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Preparation method of ethanol pervaporation hybrid film used for removing methyl alcohol in wastewater

A technology of pervaporation and hybrid membrane, applied in chemical instruments and methods, osmotic/dialysis water/sewage treatment, semi-permeable membrane separation, etc. Problems such as poor temperature resistance, to achieve the effects of low cost, simple preparation method and high temperature resistance

Inactive Publication Date: 2011-04-27
SHANDONG TIANWEI MEMBRANE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Chinese patent ZL200710040764.3 discloses a hydrophilic organic-inorganic composite pervaporation separation membrane and its preparation method and application. Using an inorganic ceramic membrane as a The method of ring reaction is used to prepare organic-inorganic composite pervaporation separation membrane; however, this method prepares a pure organic polymer separation layer on the surface of the ceramic membrane, which has the disadvantage of poor temperature resistance of the membrane and can only be used for 95% high-concentration methanol, etc. The dehydration of alcohols is a preferential water-permeable hybrid membrane, which has limited application value in the field of alcohol-containing wastewater treatment
[0003] Chinese patent 200810060981.3 discloses a method for preparing a pervaporation membrane for separating alcohol-water systems, using polydimethylsiloxane as a raw material to crosslink silicate compounds; the pervaporation membrane prepared by this method can be used for Concentration of 8% methanol and other alcoholic aqueous solutions preferentially penetrates alcohol hybrid membranes, but there are disadvantages such as low temperature resistance of the membranes, the use of highly toxic solvents in the preparation process, single types of raw materials, and limited sources.

Method used

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  • Preparation method of ethanol pervaporation hybrid film used for removing methyl alcohol in wastewater
  • Preparation method of ethanol pervaporation hybrid film used for removing methyl alcohol in wastewater
  • Preparation method of ethanol pervaporation hybrid film used for removing methyl alcohol in wastewater

Examples

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Embodiment 1

[0021] Embodiment 1: prepare the product for Pervaporation Permeabilization Alcohol Hybrid Membrane for Removing Methanol from Wastewater

[0022] In an air or nitrogen atmosphere, add 3 g of polyvinyl alcohol (referred to as PVA) with a molecular weight of 1750 to a 250 mL container equipped with a stirrer, add water to prepare a 3% polyvinyl alcohol aqueous solution; at 90 ° C Stir continuously until PVA is completely dissolved, continue stirring for 5h, add 3mL of silane coupling agent N-β-aminoethyl-γ-aminopropyltrimethoxysilane (A-1120) and 1mL of dilute hydrochloric acid with a concentration of 0.1M , carry out sol-gel reaction at 30°C for 24 hours, continue to stir for 10 hours, then add dropwise 3 mL of acetaldehyde solution of a cross-linking agent with a mass percent concentration of 40% to carry out cross-linking reaction for 24 hours, until a solution is obtained, and the solution is left standing to remove Bubble. When the molecular weight of PVA is larger, PVA ...

Embodiment 2

[0034] Embodiment 2: with reactant mass ratio polyvinyl alcohol (PVA): N-β-aminoethyl-γ-aminopropyltrimethoxysilane (A-1120): phenylacetaldehyde=0.1: 5: 0.3 preparation Pervaporation permeabilization hybrid membrane for methanol removal in wastewater

[0035] Using the same reaction device and operating steps as in Example 1, in an air or nitrogen atmosphere, at a temperature of 0°C, dissolve 0.1g of PVA raw material with a molecular weight of 1750 in water, and add water to prepare a 0.1% concentration by mass. Polyvinyl alcohol aqueous solution, keep stirring until PVA is completely dissolved, continue stirring for 2h, add 5mL silane coupling agent N-β-aminoethyl-γ-aminopropyltrimethoxysilane (A-1120) and 10mL concentration of 0.01M sol-gel reaction at 150° C. for 1 h, and then dropwise added 3 mL of a 10% cross-linking agent phenylacetaldehyde solution at 120° C. for 12 h to obtain a solution. Then use the solution to stand, after defoaming, the Al 2 o 3 Dip the coating ...

Embodiment 3

[0044] Example 3: Preparation of polyvinyl alcohol (PVA):anilinomethyltriethoxysilane (ND-42):butyl titanate:acetaldehyde=10:2:2:0.3 for removing Pervaporation of Methanol in Wastewater Through Alcohol Hybrid Membrane

[0045] Using the same reaction device and operating steps as in Example 1, in an air or nitrogen atmosphere, 10 g of polyvinyl alcohol (PVA) with a molecular weight of 1750 was added to a 250 mL container equipped with a stirrer, and water was added to form a mass percent concentration of 10% polyvinyl alcohol aqueous solution; under the temperature condition of 80 ℃, keep stirring until the PVA is completely dissolved, continue stirring for 5h, add 2mL silane coupling agent anilinomethyltriethoxysilane (ND-42) and 5mL concentration of 0.01 M dilute hydrochloric acid, conduct sol-gel reaction at 30°C for 48h, add 2mL butyl titanate and 15mL solvent N,N-dimethylformamide (DMF) respectively, continue stirring for 12h, then add dropwise 30mL mass percent The cros...

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Abstract

The invention discloses a preparation method of a ethanol pervaporation hybrid film used for removing methyl alcohol in wastewater, which is characterized by comprising the steps of: in inert gas or air, at a temperature of 0-200 DEG C, adding silane coupling agent which is 01.-2 times of the mol of polyvinyl alcohol to polyvinyl alcohol water solution with mass percent concentration of 0.1-10 percent, carrying out sol-gel reaction for 1-48h under the action of diluted acid with mol concentration of 0.001-0.1M, then adding 0.1-30 percent of cross-linking agent in terms of the mass percent of polyvinyl alcohol for cross-linking reaction until obtaining a solution, standing and defoaming the solution and then coating a film to obtain a diaphragm, and then drying the obtained diaphragm in the inert gas or air with the temperature of 0-200 DEG C and the relative humidity of 50-90 percent to obtain the ethanol pervaporation hybrid film used for removing the methyl alcohol The film has highthermal stability and good separating property, is a hybrid film through which the methyl alcohol can permeate preferentially, and can be used for separating and purifying the methyl alcohol wastewater.

Description

technical field [0001] The invention belongs to the technical field of wastewater treatment, and in particular relates to a method for preparing a pervaporation-permeable hybrid membrane for removing methanol in wastewater by using polyvinyl alcohol and a silane coupling agent to perform sol-gel reaction and crosslinking reaction. Background technique [0002] Chinese patent ZL200710040764.3 discloses a hydrophilic organic-inorganic composite pervaporation separation membrane and its preparation method and application. Using an inorganic ceramic membrane as a The method of ring reaction is used to prepare organic-inorganic composite pervaporation separation membrane; however, this method prepares a pure organic polymer separation layer on the surface of the ceramic membrane, which has the disadvantage of poor temperature resistance of the membrane and can only be used for 95% high-concentration methanol, etc. The dehydration of alcohols is a preferential water-permeable hybr...

Claims

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Application Information

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IPC IPC(8): B01D71/38B01D67/00B01D69/10C02F1/44C02F101/34
Inventor 刘俊生聂君得邵国泉张凌云
Owner SHANDONG TIANWEI MEMBRANE TECH
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