Method for modifying titanium silicalite molecular sieve by precious metal source

A titanium-silicon molecular sieve and noble metal technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of poor stability and low catalyst activity of titanium-silicon materials, and achieve the effects of increased volume utilization, improved environmental protection efficiency, and low consumption

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

Although the method of supporting noble metals on titanium-silicon materials to generate H2O2 in situ for selective oxidation of organic matter has mild conditions and good selectivity (up to 95% ), but the titanium-silicon catalysts loaded with precious metals have low activity and poor stability

Method used

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  • Method for modifying titanium silicalite molecular sieve by precious metal source
  • Method for modifying titanium silicalite molecular sieve by precious metal source

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026]Mix the metered tetraethyl orthosilicate, palladium chloride, sodium citrate and tetraethylammonium hydroxide, add an appropriate amount of distilled water, mix well, stir at room temperature for 1.0h, and then stir at 75°C for 3h to obtain modification Liquid, its molar composition is silicon: titanium: organic base: water: precious metal source: reducing agent = 1: 0: 0.85: 20: 0.05: 0.05 (wherein silicon and titanium are SiO 2 and TiO 2 Calculated, precious metals are calculated as elemental substances). Take 12 g of TS-1 molecular sieves and mix with 10 g of the modified solution obtained above. The above mixture was filled into a 50 mL polytetrafluoroethylene liner and placed in a 100 mL polytetrafluoroethylene liner, and then reacted in a sealed autoclave at 175° C. for 12 h. The obtained product was dried at 150° C. for 120 minutes, and then calcined at 580° C. for 5 hours to obtain noble metal modified TS-1 molecular sieve A.

Embodiment 2

[0028] Mix the measured amount of amorphous silica gel, palladium acetate, hydrazine hydrate and tetrapropylammonium hydroxide, and add an appropriate amount of distilled water. After mixing evenly, stir at room temperature for 1.5h, then add n-butyl titanate and stir for 0.5h, then at 70°C Down stirring 3h obtains modified solution, and its molar composition is silicon: titanium: organic base: water: precious metal source: reducing agent=1: 0.02: 0.75: 25: 0.025: 0.15 (wherein silicon and titanium are SiO 2 and TiO 2 Calculated, precious metals are calculated as elemental substances). Take 10g of TS-1 molecular sieve and mix with 8.5g of the modified solution obtained above. The mixture was filled into 50 mL polytetrafluoroethylene liner, and then placed in 100 mL polytetrafluoroethylene liner, and then reacted at 180° C. for 24 h in a sealed autoclave. The obtained product was dried at 150° C. for 120 minutes, and then calcined at 650° C. for 2 hours to obtain noble metal ...

Embodiment 3

[0030] Mix the measured tetraethyl orthosilicate, tetraethyl titanate, palladium carbonate, formaldehyde and tetrapropylammonium hydroxide, and add an appropriate amount of distilled water, mix well, stir at room temperature for 1.0h, and then stir at 80°C for 3h Obtain modified solution, its molar composition is silicon: titanium: organic base: water: precious metal source: reducing agent=1: 0.02: 0.75: 35: 0.02: 0.025 (wherein silicon and titanium are SiO 2 and TiO 2 Calculated, precious metals are calculated as elemental substances). Take 15g of TS-1 molecular sieve and mix evenly with 13g of the modified solution obtained above. The mixture was charged into a 50 mL polytetrafluoroethylene liner and placed in a 100 mL polytetrafluoroethylene liner, and then reacted at 160° C. for 62 h in a sealed autoclave. The obtained product was dried at 135° C. for 240 minutes, and then calcined at 560° C. for 3 hours to obtain noble metal modified TS-1 molecular sieve C.

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Abstract

A method for modifying a titanium silicalite molecular sieve by a precious metal source is characterized in that a mixture of modification liquid and a titanium silicalite molecular sieve is treated in a closed reaction vessel at 120-200 DEG C for at least 2 hours, and then the product is dried and roasted, 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; the modification liquid comprises a silicone source, a titanium source, water, organic base, a precious metal source, and a reducing agent; the weight ratio of the titanium silicalite molecular sieve to the modification liquid is 100:(1-150); and the treating capacity of the titanium silicalite molecular sieve is at least 10 g per liter of the reaction vessel volume. The method needs no mother liquor separation, omits procedures of filtration or washing, greatly reduces environment pollution, improves volume utilization efficiency of high pressure equipment, increases productivity, reduces preparation cost, and improves the environmental protection and economic benefits of the synthesis.

Description

technical field [0001] The invention relates to a method for modifying titanium-silicon molecular sieves with precious metals under water vapor. Background technique [0002] Titanium-silicon molecular sieve is a new type of 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 incomparable advantages of energy saving, economy and environmental friendliness of traditional oxidati...

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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