CN102008901B - Preparation method of multifunctional water treatment nano material composite membrane - Google Patents
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000012528 membrane Substances 0.000 title claims abstract description 83
- 239000002131 composite material Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 68
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 58
- 238000010612 desalination reaction Methods 0.000 claims abstract description 10
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 239000000178 monomer Substances 0.000 claims description 104
- 239000002904 solvent Substances 0.000 claims description 80
- 239000000243 solution Substances 0.000 claims description 71
- 239000002994 raw material Substances 0.000 claims description 63
- 238000012695 Interfacial polymerization Methods 0.000 claims description 61
- 239000012985 polymerization agent Substances 0.000 claims description 51
- 239000004094 surface-active agent Substances 0.000 claims description 51
- 239000000843 powder Substances 0.000 claims description 50
- 239000012074 organic phase Substances 0.000 claims description 49
- 239000000203 mixture Substances 0.000 claims description 48
- 238000002156 mixing Methods 0.000 claims description 43
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 30
- 239000012071 phase Substances 0.000 claims description 29
- 239000007864 aqueous solution Substances 0.000 claims description 27
- 239000003795 chemical substances by application Substances 0.000 claims description 27
- 230000003213 activating effect Effects 0.000 claims description 25
- 239000003054 catalyst Substances 0.000 claims description 24
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 24
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- 239000004745 nonwoven fabric Substances 0.000 claims description 20
- 238000002791 soaking Methods 0.000 claims description 20
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- QFTYSVGGYOXFRQ-UHFFFAOYSA-N dodecane-1,12-diamine Chemical compound NCCCCCCCCCCCCN QFTYSVGGYOXFRQ-UHFFFAOYSA-N 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 14
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 229920002492 poly(sulfone) Polymers 0.000 claims description 11
- 239000011780 sodium chloride Substances 0.000 claims description 11
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 10
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 10
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 9
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 8
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 8
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 8
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- 239000004695 Polyether sulfone Substances 0.000 claims description 7
- 229920002873 Polyethylenimine Polymers 0.000 claims description 7
- 239000012948 isocyanate Substances 0.000 claims description 7
- 150000002576 ketones Chemical class 0.000 claims description 7
- 229920006393 polyether sulfone Polymers 0.000 claims description 7
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- UENRXLSRMCSUSN-UHFFFAOYSA-N 3,5-diaminobenzoic acid Chemical compound NC1=CC(N)=CC(C(O)=O)=C1 UENRXLSRMCSUSN-UHFFFAOYSA-N 0.000 claims description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 5
- 125000003118 aryl group Chemical group 0.000 claims description 5
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical compound ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 claims description 5
- FDQSRULYDNDXQB-UHFFFAOYSA-N benzene-1,3-dicarbonyl chloride Chemical compound ClC(=O)C1=CC=CC(C(Cl)=O)=C1 FDQSRULYDNDXQB-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- CMDGQTVYVAKDNA-UHFFFAOYSA-N propane-1,2,3-triol;hydrate Chemical compound O.OCC(O)CO CMDGQTVYVAKDNA-UHFFFAOYSA-N 0.000 claims description 5
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 5
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 238000007654 immersion Methods 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000007790 scraping Methods 0.000 claims 2
- 239000013535 sea water Substances 0.000 abstract description 3
- 229940079593 drug Drugs 0.000 abstract 1
- 239000003814 drug Substances 0.000 abstract 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- 210000004379 membrane Anatomy 0.000 description 51
- 239000010408 film Substances 0.000 description 35
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 12
- 150000003839 salts Chemical class 0.000 description 6
- 150000004984 aromatic diamines Chemical class 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 210000002469 basement membrane Anatomy 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a preparation method of a multifunctional water treatment nano material composite membrane, which comprises the steps of: carrying out high-temperature sintering and quenching treatment and superfine crushing on a plurality of metal oxides to prepare a nano framework material; and then carrying out multiple polymerization on the nano framework material with materials of a high polymer and the like to prepare an inorganic-organic multifunctional water treatment composite membrane. The composite membrane can be widely applied to equipment and projects in the industrial fields of desalination of sea water, desalination of brackish water, water treatment, electrons and medicines, has greatly reduced preparation cost and operation cost, and has remarkable social benefit and economic benefit.
Description
Technical Field
The invention relates to a preparation method of a permeation membrane for water treatment equipment, in particular to a preparation method of a multipurpose water treatment nano material composite membrane
Background
The existing seawater or brackish water desalination method mostly adopts a high molecular membrane reverse osmosis method, a thin film evaporation method, a dialysis method, a low-temperature multi-effect distillation method and the like. The above methods are very expensive in terms of the costs and engineering costs of treating the water. The key material used by the desalination membrane, namely the macromolecular organic membrane, has the defects of low water permeability, relatively small effective area, low strength, corrosion resistance, easy degradation, cracking, failure, difficult cleaning and the like. Therefore, it is not easy to be widely used and popularized.
Disclosure of Invention
The invention aims to overcome or solve the problems existing in the prior art and provide a preparation method of a multipurpose water treatment nano material composite membrane.
The object of the invention is achieved in that the method comprises: 1) preparing a nano framework material: 2) preparing a composite base film: 3) preparing a nano material composite membrane for water treatment: wherein:
1) preparing a nano framework material: the nanometer skeleton material is prepared with titania 5-12 weight portions, silica 1-8 weight portions, magnesia 15-25 weight portions, alumina 20-30 weight portions and ferric oxide 6-18 weight portions;
the preparation steps are as follows:
respectively grinding the raw materials into 500-mesh fine powder, uniformly mixing the fine powder according to the proportion, sintering the fine powder for 1 to 2 hours at 1300-1600 ℃, pouring the fine powder into a 5 to 10 percent sodium chloride aqueous solution at minus 5 ℃, rapidly cooling the fine powder, cleaning the fine powder by using clear water for desalination, drying the fine powder, and crushing the fine powder into fine powder by using a superfine crusher, wherein the granularity of the fine powder is 5 to 10 nanometers, so as to obtain a nanometer framework material for later use;
2) the composite base film is prepared from the following raw materials in parts by weight:
0.1-6 parts of nano framework material, 1-30 parts of film forming agent, 45-100 parts of solvent and 0.1-5 parts of surfactant; wherein,
film-forming agent: is one or more of polyethylene glycol, polyethyleneimine, polysulfone, sulfonated polysulfone and sulfonated polyether sulfone ketone.
Solvent: is one or a mixture of more than two of pure water, isopropanol, N-dimethylacetamide, ethanol and N, N-dimethylformamide;
surfactant (b): is one or a mixture of more than two of dodecyl diamine, sodium dodecyl sulfonate and sodium dodecyl sulfate;
the preparation steps are as follows: weighing the nano-framework material, the film forming agent, the solvent and the surfactant according to a proportion, adding the nano-framework material, the film forming agent, the solvent and the surfactant into a container, uniformly stirring, controlling the temperature to be 40 ℃, uniformly coating the nano-framework material on a non-woven fabric carrier with the thickness of 20-120 micrometers, soaking the non-woven fabric carrier in 10% ethanol water solution for 2 minutes, soaking the non-woven fabric carrier in 35% glycerol water solution for 20 minutes, and finally rinsing the non-woven fabric carrier in clean water for 20 minutes to obtain a composite base film which is;
3) preparing a water treatment nano material composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; a membrane interface activating solution, wherein:
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 5-30 parts of a water-phase monomer; 0.1-5 parts of a surfactant; 0.5-5 parts of a catalyst; 100 parts of a solvent; wherein:
water-phase monomer: is one or a mixture of more than two of m-phenylenediamine, aromatic diamine or aromatic triamine, 5-sulfoacid group m-phenylenediamine, polyethyleneimine or dodecyl diamine;
surfactant (b): is one or a mixture of more than two of dodecyl diamine, sodium dodecyl sulfonate or sodium dodecyl sulfonate;
catalyst: is one or the mixture of more than two of sulfuric acid, hexadecyl trimethyl ammonium chloride or 3, 5 diaminobenzoic acid;
solvent: is deionized water;
the preparation steps are as follows: adding a water phase monomer, a surfactant and a catalyst into a solvent according to a proportion and uniformly mixing for later use;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
0.1-5 parts of organic phase monomer; 100 parts of a solvent; wherein:
organic phase monomer: is one or the mixture of more than two of trimesoyl chloride, isophthaloyl dichloride or 5-isocyanate isophthaloyl dichloride;
solvent: is one or a mixture of more than two of deionized water, isopropanol or N, N-dimethylacetamide, isooctane, ethanol or N-hexane or N, N-dimethylformamide;
the preparation steps are as follows:
weighing organic phase monomers according to the proportion, adding the organic phase monomers into a solvent, and uniformly stirring for later use;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the preparation method of the water treatment nano material composite membrane comprises the following steps:
(1) immersing one side of the composite base film obtained in the step 2) into a water-phase monomer interfacial polymerization agent solution for immersion for 5-50 minutes, controlling the temperature at 20 ℃, taking out, drying the surface by using hot air at 30-90 ℃, immersing into an organic monomer interfacial polymerization agent solution for interfacial polymerization for 5-60 seconds, controlling the reaction temperature at 15-25 ℃, taking out, drying in the air for 2 minutes in the shade, controlling the temperature at 20 ℃, and then putting into an oven for heat treatment at 40-120 ℃ for 1-50 minutes to obtain an interfacial polymerization composite film for later use;
(2) and soaking the interface polymerization composite membrane in deionized water at normal temperature to remove the solvent for 30 minutes, soaking in membrane interface activating solution for 30 minutes, rinsing with deionized water at normal temperature for three times to obtain the finished product water treatment nano material composite membrane, and storing the prepared membrane in a 1% sodium bisulfite solution.
