Modification method of titanium silicone molecular sieve and its application

A titanium-silicon molecular sieve, molecular sieve technology, applied in molecular sieve catalysts, molecular sieves and alkali exchange compounds, chemical instruments and methods, etc. Separation difficulties and other problems, to achieve the effect of improving the selectivity of propylene oxide, reducing energy consumption, and improving activity

Inactive Publication Date: 2004-12-22
DALIAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is impossible to obtain highly selective propylene oxide under the condition of high conversion rate of hydrogen peroxide
[0004] The main problem that above-mentioned prior art exists is: (1) can't obtain highly selective propylene oxide under the higher condition of hydrogen peroxide conversion rate, (2) under the higher condition of hydrogen peroxide conversion rate, there is a small amount of propylene glycol monomethyl Ether generation
The direct discharge of water containing a small amount of propylene glycol monomethyl ether will cause environmental pollution, and the separation of propylene glycol monomethyl ether and water is very difficult
Since water and propylene glycol monomethyl ether form an azeotrope, it is necessary to add benzene as an entrainer to remove a large amount of water to separate water and propylene glycol monomethyl ether, and the solvent methanol also needs to be separated and recycled, which results in too much energy consumption , thus restricting the industrial application of titanium-silicon molecular sieves

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The preparation of TS-1 was carried out according to Comparative Example 1. 0.6075 g of Cu(NO 3 ) 2 ·3H 2 O was dissolved in 14 mL of deionized water, 5 g of TS-1 was added, and allowed to stand for 24 hours. Then, the water was evaporated to dryness in an 80°C water bath under constant stirring, and dried in an oven at 120°C for 2 hours. The dried catalyst was raised from room temperature to 540°C in 3 hours in a temperature-programmed manner, and kept at this temperature Calcining at lower temperature for 5 hours, a CuO-modified TS-1 catalyst was prepared, wherein CuO accounted for 4% (mass percentage) of the content of TS-1.

Embodiment 2

[0018] The preparation of TS-1 was carried out according to Comparative Example 1. 0.9113 g of Cu(NO 3 ) 2 ·3H 2 O was dissolved in 14 mL of deionized water, 5 g of TS-1 was added, and allowed to stand for 24 hours. Then, the water was evaporated to dryness in an 80°C water bath under constant stirring, and dried in an oven at 120°C for 2 hours. The dried catalyst was raised from room temperature to 540°C in 3 hours in a temperature-programmed manner, and kept at this temperature Calcining at lower temperature for 5 hours, a CuO-modified TS-1 catalyst was prepared, wherein CuO accounted for 6% (mass percentage) of the content of TS-1.

Embodiment 3

[0020] The preparation of TS-1 was carried out according to Comparative Example 1. 0.3024 g of Pb(NO 3 ) 2 Dissolve in 14 ml of deionized water, add 5 g of TS-1, and let stand for 24 hours. Then, the water was evaporated to dryness in an 80°C water bath under constant stirring, and dried in an oven at 120°C for 2 hours. The dried catalyst was raised from room temperature to 300°C in 3 hours in a temperature-programmed manner, and kept at this temperature The PbO-modified TS-1 catalyst was prepared by calcination at lower temperature for 5 hours, wherein PbO accounted for 4% (mass percentage) of the content of TS-1.

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Abstract

A process for modifying Ti-Si molecular sieve TS-1 with MFI structure includes proportionally adding TS-1 to the aqueous solution of metal salt, laying aside for 6-100 hr, evaporating water by water both at 30-100 deg.C, drying at 110-200 deg.C for 1-20 hr, programmed heating to 200-800 deg.C within 1-12 hr, and calcining at this temp for 2-20 hr. It can be used in epoxidizing reaction of propylene to increase the conversion rate of H2O2 and the selectivity to epoxy propane.

Description

technical field [0001] The invention belongs to the preparation method of metal oxide modified titanium silicon molecular sieve catalyst and its application in propylene epoxidation reaction. Background technique [0002] Titanium silicate molecular sieve is a new heteroatom molecular sieve developed in the early 1980s. The synthesized molecular sieves include TS-1 with MFI structure, TS-2 with MEL structure and TS-48 with larger pore structure. Taramasso et al. first used tetrapropylammonium hydroxide (TPAOH) as template and tetraethyl titanate as titanium source, and synthesized titanium silicon molecular sieve TS-1 for the first time. Aiming at the disadvantages of this method, such as the low content of titanium entering the framework, Thangaraj et al. used tetrabutyl titanate (TBOT) with weak hydrolytic activity instead of tetraethyl titanate (TEOT) for pre-hydrolysis treatment, so that the titanium source and the silicon source The hydrolysis rate of the molecular sie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C01B39/46
Inventor 王祥生成卫国李钢郭新闻苏泉声
Owner DALIAN UNIV OF TECH
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