CN105924561A - Preparation method of modified teflon resin - Google Patents
Preparation method of modified teflon resin Download PDFInfo
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- CN105924561A CN105924561A CN201610430741.2A CN201610430741A CN105924561A CN 105924561 A CN105924561 A CN 105924561A CN 201610430741 A CN201610430741 A CN 201610430741A CN 105924561 A CN105924561 A CN 105924561A
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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
- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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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
Abstract
The invention discloses a preparation method of modified teflon resin. The preparation method includes: adding deionized water, tetrafluoroethylene monomer, activating agent, emulsifier, initiator, stabilizing agent and second monomer into a reaction kettle, performing polymerization reaction under the reaction temperature of 60-110 DEG C and the pressure of 1.0-3.0MPa, ending the reaction when the reaction pressure lowers to 0.1-0.3MPa, cooling and discharging the reaction product, separating the stabilizing agent, adding deionized water into the reaction product after the stabilizing agent is separated to allow solid content to be 10-20wt%, then adding ammonia water to regulate the pH of the reaction product to be 8-10, performing coagulation under the stirring rotation speed of 80-90r/minute and the temperature of 15-35 DEG C, separating out the upper coagulation product, and drying to obtain the modified teflon resin. The preparation method is good in product quality, simple in process, low in cost, energy-saving and environmentally friendly.
Description
Technical field
The present invention relates to the preparation method of fluorine resin, particularly to the preparation method of a kind of modified polytetrafluoroethylresin resin.
Background technology
Polytetrafluoroethylene (PTFE) (PTFE) is the high crystallinity polymer of tetrafluoroethylene monomer (TFE), is that a kind of white has wax-like
The thermoplastic of sensation.In PTFE, fluorine atom replaces the hydrogen atom in polyethylene so that carbon carbon bond is by polyethylene
Plane, wide-spread tortuous conformation be gradually torqued into the helical structure of PTFE, this helical structure just surrounds
Outside PTFE is easily by the carbon chain backbone of chemical erosion, thus define the protective layer of " fluoro " the most complete, make
PTFE shows good mechanical performance, electrical property, chemical-resistance, weather resisteant and non-stick and lubricity, quilt
Synthetic material circle is referred to as " King ".
In application aspect, PTFE is anticorrosion pipeline, pipe fitting, bellows, the pump housing, valve, still, groove, tower and each
Plant the preferred material of the applied corrosion resistant lining of standard device.It addition, as encapsulant, lubriation material machinery, petrochemical industry,
Communications and transportation, medicine, food, light industry, weave, the industry such as building uses quite varied.Process according to PTFE film
After there is selective penetrated property, can be used for separating material, selectively through gas or liquid, its perforated membrane is additionally operable to gas-liquid
Separate and Liquid liquid Separation, and filtering corrosive liquid.Along with the continuous expansion of the market demand, the physics of single PTFE,
Chemistry and the performance such as processing can not meet the market demand, and the not creep resistance of particularly PTFE, melt viscosity are high-leveled and difficult
With machine-shaping, the performance deficiencies such as particularly welding processing processability is poor, poor thermal conductivity, adhesion are poor are seriously made
The about development prospect of PTFE, therefore improves PTFE by PTFE carries out the methods such as filler modified, blending and modifying
Performance particularly welding processing processability, the application market of PTFE can be widened greatly.
Modified polytetrafluoro is prepared as China Patent Publication No. CN101125900A discloses a kind of second comonomer that adds
The method of vinyl.Changing the second comonomer used in method is perfluoropropylvinylether, and initiator can be
Alkali metal or the persulfate of alkaline-earth metal, it is also possible to be redox initiation system.Wherein perfluoropropylvinylether
Add the mode using vacuum to suck, it is to avoid the use of dispersant, but also cause the tensile property of its product relatively
Low, welding processing processability is poor, and production efficiency is the highest.
CN101724117A provides the preparation method of a kind of large molded sheet PTFE resin, is included in condensate
Adding in system and stablize the appropriate amount of acid value stabilization agent of polymerization rate, perfluoroether monomer etc., gained resin has preferably
Wearability, carries out water process to polymer, makes the end group of big molecule be fully hydrolyzed, and reduces the hygroscopicity of polymerizate, but
Owing in this invention, modifying agent feed postition is that intermittence is added, the gained resin uniformity is the highest, thus affects its mechanicalness
Can, particularly welding processing processability is poor.
