CN106669453A - Superfine polytetrafluoroethylene fiber pipe type membrane - Google Patents
Superfine polytetrafluoroethylene fiber pipe type membrane Download PDFInfo
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- CN106669453A CN106669453A CN201510766523.1A CN201510766523A CN106669453A CN 106669453 A CN106669453 A CN 106669453A CN 201510766523 A CN201510766523 A CN 201510766523A CN 106669453 A CN106669453 A CN 106669453A
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- vestibule
- porous material
- tubular membrane
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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
- B01D69/04—Tubular membranes
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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
Abstract
The invention provides a superfine polytetrafluoroethylene fiber pipe type membrane which comprises a polytetrafluoroethylene material body, wherein polytetrafluoroethylene takes the shape of fiber; the diameter of the fiber is 30-200 nm; the polytetrafluoroethylene material body is provided with pore cavities of which the apertures are 10-1000 nm and cavity walls formed by three-dimensional spaces surrounding the pore cavities; the pore cavities are uniformly distributed; the pore cavities are communicated in a three-dimensional manner; the pore cavities are in uniform distribution means that the pore cavities are in uniform distribution in a porous material by any unit-grade volume; the porosity is greater than or equal to 75%; the tensile strength is 15 N/mm<2> or higher; and the water-pressure resistance is 3 kg/cm<2> or higher. A specific and definite measurement mode is provided for on pore cavity distribution uniformity of the polytetrafluoroethylene fiber pipe type membrane, the pore distribution uniformity of the porous material and a multi-stage porous material of the porous material is measured by small-unit grade volume, the porous structure is high in uniformity, and thus uniformity consistency of different properties of the porous material can be ensured.
Description
Technical field
The present invention relates to a kind of porous material, specifically a kind of polytetrafluoroethylene fibre tubular membrane.
Background technology
Solid containing certain amount hole, porous material, is a kind of material that network structure is made up of insertion or blind bore hole.For continuous media material, porous material typically has the advantages that relative density is low, specific strength is high, specific surface area is high, lightweight, sound insulation, heat-insulated, good penetrability.According to the difference of pore size, porous material can be divided into micropore again（Aperture is less than 2 nm）It is material, mesoporous（Aperture 2-50 nm）Material and macropore（Aperture is more than 50 nm）Material.
Porous material is distinguished by its material, can be divided into metal polyporous material and non-metal porous material.Non-metal porous material typically has the features such as specific surface area is big, density is little, thermal conductivity is little, relative density is little, porosity is big, in catalyst（Including carrier）, adsorbent, insulation, thermal insulation, sewage and exhaust-gas treatment, filter liquid and gas（Or even bacterium）, light building material, the field such as environmental protection, improved soil, chemical industry is with a wide range of applications.Wherein, polytetrafluoroethylporous porous membrane material is with the performance such as its temperature stability, chemical stability, electric insulation, fire-retardant, self-lubricating, and its range of application is extremely wide.However, the randomness, scrambling due to pore structure, it still can not meet many application performances.
In many applications, it is required for its porous material itself uniform, its pore size, hole are evenly distributed so that performance uniformity, but in fact, many porous materials do not reach this requirement, its uniformity supplies；Despite material call oneself and reached higher uniformity, but its uniformity is still the uniformity under large volume yardstick, if being weighed with small size yardstick, such as take up an official post in material and take the said three-dimensional body that polylith volume is not more than a cubic centimetre, its quality is surveyed respectively, its uniformity coefficient difference is still very big, thus result in polytetrafluoroethylporous porous membrane material various performances such as intensity, elastic modelling quantity, flux etc. it is uneven, have a strong impact on its function.
The content of the invention
It is an object of the invention to provide architecture, controllable, high uniformity polytetrafluoroethylene fibre tubular membrane.
The purpose of the present invention is realized by following measures：
A kind of polytetrafluoroethylsuperfine superfine fiber tubular membrane, including polytetrafluoroethylmaterial material body, polytetrafluoroethylene (PTFE) is in threadiness, fibre diameter is 30～200nm, the cavity wall that body has the vestibule in 10nm～1000nm apertures and formed around vestibule in three dimensions, its vestibule is in uniform distribution, the three-dimensional insertion of each vestibule, and vestibule refers to each vestibule on the porous material under arbitrary unit level volume in uniform distribution in uniform distribution；Porosity of=75%, tensile strength 15N/mm2More than, water pressure resistance 3kg/cm2More than.
