CN102030955A - Method for manufacturing polytetrafluoroethylene microporous membrane - Google Patents
Method for manufacturing polytetrafluoroethylene microporous membrane Download PDFInfo
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- CN102030955A CN102030955A CN 201010558742 CN201010558742A CN102030955A CN 102030955 A CN102030955 A CN 102030955A CN 201010558742 CN201010558742 CN 201010558742 CN 201010558742 A CN201010558742 A CN 201010558742A CN 102030955 A CN102030955 A CN 102030955A
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- microporous teflon
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 36
- 239000012982 microporous membrane Substances 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 21
- -1 polytetrafluoroethylene Polymers 0.000 title claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000000314 lubricant Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000007669 thermal treatment Methods 0.000 claims abstract description 12
- 238000005096 rolling process Methods 0.000 claims abstract description 5
- 238000003490 calendering Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 49
- 239000004809 Teflon Substances 0.000 claims description 31
- 229920006362 Teflon® Polymers 0.000 claims description 31
- 210000004379 membrane Anatomy 0.000 claims description 31
- 239000002994 raw material Substances 0.000 claims description 24
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 18
- 239000003350 kerosene Substances 0.000 claims description 14
- 238000000465 moulding Methods 0.000 claims description 8
- 238000009998 heat setting Methods 0.000 claims description 7
- 230000007246 mechanism Effects 0.000 claims description 4
- 230000002457 bidirectional effect Effects 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000013461 design Methods 0.000 claims description 2
- 230000036316 preload Effects 0.000 claims description 2
- 238000004513 sizing Methods 0.000 abstract 2
- 239000000843 powder Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 15
- 238000012545 processing Methods 0.000 description 9
- 230000009286 beneficial effect Effects 0.000 description 7
- 239000007787 solid Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 238000009434 installation Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000000428 dust Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
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Abstract
The invention aims to provide a method for manufacturing a polytetrafluoroethylene microporous membrane with high porosity, fine bore diameter, high uniformity and low production cost, which comprises the following steps of: mixing polytetrafluoroethylene micro powder and a lubricating agent, stirring, standing, prepressing forming, pushing forming, calendaring forming, drying, performing longitudinal thermal stretching, performing lateral thermal stretching, performing thermal treatment, sizing and rolling, wherein the using temperatures of drying, longitudinal thermal stretching, lateral thermal stretching, thermal treatment and sizing in the manufacturing process are improved sequentially.
Description
Technical field
The present invention relates to a kind of manufacture method of tetrafluoroethylene, especially a kind of manufacture method of microporous teflon membran.
Background technology
Polytetrafluoroethylene (PTFE) is a kind of macromolecular thermoplastic material, has corrosion-resistant, resistant of high or low temperature, low, the uninflammability advantages such as (LOI are 95%) of frictional coefficient, in field of aerospace, industry, medical treatment with in life important use arranged.Especially along with the fast development of modern industrialization process, oneself becomes a serious day by day global problem topsoil, and the improvement of pollutent has become key subjects, and is higher for the performance requriements of filtering material.Has significant advantage because polytetrafluoroethylene fiber has excellent chemical stability, erosion resistance, thermotolerance, high lubricated not viscosity, weathering resistance are compared with the existing fiber that is used for filtering material, can be widely used in filtration, the purifying treatment of various flue gases, dust, liquid, therefore extensive day by day in the application in dust removal and filtration field.
Though tetrafluoroethylene is a thermoplastic macromolecule material, different with general thermal plasticity high polymer, only can produce transparent glutinous consolidation glue during fusion, and can melt-flow, also be not dissolved in any flux.Therefore because factors such as the inertness of tetrafluoroethylene, infusibility, thermostability are brought very big difficulty to its processing.The polytetrafluoroethylene film that existing complete processing makes, for example the patent No. is called the microporous teflon membran that disclosed working method makes in the microporous teflon membran process patent file for the zl02108850.0 name, have following shortcoming: the thickness of (1) film does not accomplish that Air permenbility is little below 2 microns; (2) the film Air permenbility that causes in uneven thickness of film is inhomogeneous.
Summary of the invention
The purpose of this invention is to provide that a kind of porosity height, aperture are tiny, the manufacture method of good uniformity, microporous teflon membran that production cost is low.
