Precious metal modification method of titanium silicalite molecular sieve

A titanium-silicon molecular sieve and precious metal technology, applied in crystalline aluminosilicate zeolite and other directions, can solve the problems of large waste water discharge, low effective utilization rate, heavy environmental burden, etc., and achieve product yield improvement, environmental protection benefits and economic benefits. The effect of improving and improving the volume utilization rate

Active Publication Date: 2013-07-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In-situ generation of H by supporting noble metals on titanium-silicon materials 2 o 2 Although the method for selective oxidation of organic matter has mild conditions and good selectivity (up to 95%), the traditional loading method has low activity and poor stability. 2 Low effective utilization
More importantly, a large amount of water is often used in the preparation process, resulting in a large amount of wastewater discharge and a heavy environmental burden.

Method used

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  • Precious metal modification method of titanium silicalite molecular sieve
  • Precious metal modification method of titanium silicalite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] This example is used to illustrate the method for modifying titanium-silicon molecular sieves with noble metals according to the present invention.

[0024]Take 10g of TS-1 molecular sieve and mix with 4.8g of 28% tetraethylammonium hydroxide solution (containing 0.05g of palladium chloride). Put the above mixture into 50mL polytetrafluoroethylene liner and put it on the support of 100mL polytetrafluoroethylene liner, add water 2mL under the support at the same time, then react in a sealed autoclave at 145°C for 12h. The obtained noble metal-modified molecular sieve was dried at 100° C. for 180 minutes, and then calcined at 650° C. for 3 hours to obtain noble metal-modified TS-1 molecular sieve A.

Embodiment 2

[0026] This example is used to illustrate the method for modifying titanium-silicon molecular sieves with noble metals according to the present invention.

[0027] Take 12g of TS-1 molecular sieve, and mix it evenly with 1g of triethanolamine and 5g of 16.3% tetrapropylammonium hydroxide solution (containing 0.1g of platinum nitrate). Put the above mixture into 50mL polytetrafluoroethylene liner and put it on the support of 100mL polytetrafluoroethylene liner, add water 3mL under the support at the same time, then react in a sealed autoclave at 160°C for 56h. The obtained noble metal-modified molecular sieve was dried at 150° C. for 120 minutes, and then calcined at 540° C. for 6 hours to obtain noble metal-modified TS-1 molecular sieve B.

Embodiment 3

[0029] This example is used to illustrate the method for modifying titanium-silicon molecular sieves with noble metals according to the present invention.

[0030] Take 12g of TS-1 molecular sieves and mix them evenly with 0.5g of n-propylamine and 7.5g of 16.3% tetrapropylammonium hydroxide solution (containing 0.02g of palladium acetate). Put the above mixture into 50mL polytetrafluoroethylene liner, place it on the support of 100mL polytetrafluoroethylene liner, and then react in a sealed autoclave at 175°C for 48h. The obtained noble metal-modified molecular sieve was dried at 90° C. for 240 minutes, and then calcined at 700° C. for 2 hours to obtain noble metal-modified TS-1 molecular sieve C.

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Abstract

A precious metal modification method of a titanium silicalite molecular sieve is characterized in that the method comprises the following steps: mixing a titanium silicalite molecular sieve, a precious metal source, and an organic alkali solution, treating the mixture in a closed reaction vessel at 100-200 DEG C for at least 2 hours, taking the product out at normal temperature and normal pressure, drying, and roasting to obtain the precious metal modified titanium silicalite molecular sieve product, wherein the water contained in the reaction vessel can form saturated water steam under the reaction condition, and has a weight ratio to the titanium silicalite molecular sieve being less than 1.2, and the treating capacity of the titanium silicalite molecular sieve is at least 10 g per liter of the reaction vessel volume. The method is low in cost, few in three-wastes, and high in efficiency, and the molecular sieve has good catalytic performance.

Description

technical field [0001] The invention relates to a method for modifying a titanium-silicon molecular sieve, and more specifically relates to a method for modifying a titanium-silicon molecular sieve synthesized under the prior art conditions with precious metals. Background technique [0002] Silicon molecular sieve is a new heteroatom molecular sieve developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MEL structure, MCM-22 with MWW structure and TS-48 with larger pore structure have been synthesized. Titanium-silicon molecular sieves are used as catalysts, and non-polluting low-concentration hydrogen peroxide can be used as oxidants, which can catalyze various types of organic oxidation reactions, such as epoxidation of alkenes, partial oxidation of alkanes, oxidation of alcohols, and oxidation of phenols. Hydroxylation, ammoxidation of cyclic ketones, etc., avoid the problems of complex oxidation process and environmental pollution, and have the in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
Inventor 史春风龙立华林民朱斌汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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