CN107868145B - A kind of cohesion washing methods of fluorine resin F2314 - Google Patents
A kind of cohesion washing methods of fluorine resin F2314 Download PDFInfo
- Publication number
- CN107868145B CN107868145B CN201610848757.5A CN201610848757A CN107868145B CN 107868145 B CN107868145 B CN 107868145B CN 201610848757 A CN201610848757 A CN 201610848757A CN 107868145 B CN107868145 B CN 107868145B
- Authority
- CN
- China
- Prior art keywords
- fluororesin
- lotion
- deionized water
- temperature
- fluorine resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
Abstract
The present invention relates to a kind of cohesion washing methods of fluorine resin F2314 lotion, which comprises the steps of: 1) specific gravity that the lotion of Fluororesin F2314 is adjusted with deionized water is 1.05~1.12, obtains dilute emulsion；2) dilute emulsion is agglomerated into 5~8h under conditions of temperature is -15~-5 DEG C；3) by the lotion after the agglomeration process temperature be 30~70 DEG C under conditions of thaw 10~15h, be precipitated 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 lotion to emulsion polymerization, the successful demulsification to Fluororesin F2314 can be realized, obtained powdered Fluororesin F2314, the contact area for increasing material and washing water can obtain qualified product with less washing times and water consumption.
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 technique
Fluororesin F2314 has excellent physical and chemical performance, has good adhesive property, the material is mainly to powder
Material plays bonding coating function, and performance change has larger impact to the processability and mechanical property of dusty material.
Since this kind of material is related to military engineering and sophisticated technology, the report in relation to its research overview, technology contents is few.
The external only a few countries such as the U.S. and Russia produce.Such external material all carries out China stringent embargo.
Industrialized polymerization is mainly emulsion polymerization to Fluororesin F2314, and 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 such as freezing, mechanical stirring, chemical demulsification are such as saltoutd.At present
It is directed to Fluororesin F2314 efficient cohesion washing methods not yet, causes flocculating result bad, uses water in the process of washing
Amount is big.
Summary of the invention
The object of the present invention is to provide the cohesion washing methods of fluorine resin F2314 a kind of, include the following steps:
1) specific gravity that the lotion of Fluororesin F2314 is adjusted with deionized water is 1.05~1.12, obtains dilute emulsion；
2) dilute emulsion is agglomerated into 5~8h in the industrial brine that temperature is -15~-5 DEG C；
3) by the lotion after the agglomeration process temperature be 30~70 DEG C under conditions of thaw 10~15h, be precipitated fluorine tree
Rouge F2314 crude product；
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 specific gravity 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
Diameter is too big and leads to be not easy washes clean, wastes water source and manpower and material resources, will not be not easy and washing moisture because partial size is too small
From, thawing condition described in claim 1 is further selected, carrying down for fluorinated resin particle will not be carried out, it can also be shorter
In time, complete to thaw in more energy efficient mode.
Preferably, in the step 1), the specific gravity for adjusting the lotion of Fluororesin F2314 is 1.06~1.1.Fluorine resin cream
The specific gravity of liquid reflects the content of resin in lotion, and size will affect the partial size that resin is formed by after cohesion, if specific gravity mistake
Greatly, lotion is more sticky, and the resin partial size formed in coacervation process is excessive, if specific gravity is too small, the resin that is formed in coacervation process
Partial size filtering, this is unfavorable for subsequent washing.Degree of control specific gravity is 1.06~1.1, is more advantageous to the tree to form moderate in grain size
Rouge.
Preferably, in the step 2), condensation temperature is -12~-6 DEG C.The temperature of cohesion influences the formation of resin particle
Speed ultimately forms the size of resin particle with the concentration joint effect of lotion, too high or too low for temperature, is unfavorable for being formed suitable
The resin particle of suitable size is more advantageous to form the resin that partial size is 280~360 μm at the temperature disclosed above.
Preferably, in the step 2), pool time is 6~8h.Under this time, F2314 lotion energy both can guarantee
Enough cohesions just completely, will not also bring the waste of the energy because pool time is too long.
Preferably, in the step 3), thaw point is 40~60 DEG C.At these temperatures, thawing time can be shortened, again
It can make F2314 particle not conglomeration, keeping average grain diameter is 280~360 μm.
Preferably, in the step 3), thawing time is 10~12h.Under above-mentioned temperature conditions, F2314 lotion can be with
It thaws 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 resin and deionized water is 1:(2~3 when washing).
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 conductivity of deionized water is less than 5 μ s/cm after washing.
Preferably, the Nacl is NaCl and MgCl2Mixed solution, wherein the mass percent of NaCl be 25~
30%, MgCl2Mass percent be 15~20%.
