CN114534520A - High-temperature-resistant modified filter membrane - Google Patents
High-temperature-resistant modified filter membrane Download PDFInfo
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- CN114534520A CN114534520A CN202210172010.8A CN202210172010A CN114534520A CN 114534520 A CN114534520 A CN 114534520A CN 202210172010 A CN202210172010 A CN 202210172010A CN 114534520 A CN114534520 A CN 114534520A
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- polyvinylidene chloride
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- 239000012528 membrane Substances 0.000 title claims abstract description 66
- 229920001328 Polyvinylidene chloride Polymers 0.000 claims abstract description 69
- 239000005033 polyvinylidene chloride Substances 0.000 claims abstract description 69
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000000853 adhesive Substances 0.000 claims abstract description 41
- 230000001070 adhesive effect Effects 0.000 claims abstract description 41
- 239000000203 mixture Substances 0.000 claims abstract description 41
- -1 polypropylene Polymers 0.000 claims abstract description 30
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000012965 benzophenone Substances 0.000 claims abstract description 28
- 239000004743 Polypropylene Substances 0.000 claims abstract description 27
- 229920001155 polypropylene Polymers 0.000 claims abstract description 27
- 239000012760 heat stabilizer Substances 0.000 claims abstract description 26
- 239000002270 dispersing agent Substances 0.000 claims abstract description 25
- 239000011256 inorganic filler Substances 0.000 claims abstract description 25
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 25
- 239000004014 plasticizer Substances 0.000 claims abstract description 25
- 229920000800 acrylic rubber Polymers 0.000 claims abstract description 19
- XBXHCBLBYQEYTI-UHFFFAOYSA-N piperidin-4-ylmethanol Chemical compound OCC1CCNCC1 XBXHCBLBYQEYTI-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000004593 Epoxy Substances 0.000 claims abstract description 9
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims abstract description 9
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 claims abstract description 9
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 41
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 35
- 239000002904 solvent Substances 0.000 claims description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 20
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 16
- QNVRIHYSUZMSGM-UHFFFAOYSA-N hexan-2-ol Chemical compound CCCCC(C)O QNVRIHYSUZMSGM-UHFFFAOYSA-N 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- BSWXAWQTMPECAK-UHFFFAOYSA-N 6,6-diethyloctyl dihydrogen phosphate Chemical compound CCC(CC)(CC)CCCCCOP(O)(O)=O BSWXAWQTMPECAK-UHFFFAOYSA-N 0.000 claims description 8
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 229920001577 copolymer Polymers 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 8
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 8
- 229920006226 ethylene-acrylic acid Polymers 0.000 claims description 8
- 239000000194 fatty acid Substances 0.000 claims description 8
- 229930195729 fatty acid Natural products 0.000 claims description 8
- 150000004665 fatty acids Chemical class 0.000 claims description 8
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000391 magnesium silicate Substances 0.000 claims description 8
- 229910052919 magnesium silicate Inorganic materials 0.000 claims description 8
- 235000019792 magnesium silicate Nutrition 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 8
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 8
- 229920001522 polyglycol ester Polymers 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 239000004408 titanium dioxide Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Natural products OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 4
- 238000006065 biodegradation reaction Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 20
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 6
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000003063 flame retardant Substances 0.000 description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- ANRQGKOBLBYXFM-UHFFFAOYSA-M phenylmagnesium bromide Chemical compound Br[Mg]C1=CC=CC=C1 ANRQGKOBLBYXFM-UHFFFAOYSA-M 0.000 description 5
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 description 4
- QILSFLSDHQAZET-UHFFFAOYSA-N diphenylmethanol Chemical compound C=1C=CC=CC=1C(O)C1=CC=CC=C1 QILSFLSDHQAZET-UHFFFAOYSA-N 0.000 description 4
- 239000012990 dithiocarbamate Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 235000019445 benzyl alcohol Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BSSMSDMDCCVWTE-UHFFFAOYSA-N 4-(benzhydryloxymethyl)piperidine Chemical compound C1CNCCC1COC(C=1C=CC=CC=1)C1=CC=CC=C1 BSSMSDMDCCVWTE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
Classifications
-
- 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
- B01D71/44—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds, not provided for in a single one of groups B01D71/26-B01D71/42
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/10—Biological treatment of water, waste water, or sewage
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a high-temperature-resistant modified filter membrane, which comprises a polypropylene base membrane and a modified membrane, wherein the upper surface and the lower surface of the polypropylene base membrane are respectively coated with a layer of modified membrane, and the modified membrane comprises the following raw materials, by weight, 50-60 parts of polyvinylidene chloride, 5-6 parts of ethylene-alkyl acrylate copolymer, 5-7 parts of benzophenone, 1-3 parts of butyl lithium, 2-4 parts of 4-hydroxymethyl piperidine, 0.5-1 part of heat stabilizer, 1-3 parts of dispersant, 5-7 parts of adhesive, 0.5-1 part of inorganic filler and 2.5-3 parts of plasticizer, wherein the heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate. The polyvinylidene chloride has symmetrical performance, stronger flame retardance, corrosion resistance and biodegradation resistance, and the polyvinylidene chloride modified by the ethylene-alkyl acrylate copolymer has the effects of improving the flexibility, cold resistance and heat resistance.
Description
Technical Field
The invention relates to the technical field of filter membrane preparation, in particular to a high-temperature-resistant modified filter membrane.
Background
The filter membrane can separate solute in a solution, and with continuous improvement of science and technology, modification of the membrane becomes a main means for enhancing the performance of the membrane in all aspects, the main method for modification is a physical and chemical method, and the overall performance is enhanced by introducing other high polymer resins to make up for defects.
Polyvinylidene chloride has symmetrical performance, has stronger flame retardance, corrosion resistance and biodegradation resistance, and is widely applied in the field of filter membrane preparation, but polyvinylidene chloride has the defect of poor thermal stability, and needs to be dried and dried after membrane preparation is finished, and polyvinylidene chloride can be decomposed due to higher temperature in the drying and drying process, so that the tensile strength and the thermal stability of a product are reduced, and hydrogen chloride gas can be released, so that the quality of the membrane can be influenced, and the human body and the environment can be damaged, therefore, the high-temperature-resistant modified filter membrane and the preparation process thereof are particularly important.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant modified filter membrane and a preparation process thereof, which aim to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a high-temperature-resistant modified filter membrane comprises a polypropylene base membrane and modified membranes, wherein the upper surface and the lower surface of the polypropylene base membrane are respectively coated with a layer of the modified membrane.
Furthermore, the modified film comprises the following raw materials, by weight, 50-60 parts of polyvinylidene chloride, 5-6 parts of an ethylene-alkyl acrylate copolymer, 5-7 parts of benzophenone, 1-3 parts of butyl lithium, 2-4 parts of 4-hydroxymethyl piperidine, 0.5-1 part of a heat stabilizer, 1-3 parts of a dispersant, 5-7 parts of an adhesive, 0.5-1 part of an inorganic filler and 2.5-3 parts of a plasticizer.
Further, the heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate.
Further, the plasticizer is one or a mixture of two of dioctyl adipate and citric acid ester.
Furthermore, the adhesive is one or a mixture of two of ethylene-vinyl acetate copolymer and acrylic acid and acrylonitrile copolymer.
Further, the inorganic filler is one or a mixture of calcium carbonate, titanium dioxide and magnesium silicate.
Further, the dispersant is one or a mixture of more of triethyl hexyl phosphoric acid, methyl amyl alcohol and fatty acid polyglycol ester.