Modified ptfe resin disclosing a kind of high welding performance in CN103694398B and preparation method thereof, by adjusting
The material addition step of whole polymerization monomer, effectively controls reaction process, and the polymer architecture obtained is tight, and porosity is low but anti-
Answering process complicated, it is more difficult to control, and production efficiency is low, and cost is high, and welding processing processability is poor.
Summary of the invention
In place of the present invention is directed to the deficiencies in the prior art, it is provided that a kind of technique is simple, good product quality, low cost, energy-conservation
The preparation method of the modified polytetrafluoroethylresin resin of environmental protection.
For solving the problems referred to above, the technical solution used in the present invention is: the preparation method of a kind of modified polytetrafluoroethylresin resin,
Comprise the following steps:
(1) by weight, by deionized water 500 parts, tetrafluoroethylene monomer 100～150 parts, activator 0.1～0.18
Part, emulsifying agent 15～22 parts, initiator 0.04～0.08 part, stabilizer 16～21 parts, second comonomer 0.01～0.1 part of throwing
Entering reactor, reaction temperature 60～110 DEG C, pressure is to carry out polymerisation, to reaction under conditions of 1.0～3.0Mpa
When pressure is down to 0.1～0.3Mpa, terminates reaction, cooling discharge, separate stabilizer；
(2), after addition deionized water makes solid content be 10～20wt% in the material after separating stabilizer, ammoniacal liquor is added
Regulation material pH value is 8～10, condenses 8～12min, isolate at 80～90r/min speeds of agitator and 15～35 DEG C
Layer condensation product；
(3) condensation product step (2) obtained is dried at 110～200 DEG C and obtains modified Teflon in 7～12 hours
Resin.
Further:
Described activator is preferably acetic acid or hydrochloric acid.
Described emulsifying agent is preferably perfluorooctanoic acid or perfluoro octyl sulfonic acid potassium.
Described initiator is preferably peroxysuccinic acid or ammonium persulfate.
Described stabilizer is preferably paraffin or chlorofluorocarbon oil.
Described second comonomer is preferably in perfluoro methyl vinyl ether, perfluoroethylvinyl ether, perfluoro propyl vinyl ether
One.Described second comonomer is more preferably perfluoro propyl vinyl ether.
Reaction temperature described in step (1) is preferably 70～100 DEG C, and pressure is preferably 2.0～2.5Mpa.
Solid content described in step (2) is preferably 12～15wt% (wt%, weight/mass percentage composition).
During dry described in step (3), temperature is preferably 130～180 DEG C, and the time is preferably 8～11 hours.
Activator is provided that to polymerization system initial polymerization speed faster.But activator adds too much, polymerization rate
Comparatively fast, it is difficult to control, activator adds very little, and polymerization initial velocity is relatively slow, affects the W-response time, therefore this
The addition number of bright middle activator is 0.1～0.18 part.Activator can select organic acid and inorganic acid, example hydrochloric acid, second
Acid, ethanedioic acid etc., preferably hydrochloric acid or acetic acid.
Emulsifying agent can reduce the surface tension between material makes material be easier to dissolve each other.But emulsifying agent adds too much, and cost increases,
Add very little, the serious breakdown of emulsion of emulsion after reaction, can be caused, cause a large amount of consumption, the therefore addition of emulsifying agent in the present invention
Number is 15～22 parts.Emulsifying agent can select perfluorooctanoic acid salt, perfluorinated sulfonate, such as perfluorooctanoic acid, perfluoro caprylic acid
Sodium, perfluorobutyl potassium sulfonate, perfluoro hexyl potassium sulfonate, perfluoro octyl sulfonic acid potassium, preferably perfluorooctanoic acid or perfluor are pungent
Base potassium sulfonate.
Initiator is provided that the free radical of chain initiation reaction, it is possible to initiated polymerization.But initiator adds too many, temperature
Pressure is difficult to regulate and control, and affects the quality of resin, adds very little, and reaction is difficult to, therefore initiator in the present invention
Adding number is 0.04～0.08 part.Initiator can be selected for alkyl peroxide, persulfuric acid, azo compound, alkyl
Hydroperoxide, such as peroxidating two acyl, ammonium persulfate, azodiisobutyronitrile, peroxysuccinic acid, hydrogen peroxide etc.,
It is preferably peroxysuccinic acid or ammonium persulfate.
