CN107936168A - A kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin - Google Patents
A kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin Download PDFInfo
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- CN107936168A CN107936168A CN201711234780.6A CN201711234780A CN107936168A CN 107936168 A CN107936168 A CN 107936168A CN 201711234780 A CN201711234780 A CN 201711234780A CN 107936168 A CN107936168 A CN 107936168A
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- 239000011347 resin Substances 0.000 title claims abstract description 17
- 229920005989 resin Polymers 0.000 title claims abstract description 17
- 239000006185 dispersion Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 52
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 43
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- MKTOIPPVFPJEQO-UHFFFAOYSA-N 4-(3-carboxypropanoylperoxy)-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OOC(=O)CCC(O)=O MKTOIPPVFPJEQO-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 15
- 239000012498 ultrapure water Substances 0.000 claims abstract description 14
- 239000000178 monomer Substances 0.000 claims abstract description 11
- 238000006392 deoxygenation reaction Methods 0.000 claims abstract description 9
- 239000003381 stabilizer Substances 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000007858 starting material Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000003999 initiator Substances 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims abstract description 3
- 230000002045 lasting effect Effects 0.000 claims abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 14
- 239000001301 oxygen Substances 0.000 claims description 14
- 229910052760 oxygen Inorganic materials 0.000 claims description 14
- 239000012188 paraffin wax Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 8
- 239000006210 lotion Substances 0.000 claims description 8
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical compound FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 claims description 7
- UUAGAQFQZIEFAH-UHFFFAOYSA-N chlorotrifluoroethylene Chemical group FC(F)=C(F)Cl UUAGAQFQZIEFAH-UHFFFAOYSA-N 0.000 claims description 5
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical group OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims description 5
- -1 perfluoroalkyl vinyl ether Chemical compound 0.000 claims description 4
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims description 2
- 238000011105 stabilization Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 125000001153 fluoro group Chemical class F* 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- 230000006835 compression Effects 0.000 abstract description 3
- 238000007906 compression Methods 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000006116 polymerization reaction Methods 0.000 description 10
- 238000013019 agitation Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000003507 refrigerant Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- BZPCMSSQHRAJCC-UHFFFAOYSA-N 1,2,3,3,4,4,5,5,5-nonafluoro-1-(1,2,3,3,4,4,5,5,5-nonafluoropent-1-enoxy)pent-1-ene Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(F)=C(F)OC(F)=C(F)C(F)(F)C(F)(F)C(F)(F)F BZPCMSSQHRAJCC-UHFFFAOYSA-N 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000010702 perfluoropolyether Substances 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 2
- BLTXWCKMNMYXEA-UHFFFAOYSA-N 1,1,2-trifluoro-2-(trifluoromethoxy)ethene Chemical compound FC(F)=C(F)OC(F)(F)F BLTXWCKMNMYXEA-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011981 development test Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- XUCNUKMRBVNAPB-UHFFFAOYSA-N fluoroethene Chemical compound FC=C XUCNUKMRBVNAPB-UHFFFAOYSA-N 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000002730 succinyl group Chemical group C(CCC(=O)*)(=O)* 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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
- 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
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
-
- 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
- C08F214/262—Tetrafluoroethene with fluorinated vinyl ethers
-
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/30—Inorganic compounds
-
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/32—Organic compounds
- C08F4/34—Per-compounds with one peroxy-radical
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin, high purity water is added in polymeric kettle, after stabilizer and perfluor class surfactant, vacuumize, after deoxygenation, add part tetrafluoroethene, after being heated to reaction temperature, add modified monomer, tetrafluoroethene is continuously added into reaction pressure, add water soluble starter, keep reaction pressure and reaction temperature, tetrafluoroethene stops reaction after reaching addition, wherein water soluble starter is ammonium persulfate and the composite initiator of disuccinic acid peroxide, ammonium persulfate is 1 with disuccinic acid peroxide mass ratio:5 ~ 100, in terms of high purity water mass ratio, disuccinic acid peroxide addition is 0.001% ~ 0.05%, disuccinic acid peroxide adds after reaction pressure reaches, lasting stirring reaction adds ammonium persulfate after 20 ~ 90 minutes, polytetrafluoroethyldispersion dispersion resin with high compression ratio, molecular resin amount narrowly distributing are used to prepare using this method, the product of preparation has the characteristics that straight, smooth, continuous, uniform wall thickness is stablized.
