CN107868145A - A kind of fluorine resin F2314 cohesion washing methods - Google Patents
A kind of fluorine resin F2314 cohesion washing methods Download PDFInfo
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- CN107868145A CN107868145A CN201610848757.5A CN201610848757A CN107868145A CN 107868145 A CN107868145 A CN 107868145A CN 201610848757 A CN201610848757 A CN 201610848757A CN 107868145 A CN107868145 A CN 107868145A
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- fluororesin
- emulsion
- deionized water
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- 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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Abstract
The present invention relates to a kind of cohesion washing methods of fluorine resin F2314 emulsions, it is characterised in that comprises the following steps：1) proportion that the emulsion of Fluororesin F2314 is adjusted with deionized water is 1.05~1.12, obtains dilute emulsion；2) dilute emulsion is condensed into 5~8h under conditions of temperature is 15~5 DEG C；3) by the emulsion after the agglomeration process temperature be 30~70 DEG C under conditions of thaw 10~15h, separate out Fluororesin F2314 crude product；4) the Fluororesin F2314 crude product is washed with deionized water, obtains fluorine resin F2314.Method of the present invention only passes through the freeze agglomeration of the Fluororesin F2314 emulsion to emulsion polymerization, the successful demulsification to Fluororesin F2314 can be achieved, obtained powdered Fluororesin F2314, the contact area of material and washings is added, with less washing times and water consumption with regard to qualified product can be obtained.
Description
Technical field
The present invention relates to fluoro-containing macromolecule material field, and in particular to a kind of cohesion washing methods of Fluororesin F2314.
Background technology
Fluororesin F2314 has excellent physical and chemical performance, has good adhesive property, the material is mainly to powder
Material plays cohesive coating function, and its performance change has considerable influence to the processability and mechanical property of dusty material.
Because this kind of material is related to military engineering and sophisticated technology, the report about its research overview, technology contents is few.
The external only a few countries such as U.S. and Russia produce.Such external material all carries out China strict embargo.
Industrialized polymerization is mainly emulsion polymerization to Fluororesin F2314, and the emulsion that emulsion polymerization is formed must
Must just it 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 such as freezing, mechanical agitation, chemical demulsification are such as saltoutd.At present
It is directed to Fluororesin F2314 and does not condense washing methods efficiently also, causes flocculating result bad, water is used during washing
Amount is big.
The content of the invention
It is an object of the invention to provide a kind of fluorine resin F2314 cohesion washing methods, comprise the following steps：
1) proportion that the emulsion of Fluororesin F2314 is adjusted with deionized water is 1.05~1.12, obtains dilute emulsion；
2) dilute emulsion is condensed into 5~8h in the industrial brine that temperature is -15~-5 DEG C；
3) by the emulsion after the agglomeration process temperature be 30~70 DEG C under conditions of thaw 10~15h, separate out fluorine tree
Fat F2314 crude products；
4) the Fluororesin F2314 crude product is washed with deionized water, obtains fluorine resin F2314.
Using method of the present invention, by adjusting the suitable proportion and coherence condition of fluorine resin, gained after cohesion
Fluororesin F2314 average grain diameter be 280~360 μm, this particle size, both will not be because of grain during subsequent wash
Footpath is too big and causes to be not easy washes clean, wastes water source and manpower and materials, will not be also not easy and washing moisture because particle diameter is too small
From, the further thawing condition selected described in claim 1, carrying down for fluorinated resin particle will not be carried out, can also be shorter
In time, complete to thaw in a manner of more energy efficient.
Preferably, in the step 1), the proportion for adjusting the emulsion of Fluororesin F2314 is 1.06~1.1.Fluorine resin breast
The proportion of liquid reflects the content of resin in emulsion, and its size can influence the particle diameter of the resin formed after cohesion, if proportion mistake
Greatly, emulsion is more sticky, and the resin particle diameter formed in coacervation process is excessive, if proportion is too small, the resin that is formed in coacervation process
Particle diameter filters, and this is unfavorable for follow-up washing.Degree of control proportion is 1.06~1.1, is more beneficial for being formed the tree of moderate in grain size
Fat.
Preferably, in the step 2), condensation temperature is -12~-6 DEG C.The temperature of cohesion influences the formation of resin particle
Speed, the size of resin particle is ultimately formed with the concentration joint effect of emulsion, it is too high or too low for temperature, it is unfavorable for being formed suitable
The resin particle of suitable size, at the temperature disclosed above, it is more beneficial for forming the resin that particle diameter is 280~360 μm.
