A kind of preparation method of nanoporous carbon ceramic membrane nanofiltration composite membrane

A nanoporous carbon and ceramic membrane technology, applied in the field of ceramic membranes, can solve problems such as complex procedures, uneven pore size distribution, and limited application range, and achieve the effect of simple preparation process, easy promotion, and enhanced hydrophilicity

Active Publication Date: 2022-06-21
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Researchers have made a lot of efforts to develop porous carbon materials with different precursor sources and structural morphologies. For example, using cheap biomass materials to carbonize mesoporous carbons has significantly reduced costs, but such porous carbons have well-ordered channels. The degree of density is low, and the pore size distribution is uneven, which limits the scope of application; the porous carbon prepared by carbonizing mesoporous molecular sieves and nanoparticles as hard templates, covering the surface with organic matter, has regular and highly ordered channels, but the procedure of this method is relatively Complex and costly, not conducive to mass production

Method used

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  • A kind of preparation method of nanoporous carbon ceramic membrane nanofiltration composite membrane
  • A kind of preparation method of nanoporous carbon ceramic membrane nanofiltration composite membrane
  • A kind of preparation method of nanoporous carbon ceramic membrane nanofiltration composite membrane

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Effect test

Embodiment 1

[0037] (1) Preparation of boehmite sol: under nitrogen protection, 0.05 mol of aluminum sec-butoxide was added dropwise to 7 mol of deionized water with stirring, and the reaction temperature was kept at 80 °C to avoid the formation of aluminum hydroxide, The solution was kept at 90 °C for 1 h to remove the generated butanol, then the solution was cooled to 60 °C and 1 mol / L nitric acid solution was added to adjust the pH to 2.5. The resulting colloidal solution was refluxed at 90 °C for 20 h to obtain a boehmite sol solution.

[0038] (2) Preparation of sol-gel solution: Mix tetraethoxysilane (TEOS), water and ethanol in a molar ratio of 1:8.2:6.75 in a 250ml beaker, and adjust the solution with HCl with a concentration of 1mol / L pH to 2, magnetic stirring for 60 min; 8.543 g of CTAB was added, the mass fraction (wt%) of CTAB in the solution was 9.3, and a sol-gel solution was obtained after magnetic stirring for 120 min.

[0039] (3) Single-channel tubular Al with a pore si...

Embodiment 2

[0043] As in Example 1, the difference is that the number of MOF growth cycles is 6-15, and step (5) is not performed. The effect of cycle times on the rejection performance of ZIF-67 ceramic membrane nanofiltration composite membrane was investigated. With the increase of the number of cycles, the dye rejection rate of the composite membrane increased continuously, and the flux decreased accordingly. When the number of cycles reaches more than 12 times, the retention rate is more than 90%. It can be speculated that the continuous increase of the number of cycles leads to the gradual reduction of the inner space of the membrane pore channel, the pores in the membrane are gradually filled with MOF crystals, and the volume of macropores and mesopores is gradually reduced. decreases, the micropore volume increases, and then the dye retention rate is higher, and the flux gradually decreases. like image 3 As shown, when the number of cycles reaches 15, the retention rate of Cong...

Embodiment 3

[0045] As in Example 1, the difference lies in the fact that the precursor reaction solution Co(NO 3 ) 2 ·6H 2 The O concentration was 0.025-0.05 mol / L, and step (5) was not carried out. The effect of the concentration of precursor reaction solution on the rejection performance of ZIF-67 ceramic membrane nanofiltration composite membrane was investigated. Due to the regular shape and small size of ZIF-67 crystals formed by crystallization of low-concentration precursor solution, the probability of crystal growth in mesopores is greater, the film formation is more dense, and the flux is relatively low. With the increase of the concentration, the generated crystal particles are larger, and it is difficult to crystallize in the mesopores, resulting in the decrease of the retention performance of the composite membrane. like Figure 4 shown, Co(NO) with a concentration of 0.05 mol / L 3 ) 2 ·6H 2 The dye rejection rate of O ethanol solution was the highest, reaching 96.4%.

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Abstract

The invention relates to a preparation method of a nanoporous carbon ceramic membrane nanofiltration composite membrane, which uses a sol-gel method to sequentially prepare γ-Al on a commercial macroporous ceramic support body 2 o 3 And the mesoporous silicon layer, and then introduce the metal organic framework compound into the mesopore to adjust the pore size to form a selective separation layer of the ceramic membrane, and prepare the nanoporous carbon ceramic nanofiltration composite membrane with MOFs as the sacrificial template. The invention uses a liquid phase epitaxial growth method to pass a metal salt solution through a mesoporous silicon-modified ceramic membrane at a certain flow rate, and then pass an organic ligand solution through the ceramic membrane to generate MOFs seeds in the mesoporous pores. This process is cycled several times, and directional coordination reactions continue to occur in the mesopores to reduce the pore size, and then it is carbonized at high temperature to form nanoporous carbon. While retaining the carbon skeleton structure of MOFs, it has acid resistance, alkali resistance and oxidation resistance. The preparation of the invention is an efficient method for preparing an effective ceramic nanofiltration membrane, and is suitable for large-scale production.

Description

technical field [0001] The invention belongs to the technical field of ceramic membranes, and in particular relates to a preparation method of a nanoporous carbon ceramic membrane nanofiltration composite membrane, which is suitable for industrial application. Background technique [0002] Porous carbon materials are considered as ideal carriers for the preparation of functional materials due to their large specific surface area, uniform pore structure, rigid framework, excellent chemical properties and good thermal stability. field has a wide range of applications. Among them, the pore structure, surface properties, precursor sources and preparation methods of porous carbon all have an important impact on the material cost and application performance, and how to easily control the composition and structure of porous carbon materials and reduce the preparation cost has always been the focus of research. In this regard, researchers have made a lot of efforts to develop porou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D69/12B01D71/02B01D67/00B01D61/02
CPCB01D69/12B01D71/021B01D67/0002B01D61/027
Inventor 庞龙刘惠美张彦彦黄子玲金宝丹
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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