Description
Technical field
The present invention relates to a kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin, belong to technical field of macromolecules.
Background technology
Polytetrafluoroethylene (PTFE) has excellent chemical resistance, heat endurance, dielectric properties, non-stick, weather-proof and rub resistance, and
Surface tension is low, and electrical insulating property is excellent, it has also become industrial indispensable engineering material.Meanwhile polytetrafluoroethylene (PTFE) is also deposited
In some inherent defects, such as high viscosity under high-crystallinity, melting temperature, many difficulties are brought to process, so that poly- four
Vinyl fluoride is above restricted in application.
The higher pure polytetrafluoroethyldispersion dispersion resin of molecular weight is not suitable for processing the product of thinner thickness, such as the bag of cable
Coating and capillary etc., because needing very high extrusion pressure in process, and excessive pressure can cause product to occur
Crackle.
Uniform wall thickness stabilization is very important for the clad and capillary of cable, the even influence product of wall unevenness
Mechanical strength, electric property and appearance.Product wall thickness is uniform and stable except having outside the Pass with processing method, the molecular weight point with resin
It is furnished with much relations.
The content of the invention
The technical problem to be solved by the invention is to provide a kind of modification with high compression ratio and narrow molecular weight distribution to gather
The preparation method of tetrafluoroethene dispersion resin.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
A kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin, adds high purity water, stabilizer and perfluor in polymeric kettle
After class surfactant, polymeric kettle is vacuumized and deoxygenation, after oxygen content is less than 20ppm in polymeric kettle, addition portion
Divide tetrafluoroethylene monomer, after heating polymeric kettle to reaction temperature, add modified monomer, continuously add tetrafluoroethylene monomer to reaction
Pressure, after reaching reaction pressure, adds water soluble starter, starts polymerisation, persistently adds tetrafluoroethylene monomer and remains anti-
Pressure is answered, keeps polymeric kettle reaction temperature, stops reaction after tetrafluoroethylene monomer reaches addition, by reaction lotion through cooling
After isolate stabilizer, stirring cohesion is drying to obtain, wherein in terms of high purity water mass ratio, stabilizer addition is 3% ~ 8%, perfluor
Class surfactant addition is 0.05 ~ 0.5%, and tetrafluoroethylene monomer addition is 30 ~ 55%, is always added with tetrafluoroethylene monomer
Mass ratio meter is measured, the amount of modified monomers is 0.05 ~ 1.5%, and the reaction pressure is 1.5 ~ 3.5MPa, the reaction temperature control
System is between 65 ~ 105 DEG C.
The water soluble starter is the composite initiator of ammonium persulfate and disuccinic acid peroxide, ammonium persulfate and peroxidating
Succinyl mass ratio is 1:5 ~ 100, in terms of high purity water mass ratio, disuccinic acid peroxide addition is 0.001% ~ 0.05%, wherein
Disuccinic acid peroxide adds after reaction pressure reaches, and lasting stirring reaction adds ammonium persulfate after 20 ~ 90 minutes.
The half-life period of disuccinic acid peroxide is longer than ammonium persulfate at the reaction temperatures, adds after first adding disuccinic acid peroxide
Entering ammonium persulfate can be such that free radical more uniformly generates, the narrow molecular weight distribution of primary particle.
The modified monomer is one kind in chlorotrifluoroethylene, hexafluoropropene, vinylidene or perfluoroalkyl vinyl ether
Or multiple combinations.
