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Method for preparing high-performance B-ZSM-5 molecular sieve membrane in dilute synthesis solution

A technology of B-ZSM-5 and dilute synthetic liquid, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., to achieve the effect of improving separation performance

Active Publication Date: 2015-09-09
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The B-ZSM-5 molecular sieve membranes reported above are all at H 2 O / SiO 2 Prepared in a synthetic solution with a molar ratio of less than 120, for H 2 O / SiO 2 The preparation of high-performance B-ZSM-5 membranes in synthetic solutions higher than 200 has not been reported

Method used

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  • Method for preparing high-performance B-ZSM-5 molecular sieve membrane in dilute synthesis solution
  • Method for preparing high-performance B-ZSM-5 molecular sieve membrane in dilute synthesis solution
  • Method for preparing high-performance B-ZSM-5 molecular sieve membrane in dilute synthesis solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1 Preparation of B-ZSM-5 seed layer

[0030] First, use hot dipping to coat large seed crystals, using such as figure 2 The B-ZSM-5 molecular sieve with a size of 1μm shown in a is used as a large seed crystal. First, the two ends of the alumina carrier tube are sealed with a polytetrafluoroethylene plug, so that the seed crystal can only be introduced to the outer surface of the carrier tube. Place the sealed carrier tube in an oven at 175°C and heat it for 3 hours to cause a pressure difference between the inside and outside of the carrier tube. Put the hot carrier tube into a large seed suspension with a mass concentration of 2wt% for 20 seconds, and then slowly take it out vertically. Then immediately remove the Teflon plug to release the water in the tube, dry it at room temperature, dry it overnight in a 50℃ oven, then put it in a 175℃ oven to solidify the seed layer, and then wipe the carrier tube with degreased cotton Molecular sieve remaining on the surfa...

Embodiment 2

[0032] Example 2 Preparation of B-ZSM-5 molecular sieve membrane

[0033] The carrier used in this experiment to synthesize B-ZSM-5 molecular sieve membrane is the tubular macroporous α-Al provided by Foshan Ceramic Research Institute 2 O 3 The carrier has an inner diameter and an outer diameter of 8 mm and 13 mm, respectively, a length of 80 mm, a porosity of about 36%, and an average pore diameter of about 1-3 μm.

[0034] Preparation of B-ZSM-5 molecular sieve membrane: Seal both ends of the carrier tube coated with the seed layer and put it into a high-pressure reactor with a PTFE liner. The crystallization mother liquor of the membrane should be equipped with B-ZSM -5 seed crystals are prepared by the method of synthetic solution, and its molar composition is 1TEOS:0.2TPAOH:0.06B(OH) 3 :600H 2 O, the synthetic solution after stirring and clarification is slowly poured into the autoclave, sealed and put into a 175℃ oven to react for 24h. After the reaction, the membrane tube is ...

Embodiment 3

[0035] Example 3 Pervaporation performance test

[0036] The template-removed B-ZSM-5 molecular sieve membrane passes such as Figure 5 The shown pervaporation device tests its separation performance, in which the heating belt heats the raw material liquid to a certain temperature, the magnetic stirrer stirs the raw material liquid to keep the temperature and concentration of the raw material liquid uniform, and the membrane tube is sealed at one end with a separator and put in the material liquid The other end of the tank is connected to a vacuum pump through a cold trap cooled by liquid nitrogen, and the osmotic pressure is maintained at about tens of Pa. Driven by the pressure difference, the vapor permeating the membrane is condensed in the cold trap by liquid nitrogen. The pervaporation performance of the membrane is represented by the permeation flux J and the separation coefficient S. The permeation flux J represents the unit membrane area per unit time (t / h) (A / m 2 ) The t...

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Abstract

The invention provides a method for preparing a high-performance B-ZSM-5 molecular sieve membrane in a dilute synthesis solution. According to the method, B-ZSM-5 zeolite molecular sieves of different sizes are adopted as seed crystals and a thin and dense seed crystal layer is formed directly on the surface of a macroporous carrier tube. After that, the seed crystals and the seed crystal layer are subjected to hydro-thermal synthesis in a dilute synthesis solution, wherein the ratio of H2O to SiO2 is 200-1200. Finally, a high-performance B-ZSM-5 molecular sieve membrane is formed on the surface of a macroporous carrier. According to the method, boron is led into a zeolite framework in the isomorphism manner, so that the separation performance of the B-ZSM-5 molecular sieve membrane is greatly improved. The pervaporation performance of the prepared B-ZSM-5 molecular sieve membrane is tested in an ethanol / water system, wherein the weight ratio of ethanol to water is 5 to 95. The result of the test shows that, at 60 DEG C, the permeation flux and the separating factor of the B-ZSM-5 molecular sieve membrane are respectively 2.60 kg / m<2>*h, and 54.98. Due to the adoption of the dilute synthesis solution, the application amounts of a silicon source and a template agent for synthesizing the membrane are reduced. Therefore, the method is suitable for the recovery of fuel ethanol during the fermentation-based ethanol production process.

Description

Technical field [0001] The invention belongs to the field of inorganic materials used for pervaporation separation, and relates to a B-ZSM-5 zeolite molecular sieve of different sizes as seed crystals. A thin and dense seed layer is directly introduced on the surface of a macroporous carrier tube, and then placed in a thin layer. Synthetic fluid (H 2 O / SiO 2 =200-1200) in the process of hydrothermal synthesis, and finally prepared a high-performance B-ZSM-5 molecular sieve membrane on the surface of the macroporous carrier. Background technique [0002] At present, fossil resources are increasingly depleted, and the environmental pollution caused by burning fossil fuels is becoming more and more serious. As a new, green, and efficient renewable energy to replace some fossil fuels, ethanol is of great significance for alleviating the current resource shortage and environmental degradation. At present, the method of preparing fuel ethanol mainly adopts the biomass fermentation meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D69/10B01D67/00B01D61/36C07C31/08
Inventor 杨建华柴丽均王金渠鲁金明殷德宏张艳
Owner DALIAN UNIV OF TECH
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