CN109966928A - A kind of preparation method of high-throughput high-intensitive polyamide flat micro-filtration - Google Patents
A kind of preparation method of high-throughput high-intensitive polyamide flat micro-filtration Download PDFInfo
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- CN109966928A CN109966928A CN201910204842.1A CN201910204842A CN109966928A CN 109966928 A CN109966928 A CN 109966928A CN 201910204842 A CN201910204842 A CN 201910204842A CN 109966928 A CN109966928 A CN 109966928A
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- polyamide
- filter membrane
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- 239000004952 Polyamide Substances 0.000 title claims abstract description 110
- 229920002647 polyamide Polymers 0.000 title claims abstract description 110
- 238000001471 micro-filtration Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000012528 membrane Substances 0.000 claims abstract description 59
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000005266 casting Methods 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 21
- 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 18
- 235000019253 formic acid Nutrition 0.000 claims abstract description 18
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 15
- 239000000654 additive Substances 0.000 claims abstract description 13
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000001298 alcohols Chemical class 0.000 claims abstract description 8
- 238000000465 moulding Methods 0.000 claims description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 12
- 229920002292 Nylon 6 Polymers 0.000 claims description 10
- 238000005516 engineering process Methods 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 6
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- 206010013786 Dry skin Diseases 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 230000004907 flux Effects 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- 238000002474 experimental method Methods 0.000 abstract description 5
- 230000003321 amplification Effects 0.000 abstract description 3
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 28
- 210000004379 membrane Anatomy 0.000 description 16
- 238000000034 method Methods 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 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 class CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical class CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 150000001408 amides Chemical class 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 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
- 210000002469 basement membrane Anatomy 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000001514 detection method Methods 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
- 229960004756 ethanol Drugs 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- YKWNUSJLICDQEO-UHFFFAOYSA-N ethoxyethane;propan-2-ol Chemical compound CC(C)O.CCOCC YKWNUSJLICDQEO-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 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
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000001728 nano-filtration Methods 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
- 239000013535 sea water Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000010148 water-pollination Effects 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 present invention relates to a kind of preparation processes of fatty polyamide membrane material, provide a kind of preparation method of high-throughput high-intensitive polyamide flat micro-filtration.It comprises the concrete steps that: fatty polyamide material is dissolved in formic acid, obtain polyamide solution, alcohols and ether additive are sequentially added later, deployed polyamide casting solution is uniformly coated on non-woven fabrics, and polyamide filter membrane is prepared by the dry process for forming in phase inversion.Preparation process of the present invention is simple, easy to operate, and cost is relatively low, is conducive to industrial amplification.It is tested by experiment, the flux of film can reach 5000L/ (m2﹒ h) more than, the breaking strength of film can reach 15MPa or more.
Description
Technical field
The invention belongs to the preparation of separation membrane material and its application fields, and in particular to a kind of high-throughput high-intensitive polyamide
The preparation method of microfiltration membranes.Preparation manipulation is simple, and process is simple, prepared polyamide filter membrane flux with higher and fracture
Intensity, Bacteria Detection, the bacterium retention etc. that can be used in food and medicine field.
Background technique
In recent years, membrane technology has been separation science injection with characteristics such as its low energy consumption, low cost, high-efficient, easy amplifications
New vitality, and it is applied to chemical industry, environmental protection, food, medicine, electronics, electric power, metallurgy, light textile, seawater more and more widely
The fields such as desalination have vast potential for future development.Membrane material is the core of membrane technology, and the machine-shaping process of film and the hole of film are tied
Structure, mechanical property etc. are in close relations.
Polyamide is commonly called as nylon, is with a long history, widely used general engineering plastic, has good comprehensive performance,
Including mechanical property, heat resistance, wear resistance, chemical resistance etc..And using polyamide as nylon membrane made from raw material, have
Good hydrophily is applicable not only to the aqueous solution containing acid-base property, is also applied for all kinds of organic solvents, for example, alcohols, hydro carbons,
Ethers, esters, ketone, benzene and substituted benzene, dimethylformamide, dimethyl sulfoxide etc. are the most wide micropores of the scope of application
One of filter membrane has been widely used for every field at present.But polyamide filter membrane also has the shortcomings that: such as fatty polyamide
The mechanical strength of film is not high, and filming performance is poor；The flux of nylon leaching film not high [preparation of what honey nylon-microporous membrane and film
The hole structural property research Zhejiang [D]: Zhejiang University, 2008].
Currently, for polyamide filter membrane, there are many documents and patent to report.CN108854578A provides one kind
The preparation method of the tubular membrane of aromatic polyamides non-woven cloth support tube；CN108187512A provides a kind of high-throughput polyamide
Nano filtering composite membrane and preparation method thereof；CN107583469A provides that a kind of polyamide containing amino modified nanoparticle is compound to be received
The preparation method of filter membrane；CN106621848A relates to a kind of fatty polyamide hollow-fibre membrane and preparation method and application.
But relevant report is all mainly to be studied using polyamide as basal lamina material, or prepare based on polyamide nanofiltration membrane, and single
The research for preparing the polyamide flat micro-filtration of high-throughput high intensity purely is rarely reported.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high-throughput high-intensitive polyamide flat micro-filtration, this method
Mainly configured polyamide casting solution is uniformly coated on non-woven fabrics, passes through the dry process for forming in phase inversion
It carries out preparing polyamide flat micro-filtration film, and creatively takes post forming means in molding process, no
The mechanical strength of fatty polyamide flat micro-filtration is only substantially increased, while also substantially increasing the logical of polyamide microfiltration membranes
Amount, overcomes the problem that current fatty polyamide flat micro-filtration mechanical strength is not high, filming performance is poor and flux is small.
Specific step is as follows:
(1) it prepares polyamide casting solution: dried polyamide raw material being dissolved in formic acid solvent, reaction is stirred at room temperature
4 ~ 5h is added alcohols additive and stirs 1h, add ether additive and continue to stir after polyamide is dissolved completely in formic acid
Polyamide casting solution is obtained after 1h.
(2) it prepares polyamide filter membrane: the polyamide casting solution prepared being uniformly coated on non-woven fabrics, perseverance is placed into
In the seal gas environment of constant temperature and humidity, first molding polyamide is prepared by the dry process for forming in phase inversion and is filtered
Film.
(3) aftertreatment technology: first molding polyamide filter membrane is taken out from seal gas environment, places into one newly
The closed air environment of constant temperature and humidity in stand, allow first molding polyamide filter membrane to carry out post forming.Then it takes out secondary
Polyamide filter membrane after molding, which is put into air dry oven drying, can be obtained the polyamide filter membrane of high-throughput high intensity.
For the present invention in preparing polyamide filter membrane, the polyamide is one of polyamide 66 or polyamide 6；It is described
Alcohols additive be methanol, ethyl alcohol perhaps one of isopropanol ether additive be in n-butyl ether or ethylene-propylene ether one
Kind.
First dry process for forming parameter of the present invention is as follows: air temperature control is at 20 ~ 25 DEG C, air humidity control
System is in 70 ~ 90%RH, and molding time control is in 30 ~ 40min under closed environment.
In aftertreatment technology of the present invention, the technological parameter of post forming is as follows: air temperature control is 20 ~ 25
DEG C, air humidity control is controlled in 15 ~ 20min, the temperature of air dry oven 45 in 40 ~ 60%RH, the control of post forming time
~ 50 DEG C, drying time is controlled in 20 ~ 30min.
As an improvement the described non-woven fabrics the grammes per square metre scope prepared during polyamide filter membrane is in 30 ~ 60g/m2, thick
Range is spent in 70 ~ 120um, and longitudinal fracture intensity is in 30N/15mm or more, cross-breaking strength 20N/15mm or more.
The present invention makes polyamide flat micro-filtration obtained have flourishing 3 D pore canal by dry method post forming means
Structure flows in and out the channel provided convenience for separating liquid.And by introducing non-woven fabrics as support layer material, significantly
The mechanical strength for improving polyamide flat micro-filtration keeps its use scope wider.The preparation method mistake that the present invention uses simultaneously
Journey is easy to operate, and preparation process is simple, and cost is relatively low, is conducive to realize industrialization amplification.
Detailed description of the invention
Fig. 1 is the surface texture electron microscope of polyamide microfiltration membranes in embodiment one.
Fig. 2 is the section structure electron microscope of polyamide microfiltration membranes in embodiment one.
Fig. 3 is the surface texture electron microscope of polyamide microfiltration membranes in embodiment three.
Specific embodiment
The present invention will be further described below with reference to the accompanying drawings and embodiments:
Embodiment one:
It prepares polyamide casting solution: polyamide 66 being put into the drying 24 hours of 50 DEG C of air dry oven before synthesis, is taken dried
The formic acid 68g that polyamide 66 (nylon66 fiber) 15g and mass fraction are 95%, polyamide 66 is dissolved in formic acid and is stirred.?
After being stirred to react 4h at room temperature, after polyamide 66 is completely dissolved in formic acid, dehydrated alcohol 6g is added, and continues to stir 1h.To nothing
After water-ethanol is completely dissolved in solution, n-butyl ether 8g is added, and continue agitating solution 1h, n-butyl ether is made to be completely dissolved in solution.Just it makes
It is standby to complete polyamide casting solution.
It prepares polyamide filter membrane: the polyamide casting solution prepared is uniformly coated on non-woven fabrics (wherein non-woven fabrics
Grammes per square metre is 48g/m2, nonwoven thickness is 100 μm), it is then placed in 25 DEG C, in the seal gas environment of 80%RH, passes through inversion of phases
First molding polyamide filter membrane is prepared in dry process for forming in method.Molding time is 30min.
Aftertreatment technology: first molding polyamide filter membrane is taken out from seal gas environment, places into 25 DEG C, 50%
It is stood in the closed air environment of RH, first molding polyamide filter membrane is allowed to carry out post forming, time of repose 15min.So
Polyamide filter membrane after taking out post forming afterwards is put into the drying 20min of the air dry oven at 45 DEG C, and it is flat that polyamide can be obtained
Plate microfiltration membranes.
Implementation result: experiment measure polyamide flat micro-filtration with a thickness of 110 μm, the average pore size of film is distributed as 0.45
μm, pure water flux under the conditions of 0.1MPa, 25 DEG C is 7250L/ (m2﹒ h).The tensile strength of film is 19.58MP, extension at break
Rate is 9.18%.
Embodiment two:
It prepares polyamide casting solution: polyamide 66 being put into the drying 24 hours of 50 DEG C of air dry oven before synthesis, is taken dried
The formic acid 68g that polyamide 66 (nylon66 fiber) 16g and mass fraction are 95%, polyamide 66 is dissolved in formic acid and is stirred.?
After being stirred to react 4h at room temperature, after polyamide 66 is completely dissolved in formic acid, isopropanol 7g is added, and continues to stir 1h.To isopropyl
After alcohol is completely dissolved in solution, n-butyl ether 7g is added, and continue agitating solution 1h, n-butyl ether is made to be completely dissolved in solution.Just it has prepared
At polyamide casting solution.
It prepares polyamide filter membrane: the polyamide casting solution prepared is uniformly coated on non-woven fabrics (wherein non-woven fabrics
Grammes per square metre is 40g/m2, nonwoven thickness is 95 μm), it is then placed in 25 DEG C, in the seal gas environment of 85%RH, passes through inversion of phases
First molding polyamide filter membrane is prepared in dry process for forming in method.Molding time is 30min.
Aftertreatment technology: first molding polyamide filter membrane is taken out from seal gas environment, places into 25 DEG C, 60%
It is stood in the closed air environment of RH, first molding polyamide filter membrane is allowed to carry out post forming, time of repose 15min.So
Polyamide filter membrane after taking out post forming afterwards is put into the drying 20min of the air dry oven at 45 DEG C, and it is flat that polyamide can be obtained
Plate microfiltration membranes.
Implementation result: experiment measure polyamide flat micro-filtration with a thickness of 105 μm, the average pore size of film is distributed as 0.40
μm, pure water flux under the conditions of 0.1MPa, 25 DEG C is 6830L/ (m2﹒ h).The tensile strength of film is 17.38MP, extension at break
Rate is 8.48%.
Embodiment three:
It prepares polyamide casting solution: polyamide 6 being put into the drying 24 hours of 50 DEG C of air dry oven before synthesis, take dried gather
Amide 6(nylon 6) formic acid 70g that 14g and mass fraction are 95%, polyamide 6 is dissolved in formic acid and is stirred.In room temperature
Under be stirred to react 4h after, after polyamide 6 is completely dissolved in formic acid, be added dehydrated alcohol 6g, and continue stir 1h.To dehydrated alcohol
After being completely dissolved in solution, ethylene-propylene ether 8g is added, and continue agitating solution 1h, ethylene-propylene ether is made to be completely dissolved in solution.Just completion is prepared
Polyamide casting solution.
It prepares polyamide filter membrane: the polyamide casting solution prepared is uniformly coated on non-woven fabrics (wherein non-woven fabrics
Grammes per square metre is 40g/m2, nonwoven thickness is 95 μm), it is then placed in 25 DEG C, in the seal gas environment of 90%RH, passes through inversion of phases
First molding polyamide filter membrane is prepared in dry process for forming in method.Molding time is 25min.
Aftertreatment technology: first molding polyamide filter membrane is taken out from seal gas environment, places into 25 DEG C, 55%
It is stood in the closed air environment of RH, first molding polyamide filter membrane is allowed to carry out post forming, time of repose 15min.So
Polyamide filter membrane after taking out post forming afterwards is put into the drying 20min of the air dry oven at 45 DEG C, and it is flat that polyamide can be obtained
Plate microfiltration membranes.
Implementation result: experiment measure polyamide flat micro-filtration with a thickness of 103 μm, the average pore size of film is distributed as 0.8 μ
M, pure water flux under the conditions of 0.1Mpa, 25 DEG C are 9380L/ (m2﹒ h).The tensile strength of film is 18.18MP, extension at break
Rate is 9.06%.
Example IV:
It prepares polyamide casting solution: polyamide 6 being put into the drying 24 hours of 50 DEG C of air dry oven before synthesis, take dried gather
Amide 6(nylon 6) formic acid 68g that 16g and mass fraction are 95%, polyamide 6 is dissolved in formic acid and is stirred.In room temperature
Under be stirred to react 4h after, after polyamide 6 is completely dissolved in formic acid, be added methanol 7g, and continue stir 1h.It is completely dissolved in methanol
After solution, ethylene-propylene ether 7g is added, and continue agitating solution 1h, ethylene-propylene ether is made to be completely dissolved in solution.Just it prepares and completes polyamide
Casting solution.
It prepares polyamide filter membrane: the polyamide casting solution prepared is uniformly coated on non-woven fabrics (wherein non-woven fabrics
Grammes per square metre is 55g/m2, nonwoven thickness is 115 μm), it is then placed in into 25 DEG C, the seal gas environment of 90%RH, passes through phase and turn
First molding polyamide filter membrane is prepared in dry process for forming in change method.Molding time is 30min.
Aftertreatment technology: first molding polyamide filter membrane is taken out from seal gas environment, places into 25 DEG C, 60%
It is stood in the closed air environment of RH, first molding polyamide filter membrane is allowed to carry out post forming, time of repose 15min.So
Polyamide filter membrane after taking out post forming afterwards is put into the drying 20min of the air dry oven at 45 DEG C, and it is flat that polyamide can be obtained
Plate microfiltration membranes.
Implementation result: experiment measure polyamide flat micro-filtration with a thickness of 98 μm, the average pore size of film is distributed as 0.35 μ
M, pure water flux under the conditions of 0.1MPa, 25 DEG C are 5320L/ (m2﹒ h).The tensile strength of film is 20.16MP, extension at break
Rate is 9.36%.
Claims (6)
1. a kind of preparation method of high-throughput high-intensitive polyamide flat micro-filtration comprising:
(1) it prepares polyamide casting solution: polyamide raw material is put into 50 DEG C of dryings 12 hours or more of air dry oven, then will
Dried polyamide raw material are dissolved in formic acid solvent, and 4 ~ 5h of reaction is stirred at room temperature, and are dissolved completely in first to polyamide
After acid, alcohols additive is added and stirs 1h, adds ether additive and continue to obtain polyamide casting solution after stirring 1h；
(2) it prepares polyamide filter membrane: the polyamide casting solution prepared being uniformly coated on non-woven fabrics, constant temperature is then placed in
In the seal gas environment of constant humidity, first molding polyamide is prepared by the dry process for forming in phase inversion and is filtered
Film；
(3) aftertreatment technology: first molding polyamide filter membrane is taken out from seal gas environment, places into a new perseverance
It is stood in the closed air environment of constant temperature and humidity, first molding polyamide filter membrane is allowed to carry out post forming；Then post forming is taken out
Polyamide filter membrane afterwards, which is put into air dry oven drying, can be obtained the polyamide filter membrane of high-throughput high intensity.
2. the preparation method of high-throughput high-intensitive polyamide flat micro-filtration according to claim 1, it is characterised in that: institute
That states prepares in polyamide casting solution, and the polyamide raw material are one of polyamide 66 or polyamide 6；The first
The content of formic acid is at least 90% or more in sour solvent；Alcohols additive is one of methanol, ethyl alcohol or isopropanol, ethers
Additive is one of n-butyl ether or ethylene-propylene ether, and alcohols additive and ether additive are the pure rank of analysis or more.
3. the preparation method of high-throughput high-intensitive polyamide flat micro-filtration according to claim 1 or 2, feature exist
In: described prepares in polyamide casting solution, and polyamide accounts for the 14 ~ 16% of entire casting solution mass fraction, and formic acid accounts for entire casting film
The 68 ~ 71% of liquid mass fraction, alcohols additive account for the 6 ~ 7% of entire casting solution mass fraction, and ether additive accounts for entire casting film
The 7 ~ 9% of liquid mass fraction.
4. the preparation method of high-throughput high-intensitive polyamide flat micro-filtration according to claim 1, it is characterised in that: institute
The non-woven fabrics the grammes per square metre scope for preparing polyamide filter membrane stated is in 30 ~ 60g/m2, thickness range is at 70 ~ 120 μm, longitudinal fracture intensity
In 30N/15mm or more, cross-breaking strength 20N/15mm or more.
5. the preparation method of high-throughput high-intensitive polyamide flat micro-filtration according to claim 1 or 4, feature exist
In: described to prepare the first dry process for forming parameter of polyamide filter membrane as follows: for air temperature control at 20 ~ 25 DEG C, air is wet
Degree control is in 70 ~ 90%RH, and molding time control is in 30 ~ 40min under closed environment.
6. the preparation method of high-throughput high-intensitive polyamide flat micro-filtration according to claim 1, it is characterised in that: institute
In the aftertreatment technology stated, the technological parameter of the post forming is as follows: air temperature control is at 20 ~ 25 DEG C, air humidity
Control controls the drying at 45 ~ 50 DEG C in 15 ~ 20min, the temperature of air dry oven in 40 ~ 60%RH, the control of post forming time
Time controls in 20 ~ 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910204842.1A CN109966928B (en) | 2019-03-18 | 2019-03-18 | Preparation method of high-flux high-strength polyamide flat plate micro-filtration membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910204842.1A CN109966928B (en) | 2019-03-18 | 2019-03-18 | Preparation method of high-flux high-strength polyamide flat plate micro-filtration membrane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109966928A true CN109966928A (en) | 2019-07-05 |
| CN109966928B CN109966928B (en) | 2024-02-23 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111603947A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane with support and preparation method and application thereof |
| CN111603949A (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 |
| CN112619449A (en) * | 2020-12-16 | 2021-04-09 | 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111603947A (en) * | 2020-05-21 | 2020-09-01 | 杭州科百特科技有限公司 | Nylon membrane with support and preparation method and application thereof |
| CN111603949A (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 |
| CN112619449A (en) * | 2020-12-16 | 2021-04-09 | 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 |
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