Stabilizer can improve the heat endurance of resin, prevents the generation of condensation product.But stabilizer adds too many, locate after increase
The difficulty of reason, can easily entrain in product, affects product quality, adds very little, then polymerization system poor stability, easily
Producing condensation product, therefore in the present invention, the addition number of stabilizer is 16～21 parts.In the present invention the preferred paraffin of stabilizer or
Chlorofluorocarbon oil.
Reaction speed is had an impact by reaction temperature.Reaction speed is accelerated with the rising of reaction temperature, but reaction temperature is the highest,
Heat of polymerization is relatively big, controls difficulty, and reaction temperature is the lowest, and reaction is difficult to, and therefore the reaction temperature in the present invention is 60～110
DEG C, preferably 70～100 DEG C.
Reaction speed is also had an impact by reaction pressure.Reaction speed is accelerated with the rising of reaction pressure, but pressure is the highest,
High to equipment requirement, cost of increasing input, pressure is the lowest, and tetrafluoroethene solubility in water is low, and reaction speed is slow,
Therefore the reaction pressure in the present invention is 1.0～3.0Mpa, preferably 2.0～2.5Mpa.
Polyflon performance, as the core material in modified polytetrafluoroethylresin resin preparation, is changed by second comonomer
Become and play vital effect.Second comonomer selects the perfluorovinyl sulfide ethers monomer containing alcoxyl side base.Second comonomer
The backbone structure of modified polytetrafluoroethylresin resin is sufficiently close to polyflon, therefore can keep the thing of PTFE
Reason, the performance such as chemically and electrically, and the existence of perfluoroalkoxy side base adds irregularity and the flexibility of chain, reduces poly-
The crystallinity of compound and the regularity of crystalline texture, make copolymer have low melt temperature and melt viscosity so that it is processing
Performance is greatly improved so that polyflon is provided with feasibility for welding processing shaping.And second comonomer
Another major reason selecting the perfluorovinyl sulfide ethers containing alcoxyl side base is that its consumption is few and modified effect is preferable,
With low cost, and operation is simple, is directly dissolved in reactor.Second comonomer consumption modified effect at most more preferably,
But can increase cost, so in the present invention, the addition number of second comonomer is 0.01～0.1 part.Second comonomer preferred perfluor first
In base vinyl ethers (PMVE), perfluoroethylvinyl ether (PEVE), perfluoro propyl vinyl ether (PPVE)
One, more preferably perfluoro propyl vinyl ether (PPVE).
The size of particle after condensation degree and cohesion is had an impact by solid content, and the highest then particle of solid content is relatively big, and solid content is the lowest
Then particle is less, and therefore in the present invention, solid content selects 10～20wt%, preferably 12～15wt%.
Modified resin quality is had an impact by cohesion speed of agitator.Rotating speed is the fastest more is conducive to breakdown of emulsion, but speed is too fast, then coagulate
Poly-resin particle out can be partially thin, so mixing speed controls 80～90r/min in the present invention.
Needing to provide the breakdown of emulsion environment of an acid-base balance to material during cohesion, therefore demulsification can be produced by material pH value
Raw considerable influence.PH value is the lowest, and impact cohesion is spent completely；PH value is the highest, and flocculating result will not significantly increase, because of
PH value in this present invention takes 8～10.
Resin quality is had an impact by condensation temperature and time.Temperature is the highest, and condensation degree reduces, and material loss increases, temperature
The lowest, energy consumption is big, uneconomical；Pool time is oversize, can reduce production load, and pool time is the shortest, and cohesion is incomplete,
Therefore the condensation temperature in the present invention is chosen as 15～35 DEG C, and pool time is 8～12min.
Resin quality is had an impact by baking temperature and time.Temperature is the highest or the time is oversize, big to electrical equipment loss, and
Jiao is sent out in resin jaundice；Temperature is the lowest or the time is the shortest, and resin aqueous amount is defective, so the dry temperature of resin in the present invention
Degree is 110～200 DEG C, preferably 130～180 DEG C；Drying time is 7～12 hours, preferably 8～11 hours.