A preparation process of a high-temperature resistant modified filter membrane comprises the following steps,
(1) putting polyvinylidene chloride into a methanol solution, soaking and washing for three times, taking out, drying, and controlling the temperature to be 40-45 ℃ for later use;
(2) putting the polyvinylidene chloride obtained in the step (1) into ether, adding benzophenone, completely immersing the polyvinylidene chloride in the benzophenone, carrying out ultraviolet irradiation, and drying for later use;
(3) putting the polyvinylidene chloride obtained in the step (2) into an ether solution, adding an ethylene-alkyl acrylate copolymer, carrying out ultraviolet irradiation, separating, and recovering the solvent to obtain a modified polyvinylidene chloride film;
(4) dissolving an adhesive in an organic solvent, stirring, adding a plasticizer, and stirring uniformly to obtain an adhesive solvent;
(5) adding 4-hydroxymethyl piperidine into the solvent obtained in the step (3), introducing nitrogen, stirring, adding butyl lithium, stirring, reacting for 5-10min, adding deionized water, stirring, adding a heat stabilizer and an inorganic filler, stirring uniformly, adding a dispersant, stirring, adding an adhesive solvent, stirring, placing a modified polyvinylidene chloride film, standing for 1-2h, taking out, covering the upper surface and the lower surface of a polypropylene-based film, vacuum drying, baking, and obtaining the high-temperature-resistant modified filter membrane, wherein the temperature is 90-100 ℃.
Further, in the step (5), the concentration of butyl lithium added is 1.5 mol/L.
Further, in the step (2) and the step (3), nitrogen gas is required to be introduced when ultraviolet irradiation is carried out, and the irradiation time is 10-15 min.
Compared with the prior art, the invention has the following beneficial effects: polyvinylidene chloride has symmetrical performance, has stronger flame retardance, corrosion resistance and biodegradation resistance, and has the defects that polyvinylidene chloride has poor thermal stability, can be decomposed in the subsequent drying and drying processes, so that the tensile strength and the thermal stability of a product are reduced, and hydrogen chloride gas can be released to cause damage to human bodies and the environment.
The invention selects a mode of ultraviolet irradiation to modify polyvinylidene chloride, uses benzophenone as a photoinitiator to graft an ethylene-alkyl acrylate copolymer onto polyvinylidene chloride, improves the tensile strength and cold and heat resistance of a membrane, obtains alcohol substances mainly including benzyl alcohol which can be dissolved in diethyl ether due to the fact that the carbonyl bond of the benzophenone is broken and absorbs hydrogen ions in the reaction, is extremely unstable under the action of high temperature and strong oxidant due to the nature of the benzyl alcohol, reduces the tensile strength, flame retardant property and heat stability of the product due to the fact that a part of the benzyl alcohol is attached to the surface of the membrane after the modification is finished, but can volatilize when reaching more than 290 ℃ due to the high boiling point of the benzyl alcohol, and can decompose the polyvinylidene chloride at 120 ℃, so that the conventional high-temperature alcohol removal method, The water mode is no longer applicable; aiming at the problem, 4-hydroxymethyl piperidine and butyl lithium are introduced, so that the 4-hydroxymethyl piperidine can absorb the benzhydryl alcohol in the presence of the butyl lithium, the content of the benzhydryl alcohol is reduced, the attachment of the benzhydryl alcohol is avoided, and the tensile strength and the thermal stability of the product are further ensured.
Meanwhile, the 4-hydroxymethyl piperidine can be used as a bactericide, and can generate 4- ((diphenyl methoxyl) methyl) piperidine in the process of absorbing the benzhydrol, and the product has excellent bactericidal performance, so that the bactericidal capacity is not reduced due to the consumption of the 4-hydroxymethyl piperidine.
Butyl lithium has strong reducibility, and the product film is corroded due to too high concentration, so that the qualification rate is reduced, and the added concentration needs to be controlled to be 1.5mol/L, and the qualification rate of the film is ensured.
After the preparation, the polyvinylidene chloride is dried and baked at the temperature of 90-100 ℃, although the temperature is lower, a small part of polyvinylidene chloride is still decomposed to release hydrogen chloride gas, and the generation of the hydrogen chloride can cause the reduction of the tensile strength and the thermal stability of a product film.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the 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 embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A high-temperature-resistant modified filter membrane comprises a polypropylene base membrane and modified membranes, wherein the upper surface and the lower surface of the polypropylene base membrane are respectively coated with one layer of the modified membrane.
