Method for modifying titanium-silicon molecular sieve material

A titanium-silicon molecular sieve and modification technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of low catalyst activity and poor catalyst stability, and achieve good dispersibility, easy process control, Overcoming the effect of precious metal agglomeration

Active Publication Date: 2010-01-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Appl.Catal.A: Gen., 2001, 213: 163-171 reported the research of epoxidized propylene to generate propylene oxide (PO), H 2 and O 2 React in situ to generate H on the active sites of noble metals such as Pd 2 o 2 intermediate, then generated H 2

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029]Take 20 grams of titanium-silicon molecular sieve TS-1, a concentration of 0.01g / mL (in terms of palladium atoms) ammonium palladium nitrate complex solution, ethyl orthosilicate, and hydrazine hydrate and hexadecyl trimethyl bromide Ammonium is added to the aqueous solution of tetrapropyl ammonium hydroxide (mass percentage concentration 10%) and stirred and mixed evenly, wherein titanium silicon molecular sieve (gram): tetraethyl orthosilicate (mole): hexadecyltrimethylammonium bromide (mol): tetrapropylammonium hydroxide (mol): hydrazine hydrate (mol): ammonium nitrate palladium complex (gram, calculated as palladium): water (mol)=100: 0.1: 0.005: 0.5: 3.0: 2.0 : 1000. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 150°C and autogenous pressure for 48 hours, filter the resultant, wash with water, dry it naturally, and continue drying at 180°C for 3 hours to obtain the modified titanium silicon Molecular sieve ma...

Embodiment 2

[0031] Get 20 grams of titanium-silicon molecular sieve TS-1, a concentration of 0.01g / mL (in terms of palladium atoms), palladium chloride solution, silica sol, hydrazine hydrochloride and polypropylene to the aqueous solution of sodium hydroxide (mass percentage concentration 15%) Stir and mix evenly in medium, wherein titanium silicon molecular sieve (gram): silica sol (mole, expressed as SiO 2 Calculation): polypropylene (mol): sodium hydroxide (mol): hydrazine hydrochloride (mol): palladium chloride (gram, in palladium): water (mol) = 100: 0.5: 0.9: 1.8: 0.15: 0.1: 4600. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 180°C and autogenous pressure for 24 hours, filter the resultant, wash with water, dry it naturally, and continue drying at 110°C for 3 hours to obtain the modified titanium silicon Molecular sieve material B.

Embodiment 3

[0033] Get 20 grams of titanium-silicon molecular sieve TS-1, palladium acetate solution, methyl orthosilicate, appropriate amount of sodium borohydride and Tween 80 with a concentration of 0.01g / mL (in terms of palladium atoms) and add them to tetrapropylammonium hydroxide and Stir and mix in the aqueous solution of butanediamine (mass percentage concentration 10%), wherein titanium silicon molecular sieve (gram): orthosilicate methyl ester (mole): alkali source (mole): palladium source (mole): protecting agent (mole ): water (mole)=100: 0.01: 0.03: 0.5: 0.05: 0.02: 550, then put into a sealed reactor, hydrothermally treat 120 hours at a temperature of 120°C and autogenous pressure, filter the gain, wash with water, and naturally After drying, continue drying at 150° C. for 3 hours to obtain the modified titanium-silicon molecular sieve material C.

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PUM

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Abstract

The invention discloses a method for modifying a titanium-silicon molecular sieve material, which is characterized by comprising the following steps: adding titanium-silicon molecular sieve, silicon-containing compound, protective agent, reducing agent and noble metal source into solution containing alkali source, evenly mixing the mixture, then carrying out hydro-thermal treatment for the mixture in a closed reaction kettle, and reclaiming a product. The method improves the content of framework titanium, relatively reduces the content of the titanium on the outside surface and orifices of the molecular sieve by covering inert component silicon on the outside surface and the orifices of the titanium-silicon molecular sieve, and reduces the occurrence of side reaction on the outside surface and orifices of a molecular sieve catalyst so as to improve the oxidation activity, stability and target product selectivity of the modified titanium-silicon molecular sieve material at the same time of improving the synergistic action of noble metals and titanium-silicon molecular sieve materials.

Description

technical field [0001] The invention relates to a method for modifying a titanium-silicon molecular sieve material, in particular to a method for modifying the titanium-silicon molecular sieve material with a precious metal source. 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. Among them, the titanium-silicon molecular sieve TS-1 developed and synthesized by the Italian company Enichem is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing the transition metal element titanium into the molecular sieve framework with a ZSM-5 structure. [0003] TS-1 not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07D301/12C07D303/04
Inventor 林民史春风朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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