Realize the manufacture method of the microporous teflon membran of the object of the invention, comprise the steps:
(1) the ptfe micropowder material is mixed equably with lubricant;
(2) mixed raw material is inserted at the uniform velocity slowly stirring in the stirring mechanism, be beneficial to the raw material thorough mixing;
(3) compound that stirs was left standstill 48～60 hours;
(4) mixed raw materials is carried out pre-molding;
(5) the mould material with pre-molding pushes, and is pressed into the cylindrical die material;
(6) the cylindrical die material after will pushing is made the tetrafluoroethylene base band through calendering, is beneficial to later process processing;
(7) the polytetrafluoroethylene (PTFE) base band after will rolling carries out drying, removes lubricant wherein, so that the stretching of later process;
(8) dried tetrafluoroethylene base band is introduced drawing mechanism and carry out two-way thermal stretch, the earlier vertical thermal stretch of the employing bidirectional extending method of horizontal thermal stretch again makes microporous teflon membran;
(9) will heat-treat and finalize the design through the microporous teflon membran of two-way thermal stretch, to guarantee its functional, stable molding.
Dry in the manufacturing processed, vertical thermal stretch, horizontal hot-drawn reach thermal treatment, the typing use temperature improves successively.
The lubricant of described step (1) is an aviation kerosene, and described ptfe micropowder is 39: 11～21: 4 with the mixed weight ratio of aviation kerosene.
The stirring velocity of described step (2) is 2r/min～5r/min, and whipping temp is 20 ℃～30 ℃, and churning time is greater than 90min; Leaving standstill of the mixing raw material of described step (3) is to carry out under 40 ℃～60 ℃ temperature.
The pre-molding of described step (4) carries out on preformer, and preload pressure is 0.5MPa～0.8MPa, and the precompressed temperature is 20 ℃～30 ℃.
The pushing of described step (5) is to adopt the pushing machine to be pressed into the cylindrical die material, and pushing pressure is 3.5MPa～4.2MPa, and the pushing temperature is 160 ℃～180 ℃.
The rolling temperature of described step (6) is 45 ℃～55 ℃, and linear velocity is 0.5m/min～0.8m/min.
The drying temperature of described step (7) is controlled at 300 ± 10 ℃.The exsiccant purpose is to remove lubricating auxiliary agent in the pre-shaped articles, for follow-up two-way stretch is laid a solid foundation.
Vertical thermal stretch temperature of described step (8) is 310 ℃～330 ℃; Laterally the thermal stretch temperature is 330 ℃～350 ℃; The raising of thermal stretch temperature helps the increase in microporous membrane aperture; But temperature is too high unfavorable to the moulding of microporous membrane on the contrary, and the temperature of rationally grasping thermal stretch could effectively be controlled the over-all properties of microporous membrane.
The thermal stretch of described step (8) keeps the temperature-stable and the uniform tension in order of drawing zone, and stretch ratio was controlled at 1: 2～1: 10, and draw speed is 3m/min～10m/min.Good to guarantee that microporous membrane is shaped, porosity is even, the aperture is stable, powerful good evenness.
The thermal treatment temp of described step (9) is controlled at 375 ℃～410 ℃, and microporous membrane travelling speed in heat-treating machine is 0.5m/min～1.5m/min; When heat setting type, adopt constant tension force, to guarantee the stable of microporous membrane form, make the regulation package through wrap-up more at last.
The advantage of the manufacture method of stretching method microporous teflon membran of the present invention is as follows:
(1) ptfe micropowder material adds a kind of lubricant, through stirring, leave standstill the thorough mixing that helps raw material.
(2) mixed raw material makes the tetrafluoroethylene product more even through the extruding of 3 differing tempss.
(3) from base film drying, vertically thermal stretch, laterally hot-drawn reaches thermal treatment, gradient temperature is used in typing, performances such as the aperture of microporous membrane, porosity are significantly improved;
(4) processing units is simple, easy to operate, yield rate is high, production cost is low.
(5) microporous teflon membran that makes of method of the present invention is under identical air penetrability, and the thickness of film significantly increases, and makes microporous teflon membran of the present invention have very high wear resisting property, prolongs one times work-ing life.
Description of drawings
Fig. 1 is the process flow sheet of the manufacture method of microporous teflon membran of the present invention.
Embodiment
The manufacture method of microporous teflon membran of the present invention is as follows:
Ptfe micropowder material and aviation kerosene were mixed by weight 39: 11～21: 4, and the ratio of preferably using with is 81: 19; Raw materials mixed is stirred, and stirring velocity is 2～5r/min, and whipping temp is 20～30 ℃, and churning time is 90min, makes raw material obtain thorough mixing.
The mixing raw material that stirs is placed under 40～60 ℃ the temperature, left standstill 48～60 hours, be beneficial to the ptfe micropowder material lubricant is absorbed comprehensively, make the two obtain thorough mixing, make the required prefabricated material of processing.
