3-11, the distributor 3-11 are provided in the accumulator still 3-1 for being passed through
Gas is uniformly distributed, and the lower parts the accumulator still 3-1 are provided with the outlet of washes, and the lower parts the tower body 3-2 are provided with brokenly
The entrance of fluoropolymer suspension after breast, the tower body 3-2 are internally provided with baffle 3-21, the baffle 3-21 for extending
The residence time of washings and fluoropolymer suspension in tower, the middle parts tower body 3-2 are provided with multiple multiphase flow pump 3-
22, the multiphase flow pump 3-22 are symmetrically staggered installation of in the both sides tower body 3-2 of the scrubbing tower, for the same multiphase flow pump
3-22, the height of entrance is higher than the height of its outlet, and entrance is located in the same baffle separate space, on the tower body 3-2
Portion is provided with the entrance of deionized water, and the tops the standing tank 3-3, which are provided with, washes rear fluoropolymer-containing outlet.The standing tank
3-3 is used for the layering of resin and water, reduces the moisture content for washing rear resin；The scrubbing tower tower body 3-2 is that resin and water generation are inverse
Flow the main place of washing；The accumulator still 3-1 is for reducing resin clip band in washes；The multiphase flow pump 3-22 is used for
Strengthen the local dip inside scrubbing tower tower body, the mixed effect of reinforced resin and deionized water；The distributor 3-11 is used for
Nitrogen is formed to uniform minute bubbles in water.
Claims (8)
1. a kind of method continuously washed for fluoropolymer, includes the following steps：It is obtained with emulsion polymerization fluorine-containing poly-
Conjunction object lotion is raw material, obtains polymer suspension after machinery is demulsified, which is characterized in that fluoropolymer emulsion is broken through machinery
After breast, be continuously passed through scrubbing tower lower part, deionized water be continuously passed through from scrubbing tower top, the fluoropolymer suspension with go
Ionized water counter current contacting is washed, and washes rear fluoropolymer from the position discharge higher than the deionized water entrance and through centrifugal drying
Qualified products are obtained, washes is discharged from the position less than the fluoropolymer emulsion entrance；
In washing process, enhanced to fluoropolymer-containing suspended in tower by the way that the multiphase flow pump in the tower body of scrubbing tower is arranged
The mixing of both liquid and deionized water；The multiphase flow pump is symmetrically staggered installation of in the tower body both sides of the scrubbing tower；For
The same multiphase flow pump, the height of entrance is higher than the height of its outlet, and entrance is located at the separate space of same baffle formation
It is interior；The ratio between the multiphase flow pump and the mass flow of deionized water of the washing are 4~10 times.
2. a kind of method continuously washed for fluoropolymer as described in claim 1, which is characterized in that described fluorine-containing poly-
Conjunction object is polytetrafluoroethylene (PTFE), Kynoar, perfluoroethylene-propylene, ethylene-chlorotrifluoro-ethylene copolymer, tetrafluoroethene-hexafluoro
One kind in propylene copolymer, vinylidene fluoride-hexafluoropropylene copolymer and tetrafluoroethylene-perfluoro alkyl alkene ether copolymer.
3. a kind of method continuously washed for fluoropolymer as described in claim 1, which is characterized in that described fluorine-containing poly-
The solid holdup for closing object emulsion materials is 5%~30%g/g.
4. a kind of method continuously washed for fluoropolymer as described in claim 1, which is characterized in that fluorine-containing after demulsification
Polymer apparent density is 0.2g/cm3~0.8g/cm3。
5. a kind of method continuously washed for fluoropolymer as described in claim 1, which is characterized in that in washing process
The ratio between the deionized water and the mass flow of charging of fluoropolymer suspension after the demulsification are 1:1~5:1.
6. a kind of method continuously washed for fluoropolymer as described in claim 1, which is characterized in that in washing process
The deionized water temperature is 25 DEG C~70 DEG C.
7. a kind of method continuously washed for fluoropolymer as described in claim 1, which is characterized in that washing process
In, it is passed through the fluoropolymer entrainment that gas reduces washes in the lower part of the scrubbing tower, the gas is nitrogen.
