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Layered zirconium phosphate-based molecular sieve membrane and preparation method thereof

A zirconium phosphate-based and molecular sieve technology is applied in the field of membrane separation, which can solve problems such as poor stability, and achieve the effects of low preparation cost, reduction of grain boundary defects, and good industrial application prospects.

Active Publication Date: 2020-02-25
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the stability of the membrane material is also an important factor that cannot be ignored when it is used under actual conditions. Poor stability is still the limitation of some molecular sieve membranes (such as two-dimensional layered membranes assembled by interlayer forces). The disadvantages

Method used

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  • Layered zirconium phosphate-based molecular sieve membrane and preparation method thereof
  • Layered zirconium phosphate-based molecular sieve membrane and preparation method thereof
  • Layered zirconium phosphate-based molecular sieve membrane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0038] (1) Spin-coating ZrO 2 The sol solution is coated on the surface of the alumina carrier and then calcined at 400° C. for 4 hours.

[0039] (2) Mix 0.15 g of phenylphosphonic acid ligand and 0.05 g of hydrofluoric acid (40 wt%) with 15 g of deionized water, and stir evenly to obtain a reaction precursor solution.

[0040] (3) Put the gel-modified alumina carrier into the lining of the hydrothermal reaction kettle, and then add the reaction precursor solution, and react in an oven at 100°C for 24h.

[0041] (4) After the reaction in step (3) is completed, the reacted carrier is taken out, rinsed with deionized water, and dried at 70° C. for 12 hours to obtain a dense and continuous zirconium phenylphosphonate film.

[0042] Front-side SEM characterization of zirconium phenylphosphonate films as figure 1 As shown in a, the zirconium phenylphosphonate film is dense and continuous without defects. Cross-sectional scanning electron microscope characterization as figure 1 ...

Embodiment 2

[0044] (1) Spin-coating ZrO 2 The sol solution is coated on the surface of the stainless steel mesh carrier and then calcined at 400° C. for 4 hours.

[0045] (2) Mix 0.15 g of phenylphosphonic acid ligand and 0.05 g of hydrofluoric acid (40 wt%) with 15 g of deionized water, and stir evenly to obtain a reaction precursor solution.

[0046] (3) Put the gel-modified stainless steel mesh carrier into the lining of the hydrothermal reaction kettle, and then put the reaction precursor solution into it, and react in an oven at 100°C for 24h.

[0047](4) After the reaction in the step (3) is completed, the reacted carrier is taken out, rinsed with deionized water, and dried at 70° C. for 12 hours to obtain a zirconium phenylphosphonate membrane.

[0048] Front-side SEM characterization of zirconium phenylphosphonate films as image 3 As shown, the zirconium phenylphosphonate film grows well.

Embodiment 3

[0050] (1) Spin-coating ZrO 2 The sol solution is coated on the surface of the alumina carrier and then calcined at 400° C. for 4 hours.

[0051] (2) Mix 0.135g of phosphoric acid ligand (85wt%) and 0.05g of hydrofluoric acid (40wt%) with 15g of deionized water, and stir evenly to obtain a reaction precursor solution.

[0052] (3) Put the gel-modified alumina carrier into the lining of the hydrothermal reaction kettle, and then add the reaction precursor solution, and react in an oven at 100°C for 24h.

[0053] (4) After the reaction in step (3) is completed, the reacted carrier is taken out, rinsed with deionized water, and dried at 70° C. for 12 hours to obtain a zirconium phosphate film.

[0054] The scanning electron microscope characterization of the zirconium phosphate film was as follows: Figure 4 As shown, the zirconium phosphate film grows well.

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Abstract

The invention provides a layered zirconium phosphate-based molecular sieve membrane and a preparation method thereof. The zirconium phosphate-based molecular sieve membrane comprises a zirconium phosphate functional membrane layer and a carrier; and the zirconium phosphate membrane layer is of a layered structure. The preparation method of the zirconium phosphate-based molecular sieve membrane comprises the following steps: coating the surface of a carrier with a zirconium oxide sol, and carrying out high-temperature calcination to obtain a zirconium oxide gel layer modified carrier; dissolving a reaction reagent and a reaction aid in deionized water to obtain a reaction precursor solution; putting the zirconium oxide gel layer modified carrier and the reaction precursor solution into a reaction kettle, and carrying out a hydrothermal reaction; and washing and drying the obtained reaction product after the reaction is finished in order to obtain the layered zirconium phosphate-based molecular sieve membrane. The layered zirconium phosphate-based molecular sieve membrane prepared in the method has the advantages of good intergrowth property, flexibility in regulation of the interlayer distance, excellent gas and liquid separation property, good thermal, chemical and mechanical stabilities, simple preparation process, low cost, high universality and good industrial separation application prospect.

Description

technical field [0001] The invention belongs to the technical field of membrane separation, and in particular relates to a layered zirconium phosphate-based molecular sieve membrane and a preparation method thereof. Background technique [0002] As a very important link in the chemical production process, the energy consumption of the separation process accounts for 45% to 55% of the total industrial energy consumption in the world. The traditional separation methods represented by rectification are complicated to operate and consume a lot of energy. Therefore, it is urgent to develop new separation methods to reduce the heavy energy burden. In contrast, membrane separation technology has become a new direction for future development due to its low energy consumption, high efficiency, pollution-free and continuous operation. In recent years, the field of membrane separation has received extensive attention and developed rapidly, but it is still a big problem to prepare memb...

Claims

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Application Information

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IPC IPC(8): B01D71/02B01D67/00B01D53/22
CPCB01D71/028B01D67/0039B01D53/228
Inventor 刘毅纪涛涛
Owner DALIAN UNIV OF TECH
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