CN114618233A - ECTFE melt-blown filter material and preparation method thereof - Google Patents
ECTFE melt-blown filter material and preparation method thereof Download PDFInfo
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- CN114618233A CN114618233A CN202011470953.6A CN202011470953A CN114618233A CN 114618233 A CN114618233 A CN 114618233A CN 202011470953 A CN202011470953 A CN 202011470953A CN 114618233 A CN114618233 A CN 114618233A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
- B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
- B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
- B01D39/163—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin sintered or bonded
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0622—Melt-blown
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/12—Special parameters characterising the filtering material
Abstract
The invention discloses an ECTFE melt-blown filter material and a preparation method thereof, wherein the average pore diameter of the ECTFE melt-blown filter material is 0.1-100 mu m, the fiber diameter is 0.05-50 mu m, the longitudinal tensile breaking strength is 15-100N, and the transverse tensile breaking strength is 10-50N. The ECTFE melt-blown filter material has the advantages of high tensile strength, high elongation at break and high filter precision, and is suitable for harsh environments such as high temperature resistance, acid and alkali resistance, corrosion resistance and the like.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to an ECTFE melt-blown filter material.
Background
The melt-blown non-woven technology is an important means for efficiently producing and processing industrial textiles, the product has the characteristics of short process flow, high production efficiency, superfine fiber, large specific surface area, high porosity and the like, and has unique advantages in the fields of medical and health protection, efficient filtration, warm keeping, heat insulation, sound absorption, noise reduction, battery diaphragms and the like. The early application of melt-blown non-woven fabrics was mainly filter materials, and the melt-blown non-woven fabrics were suitable for gas-solid separation or liquid-solid separation. The net-shaped pores of the melt-blown non-woven fabric filter material enhance the dispersion effect and can improve the filtering effect, and the melt-blown non-woven fabric filter material has a superfine fiber structure with small and many micropores and has strong interception and screen blocking effects on particles. At present, melt-blown non-woven products in domestic markets are mainly polypropylene (PP), and other polymer melt-blown non-woven products including Polyester (PET), Polyamide (PA), Polyethylene (PE), Polyurethane (PU), polylactic acid (PLA), polyphenylene sulfide (PPS), ethylene-chlorotrifluoroethylene copolymer (ECTFE) and the like are still in the research and development stage.
ECTFE is a copolymer of ethylene and chlorotrifluoroethylene alternating in a ratio of 1:1, a semi-crystalline, thermoplastic polymer, with an embrittlement temperature of less than-76 ℃, a melting point of between 220 and 260 ℃ and can be used for a long time at a temperature above 150 ℃. The ECTFE has excellent solvent resistance, comprises common corrosive chemicals and organic solvents, is particularly suitable for high-temperature and high-corrosion separation environments, has wide application prospect in the separation field, and is a potential ideal filter material.
ECTFE is generally processed by a hot-melt method because it does not have a solvent suitable for ECTFE at room temperature. Melt blown nonwoven technology is the primary process for ECTFE following thermal phase separation. The melt-blown non-woven technology is one of polymer direct web-forming methods, and is characterized in that high polymer melt extruded by a screw extruder is subjected to extreme stretching by high-speed high-temperature air blowing or other means to form superfine fibers, then the superfine fibers are gathered on a web-forming roller or a web-forming curtain to form a web, and finally the web is reinforced by self-bonding to form the melt-blown non-woven fabric. US patent US5470663A suggests that vinyl fluoride polymer processing can be carried out by melt blowing techniques. The ECTFE melt index adopted in the patent is lower than 1500g/10min (190 ℃, 2.16kg), and the processing of the raw material with higher melt index can not be realized.
Disclosure of Invention
In order to solve the technical problems, the invention provides an ECTFE melt-blown filter material which has high filter precision, high mechanical strength and wide application range.
The purpose of the invention is realized by the following technical scheme:
the ECTFE melt-blown filter material has the average pore size of 0.1-100 microns, the fiber diameter of 0.05-50 microns, the longitudinal tensile breaking strength of 15-100N and the transverse tensile breaking strength of 10-50N.
Preferably, the average pore diameter of the melt-blown filter material is 0.1-50 μm, the fiber diameter is 0.05-30 μm, the longitudinal tensile breaking strength is 15-50N, and the transverse tensile breaking strength is 10-30N; more preferably, the average pore diameter of the melt-blown filter material is 0.1 to 10 μm, the fiber diameter is 0.05 to 20 μm, the longitudinal tensile breaking strength is 15 to 30N, and the transverse tensile breaking strength is 10 to 15N.
The ECTFE melt-blown filter material is prepared from one ECTFE resin or a mixture of two or more ECTFE resins with different melt indexes, and the melt index of the ECTFE resin is 300g/10 min-2000 g/10min (2.16kg, 230 ℃).
The invention adjusts the corresponding performance of the ECTFE melt-blown filter material by selecting ECTFE resins with different melt indexes as raw materials. The larger the melt index of the ECTFE resin is, the smaller the melt viscosity is, the better the melt fluidity is, the more easily the ECTFE resin is blown by the drawing wind, and the smaller the pore diameter of the prepared ECTFE melt-blown filter material fiber is. However, the ECTFE melt index of the ECTFE resin is too high, which causes the mechanical properties such as tensile breaking strength of the ECTFE melt-blown filter material to be reduced.
Preferably, the ECTFE melt-blown filter material is prepared from a mixture of ECTFE resins with two or more different melt indexes. The ECTFE resin mixture with different melt indexes is heated and plasticized by a double screw to form a melt, and the melt is distributed in a gradient manner in the screw, so that the fluidity is enhanced, and the superfine fiber with good mechanical property is obtained.
Specifically, the ECTFE resin mixture of different melt indices comprises ECTFE resin a and ECTFE resin B. The melt index of the ECTFE resin A is 800g/10 min-1200 g/10min (2.16kg, 230 ℃); the melt index of the ECTFE resin B is 300g/10 min-2000 g/10min (2.16kg, 230 ℃), and the ECTFE resin B can be specifically selected according to different application occasions and filtration requirements. When the ECTFE melt-blown filter material needs to have higher tensile breaking strength, the melt index of the ECTFE resin B is 300g/10 min-800 g/10min (2.16kg, 230 ℃); when higher filtration accuracy is required for the ECTFE melt-blown filter material, the melt index of the ECTFE resin B is 1200g/10 min-2000 g/10min (2.16kg, 230 ℃).
The invention also provides a preparation method of the ECTFE melt-blown filter material, which has the advantages of short process flow and high production efficiency, and comprises the following specific steps:
s1, heating the ECTFE resin and the antioxidant in an extruder to obtain an ECTFE melt, wherein the heating temperature is 180-280 ℃;
s2, forming superfine fibers by the ECTFE melt under the blowing of high-speed high-temperature air flow, and forming a fiber web on a web roller or a web forming curtain;
s3, the fiber web is made into the ECTFE melt-blown filter material through self-bonding or hot pressing.
Specifically, the ECTFE resin and the antioxidant are firstly and uniformly mixed in a kneader or a mixer, then the mixture is added into a double-screw extruder, a homogeneous ECTFE melt is obtained after heating and melting, and the homogeneous ECTFE melt passes through a spinning die and is blown by high-speed high-temperature air flow to form superfine fibers.
Preferably, the ECTFE resin is a powder or a pellet.
The fluoropolymer discoloration is essentially caused by the color-changing groups, such as conjugated unsaturated bonds and the like. A hydrogen halide gas is generated along with the generation of the conjugated unsaturated bond. HF gas is generated in the reaction system, and the adopted processing equipment is preferably made of Hastelloy materials, so that corrosion is prevented. Therefore, the screw and the barrel of the double-screw extruder are made of hastelloy.
Extruder screw length to diameter ratio is an important parameter of the screw. When other conditions are fixed, the length-diameter ratio is increased, namely the length of the screw is increased, so that the retention time of the ECTFE resin in the screw is prolonged, the ECTFE resin is ensured to be melted for a sufficient time, and the quality of the ECTFE melt-blown filter material is improved. And the length is increased, the pressure flow and the leakage flow can be reduced, and the production capacity of the extruder is improved. However, an excessively large aspect ratio tends to cause thermal decomposition of the ECTFE resin due to an excessively long residence time in the screw. Therefore, the selection of the aspect ratio should be determined in accordance with the processability, product quality and productivity of the ECTFE resin. The length-diameter ratio of the screw is 15: 1-60: 1, preferably 35: 1-40: 1.
the antioxidant has the function of delaying and inhibiting the oxidation process of the polymer, and achieves the effects of preventing the yellowing of the polymer and the like mainly by inhibiting the generation of free radicals and the decomposition of hydroperoxide. Preferably, the antioxidant is selected from tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-di-tert-butylphenyl) propionic acid ] pentaerythritol diphosphite, dioctadecylpentaerythritol diphosphite, 5, 7-di-tert-butyl-3- (3, 4-dimethylphenyl) -3H-benzofuran-2-one, ditolyl-dibutyl-benzofuranone, 1, 3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) s-triazine-2, 4, 6- (1H, 3H, 5H) trione, 3, 9-bis (2, 4-di-tert-butylphenoxy) -2,4,8, 10-tetraoxo-3, 9-diphosphobicyclo [5.5] undecane, beta- (3, at least one of octadecyl 5-di-tert-butyl-4-hydroxyphenyl) propionate, dioctadecyl thiodipropionate, pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], zinc stearate, calcium stearate and rare earth zinc stearate.
Preferably, the antioxidant is 0.0008-0.02 in parts.
According to the preparation method of the ECTFE melt-blown filter material, preferably, the temperature of the high-speed high-temperature air flow is 200-300 ℃, and the air pressure is 0.015-0.1 MPa; the temperature of the net roller or the net forming curtain is 5-40 ℃.
According to the preparation method of the ECTFE melt-blown filter material, the distance between the net roller or the net curtain and the die lip for spraying and blowing the superfine fibers is preferably 5 cm-50 cm. Further preferably, the distance between the net roller or the net forming curtain and the die lip for spraying and blowing the superfine fibers is 0 cm-30 cm.
Under the condition of a certain hot air flow velocity, the larger the distance between the net roller and the die lip is, the longer the time for the melt spinning yarns to reach the net roller from the die lip is, and the longer the time is, the more obvious the temperature reduction is. After the melt spinning temperature is reduced, the melt spinning is not easy to be drawn and stretched by hot air to become thin, so the diameter of the melt spinning is seriously influenced by the distance between the net roller and the die lip, namely the larger the distance between the net roller and the die lip is, the thicker the diameter of the melt spinning is.
According to the preparation method of the ECTFE melt-blown filter material, in the step S3, the hot-pressing temperature is 100-200 ℃, the hot-pressing pressure is 0.01-5 MPa, and the hot-pressing time is 0-10S.
The invention also provides application of any ECTFE melt-blown filter material, which can be used as a filter membrane in a filter assembly and applied to TFT-LCD etching and cleaning. Preferably, other components of the filter assembly comprise a core column, a support net, a shell, an end cover and the like, and are all processed by ECTFE melt-blown filter materials with the melt index of 5g/10 min-25 g/10min (230 ℃, 21.6 kg).
Compared with the prior art, the invention has the beneficial effects that: the ECTFE melt-blown filter material provided by the invention has the advantages of high tensile strength, high elongation at break and high filter precision, and is suitable for harsh environments such as high temperature resistance, acid and alkali resistance, corrosion resistance and the like.
Drawings
FIG. 1 is a schematic view of a melt blowing process of the present invention;
FIG. 2 is a front view of a melt-blown filter material according to example 1 of the present invention;
FIG. 3 is an enlarged view of the front structure of the melt-blown filter material in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the invention to these embodiments. It will be appreciated by those skilled in the art that the present invention encompasses all alternatives, modifications and equivalents as may be included within the scope of the claims.
Example 1
600g of ECTFE resin having a melt index of 600g/10min (230 ℃ C., 2.16kg) and 6g of tris (2, 4-di-t-butylphenyl) phosphite were weighed out in total for the ECTFE resin having a melt index of 1200g/10min (230 ℃ C., 2.16kg), and mixed uniformly by means of a kneader to obtain a solid mixture. And then adding the solid material into an extruder in a manual feeding mode, completely melting and extruding at 210 ℃ through an extruder screw, and blowing by adopting high-speed high-temperature airflow to obtain the ECTFE superfine fiber which is collected on a roller. The hot rolling was carried out at 100 ℃ under 0.05MPa for 10 seconds. The prepared melt-blown filter material has the longitudinal tensile breaking strength of 17N, the transverse tensile breaking strength of 12N, the fiber diameter of 0.08 mu m and the average pore diameter of 0.5 mu m.
Example 2
600g of ECTFE resin having a melt index of 600g/10min (230 ℃ C., 2.16kg) and 6g of tris (2, 4-di-t-butylphenyl) phosphite were weighed and mixed well by a kneader to obtain a solid mixture. And then adding the solid material into an extruder in a manual feeding mode, completely melting and extruding at 210 ℃ through an extruder screw, and blowing by adopting high-speed high-temperature airflow to obtain the ECTFE superfine fiber which is collected on a roller. The hot rolling was carried out at 100 ℃ under 0.05MPa for 10 seconds. The prepared melt-blown filter material has the longitudinal tensile breaking strength of 20N, the transverse tensile breaking strength of 13N, the fiber diameter of 0.3 mu m and the average pore diameter of 0.8 mu m.
The tensile breaking strength was higher than that of example 1. This is because as the melt index of the polymer decreases, the spherulite size of the melt-blown film filter material prepared becomes larger and the tensile breaking strength becomes larger.
Comparative example 1
Comparative example 1 was conducted as in example 1 except that: the raw materials used were ECTFE resin having a melt index of 600g/10min (230 ℃ C., 2.16kg) and a total of 600g of ECTFE resin having a melt index of 2500g/10min (230 ℃ C., 2.16 kg).
The prepared melt-blown membrane filter material has the longitudinal tensile breaking strength of 8N, the transverse tensile breaking strength of 6N, the fiber fineness of 0.06 mu m and the average pore diameter of 0.3 mu m.
Comparative example 2
Comparative example 2 was conducted as in example 1 except that: the antioxidant tris (2, 4-di-tert-butylphenyl) phosphite is not added.
As can be seen from comparative example 2, as the ECTFE resin is used in the extruder for a longer period of time, black spots appear on the surface of the microfine fiber.
Comparative example 3
Comparative example 3 was conducted as in example 1 except that: the ECTFE resin melt-blowing experiment is carried out by adopting 316 material melt-blowing equipment, and as a result, carbonization occurs in a cylinder and a spinning die.
Example 3
The ECTFE melt-blown filter material obtained in example 1 was immersed in 5% HCl aqueous solution, 5% NaOH aqueous solution, 1% NaOH and 1% NaClO mixed aqueous solution for 72 hours, and the filter material color, appearance and mechanical properties were not significantly changed.
Comparative example 4
Comparative example 4 was conducted as in example 1 except that: PVDF resin is used as a raw material to prepare the filter material.
And then the prepared filter material is placed in 5 percent HCl aqueous solution, 5 percent NaOH aqueous solution, 1 percent NaOH and 1 percent NaClO mixed aqueous solution for 72 hours, the color of the filter material is changed into black, and the mechanical property is reduced by more than 50 percent.
Claims (10)
1. An ECTFE melt-blown filter material characterized by: the average pore diameter of the melt-blown filter material is 0.1-100 mu m, the fiber diameter is 0.05-50 mu m, the longitudinal tensile breaking strength is 15-100N, and the transverse tensile breaking strength is 10-50N.
2. The ECTFE melt blown filter material of claim 1, wherein: the average pore diameter of the melt-blown filter material is 0.1-50 mu m, the fiber diameter is 0.05-30 mu m, the longitudinal tensile breaking strength is 15-50N, and the transverse tensile breaking strength is 10-30N.
3. The ECTFE melt blown filter material of claim 1, wherein: the average pore diameter of the melt-blown filter material is 0.1-10 mu m, the fiber diameter is 0.05-20 mu m, the longitudinal tensile breaking strength is 15-30N, and the transverse tensile breaking strength is 10-15N.
4. The ECTFE melt blown filter material of any one of claims 1 to 3, wherein: the ECTFE melt-blown filter material is prepared from one ECTFE resin or a mixture of two or more ECTFE resins with different melt indexes, wherein the melt index of the ECTFE resin is 300g/10 min-2000 g/10min (2.16kg, 230 ℃).
5. The process for preparing the ECTFE melt blown filter material of any one of claims 1 to 4 wherein: the preparation method comprises the following steps:
s1, heating the ECTFE resin and the antioxidant in an extruder to obtain an ECTFE melt, wherein the heating temperature is 180-280 ℃;
s2, forming superfine fibers by the ECTFE melt under the blowing of high-speed high-temperature air flow, and forming a fiber web on a web roller or a web forming curtain;
s3, the fiber web is made into the ECTFE melt-blown filter material through self-bonding or hot pressing.
6. The process for preparing the ECTFE melt blown filter material of claim 5 wherein: in step S1, the extruder is a twin-screw extruder, the screw and barrel of the twin-screw extruder are made of hastelloy, the length-diameter ratio of the screw is 15: 1-60: 1.
7. the process for preparing the ECTFE melt blown filter material of claim 5 wherein: the antioxidant is selected from tris (2, 4-di-tert-butylphenyl) phosphite, bis (2, 4-di-tert-butylphenyl) propionic acid ] pentaerythritol diphosphite, dioctadecyl pentaerythritol diphosphite, 5, 7-di-tert-butyl-3- (3, 4-dimethylphenyl) -3H-benzofuran-2-one, ditolyl dibutylbenzofuranone, 1, 3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) s-triazine-2, 4, 6- (1H, 3H, 5H) trione, 3, 9-bis (2, 4-di-tert-butylphenoxy) -2,4,8, 10-tetraoxo-3, 9-diphosphobicyclo [5.5] undecane, beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester, At least one of dioctadecyl thiodipropionate, pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], zinc stearate, calcium stearate and rare earth zinc stearate.
8. The method of making the ECTFE melt blown filter material of claim 5, wherein: in step S2, the temperature of the high-speed high-temperature airflow is 200-300 ℃, and the wind pressure is 0.015-0.1 MPa; the temperature of the net roller or the net forming curtain is 5-40 ℃.
9. The method of making the ECTFE melt blown filter material of claim 5, wherein: in step S3, the hot pressing temperature is 100-200 ℃, the hot pressing pressure is 0.01-5 MPa, and the hot pressing time is 0-10S.
10. Use of the ECTFE melt blown filter material of any one of claims 1 to 4 wherein: the melt-blown filter material is used as a filter membrane in a filter assembly and is applied to TFT-LCD etching and cleaning.
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| CN110087754A (en) * | 2016-12-15 | 2019-08-02 | 阿莫绿色技术有限公司 | Filter filtration material, its manufacturing method and the filter unit including it |
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| US5401458A (en) * | 1993-10-25 | 1995-03-28 | Exxon Chemical Patents Inc. | Meltblowing of ethylene and fluorinated ethylene copolymers |
| JPH07229048A (en) * | 1994-02-16 | 1995-08-29 | Toyobo Co Ltd | Nonwoven fabric and its production |
| JPH08318115A (en) * | 1995-05-26 | 1996-12-03 | Toyobo Co Ltd | Production of filter, filter cartridge and nonwoven fabric for filter |
| JP2009230986A (en) * | 2008-03-21 | 2009-10-08 | Asahi Glass Co Ltd | Electrolyte membrane for solid polymer fuel cell, its manufacturing method, and membrane electrode assembly for solid polymer fuel cell |
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