The invention has the following excellent effects: the composite nano material film is prepared by compounding inorganic nano material and organic polymer material, and the compounding of the composite nano material film embodies a new material integrating multiple special properties and effects of inorganic-organic nano particles. The preparation method has the characteristics of both inorganic films and organic films, and provides the preparation method of the novel material which has good stability, high strength and efficiency, corrosion resistance, difficult degradation and high sensitivity, and can be widely applied to the fields of seawater and brackish water desalination, water treatment, environmental protection, national defense science and technology and the like.
Detailed Description
Example 1:
1) preparing a nano framework material: the nanometer skeleton material is prepared from the following raw materials, by weight, 5 parts of titanium oxide, 1 part of silicon oxide, 15 parts of magnesium oxide, 20 parts of aluminum oxide and 6 parts of ferric oxide;
the preparation steps are as follows:
respectively grinding the raw materials into 500-mesh fine powder, uniformly mixing the fine powder according to the proportion, sintering the fine powder for 1 to 2 hours at 1300-1600 ℃, pouring the fine powder into a 5 to 10 percent sodium chloride aqueous solution at minus 5 ℃, rapidly cooling the fine powder, cleaning the fine powder by using clear water for desalination, drying the fine powder, and crushing the fine powder into fine powder by using a superfine crusher, wherein the granularity of the fine powder is 5 to 10 nanometers, so as to obtain a nanometer framework material for later use;
2) the composite base film is prepared from the following raw materials in parts by weight:
1 part of nano framework material, 1 part of film forming agent, 45 parts of solvent and 0.1 part of surfactant; wherein,
the film forming agent is a mixture of polyethylene glycol, polyethyleneimine, polysulfone, sulfonated polysulfone and sulfonated polyether sulfone ketone, and the mixing ratio is 1: 1.
The solvent is a mixture of pure water, isopropanol and N, N-dimethylacetamide, and the mixing ratio is 1: 1;
the surfactant is dodecyl diamine, sodium dodecyl sulfonate, or sodium dodecyl sulfate;
the preparation steps are as follows: weighing the nano-framework material, the film forming agent, the solvent and the surfactant according to a proportion, adding the nano-framework material, the film forming agent, the solvent and the surfactant into a container, uniformly stirring, controlling the temperature to be 40 ℃, uniformly coating the nano-framework material on a non-woven fabric carrier with the thickness of 20-120 micrometers, soaking the non-woven fabric carrier in 10% ethanol water solution for 2 minutes, soaking the non-woven fabric carrier in 35% glycerol water solution for 20 minutes, and finally rinsing the non-woven fabric carrier in clean water for 20 minutes to obtain a composite base film which is;
3) preparing a water treatment nano material composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; a membrane interface activating solution, wherein:
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 5 parts of a water-phase monomer; 0.1 part of surfactant; 0.5 part of a catalyst; 100 parts of a solvent; wherein:
water-phase monomer: is a mixture of aromatic diamine and aromatic triamine; the mixing ratio is 1: 1;
surfactant (b): is dodecyl diamine;
catalyst: is sulfuric acid;
solvent: is deionized water;
the preparation steps are as follows: adding a water phase monomer, a surfactant and a catalyst into a solvent according to a proportion and uniformly mixing for later use;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
0.1 part of organic phase monomer; 100 parts of a solvent; wherein:
organic phase monomer: is trimesoyl chloride;
solvent: is deionized water;
the preparation steps are as follows:
weighing organic phase monomers according to the proportion, adding the organic phase monomers into a solvent, and uniformly stirring for later use;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the preparation method of the water treatment nano material composite membrane comprises the following steps:
(1) immersing one side of the composite base film obtained in the step 2) into a water-phase monomer interfacial polymerization agent solution for immersion for 5-50 minutes, controlling the temperature at 20 ℃, taking out, drying the surface by using hot air at 30-90 ℃, immersing into an organic monomer interfacial polymerization agent solution for interfacial polymerization for 5-60 seconds, controlling the reaction temperature at 15-25 ℃, taking out, drying in the air for 2 minutes in the shade, controlling the temperature at 20 ℃, and then putting into an oven for heat treatment at 40-120 ℃ for 1-50 minutes to obtain an interfacial polymerization composite film for later use;
(2) and soaking the interface polymerization composite membrane in deionized water at normal temperature to remove the solvent for 30 minutes, soaking in membrane interface activating solution for 30 minutes, rinsing with deionized water at normal temperature for three times to obtain the finished product water treatment nano material composite membrane, and storing the prepared membrane in a 1% sodium bisulfite solution.
The obtained composite membrane is intercepted and separated by 32000ppm sodium chloride solution, and the salt rejection rate is 99.9%.
Example 2
1) Preparing a nano framework material: the nanometer skeleton material is prepared from the following raw materials, by weight, 12 parts of titanium oxide, 8 parts of silicon oxide, 25 parts of magnesium oxide, 30 parts of aluminum oxide and 18 parts of ferric oxide;
the preparation procedure was the same as in example 1.
2) The composite base film is prepared from the following raw materials in parts by weight:
0.1 part of nano framework material, 16 parts of film forming agent, 100 parts of solvent and 0.1 part of surfactant;
wherein:
the film forming agent is the mixture of polysulfone, sulfonated polysulfone and sulfonated polyether sulfone ketone in the mixing ratio of 1 to 1.
The solvent is a mixture of ethanol and N, N-dimethylformamide; the mixing ratio is 1: 1.
The surfactant is dodecyl diamine, sodium dodecyl sulfonate, or sodium dodecyl sulfate; the mixing ratio is 1: 1.
The preparation procedure was the same as in example 1.
3) Preparing a water treatment nano material composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; a membrane interface activating solution, wherein:
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 20 parts of water-phase monomers; 0.15 part of a surfactant; 0.1 part of catalyst; 100 parts of a solvent; wherein:
water-phase monomer: is a mixture of m-phenylenediamine and 5-sulfoacid m-phenylenediamine, and the mixing ratio is 1: 1;
surfactant (b): is a mixture of sodium dodecyl sulfate and sodium dodecyl sulfate, and the mixing ratio is 1: 1;
catalyst: is a mixture of hexadecyl trimethyl ammonium chloride and 3, 5 diaminobenzoic acid, and the mixing ratio is 1: 1;
solvent: is deionized water;
the preparation procedure was the same as in example 1;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
0.15 part of organic phase monomer; 100 parts of a solvent; wherein:
organic phase monomer: is a mixture of isophthaloyl dichloride and 5-isocyanate isophthaloyl dichloride with the mixing ratio of 1: 1;
solvent: is a mixture of N, N-dimethylacetamide and hexane with the mixing ratio of 1: 1;
the preparation procedure was the same as in example 1;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the preparation procedure of the water treatment nano-material composite membrane is the same as that of example 1.
The obtained composite membrane is intercepted and separated by 32000ppm sodium chloride solution, and the salt rejection rate is 99.7%.
Example 3
1) Preparing a nano framework material:
the nanometer skeleton material is prepared from the following raw materials, by weight, 10 parts of titanium oxide, 6 parts of silicon oxide, 22 parts of magnesium oxide, 28 parts of aluminum oxide and 16 parts of ferric oxide;
the preparation procedure was the same as in example 1;
2) the composite base film is prepared from the following raw materials in parts by weight:
0.15 part of nano framework material, 20 parts of film forming agent, 80 parts of solvent and 3 parts of surfactant;
wherein:
the film forming agent is a mixture of sulfonated polysulfone and sulfonated polyether sulfone ketone, and the mixing ratio is 1: 1;
the solvent is a mixture of pure water, isopropanol and N, N-dimethylformamide with the mixing ratio of 1: 1;
the surfactant is a mixture of dodecyl diamine, sodium dodecyl sulfonate and sodium dodecyl sulfate, and the mixing ratio is 1: 1;
the preparation procedure was the same as in example 1;
3) preparing a water treatment composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; the membrane interface activating solution is used for activating the membrane interface,
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 5-30 parts of a water-phase monomer; 0.1-5 parts of a surfactant; 0.5-5 parts of a catalyst; 100 parts of a solvent; wherein:
water-phase monomer: is a mixture of m-phenylenediamine and dodecyl diamine, and the mixing ratio is 1: 1;
surfactant (b): is a mixture of dodecyl diamine and sodium dodecyl sulfonate with the mixing ratio of 1: 1;
catalyst: cetyl trimethyl ammonium chloride;
solvent: is deionized water;
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 20 parts of water-phase monomers; 3 parts of a surfactant; 3 parts of a catalyst; 10 parts of a solvent;
wherein: organic phase monomer: is a mixture of trimesoyl chloride and 5-isocyanate isophthalic acid chloride, and the mixing ratio is 1: 1;
solvent: is a mixture of isopropanol, hexane and N, N-dimethylformamide, and the mixing ratio is 1: 1;
the preparation procedure was the same as in example 1;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
0.3 part of organic phase monomer; 100 parts of a solvent;
wherein: organic phase monomer: 5-isocyanate isophthaloyl chloride;
solvent: is a mixture of hexane and n-hexane, and the mixing ratio is 1: 1;
the preparation procedure was the same as in example 1;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the water treatment composite membrane was prepared in the same manner as in example 1.
The obtained composite membrane is intercepted and separated by 32000ppm sodium chloride solution, and the salt rejection rate is 99.5%.