The modified monomer is added using discontinuous manner, i.e., single disposably adds or composition is separated and repeatedly added.
The perfluor class surfactant is perfluorooctanoic acid or perfluoropolyethercarboxylate.
The stabilizer is paraffin, and fusing point is 60 ~ 61 DEG C.
The polymeric kettle is horizontal agitated vessel, and internal stirrers are hinge paddle type stirrer.There are multiple sculls on agitating shaft
Leaf, is distributed in different directions, has not only reduced demulsification caused by whipping process, but also increase mass transfer effect, has improved reaction uniformity.
The beneficial effect that the present invention is reached：Stablized using this method polymerization process emulsion system, the demulsification of generation is lacked, former
Material list consumption is low.The molecular resin amount narrowly distributing of this method production, the product of preparation have that straight, smooth, continuous, uniform wall thickness is steady
The characteristics of determining, available for the product of processing thinner thickness, the clad and capillary of such as cable.
Embodiment
The invention will be further described below.Following embodiments are only used for the technical side for clearly illustrating the present invention
Case, and be not intended to limit the protection scope of the present invention and limit the scope of the invention.
Embodiment 1：
High purity water 2000L, paraffin 80kg and perfluorooctanoic acid 3.2kg are added into 3000L polymeric kettles, to poly- after addition
Kettle is closed to be vacuumized, fill High Purity Nitrogen alternating deoxygenation.After polymeric kettle oxygen content is less than 20ppm, polymeric kettle can be taken out again true
Sky, then toward adding tetrafluoroethylene monomer in polymeric kettle.After oxygen content is less than 20ppm in kettle, polymeric kettle can be heated to 93 DEG C,
Disposable to add hexafluoropropene 0.8kg, it is 2.5MPa to continuously add tetrafluoroethene to polymeric kettle pressure, is added after reaching reaction pressure
Enter disuccinic acid peroxide 500g, reaction persistently adds tetrafluoroethene and maintains pressure in kettle after starting be 2.5MPa, and passes through polymerization
It is 93 ± 1 DEG C that kettle chuck refrigerant, which maintains temperature in the kettle, and reaction adds ammonium persulfate 12g after forty minutes.Tetrafluoroethene addition reaches
Stop reaction after to 800kg.Lotion is drying to obtain product through refrigerated separation paraffin after being agglomerated by mechanical agitation.
Embodiment 2：
High purity water 2000L, paraffin 100kg and perfluorooctanoic acid 2.5kg are added into 3000L polymeric kettles, it is right after addition
Polymeric kettle is vacuumized, fills High Purity Nitrogen alternating deoxygenation.After polymeric kettle oxygen content is less than 20ppm, polymeric kettle can be taken out again
Vacuum, then toward adding tetrafluoroethylene monomer in polymeric kettle.After oxygen content is less than 20ppm in kettle, polymeric kettle can be heated to 100
DEG C, disposable to add chlorotrifluoroethylene 2kg, it is 2.0MPa to continuously add tetrafluoroethene to polymeric kettle pressure, reaches reaction pressure
Disuccinic acid peroxide 300g is added afterwards, and reaction persistently adds tetrafluoroethene and maintains pressure in kettle after starting be 2.0MPa, and is passed through
It is 100 ± 1 DEG C that jacket of polymerization refrigerant, which maintains temperature in the kettle, and reaction adds ammonium persulfate 12g after twenty minutes.Tetrafluoroethene adds
Amount stops reaction after reaching 700kg.Lotion is drying to obtain product through refrigerated separation paraffin after being agglomerated by mechanical agitation.