The modified film comprises the following raw materials, by weight, 50 parts of polyvinylidene chloride, 5 parts of an ethylene-alkyl acrylate copolymer, 5 parts of benzophenone, 1 part of butyl lithium, 2 parts of 4-hydroxymethyl piperidine, 0.5 part of a heat stabilizer, 1 part of a dispersing agent, 5 parts of an adhesive, 0.5 part of an inorganic filler and 2.5 parts of a plasticizer.
The heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate.
The plasticizer is one or a mixture of two of dioctyl adipate and citrate.
The adhesive is one or a mixture of two of ethylene-vinyl acetate copolymer and acrylic acid and acrylonitrile copolymer.
The inorganic filler is one or a mixture of calcium carbonate, titanium dioxide and magnesium silicate.
The dispersing agent is one or a mixture of triethyl hexyl phosphoric acid, methyl amyl alcohol and fatty acid polyglycol ester.
A preparation process of a high-temperature resistant modified filter membrane comprises the following steps,
(1) putting polyvinylidene chloride into a methanol solution, soaking and washing for three times, taking out, and drying at the temperature of 40 ℃ for later use;
(2) putting the polyvinylidene chloride obtained in the step (1) into ether, adding benzophenone, completely immersing the polyvinylidene chloride in the benzophenone, carrying out ultraviolet irradiation, introducing nitrogen, and drying for later use, wherein the irradiation time is 10 min;
(3) putting the polyvinylidene chloride obtained in the step (2) into an ether solution, adding an ethylene-alkyl acrylate copolymer, carrying out ultraviolet irradiation, introducing nitrogen, carrying out irradiation for 10min, separating, and recovering a solvent to obtain a modified polyvinylidene chloride film;
(4) dissolving an adhesive in an organic solvent, stirring, adding a plasticizer, and stirring uniformly to obtain an adhesive solvent;
(5) adding 4-hydroxymethyl piperidine into the solvent obtained in the step (3), introducing nitrogen, stirring, adding 1.5mol/L butyl lithium, stirring for 5min, adding deionized water, stirring, adding a heat stabilizer and an inorganic filler, stirring uniformly, adding a dispersant, stirring, adding an adhesive solvent, stirring, adding a modified polyvinylidene chloride film, standing for 1h, taking out, covering the upper surface and the lower surface of the polypropylene-based film, vacuum drying, baking at the temperature of 90 ℃ to obtain the high-temperature-resistant modified filter film.
Example 2
A high-temperature-resistant modified filter membrane comprises a polypropylene base membrane and modified membranes, wherein the upper surface and the lower surface of the polypropylene base membrane are respectively coated with one layer of the modified membrane.
The modified film comprises the following raw materials, by weight, 55 parts of polyvinylidene chloride, 5 parts of an ethylene-alkyl acrylate copolymer, 6 parts of benzophenone, 2 parts of butyl lithium, 3 parts of 4-hydroxymethyl piperidine, 0.7 part of a heat stabilizer, 2 parts of a dispersing agent, 6 parts of an adhesive, 0.7 part of an inorganic filler and 2.8 parts of a plasticizer.
The heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate.
The plasticizer is one or a mixture of two of dioctyl adipate and citrate.
The adhesive is one or a mixture of two of ethylene-vinyl acetate copolymer and acrylic acid and acrylonitrile copolymer.
The inorganic filler is one or a mixture of calcium carbonate, titanium dioxide and magnesium silicate.
The dispersing agent is one or a mixture of triethyl hexyl phosphoric acid, methyl amyl alcohol and fatty acid polyglycol ester.
A preparation process of a high-temperature resistant modified filter membrane comprises the following steps,
(1) putting polyvinylidene chloride into a methanol solution, soaking and washing for three times, taking out, and drying at the temperature of 43 ℃ for later use;
(2) putting the polyvinylidene chloride obtained in the step (1) into ether, adding benzophenone, completely immersing the polyvinylidene chloride in the benzophenone, carrying out ultraviolet irradiation, introducing nitrogen, and drying for later use, wherein the irradiation time is 13 min;
(3) putting the polyvinylidene chloride obtained in the step (2) into an ether solution, adding an ethylene-alkyl acrylate copolymer, carrying out ultraviolet irradiation, introducing nitrogen, carrying out irradiation for 13min, separating, and recovering a solvent to obtain a modified polyvinylidene chloride film;
(4) dissolving an adhesive in an organic solvent, stirring, adding a plasticizer, and stirring uniformly to obtain an adhesive solvent;
(5) adding 4-hydroxymethyl piperidine into the solvent obtained in the step (3), introducing nitrogen, stirring, adding 1.5mol/L butyl lithium, stirring for reaction for 7min, adding deionized water, stirring, adding a heat stabilizer and an inorganic filler, stirring uniformly, adding a dispersant, stirring, adding an adhesive solvent, stirring, adding a modified polyvinylidene chloride film, standing for 1.5h, taking out, covering the upper surface and the lower surface of the polypropylene-based film, vacuum drying, baking, and keeping the temperature at 95 ℃ to obtain the high-temperature-resistant modified filter film.
Example 3
A high-temperature-resistant modified filter membrane comprises a polypropylene base membrane and modified membranes, wherein the upper surface and the lower surface of the polypropylene base membrane are respectively coated with one layer of the modified membrane.
The modified film comprises the following raw materials, by weight, 60 parts of polyvinylidene chloride, 6 parts of an ethylene-alkyl acrylate copolymer, 7 parts of benzophenone, 3 parts of butyl lithium, 4 parts of 4-hydroxymethyl piperidine, 1 part of a heat stabilizer, 3 parts of a dispersing agent, 7 parts of an adhesive, 1 part of an inorganic filler and 3 parts of a plasticizer.
The heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate.
The plasticizer is one or a mixture of two of dioctyl adipate and citrate.
The adhesive is one or a mixture of two of ethylene-vinyl acetate copolymer and acrylic acid and acrylonitrile copolymer.
The inorganic filler is one or a mixture of calcium carbonate, titanium dioxide and magnesium silicate.
The dispersing agent is one or a mixture of triethyl hexyl phosphoric acid, methyl amyl alcohol and fatty acid polyglycol ester.
A preparation process of a high-temperature resistant modified filter membrane comprises the following steps,
(1) putting polyvinylidene chloride into a methanol solution, soaking and washing for three times, taking out, and drying at the temperature of 45 ℃ for later use;
(2) putting the polyvinylidene chloride obtained in the step (1) into ether, adding benzophenone, completely immersing the polyvinylidene chloride in the benzophenone, carrying out ultraviolet irradiation, introducing nitrogen, and drying for later use, wherein the irradiation time is 15 min;
(3) putting the polyvinylidene chloride obtained in the step (2) into an ether solution, adding an ethylene-alkyl acrylate copolymer, carrying out ultraviolet irradiation, introducing nitrogen, carrying out irradiation for 15min, separating, and recovering a solvent to obtain a modified polyvinylidene chloride film;
(4) dissolving an adhesive in an organic solvent, stirring, adding a plasticizer, and stirring uniformly to obtain an adhesive solvent;
(5) adding 4-hydroxymethyl piperidine into the solvent obtained in the step (3), introducing nitrogen, stirring, adding 1.5mol/L butyl lithium, stirring, reacting for 10min, adding deionized water, stirring, adding a heat stabilizer and an inorganic filler, stirring uniformly, adding a dispersant, stirring, adding an adhesive solvent, stirring, adding a modified polyvinylidene chloride film, standing for 2h, taking out, covering the upper surface and the lower surface of the polypropylene-based film, vacuum drying, baking, and keeping the temperature at 100 ℃ to obtain the high-temperature-resistant modified filter film.
Comparative example 1
A high-temperature-resistant modified filter membrane comprises a polypropylene base membrane and modified membranes, wherein the upper surface and the lower surface of the polypropylene base membrane are respectively coated with one layer of the modified membrane.
The modified film comprises the following raw materials, by weight, 60 parts of polyvinylidene chloride, 6 parts of an ethylene-alkyl acrylate copolymer, 7 parts of benzophenone, 3 parts of butyl lithium, 4 parts of dithiocarbamate, 1 part of a heat stabilizer, 3 parts of a dispersing agent, 7 parts of an adhesive, 1 part of an inorganic filler and 3 parts of a plasticizer.
The heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate.
The plasticizer is one or a mixture of two of dioctyl adipate and citrate.
The adhesive is one or a mixture of two of ethylene-vinyl acetate copolymer and acrylic acid and acrylonitrile copolymer.
The inorganic filler is one or a mixture of calcium carbonate, titanium dioxide and magnesium silicate.
The dispersing agent is one or a mixture of triethyl hexyl phosphoric acid, methyl amyl alcohol and fatty acid polyglycol ester.
A preparation process of a high-temperature resistant modified filter membrane comprises the following steps,
(1) putting polyvinylidene chloride into a methanol solution, soaking and washing for three times, taking out, and drying at the temperature of 45 ℃ for later use;
(2) putting the polyvinylidene chloride obtained in the step (1) into ether, adding benzophenone, completely immersing the polyvinylidene chloride in the benzophenone, carrying out ultraviolet irradiation, introducing nitrogen, and drying for later use, wherein the irradiation time is 15 min;
(3) putting the polyvinylidene chloride obtained in the step (2) into an ether solution, adding an ethylene-alkyl acrylate copolymer, carrying out ultraviolet irradiation, introducing nitrogen, carrying out irradiation for 15min, separating, and recovering a solvent to obtain a modified polyvinylidene chloride film;
(4) dissolving an adhesive in an organic solvent, stirring, adding a plasticizer, and stirring uniformly to obtain an adhesive solvent;
(5) and (3) adding dithiocarbamate into the solvent obtained in the step (3), stirring, adding butyl lithium with the concentration of 1.5mol/L, stirring, reacting for 10min, adding deionized water, stirring, adding a heat stabilizer and an inorganic filler, stirring uniformly, adding a dispersant, stirring, adding an adhesive solvent, stirring, adding a modified polyvinylidene chloride film, standing for 2h, taking out, covering the upper surface and the lower surface of the polypropylene-based film, vacuum drying, baking, and keeping the temperature at 100 ℃ to obtain the high-temperature-resistant modified filter film.
Comparative example 2
A high-temperature-resistant modified filter membrane comprises a polypropylene base membrane and modified membranes, wherein the upper surface and the lower surface of the polypropylene base membrane are respectively coated with one layer of the modified membrane.
The modified film comprises the following raw materials, by weight, 60 parts of polyvinylidene chloride, 6 parts of an ethylene-alkyl acrylate copolymer, 7 parts of benzophenone, 4 parts of 4-hydroxymethylpiperidine, 1 part of a heat stabilizer, 3 parts of a dispersing agent, 7 parts of an adhesive, 1 part of an inorganic filler and 3 parts of a plasticizer.
The heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate.
The plasticizer is one or a mixture of two of dioctyl adipate and citrate.
The adhesive is one or a mixture of two of ethylene-vinyl acetate copolymer and acrylic acid and acrylonitrile copolymer.
The inorganic filler is one or a mixture of calcium carbonate, titanium dioxide and magnesium silicate.
The dispersing agent is one or a mixture of triethyl hexyl phosphoric acid, methyl amyl alcohol and fatty acid polyglycol ester.