Compared with prior art, the invention have the advantages that
1, technique is simple, low cost, energy-conserving and environment-protective, the method for the present invention simplifies production technology, reduces work strong
Degree and energy consumption, it is simple to operation, improve production efficiency low, reduce production cost；
2, good product quality, energy-conserving and environment-protective, improve the hot strength of TFE, elongation at break, welding
The indexs such as face tensile break strength, bulk density, more than modified Teflon product hot strength 35.8Mpa of production,
Elongation at break more than 444%, solder side tensile break strength at more than 13.5Mpa, bulk density at more than 497g/L,
Both remain the premium properties such as the hot strength of original white resin, elongation at break, meet again resin welding processing
The needs of type, provide more alternative product type for market, have widened the application market of PTFE greatly.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but the present invention is not limited solely to following enforcement
Example.
Embodiment 1: in the autoclave that volume is 1L, adds 500g deionized water, and 0.15g acetic acid, 17g is complete
Fluorine ammonium caprylate, 18g paraffin, second comonomer perfluoro propyl vinyl ether 0.1g, then closed reactor, enters reactor
Row vacuumizes, nitrogen replacement operator, and carries out oxygen content test, when in reactor, oxygen content≤10ppm is qualified.Oxygen contains
Measure qualified after by still temperature rise to 60 DEG C, and in reactor put into TFE monomer to still pressure 2.0Mpa after, use high-pressure pump
Add 0.04g initiator peroxysuccinic acid and start reaction, course of reaction is continually fed into TFE monomer and exists to maintain pressure
2.0Mpa, when TFE addition is 150g, stops adding TFE monomer in reactor, and overbottom pressure is reacted to 0.3Mpa,
Reaction terminates, and by TFE MONOMER RECOVERY in reactor.Stand 5 minutes, open atmospheric valve, cooling discharge, isolate
Paraffin；Then the material after separating paraffin is put into cohesion medial launder, adds deionized water and make solid content be 15wt%；Again
Putting in knockouts by cohesion medial launder material, open stirring, adding ammoniacal liquor regulation material pH value is 9, at 80r/min
Condense 10min at speed of agitator and 30 DEG C, isolate upper strata condensation product；Upper strata condensation product is dried at 170 DEG C 10
Hour i.e. can get modified Teflon white resin 140g.Performance is shown in Table 1.
Embodiment 2: in the autoclave that volume is 1L, adds 500g deionized water, and 0.13g hydrochloric acid, 15g is complete
Fluorine octyl sulfonic acid potassium, 20g paraffin, second comonomer perfluoro methyl vinyl ether 0.05g, then closed reactor, to reaction
Still carries out vacuumizing, nitrogen replacement operator, and carries out oxygen content test, when in reactor, oxygen content≤10ppm is qualified.
By still temperature rise to 100 DEG C after oxygen content is qualified, and in reactor put into TFE monomer to still pressure 3.0Mpa after, use
High-pressure pump adds 0.05g initiator potassium persulfate and starts reaction, is continually fed into TFE monomer to maintain pressure in course of reaction
At 3.0Mpa, when TFE addition is 120g, stopping adding TFE monomer in reactor, overbottom pressure is reacted to 0.2Mpa,
Reaction terminates, and by TFE MONOMER RECOVERY in reactor.Stand 5 minutes, open atmospheric valve, cooling discharge, isolate
Paraffin；Then the material after separating paraffin is put into cohesion medial launder, adds deionized water and make solid content be 10wt%；Again
Putting in knockouts by cohesion medial launder material, open stirring, adding ammoniacal liquor regulation material pH value is 8, at 80r/min
Condense 8min at speed of agitator and 35 DEG C, isolate upper strata condensation product；Upper strata condensation product is dried at 110 DEG C 12 little
Time can get modified Teflon white resin 130g.Performance is shown in Table 1.
Embodiment 3: in the autoclave that volume is 1L, adds 500g deionized water, and 0.1g acetic acid, 20g is complete
Fluorine octyl sulfonic acid potassium, 16g chlorofluorocarbon oil, second comonomer perfluoroethylvinyl ether 0.01g, then closed reactor, to instead
Answer still to carry out vacuumizing, nitrogen replacement operator, and carry out oxygen content test, when in reactor, oxygen content≤10ppm is qualified.
By still temperature rise to 80 DEG C after oxygen content is qualified, and in reactor put into TFE monomer to still pressure 2.5Mpa after, with height
Press pump adds 0.08g initiator peroxysuccinic acid and starts reaction, is continually fed into TFE monomer to maintain pressure in course of reaction
Power is at 2.5Mpa, when TFE addition is 100g, stops adding TFE monomer in reactor, and overbottom pressure is reacted extremely
0.1Mpa, reaction terminates, and by TFE MONOMER RECOVERY in reactor.Stand 5 minutes, open atmospheric valve, lower the temperature and
Material, isolates chlorofluorocarbon oil；Then the material after separating chlorofluorocarbon oil is put into cohesion medial launder, adds deionized water and makes admittedly to contain
Amount is 20wt%；Again cohesion medial launder material is put in knockouts, open stirring, add ammoniacal liquor regulation material PH
Value is 10, condenses 10min, isolate upper strata condensation product at 90r/min speed of agitator and 20 DEG C；By upper strata condensation product
It is dried at 180 DEG C and i.e. can get modified Teflon white resin 110g in 10 hours.Performance is shown in Table 1.
Embodiment 4: in the autoclave that volume is 1L, adds 500g deionized water, and 0.14g acetic acid, 22g is complete
Fluorine ammonium caprylate, 21g chlorofluorocarbon oil, second comonomer perfluoro propyl vinyl ether 0.06g, then closed reactor, to reactor
Carry out vacuumizing, nitrogen replacement operator, and carry out oxygen content test, when in reactor, oxygen content≤10ppm is qualified.Oxygen
By still temperature rise to 110 DEG C after content is qualified, and in reactor put into TFE monomer to still pressure 1.0Mpa after, with height
Press pump adds 0.07g initiator ammonium persulfate and starts reaction, is continually fed into TFE monomer and exists to maintain pressure in course of reaction
1.0Mpa, when TFE addition is 130g, stops adding TFE monomer in reactor, and overbottom pressure is reacted to 0.2Mpa,
Reaction terminates, and by TFE MONOMER RECOVERY in reactor.Stand 5 minutes, open atmospheric valve, cooling discharge, isolate
Chlorofluorocarbon oil；Then the material after separating chlorofluorocarbon oil is put into cohesion medial launder, adds deionized water and makes solid content be 18wt%；
Putting in knockouts by cohesion medial launder material again, open stirring, adding ammoniacal liquor regulation material pH value is 8,
Condense 12min at 85r/min speed of agitator and 15 DEG C, isolate upper strata condensation product；Upper strata condensation product is done at 200 DEG C
Within dry 7 hours, i.e. can get modified Teflon white resin 135g.Performance is shown in Table 1.
Embodiment 5: in the autoclave that volume is 1L, adds 500g deionized water, and 0.18g hydrochloric acid, 18g is complete
Fluorine ammonium caprylate, 20g paraffin, second comonomer perfluoro methyl vinyl ether 0.08g, then closed reactor, enters reactor
Row vacuumizes, nitrogen replacement operator, and carries out oxygen content test, when in reactor, oxygen content≤10ppm is qualified.Oxygen contains
Measure qualified after by still temperature rise to 70 DEG C, and in reactor put into TFE monomer to still pressure 1.5Mpa after, use high-pressure pump
Add 0.05g initiator ammonium persulfate and start reaction, course of reaction is continually fed into TFE monomer and exists to maintain pressure
1.5Mpa, when TFE addition is 120g, stops adding TFE monomer in reactor, and overbottom pressure is reacted to 0.3Mpa,
Reaction terminates, and by TFE MONOMER RECOVERY in reactor.Stand 5 minutes, open atmospheric valve, cooling discharge, isolate
Paraffin；Then the material after separating paraffin is put into cohesion medial launder, adds deionized water and make solid content be 15wt%；Again
Putting in knockouts by cohesion medial launder material, open stirring, adding ammoniacal liquor regulation material pH value is 9, at 90r/min
Condense 9min at speed of agitator and 30 DEG C, isolate upper strata condensation product；Upper strata condensation product is dried at 150 DEG C 9 little
Time can get modified Teflon white resin 130g.Performance is shown in Table 1.
Comparative example: in the autoclave that volume is 1L, adds 500g deionized water, and 0.15g acetic acid, 17g is complete
Fluorine ammonium caprylate, 18g paraffin, then closed reactor, reactor is vacuumized, nitrogen replacement operator, and carry out
Oxygen content is tested, when in reactor, oxygen content≤10ppm is qualified.By still temperature rise to 60 degree after oxygen content is qualified, and to
After input TFE monomer presses 2.0Mpa to still in reactor, add 0.04g initiator peroxysuccinic acid with high-pressure pump and open
Begin reaction, course of reaction is continually fed into TFE monomer to maintain pressure at 2.0Mpa, when TFE addition is 150g
Time, stopping adding TFE monomer in reactor, overbottom pressure is reacted to 0.3Mpa, and reaction terminates, and by TFE in reactor
MONOMER RECOVERY.Stand 5 minutes, open atmospheric valve, cooling discharge, isolate paraffin；Then by the thing after separating paraffin
Material is put into cohesion medial launder, adds deionized water and makes solid content be 15%；Again cohesion medial launder material is put into knockouts
In, open stirring, adding ammoniacal liquor regulation material PH is 9, condenses 10min, separate at 80r/min rotating speed and 30 DEG C
Go out upper strata condensation product；Upper strata condensation product is dried at 170 DEG C and within 10 hours, i.e. can get common polytetrafluoroethylene (PTFE) white resin
138g.Performance is shown in Table 1.
The measurement result of the physical and mechanical properties of the resin that table 1 embodiment and comparative example prepare (measures and presses GB7136-86
Perform)
Claims (10)
1. the preparation method of a modified polytetrafluoroethylresin resin, it is characterised in that comprise the following steps:
(1) by weight, by deionized water 500 parts, tetrafluoroethylene monomer 100～150 parts, activator 0.1～0.18
Part, emulsifying agent 15～22 parts, initiator 0.04～0.08 part, stabilizer 16～21 parts, second comonomer 0.01～0.1 part of throwing
Entering reactor, reaction temperature 60～110 DEG C, pressure is to carry out polymerisation, to reaction under conditions of 1.0～3.0Mpa
When pressure is down to 0.1～0.3Mpa, terminates reaction, cooling discharge, separate stabilizer；
(2), after addition deionized water makes solid content be 10～20wt% in the material after separating stabilizer, ammoniacal liquor is added
Regulation material pH value is 8～10, condenses 8～12min, isolate at 80～90r/min speeds of agitator and 15～35 DEG C
Layer condensation product；
(3) condensation product step (2) obtained is dried at 110～200 DEG C and obtains modified Teflon in 7～12 hours
Resin.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 1, it is characterised in that described activator
For acetic acid or hydrochloric acid.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 1, it is characterised in that described emulsifying agent
For perfluorooctanoic acid or perfluoro octyl sulfonic acid potassium.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 1, it is characterised in that described initiator
For peroxysuccinic acid or ammonium persulfate.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 1, it is characterised in that described stabilizer
For paraffin or chlorofluorocarbon oil.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 1, it is characterised in that described second is single
Body is the one in perfluoro methyl vinyl ether, perfluoroethylvinyl ether, perfluoro propyl vinyl ether.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 6, it is characterised in that described second is single
Body is perfluoro propyl vinyl ether.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 1, it is characterised in that step (1)
Described reaction temperature is 70～100 DEG C, and pressure is 2.0～2.5Mpa.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 1, it is characterised in that step (2)
Described solid content is 12～15wt%.
The preparation method of modified polytetrafluoroethylresin resin the most according to claim 1, it is characterised in that step (3)
The described temperature being dried is 130～180 DEG C, and the time is 8～11 hours.
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| CN111253512A (en) * | 2020-03-05 | 2020-06-09 | 苏州世华新材料科技股份有限公司 | Tetrafluoroethylene-alkyl acrylate-perfluoroalkyl vinyl ether dispersion resin and microporous membrane prepared from same |
| CN112058200A (en) * | 2020-08-27 | 2020-12-11 | 浙江巨圣氟化学有限公司 | Temperature-controlled polymerization kettle and method for modifying PTFE resin by PPVE for heat exchange tube |
| CN113651913A (en) * | 2021-09-10 | 2021-11-16 | 浙江巨化股份有限公司氟聚厂 | Preparation method of high-strength polytetrafluoroethylene resin |
| CN113913062A (en) * | 2021-11-08 | 2022-01-11 | 安徽富瑞雪化工科技股份有限公司 | Polytetrafluoroethylene resin modified acrylic acid aqueous emulsion and preparation method and application thereof |
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| CN113913062A (en) * | 2021-11-08 | 2022-01-11 | 安徽富瑞雪化工科技股份有限公司 | Polytetrafluoroethylene resin modified acrylic acid aqueous emulsion and preparation method and application thereof |
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