Preferably, method of the present invention includes the following steps:
1) specific gravity that the lotion 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 agglomerated with -15 DEG C of industrial chilled brines；
3) by the lotion after the agglomeration process temperature be 40~60 DEG C under conditions of thaw 10~12h, be precipitated fluorine tree
Rouge F2314 crude product；
4) the Fluororesin F2314 crude product is washed with deionized water, obtains fluorine resin F2314.
Further preferably, method of the present invention includes the following steps:
1) specific gravity that the lotion 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) lotion after the agglomeration process is thawed 12h under conditions of temperature is 55 DEG C, it is thick that Fluororesin F2314 is precipitated
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 when washing
The volume ratio of F2314 resin and deionized water is 1:(2~3)
The industrial brine is NaCl and MgCl2Mixed solution, wherein the mass percent of NaCl be 25~30%,
MgCl2Mass percent be 15~20%.
Method of the present invention has the following beneficial effects:
Preparation method provided by the invention is easy to operate, only passes through the freezing of the Fluororesin F2314 lotion to emulsion polymerization
Cohesion, can be realized the successful demulsification to Fluororesin F2314, obtained powdered Fluororesin F2314 increases material and washes
Wash the contact area of water.
Further, the application adjusts suitable condensation temperature, can form grain by the suitable specific gravity of control fluorine-containing latex
Diameter is that 280~360 μm of Fluororesin F2314 particle further controls the condition of defrosting, can protect not conglomeration between particle,
Wash time finally is shortened, qualified product can be obtained with less washing times and water consumption.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Industrial brine used in embodiment is the mixed solution of NaCl and MgCl2, and wherein the mass percent of NaCl is
30%, MgCl2Mass percent be 20%.
Embodiment 1
The present embodiment is related to the cohesion washing methods of fluorine resin F2314 a kind of, includes the following steps:
1) deionized water is added into Fluororesin F2314 lotion, adjusting lotion specific gravity is 1.08；
2) the Fluororesin F2314 lotion after adjustment specific gravity is put into -10 DEG C of salt water, is freezed with -15 DEG C of industrial brines, coagulated
Poly- 7h；
3) lotion after the agglomeration process is thawed 12h under conditions of temperature is 55 DEG C, it is thick that Fluororesin F2314 is precipitated
Product；
4) by the Fluororesin F2314 crude product after the defrosting, with temperature be 60 DEG C deionized water (Fluororesin F2314 with
Deionized water volume ratio is 1:2) washing, wash time is in 5min, repeatedly washing 4 times, the conductance of deionized water after measurement washing
Rate is qualification lower than 5 μ s/cm, and Fluororesin F2314 is white powdered after washing.
Embodiment 2
The present embodiment is related to the cohesion washing methods of fluorine resin F2314 a kind of, includes the following steps:
1) deionized water is added into Fluororesin F2314 lotion, adjusting lotion specific gravity is 1.05；
2) the Fluororesin F2314 lotion after adjustment specific gravity is put into -15 DEG C of industrial brines, agglomerates 5h；
3) lotion after the agglomeration process is thawed 15h under conditions of temperature is 30 DEG C, it is thick that Fluororesin F2314 is precipitated
Product；
4) deionized water for being 100 DEG C with temperature (Fluororesin F2314 and deionized water volume ratio are 1:3) is to the defrosting
Fluororesin F2314 crude product afterwards is washed, and wash time is washed 5 times repeatedly in 4min, the electricity of deionized water after measurement washing
Conductance is qualification lower than 5 μ s/cm, and Fluororesin F2314 is white powdered after washing.
Embodiment 3
The present embodiment is related to the cohesion washing methods of fluorine resin F2314 a kind of, includes the following steps:
1) deionized water is added into Fluororesin F2314 lotion, adjusting lotion specific gravity is 1.12；
2) the Fluororesin F2314 lotion after adjustment specific gravity is put into -5 DEG C of salt water, agglomerates 8h；
3) lotion after the agglomeration process is thawed 10h under conditions of temperature is 70 DEG C, it is thick that Fluororesin F2314 is precipitated
Product；
4) deionized water for being 30 DEG C with temperature (Fluororesin F2314 and deionized water volume ratio are 1:3) is to the defrosting
Fluororesin F2314 crude product afterwards is washed, wash time 10min, is washed 6 times repeatedly, deionized water after measurement washing
Conductivity is qualification lower than 5 μ s/cm, and Fluororesin F2314 is white powdered after washing.