Embodiment 3：
High purity water 2000L, paraffin 100kg and perfluorooctanoic acid 4kg are added into 3000L polymeric kettles, to poly- after addition
Kettle is closed to be vacuumized, fill High Purity Nitrogen alternating deoxygenation.After polymeric kettle oxygen content is less than 20ppm, polymeric kettle can be taken out again true
Sky, then toward adding tetrafluoroethylene monomer in polymeric kettle.After oxygen content is less than 20ppm in kettle, polymeric kettle can be heated to 75 DEG C,
Disposable to add hexafluoropropene 3kg, perfluoro propyl vinyl ether 1kg, continuously adding tetrafluoroethene to polymeric kettle pressure is
1.5MPa, adds disuccinic acid peroxide 150g, reaction is persistently added tetrafluoroethene and maintained in kettle after starting after reaching reaction pressure
Pressure is 1.5MPa, and it is 75 ± 1 DEG C to maintain temperature in the kettle by jacket of polymerization refrigerant, and reaction adds persulfuric acid after 70 minutes
Ammonium 16g.Tetrafluoroethene addition stops reaction after reaching 950kg.Lotion is through refrigerated separation paraffin, after being agglomerated by mechanical agitation
It is drying to obtain product.
Embodiment 4：
High purity water 2000L, paraffin 130kg and perfluoropolyether 5kg are added into 3000L polymeric kettles, to polymerization after addition
Kettle is vacuumized, fills High Purity Nitrogen alternating deoxygenation.After polymeric kettle oxygen content is less than 20ppm, polymeric kettle can be vacuumized again,
Then toward adding tetrafluoroethylene monomer in polymeric kettle.After oxygen content is less than 20ppm in kettle, polymeric kettle can be heated to 70 DEG C, one
Secondary property adds hexafluoropropene 2kg, perfluoro propyl vinyl ether 1kg, and it is 1.7MPa to continuously add tetrafluoroethene to polymeric kettle pressure,
Disuccinic acid peroxide 300g is added after reaching reaction pressure, reaction persistently adds pressure in tetrafluoroethene maintenance kettle and is after starting
1.7MPa, and it is 70 ± 1 DEG C to maintain temperature in the kettle by jacket of polymerization refrigerant, reaction adds ammonium persulfate 15g after 80 minutes.
When tetrafluoroethene addition reaches 500kg, property adds chlorotrifluoroethylene 2kg again.Tetrafluoroethene addition reaches 1100kg
Stop reaction afterwards.Lotion is drying to obtain product through refrigerated separation paraffin after being agglomerated by mechanical agitation.
Embodiment 5：
High purity water 2000L, paraffin 130kg and perfluoropolyether 6kg are added into 3000L polymeric kettles, to polymerization after addition
Kettle is vacuumized, fills High Purity Nitrogen alternating deoxygenation.After polymeric kettle oxygen content is less than 20ppm, polymeric kettle can be vacuumized again,
Then toward adding tetrafluoroethylene monomer in polymeric kettle.After oxygen content is less than 20ppm in kettle, polymeric kettle can be heated to 95 DEG C, one
Secondary property adds chlorotrifluoroethylene 4kg, perfluoro propyl vinyl ether 2kg, and continuously adding tetrafluoroethene to polymeric kettle pressure is
2.0MPa, adds disuccinic acid peroxide 700g, reaction is persistently added tetrafluoroethene and maintained in kettle after starting after reaching reaction pressure
Pressure is 2.0MPa, and it is 95 ± 1 DEG C to maintain temperature in the kettle by jacket of polymerization refrigerant, and reaction adds persulfuric acid after 30 minutes
Ammonium 10g.When tetrafluoroethene addition reaches 300kg, property adds hexafluoropropene 3kg again.Tetrafluoroethene addition reaches
Stop reaction after 1000kg.Lotion is drying to obtain product through refrigerated separation paraffin after being agglomerated by mechanical agitation.