Specifically, above-mentioned polytetrafluoroethylene fibre tubular membrane, vestibule with 30～1000nm apertures and the cavity wall formed around vestibule in three dimensions, arrange subordinate's vestibule of 10～100nm, vestibules at different levels each three-dimensional insertion and vestibule at different levels also insertion each other each other in cavity wall；Vestibule is in uniform distribution, and vestibule refers to each vestibule on the porous material under arbitrary unit level volume in uniform distribution in uniform distribution.
Specifically, above-mentioned unit level volume refers to cubic centimetre level or cubic millimeter level or more subsection level volume.
More specifically, above-mentioned vestibule is referred in uniform distribution be not more than each said three-dimensional body of a cubic centimetre and formed objects in the take up an official post volume that takes of the porous material, their quality is substantially suitable.
More specifically, above-mentioned quality quite refers to the said three-dimensional body for appointing the multiple volumes for taking to be not more than a cubic centimetre and formed objects on the porous material substantially, claim its quality respectively, the mean value of their quality is obtained, and arbitrary three-dimensional weight is not more than the 4% of said three-dimensional body mass average value relative to the absolute value of the bias of mass average value.
Further, the multistage material take up an official post the volume that takes be not more than one cubic millimeter formed objects said three-dimensional body, their quality are substantially suitable.
More specifically, the quality quite refers to the said three-dimensional body of the formed objects for appointing the multiple volumes for taking to be not more than a cubic millimeter on the porous material substantially, claim its quality respectively, the mean value of their quality is obtained, and arbitrary three-dimensional weight is not more than the 4% of said three-dimensional body mass average value relative to the absolute value of the bias of mass average value.
Preferably, above-mentioned polytetrafluoroethylene fibre tubular membrane is made up of multistage porous material, body is the vestibule being classified with material pore size, and the cavity wall in three dimensions around vestibule is constituted, subordinate's vestibule, vestibules at different levels each three-dimensional insertion and vestibule at different levels also insertion each other each other are set in cavity wall.More specifically, next stage porous material constitutes the cavity wall of upper level vestibule.The cavity wall of higher level's vestibule is constituted by the multistage porous material of its subordinate is compound, or is constituted by the porous materials at different levels of its subordinate are compound, and material can be caused to meet specific functional requirement.
Specifically, every grade of porous material of material body is a continuous structure body certainly.Maximum external boundary per one-level porous material is suitable with whole material body space boundary.I.e. every grade porous material can be present in body as the porous material of one-level independence, and with its physical and chemical performance alone.Such structure can cause the physical and chemical performance of porous materials at different levels difference, have different physical and chemical performances in the whole space of relatively-stationary material, better meet many functional requirements.
Beneficial effect
1., the invention provides a kind of polytetrafluoroethylene fibre tubular membrane with loose structure, specify that its version, the hierarchy form of its vestibule and its uniformity structure can meet several functions demand.
2. the present invention is evenly distributed to the vestibule of polytetrafluoroethylene fibre tubular membrane and proposes concrete and clear and definite metric form, specify that it is to get off to measure porous material and the pore size distribution uniformity of its multilevel hierarchy with the yardstick of subsection level volume, such loose structure is high uniformity, so as to ensure that the uniformity consistency of each performance of porous material.
3. polytetrafluoroethylene fibre tubular membrane of the present invention is three-dimensional insertion, including every grade of hole three-dimensional communication, and hole at different levels mutually three-dimensional insertion, and connectivity is good, can fully meet the functional requirement of material.
4. the polytetrafluoroethylene fibre tubular membrane of the present invention is the hydrophobic surface with multistage coarse structure.Surface water contact angle can reach more than 160 °.
5. polytetrafluoroethylstephanoporate stephanoporate tunica fibrosa, the such as film properties such as pore size distribution, hierarchy, porosity, hole shape architectural characteristic, technique etc. and mechanical strength, water pressure resistance are relevant, the polytetrafluoroethylene fibre tubular membrane of invention is without the need for supporting, form stable, thickness is controllable, it is applied to Membrane Materials process, flux>42L/m2H, more than 99.8%, tensile strength can reach 30N/mm to rejection2More than, water pressure resistance 5kg/cm2More than.