Embodiment 4
The present embodiment is related to the cohesion washing methods of fluorine resin F2314 a kind of, includes the following steps:
1) deionized water is added into Fluororesin F2314 lotion, adjusting lotion specific gravity is 1.06；
2) the Fluororesin F2314 lotion after adjustment specific gravity is put into -12 DEG C of salt water, agglomerates 6h；
3) lotion after the agglomeration process is thawed 12h under conditions of temperature is 40 DEG C, it is thick that Fluororesin F2314 is precipitated
Product；
4) deionized water for being 40 DEG C with temperature (Fluororesin F2314 and deionized water volume ratio are 1:3) is to the defrosting
Fluororesin F2314 crude product afterwards is washed, wash time 10min, is washed 4 times repeatedly, deionized water after measurement washing
Conductivity is qualification lower than 5 μ s/cm, and Fluororesin F2314 is white powdered after washing.
Embodiment 5
The present embodiment is related to the cohesion washing methods of fluorine resin F2314 a kind of, includes the following steps:
1) deionized water is added into Fluororesin F2314 lotion, adjusting lotion specific gravity is 1.1；
2) the Fluororesin F2314 lotion after adjustment specific gravity is put into -6 DEG C of salt water, agglomerates 8h；
3) lotion after the agglomeration process is thawed 10h under conditions of temperature is 60 DEG C, it is thick that Fluororesin F2314 is precipitated
Product；
4) deionized water for being 70 DEG C with temperature (Fluororesin F2314 and deionized water volume ratio are 1:3) is 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 is qualification lower than 5 μ s/cm, and Fluororesin F2314 is white powdered after washing.
Comparative example 1
Compared with Example 1, difference is, in the step 1), the specific gravity for adjusting the lotion is 1.02.
Comparative example 2
Compared with Example 1, difference is, in the step 1), the specific gravity for adjusting the lotion is 1.2.
Comparative example 3
Compared with Example 1, difference is, in the step 2), the Fluororesin F2314 lotion after adjustment specific gravity is put
Enter in -20 DEG C of salt water, agglomerates 7h.
Comparative example 4
Compared with Example 1, difference is, in the step 2), the Fluororesin F2314 lotion after adjustment specific gravity is put
Enter in -2 DEG C of salt water, agglomerates 7h.
Comparative example 5
Compared with Example 1, difference is, in the step 3), is in temperature by the lotion after the agglomeration process
Thaw 12h under conditions of 80 DEG C.
Experimental example
Comparative example 2
Compared with Example 1, difference is, in the step 1), the specific gravity for adjusting the lotion is 1.2.
It can be seen from the above result that washing 4~5 times are that can reach requirement, 4 He of comparative example using method of the present invention
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
It is smaller than 5us/cm, but causes partial size smaller since specific gravity is smaller, is easy blocking filter cloth in the process of washing.Comparison
Although method in example 3 also passes through 4 washings can reach requirement, but temperature is too low can bring bigger energy consumption.
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 (11)
1. a kind of cohesion washing methods of fluorine resin F2314 lotion, which comprises the steps of:
1) specific gravity that the lotion of Fluororesin F2314 is adjusted with deionized water is 1.05 ~ 1.12, obtains dilute emulsion；
2) dilute emulsion is agglomerated into 5 ~ 8h in the industrial brine that temperature is -15 ~ -5 DEG C；
3) by the lotion after the agglomeration process temperature be 30 ~ 70 DEG C under conditions of thaw 10 ~ 15h, be precipitated Fluororesin F2314
Crude product；
4) the Fluororesin F2314 crude product is washed with deionized water, obtains fluorine resin F2314.
2. the method according to claim 1, wherein adjusting the lotion of Fluororesin F2314 in the step 1)
Specific gravity is 1.06 ~ 1.1.
3. the method according to claim 1, wherein condensation temperature is -12 ~ -6 DEG C in the step 2.
4. the method according to claim 1, wherein pool time is 6 ~ 8h in the step 2.
5. the method according to claim 1, wherein thaw point is 40 ~ 60 DEG C in the step 3).
6. the method according to claim 1, wherein thawing time is 10 ~ 12h in the step 3).
7. the method according to claim 1, wherein 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:(2 ~ 3 when washing).
8. method according to claim 1 or claim 7, which is characterized in that in the step 4), the conductance of deionized water after washing
Rate is less than 5 μ s/cm.
9. the method according to claim 1, wherein the Nacl is NaCl and MgCl2Mixed solution,
The mass percent of middle NaCl is 25 ~ 30%, MgCl2Mass percent be 15 ~ 20%.
10. according to the method described in claim 8, it is characterized in that, the Nacl is NaCl and MgCl2Mixed solution,
The mass percent of middle NaCl is 25 ~ 30%, MgCl2Mass percent be 15 ~ 20%.
