CN109966928B - Preparation method of high-flux high-strength polyamide flat plate micro-filtration membrane - Google Patents
Preparation method of high-flux high-strength polyamide flat plate micro-filtration membrane Download PDFInfo
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- 239000004952 Polyamide Substances 0.000 title claims abstract description 115
- 229920002647 polyamide Polymers 0.000 title claims abstract description 115
- 239000012528 membrane Substances 0.000 title claims abstract description 103
- 238000001471 micro-filtration Methods 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 31
- 238000005266 casting Methods 0.000 claims abstract description 26
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 25
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 235000019253 formic acid Nutrition 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000004907 flux Effects 0.000 claims abstract description 15
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 13
- 238000000614 phase inversion technique Methods 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 7
- 238000000576 coating method Methods 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 14
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 229920002292 Nylon 6 Polymers 0.000 claims description 12
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 6
- NVJUHMXYKCUMQA-UHFFFAOYSA-N 1-ethoxypropane Chemical compound CCCOCC NVJUHMXYKCUMQA-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- 239000004953 Aliphatic polyamide Substances 0.000 abstract description 6
- 229920003231 aliphatic polyamide Polymers 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 230000003321 amplification Effects 0.000 abstract description 3
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 21
- 239000011148 porous material Substances 0.000 description 7
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000004677 Nylon Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000001728 nano-filtration Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 238000007605 air drying Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 235000012907 honey Nutrition 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/147—Microfiltration
-
- 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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
-
- 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
-
- 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
- B01D69/06—Flat membranes
-
- 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
- B01D71/56—Polyamides, e.g. polyester-amides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/02—Details relating to pores or porosity of the membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a preparation process of an aliphatic polyamide membrane material, and provides a preparation method of a polyamide flat plate micro-filtration membrane with high flux and high strength. The method comprises the following specific steps: dissolving an aliphatic polyamide material in formic acid to obtain a polyamide solution, sequentially adding alcohol and ether additives, uniformly coating the prepared polyamide casting solution on non-woven fabrics, and preparing the polyamide filter membrane by a dry forming process in a phase inversion method. The preparation method has the advantages of simple preparation process, simple operation and lower cost, and is beneficial to industrial amplification. Through experimental tests, the flux of the membrane can reach 5000L/(m) 2 And h) or more, the breaking strength of the film can reach 15MPa or more.
Description
Technical Field
The invention belongs to the field of preparation and application of separation membrane materials, and particularly relates to a preparation method of a high-flux high-strength polyamide microfiltration membrane. The preparation method has the advantages of simple operation and simple working procedures, and the prepared polyamide filter membrane has higher flux and breaking strength and can be used for bacteria detection, bacteria interception and the like in the fields of foods and medicines.
Background
In recent years, the membrane technology has been injected with new vitality for separation science due to the characteristics of low energy consumption, low cost, high efficiency, easy amplification and the like, and is more and more widely applied to the fields of chemical industry, environmental protection, food, medicine, electronics, electric power, metallurgy, light spinning, sea water desalination and the like, and has wide development prospect. The membrane material is the core of the membrane technology, and the processing and forming process of the membrane has close relation with the pore structure, mechanical property and the like of the membrane.
Polyamide, commonly called nylon, is a general engineering plastic with long history and wide application, and has good comprehensive properties including mechanical properties, heat resistance, abrasion resistance, chemical resistance and the like. The nylon membrane prepared from polyamide has good hydrophilicity, is suitable for aqueous solution containing acid and alkali, is also suitable for various organic solvents such as alcohols, hydrocarbons, ethers, esters and ketones, benzene and benzene homologues, dimethylformamide, dimethyl sulfoxide and the like, is one of microporous filter membranes with the widest application range, and is widely applied to various fields at present. Polyamide filters, however, also have some disadvantages: for example, the mechanical strength of the aliphatic polyamide membrane is not high, and the film forming performance is poor; the flux of the nylon filter membrane is not high [ what honey. Preparation of nylon microporous membrane and research on membrane pore structure performance [ D ]. Zhejiang: university of Zhejiang, 2008.
At present, many documents and patents are reported on polyamide filter membranes. CN108854578A provides a method for preparing a tubular membrane of an aromatic polyamide nonwoven fabric supporting tube; CN108187512a provides a high flux polyamide nanofiltration composite membrane and a preparation method thereof; CN107583469a provides a preparation method of a polyamide composite nanofiltration membrane containing amino modified nano particles; CN106621848A relates to an aliphatic polyamide hollow fiber membrane, a preparation method and application. However, the related reports mainly adopt polyamide as a base membrane material for research, or the preparation of a polyamide nanofiltration membrane is mainly carried out, and the research of simply preparing a polyamide flat plate microfiltration membrane with high flux and high strength is rarely reported.
Disclosure of Invention
The invention aims to provide a preparation method of a polyamide flat micro-filtration membrane with high flux and high strength, which is mainly characterized in that prepared polyamide casting membrane liquid is uniformly coated on non-woven fabrics, a dry forming process in a phase inversion method is used for preparing a polyamide flat micro-filtration membrane film, and a secondary forming means is creatively adopted in the forming process, so that the mechanical strength of an aliphatic polyamide flat micro-filtration membrane is greatly improved, the flux of the polyamide micro-filtration membrane is also greatly improved, and the problems of low mechanical strength, poor film forming performance and low flux of the conventional aliphatic polyamide flat micro-filtration membrane are overcome.
The method comprises the following specific steps:
(1) Preparing a polyamide casting film liquid: and dissolving the dried polyamide raw material in a formic acid solvent, stirring at room temperature for reaction for 4-5 hours, adding an alcohol additive after the polyamide is completely dissolved in the formic acid, stirring for 1 hour, and adding an ether additive and continuously stirring for 1 hour to obtain the polyamide casting solution.
(2) Preparation of a polyamide filter membrane: and uniformly coating the prepared polyamide casting solution on non-woven fabrics, then placing the non-woven fabrics in a constant-temperature and constant-humidity sealed air environment, and preparing the primary molded polyamide filter membrane through a dry molding process in a phase inversion method.
(3) The post-treatment process comprises the following steps: and taking out the primarily molded polyamide filter membrane from the sealed air environment, putting the primarily molded polyamide filter membrane into a new constant temperature and humidity sealed air environment, standing, and performing secondary molding on the primarily molded polyamide filter membrane. And then taking out the secondarily formed polyamide filter membrane, and putting the secondarily formed polyamide filter membrane into a blast drying oven for drying to obtain the polyamide filter membrane with high flux and high strength.
In the preparation of the polyamide filter membrane, the polyamide is one of polyamide 66 or polyamide 6; the alcohol additive is one of methanol, ethanol or isopropanol, and the ether additive is one of n-butyl ether or ethyl propyl ether.
The primary dry forming process parameters of the invention are as follows: the air temperature is controlled at 20-25 ℃, the air humidity is controlled at 70-90% RH, and the molding time is controlled at 30-40 min in a closed environment.
In the post-treatment process, the process parameters of the secondary molding are as follows: the air temperature is controlled at 20-25 ℃, the air humidity is controlled at 40-60% RH, the secondary forming time is controlled at 15-20 min, the temperature of the air blast drying oven is controlled at 45-50 ℃, and the drying time is controlled at 20-30 min.
As an improvement, the gram weight range of the non-woven fabric in the process of preparing the polyamide filter membrane is 30-60 g/m 2 The thickness range is 70-120 um, the longitudinal breaking strength is more than 30N/15mm, and the transverse breaking strength is more than 20N/15 mm.
The invention makes the prepared polyamide flat micro-filtration membrane have developed three-dimensional pore canal structure by a dry secondary forming means, and provides a convenient channel for the inflow and outflow of the separation liquid. By introducing non-woven fabrics as the supporting layer material, the mechanical strength of the polyamide flat micro-filtration membrane is greatly improved, so that the application range of the polyamide flat micro-filtration membrane is wider. Meanwhile, the preparation method adopted by the invention has simple process operation, simple preparation process and lower cost, and is beneficial to realizing industrialized amplification.
Drawings
FIG. 1 is an electron microscopic image of the surface structure of a polyamide micro-filtration membrane in example one.
FIG. 2 is an electron microscopic image of a cross-sectional structure of a polyamide micro-filtration membrane in example one.
FIG. 3 is an electron microscopic image of the surface structure of the polyamide micro-filtration membrane in the third embodiment.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
embodiment one:
preparing a polyamide casting film liquid: before synthesis, the polyamide 66 was dried in a blow dryer at 50℃for 24 hours, 15g of the dried polyamide 66 (nylon 66) and 68g of formic acid having a mass fraction of 95% were taken, and the polyamide 66 was dissolved in formic acid and stirred. After stirring at room temperature for 4 hours, 6g of absolute ethanol was added after the polyamide 66 was completely dissolved in formic acid, and stirring was continued for 1 hour. After the absolute ethyl alcohol is completely dissolved in the solution, 8g of n-butyl ether is added, and the solution is stirred for 1 hour continuously, so that the n-butyl ether is completely dissolved in the solution. The polyamide casting solution is prepared.
Preparation of a polyamide filter membrane: uniformly coating the prepared polyamide casting solution on a non-woven fabric (wherein the gram weight of the non-woven fabric is 48 g/m) 2 The thickness of the non-woven fabric is 100 μm), and then the non-woven fabric is placed in a sealed air environment with the temperature of 25 ℃ and the RH of 80%, and the primary molded polyamide filter membrane is prepared by a dry molding process in a phase inversion method. The molding time was 30min.
The post-treatment process comprises the following steps: taking out the primarily molded polyamide filter membrane from the sealed air environment, and then placing the primarily molded polyamide filter membrane into a sealed air environment with the temperature of 25 ℃ and the RH of 50%, and standing for 15min to allow the primarily molded polyamide filter membrane to undergo secondary molding. And then taking out the secondarily formed polyamide filter membrane, and putting the polyamide filter membrane into a blast drying oven at 45 ℃ for drying for 20min to obtain the polyamide flat plate micro-filtration membrane.
The implementation effect is as follows: the experiment shows that the thickness of the polyamide flat plate micro-filtration membrane is 110 mu m, the average pore diameter distribution of the membrane is 0.45 mu m, and the pure water flux under the conditions of 0.1MPa and 25 ℃ is 7250L/(m) 2 And (h) a step of. The tensile strength of the film was 19.58MP and the elongation at break was 9.18%.
Embodiment two:
preparing a polyamide casting film liquid: before synthesis, the polyamide 66 was dried in a blow dryer at 50℃for 24 hours, 16g of the dried polyamide 66 (nylon 66) and 68g of formic acid having a mass fraction of 95% were taken, and the polyamide 66 was dissolved in formic acid and stirred. After stirring the reaction at room temperature for 4 hours, after the polyamide 66 was completely dissolved in formic acid, 7g of isopropyl alcohol was added and stirring was continued for 1 hour. After the isopropanol was completely dissolved in the solution, 7g of n-butyl ether was added and the solution was stirred for 1 hour to completely dissolve the n-butyl ether in the solution. The polyamide casting solution is prepared.
Preparation of a polyamide filter membrane: uniformly coating the prepared polyamide casting solution on a non-woven fabric (wherein the gram weight of the non-woven fabric is 40 g/m) 2 The thickness of the non-woven fabric is 95 μm), and then the non-woven fabric is placed in a sealed air environment with the temperature of 25 ℃ and the RH of 85%, and the primary molded polyamide filter membrane is prepared by a dry molding process in a phase inversion method. The molding time was 30min.
The post-treatment process comprises the following steps: taking out the primarily molded polyamide filter membrane from the sealed air environment, and then placing the primarily molded polyamide filter membrane into a sealed air environment with the temperature of 25 ℃ and the RH of 60%, and standing for 15min to allow the primarily molded polyamide filter membrane to undergo secondary molding. And then taking out the secondarily formed polyamide filter membrane, and putting the polyamide filter membrane into a blast drying oven at 45 ℃ for drying for 20min to obtain the polyamide flat plate micro-filtration membrane.
The implementation effect is as follows: the experiment shows that the thickness of the polyamide flat plate micro-filtration membrane is 105 mu m, the average pore diameter distribution of the membrane is 0.40 mu m, and the pure water flux under the conditions of 0.1MPa and 25 ℃ is 6830L/(m) 2 And (h) a step of. The tensile strength of the film was 17.38MP and the elongation at break was 8.48%.
Embodiment III:
preparing a polyamide casting film liquid: before synthesis, the polyamide 6 was dried in a forced air drying oven at 50℃for 24 hours, 14g of the dried polyamide 6 (nylon 6) and 70g of formic acid having a mass fraction of 95% were taken, and the polyamide 6 was dissolved in formic acid and stirred. After stirring at room temperature for 4 hours, 6g of absolute ethanol was added after the polyamide 6 was completely dissolved in formic acid, and stirring was continued for 1 hour. After the absolute ethyl alcohol is completely dissolved in the solution, 8g of ethyl propyl ether is added, and the solution is continuously stirred for 1h, so that the ethyl propyl ether is completely dissolved in the solution. The polyamide casting solution is prepared.
Preparation of a polyamide filter membrane: uniformly coating the prepared polyamide casting solution on a non-woven fabric (wherein the gram weight of the non-woven fabric is 40 g/m) 2 The thickness of the non-woven fabric is 95 μm), and then the non-woven fabric is placed in a sealed air environment with the temperature of 25 ℃ and the RH of 90%, and the primary molded polyamide filter membrane is prepared by a dry molding process in a phase inversion method. The molding time was 25min.
The post-treatment process comprises the following steps: taking out the primarily molded polyamide filter membrane from the sealed air environment, and then placing the primarily molded polyamide filter membrane into a sealed air environment with the temperature of 25 ℃ and the RH of 55%, and standing for 15min to allow the primarily molded polyamide filter membrane to undergo secondary molding. And then taking out the secondarily formed polyamide filter membrane, and putting the polyamide filter membrane into a blast drying oven at 45 ℃ for drying for 20min to obtain the polyamide flat plate micro-filtration membrane.
The implementation effect is as follows: the experiment shows that the thickness of the polyamide flat plate micro-filtration membrane is 103 mu m, the average pore size distribution of the membrane is 0.8 mu m, and the pure water flux under the conditions of 0.1Mpa and 25 ℃ is 9380L/(m) 2 And (h) a step of. The tensile strength of the film was 18.18MP and the elongation at break was 9.06%.
Embodiment four:
preparing a polyamide casting film liquid: before synthesis, the polyamide 6 was dried in a forced air drying oven at 50℃for 24 hours, 16g of the dried polyamide 6 (nylon 6) and 68g of formic acid having a mass fraction of 95% were taken, and the polyamide 6 was dissolved in formic acid and stirred. After stirring the reaction at room temperature for 4 hours, 7g of methanol was added after the polyamide 6 was completely dissolved in formic acid, and stirring was continued for 1 hour. After the methanol was completely dissolved in the solution, 7g of ethyl propyl ether was added, and the solution was stirred for 1 hour to completely dissolve ethyl propyl ether in the solution. The polyamide casting solution is prepared.
Preparation of a polyamide filter membrane: uniformly coating the prepared polyamide casting film liquid on the non-woven fabricOn cloth (wherein the nonwoven fabric has a grammage of 55g/m 2 The thickness of the non-woven fabric is 115 mu m), and then the non-woven fabric is placed in a sealed air environment with the temperature of 25 ℃ and the RH of 90%, and the primary molded polyamide filter membrane is prepared by a dry molding process in a phase inversion method. The molding time was 30min.
The post-treatment process comprises the following steps: taking out the primarily molded polyamide filter membrane from the sealed air environment, and then placing the primarily molded polyamide filter membrane into a sealed air environment with the temperature of 25 ℃ and the RH of 60%, and standing for 15min to allow the primarily molded polyamide filter membrane to undergo secondary molding. And then taking out the secondarily formed polyamide filter membrane, and putting the polyamide filter membrane into a blast drying oven at 45 ℃ for drying for 20min to obtain the polyamide flat plate micro-filtration membrane.
The implementation effect is as follows: the experiment shows that the thickness of the polyamide flat plate micro-filtration membrane is 98 mu m, the average pore diameter distribution of the membrane is 0.35 mu m, and the pure water flux under the conditions of 0.1MPa and 25 ℃ is 5320L/(m) 2 And (h) a step of. The tensile strength of the film was 20.16MP and the elongation at break was 9.36%.
Claims (4)
1. A method for preparing a high-flux high-strength polyamide flat micro-filtration membrane, which comprises the following steps:
(1) Preparing a polyamide casting film liquid: placing a polyamide raw material into a blast drying oven to be dried for more than 12 hours at 50 ℃, dissolving the dried polyamide raw material into a formic acid solvent, stirring and reacting for 4-5 hours at room temperature, adding an alcohol additive and stirring for 1 hour after the polyamide is completely dissolved in the formic acid, and then adding an ether additive and continuously stirring for 1 hour to obtain a polyamide casting solution;
(2) Preparation of a polyamide filter membrane: uniformly coating the prepared polyamide casting solution on non-woven fabrics, then placing the non-woven fabrics in a constant-temperature and constant-humidity sealed air environment, and preparing the primary molded polyamide filter membrane through a dry molding process in a phase inversion method;
(3) The post-treatment process comprises the following steps: taking out the primarily molded polyamide filter membrane from the sealed air environment, putting the primarily molded polyamide filter membrane into a new constant temperature and humidity sealed air environment, standing, and performing secondary molding on the primarily molded polyamide filter membrane; then taking out the secondarily formed polyamide filter membrane, and putting the secondarily formed polyamide filter membrane into a blast drying oven for drying to obtain a polyamide filter membrane with high flux and high strength;
the primary dry forming process parameters in the step of preparing the polyamide filter membrane are as follows: controlling the air temperature at 20-25 ℃, controlling the air humidity at 70-90% RH, and controlling the molding time at 30-40 min in a closed environment; in the post-treatment process, the process parameters of the secondary molding are as follows: the air temperature is controlled at 20-25 ℃, the air humidity is controlled at 40-60% RH, the secondary forming time is controlled at 15-20 min, the temperature of the air blast drying oven is controlled at 45-50 ℃, and the drying time is controlled at 20-30 min.
2. The method for preparing the high-flux high-strength polyamide flat micro-filtration membrane according to claim 1, which is characterized in that: in the preparation of the polyamide casting film liquid, the polyamide raw material is one of polyamide 66 or polyamide 6; the content of the formic acid in the formic acid solvent is at least 90%; the alcohol additive is one of methanol, ethanol or isopropanol, the ether additive is one of n-butyl ether or ethyl propyl ether, and the alcohol additive and the ether additive are both more than the analytical grade.
3. The method for preparing the high-flux high-strength polyamide flat micro-filtration membrane according to claim 1 or 2, which is characterized in that: in the preparation of the polyamide casting solution, polyamide accounts for 14-16% of the total casting solution in mass fraction, formic acid accounts for 68-71% of the total casting solution in mass fraction, alcohol additives account for 6-7% of the total casting solution in mass fraction, and ether additives account for 7-9% of the total casting solution in mass fraction.
4. The method for preparing the high-flux high-strength polyamide flat micro-filtration membrane according to claim 1, which is characterized in that: the gram weight of the non-woven fabric for preparing the polyamide filter membrane is in the range of 30-60 g/m 2 The thickness range is 70-120 mu m, the longitudinal breaking strength is more than 30N/15mm, and the transverse breaking strength is more than 20N/15 mm.
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|---|---|---|---|---|
| CN111603947B (en) * | 2020-05-21 | 2023-08-01 | 杭州科百特科技有限公司 | Nylon membrane with support and preparation method and application thereof |
| CN111603946A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN111603949B (en) * | 2020-05-21 | 2023-06-30 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
| CN112619449B (en) * | 2020-12-16 | 2023-05-02 | 杭州科百特科技有限公司 | Nylon membrane and preparation method and application thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4774038A (en) * | 1985-06-21 | 1988-09-27 | Domnick Hunter Filters Limited | Polyamide membranes |
| US5006247A (en) * | 1989-08-15 | 1991-04-09 | Minnesota Mining And Manufacturing Company | Asymmetric porous polyamide membranes |
| CN1071100A (en) * | 1991-09-27 | 1993-04-21 | 中国科学院大连化学物理研究所 | The preparation of sulfonated polyary-ether-sulfone nanometer filter film |
| CN1552508A (en) * | 2003-05-30 | 2004-12-08 | 上海一鸣过滤技术有限公司 | Microporous barrier and preparing method thereof |
| CN1958736A (en) * | 2006-10-20 | 2007-05-09 | 清华大学 | Polyimide asymmetric membrane for desulfurization of gasoline, and preparation method |
| CN101979132A (en) * | 2010-11-05 | 2011-02-23 | 天津森诺过滤技术有限公司 | Method for preparing asymmetric nanofiltration membrane by blending polyether sulfone and sulfonated polysulfone high polymers |
| CN102114391A (en) * | 2009-12-30 | 2011-07-06 | 中国科学院生态环境研究中心 | Method for preparing polyisophthaloyl metaphenylene diamide nanofiltration membrane |
| CN102658037A (en) * | 2012-04-26 | 2012-09-12 | 青岛科技大学 | Method for preparing polyvinylidene fluoride panel microporous membrane |
| CN107185416A (en) * | 2017-06-29 | 2017-09-22 | 河南省科学院能源研究所有限公司 | A kind of high temperature resistant separation furfural press filtration film, preparation method and applications |
| CN107970782A (en) * | 2017-11-27 | 2018-05-01 | 中国科学院生态环境研究中心 | Polymer film with high intercommunicating pore structure and preparation method thereof |
| CN109012236A (en) * | 2018-08-07 | 2018-12-18 | 中国乐凯集团有限公司 | Casting solution, ultrafiltration membrane and the method for preparing ultrafiltration membrane |
-
2019
- 2019-03-18 CN CN201910204842.1A patent/CN109966928B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4774038A (en) * | 1985-06-21 | 1988-09-27 | Domnick Hunter Filters Limited | Polyamide membranes |
| US5006247A (en) * | 1989-08-15 | 1991-04-09 | Minnesota Mining And Manufacturing Company | Asymmetric porous polyamide membranes |
| CN1071100A (en) * | 1991-09-27 | 1993-04-21 | 中国科学院大连化学物理研究所 | The preparation of sulfonated polyary-ether-sulfone nanometer filter film |
| CN1552508A (en) * | 2003-05-30 | 2004-12-08 | 上海一鸣过滤技术有限公司 | Microporous barrier and preparing method thereof |
| CN1958736A (en) * | 2006-10-20 | 2007-05-09 | 清华大学 | Polyimide asymmetric membrane for desulfurization of gasoline, and preparation method |
| CN102114391A (en) * | 2009-12-30 | 2011-07-06 | 中国科学院生态环境研究中心 | Method for preparing polyisophthaloyl metaphenylene diamide nanofiltration membrane |
| CN101979132A (en) * | 2010-11-05 | 2011-02-23 | 天津森诺过滤技术有限公司 | Method for preparing asymmetric nanofiltration membrane by blending polyether sulfone and sulfonated polysulfone high polymers |
| CN102658037A (en) * | 2012-04-26 | 2012-09-12 | 青岛科技大学 | Method for preparing polyvinylidene fluoride panel microporous membrane |
| CN107185416A (en) * | 2017-06-29 | 2017-09-22 | 河南省科学院能源研究所有限公司 | A kind of high temperature resistant separation furfural press filtration film, preparation method and applications |
| CN107970782A (en) * | 2017-11-27 | 2018-05-01 | 中国科学院生态环境研究中心 | Polymer film with high intercommunicating pore structure and preparation method thereof |
| CN109012236A (en) * | 2018-08-07 | 2018-12-18 | 中国乐凯集团有限公司 | Casting solution, ultrafiltration membrane and the method for preparing ultrafiltration membrane |
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