Specific embodiment
Specific embodiment gives detailed embodiment premised on technical solution of the present invention, but protection scope of the present invention is not limited only to following embodiments.Without departing from change above-mentioned technological thought of the invention in the case of, according to the ordinary technical knowledge and/or customary means of this area, it is clear that the replacement or change of various ways can also be made, and all should be included within the scope of the present invention.
Embodiment
1
The polytetrafluoroethylene fibre tubular membrane of the present invention, with second hole structure, wherein, there is the second level vestibule for being uniformly distributed, being mutually communicated in the cavity wall of the first order vestibule be uniformly distributed, being mutually communicated, and the also insertion each other each other of two-stage hole, the insertion is three-dimensional insertion.Every grade of porous material of material body is a continuous structure body certainly.Total effective drainage porosity is 75%, and fibre diameter is 150 ± 20 nm, and macropore average pore size is 0.45 μm, there is the insertion aperture of average pore size 30nm in the cavity wall of macropore.
It is machined into method to take up an official post in the porous material said three-dimensional body of the same size for taking 9 10mm × 10mm × 10mm, its quality is tested with plum Teller-support benefit XP26 Microbalance balances, as a result it is as shown in table 1, wherein, it is expressed as a percentage relative to the absolute value of the bias of mean value, its value be relative to mean value absolute value of the bias divided by mass average value, as shown in Table 1, its mass deviation is not more than 4%.
Table 1
| Piece number | Quality（mg） | Relative to the absolute value of the bias of mean value（%） |
| 1 | 655.308 | 0.9% |
| 2 | 649.324 | 1.8% |
| 3 | 657.930 | 0.5% |
| 4 | 673.733 | 1.9% |
| 5 | 657.430 | 0.6% |
| 6 | 666.089 | 0.8% |
| 7 | 662.578 | 0.2% |
| 8 | 667.628 | 1.0% |
| 9 | 660.041 | 0.2% |
| Mass average value | 661.118 |
The preparation method of the porous polytetrafluoroethylene material is：
（1）By the ptfe emulsion of solid content 60%, particle diameter 30nm shitosans, 5%（Mass ratio）Polyacrylic acid solution, 20wt% starch emulsions, uniform mixing, according to 50：25：4：4 mass ratio, is made into spinning solution；
（2）Under vacuum, polytetrafluoroethylene (PTFE) precursor film is produced using electrospinning process in orientation electrostatic spinning fiber silk device；
（3）Precursor film is wound into 5 layers to diameter 4-25mm cylinders hold mode, is sent into tube furnace and is sintered in vacuum or protective atmosphere, sintered and sintered using temperature programmed control zonal cooling, with the speed of 5 DEG C/min from room temperature to 160 DEG C, at 160 DEG C 80min is incubated；With the ramp of 5 DEG C/min to 280 DEG C, at 280 DEG C 60min is incubated；With the ramp of 2 DEG C/min to 360 DEG C, at 360 DEG C 20min is incubated；With the ramp of 6 DEG C/min to 400 DEG C, at 400 DEG C 60min is incubated.
（4）Temperature programmed control cooling after sintering, according to routine techniques subsequent treatment, obtains the porous Teflon Fiber tube type film with two-stage pore structure, and thickness is 156 μm, tubular membrane diameter 4-25mm.
, without the need for supporting, form stable, thickness is controllable, can be used for gas-liquid separation and Liquid liquid Separation for the polytetrafluoroethylene fibre tubular membrane, realizes that Accurate Classification is filtered, such as it is applied to two-spot or many vigour（Liquid）The filtration of body, its flux is big, and rejection is high, is difficult to be contaminated（Such as the infiltration fouling membrane of multi-component liquid）, the advantage with efficient long-acting.168 ° of film water contact angle；Tensile strength 30N/mm2, water pressure resistance 5kg/cm2。
Such as, in being applied to the Membrane Materials of acid/alcohol-water-non-volatile solute system, total flux can reach 42kg/m2More than h, in system non-volatile solute rejection more than 99.8%, volatilization alcohol/acid separation factor=[alcohol/acid mass fraction in distillate ×（1- material liquids alcohol/acid mass fraction）] ÷ [material liquid alcohol/acid mass fraction ×（1- distillates alcohol/acid mass fraction）] can reach more than 10.
Embodiment
2
The polytetrafluoroethylene fibre tubular membrane of the present invention, with three-level pore structure, wherein, there is the second level vestibule for being uniformly distributed, being mutually communicated in the cavity wall of the first order vestibule be uniformly distributed, being mutually communicated, and the also insertion each other each other of two-stage hole, the insertion is three-dimensional insertion.Every grade of porous material of material body is a continuous structure body certainly.Total effective drainage porosity is 85%, and fibre diameter is 180 ± 20 nm, and macropore average pore size is 800nm, there is the insertion second hole of average pore size 60nm in the cavity wall of macropore, there is the third level hole of average pore size 10nm insertion on the hole wall in second level hole.
It is machined into method to take up an official post in the porous material said three-dimensional body of the same size for taking 9 10mm × 10mm × 10mm, its quality is tested with plum Teller-support benefit XP26 Microbalance balances, as a result it is as shown in table 1, wherein, it is expressed as a percentage relative to the absolute value of the bias of mean value, its value be relative to mean value absolute value of the bias divided by mass average value, as shown in Table 2, its mass deviation is not more than 4%.
Table 2
| Piece number | Quality（mg） | Relative to the absolute value of the bias of mean value（%） |
| 1 | 512.939 | 0.0% |
| 2 | 501.857 | 2.1% |
| 3 | 512.371 | 0.1% |
| 4 | 516.202 | 0.7% |
| 5 | 526.150 | 2.6% |
| 6 | 522.125 | 1.8% |
| 7 | 514.616 | 0.4% |
| 8 | 502.281 | 2.0% |
| 9 | 506.518 | 1.2% |
| Mass average value | 512.784 |
The preparation method of the porous polytetrafluoroethylene material is：
（1）By PTFE fine powder end, the polyethylene glycol mixing that molecular weight is 1000,380 DEG C are heated with stirring to, persistently stir 60min, be quickly cooled to room temperature and crushed, carried out crushing at subzero degree Celsius and obtain polytetrafluoroethylgranule granule；
（2）Particle diameter is distributed as the emulsion of solid content 60% for 200nm polytetrafluoroethylgranule granules, by its with particle diameter 100nm shitosans, 5%（Mass ratio）Polyacrylic acid solution, 20wt% starch emulsions, uniform mixing, according to 50：25：4：4 mass ratio, is made into spinning solution；
（3）Under vacuum, polytetrafluoroethylene (PTFE) precursor film is produced using electrospinning process in orientation electrostatic spinning fiber silk device；
（4）Precursor film is wound into 5 layers to diameter 4-25mm cylinders hold mode, is sent into tube furnace and is sintered in vacuum or protective atmosphere, sintered and sintered using temperature programmed control zonal cooling, with the speed of 5 DEG C/min from room temperature to 160 DEG C, at 160 DEG C 80min is incubated；With the ramp of 5 DEG C/min to 290 DEG C, at 290 DEG C 60min is incubated；With the ramp of 2 DEG C/min to 360 DEG C, at 360 DEG C 20min is incubated；With the ramp of 6 DEG C/min to 400 DEG C, at 400 DEG C 60min is incubated；
（5）Temperature programmed control cooling after sintering, according to routine techniques subsequent treatment, obtains the porous ptfe tube formula film with three-level pore structure, and thickness is 163 μm, tubular membrane diameter 4-25mm.
, without the need for supporting, form stable, thickness is controllable, can be used for gas-liquid separation and Liquid liquid Separation for the polytetrafluoroethylene fibre tubular membrane, realizes that Accurate Classification is filtered, such as it is applied to two-spot or many vigour（Liquid）The filtration of body, its flux is big, and rejection is high, is difficult to be contaminated（Such as the infiltration fouling membrane of multi-component liquid）, the advantage with efficient long-acting.170 ° of film water contact angle；Tensile strength 28N/mm2, water pressure resistance 7kg/cm2。
Such as, it is applied to polynary（Or mixing）In the Membrane Materials of alcohol/acid-water-non-volatile solute system, total flux can reach 42kg/m2More than h, in system non-volatile solute rejection more than 99.9%, volatilization alcohol/acid separation factor=[alcohol/acid mass fraction in distillate ×（1- material liquid ethanol mass fractions）] ÷ [material liquid alcohol/acid mass fraction ×（1- distillates alcohol/acid mass fraction）] can reach more than 10.
Claims (11)
1. a kind of polytetrafluoroethylene fibre tubular membrane, including polytetrafluoroethylmaterial material body, polytetrafluoroethylene (PTFE) is in threadiness, fibre diameter is 30～200nm, the cavity wall that body has the vestibule in 10nm～1000nm apertures and formed around vestibule in three dimensions, vestibule is in uniform distribution, the three-dimensional insertion of each vestibule, and vestibule refers to each vestibule on the porous material under arbitrary unit level volume in uniform distribution in uniform distribution；Porosity of=75%, tensile strength 15N/mm2More than, water pressure resistance 3kg/cm2More than.
2. polytetrafluoroethylene fibre tubular membrane as claimed in claim 1, vestibule with 30～1000nm apertures and the cavity wall formed around vestibule in three dimensions, subordinate's vestibule of 10～100nm, vestibules at different levels each three-dimensional insertion and vestibule at different levels also insertion each other each other are set in cavity wall；Vestibule is in uniform distribution, and vestibule refers to each vestibule on the porous material under arbitrary unit level volume in uniform distribution in uniform distribution.
3. polytetrafluoroethylene fibre tubular membrane as claimed in claim 1 or 2, the unit level volume refers to cubic centimetre level or cubic millimeter level or more subsection level volume.
4. the polytetrafluoroethylene fibre tubular membrane as described in claim 1,2 or 3, institute's vestibule is referred in uniform distribution and be not more than each said three-dimensional body of a cubic centimetre and formed objects in the take up an official post volume that takes of the porous material, and their quality is substantially suitable.
5. polytetrafluoroethylene fibre tubular membrane as claimed in claim 4, the quality quite refers to the said three-dimensional body for appointing the multiple volumes for taking to be not more than a cubic centimetre and formed objects on the porous material substantially, claim its quality respectively, the mean value of their quality is obtained, and arbitrary three-dimensional weight is not more than the 4% of said three-dimensional body mass average value relative to the absolute value of the bias of mass average value.
6. the polytetrafluoroethylene fibre tubular membrane as described in claim 1-5 is arbitrary, the multistage material take up an official post the volume that takes be not more than one cubic millimeter formed objects said three-dimensional body, their quality are substantially suitable.
7. polytetrafluoroethylene fibre tubular membrane as claimed in claim 6, the quality quite refers to the said three-dimensional body of the formed objects for appointing the multiple volumes for taking to be not more than a cubic millimeter on the porous material substantially, claim its quality respectively, the mean value of their quality is obtained, and arbitrary three-dimensional weight is not more than the 4% of said three-dimensional body mass average value relative to the absolute value of the bias of mass average value.
8. the polytetrafluoroethylene fibre tubular membrane as described in claim 1-7 is arbitrary, it is made up of multistage porous material, body is the vestibule being classified with material pore size, and the cavity wall in three dimensions around vestibule is constituted, subordinate's vestibule, vestibules at different levels each three-dimensional insertion and vestibule at different levels also insertion each other each other are set in cavity wall.
9. the polytetrafluoroethylene fibre tubular membrane as described in claim 1-8 is arbitrary, next stage porous material constitutes the cavity wall of upper level vestibule.
10. the polytetrafluoroethylene fibre tubular membrane as described in claim 1-8 is arbitrary, the cavity wall of higher level's vestibule is constituted by the multistage porous material of its subordinate is compound.
The 11. polytetrafluoroethylene fibre tubular membranes as described in claim 1-8 is arbitrary, the cavity wall of higher level's vestibule is constituted by the porous materials at different levels of its subordinate are compound.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510766523.1A CN106669453B (en) | 2015-11-11 | 2015-11-11 | Polytetrafluoroethylene superfine fiber tubular membrane |
| PCT/CN2016/105251 WO2017080464A1 (en) | 2015-11-11 | 2016-11-09 | Polytetrafluoroethylene superfine fiber tubular membrane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510766523.1A CN106669453B (en) | 2015-11-11 | 2015-11-11 | Polytetrafluoroethylene superfine fiber tubular membrane |
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| CN106669453B CN106669453B (en) | 2020-11-06 |
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| CN106669453B (en) | 2020-11-06 |
| WO2017080464A1 (en) | 2017-05-18 |
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