8. a kind of utilizing the device for fluoropolymer continuous washing method described in claim 1, including demulsification kettle, centre
Slot and scrubbing tower, the medial launder are arranged between demulsification kettle and the scrubbing tower, which is characterized in that the scrubbing tower includes slow
Water rushes kettle, tower body and standing tank, the accumulator still are connected to the lower part of the tower body, and the standing tank is connected to the upper of the tower body
Portion is provided with distributor in the accumulator still, and for being passed through being uniformly distributed for gas, the accumulator still lower part is set the distributor
It is equipped with the outlet of washes, the tower body lower part is provided with the entrance of fluoropolymer suspension after demulsification, in the tower body
Portion is provided with baffle, and the baffle is for extending washings and fluoropolymer suspension in the residence time of tower body, the tower
It is provided with multiple multiphase flow pumps in the middle part of body, the multiphase flow pump is symmetrically staggered installation of in the tower body both sides of the scrubbing tower, right
In the same multiphase flow pump, the height of entrance is higher than the height of its outlet, and entrance be located at that the same baffle formed every
Intracavitary, the tower body top are provided with the entrance of deionized water, the standing tank top be provided with wash it is rear it is fluoropolymer-containing go out
Mouthful.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510089639.6A CN105985459B (en) | 2015-02-27 | 2015-02-27 | A method of it is continuously washed for fluoropolymer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510089639.6A CN105985459B (en) | 2015-02-27 | 2015-02-27 | A method of it is continuously washed for fluoropolymer |
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| CN105985459B true CN105985459B (en) | 2018-08-17 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110317286A (en) * | 2018-03-30 | 2019-10-11 | 浙江蓝天环保高科技股份有限公司 | A method of improving polyvinylidene fluoride resin degree of purity |
| CN109107221A (en) * | 2018-08-21 | 2019-01-01 | 金发科技股份有限公司 | A kind of liquid-solid extraction purification devices and purification process |
| CN111450787A (en) * | 2020-03-31 | 2020-07-28 | 无锡银燕化工装备科技有限公司 | Reactor for continuous washing |
| CN114736319B (en) * | 2021-01-07 | 2023-12-26 | 中昊晨光化工研究院有限公司 | Apparatus system and method for purifying polymer from polymeric emulsion |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4128517A (en) * | 1977-11-01 | 1978-12-05 | Pennwalt Corporation | Method of washing polymer latices by aerating |
| US4228005A (en) * | 1977-05-27 | 1980-10-14 | E. I. Du Pont De Nemours And Company | Mechanical dewatering apparatus for elastomer slurries |
| CN102765835A (en) * | 2012-08-14 | 2012-11-07 | 陕西太阳景环保科技有限公司 | Closed multistage purified water device and production process |
-
2015
- 2015-02-27 CN CN201510089639.6A patent/CN105985459B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4228005A (en) * | 1977-05-27 | 1980-10-14 | E. I. Du Pont De Nemours And Company | Mechanical dewatering apparatus for elastomer slurries |
| US4128517A (en) * | 1977-11-01 | 1978-12-05 | Pennwalt Corporation | Method of washing polymer latices by aerating |
| CN102765835A (en) * | 2012-08-14 | 2012-11-07 | 陕西太阳景环保科技有限公司 | Closed multistage purified water device and production process |
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Effective date of registration: 20190724 Address after: 312369 No. 1 Jingjiu Road, Shangyu Economic and Technological Development Zone, Hangzhou Bay, Shaoxing City, Zhejiang Province Co-patentee after: Zhejiang Lantian Environment Protecting Sci-Tech Co., Ltd. Patentee after: Sinochem Blue Sky Fluorine Material Co., Ltd. Address before: 312369 Shangyu, Shaoxing, Hangzhou Bay Fine Chemical Industrial Park, No. 31, No. five weft Road, No. Co-patentee before: Zhejiang Lantian Environment Protecting Sci-Tech Co., Ltd. Patentee before: ZHEJIANG CHEMICAL INSTITUTE TECHNOLOGY CO., LTD. |
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