A preparation process of a high-temperature resistant modified filter membrane comprises the following steps,
(1) putting polyvinylidene chloride into a methanol solution, soaking and washing for three times, taking out, and drying at the temperature of 45 ℃ for later use;
(2) putting the polyvinylidene chloride obtained in the step (1) into ether, adding benzophenone, completely immersing the polyvinylidene chloride in the benzophenone, carrying out ultraviolet irradiation, introducing nitrogen, and drying for later use, wherein the irradiation time is 15 min;
(3) putting the polyvinylidene chloride obtained in the step (2) into an ether solution, adding an ethylene-alkyl acrylate copolymer, carrying out ultraviolet irradiation, introducing nitrogen, carrying out irradiation for 15min, separating, and recovering a solvent to obtain a modified polyvinylidene chloride film;
(4) dissolving an adhesive in an organic solvent, stirring, adding a plasticizer, and stirring uniformly to obtain an adhesive solvent;
(5) adding 4-hydroxymethyl piperidine into the solvent obtained in the step (3), stirring, reacting for 10min, adding deionized water, stirring, adding a heat stabilizer and an inorganic filler, stirring uniformly, adding a dispersant, stirring, adding an adhesive solvent, stirring, adding a modified polyvinylidene chloride film, standing for 2h, taking out, covering the upper surface and the lower surface of a polypropylene-based film, drying in vacuum, baking, and keeping the temperature at 100 ℃ to obtain the high-temperature-resistant modified filter membrane.
Comparative example 3
A high-temperature-resistant modified filter membrane comprises a polypropylene base membrane and modified membranes, wherein the upper surface and the lower surface of the polypropylene base membrane are respectively coated with one layer of the modified membrane.
The modified film comprises the following raw materials, by weight, 60 parts of polyvinylidene chloride, 6 parts of an ethylene-alkyl acrylate copolymer, 7 parts of benzophenone, 3 parts of phenyl magnesium bromide, 4 parts of 4-hydroxymethyl piperidine, 1 part of a heat stabilizer, 3 parts of a dispersing agent, 7 parts of an adhesive, 1 part of an inorganic filler and 3 parts of a plasticizer.
The heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate.
The plasticizer is one or a mixture of two of dioctyl adipate and citrate.
The adhesive is one or a mixture of two of ethylene-vinyl acetate copolymer and acrylic acid and acrylonitrile copolymer.
The inorganic filler is one or a mixture of calcium carbonate, titanium dioxide and magnesium silicate.
The dispersing agent is one or a mixture of triethyl hexyl phosphoric acid, methyl amyl alcohol and fatty acid polyglycol ester.
A preparation process of a high-temperature resistant modified filter membrane comprises the following steps,
(1) putting polyvinylidene chloride into a methanol solution, soaking and washing for three times, taking out, and drying at the temperature of 45 ℃ for later use;
(2) putting the polyvinylidene chloride obtained in the step (1) into ether, adding benzophenone, completely immersing the polyvinylidene chloride in the benzophenone, carrying out ultraviolet irradiation, introducing nitrogen, and drying for later use, wherein the irradiation time is 15 min;
(3) putting the polyvinylidene chloride obtained in the step (2) into an ether solution, adding an ethylene-alkyl acrylate copolymer, carrying out ultraviolet irradiation, introducing nitrogen, carrying out irradiation for 15min, separating, and recovering a solvent to obtain a modified polyvinylidene chloride film;
(4) dissolving an adhesive in an organic solvent, stirring, adding a plasticizer, and stirring uniformly to obtain an adhesive solvent;
(5) adding 4-hydroxymethyl piperidine into the solvent obtained in the step (3), introducing nitrogen, stirring, adding phenyl magnesium bromide, stirring, reacting for 10min, adding deionized water, stirring, adding a heat stabilizer and an inorganic filler, stirring uniformly, adding a dispersant, stirring, adding an adhesive solvent, stirring, adding a modified polyvinylidene chloride film, standing for 2h, taking out, covering the upper surface and the lower surface of the polypropylene-based film, vacuum drying, baking, and keeping the temperature at 100 ℃ to obtain the high-temperature-resistant modified filter film.
Experiment of
A control experiment was conducted by using the control at the site of example 3, including comparative example 1, comparative example 2, and comparative example 3, in which dithiocarbamate was used as the bactericide in comparative example 1, butyl lithium was not added in comparative example 2, and phenylmagnesium bromide was used in comparative example 3.