Prefabricated material inserted carry out precompressed in the preformer, required pressure is 0.5～0.8MPa, and press temperature is 20～30 ℃, makes cylindrical mould material; The cylindrical die goods are inserted the compacting of pushing machine, press temperature is 160～180 ℃ again, and required pressure is 3.5～4.2MPa, makes the cylindrical die material again.
The cylindrical die material is made the tetrafluoroethylene base band 45～55 ℃ temperatures, and linear velocity is 0.5～0.8m/min.
The tetrafluoroethylene base band that extrudes is introduced drying installation, and drying temperature is controlled at 300 ± 10 ℃, and the exsiccant purpose is the lubricant aviation kerosene of removing in the base band, for follow-up two-way stretch is laid a solid foundation.
Enter the thermal stretch district through dried polytetrafluoroethylene (PTFE) base band, vertically the thermal stretch temperature is controlled at 310～330 ℃; Laterally the thermal stretch temperature is controlled at 330～350 ℃.Require to keep the temperature-stable and the uniform tension in order of drawing zone during the thermal stretch of microporous membrane process, good to guarantee that microporous membrane is shaped, porosity is even, the aperture is stable, powerful good evenness.
Enter the heat-treatment zone through the microporous teflon membran after the thermal stretch, the thermal treatment setting temperature is controlled at 375～410 ℃, and microporous membrane travelling speed in heat-treating machine is 0.5～1.5m/min; Simultaneously,, adopt constant tension force,, make the regulation package through wrap-up more at last to guarantee the stable of microporous membrane form at heat-setting process.
Ptfe micropowder material and aviation kerosene were mixed by weight 39: 11～21: 4, and the ratio of preferably using with is 81: 19; Raw materials mixed is stirred, and stirring velocity is 2～5r/min, and whipping temp is 20～30 ℃, and churning time is 90min, makes raw material obtain thorough mixing.
The mixing raw material that stirs is placed under 40～60 ℃ the temperature, left standstill 48～60 hours, be beneficial to the ptfe micropowder material lubricant is absorbed comprehensively, make the two obtain thorough mixing, make the required prefabricated material of processing.
Prefabricated material inserted carry out precompressed in the preformer, required pressure is 0.5～0.8MPa, and press temperature is 20～30 ℃, makes cylindrical mould material; The cylindrical die goods are inserted the compacting of pushing machine, press temperature is 160～180 ℃ again, and required pressure is 3.5～4.2MPa, makes the cylindrical die material again.
The cylindrical die material is made the tetrafluoroethylene base band 45～55 ℃ temperatures, and linear velocity is 0.5～0.8m/min.
The tetrafluoroethylene base band that extrudes is introduced drying installation, and drying temperature is controlled at 300 ± 10 ℃, and the exsiccant purpose is the lubricant aviation kerosene of removing in the base band, for follow-up two-way stretch is laid a solid foundation.
Enter the thermal stretch district through dried polytetrafluoroethylene (PTFE) base band, vertically the thermal stretch temperature is controlled at 310～330 ℃; Laterally the thermal stretch temperature is controlled at 330～350 ℃.Require to keep the temperature-stable and the uniform tension in order of drawing zone during the thermal stretch of microporous membrane process, good to guarantee that microporous membrane is shaped, porosity is even, the aperture is stable, powerful good evenness.
Enter the heat-treatment zone through the microporous teflon membran after the thermal stretch, the thermal treatment setting temperature is controlled at 375～410 ℃, and microporous membrane travelling speed in heat-treating machine is 0.5～1.5m/min; Simultaneously,, adopt constant tension force,, make the regulation package through wrap-up more at last to guarantee the stable of microporous membrane form at heat-setting process.
Embodiment one
With ptfe micropowder material and aviation kerosene is to mix at 81: 19 by weight; Raw materials mixed is stirred, and stirring velocity is 2r/min, and whipping temp is 20 ℃, and churning time is 90min, makes raw material obtain thorough mixing.
The mixing raw material that stirs is placed under 40 ℃ the temperature, left standstill 48 hours, be beneficial to the ptfe micropowder material lubricant is absorbed comprehensively, make the two obtain thorough mixing, make the required prefabricated material of processing.
Prefabricated material inserted carry out precompressed in the preformer, required pressure is 0.5MPa, and press temperature is 20 ℃, makes cylindrical mould material; The cylindrical die goods are inserted the compacting of pushing machine, press temperature is 160 ℃ again, and required pressure is 3.5MPa, makes the cylindrical die material again.
The cylindrical die material is made the tetrafluoroethylene base band 45 ℃ temperatures, and linear velocity is 0.5m/min.
The tetrafluoroethylene base band that extrudes is introduced drying installation, and drying temperature is controlled at 300 ± 10 ℃, and the exsiccant purpose is the lubricant aviation kerosene of removing in the base band, for follow-up two-way stretch is laid a solid foundation.
Enter the thermal stretch district through dried polytetrafluoroethylene (PTFE) base band, vertically the thermal stretch temperature is controlled at 310 ℃; Laterally the thermal stretch temperature is controlled at 330 ℃.Require to keep the temperature-stable and the uniform tension in order of drawing zone during the thermal stretch of microporous membrane process, good to guarantee that microporous membrane is shaped, porosity is even, the aperture is stable, powerful good evenness.
Enter the heat-treatment zone through the microporous teflon membran after the thermal stretch, the thermal treatment setting temperature is controlled at 375 ℃, and microporous membrane travelling speed in heat-treating machine is 0.5m/min; Simultaneously,, adopt constant tension force,, make the regulation package through wrap-up more at last to guarantee the stable of microporous membrane form at heat-setting process.
Embodiment two
Ptfe micropowder material and aviation kerosene were mixed by weight 39: 11; Raw materials mixed is stirred, and stirring velocity is 4r/min, and whipping temp is 25 ℃, and churning time is 100min, makes raw material obtain thorough mixing.
The mixing raw material that stirs is placed under 50 ℃ the temperature, left standstill 55 hours, be beneficial to the ptfe micropowder material lubricant is absorbed comprehensively, make the two obtain thorough mixing, make the required prefabricated material of processing.
Prefabricated material inserted carry out precompressed in the preformer, required pressure is 0.7MPa, and press temperature is 25 ℃, makes cylindrical mould material; The cylindrical die goods are inserted the compacting of pushing machine, press temperature is 170 ℃ again, and required pressure is 3.8MPa, makes the cylindrical die material again.
The cylindrical die material is made the tetrafluoroethylene base band 50 ℃ temperatures, and linear velocity is 0.7m/min.
The tetrafluoroethylene base band that extrudes is introduced drying installation, and drying temperature is controlled at 300 ± 10 ℃, and the exsiccant purpose is the lubricant aviation kerosene of removing in the base band, for follow-up two-way stretch is laid a solid foundation.
Enter the thermal stretch district through dried polytetrafluoroethylene (PTFE) base band, vertically the thermal stretch temperature is controlled at 320 ℃; Laterally the thermal stretch temperature is controlled at 340 ℃.Require to keep the temperature-stable and the uniform tension in order of drawing zone during the thermal stretch of microporous membrane process, good to guarantee that microporous membrane is shaped, porosity is even, the aperture is stable, powerful good evenness.
Enter the heat-treatment zone through the microporous teflon membran after the thermal stretch, the thermal treatment setting temperature is controlled at 400 ℃, and microporous membrane travelling speed in heat-treating machine is 1m/min; Simultaneously,, adopt constant tension force,, make the regulation package through wrap-up more at last to guarantee the stable of microporous membrane form at heat-setting process.
Embodiment three
Ptfe micropowder material and aviation kerosene were mixed by weight 21: 4; Raw materials mixed is stirred, and stirring velocity is 5r/min, and whipping temp is 30 ℃, and churning time is 120min, makes raw material obtain thorough mixing.
The mixing raw material that stirs is placed under 60 ℃ the temperature, left standstill 60 hours, be beneficial to the ptfe micropowder material lubricant is absorbed comprehensively, make the two obtain thorough mixing, make the required prefabricated material of processing.
Prefabricated material inserted carry out precompressed in the preformer, required pressure is 0.8MPa, and press temperature is 30 ℃, makes cylindrical mould material; The cylindrical die goods are inserted the compacting of pushing machine, press temperature is 180 ℃ again, and required pressure is 4.2MPa, makes the cylindrical die material again.
The cylindrical die material is made the tetrafluoroethylene base band 55 ℃ temperatures, and linear velocity is 0.8m/min.
The tetrafluoroethylene base band that extrudes is introduced drying installation, and drying temperature is controlled at 300 ± 10 ℃, and the exsiccant purpose is the lubricant aviation kerosene of removing in the base band, for follow-up two-way stretch is laid a solid foundation.
