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Preparation method of hydrophobic and oleophobic ZrO2 nanofiltration membrane

A hydrophobic and oleophobic, nanofiltration membrane technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc. high purity effect

Active Publication Date: 2015-04-01
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the ceramic membrane prepared by the sol-gel method is easy to break during the process of smearing, drying, and calcination, and the formation of pinholes is the biggest obstacle to its large-scale application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Step 1, 3.22g zirconium oxychloride (ZrOCl 2 ·8H 2 O), 0.26g yttrium trichloride (YCl 3 ·6H 2 (2), 993mL isopropanol and 1.53mL acetylacetone are mixed, react 12h under the stirring condition of 70 ℃, then add 3.4mL hydrogen peroxide (30wt%) in the reactant after reaction, stir, obtain ZrO 2 Sol;

[0028] Step 2, get ZrO described in step 1 2 95wt% of the sol is placed in a high-pressure reactor, and the temperature is 180 °C under the condition of solvent heat treatment for 5 hours, and after drying, ZrO with a size of 5nm to 20nm is obtained. 2 Nano powder;

[0029] Step 3, ZrO described in remaining step 1 with isopropanol 2 Sol diluted to ZrO 2 The concentration is 0.005M, and then to the diluted ZrO 2 Add ethylene glycol in the sol, stir to obtain dispersant; The addition of described ethylene glycol is the diluted ZrO 2 95% of the total volume of sol and ethylene glycol;

[0030] Step 4, ZrO described in 1g step 2 2 Nano-powder is dispersed in the dispe...

Embodiment 2

[0036] Step 1, 3.22g zirconium oxychloride (ZrOCl 2 ·8H 2 O), 0.098g yttrium trichloride (YCl 3 ·6H 2 (0), 49.65mL isopropanol and 0.82mL acetylacetone are mixed, react 5h under the stirring condition of 90 ℃, then add 2.5mL hydrogen peroxide (30wt%) in the reactant after reaction, stir, obtain ZrO 2 Sol;

[0037] Step 2, get ZrO described in step 1 2 95wt% of the sol is placed in a high-pressure reactor, and the solvent heat treatment is performed at a temperature of 120°C for 22 hours. After drying, ZrO with a size of 15nm to 30nm is obtained. 2 Nano powder;

[0038] Step 3, ZrO described in remaining step 1 with isopropanol 2 Sol diluted to ZrO 2 The concentration is 0.0005M, and then to the diluted ZrO 2 Add ethylene glycol in the sol, stir to obtain dispersant; The addition of described ethylene glycol is the diluted ZrO 2 90% of the total volume of sol and ethylene glycol;

[0039] Step 4, ZrO described in 1g step 2 2 The nanopowder is dispersed in 199g of the...

Embodiment 3

[0045] Step 1, 3.22g zirconium oxychloride (ZrOCl 2 ·8H 2 O), 0.13g yttrium trichloride (YCl 3 ·6H 2 (2), 611mL isopropanol and 1.22mL acetylacetone, reacted 8h under the stirring condition of 80 ℃, then added 2.8mL hydrogen peroxide (30wt%) in the reactant after the reaction, stirred evenly, obtained ZrO 2 Sol;

[0046] Step 2, get ZrO described in step 1 2 95wt% of the sol is placed in a high-pressure reactor, and the temperature is 150 °C under the condition of solvent heat treatment for 15 hours, and after drying, ZrO with a size of 12nm to 21nm is obtained. 2 Nano powder;

[0047] Step 3, ZrO described in remaining step 1 with isopropanol 2 Sol diluted to ZrO 2 The concentration is 0.001M, and then to the diluted ZrO 2 Add ethylene glycol in the sol, stir to obtain dispersant; The addition of described ethylene glycol is the diluted ZrO 2 93% of the total volume of sol and ethylene glycol;

[0048] Step 4, ZrO described in 1g step 2 2 The nano powder is dispers...

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PUM

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Abstract

The invention discloses a preparation method of a hydrophobic and oleophobic ZrO2 nanofiltration membrane. The preparation method comprises the following steps of 1, preparing ZrO2 sol, 2, carrying out solvothermal treatment on the ZrO2 sol and carrying out drying to obtain ZrO2 nano-powder, 3, diluting the ZrO2 sol, adding glycol into the dilute ZrO2 sol, and carrying out uniform stirring to obtain a dispersant, 4, dispersing the ZrO2 nano-powder in the dispersant, and carrying out uniform stirring to obtain a coating liquid, 5, coating the coating liquid on a metal porous pipe, carrying out drying, and carrying out sintering to obtain a porous ZrO2 filter membrane, 6, repeating the step 4 to obtain a metal-based ZrO2 composite filter membrane, and 7, carrying out modification by perfluoroalkyl silane to obtain the hydrophobic and oleophobic ZrO2 nanofiltration membrane. The preparation method realizes combination of a sol-solvent thermal treatment method and solid particle sintering, and realizes preparation of the hydrophobic and oleophobic ZrO2 nanofiltration membrane at a low temperature. The hydrophobic and oleophobic ZrO2 nanofiltration membrane has a contact angle of 115-137 degrees with water and a contact angle of 112-128 degrees with oil.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials and film preparation, in particular to a hydrophobic and oleophobic ZrO 2 Preparation method of nanofiltration membrane. Background technique [0002] Membrane separation technology is a new type of separation technology that uses the difference in selective permeation properties of membranes for the components in the mixture to achieve separation, purification and concentration. The membrane separation method can generally be carried out at room temperature, has the advantages of low pollution, and has the advantages of simple separation device, easy operation and control, easy maintenance, and high separation efficiency. Therefore, it is widely used in water treatment, food and beverage, medicine, chemical industry, electronics, energy and environmental protection and other fields. Membrane separation technology is considered to be "one of the most promising high-tech technologies from t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D71/02B01D69/12B01D67/00
Inventor 李广忠汤慧萍李纲王建张文彦康新婷李亚宁迟煜頔葛渊沈垒
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH