CN105013345B - A kind of preparation method of polytetrafluoroethylene (PTFE) super-hydrophobic film - Google Patents
A kind of preparation method of polytetrafluoroethylene (PTFE) super-hydrophobic film Download PDFInfo
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- CN105013345B CN105013345B CN201410162962.7A CN201410162962A CN105013345B CN 105013345 B CN105013345 B CN 105013345B CN 201410162962 A CN201410162962 A CN 201410162962A CN 105013345 B CN105013345 B CN 105013345B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0004—Organic membrane manufacture by agglomeration of particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/04—Hydrophobization
Abstract
Sintered the invention provides a kind of preparation method of poly tetrafluoroethylene, including into fine carrier system fibre, it is characterised in that：Sintering is using temperature programmed control zonal cooling sintering, under flowing atmosphere, and with 3~10 DEG C/min speed from room temperature to 120 DEG C~200 DEG C, 30~120min is incubated at 120 DEG C~200 DEG C；360 DEG C~400 DEG C are warming up to from 120 DEG C~200 DEG C with 2~8 DEG C/min speed, 5~120min is incubated at 360 DEG C~400 DEG C；Cooling treatment is carried out after sintering, it is described to be cooled under flowing atmosphere, 150~200 DEG C are cooled to from 360 DEG C~400 DEG C with 3~15 DEG C/min speed, 30~120min is incubated at 150~200 DEG C, then natural cooling.The present invention has been made with beading superfine fibre poly tetrafluoroethylene, forms the hydrophobic surface with multistage coarse structure together；Surface water contact angle >=150 °, porosity is up to more than 80%；And the givey problem of fiber in polytetrafluoroethylene (PTFE) precursor film sintering is solved, fibre morphology and surface are intact, and intensity and toughness also improve a lot, and can bear certain vacuum pressure.
Description
Technical field
The present invention relates to a kind of preparation method of the separation membrane material for separation field, and in particular to a kind of hydrophobic membrane material
Preparation method.
Technical background
Hydrophobicity is the critical nature of polytetrafluoroethylene (PTFE) (PTFE) material, is that polytetrafluoroethylporous porous membrane is applied to membrane material
The main performance of material.Although polytetrafluoroethylmaterial material has low-surface-energy, the water contact angle of smooth polytetrafluoroethylene (PTFE) plane
Between 98 to 112 °, hydrophobic performance is not good.
Prepared by current polytetrafluoroethylporous porous membrane uses bidirectional extending method more.This method will expect higher porosity
Film when, it is necessary to film carry out vast scale stretching, it is impossible to Surface Structures are controlled, and thickness only more than ten microns with
Under, backing material is needed in use, and backing material often has one in heat resistance or chemical stability or hydrophobic performance in itself
Foregone conclusion limit, thus limit the application of this biaxial stretching film.The shape for being often difficult to control to film is stretched at high proportion simultaneously, therefore
Mainly based on Flat Membrane.Chinese patent CN1775847A, CN102007242A, CN101543734B, CN102151494A etc.
Patent is all based on above stretch processes and carries out polytetrafluoroethylporous porous membrane preparation.
Support methods are the important method for preparing polytetrafluoroethylene fibre, the patent such as CN101994161A and CN102282301A
The preparation of polytetrafluoroethylsuperfine superfine fiber is reported using electrostatic spinning technique.High temperature sintering is directed in these reports
The step of removing into fine carrier, but these sintering processes are concerned only with into the removal of fine template.Specifically：CN101994161A
Purpose be to prepare a kind of polytetrafluoroethylsuperfine superfine fiber, its preparation method is to make carrier using polyvinyl alcohol, passes through Static Spinning
Silk method is weaved out polytetrafluoroethylene fibre precursor, post-processing approach be by polytetrafluoroethylene fibre precursor at 100~120 DEG C
Dry 5~15 minutes, sintered 30~90 minutes at 280~350 DEG C；The purpose of sintering be in order that polyvinyl alcohol decompose and
Remove.And CN102282301A is mainly to provide a kind of improved method of polytetrafluoroethylene (PTFE) pad, its purpose is to improve electricity
The technological parameter (spinning fluid viscosity) of spinning obtains the polytetrafluoroethylene fibre pad precursor of uniform diameter, is sintered at 400 DEG C
Polytetrafluoroethylene fibre pad is obtained, the ash content of carrier (fibre-forming polymer) is less than 5%.CN101994161A and CN102282301A
Etc. patent using electrostatic spinning technique to polytetrafluoroethylsuperfine superfine fiber (pad), only account for how obtaining polytetrafluoroethylene (PTFE) ultra-fine
Fiber (pad), it may be said that have to conventional polytetrafluoroethylsuperfine superfine fiber (pad).
The content of the invention
It is an object of the invention to provide a kind of preparation method of poly tetrafluoroethylene, by controlling containing gathering into fine carrier
The post processing sintering condition of tetrafluoroethene precursor film, by the method for temperature programmed control precision control sintering condition and cooling condition with
Obtain the superfine fibre reticular membrane that fibre morphology remains intact and has beading structure, the special construction of this nanoscale with
Superfine fibre forms the hydrophobic surface with multistage coarse structure together.Thus with ultra-hydrophobicity.
The purpose of the present invention with g technical measures by being realized：
A kind of preparation method of poly tetrafluoroethylene, including sintered into fine carrier system fibre, it is characterised in that：Sintering uses journey
Sequence temperature control zonal cooling is sintered, under flowing atmosphere, with 3~10 DEG C/min speed from room temperature to 120 DEG C~200 DEG C,
30~120min is incubated at 120 DEG C~200 DEG C；With 2~8 DEG C/min speed 360 DEG C~400 are warming up to from 120 DEG C~200 DEG C
DEG C, it is incubated 5~120min at 360 DEG C~400 DEG C；Carry out cooling treatment after sintering, it is described to be cooled under flowing atmosphere, with 3~
15 DEG C/min speed is cooled to 150~200 DEG C from 360 DEG C~400 DEG C, is incubated 30~120min at 150~200 DEG C, then
Natural cooling.By controlling the post processing sintering condition containing the polytetrafluoroethylene (PTFE) precursor film into fine carrier, under stress,
Under carrier protective effect, polytetrafluoroethylgranule granule starts reorientation arrangement, is then decomposed in appropriate opportunity carrier, polytetrafluoroethyl-ne
Alkene particle is further orientated rearrangement, forms catenate superfine fibre network structure.Carried out using described programme-control condition
The super-hydrophobic polytetrafluoroethylfiber fiber film with special construction can be made in preparation.If not in the programme-control condition of the present invention
Under, sintered 30-90 minutes as CN101994161A is set forth at 280-350 DEG C, then can not obtain with multilevel roughness, water
The super-hydrophobic polytetrafluoroethylfiber fiber film that more than 150 ° of contact angle, and film is without flexibility.If not using programme-control (such as in addition
CN102282301A obtains polytetrafluoroethylene fibre pad in sintering at 400 DEG C, and the ash content of carrier (fibre-forming polymer) is less than 5%.)
Original form of fiber can not be then kept, causes fiber to collapse to flat.By controlling the cooling condition after sintering, further
The micro-fractures on fiber are reduced, seamless fiber surface, the intensity and toughness of reinforcing fiber is formed.
The preparation method of above-mentioned poly tetrafluoroethylene, includes preforming step before being sintered after system is fine, it is described it is preforming be by
Polytetrafluoroethylene (PTFE) precursor film is wrapped on branch hold mode, big by winding layer numerical control polytetrafluoroethylene (PTFE) film thickness and average pore size
It is small.The winding of fiber is superimposed with the stress orientation beneficial to sintering process.
Specifically, a kind of preparation method of poly tetrafluoroethylene, comprises the following steps：
(1) preparation of spinning solution；It is the uniform of 0.5%~30% mass concentration that water-soluble polymer, which is dissolved in water to be made into concentration,
Solution, then stirring adds ptfe emulsion, obtains uniform mixed liquor；Exist into fine carrier and polytetrafluoroethylene (PTFE) dry weight ratio
1:1~50；
(2) make fine；Fiber is prepared using the method for spinning or stretching to the spinning solution progress spinning prepared in (1) to be gathered
Tetrafluoroethene precursor film；
(3) it is preforming：It is anticipated that use specification, the winding of polytetrafluoroethylene (PTFE) precursor film will be obtained obtained by (2)
On the branch hold mode of respective shapes, the film of the different shapes such as flat, tubular type, hollow fiber form or rolling and specification is formed, is led to
Cross winding layer numerical control film thick；
(4) sinter；The preforming polytetrafluoroethylene (PTFE) precursor film obtained in (3) is put into high temperature furnace even together with branch hold mode
Continuous be passed through under conditions of flowing atmosphere is sintered；Sintering is using temperature programmed control zonal cooling sintering, with 3~10 DEG C/min speed
Rate is incubated 30~120min from room temperature to 120 DEG C~200 DEG C at 120 DEG C~200 DEG C；With 2~8 DEG C/min speed from
120 DEG C~200 DEG C are warming up to 360 DEG C~400 DEG C, and 5~120min is incubated at 360 DEG C~400 DEG C；
(5) cool down：Under flowing atmosphere, 150~200 are cooled to from 360 DEG C~400 DEG C with 3~15 DEG C/min speed
DEG C, 30~120min is incubated at 150~200 DEG C, then natural cooling.
Above-mentioned flowing atmosphere is that nitrogen, air or inert gas are at least one.
Beneficial effect
1. the poly tetrafluoroethylene of unique structure has been made in the present invention, with being formed by beading filament is crisscross
Hole three-dimensional communication structure, is the hydrophobic surface that one of formation has multistage coarse structure, and beading filament refers to polytetrafluoro
Mutually the filament to be formed is cohered in point and/or face between ethene particle；Hole is in labyrinth hole, and maximum diameter of hole is 1.0 μm, minimum aperture
Footpath is 0.01 μm, and average pore size is 0.1 μm~0.5 μm；Filament is nanofiber, and average diameter is 500 ± 50nm.
2. the present invention is fabulous to solve the givey problem of fiber in polytetrafluoroethylene (PTFE) precursor film sintering, and obtains
Have between beading superfine fibre reticular membrane, fiber and to be changed into inter-adhesive from unordered stacking, fibre morphology and surface are intact,
Intensity and toughness also improve a lot, and can bear certain vacuum pressure (can under 0.7kPa vacuums still stably operable).
3. the polytetrafluoroethylporous porous membrane obtained by the present invention, with special super-hydrophobicity structure, obtained PTFE fiber
Surface forms a large amount of rough surfaces, and surface water contact angle >=150 °, porosity is up to more than 80%.
4th, the polytetrafluoroethylporous porous membrane obtained by the present invention is without support, and thickness is controllable, applied to membrane distillation process, leads to
Amount>20L/m2H, rejection is more than 99%.
5th, the winding process progress of the invention proposed before sintering is preforming, and shape and thickness to final products film can
It is controlled, there is provided the thickness needed for film and intensity while high porosity (more than 80%) is ensured.In contrast to obtain
High porosity and poly tetrafluoroethylene obtained by the stretch processes stretched at high proportion, the inventive method are without support, shape
Formula is various, and thickness is controllable.
6th, the polytetrafluoroethylene (PTFE) super-hydrophobic film preparation method that the present invention is provided, using sintering condition rate-determining steps, makes carrier
Decomposed on appropriate opportunity, and polytetrafluoroethylgranule granule melting orientation is reset, and has obtained having beading superfine fibre reticular membrane, this
The special construction for planting nanoscale forms the hydrophobic surface with multistage coarse structure together with superfine fibre.Thus with super thin
Aqueous energy.
7th, present invention, avoiding the use of lubricant in biaxial tension etc., in the absence of the removing problem of lubricant, technique letter
Single, without extrusion, the Complicated Flow such as press mold pollutes small.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of poly tetrafluoroethylene made from preparation method of the present invention；It can be seen from accompanying drawing
Observe：The poly tetrafluoroethylene of the present invention has by the crisscross hole three-dimensional communication structure formed of beading filament, hole
Gap is in labyrinth hole, and even pore distribution connection, nanofiber form is homogeneous intact.
Embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that be that the present embodiment can only be used
It is further described in the present invention, it is impossible to be interpreted as limiting the scope of the invention, the people that is skilled in technique in the field
Member can make some nonessential modifications and adaptations according to the content of the invention described above.
Embodiment 1
The ptfe emulsion of solid content 60% is added drop-wise in the polyvinyl alcohol water solution that mass fraction is 12% and stirred
Mix uniform, be made into spinning solution.Then polytetrafluoroethylene (PTFE) precursor film is made using electrospinning process.
It is wound on diameter 5cm cylinder branch hold modes, winds 5 layers, and be sent in tube furnace logical nitrogen, sintering process program control
Temperature, from room temperature to 140 DEG C of programming rates, 7 DEG C/min, 140 DEG C of insulation 80min are warming up to 373 DEG C from 140 DEG C, programming rate is 8
DEG C/min, reach after sintering temperature, i.e. 373 DEG C of sintering stage temperature, be incubated 100min.
Cooling：Under the flowing atmosphere of nitrogen, 180 DEG C are cooled to from 373 DEG C with 8 DEG C/min speed, in 180 DEG C of insulations
80min, then natural cooling.
Extract cylinder branch hold mode after being taken out after cooling out, obtain the cylindric poly tetrafluoroethylene that thickness is 180 μm, cutting off can
Obtain flat porous membrane.174 ° of the film hydrophobic contact angle, porosity 89%, 0.5 μm of average pore size, tensile strength
498psi, elongation 375%, when being operated for membrane distillation, flux 28L/m2H, rejection 99.5%.
Embodiment 2
The ptfe emulsion of solid content 60% is added drop-wise in the polyacrylic acid aqueous solution that mass fraction is 9% and stirred
Uniformly, it is made into spinning solution.Then polytetrafluoroethylene (PTFE) precursor film is made using electrospinning process.
It is wound on diameter 5cm cylinder branch hold modes, winds 5 layers, and be sent in tube furnace logical nitrogen, sintering process program control
Temperature, from room temperature to 150 DEG C of programming rates, 6 DEG C/min, is incubated 70min at 150 DEG C, 390 DEG C, programming rate is warming up to from 150 DEG C
For 6 DEG C/min, reach after sintering temperature, i.e. 392 DEG C of sintering stage temperature, be incubated 10min.
Cooling：Under the flowing atmosphere of air, 200 DEG C are cooled to from 390 DEG C with 15 DEG C/min speed, in 200 DEG C of guarantors
Warm 30min, then natural cooling.
Extract cylinder branch hold mode after being taken out after cooling out, obtain the cylindric poly tetrafluoroethylene that thickness is 201um, cutting off can
Obtain flat porous membrane.170 ° of the film hydrophobic contact angle, porosity 85%, 0.45 μm of average pore size, tensile strength
455psi, elongation 308%, when being operated for membrane distillation, flux 25L/m2H, rejection 99.3%.
Embodiment 3
The ptfe emulsion of solid content 60% is added drop-wise in the Na-alginate aqueous solution that mass fraction is 5% and stirred
Uniformly, it is made into spinning solution.Then polytetrafluoroethylene (PTFE) precursor film is made using electrospinning process.