Preferably, in the step 2), pool time is 6~8h.Under this time, F2314 emulsion energy can be both ensured
Enough cohesions just are complete, will not also bring the waste of the energy because pool time is long.
Preferably, in the step 3), thaw point is 40~60 DEG C.At these temperatures, thawing time can be shortened, again
F2314 particle not conglomerations can be made, it is 280~360 μm to keep average grain diameter.
Preferably, in the step 3), thawing time is 10~12h.In the case of said temperature, F2314 emulsions can be with
Thaw completely.
Preferably, in the step 4), the temperature of the deionized water is 30~100 DEG C, the time washed every time is 2~
12min, the volume ratio of fluorine resin F2314 resins and deionized water is 1 during washing:(2~3).
Further preferably, in the step 4), the temperature of the deionized water is 40~70 DEG C, and the time washed every time is
4~10min.
Preferably, in the step 4), the electrical conductivity of deionized water is less than 5 μ s/cm after washing.
Preferably, the Nacl is NaCl and MgCl2Mixed solution, wherein NaCl mass percent be 25~
30%, MgCl2Mass percent be 15~20%.
Preferably, method of the present invention comprises the following steps：
1) proportion that the emulsion of Fluororesin F2314 is adjusted with deionized water is 1.06~1.1, obtains dilute emulsion；
2) by the dilute emulsion under conditions of temperature is -12~-6 DEG C, 6~8h is condensed with -15 DEG C of industrial chilled brines；
3) by the emulsion after the agglomeration process temperature be 40~60 DEG C under conditions of thaw 10~12h, separate out fluorine tree
Fat F2314 crude products；
4) the Fluororesin F2314 crude product is washed with deionized water, obtains fluorine resin F2314.
Further preferably, method of the present invention comprises the following steps:
1) proportion that the emulsion of Fluororesin F2314 is adjusted with deionized water is 1.08, obtains dilute emulsion；
2) dilute emulsion is used into -15 DEG C of industrial brine freeze agglomeration 1h under conditions of temperature is -10 DEG C；
3) by the emulsion after the agglomeration process be 55 DEG C in temperature under conditions of thaw 12h, it is thick to separate out Fluororesin F2314
Product；
4) the Fluororesin F2314 crude product is washed with deionized water, obtains fluorine resin F2314；
The temperature of the deionized water is 30~100 DEG C, and the time washed every time is 2~10min, fluorine resin during washing
The volume ratio of F2314 resins and deionized water is 1:(2~3)
The industrial brine is NaCl and MgCl2Mixed solution, wherein NaCl mass percent be 25~30%,
MgCl2Mass percent be 15~20%.
Method of the present invention has the advantages that：
Preparation method provided by the invention is simple to operate, only passes through the freezing of the Fluororesin F2314 emulsion to emulsion polymerization
Cohesion, you can realize the successful demulsification to Fluororesin F2314, obtained powdered Fluororesin F2314, add material with washing
Wash the contact area of water.
Further, the application adjusts suitable condensation temperature, can form grain by controlling the suitable proportion of fluorine-containing latex
Footpath is 280~360 μm of Fluororesin F2314 particle, further, controls the condition of defrosting, can protect not conglomeration between particle,
Wash time finally is shortened, with less washing times and water consumption with regard to qualified product can be obtained.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.
Industrial brine used is NaCl and MgCl2 mixed solution in embodiment, and wherein NaCl mass percent is
30%, MgCl2Mass percent be 20%.
Embodiment 1
The present embodiment is related to a kind of fluorine resin F2314 cohesion washing methods, comprises the following steps：
1) deionized water is added into Fluororesin F2314 emulsion, regulation emulsion proportion is 1.08；
2) the Fluororesin F2314 emulsion after adjustment proportion is put into -10 DEG C of salt solution, freezed with -15 DEG C of industrial brines, coagulated
Poly- 7h；
3) by the emulsion after the agglomeration process be 55 DEG C in temperature under conditions of thaw 12h, it is thick to separate out Fluororesin F2314
Product；
4) by the Fluororesin F2314 crude product after the defrosting, with deionized water that temperature is 60 DEG C (Fluororesin F2314 with
Deionized water volume ratio is 1:2) wash, wash time is in 5min, repeatedly washing 4 times, the conductance of deionized water after measurement washing
Rate, it is qualified less than 5 μ s/cm, Fluororesin F2314 is white powdered after washing.
Embodiment 2
The present embodiment is related to a kind of fluorine resin F2314 cohesion washing methods, comprises the following steps：
1) deionized water is added into Fluororesin F2314 emulsion, regulation emulsion proportion is 1.05；
2) the Fluororesin F2314 emulsion after adjustment proportion is put into -15 DEG C of industrial brines, condenses 5h；
3) by the emulsion after the agglomeration process be 30 DEG C in temperature under conditions of thaw 15h, it is thick to separate out Fluororesin F2314
Product；
4) (Fluororesin F2314 and deionized water volume ratio are 1 to the deionized water for being 100 DEG C with temperature:3) to the defrosting
Fluororesin F2314 crude product afterwards is washed, and wash time is in 4min, repeatedly washing 5 times, the electricity of deionized water after measurement washing
Conductance, it is qualified less than 5 μ s/cm, Fluororesin F2314 is white powdered after washing.
Embodiment 3
The present embodiment is related to a kind of fluorine resin F2314 cohesion washing methods, comprises the following steps：
1) deionized water is added into Fluororesin F2314 emulsion, regulation emulsion proportion is 1.12；
2) the Fluororesin F2314 emulsion after adjustment proportion is put into -5 DEG C of salt solution, condenses 8h；
3) by the emulsion after the agglomeration process be 70 DEG C in temperature under conditions of thaw 10h, it is thick to separate out Fluororesin F2314
Product；
4) (Fluororesin F2314 and deionized water volume ratio are 1 to the deionized water for being 30 DEG C with temperature:3) to the defrosting
Fluororesin F2314 crude product afterwards is washed, wash time 10min, is washed 6 times repeatedly, deionized water after measurement washing
Electrical conductivity, it is qualified less than 5 μ s/cm, Fluororesin F2314 is white powdered after washing.
Embodiment 4
The present embodiment is related to a kind of fluorine resin F2314 cohesion washing methods, comprises the following steps：
1) deionized water is added into Fluororesin F2314 emulsion, regulation emulsion proportion is 1.06；
2) the Fluororesin F2314 emulsion after adjustment proportion is put into -12 DEG C of salt solution, condenses 6h；
3) by the emulsion after the agglomeration process be 40 DEG C in temperature under conditions of thaw 12h, it is thick to separate out Fluororesin F2314
Product；
4) (Fluororesin F2314 and deionized water volume ratio are 1 to the deionized water for being 40 DEG C with temperature:3) to the defrosting
Fluororesin F2314 crude product afterwards is washed, wash time 10min, is washed 4 times repeatedly, deionized water after measurement washing
Electrical conductivity, it is qualified less than 5 μ s/cm, Fluororesin F2314 is white powdered after washing.
Embodiment 5
The present embodiment is related to a kind of fluorine resin F2314 cohesion washing methods, comprises the following steps：
1) deionized water is added into Fluororesin F2314 emulsion, regulation emulsion proportion is 1.1；
2) the Fluororesin F2314 emulsion after adjustment proportion is put into -6 DEG C of salt solution, condenses 8h；
3) by the emulsion after the agglomeration process be 60 DEG C in temperature under conditions of thaw 10h, it is thick to separate out Fluororesin F2314
Product；
4) (Fluororesin F2314 and deionized water volume ratio are 1 to the deionized water for being 70 DEG C with temperature:3) to the defrosting
Fluororesin F2314 crude product afterwards is washed, wash time 4min, is washed 5 times repeatedly, the electricity of deionized water after measurement washing
Conductance, it is qualified less than 5 μ s/cm, Fluororesin F2314 is white powdered after washing.
Comparative example 1
Compared with Example 1, its difference is, in the step 1), the proportion for adjusting the emulsion is 1.02.
Comparative example 2
Compared with Example 1, its difference is, in the step 1), the proportion for adjusting the emulsion is 1.2.
Comparative example 3
Compared with Example 1, its difference is, in the step 2), the Fluororesin F2314 emulsion after adjustment proportion is put
Enter in -20 DEG C of salt solution, condense 7h.
Comparative example 4
Compared with Example 1, its difference is, in the step 2), the Fluororesin F2314 emulsion after adjustment proportion is put
Enter in -2 DEG C of salt solution, condense 7h.
Comparative example 5
Compared with Example 1, its difference is, in the step 3), is in temperature by the emulsion after the agglomeration process
Thaw 12h under conditions of 80 DEG C.
Experimental example
Comparative example 2
Compared with Example 1, its difference is, in the step 1), the proportion for adjusting the emulsion is 1.2.
From result above, using method of the present invention, wash 4~5 times and can reach requirement, the He of comparative example 4
Method in comparative example 5, even if washing 7 times, also it is unable to reach requirement.Its conductance after although the method in comparative example 1 is washed 4 times
5us/cm is smaller than, but causes particle diameter smaller because proportion is smaller, filter cloth is easily blocked during washing.Contrast
Although method in example 3 also passes through 4 washings and can reach requirement, but temperature is too low can bring bigger energy consumption.
Although above the present invention is made to retouch in detail with general explanation, embodiment and experiment
State, 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, are belonged to claimed
Scope.
Claims (10)
1. a kind of cohesion washing methods of fluorine resin F2314 emulsions, it is characterised in that comprise the following steps：
1) proportion that the emulsion of Fluororesin F2314 is adjusted with deionized water is 1.05~1.12, obtains dilute emulsion；
2) dilute emulsion is condensed into 5~8h in the industrial brine that temperature is -15~-5 DEG C；
3) by the emulsion after the agglomeration process temperature be 30~70 DEG C under conditions of thaw 10~15h, separate out fluororesin
F2314 crude products；
4) the Fluororesin F2314 crude product is washed with deionized water, obtains fluorine resin F2314.
2. according to the method for claim 1, it is characterised in that in the step 1), adjust the emulsion of Fluororesin F2314
Proportion is 1.06~1.1.
3. according to the method for claim 1, it is characterised in that in the step 2), condensation temperature is -12~-6 DEG C.
4. according to the method for claim 1, it is characterised in that in the step 2), pool time is 6~8h.
5. according to the method for claim 1, it is characterised in that in the step 3), thaw point is 40~60 DEG C.
6. according to the method for claim 1, it is characterised in that in the step 3), thawing time is 10~12h.
7. according to the method for claim 1, it is characterised in that in the step 4), the temperature of the deionized water is 30
~100 DEG C, the time washed every time is 2~12min, and the volume ratio of fluorine resin F2314 and deionized water is 1 during washing:(2
~3).
8. the method according to claim 1 or 7, it is characterised in that in the step 4), the conductance of deionized water after washing
Rate is less than 5 μ s/cm.
9. according to the method described in any one of claim 1~8, it is characterised in that the Nacl is NaCl and MgCl2It is mixed
Solution is closed, wherein NaCl mass percent is 25~30%, MgCl2Mass percent be 15~20%.
10. according to the method for claim 1, it is characterised in that comprise the following steps:
1) proportion that the emulsion of Fluororesin F2314 is adjusted with deionized water is 1.08, obtains dilute emulsion；
2) dilute emulsion is used into -15 DEG C of industrial brine freeze agglomeration 1h under conditions of temperature is -10 DEG C；
3) by the emulsion after the agglomeration process be 55 DEG C in temperature under conditions of thaw 12h, separate out Fluororesin F2314 crude product；
4) the Fluororesin F2314 crude product is washed with deionized water, obtains fluorine resin F2314；
The temperature of the deionized water is 30~100 DEG C, and the time washed every time is 2~10min, fluorine resin during washing
The volume ratio of F2314 resins and deionized water is 1:(2~3)
The industrial brine is NaCl and MgCl2Mixed solution, wherein NaCl mass percent is 25~30%, MgCl2's
Mass percent is 15~20%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109320634A (en) * | 2017-07-31 | 2019-02-12 | 中昊晨光化工研究院有限公司 | A kind of cohesion washing methods of fluorinated ethylene propylene resin |
| CN111675814A (en) * | 2020-04-27 | 2020-09-18 | 山东东岳高分子材料有限公司 | High-fluidity fluororesin slurry and preparation method 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109320634A (en) * | 2017-07-31 | 2019-02-12 | 中昊晨光化工研究院有限公司 | A kind of cohesion washing methods of fluorinated ethylene propylene resin |
| CN109320634B (en) * | 2017-07-31 | 2019-11-22 | 中昊晨光化工研究院有限公司 | A kind of cohesion washing methods of fluorinated ethylene propylene resin |
| CN111675814A (en) * | 2020-04-27 | 2020-09-18 | 山东东岳高分子材料有限公司 | High-fluidity fluororesin slurry and preparation method thereof |
| CN111675814B (en) * | 2020-04-27 | 2022-06-07 | 山东东岳高分子材料有限公司 | High-fluidity fluororesin slurry and preparation method 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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