Enter the thermal stretch district through dried polytetrafluoroethylene (PTFE) base band, vertically the thermal stretch temperature is controlled at 330 ℃; Laterally the thermal stretch temperature is controlled at 350 ℃.Require to keep the temperature-stable and the uniform tension in order of drawing zone during the thermal stretch of microporous membrane process, good to guarantee that microporous membrane is shaped, porosity is even, the aperture is stable, powerful good evenness.
Enter the heat-treatment zone through the microporous teflon membran after the thermal stretch, the thermal treatment setting temperature is controlled at 410 ℃, and microporous membrane travelling speed in heat-treating machine is 1.5m/min; Simultaneously,, adopt constant tension force,, make the regulation package through wrap-up more at last to guarantee the stable of microporous membrane form at heat-setting process.
Two-way hot-drawing method microporous teflon membran of the present invention, degree of crystallinity are up to more than 99%, and internal crystallization is banded polycrystalline aggregate, can guarantee uniformity coefficient, the micropore film strength of hole.
Claims (10)
1. the manufacture method of a microporous teflon membran comprises the steps:
(1) the ptfe micropowder material is mixed equably with lubricant;
(2) mixed raw material is inserted at the uniform velocity slowly stirring in the stirring mechanism;
(3) compound that stirs was left standstill 48～60 hours;
(4) mixed raw materials is carried out pre-molding;
(5) the mould material with pre-molding pushes, and is pressed into the cylindrical die material;
(6) the cylindrical die material after will pushing is made the tetrafluoroethylene base band through calendering;
(7) the polytetrafluoroethylene (PTFE) base band after will rolling carries out drying, removes lubricant wherein;
(8) dried tetrafluoroethylene base band is introduced drawing mechanism and carry out two-way thermal stretch, the earlier vertical thermal stretch of the employing bidirectional extending method of horizontal thermal stretch again makes microporous teflon membran;
(9) will heat-treat and finalize the design through the microporous teflon membran of two-way thermal stretch,
Dry in the manufacturing processed, vertical thermal stretch, horizontal hot-drawn reach thermal treatment, the typing use temperature improves successively.
2. the manufacture method of microporous teflon membran according to claim 1, it is characterized in that: the lubricant of described step (1) is an aviation kerosene, described ptfe micropowder is 39: 11～21: 4 with the mixed weight ratio of aviation kerosene.
3. the manufacture method of microporous teflon membran according to claim 1, it is characterized in that: the stirring velocity of described step (2) is 2r/min～5r/min, and whipping temp is 20 ℃～30 ℃, and churning time is greater than 90min; Leaving standstill of the mixing raw material of described step (3) is to carry out under 40 ℃～60 ℃ temperature.
4. the manufacture method of microporous teflon membran according to claim 1, it is characterized in that: the pre-molding of described step (4) carries out on preformer, and preload pressure is 0.5MPa～0.8MPa, and the precompressed temperature is 20 ℃～30 ℃.
5. the manufacture method of microporous teflon membran according to claim 1 is characterized in that: the pushing of described step (5) is to adopt the pushing machine to be pressed into the cylindrical die material, and pushing pressure is 3.5MPa～4.2MPa, and pushing temperature is 160 ℃～180 ℃.
6. the manufacture method of microporous teflon membran according to claim 1, it is characterized in that: the rolling temperature of described step (6) is 45 ℃～55 ℃, and linear velocity is 0.5m/min～0.8m/min.
7. the manufacture method of microporous teflon membran according to claim 1, it is characterized in that: the drying temperature of described step (7) is controlled at 300 ± 10 ℃.
8. the manufacture method of microporous teflon membran according to claim 1, it is characterized in that: vertical thermal stretch temperature of described step (8) is 310 ℃～330 ℃; Laterally the thermal stretch temperature is 330 ℃～350 ℃.
9. the manufacture method of microporous teflon membran according to claim 1, it is characterized in that: the thermal stretch of described step (8) keeps the temperature-stable and the uniform tension in order of drawing zone, stretch ratio was controlled at 1: 2～1: 10, and draw speed is 3m/min～10m/min.
10. the manufacture method of microporous teflon membran according to claim 1, it is characterized in that: the thermal treatment temp of described step (9) is controlled at 375 ℃～410 ℃, and microporous membrane travelling speed in heat-treating machine is 0.5m/min～1.5m/min; When heat setting type, adopt constant tension force.
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| CN103302862A (en) * | 2013-05-06 | 2013-09-18 | 天津市天塑科技集团有限公司技术中心 | Preparation method of polytetrafluoroethylene biaxial stretching hydrophilic microporous filter belt |
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