It is wound on diameter 5cm cylinder branch hold modes, winds 5 layers, and be sent in tube furnace logical nitrogen, sintering process program control
Temperature, from room temperature to 180 DEG C of programming rates, 4 DEG C/min, 180 DEG C of insulation 40min are warming up to 376 DEG C from 180 DEG C, programming rate is 3
DEG C/min, reach after sintering temperature, i.e. 376 DEG C of sintering stage temperature, be incubated 80min.
Cooling：Under the flowing atmosphere of air, 190 DEG C are cooled to from 376 DEG C with 5 DEG C/min speed, in 190 DEG C of insulations
40min, then natural cooling.
Extract cylinder branch hold mode after being taken out after cooling out, obtain the cylindric poly tetrafluoroethylene that thickness is 179um, cutting off can
Obtain flat porous membrane.163 ° of the film hydrophobic contact angle, porosity 82%, 0.2 μm of average pore size, tensile strength
465psi, elongation 310%, when being operated for membrane distillation, flux 26L/m2H, rejection 99.5%.
Embodiment 4
The ptfe emulsion of solid content 60% is added drop-wise in the aqueous gelatin solution that mass fraction is 7% and stirs equal
It is even, it is made into spinning solution.Then polytetrafluoroethylene (PTFE) precursor film is made using electrospinning process.
It is wound on diameter 5cm cylinder branch hold modes, winds 6 layers, and be sent to blowing air in tube furnace, sintering process program control
Temperature, from room temperature to 120 DEG C of programming rates, 10 DEG C/min, 120 DEG C of insulation 120min are warming up to 388 DEG C, programming rate from 120 DEG C
For 4 DEG C/min, reach after sintering temperature, i.e. 388 DEG C of sintering stage temperature, be incubated 26min.
Cooling：Under the flowing atmosphere of argon gas, 150 DEG C are cooled to from 388 DEG C with 15 DEG C/min speed, in 150 DEG C of guarantors
Warm 120min, then natural cooling.
Extract cylinder branch hold mode after being taken out after cooling out, obtain the cylindric poly tetrafluoroethylene that thickness is 198um, cut off
It can obtain flat porous membrane.158 ° of the film hydrophobic contact angle, porosity 85%, 0.45 μm of average pore size, tensile strength
460psi, elongation 320%, when being operated for membrane distillation, flux 30L/m2H, rejection 99.2%.
Embodiment 5
The ptfe emulsion of solid content 60% is added drop-wise in the polyvinyl alcohol water solution that mass fraction is 13% and stirred
Mix uniform, be made into spinning solution.Then polytetrafluoroethylene (PTFE) precursor film is made using electrospinning process.
It is wound on diameter 0.5cm cylinder branch hold modes, winds 5 layers, and be sent in Muffle furnace logical nitrogen, sintering process program
Temperature control, from room temperature to 130 DEG C of programming rates, 8 DEG C/min, 130 DEG C of insulation 100min are warming up to 385 DEG C, programming rate from 130 DEG C
For 7 DEG C/min, reach after sintering temperature, i.e. 385 DEG C of sintering stage temperature, be incubated 35min.
Cooling：Under the flowing atmosphere of nitrogen, 160 DEG C are cooled to from 385 DEG C with 12 DEG C/min speed, in 160 DEG C of guarantors
Warm 100min, then natural cooling.
Extract cylinder branch hold mode after being taken out after cooling out, obtain the tubular membrane that thickness is 165um.The film hydrophobic contact angle
172 °, porosity 84%, 0.15 μm of average pore size, tensile strength 480psi, elongation 325%, for tubular membrane membrane distillation behaviour
When making, flux 35L/m2H, rejection 99.6%.
Embodiment 6
The ptfe emulsion of solid content 60% is added drop-wise in the sodium alginate aqueous solution that mass fraction is 8% and stirred
Uniformly, it is made into spinning solution.Then polytetrafluoroethylene (PTFE) precursor film is made using electrospinning process.