3 parts of each of example 1, example 2, example 3, comparative example 1, comparative example 2 and comparative example 3 were subjected to tensile strength test by GB/T1040-2006, heat shrinkage test by GB/T13542.2-2009 method and flame retardancy test by GB2408-80, and the results were as follows,
watch 1
The tensile strength, heat shrinkage rate and flame retardant property of comparative example 1 were lower than those of examples 1, 2 and 3 at the same thickness because the degerming agent in comparative example 1 used dithiocarbamate, so that excessive benzophenone remained on the solvent and film surface, and the tensile strength, heat shrinkage rate and flame retardant property were lowered.
Under the same thickness, the tensile strength, the thermal shrinkage rate and the flame retardant performance of comparative example 2 and comparative example 3 are lower than those of example 1, example 2 and example 3, because no butyl lithium is added in comparative example 2, phenyl magnesium bromide is used in comparative example 3, the butyl lithium is used as a catalyst on one hand and can absorb hydrogen chloride on the other hand, so that the tensile strength, the thermal shrinkage rate and the flame retardant performance of the product are ensured, the butyl lithium is not contained in comparative example 2, so that the performance of various aspects of the product is reduced, and the phenyl magnesium bromide is used instead in comparative example 3 and can only be used as a catalyst and cannot absorb hydrogen chloride, so that the tensile strength, the thermal shrinkage rate and the flame retardant performance of a product film are reduced.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. A high temperature resistant modified filter membrane is characterized in that: the polypropylene film comprises a polypropylene base film and modified films, wherein the upper surface and the lower surface of the polypropylene base film are respectively coated with a layer of modified film;
the modified film comprises the following raw materials, by weight, 50 parts of polyvinylidene chloride, 5 parts of an ethylene-alkyl acrylate copolymer, 5 parts of benzophenone, 1 part of butyl lithium, 2 parts of 4-hydroxymethyl piperidine, 0.5 part of a heat stabilizer, 1 part of a dispersing agent, 5 parts of an adhesive, 0.5 part of an inorganic filler and 2.5 parts of a plasticizer;
the heat stabilizer is one or a mixture of barium stearate, lithium stearate and epoxy stearate; the plasticizer is one or a mixture of dioctyl adipate and citric acid ester; the adhesive is one or a mixture of two of ethylene-vinyl acetate copolymer and acrylic acid and acrylonitrile copolymer; the inorganic filler is one or a mixture of calcium carbonate, titanium dioxide and magnesium silicate; the dispersing agent is one or a mixture of triethyl hexyl phosphoric acid, methyl amyl alcohol and fatty acid polyglycol ester;
the preparation process of the filter membrane comprises the following steps:
(1) putting polyvinylidene chloride into a methanol solution, soaking and washing for three times, taking out, and drying at the temperature of 40 ℃ for later use;
(2) putting the polyvinylidene chloride obtained in the step (1) into ether, adding benzophenone, completely immersing the polyvinylidene chloride in the benzophenone, carrying out ultraviolet irradiation, introducing nitrogen, and drying for later use, wherein the irradiation time is 10 min;
(3) putting the polyvinylidene chloride obtained in the step (2) into an ether solution, adding an ethylene-alkyl acrylate copolymer, carrying out ultraviolet irradiation, introducing nitrogen, carrying out irradiation for 10min, separating, and recovering a solvent to obtain a modified polyvinylidene chloride film;
(4) dissolving an adhesive in an organic solvent, stirring, adding a plasticizer, and stirring uniformly to obtain an adhesive solvent;
(5) adding 4-hydroxymethyl piperidine into the solvent obtained in the step (3), introducing nitrogen, stirring, adding 1.5mol/L butyl lithium, stirring for 5min, adding deionized water, stirring, adding a heat stabilizer and an inorganic filler, stirring uniformly, adding a dispersant, stirring, adding an adhesive solvent, stirring, adding a modified polyvinylidene chloride film, standing for 1h, taking out, covering the upper surface and the lower surface of the polypropylene-based film, vacuum drying, baking at the temperature of 90 ℃ to obtain the high-temperature-resistant modified filter film.
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