11. the method according to claim 1, wherein including the following steps:
1) specific gravity that the lotion 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 7h under conditions of temperature is -10 DEG C；
3) lotion after the agglomeration process is thawed 12h under conditions of temperature is 55 DEG C, Fluororesin F2314 crude product is precipitated；
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 F2314 when washing
The volume ratio of resin and deionized water is 1:(2 ~ 3)
The industrial brine is NaCl and MgCl2Mixed solution, wherein the mass percent of NaCl be 25 ~ 30%, MgCl2Matter
Measuring percentage is 15 ~ 20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610848757.5A CN107868145B (en) | 2016-09-26 | 2016-09-26 | A kind of cohesion washing methods of fluorine resin F2314 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610848757.5A CN107868145B (en) | 2016-09-26 | 2016-09-26 | A kind of cohesion washing methods of fluorine resin F2314 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107868145A CN107868145A (en) | 2018-04-03 |
| CN107868145B true CN107868145B (en) | 2019-07-09 |
Family
ID=61751685
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610848757.5A Active CN107868145B (en) | 2016-09-26 | 2016-09-26 | A kind of cohesion washing methods of fluorine resin F2314 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107868145B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186668A (en) * | 2007-11-07 | 2008-05-28 | 中昊晨光化工研究院 | Method for preparing fluorine-containing rubber used for paint |
| CN104497189A (en) * | 2014-10-28 | 2015-04-08 | 浙江巨圣氟化学有限公司 | Preparation method of thermally-stable raw fluorubber |
-
2016
- 2016-09-26 CN CN201610848757.5A patent/CN107868145B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186668A (en) * | 2007-11-07 | 2008-05-28 | 中昊晨光化工研究院 | Method for preparing fluorine-containing rubber used for paint |
| CN104497189A (en) * | 2014-10-28 | 2015-04-08 | 浙江巨圣氟化学有限公司 | Preparation method of thermally-stable raw fluorubber |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107868145A (en) | 2018-04-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107868145B (en) | A kind of cohesion washing methods of fluorine resin F2314 | |
| CN104219797A (en) | Graphene electrothermal film | |
| CN103752292B (en) | For the preparation method of the porous Ca-alginate gel beads of heavy metal-polluted water treatment | |
| CN103887488B (en) | Lithium ion battery peach kernel shape SnO 2the preparation method of-Graphene-carbon composite | |
| CN101439870B (en) | Preparation of nano-scale indium and tin oxides blue powder | |
| CN104530265B (en) | A kind of fluoropolymer powder and preparation method thereof | |
| CN109320634B (en) | A kind of cohesion washing methods of fluorinated ethylene propylene resin | |
| CN104745019B (en) | A kind of preparation method of automatically cleaning characteristic nano silicon/titania modified PVDF super-hydrophobic composite films | |
| CN102875711B (en) | Condensing washing method of polyvinylidene fluoride emulsion | |
| CN106044753B (en) | Preparation method of high-orientation graphene film | |
| CN101370856B (en) | Method for the preparation of fluoropolymer powdered materials | |
| CN113371765A (en) | Preparation method of electromagnetic wave-absorbing material based on modification of MXene by NiFe layered double-metal oxide and product thereof | |
| CN104212413B (en) | A kind of ice-covering-proof material of liquid filling cellular silicone and preparation method | |
| CN109021932A (en) | Graphene oxide/silver particles complex intensifying paraffin wax type phase-changing energy storage material and preparation method thereof | |
| Hanh et al. | Icephobic approach on hierarchical structure polymer thin-film | |
| CN105363039B (en) | A kind of sea grass polysaccharide microcapsules and preparation method thereof | |
| CN107383518B (en) | Preparation method of polyethylene-graphene compound | |
| CN104790204A (en) | Preparation method of super-hydrophobic-hydrophilic reversible intelligent conversion cotton fabric | |
| Yan et al. | Biomineralization of uniform gallium oxide rods with cellular compatibility | |
| Lue et al. | Modeling water states in polyvinyl alcohol-fumed silica nano-composites | |
| CN106543976A (en) | A kind of TiO of high dispersion stability2‑H2O nano-fluids and its preparation method and application | |
| Ding et al. | Water vapor induced phase separation: A simple and efficient method for fabricating polyetherimide microspheres | |
| CN104497852A (en) | Preparation methods of superhydrophobic methyltrimethoxysilane/ZnO composite sol and composite coating | |
| CN107057112A (en) | The preparation method of graphene/white carbon black composite material | |
| CN104194638B (en) | The preparation method of the brilliant rosin of resistive connection |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |