CN114130373A - Nitrocellulose membrane and preparation method thereof - Google Patents
Nitrocellulose membrane and preparation method thereof Download PDFInfo
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- CN114130373A CN114130373A CN202111482600.2A CN202111482600A CN114130373A CN 114130373 A CN114130373 A CN 114130373A CN 202111482600 A CN202111482600 A CN 202111482600A CN 114130373 A CN114130373 A CN 114130373A
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- 229920001220 nitrocellulos Polymers 0.000 title claims abstract description 190
- 239000000020 Nitrocellulose Substances 0.000 title claims abstract description 189
- 239000012528 membrane Substances 0.000 title claims abstract description 186
- 238000002360 preparation method Methods 0.000 title description 16
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 claims abstract description 188
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 43
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 43
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 239000006184 cosolvent Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 12
- 238000007790 scraping Methods 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 229920002492 poly(sulfone) Polymers 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000007493 shaping process Methods 0.000 claims description 5
- 239000005341 toughened glass Substances 0.000 claims description 5
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 229920006393 polyether sulfone Polymers 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 23
- 230000008569 process Effects 0.000 abstract description 18
- 230000027455 binding Effects 0.000 abstract description 5
- 238000009740 moulding (composite fabrication) Methods 0.000 description 23
- 238000006243 chemical reaction Methods 0.000 description 20
- 239000007787 solid Substances 0.000 description 13
- 239000007788 liquid Substances 0.000 description 12
- 239000004094 surface-active agent Substances 0.000 description 12
- 239000012535 impurity Substances 0.000 description 10
- 239000003153 chemical reaction reagent Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001514 detection method Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- 239000012530 fluid Substances 0.000 description 7
- 239000011521 glass Substances 0.000 description 6
- 102000004169 proteins and genes Human genes 0.000 description 6
- 108090000623 proteins and genes Proteins 0.000 description 6
- 238000009826 distribution Methods 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 230000035945 sensitivity Effects 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000007853 buffer solution Substances 0.000 description 3
- 238000005354 coacervation Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 239000011268 mixed slurry Substances 0.000 description 3
- 238000005063 solubilization Methods 0.000 description 3
- 230000007928 solubilization Effects 0.000 description 3
- 238000004113 cell culture Methods 0.000 description 2
- 238000003745 diagnosis Methods 0.000 description 2
- RXKJFZQQPQGTFL-UHFFFAOYSA-N dihydroxyacetone Chemical class OCC(=O)CO RXKJFZQQPQGTFL-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000009396 hybridization Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000003119 immunoblot Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 230000009871 nonspecific binding Effects 0.000 description 2
- 102000039446 nucleic acids Human genes 0.000 description 2
- 108020004707 nucleic acids Proteins 0.000 description 2
- 150000007523 nucleic acids Chemical class 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000711573 Coronaviridae Species 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000000427 antigen Substances 0.000 description 1
- 102000036639 antigens Human genes 0.000 description 1
- 108091007433 antigens Proteins 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002301 cellulose acetate Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229960000913 crospovidone Drugs 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 235000013809 polyvinylpolypyrrolidone Nutrition 0.000 description 1
- 229920000523 polyvinylpolypyrrolidone Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000001262 western blot Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
- B01J20/28038—Membranes or mats made from fibers or filaments
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/282—Porous sorbents
- B01J20/285—Porous sorbents based on polymers
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a nitrocellulose membrane, which is prepared from a nitrocellulose membrane solution, wherein the nitrocellulose membrane solution comprises the following raw materials in parts by weight: 20-21 parts of a solvent; 0.2-0.3 part of cosolvent; 2-3 parts of a non-solvent; 5-6 parts of a forming agent; 0.02-0.08 part of hydrotalcite; 3-4 parts of cellulose nitrate particles. According to the cellulose nitrate membrane prepared by the invention, the added hydrotalcite has a special layered structure, so that functional high-molecular substances can enter the gaps of the hydrotalcite, the hydrotalcite is propped open without changing the structure of the hydrotalcite, the cellulose nitrate membrane of the porous supporting layer improves the effective pore diameter, the hydrophilicity of the cellulose nitrate membrane is effectively improved, and meanwhile, the cellulose nitrate membrane has strong binding force and can overcome the problem that blended particles are not uniformly distributed and are easy to agglomerate. The pore size is effective and perfect, which is helpful to reduce the chance of combining with non-specificity and reduce the false positive generated in the using process of using the nitrocellulose membrane as a carrier.
Description
Technical Field
The invention relates to the technical field of cellulose films, in particular to a nitrocellulose membrane and a preparation method thereof.
Background
The Nitrocellulose (NC) membrane is the earliest commercialized microporous filter membrane, has extremely strong nonspecific adsorption capacity to macromolecular substances such as protein, nucleic acid and the like, and is widely applied to the fields of molecular hybridization, immunoblotting, cell culture, medical diagnosis and the like. The carrier for the C/T line in the colloidal test paper is the place where the reaction between the antibody and the antigen occurs; the nitrocellulose membrane is a transfer medium which is most widely used in western blotting, has strong binding capacity to protein, and is suitable for various color development methods, including isotope, chemiluminescence, conventional color development, dyeing and fluorescence color development; low background and high signal-to-noise ratio.
The nitrocellulose membrane is also one of main carriers of a novel coronavirus antibody detection reagent, the requirement of the detection reagent is increased day by day along with the long-time spread of epidemic situation, only one or two enterprises in China can produce the nitrocellulose membrane at present, most of the nitrocellulose membranes depend on import, and the market conditions are in short supply.
The combination of the nitrocellulose membrane and the protein is supposed to be maintained for a long time by utilizing the hydrophilic combination of the membrane and the mutual electrostatic acting force, which reflects the effect of the pore diameter of the nitrocellulose membrane on the combination force and the hydrophilic function. As the membrane pore size decreases, the actual available surface area of the membrane increases, as does the amount of membrane bound protein, and the surface area is evaluated as a surface area ratio. In addition. The smaller the pore size of the membrane, the lower the chromatographic speed, and the longer the time for the gold-labeled complex to pass through the T line, the more complete the reaction. Although the smaller the pore diameter of the nitrocellulose membrane is, the higher the sensitivity is; but also slows down the running speed and increases the chance of non-specific binding, i.e. the higher the false positives. Therefore, it is necessary to select a nitrocellulose membrane suitable for the actual detection reaction and find a suitable equilibrium point, i.e., the reaction sensitivity is high and the possibility of non-specific binding is reduced.
The main preparation process of the nitrocellulose membrane comprises the following steps: preparing membrane slurry, spreading the membrane by a roller, drying and forming, rolling and slitting.
In the preparation process of adding the surfactant treatment solution, the nitrocellulose membrane is soaked in the treatment solution, the surface of the nitrocellulose membrane is treated, in order to ensure the continuity of membrane production, new treatment solution is continuously replaced according to the actual production condition, solute is timely supplemented to the treatment solution, and impurities are reduced. When the treating fluid soaked with the NC membrane in the fluid bath is replaced every time, in order to not affect production and ensure production efficiency, only 66% of the treating fluid in the fluid bath can be replaced, so that impurities contained in the remaining treating fluid which is not replaced cannot be discharged in time, and the treating fluid which is not completely replaced is continuously and uninterruptedly produced and used, so that the impurities of the treating fluid are easily attached to the surface of the nitrocellulose membrane; meanwhile, when the nitrocellulose membrane is produced, a large amount of bubbles exist on the surface of the nitrocellulose membrane, and the quality of the nitrocellulose membrane is influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a nitrocellulose membrane with good hydrophilicity and proper pore diameter and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a nitrocellulose membrane which is prepared from a nitrocellulose membrane solution, wherein the nitrocellulose membrane solution comprises the following raw materials in parts by weight:
through the technical scheme, the cellulose nitrate particles can be fully stirred and can be completely dissolved in the solvent, impurities of the formed NC film are reduced, the cosolvent can be beneficial to fully dissolving different components, the non-solvent is mainly used as a high-molecular surfactant, and the addition of the forming agent is beneficial to the final forming of the NC film. The membrane liquid prepared by the method has the advantages of easily obtained raw materials and simple preparation.
The hydrotalcite is added based on the special layered structure, functional high molecular substances can enter the gaps of the hydrotalcite, so that the hydrotalcite is propped open without changing the structure of the hydrotalcite, the nitrocellulose membrane of the porous supporting layer perfects the effective pore size, the hydrophilicity of the nitrocellulose membrane is effectively improved, and meanwhile, the hydrotalcite has strong binding force, and the problem that blended particles are uneven in distribution and easy to agglomerate can be solved.
Preferably, the solvent comprises one or two of N, N-dimethylformamide and N, N-dimethylacetamide in any weight ratio. As an aprotic highly polar solvent, the compound has strong dissolving power, high thermal stability, chemical stability and wide soluble substance range, and can activate compound molecules.
Preferably, the cosolvent comprises one or two of acetone and butanone in any weight ratio. It can be mixed with main solvent, and can be used as the simplest ketone in saturated aliphatic ketone series, and has high polarity, and can dissolve cellulose acetate and nitrocellulose.
Preferably, the non-solvent comprises one or both of polyvinylpyrrolidone and crospovidone in any weight ratio. As a high molecular surfactant, the surfactant has the functions of film forming, solubilization or coacervation in the system, has good affinity with a plurality of organic matters, and improves the hydrophilicity of the organic matters.
Preferably, the forming agent comprises one or more of polysulfone, polyarylsulfone and polyethersulfone. The polymer has the outstanding advantages of excellent mechanical property, high thermal stability, hydrolysis resistance, good dimensional stability and small molding shrinkage, and plays an important role in molding in the system of the invention.
Cellulose nitrate particle is a very common organic chemical, and is dissolved under certain conditions under the action of solvent and cosolvent to form mixed slurry, and in the slurry, a certain proportion of reagent is added to regulate the property of finally formed film, and the reagent mainly contains surfactant, high-molecular polymer and forming agent, and is dissolved in a buffer system.
The invention also provides a preparation method of the nitrocellulose membrane, which comprises the following steps:
preparing a nitrocellulose membrane solution according to the proportion of each substance;
step two, defoaming the nitrocellulose membrane solution obtained in the step one to obtain a nitrocellulose membrane casting solution;
step three, carrying out film scraping forming on the concentrated solution of the cellulose nitrate membrane defoamed in the step two, wiping the solution with absolute ethyl alcohol by using a scraper tool, washing the solution with pure water, drying the solution to obtain a clean toughened glass plate, and then scraping the film on the clean toughened glass plate;
step four, shaping the nitrocellulose membrane formed by scraping in the step three, putting the shaped nitrocellulose membrane into a gel bath with a fixed temperature, and treating to obtain a shaped nitrocellulose membrane;
and step five, drying the shaped nitrocellulose membrane obtained in the step four to obtain a finished nitrocellulose membrane product.
By adopting the technical scheme, the cellulose nitrate membrane liquid is fully stirred in the preparation process, the bubble content of the NC membrane is effectively reduced by controlling the temperature and the stirring time in the stirring process, and the prepared membrane liquid is subjected to standing and defoaming treatment, so that a large amount of bubbles generated on the surface of the NC membrane are effectively avoided, and the influence on the quality of the NC membrane liquid is reduced. The NC membrane with different thicknesses can be obtained by adjusting the distance between the scraper and the glass plate in the film scraping and over-forming process, the NC membrane is gradually solidified into the formed NC membrane by controlling the temperature of the gel bath, redundant impurities can be removed by putting the formed NC membrane into deionized water, and finally the vacuum drying process can effectively reduce the generation of bacteria on the surface of the NC membrane and ensure the quality of the nitrocellulose membrane.
Preferably, in the step one, the stirring temperature is between 60 and 65 ℃ and the stirring time is longer than 24 hours in the preparation of the nitrocellulose membrane solution.
By the technical scheme, the nitrocellulose membrane liquid can be fully stirred, and all components are completely dissolved. The temperature is 60-65 ℃, the stirring time is more than 24h, so that the hydrotalcite can be fully propped by other components to form a nitrocellulose membrane with a porous support layer, the effective aperture of the NC membrane is improved, and the hydrophilicity is improved.
Preferably, the nitrocellulose membrane solution needs to be defoamed in a standing manner, and the defoaming time is longer than 24 h.
Through the technical scheme, the nitrocellulose membrane liquid is completely dissolved after being fully stirred, and is subjected to standing and defoaming treatment in a drying environment, so that a large amount of bubbles generated on the surface of an NC membrane are effectively avoided, and the influence on the quality of the NC membrane is reduced.
Preferably, the ethanol content of the gel bath is 30-40%, the temperature is 30-35 ℃, and the time is more than 1 min. And in the scraper blade coating forming process of the membrane liquid, the thickness of the nitrocellulose membrane is controlled by adjusting the distance between the scraper and the glass plate. The control of the ethanol content in the gel bath is helpful for controlling the film forming speed, the process does not cause the aperture of the NC film to be enlarged, but improves the porosity of the film, the control of the temperature is helpful for washing off unreacted substances in the forming process of the nitrocellulose film, the water temperature is too high, the film forming speed is slow, the gel bath time is too short, and the unreacted substances in the NC film cannot be sufficiently washed off.
Through the technical scheme, the thickness of the nitrocellulose membrane can be controlled by adjusting the distance between the scraper and the toughened glass plate, the requirement for preparing NC membranes with different thicknesses is met, and more selectivity is provided.
Preferably, the nitrocellulose membrane is left in deionized water after being separated from the gel bath, and the standing time is more than 4 hours.
Through the technical scheme, the NC membrane after being shaped by the gel bath is peeled off and put into deionized water, so that unreacted substances or impurities attached to the NC membrane can be removed, and meanwhile, the NC membrane is prevented from being contacted with bacterial pollutants in the air under a wet state, so that the NC membrane is prevented from being polluted and the quality of the NC membrane is influenced.
Preferably, the nitrocellulose membrane is kept still in deionized water, and is required to be taken out and dried at the temperature of 44-50 ℃ after being kept still.
Through the technical scheme, the NC membrane taken out of the deionized water is placed in the vacuum drying box, so that the air isolation is facilitated, the influence of the humidity in the air on the NC membrane is avoided, and the content of bubbles on the surface of the NC membrane is reduced.
Preferably, the preparation of the cellulose nitrate membrane liquid comprises the following steps:
mixing the solvent, the cellulose nitrate particles and the hydrotalcite in proportion, and then stirring at room temperature;
and step two, adding the cosolvent, the forming agent and the non-solvent into the mixed solution, and continuously stirring at the temperature of 60-65 ℃ for 24-36 hours.
According to the technical scheme, the solvent, the hydrotalcite and the cellulose nitrate particles are mixed and stirred, so that the uniform mixing is facilitated, the solvent, the forming agent and the non-solvent are added and continuously stirred after the mixing, the dissolution of the cellulose nitrate is facilitated, the impurities of the formed NC membrane are reduced, the cosolvent can facilitate the full dissolution of different components, the non-solvent is mainly used as a high-molecular surfactant, and the addition of the forming agent facilitates the final shaping of the NC membrane.
In conclusion, the invention has the following beneficial effects:
1. according to the nitrocellulose membrane prepared by the method, the hydrotalcite is creatively added, a functional high-molecular substance can enter the interlayer of the hydrotalcite by utilizing the special layered structure of the hydrotalcite, so that the hydrotalcite is propped open without changing the structure of the hydrotalcite, the effective aperture of the nitrocellulose membrane is perfected by the nitrocellulose membrane of the porous supporting layer, and the hydrophilicity of the nitrocellulose membrane is effectively improved.
2. In the process of preparing the cellulose nitrate membrane, cellulose nitrate particles are dissolved under the action of a solvent and a cosolvent to form mixed slurry, a certain proportion of reagent is added into the slurry to adjust the property of the finally formed membrane, and the reagent mainly comprises a surfactant, a high molecular polymer, a forming agent and the like and is dissolved in a buffer system. The hydrophilic hydrotalcite fully stirred can be uniformly distributed in the NC membrane, so that the membrane structure is smoother, pore channels are uniformly distributed, and the porosity is improved.
3. In the invention, the types of the solvent, the cosolvent, the surfactant and the forming agent are selected, so that in the preparation process, all the components can be fully dissolved and mixed, and the addition of the surfactant is beneficial to film forming property, solubilization or coacervation, and the hydrophilicity of the NC film is improved. The hydrotalcite has a layered structure, so that the hydrotalcite shows insertability in the space structure, and can ensure that high molecular substances in the mixing process enter interlayer pores of the hydrotalcite, so that the hydrotalcite is spread without changing the space structure, and the hydrophilicity of the NC membrane is greatly increased.
4. In the process of preparing the membrane liquid, the invention has three links for reducing the influence of bubbles of the NC membrane: firstly, the stirring time is longer than 24 hours, so that all the components are fully mixed, and the generation of bubbles is reduced; secondly, standing the prepared membrane liquid for more than 24 hours; and thirdly, the shaping link is placed in a vacuum drying box, so that a large amount of bubbles are prevented from being generated on the surface of the NC film.
5. The hydrotalcite has flame retardance and can improve the flammability characteristics of the cellulose nitrate particles. The hydrotalcite has a special layered structure, functional high molecular substances can enter the gaps of the hydrotalcite to be propped open without changing the structure of the hydrotalcite, the nitrocellulose membrane of the porous supporting layer perfects the effective pore size, the chance of non-specific combination with an NC membrane in the using process is reduced, the false positive chance of detection is reduced, the hydrophilicity of the nitrocellulose membrane is effectively improved, and meanwhile, the hydrotalcite has strong binding force and can overcome the problem that blended particles are uneven in distribution and easy to agglomerate.
It should be understood that all combinations of the foregoing concepts and additional concepts described in greater detail below can be considered as part of the inventive subject matter of this disclosure unless such concepts are mutually inconsistent.
Additional aspects of the present invention, such as features and/or advantages of exemplary embodiments, will be apparent from the description which follows, or may be learned by practice of specific embodiments in accordance with the teachings of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention are clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention. Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
Nitrocellulose (NC) membranes are the earliest commercialized microporous filter membranes, have extremely strong nonspecific adsorption capacity to macromolecular substances such as proteins and nucleic acids, and are widely applied to the fields of molecular hybridization, immunoblotting, cell culture, medical diagnosis and the like. The main preparation process of the NC membrane comprises the following steps: preparing membrane slurry, spreading the membrane by a roller, drying, forming, rolling and cutting, but the NC membrane obtained by adopting the production process is easy to generate bubbles and impurities, and the aperture of the NC membrane is not easy to control. The NC membrane is obtained by adopting the following steps, so that the pore size of the NC membrane can be effectively controlled, the chance of non-specific combination is reduced in the detection process, and the false positive of the detection result is reduced.
The method for preparing the NC membrane comprises the following steps:
preparing a nitrocellulose membrane solution;
step two, defoaming the nitrocellulose membrane solution obtained in the step one to obtain a nitrocellulose membrane concentrated solution;
step three, carrying out film scraping forming on the concentrated solution of the cellulose nitrate film defoamed in the step two, and scraping the film on a clean toughened glass plate by using a scraper tool;
step four, shaping the nitrocellulose membrane formed by scraping in the step three, putting the shaped nitrocellulose membrane into a gel water bath with a fixed temperature, and performing water treatment to obtain a shaped nitrocellulose membrane;
and step five, drying the shaped nitrocellulose membrane obtained in the step four.
The nitrocellulose membrane solution is prepared from the following substances in parts by weight:
the solvent comprises one or two of N, N-dimethylformamide and N, N-dimethylacetamide in any weight ratio, is used as an aprotic high-polarity solvent, has strong dissolving power, high thermal stability and stable chemistry, has wide soluble substance range and can activate compound molecules.
The cosolvent comprises one or two of acetone and butanone in any weight ratio, can be mixed with a main solvent at will, is used as the simplest ketone in a saturated aliphatic ketone series, has high polarity, and can dissolve acetate fibers and nitric acid fibers.
The non-solvent comprises one or two of polyvinylpyrrolidone and cross-linked polyvinylpyrrolidone in any weight ratio. As a high molecular surfactant, the surfactant has the functions of film forming, solubilization or coacervation in the system, has good affinity with a plurality of organic matters, and improves the hydrophilicity of the organic matters.
The forming agent comprises one or more of polysulfone, polyarylsulfone and polyethersulfone. The polymer has the outstanding advantages of excellent mechanical property, high thermal stability, hydrolysis resistance, good dimensional stability and small molding shrinkage, and plays an important role in molding in the system of the invention.
Cellulose nitrate particle is a very common organic chemical, and is dissolved under certain conditions under the action of solvent and cosolvent to form mixed slurry, and in the slurry, a certain proportion of reagent is added to regulate the property of finally formed film, and the reagent mainly contains surfactant, high-molecular polymer and forming agent, and is dissolved in a buffer system.
The surface of the NC membrane is smooth and flat, and has no foreign matters or impurities, and the appropriate NC membrane is selected according to the capillary flow time and the binding capacity with protein. The main factors affecting the capillary flow time are membrane pore size, pore size distribution, membrane length and humidity. The smaller the pore size, the slower the flow rate and the higher the sensitivity, while the more uniform the pore distribution and the more uniform the flow rate and the better the sensitivity at the same pore size since the longer the reaction time the higher the probability of false positives. Further, in order to obtain an NC membrane having a higher effect, the hydrotalcite to be added in the present invention is an exchangeable type layered compound having a layered structure and carrying anions between layers. Hydrotalcite spatial structure has shown on the insertability and has carried between the layer volume ion and can exchange to can let the macromolecular substance who has the functionality get into hydrotalcite's interlaminar hole, make it propped open but go spatial structure can not produce very big change, meanwhile through adding hydrotalcite, the increase of to a great extent membrane hydrophilic characteristic, pore size that can effectual control nitrocellulose membrane improves the detection performance of NC membrane.
The present invention will be specifically described below with reference to specific examples, but the present invention is not limited thereto.
Example 1
(1) Preparing a nitrocellulose membrane solution: pouring 0.02g of hydrotalcite, 20g of N, N-dimethylacetamide and 3g of cellulose nitrate particles into a reaction device, stirring for more than 4 hours at room temperature, adding 0.2g of acetone, 5g of polysulfone and 2g of polyvinylpyrrolidone, and continuously stirring for 24-36 hours at the temperature of 60 ℃, and observing the content of solid matters in the reaction device until the solid matters are completely dissolved;
(2) placing the prepared NC membrane liquid into a dry environment, standing and defoaming, wherein foreign matter pollution is noticed in the process, and the dry environment is kept clean;
(3) before the film scraping process is started, the glass plate of the scraper is recommended to be cleaned by alcohol and washed and dried by deionized water. Pouring the NC membrane liquid onto a glass plate, scraping the membrane on the glass plate at a constant speed by using a scraper, and standing at room temperature for less than 1 min;
(4) standing the scraped glass plate in a gel water bath, keeping the temperature at 35 ℃ for more than 1min
(5) Taking out the NC membrane dropped off from the gel water bath, putting the NC membrane into deionized water, and standing;
(6) the NC film of deionized water was transferred to a vacuum drying oven at a drying temperature of 45 ℃.
Example 2
Example 2 preparation of nitrocellulose membrane solution step (1) was carried out by pouring 0.02g of hydrotalcite, 20g of N, N-dimethylacetamide, and 3g of nitrocellulose particles into a reaction apparatus, stirring for more than 4 hours at room temperature, adding 0.2g of acetone, 5g of polysulfone, and 2g of polyvinylpyrrolidone, stirring for 24-36 hours at 60 ℃, observing the content of solid in the reaction apparatus until completely dissolved; the subsequent steps were the same as in (2) to (6) of example 1.
Example 3
In example 3, the step (1) of preparing the nitrocellulose membrane solution is to pour 0.02g of hydrotalcite, 21g of N, N-dimethylacetamide and 4g of nitrocellulose particles into a reaction device for stirring, wherein the stirring time is longer than 4 hours, the stirring process is carried out at room temperature, and then 0.3g of acetone, 6g of polysulfone and 3g of polyvinylpyrrolidone are added into the reaction device for continuous stirring; the time is 24-36 h, the temperature is 60 ℃, and the content of solid matters in the reaction device is observed until the solid matters are completely dissolved; the subsequent steps were the same as in (2) to (6) of example 1.
Example 4
Example 4 nitrocellulose membrane preparation procedure (1) 0.08g hydrotalcite, 21g N, N-dimethylacetamide, 4g nitrocellulose particles were poured into a reaction apparatus and stirred for more than 4 hours at room temperature, and then 0.3g acetone, 6g polysulfone, 3g polyvinylpyrrolidone were added and stirred continuously; the time is 24-36 h, the temperature is 60 ℃, and the content of solid matters in the reaction device is observed until the solid matters are completely dissolved; the subsequent steps were the same as in (2) to (6) of example 1.
Example 5
In example 5, the step (1) of preparing the nitrocellulose membrane solution is to pour 0.08g of hydrotalcite, 20g of N, N-dimethylacetamide and 3g of nitrocellulose particles into a reaction device for stirring, wherein the stirring time is longer than 4 hours, the stirring process is carried out at room temperature, and then 0.2g of acetone, 5g of polysulfone and 2g of polyvinylpyrrolidone are added into the reaction device for continuous stirring; the time is 24-36 h, the temperature is 60 ℃, and the content of solid matters in the reaction device is observed until the solid matters are completely dissolved; the subsequent steps were the same as in (2) to (6) of example 1.
Comparative example 1
In the step (1) of preparing the nitrocellulose membrane solution in the comparative example 1, 20g of N, N-dimethylacetamide and 3g of nitrocellulose particles are poured into a reaction device and stirred for more than 4 hours, the stirring process is carried out at room temperature, and then 0.2g of acetone, 5g of polysulfone and 2g of polyvinylpyrrolidone are added and continuously stirred; the time is 24-36 h, the temperature is 60 ℃, and the content of solid matters in the reaction device is observed until the solid matters are completely dissolved; the subsequent steps were the same as in (2) to (6) of example 1.
Comparative example 2
In the comparative example 2, the step (1) of preparing the nitrocellulose membrane solution is to pour 0.1g of hydrotalcite, 20g of N, N-dimethylacetamide and 3g of nitrocellulose particles into a reaction device for stirring, the stirring time is longer than 4 hours, the process is carried out at room temperature, and then 0.2g of acetone, 5g of polysulfone and 2g of polyvinylpyrrolidone are added into the mixture for continuous stirring; the time is 24-36 h, the temperature is 60 ℃, and the content of solid matters in the reaction device is observed until the solid matters are completely dissolved; the subsequent steps were the same as in (2) to (6) of example 1.
Table 1 comparative table of performance tests of examples 1 to 5 and comparative examples 1 and 2:
in the table, the test methods and evaluation methods of the respective properties are as follows:
1. hydrophilicity: measurements were performed using a contact angle meter (SL200B, solonech.co., Ltd.);
2. the pore diameter of the NC membrane is as follows: the surface of the NC film in the different examples was characterized by inspection using a scanning electron microscope of HITACHI S4800, japan.
From the detection result, the prepared NC membrane layer has good hydrophilicity with the average pore diameter of 0.45 μm by taking the thickness of 100 μm as an example, and the porosity of the NC membrane supporting layer is improved by adding hydrotalcite.
In the embodiments 1-5, different components are added in the preparation of the NC membrane, and the hydrophilicity and the pore size of the prepared NC membrane meet the requirements of the invention on key technology, wherein the adding mass of the hydrotalcite is 0.02 g-0.08 g, and the NC membrane is flat, clean and free of impurities, and meets the requirements for preparing the NC membrane.
Compared with the examples 1-5, the test of the NC membrane prepared by the comparative example 1 without adding hydrotalcite shows that the hydrophilicity is poorer than that of the NC membrane prepared by the example 1, the apparent pore distribution of the membrane is less, and the NC membrane does not meet the use requirement of the NC membrane.
In comparison with examples 1 to 5, in comparative example 2, the hydrotalcite is added in an excessive amount, is hydrophilic, and the membrane pore size meets the requirements, but crystalline substances are generated on the membrane surface, so that the apparent quality of the NC membrane is influenced.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (12)
1. The nitrocellulose membrane is prepared from a nitrocellulose membrane solution, and is characterized in that the nitrocellulose membrane solution comprises the following raw materials in parts by weight:
2. the nitrocellulose membrane of claim 1, wherein the solvent comprises one or two of N, N-dimethylformamide, N-dimethylacetamide and any weight ratio.
3. The nitrocellulose membrane of claim 1, wherein the cosolvent comprises one or two of acetone and butanone in any weight ratio.
4. A nitrocellulose membrane according to claim 1, wherein the non-solvent comprises one or both of polyvinylpyrrolidone and cross-linked polyvinylpyrrolidone in any weight ratio.
5. A nitrocellulose membrane according to claim 1, wherein the forming agent comprises one or more of polysulfone, polyarylsulfone and polyethersulfone.
6. The method for producing a nitrocellulose membrane according to any one of claims 2 to 5, comprising the steps of:
preparing a nitrocellulose membrane solution according to the proportion of each substance;
step two, defoaming the nitrocellulose membrane solution obtained in the step one to obtain a nitrocellulose membrane casting solution;
step three, performing film scraping forming on the defoamed nitrocellulose membrane casting solution in the step two, and scraping a film on a clean toughened glass plate by using a scraper tool;
step four, shaping the nitrocellulose membrane formed by scraping in the step three, putting the shaped nitrocellulose membrane into a gel bath with a fixed temperature, and treating the shaped nitrocellulose membrane through the gel bath to obtain the shaped nitrocellulose membrane;
and step five, drying the shaped nitrocellulose membrane obtained in the step four to obtain a finished nitrocellulose membrane product.
7. The method for preparing a nitrocellulose membrane according to claim 6, wherein in the step one, the stirring temperature is between 60 and 65 ℃, and the stirring time is longer than 24 hours.
8. The method for preparing a nitrocellulose membrane of claim 6, wherein the nitrocellulose membrane solution needs to be defoamed by standing for more than 24 hours.
9. The method for preparing a nitrocellulose membrane of claim 6, wherein the ethanol content of the gel bath is 30-40%, the temperature is 30-35 ℃, and the time is more than 1 min.
10. The method of claim 6, wherein the nitrocellulose membrane is separated from the gel bath and left in deionized water for more than 4 hours.
11. The method for preparing a nitrocellulose membrane of claim 10, wherein the nitrocellulose membrane is left in deionized water, and after being left, the nitrocellulose membrane needs to be taken out and dried at a temperature of 44-50 ℃.
12. The method for preparing a nitrocellulose membrane according to claim 7, wherein the preparing of the nitrocellulose membrane solution comprises the following steps:
mixing the solvent, the cellulose nitrate particles and the hydrotalcite in proportion, and then stirring at room temperature;
and step two, adding the cosolvent, the forming agent and the non-solvent into the mixed solution, and continuously stirring at the stirring temperature of 60-65 ℃ for 24-36 hours.
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| CN116731563A (en) * | 2023-05-22 | 2023-09-12 | 北京北方世纪纤维素技术开发有限公司 | Flexible modified nitrocellulose casting solution, nitrocellulose membrane, preparation method and application thereof |
| CN116731399A (en) * | 2023-05-22 | 2023-09-12 | 稳健医疗(武汉)有限公司 | High-solid-content nitrocellulose casting solution, nitrocellulose membrane, preparation method and application thereof |
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| CN116731399A (en) * | 2023-05-22 | 2023-09-12 | 稳健医疗(武汉)有限公司 | High-solid-content nitrocellulose casting solution, nitrocellulose membrane, preparation method and application thereof |
| CN116731563B (en) * | 2023-05-22 | 2024-03-01 | 北京北方世纪纤维素技术开发有限公司 | Flexible modified nitrocellulose casting solution, nitrocellulose membrane, preparation method and application thereof |
| CN116731399B (en) * | 2023-05-22 | 2024-04-02 | 稳健医疗(武汉)有限公司 | High-solid-content nitrocellulose casting solution, nitrocellulose membrane, preparation method and application thereof |
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