CN109320634A - A kind of cohesion washing methods of fluorinated ethylene propylene resin - Google Patents
A kind of cohesion washing methods of fluorinated ethylene propylene resin Download PDFInfo
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- CN109320634A CN109320634A CN201710642569.1A CN201710642569A CN109320634A CN 109320634 A CN109320634 A CN 109320634A CN 201710642569 A CN201710642569 A CN 201710642569A CN 109320634 A CN109320634 A CN 109320634A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/14—Treatment of polymer emulsions
- C08F6/22—Coagulation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/26—Tetrafluoroethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/28—Hexyfluoropropene
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Abstract
The present invention relates to a kind of cohesion washing methods of fluorinated ethylene propylene resin, include the following steps: that room temperature deionized water 1) is added into perfluoroethylene-propylene emulsion, lotion specific gravity is adjusted 1.03~1.20, stirring is opened, 15~60min of physics demulsification is carried out to lotion under conditions of 500~2000 revs/min；2) it is incorporated as the flocculating agent ammonium hydrogen carbonate of resin solid content 1~5% into above-mentioned emulsion, continues stirring and is demulsified completely to perfluoroethylene-propylene emulsion；3) it is washed repeatedly with the perfluoroethylene-propylene that demulsification is precipitated in room temperature deionized water, until detection is qualified.It is demulsified, the resin in perfluoroethylene-propylene emulsion can be precipitated completely with method of the invention, compared with other methods, not will increase the dosage of subsequent wash water.And method and step of the invention is simple, and it is environmentally friendly, be conducive to industrialization large-scale production.
Description
Technical field
The present invention relates to technical field of macromolecules, and in particular to a kind of cohesion washing methods of fluorinated ethylene propylene resin.
Background technique
Polyfluorinated ethylene propylene resin (FEP) is thermoplastic resin, and processing performance is good, while having fabulous high and low temperature resistance
With fabulous chemical stability.Its most outstanding performance is electrical insulating property (for example, its dielectric constant and polytetrafluoroethylene (PTFE) one
Sample, for 2.1).The characteristic that superior electrical insulation capability and workability, low propagation of flame and low smog generate, makes the copolymerization
Object is mainly used as the insulating materials in integrated circuit board and wire and cable.The copolymer can use the processing of general thermoplastic
Method makes it be widely used in electronic and electrical industry, chemistry if the product of various forms is made in extrusion molding, molding, spray process method
Industry, mechanical industry, national defense industry, medicine etc..
Industrialized polymerization is mainly emulsion polymerization to polyfluorinated ethylene propylene.Emulsion polymerization is formed by lotion must
It must just may be further processed after cohesion.Coacervation process is exactly the process of a demulsification, and the method for demulsification is main
There are two methods of physics demulsification and chemical demulsification, physics demulsification is such as freezed, stirred, and chemical demulsification is such as saltoutd.
Breaking method used by polyfluorinated ethylene propylene is mainly mechanical demulsification at present, and lotion is passed through certain stirring shape
Formula hits molecule mutually by high speed shear and is combined into the bigger particle of volume and is precipitated from lotion, to reach demulsification effect
Fruit.Since various ions remaining in polymerization process influence whether the appearance of product, so the powder after demulsification is precipitated will be into
Row washing, is further processed after remaining ion-cleaning is removed.
Patent CN101003585A discloses the cohesion washing methods of perfluoroethylene-propylene emulsion, which is poly-
Water at low temperature is added in perfluoroethylene-propylene (copolymer) lotion kind, then uses mechanical coalescence, which cannot be by the poly- perfluor in lotion
Ethylene-propylene resin agglomerates precipitation completely, there is also about 5% or so exhaustive fluorinated ethylene propylene in the lotion agglomerated, both makes in this way
At the waste of exhaustive fluorinated ethylene propylene, but be unfavorable for it is environmental-friendly, and this method use chilled water, energy consumption is higher, no
Conducive to industrialized production.
Summary of the invention
The object of the present invention is to provide a kind of at low cost, easy to operate, fluorinated ethylene propylene resin can be demulsified completely
Cohesion washing methods, the method for the present invention includes following steps:
1) room temperature deionized water is added into perfluoroethylene-propylene emulsion, adjusts lotion specific gravity 1.03~1.15, opens
Stirring carries out 15~60min of physics demulsification to lotion under conditions of 500~2000 revs/min；
2) the flocculating agent ammonium hydrogen carbonate of the perfluoroethylene-propylene (copolymer) emulsion solid content 1~5% is incorporated as into above-mentioned emulsion, after
Continuous be stirred to perfluoroethylene-propylene emulsion is demulsified completely；
3) it is washed repeatedly with the perfluoroethylene-propylene that demulsification is precipitated in room temperature deionized water, until detection is qualified.
Preferably, the specific gravity that lotion is adjusted in the step 1) is 1.05~1.1.
It is furthermore preferred that the specific gravity for adjusting lotion in the step 1) is 1.06~1.08.It is found through experiments that, lotion specific gravity
When being adjusted to 1.05~1.1, especially 1.06~1.08, the resin average grain diameter agglomerating out using this technique 200~
300um, for resin in the particle size range, washing times are less, it is easier to washes clean, and can be demulsified completely, do not remain.
Preferably, the actual conditions stirred in the step 1) be under conditions of 1200~1600 revs/min stirring 20~
25min。
Preferably, the additive amount of flocculating agent is the 1.5~2.5% of resin solid content in the step 2).
It is furthermore preferred that the additive amount of flocculating agent is the 1.8~2% of resin solid content in the step 2).
Ammonium hydrogen carbonate the incomplete resin of mechanical coalescence in lotion can both be precipitated as flocculating agent, and and other
Flocculating agent is compared, and washes clean is easy to, and is easy that remaining ammonium bicarbonate breaks down is gone out in subsequent resin drying process.
Because ammonium hydrogen carbonate, when environment temperature is at 10 DEG C or less, chemical property is stablized, and does not decompose substantially；At 10~20 DEG C, decompose not
Significantly；It is a large amount of to decompose at 40 DEG C or more, and the drying temperature of the current perfluoroethylene-propylene of industry is at 120~180 DEG C.And add
Dosage effect at 1.5~2.5%, especially 1.8~2% is more preferable.
Preferably, in the step 3) when washing, the perfluoroethylene-propylene for the precipitation that is demulsified and the volume of room temperature deionized water
The ratio between be 1/2~2/3.
Preferably, the time washed every time in the step 3) is 2~5min.
Preferably, the present processes include the following steps:
1) room temperature deionized water is added into perfluoroethylene-propylene emulsion, adjusts lotion specific gravity 1.06~1.09, opens
Stirring carries out 23~25min of physics demulsification to lotion under conditions of 1200~1600 revs/min；
2) the flocculating agent bicarbonate of the perfluoroethylene-propylene emulsion solid content 1.5~2% is incorporated as into above-mentioned emulsion
Ammonium, continuation is stirred with identical revolving speed to perfluoroethylene-propylene emulsion to be demulsified completely；
3) it is carried out with the room temperature deionized water that the volume ratio for the perfluoroethylene-propylene being precipitated with demulsification is 1/2~2/3
Repeatedly washing, until the conductivity of washing water is lower than 3us/cm after detection.
It is furthermore preferred that the present processes include the following steps:
1) room temperature deionized water is added into perfluoroethylene-propylene emulsion, adjusts lotion specific gravity 1.06~1.08, opens
Stirring carries out 23~25min of physics demulsification to lotion under conditions of 1200~1600 revs/min；
2) the flocculating agent ammonium hydrogen carbonate of the perfluoroethylene-propylene (copolymer) emulsion solid content 1.8~2% is incorporated as into above-mentioned emulsion,
Continuation is stirred with identical revolving speed to perfluoroethylene-propylene emulsion to be demulsified completely；
3) it is carried out with the room temperature deionized water that the volume ratio for the perfluoroethylene-propylene being precipitated with demulsification is 1/2~2/3
Repeatedly washing, until the conductivity of washing water is lower than 3us/cm after detection.
Method of the present invention has the following beneficial effects:
1) adjusting and the washing in later period of the method for the present invention in early period is all made of normal-temperature water, does not need using high temperature
Water or water at low temperature, energy conservation and environmental protection；Used flocculating agent ammonium hydrogen carbonate good water solubility is easy washing removal, and remaining carbon
Sour hydrogen ammonium can remove effectively in the drying of subsequent resin, not pollute resin.
2) it is demulsified, the resin in perfluoroethylene-propylene emulsion can be precipitated completely, resin using method of the invention
Yield it is high, and compared with other methods, not will increase the dosage of subsequent wash water.
3) method and step of the invention is simple, environmentally friendly, is conducive to industrialization large-scale production.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
The present embodiment is related to a kind of preparation method of exhaustive fluorinated ethylene propylene, includes the following steps:
1) room temperature deionized water is added into perfluoroethylene-propylene emulsion, adjusts lotion specific gravity 1.08, opens stirring,
Physics demulsification 25min is carried out to lotion under conditions of 1200 revs/min；
2) be incorporated as the flocculating agent ammonium hydrogen carbonate of resin solid content 2% into above-mentioned emulsion, continue with identical revolving speed into
Row stirring is demulsified completely to perfluoroethylene-propylene emulsion；
3) it is carried out with the room temperature deionized water that the volume ratio for the perfluoroethylene-propylene being precipitated with demulsification is 1/2~2/3
Repeatedly washing, until the conductivity of washing water is lower than 3us/cm after detection.
Embodiment 2
The present embodiment is related to a kind of preparation method of exhaustive fluorinated ethylene propylene, includes the following steps:
1) room temperature deionized water is added into perfluoroethylene-propylene emulsion, adjusts lotion specific gravity 1.06, opens stirring,
Physics demulsification 23min is carried out to lotion under conditions of 1600 revs/min；
2) it is incorporated as the flocculating agent ammonium hydrogen carbonate of resin solid content 1.8% into above-mentioned emulsion, continues with identical revolving speed
It is stirred to perfluoroethylene-propylene emulsion and is demulsified completely；
3) it is carried out with the room temperature deionized water that the volume ratio for the perfluoroethylene-propylene being precipitated with demulsification is 1/2~2/3
Repeatedly washing, until the conductivity of washing water is lower than 3us/cm after detection.
Embodiment 3
The present embodiment is related to a kind of preparation method of exhaustive fluorinated ethylene propylene, includes the following steps:
1) room temperature deionized water is added into perfluoroethylene-propylene emulsion, adjusts lotion specific gravity 1.09, opens stirring,
Physics demulsification 25min is carried out to lotion under conditions of 1400 revs/min；
2) it is incorporated as the flocculating agent ammonium hydrogen carbonate of resin solid content 1.5% into above-mentioned emulsion, continues with identical revolving speed
It is stirred to perfluoroethylene-propylene emulsion and is demulsified completely；
3) it is carried out with the room temperature deionized water that the volume ratio for the perfluoroethylene-propylene being precipitated with demulsification is 1/2~2/3
Repeatedly washing, until the conductivity of washing water is lower than 3us/cm after detection.
Comparative example 1
The present embodiment is related to a kind of method being demulsified to poly- ethylene-propylene resin, and compared with Example 1, difference exists
In, omit step 2) in demulsification of saltouing, only carry out machinery demulsification.
Comparative example 2
The present embodiment is related to a kind of method being demulsified to poly- ethylene-propylene resin, and compared with Example 1, difference exists
In in step 1), the density for adjusting lotion is 1.25.
Comparative example 3
The present embodiment is related to a kind of method being demulsified to poly- ethylene-propylene resin, and compared with Example 1, difference exists
In in step 1), the density for adjusting lotion is 1.2.
Comparative example 4
The present embodiment is related to a kind of method being demulsified to poly- ethylene-propylene resin, and compared with Example 1, difference exists
In using MgCl2As demulsification liquid.
Comparative example 5
The present embodiment is related to a kind of method being demulsified to poly- ethylene-propylene resin, and compared with Example 1, difference exists
In, use aluminum aluminum sulfate as demulsification liquid.
Comparison of experiment results analysis:
It can be seen that from upper table result comparative analysis.Finally detection discovery, resin in the lotion of mechanical coalescence after having agglomerated
Solid content is there are also 3% or so, and mechanical coalescence adds and saltouts that agglomerate the solid content of lotion be only 0.001%.It is solidifying with machinery when washing
Poly- plus ammonium hydrogen carbonate, which is saltoutd, agglomerates deionized water washing 7 times with regard to qualified, and has washed 6 all qualified, washing waters with mechanical coalescence
Dosage is similar.With mechanical coalescence plus MgCl214 times and 15 times just qualified, washing waters have been washed respectively with what aluminum aluminum sulfate agglomerated
Dosage is more, if the Auto-regulating System of Density of Heavy Medium of lotion is not within the scope of this application, the solid content in the lotion of cohesion is also higher.Therefore,
Comprehensively consider and compared by emulsion solid content, slurry amount after demulsification time, cohesion, when the present processes shorten demulsification
Between, emulsion coagulation is more complete, reduces slurry amount, to substantially increase the production capacity of equipment, it is dirty to reduce environment
It contaminates, be conducive to industrialized production.
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (9)
1. a kind of cohesion washing methods of fluorinated ethylene propylene resin, which comprises the steps of:
1) room temperature deionized water is added into perfluoroethylene-propylene emulsion, adjusts lotion specific gravity 1.03~1.15, opens stirring,
15~60min of physics demulsification is carried out to lotion under conditions of 500~2000 revs/min；
2) it is incorporated as the flocculating agent ammonium hydrogen carbonate of the perfluoroethylene-propylene emulsion solid content 1~5% into above-mentioned emulsion, continues
It is stirred to perfluoroethylene-propylene emulsion and is demulsified completely；
3) it is washed repeatedly with the perfluoroethylene-propylene that demulsification is precipitated in room temperature deionized water, until detection is qualified.
2. the method according to claim 1, wherein the step 1) in adjust lotion specific gravity be 1.05~
1.1。
3. according to the method described in claim 2, it is characterized in that, the step 1) in adjust lotion specific gravity be 1.06~
1.09。
4. method according to claim 1 or 2, which is characterized in that the actual conditions stirred in the step 1) be
20~25min is stirred under conditions of 1200~1600 revs/min.
5. the method according to claim 1, wherein the additive amount of flocculating agent is described poly- complete in the step 2)
The 1.5~2.5% of fluoro ethyl propene emulsion solid content.
6. according to the method described in claim 5, it is characterized in that, the additive amount of flocculating agent is described poly- complete in the step 2)
The 1.5~2% of fluoro ethyl propene emulsion solid content.
7. the method according to claim 1, wherein the step 3) in washing when, the poly- perfluor for the precipitation that is demulsified
The ratio between volume of second propylene and room temperature deionized water is 1/2~2/3.
8. the method according to claim 1, wherein the time washed every time in the step 3) is 2~5min.
9. the method according to claim 1, wherein including the following steps:
1) room temperature deionized water is added into perfluoroethylene-propylene emulsion, adjusts lotion specific gravity 1.06~1.09, opens stirring,
23~25min of physics demulsification is carried out to lotion under conditions of 1200~1600 revs/min；
2) the flocculating agent ammonium hydrogen carbonate of the perfluoroethylene-propylene emulsion solid content 1.5~2% is incorporated as into above-mentioned emulsion, after
Continuous be stirred with identical revolving speed to perfluoroethylene-propylene emulsion is demulsified completely；
3) it is carried out repeatedly with the room temperature deionized water that the volume ratio for the perfluoroethylene-propylene being precipitated with demulsification is 1/2~2/3
Washing, until the conductivity of washing water is lower than 3us/cm after detection.
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Cited By (5)
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| CN110790956A (en) * | 2019-11-01 | 2020-02-14 | 常熟三爱富中昊化工新材料有限公司 | Preparation method of superfine fluororesin powder |
| CN112707472A (en) * | 2020-12-31 | 2021-04-27 | 南京亚之清环保服务有限公司 | Sewage treatment method and system adopting bicarbonate as demulsifier |
| 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 |
| CN114621460A (en) * | 2022-04-08 | 2022-06-14 | 四川轻化工大学 | Aqueous polyvinylidene fluoride concentrated emulsion and preparation method and application thereof |
| CN115477771A (en) * | 2021-05-31 | 2022-12-16 | 中昊晨光化工研究院有限公司 | Coagulation washing method of peroxide vulcanized fluororubber emulsion for mould pressing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN112707472A (en) * | 2020-12-31 | 2021-04-27 | 南京亚之清环保服务有限公司 | Sewage treatment method and system adopting bicarbonate as demulsifier |
| CN115477771A (en) * | 2021-05-31 | 2022-12-16 | 中昊晨光化工研究院有限公司 | Coagulation washing method of peroxide vulcanized fluororubber emulsion for mould pressing |
| CN114621460A (en) * | 2022-04-08 | 2022-06-14 | 四川轻化工大学 | Aqueous polyvinylidene fluoride concentrated emulsion and preparation method and application thereof |
| CN114621460B (en) * | 2022-04-08 | 2023-04-25 | 四川轻化工大学 | Aqueous polyvinylidene fluoride concentrated emulsion and preparation method and application thereof |
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