Example 4
1) Preparing a nano framework material:
the nanometer skeleton material is prepared with titanium oxide 8-10 weight portions, silicon oxide 3-6 weight portions, magnesium oxide 22 weight portions, aluminum oxide 28 weight portions and ferric oxide 16 weight portions;
the preparation procedure was the same as in example 1;
2) the composite base film is prepared from the following raw materials in parts by weight:
6 parts of a nano framework material, 25 parts of a film forming agent, 80 parts of a solvent and 3 parts of a surfactant;
wherein,
the film forming agent is a mixture of polyester and polyethyleneimine, and the mixing ratio is 1: 1.
The solvent is a mixture of pure water, isopropanol, hexane and N, N-dimethylformamide with the mixing ratio of 1: 1;
the surfactant is sodium lauryl sulfate;
the preparation procedure was the same as in example 1;
3) preparing a water treatment composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent aqueous solution; the interfacial activation liquid of the basement membrane,
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 20 parts of water-phase monomers; 3 parts of a surfactant; 3 parts of a catalyst; 10 parts of a solvent;
wherein:
water-phase monomer: is an aromatic diamine or an aromatic triamine;
surfactant (b): is sodium dodecyl sulfate;
catalyst: is a mixture of 3, 5 diaminobenzoic acid and sulfuric acid, and the mixing ratio is 1: 1;
solvent: is deionized water;
the preparation procedure was the same as in example 1;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
3 parts of organic phase monomer; 100 parts of a solvent;
wherein: organic phase monomer: is isophthaloyl dichloride;
solvent: is a mixture of N-hexane, hexane and N, N-dimethylformamide with a mixing ratio of 1: 1;
the preparation procedure was the same as in example 1;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the preparation of the water treatment nano material composite membrane is the same as that of example 1.
The obtained composite membrane is intercepted and separated by 32000ppm sodium chloride solution, and the salt rejection rate is 99.6%.
Example 5
1) Preparing a nano framework material:
the nanometer skeleton material is prepared from the following raw materials, by weight, 9 parts of titanium oxide, 4.5 parts of silicon oxide, 20 parts of magnesium oxide, 26 parts of aluminum oxide and 12 parts of ferric oxide;
the preparation procedure was the same as in example 1
2) The composite base film is prepared from the following raw materials in parts by weight:
5 parts of framework material, 22 parts of film forming agent, 75 parts of solvent and 2 parts of surfactant;
wherein,
the film forming agent is a mixture of polyethylene glycol, sulfonated polysulfone and sulfonated polyether sulfone ketone, and the mixing ratio is 1: 1.
The solvent is a mixture of isooctane, ethanol and N, N-dimethylformamide, and the mixing ratio is 1: 1;
the surfactant is a mixture of dodecyl diamine and sodium dodecyl sulfate, and the mixing ratio is 1: 1;
the preparation procedure was the same as in example 1;
3) preparing a water treatment nano material composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; membrane interface activating liquid;
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 15 parts of water-phase monomers; 2.5 parts of a surfactant; 2.5 parts of a catalyst; 100 parts of a solvent;
wherein:
water-phase monomer: is a mixture of 5-sulfoisophthalic amine and dodecyl diamine;
surfactant (b): is sodium dodecyl sulfate;
catalyst: is cetyltrimethylammonium chloride;
solvent: is deionized water;
the preparation procedure was the same as in example 1;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
2.5 parts of organic phase monomer; 100 parts of a solvent;
wherein: organic phase monomer: is 5-isocyanate isophthaloyl chloride;
solvent: is N, N-dimethylformamide;
the preparation procedure was the same as in example 1;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the water treatment composite membrane was prepared as in example 1.
The obtained composite membrane is intercepted and separated by 32000ppm sodium chloride solution, and the salt rejection rate is 98.8%.
Example 6
1) Preparing a nano framework material:
the nanometer skeleton material is prepared from the following raw materials, by weight, 11 parts of titanium oxide, 7 parts of silicon oxide, 17 parts of magnesium oxide, 28 parts of aluminum oxide and 8 parts of ferric oxide;
the preparation procedure was the same as in example 1;
2) the composite base film is prepared from the following raw materials in parts by weight:
10 parts of nano framework material, 3 parts of film forming agent, 100 parts of solvent and 4 parts of surfactant;
wherein,
the film forming agent is the mixture of polyethyleneimine, sulfonated polysulfone and sulfonated polyether sulfone ketone, and the mixing ratio is 1: 1.