It is wound on diameter 0.5cm cylinder branch hold modes, winds 5 layers, and be sent in tube furnace logical argon gas, sintering process program
Temperature control, from room temperature to 160 DEG C of programming rates, 5 DEG C/min, 160 DEG C of insulation 100min are warming up to 380 DEG C, programming rate from 160 DEG C
For 5 DEG C/min, reach after sintering temperature, i.e. 380 DEG C of sintering stage temperature, be incubated 60min.
Cooling:Under the flowing atmosphere of argon gas, 170 DEG C are cooled to from 380 DEG C with 10 DEG C/min speed, in 170 DEG C of guarantors
Warm 90min, then natural cooling.
Extract cylinder branch hold mode after being taken out after cooling out, obtain the tubular membrane that thickness is 188um.The film hydrophobic contact angle
164 °, porosity 84%, 0.35 μm of average pore size, tensile strength 480psi, elongation 320%, for tubular membrane membrane distillation behaviour
When making, flux 37L/m2H, rejection 99.6%.
Embodiment 7
The ptfe emulsion of solid content 60% is added drop-wise in the aqueous gelatin solution that mass fraction is 4% and stirs equal
It is even, it is made into spinning solution.Then polytetrafluoroethylene (PTFE) precursor film is made using electrospinning process.
It is wound on diameter 0.1cm cylinder branch hold modes, winds 6 layers, and be sent to blowing air in tube furnace, sintering process program
Temperature control, from room temperature to 200 DEG C of programming rates, 3 DEG C/min, 200 DEG C of insulation 30min are warming up to 385 DEG C, programming rate from 200 DEG C
For 2 DEG C/min, reach after sintering temperature, i.e., at 370 DEG C of sintering stage temperature, be incubated 120min.
Cooling：Under the flowing atmosphere of nitrogen, 185 DEG C are cooled to from 370 DEG C with 9 DEG C/min speed, in 185 DEG C of insulations
70min, then natural cooling.
Extract cylinder branch hold mode after being taken out after cooling out, obtain the hollow-fibre membrane that thickness is 198um.The film hydrophobic contact angle
174 °, porosity 85%, 0.45 μm of average pore size, tensile strength 450psi, elongation 365% steams for hollow-fibre membrane
When evaporating operation, flux 40L/m2H, rejection 99.9%.
Claims (4)
1. a kind of preparation method of poly tetrafluoroethylene, including sintered into fine carrier system fibre, it is characterised in that：Sintering is used
Temperature programmed control zonal cooling sinter, flowing atmosphere under, with 3~10 DEG C/min speed from room temperature to 120 DEG C~
200 DEG C, 30~120min is incubated at 120 DEG C~200 DEG C；With 2~8 DEG C/min speed 360 are warming up to from 120 DEG C~200 DEG C
DEG C~400 DEG C, it is incubated 5~120min at 360 DEG C~400 DEG C；Cooling treatment is carried out after sintering, it is described to be cooled in flowing atmosphere
Under, be cooled to 150~200 DEG C from 360 DEG C~400 DEG C with 3~15 DEG C/min speed, 150~200 DEG C be incubated 30~
120min, then natural cooling.
2. the preparation method of the poly tetrafluoroethylene as described in claim 1, includes preforming step, institute before being sintered after system is fine
It is that polytetrafluoroethylene (PTFE) precursor film is wrapped on branch hold mode to state preforming.
3. the preparation method of the poly tetrafluoroethylene as described in claim 1, comprises the following steps：
（1）Preparation of spinning solution：Water-soluble polymer is dissolved in water and is made into the homogeneous solution that concentration is 0.5%~30% mass concentration,
Then stirring adds ptfe emulsion, obtains uniform mixed liquor；Into fine carrier and polytetrafluoroethylene (PTFE) dry weight ratio 1:1~
50；
（2）System is fine：Using the method pair of spinning（1）The spinning solution progress spinning of middle preparation prepares fiber and obtains poly- four
PVF precursor film；
（3）It is preforming：It is anticipated that use specification, will（2）In obtained by the polytetrafluoroethylene (PTFE) precursor film that obtains be wrapped in phase
Answer on the branch hold mode of shape, form the film of flat, tubular type, hollow fiber form or rolling, be film-made by winding layer numerical control thick；
（4）Sintering：Will（3）In obtained preforming polytetrafluoroethylene (PTFE) precursor film be put into high temperature furnace and continuously leading to together with branch hold mode
Become a mandarin to take offence and be sintered under conditions of atmosphere；Sintering using temperature programmed control zonal cooling sintering, with 3~10 DEG C/min speed from
Room temperature is incubated 30~120min to 120 DEG C~200 DEG C at 120 DEG C~200 DEG C；With 2~8 DEG C/min speed from 120 DEG C
~200 DEG C are warming up to 360 DEG C~400 DEG C, and 5~120min is incubated at 360 DEG C~400 DEG C；
（5）Cooling：Under flowing atmosphere, 150 are cooled to from 360 DEG C~400 DEG C with 3~15 DEG C/min speed~
200 DEG C, 30~120min is incubated at 150~200 DEG C, then natural cooling.
4. the preparation method of the poly tetrafluoroethylene as described in claim 1,2 or 3, the flowing atmosphere be nitrogen, air or
At least one of inert gas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710777925.0A CN107837692B (en) | 2014-04-22 | 2014-04-22 | Preparation method of polytetrafluoroethylene super-hydrophobic membrane |
| CN201410162962.7A CN105013345B (en) | 2014-04-22 | 2014-04-22 | A kind of preparation method of polytetrafluoroethylene (PTFE) super-hydrophobic film |
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| CN201710777925.0A Active CN107837692B (en) | 2014-04-22 | 2014-04-22 | Preparation method of polytetrafluoroethylene super-hydrophobic membrane |
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| CN105664733B (en) * | 2016-01-21 | 2019-08-02 | 巨化集团技术中心 | A kind of preparation method of perfluor hollow fiber composite membrane |
| CN110303629B (en) * | 2019-07-22 | 2020-07-03 | 燕山大学 | Polytetrafluoroethylene surface multilevel texture and preparation method thereof |
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| TWI317363B (en) * | 2005-05-31 | 2009-11-21 | Univ Chung Yuan Christian | Composite membranes containing polytetrafluoroethylene and method for forming the same |
| CN101530750A (en) * | 2009-04-20 | 2009-09-16 | 浙江理工大学 | Preparation method of polytetrafluoroethylene superfine fiber porous membrane |
| CN101994161A (en) * | 2009-08-25 | 2011-03-30 | 东丽纤维研究所（中国）有限公司 | Method for preparing polytetrafluoroethylene superfine fiber |
| CN102205651B (en) * | 2010-12-24 | 2015-11-25 | 广东新志密封技术有限公司 | A kind of method of sintering polytetrafluoroethylene |
| JP5966282B2 (en) * | 2011-08-31 | 2016-08-10 | ダイキン工業株式会社 | Air filter media and air filter unit |
| CN102908911A (en) * | 2012-10-31 | 2013-02-06 | 辽宁省电力有限公司电力科学研究院 | Processing method of polytetrafluoroethylene microporous filtering material |
| CN103386256B (en) * | 2013-06-21 | 2015-03-25 | 浙江理工大学 | Method for preparing hollow fiber membranes and tubular membranes with microporous PTFE hybrid flat membrane wrapping method |
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2014
- 2014-04-22 CN CN201410162962.7A patent/CN105013345B/en active Active
- 2014-04-22 CN CN201710777925.0A patent/CN107837692B/en active Active
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| CN105013345A (en) | 2015-11-04 |
| CN107837692B (en) | 2020-02-14 |
| CN107837692A (en) | 2018-03-27 |
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