Embodiment 6：
High purity water 2000L, paraffin 100kg and perfluoropolyether 6kg are added into 3000L polymeric kettles, to polymerization after addition
Kettle is vacuumized, fills High Purity Nitrogen alternating deoxygenation.After polymeric kettle oxygen content is less than 20ppm, polymeric kettle can be vacuumized again,
Then toward adding tetrafluoroethylene monomer in polymeric kettle.After oxygen content is less than 20ppm in kettle, polymeric kettle can be heated to 87 DEG C, one
Secondary property adds vinylidene 2kg, perfluoro methyl vinyl ether 4kg, and it is 2.0MPa to continuously add tetrafluoroethene to polymeric kettle pressure,
Disuccinic acid peroxide 1000g is added after reaching reaction pressure, reaction persistently adds pressure in tetrafluoroethene maintenance kettle and is after starting
2.0MPa, and it is 87 ± 1 DEG C to maintain temperature in the kettle by jacket of polymerization refrigerant, reaction adds ammonium persulfate 10g after 50 minutes.
When tetrafluoroethene addition reaches 200kg, property adds hexafluoropropene 2kg again.After tetrafluoroethene addition reaches 1000kg
Stop reaction.Lotion is drying to obtain product through refrigerated separation paraffin after being agglomerated by mechanical agitation.
The modification dispersed polytetrafluoroethylresin that each embodiment obtains detects correlation by the method for HG/T2899 and HG/T3028
Can be as shown in table 1 below：
The different embodiment performance parameters of table 1
| Sequence number | SSG | Tensile strength MPa | Elongation at break % | 1600：Extrusion pressure under 1 | Extrudate appearance |
| Embodiment 1 | 2.185 | 32.2 | 363 | 72.5 | It is not straight, smooth, continuous |
| Embodiment 2 | 2.170 | 34.8 | 402 | 60.8 | It is not straight, smooth, continuous |
| Embodiment 3 | 2.170 | 31.5 | 378 | 46.3 | It is not straight, smooth, continuous |
| Embodiment 4 | 2.165 | 36.0 | 425 | 26.7 | It is straight, smooth, continuous |
| Embodiment 5 | 2.165 | 35.3 | 417 | 33.7 | It is straight, smooth, continuous |
| Embodiment 6 | 2.160 | 37.6 | 412 | 31.9 | It is straight, smooth, continuous |
Through development test, modification dispersed polytetrafluoroethylresin prepared by the method for the invention has high compression ratio, the capillary of processing
Pipe surface is smooth, meets properties of product requirement.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, some improvement and deformation can also be made, these are improved and deformation
Also it should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin, it is characterized in that, high purity water, stabilization are added in polymeric kettle
After agent and perfluor class surfactant, polymeric kettle is vacuumized and deoxygenation, when oxygen content is less than 20ppm in polymeric kettle
Afterwards, part tetrafluoroethylene monomer is added, after heating polymeric kettle to reaction temperature, modified monomer is added, continuously adds tetrafluoroethene
Monomer after reaching reaction pressure, adds water soluble starter, starts polymerisation, persistently add tetrafluoroethene to reaction pressure
Monomer maintains reaction pressure, keeps polymeric kettle reaction temperature, stops reaction after tetrafluoroethylene monomer reaches addition, will react
Lotion isolates stabilizer after cooling, and stirring cohesion is drying to obtain, wherein in terms of high purity water mass ratio, stabilizer addition is
3% ~ 8%, perfluor class surfactant addition is 0.05 ~ 0.5%, and tetrafluoroethylene monomer addition is 30 ~ 55%, the water solubility
Initiator is ammonium persulfate and the composite initiator of disuccinic acid peroxide, and ammonium persulfate is 1 with disuccinic acid peroxide mass ratio:5~
100, in terms of high purity water mass ratio, disuccinic acid peroxide addition is 0.001% ~ 0.05%, and wherein disuccinic acid peroxide is reacting
Pressure adds after reaching, and lasting stirring reaction adds ammonium persulfate after 20 ~ 90 minutes, with the total addition of tetrafluoroethylene monomer
Mass ratio meter, the amount of modified monomers are 0.05 ~ 1.5%, and the reaction pressure is 1.5 ~ 3.5MPa, the reaction temperature control
Between 65 ~ 105 DEG C.
2. a kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin according to claim 1, it is characterized in that, it is described to change
Property monomer be one or more combinations in chlorotrifluoroethylene, hexafluoropropene, vinylidene or perfluoroalkyl vinyl ether.
3. a kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin according to claim 2, it is characterized in that, it is described to change
Property monomer using discontinuous manner add.
4. a kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin according to claim 1, it is characterized in that, it is described complete
Fluorine class surfactant is perfluorooctanoic acid or perfluoropolyethercarboxylate.
5. a kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin according to claim 1, it is characterized in that, it is described steady
It is paraffin to determine agent, and fusing point is 60 ~ 61 DEG C.
6. a kind of preparation method of modified polytetrafluoroethyldispersion dispersion resin according to any one of claims 1 to 5, its feature
It is that the polymeric kettle is horizontal agitated vessel, internal stirrers are hinge paddle type stirrer.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111171209A (en) * | 2018-11-12 | 2020-05-19 | 中昊晨光化工研究院有限公司 | A kind of fluororesin and preparation method thereof |
| CN112538125A (en) * | 2020-12-14 | 2021-03-23 | 江西理文化工有限公司 | Preparation method of low molecular weight polytetrafluoroethylene resin |
| CN113736003A (en) * | 2021-09-06 | 2021-12-03 | 浙江巨化股份有限公司氟聚厂 | Method for modifying polytetrafluoroethylene resin by perfluorovinyl ethers |
| US20240141214A1 (en) * | 2021-01-20 | 2024-05-02 | Solvay Specialty Polymers Italy S.P.A. | Fluoropolymer composition |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1295258C (en) * | 2002-12-19 | 2007-01-17 | 旭硝子株式会社 | Tetrafluoroethylene copolymer |
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| CN103012649A (en) * | 2012-12-17 | 2013-04-03 | 山东东岳高分子材料有限公司 | Method for preparing polytetrafluoroethylene dispersion resin with high compression ratio |
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| CN1295258C (en) * | 2002-12-19 | 2007-01-17 | 旭硝子株式会社 | Tetrafluoroethylene copolymer |
| CN102127181A (en) * | 2011-01-31 | 2011-07-20 | 中昊晨光化工研究院 | Method for preparing polyfluortetraethylene dispersion resin |
| CN103012649A (en) * | 2012-12-17 | 2013-04-03 | 山东东岳高分子材料有限公司 | Method for preparing polytetrafluoroethylene dispersion resin with high compression ratio |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111171209A (en) * | 2018-11-12 | 2020-05-19 | 中昊晨光化工研究院有限公司 | A kind of fluororesin and preparation method thereof |
| CN112538125A (en) * | 2020-12-14 | 2021-03-23 | 江西理文化工有限公司 | Preparation method of low molecular weight polytetrafluoroethylene resin |
| CN112538125B (en) * | 2020-12-14 | 2022-11-08 | 江西理文化工有限公司 | A kind of preparation method of low molecular weight polytetrafluoroethylene resin |
| US20240141214A1 (en) * | 2021-01-20 | 2024-05-02 | Solvay Specialty Polymers Italy S.P.A. | Fluoropolymer composition |
| US12460112B2 (en) * | 2021-01-20 | 2025-11-04 | Syensqo Specialty Polymers Italy S.p.A. | Fluoropolymer composition |
| CN113736003A (en) * | 2021-09-06 | 2021-12-03 | 浙江巨化股份有限公司氟聚厂 | Method for modifying polytetrafluoroethylene resin by perfluorovinyl ethers |
| CN113736003B (en) * | 2021-09-06 | 2022-11-25 | 浙江巨化股份有限公司氟聚厂 | Method for modifying polytetrafluoroethylene resin by perfluorovinyl ethers |
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Application publication date: 20180420 |