The solvent is a mixture of isopropanol, N-dimethylacetamide and N, N-dimethylformamide with a mixing ratio of 1: 1;
the surfactant is a mixture of dodecyl diamine and sodium dodecyl sulfate, and the mixing ratio is 1: 1;
the preparation procedure was the same as in example 1;
3) preparing a water treatment nano material composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; membrane interface activating liquid;
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 8 parts of a water-phase monomer; 3 parts of a surfactant; 2 parts of a catalyst; 100 parts of a solvent;
wherein:
water-phase monomer: is a mixture of m-phenylenediamine, aromatic diamine, aromatic triamine and 5-sulfoacid group m-phenylenediamine, and the mixing ratio is 1: 1;
surfactant (b): sodium dodecyl sulfate;
catalyst: is a mixture of hexadecyl trimethyl ammonium chloride and 3, 5 diaminobenzoic acid, and the mixing ratio is 1: 1;
solvent: is deionized water;
the preparation procedure was the same as in example 1;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
2 parts of organic phase monomer; 100 parts of a solvent;
wherein: organic phase monomer: is a mixture of trimesoyl chloride, isophthaloyl dichloride and 5-isocyanate isophthalic acid dichloride, and the mixing ratio is 1: 1;
solvent: is a mixture of isooctane, ethanol, normal hexane, hexane and N, N-dimethylformamide with the mixing ratio of 1: 1;
the preparation procedure was the same as in example 1;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the preparation procedure of the water treatment composite membrane was the same as in example 1.
The obtained composite membrane is intercepted and separated by 32000ppm sodium chloride solution, and the salt rejection rate is 98.4%.
The use of the composite membrane for water treatment is the same as that of the traditional water treatment filter membrane.
In addition to the technical features described in the specification, the technology is known to those skilled in the art.
Claims (3)
1. A preparation method of a multipurpose water treatment nano material composite membrane is characterized by comprising the following steps: 1) preparing a nano framework material: 2) preparing a nano material composite base film: 3) preparing a composite membrane for water treatment: wherein:
1) preparing a nano framework material:
the nanometer skeleton material is prepared with titania 5-12 weight portions, silica 1-8 weight portions, magnesia 15-25 weight portions, alumina 20-30 weight portions and ferric oxide 6-18 weight portions;
the preparation steps are as follows:
respectively grinding the raw materials into 500-mesh fine powder, uniformly mixing the fine powder according to the proportion, sintering the fine powder for 1 to 2 hours at 1300-1600 ℃, pouring the fine powder into a 5 to 10 percent sodium chloride aqueous solution at minus 5 ℃, rapidly cooling the fine powder, cleaning the fine powder by using clear water for desalination, drying the fine powder, and crushing the fine powder into fine powder by using a superfine crusher, wherein the granularity of the fine powder is 5 to 10 nanometers, so as to obtain a nanometer framework material for later use;
2) the composite base film is prepared from the following raw materials in parts by weight:
0.1-10 parts of nano framework material, 1-30 parts of film forming agent, 45-100 parts of solvent and 0.1-5 parts of surfactant; wherein,
film-forming agent: is one or a mixture of more than two of polyethylene glycol, polyethyleneimine, polysulfone, sulfonated polysulfone and sulfonated polyether sulfone ketone;
solvent: is one or a mixture of more than two of pure water, isopropanol, N-dimethylacetamide, ethanol and N, N-dimethylformamide;
surfactant (b): is one or a mixture of more than two of dodecyl diamine, sodium dodecyl sulfonate and sodium dodecyl sulfate;
the preparation steps are as follows: weighing the nano-framework material, the film forming agent, the solvent and the surfactant according to a proportion, adding the nano-framework material, the film forming agent, the solvent and the surfactant into a container, uniformly stirring, controlling the temperature to be 40 ℃, uniformly coating the nano-framework material on a non-woven fabric carrier with the thickness of 20-120 micrometers, soaking the non-woven fabric carrier in 10% ethanol water solution for 2 minutes, soaking the non-woven fabric carrier in 35% glycerol water solution for 20 minutes, and finally rinsing the non-woven fabric carrier in clean water for 20 minutes to obtain a composite base film which is;
3) preparing a water treatment nano material composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; a membrane interface activating solution, wherein:
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 5-30 parts of a water-phase monomer; 0.1-5 parts of a surfactant; 0.1-5 parts of a catalyst; 100 parts of a solvent; wherein:
water-phase monomer: is one or a mixture of more than two of m-phenylenediamine or aromatic triamine, 5-sulfoacid group m-phenylenediamine, polyethyleneimine or dodecyl diamine;
surfactant (b): is one or the mixture of two of dodecyl diamine and dodecyl sodium sulfate;
catalyst: is one or a mixture of more than two of sulfuric acid, hexadecyl trimethyl ammonium chloride and 3, 5 diaminobenzoic acid;
solvent: is deionized water;
the preparation steps are as follows: adding a water phase monomer, a surfactant and a catalyst into a solvent according to a proportion and uniformly mixing for later use;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
0.1-5 parts of organic phase monomer; 100 parts of a solvent; wherein:
organic phase monomer: is one or the mixture of more than two of trimesoyl chloride, isophthaloyl dichloride or 5-isocyanate isophthaloyl dichloride;
solvent: is one or a mixture of more than two of deionized water, isopropanol or N, N-dimethylacetamide, isooctane, ethanol or N-hexane or N, N-dimethylformamide;
the preparation steps are as follows:
weighing organic phase monomers according to the proportion, adding the organic phase monomers into a solvent, and uniformly stirring for later use;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the preparation method of the water treatment nano material composite membrane comprises the following steps:
(1) immersing one side of the composite base film obtained in the step 2) into a water-phase monomer interfacial polymerization agent solution for immersion for 5-50 minutes, controlling the temperature at 20 ℃, taking out, drying the surface by using hot air at 30-90 ℃, immersing into an organic monomer interfacial polymerization agent solution for interfacial polymerization for 5-60 seconds, controlling the reaction temperature at 15-30 ℃, taking out, drying in the air for 2 minutes in the shade, controlling the temperature at 20 ℃, and then putting into an oven for heat treatment at 40-120 ℃ for 1-50 minutes to obtain an interfacial polymerization composite film for later use;
(2) and soaking the interface polymerization composite base membrane in deionized water at normal temperature to remove the solvent for 30 minutes, soaking in membrane interface activating solution for 30 minutes, rinsing with deionized water at normal temperature for three times to obtain the finished water treatment nano material composite membrane, and storing the prepared membrane in a 1% sodium bisulfite solution.
