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Method for preparing titanium-containing zeolite molecular sieve by natural zeolite modification

A technology of zeolite molecular sieve and natural zeolite, which is applied in the field of natural zeolite material modification, can solve the problems of redox property, solid acidity and alkalinity, and catalytic performance that cannot satisfy industrial production and environmental protection, and achieves good redox property and preparation cost. Inexpensive and value-added effects

Inactive Publication Date: 2009-08-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Modification methods such as heat treatment, acid treatment and salt treatment are usually adopted. After these treatments, the purity of natural zeolite, the smoothness of the pores and the adsorption performance are significantly improved, but the redox performance, solid acidity and alkalinity and catalytic performance are still far from satisfactory. Requirements for industrial production and environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] ●Put 30g of natural mordenite in a 500ml three-path bottle, add 300ml, 0.8M NH 4 The Cl solution was stirred at 80°C for 2 hours, washed with water, dried, and repeated twice;

[0020] Take 25g of natural mordenite treated by (1) in a 500ml three-path bottle, add 300ml, 6M HCl solution, stir at 100°C for 8 hours, wash with water, dry, and repeat the operation 3 times;

[0021] ●Take 3g of the sample treated by (2) into a quartz reaction tube, raise it from room temperature to 120°C at a rate of 5°C / min, treat it with nitrogen at 120°C for 2 hours, and then increase it from room temperature to 120°C at a rate of 2°C / min From 120°C to 400°C, use nitrogen to bring the vapor of titanium tetrachloride into the quartz reaction tube, and react at 400°C for 8 hours, stop passing the vapor of titanium tetrachloride, and continue purging with nitrogen at this temperature for 3 hours , cooling, washing, and drying to obtain a titanium-containing zeolite molecular sieve sample;

...

Embodiment 2

[0024] ●With embodiment 1;

[0025] ●Take 25g of the sample treated by (1), add 300ml of 8M HCl solution to a 500ml three-path bottle, stir at 100°C for 6 hours, wash with water, dry, and repeat the operation 3 times;

[0026] ●Take 3g of the sample treated by (1) and (2) into a quartz reaction tube, heat it from 30°C to 180°C at a heating rate of 3°C / min, maintain this temperature for 2 hours, and then heat it at a rate of 5°C / min Raise from 180°C to 500°C, use argon to bring the vapor of isopropyl titanate into the quartz tube, react at 500°C for 10 hours, continue purging with argon at this temperature for 3 hours, lower the temperature, wash, After drying, the titanium-containing zeolite molecular sieve sample was obtained; the titanium-containing mordenite sample was obtained; the sample was characterized and analyzed by XRD, ICP and UV-Vis, and the results showed that the titanium in the prepared sample had successfully entered the framework of the natural zeolite, and t...

Embodiment 3-6

[0028] In different ion exchangers according to Example 1, the Si / Ti ratio of the titanium-containing zeolite molecular sieve sample prepared by dealumination agent is shown in Table 1

[0029] natural zeolite ion exchanger Dealumination agent solid to liquid ratio Si / Ti Natural Mordenite ammonium chloride hydrochloric acid 1:5 80 natural clinoptilolite ammonium chloride oxalic acid 1:25 90 natural clinoptilolite ammonium sulfate sulfuric acid 1:10 85 Natural Mordenite ammonium nitrate nitric acid 1:15 85

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Abstract

A method for preparing a titanium-containing zeolite molecular sieve by modifying natural zeolite, using natural zeolite as a raw material, undergoing ion exchange, chemical dealumination, and gas-solid phase replacement reaction, to prepare a high-performance titanium-containing zeolite molecular sieve, molecular sieve The molar ratio (Si / Ti) of Si and Ti in the framework is 20 to 100. The present invention introduces metal titanium with special catalytic performance into the framework of natural zeolite, which greatly improves the grade of natural zeolite products and expands the range of natural zeolite. The application scope provides a low-cost, simple-operation and environment-friendly way to prepare heteroatom zeolite molecular sieves.

Description

technical field [0001] The invention belongs to the technical field of modification of natural zeolite materials, and relates to a method for preparing heteroatom molecular sieves by modification of natural zeolite, in particular to a method for preparation of titanium-containing zeolite molecular sieves by modification of natural zeolite. Background technique [0002] Zeolites are a class of aluminosilicate crystals with a regular cage or pore structure. It is precisely because of this regular and open pore structure that zeolites are widely used in catalysis, adsorption, separation, and host-guest assembly. Zeolite can be divided into natural zeolite and synthetic zeolite. Compared with natural zeolite, synthetic zeolite has many advantages (such as high purity, uniform pore size, and good ion exchange performance), but the production investment of synthetic zeolite is large, the cost is high, and the mother liquor is difficult to recover, etc., and its large-scale applic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/06B01J29/89
Inventor 肖丽萍杨靖楼辉郑小明
Owner ZHEJIANG UNIV
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