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Solvent-resistant polymer nanofiltration membrane and its preparation method and application
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A polymer and solvent-resistant technology, applied in the field of membrane separation, can solve the problems of high membrane flux and reduced membrane flux, and achieve the effects of improving swelling resistance, improving mechanical strength, and good swelling resistance
Active Publication Date: 2021-07-13
SUZHOU UNIV
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[0006] In order to solve the problem that the membrane flux of the existing nanofiltration membrane is cross-linked, the purpose of the present invention is to provide a solvent-resistant polymer nanofiltration membrane and its preparation method and application. The polymer nanofiltration membrane of the present invention is used in various Good solvent resistance, swelling resistance and high membrane flux in polar organic solvents
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[0089] Add DURENE and DABA (total mole number is 1 mol) to 300 mL of m-cresol solution at room temperature, add 44.4 g of 6FDA in batches, stir for 24 hours to form a homogeneous solution, and then add 50 mL of anhydrous toluene. The temperature of the system was gradually raised to 200° C. and kept for 6 hours. Cool down, pour the product solution into methanol, and keep stirring. The obtained product was vacuum-dried at 120° C. for 12 hours to obtain a polyimide material.
[0090] The chemical formula and synthetic route of the polyimide copolymer (PI-COOH) containing carboxyl group in the polyimide material that forms are as figure 2 As shown, wherein, m is an integer greater than or equal to 1, n is an integer greater than or equal to 1, and n / m=10-1000:1000-10.
[0091] Take the polyimide material and dissolve it in a mixed solvent of N,N-dimethylformamide and 1,4-dioxane (10:1-1:1), stir overnight, and leave it for 24 hours to obtain 10 - 40 wt% film-forming solution...
Embodiment 1
[0098] Add DURENE (0.09mol, 14.8g) and DABA (0.01mol, 1.5g) to 300mL m-cresol solution at room temperature, add 44.4g (0.1mol) of 6FDA in batches, and stir for 24 hours until a uniform solution is formed, Then 50 mL of anhydrous toluene and catalyst quinoline were added to the mixture. The temperature of the system was gradually raised to 200° C. and kept for 6 hours. Cool down, pour the product solution into methanol, and keep stirring. The obtained product was vacuum-dried at 120°C for 12 hours to obtain the polyimide material PI-COOH 10 , the degree of polymerization (m+n) is above 300, m:n=9:1.
[0099] Take the polyimide material and dissolve it in a mixed solvent of N,N-dimethylformamide and 1,4-dioxane (3:1), stir overnight, and leave it for 24 hours to obtain a 22wt% film-forming solution.
[0100] Preparation of flat film material: adjust the height of the scraper to 300 μm, control the humidity at 30-40%, pour the film-forming solution on the glass plate for scra...
Embodiment 2
[0104] The synthesis method of the polyimide material is the same as in Example 1, except that the amount of DURENE is 0.08mol (13.1g), and the amount of DABA is 0.02mol (3.0g), to obtain the polyimide material PI-COOH 20 , the degree of polymerization (m+n) is above 300, m:n=4:1.
[0105] The preparation method of the solvent-resistant polymer nanofiltration membrane is the same as that of Example 1.
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Abstract
The invention relates to a solvent-resistant polymer nanofiltration membrane and its preparation method and application. The preparation method comprises the following steps: under the action of a catalyst, a diamine monomer and a dianhydride monomer are mixed in a first polar organic solvent Cyclization of imide occurs at 160-230°C, and polyimide is formed after the reaction is complete; diamine monomers include carboxyl-containing diamine monomers and carboxyl-free diamine monomers; polyimide Dissolving in the second polar organic solvent to form a film-forming solution with a concentration of 10wt% to 40wt%; then performing phase inversion after film-forming the film-forming solution to obtain an intermediate film; using an organic solution of a metal salt to treat the intermediate film, In order to make metal ions coordinate and cross-link with carboxyl groups in polyimide, a solvent-resistant polymer nanofiltration membrane is obtained after cross-linking; wherein, the metal salt is selected from metal salts and / or multivalent metal salts. The invention also discloses the application of the solvent-resistant polymer nanofiltration membrane in separating and / or purifying compounds in organic solutions.
Description
technical field [0001] The invention relates to the technical field of membrane separation, in particular to a solvent-resistant polymer nanofiltration membrane and its preparation method and application. Background technique [0002] Organic solvent nanofiltration (OSN) is a new nanofiltration membrane separation technology developed rapidly in recent years. Driven by a transmembrane pressure of 5-30bar, OSN can separate and purify solute molecules with a molecular weight of 200-1000Da in organic solvents through the sieving effect of nanofiltration membrane pores. OSN technology has important and extensive applications in homologue separation, drug purification, dye separation, solvent recovery, etc., and has special significance in petrochemical, pharmaceutical, food, textile and other fields. However, commonly used nanofiltration membranes are mainly used in aqueous solution systems, and the membrane materials used in them have poor tolerance to organic solvents and are...
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