2. The method of claim 1,
1) preparing a nano framework material:
the nanometer skeleton material is prepared with titanium oxide 8-10 weight portions, silicon oxide 3-6 weight portions, magnesium oxide 18-22 weight portions, aluminum oxide 23-28 weight portions, and ferric oxide 8-16 weight portions;
the preparation steps are as follows:
respectively grinding the raw materials into 500-mesh fine powder, uniformly mixing the fine powder according to the proportion, sintering the fine powder for 1 to 2 hours at 1300-1600 ℃, pouring the fine powder into a 5 to 10 percent sodium chloride aqueous solution at minus 5 ℃, rapidly cooling the fine powder, cleaning the fine powder by using clear water for desalination, drying the fine powder, and crushing the fine powder into fine powder by using a superfine crusher, wherein the granularity of the fine powder is 5 to 10 nanometers, so as to obtain a nanometer framework material for later use;
2) the composite base film is prepared from the following raw materials in parts by weight:
0.1-6 parts of nano framework material, 8-25 parts of film forming agent, 60-80 parts of solvent and 1-3 parts of surfactant;
the preparation steps are as follows: weighing the nano-framework material, the film forming agent, the solvent and the surfactant according to a certain proportion, adding the nano-framework material, the film forming agent, the solvent and the surfactant into a container, uniformly stirring, controlling the temperature to be 40 ℃, uniformly scraping and coating the nano-framework material on non-woven fabrics with the thickness of 50-100 micrometers, soaking the non-woven fabrics in 10% ethanol water solution for 2 minutes, then soaking the non-woven fabrics in 35% glycerol water solution for 20 minutes, and finally rinsing the non-woven fabrics in clear water for 20 minutes to obtain a nano-material composite base film;
3) preparing a water treatment nano material composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; a membrane interface activating solution, wherein:
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 10-30 parts of a water-phase monomer; 0.1-3 parts of a surfactant; 0.1-3 parts of a catalyst; 100 parts of a solvent;
the preparation steps are as follows: adding a water phase monomer, a surfactant and a catalyst into a solvent according to a proportion and uniformly mixing for later use;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight
0.1-3 parts of organic phase monomer; 100 parts of a solvent;
the preparation steps are as follows:
weighing organic phase monomers according to the proportion, adding the organic phase monomers into a solvent, and uniformly stirring for later use;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the preparation method of the water treatment nano material composite membrane comprises the following steps:
(1) immersing one side of the composite base film obtained in the step 2) into a water-phase monomer interfacial polymerization agent solution for immersing for 10-50 minutes, controlling the temperature at 20 ℃, taking out, drying the surface by using hot air at 30-90 ℃, immersing into an organic monomer interfacial polymerization agent solution for interfacial polymerization for 5-60 seconds, controlling the reaction temperature at 15-30 ℃, taking out, drying in the air for 2 minutes in the shade, controlling the temperature at 20 ℃, and putting into an oven for heat treatment at 40-120 ℃ for 10-50 minutes to obtain an interfacial polymerization composite film for later use;
(2) and soaking the interface polymerization composite membrane in deionized water at normal temperature to remove the solvent for 30 minutes, soaking in membrane interface activating solution for 30 minutes, rinsing with deionized water at normal temperature for three times to obtain the finished product water treatment nano material composite membrane, and storing the prepared membrane in a 1% sodium bisulfite solution.
3. The method of claim 1,
1) preparing a nano framework material:
the nanometer skeleton material is prepared from the following raw materials, by weight, 9 parts of titanium oxide, 4.5 parts of silicon oxide, 20 parts of magnesium oxide, 26 parts of aluminum oxide and 12 parts of ferric oxide;
the preparation steps are as follows:
respectively grinding the raw materials into 500-mesh fine powder, uniformly mixing the fine powder according to the proportion, sintering the fine powder for 1 to 2 hours at 1300-1600 ℃, pouring the fine powder into a 5 to 10 percent sodium chloride aqueous solution at minus 5 ℃, rapidly cooling the fine powder, cleaning the fine powder by using clear water for desalination, drying the fine powder, and crushing the fine powder into fine powder by using a superfine crusher, wherein the granularity of the fine powder is 5 to 10 nanometers, so as to obtain a nanometer framework material for later use;
2) the composite base film is prepared from the following raw materials in parts by weight:
0.15 part of nano framework material, 22 parts of film forming agent, 75 parts of solvent and 2 parts of surfactant;
the preparation steps are as follows: weighing the framework material, the film forming agent, the solvent and the surfactant according to a ratio, adding the materials into a container, uniformly stirring, controlling the temperature at 40 ℃, uniformly scraping and coating the materials on non-woven fabrics with the thickness of 50-100 micrometers, soaking the non-woven fabrics in 10% ethanol water solution for 2 minutes, soaking the non-woven fabrics in 35% glycerol water solution for 20 minutes, and finally rinsing the non-woven fabrics with clear water for 20 minutes to obtain a composite base membrane which is soaked in water for later use;
3) preparing a water treatment nano material composite membrane:
the raw materials comprise: aqueous monomer interfacial polymerization agent aqueous solution; an organic phase monomer interfacial polymerization agent solution; membrane interface activating liquid;
the aqueous solution of the aqueous monomer interfacial polymerization agent is prepared from the following raw materials in parts by weight:
the raw materials comprise: 20 parts of water-phase monomers; 0.15 part of a surfactant; 0.2 part of catalyst; 100 parts of a solvent;
the preparation steps are as follows: adding a water phase monomer, a surfactant and a catalyst into a solvent according to a proportion and uniformly mixing for later use;
the organic phase monomer interfacial polymerization agent solution is prepared from the following raw materials in parts by weight;
0.15 part of organic phase monomer; 100 parts of a solvent;
the preparation steps are as follows:
weighing organic phase monomers according to the proportion, adding the organic phase monomers into a solvent, and uniformly stirring for later use;
preparation of membrane interface activating solution
60 parts of hydroxyethyl methacrylate and 40 parts of methacrylic acid are uniformly mixed for later use;
the preparation method of the water treatment nano material composite membrane comprises the following steps:
(1) immersing one side of the composite base film obtained in the step 2) into a water-phase monomer interfacial polymerization agent solution for 20-50 minutes, controlling the temperature at 20 ℃, taking out, drying the surface by using hot air at 30-90 ℃, immersing into an organic monomer interfacial polymerization agent solution for interfacial polymerization reaction for 10-60 seconds, controlling the reaction temperature at 15-25 ℃, taking out, drying in the air for 2 minutes in the shade, controlling the temperature at 20 ℃, and putting into an oven for heat treatment at 40-120 ℃ for 20-50 minutes to obtain an interfacial polymerization composite film for later use;
(2) and soaking the interface polymerization composite membrane in deionized water at normal temperature to remove the solvent for 30 minutes, soaking in membrane interface activating solution for 30 minutes, rinsing with deionized water at normal temperature for three times to obtain the finished product water treatment nano material composite membrane, and storing the prepared membrane in a 1% sodium bisulfite solution.
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| CN104475028A (en) * | 2014-11-11 | 2015-04-01 | 天津工业大学 | Novel preparation and application methods of water treatment film doped with one-dimensional-pore-passage-structured composite material |
| EP3235869B1 (en) * | 2014-12-17 | 2021-02-17 | Suzhou Institute of Nano-Tech and Nano-Bionics, Chinese Academy of Sciences | Polymer-metal compound composite ink and preparation method and use thereof |
| CN105778619B (en) * | 2014-12-17 | 2019-05-17 | 中国科学院苏州纳米技术与纳米仿生研究所 | Compound ink of polymer-nano-metal-oxide and the preparation method and application thereof |
| CN108840703A (en) * | 2018-08-16 | 2018-11-20 | 北京工业大学 | A method of desalination hydrophobic porous cordierite ceramic film is prepared by raw material low cost of high silicon industrial solid castoff |
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Effective date of registration: 20130130 Address after: 100000, Chaoyang District Road, Beijing, Jiuxianqiao, No. 20, Yi Causeway harbor, a 18 floor Patentee after: Wang Cuan Address before: 250014 Shandong Province, Lixia District of Ji'nan city by ten Road No. 12588 MINI District 202 room mansion celebrities heights Patentee before: Zhu Huifen |
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Address after: 250000 Shandong Province, Lixia District of Ji'nan city ten Yuan Dong Miao ranks No. 1 West of Building No. 203 unit Patentee after: Wang Cuan Address before: 100000, Chaoyang District Road, Beijing, Jiuxianqiao, No. 20, Yi Causeway harbor, a 18 floor Patentee before: Wang Cuan |
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Granted publication date: 20121121 Termination date: 20150928 |
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