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Method for modifying titanium-silicon molecular sieve

A titanium-silicon molecular sieve and modification technology, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of low catalyst activity, low effective utilization rate, poor stability, etc., and achieve simple and easy operation, Good catalytic oxidation activity, easy modification process

Active Publication Date: 2010-01-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process has mild reaction conditions and good selectivity. The main problems at present are low catalyst activity, poor stability, and H 2 Low effective utilization

Method used

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  • Method for modifying titanium-silicon molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Get 10 grams of titanium-silicon molecular sieve TS-1, a concentration of 0.01g / mL (in terms of palladium atoms) ammonium nitrate palladium complex solution and hexadecyltrimethylammonium bromide to join the tetrapropylammonium hydroxide Stir in an aqueous solution (mass percentage concentration 10%) to obtain a mixed solution 1, wherein titanium silicon molecular sieve (gram): hexadecyltrimethylammonium bromide (mole): tetrapropyl ammonium hydroxide (mole): ammonium nitrate Palladium complex (g, calculated as palladium): water (mol) = 100: 0.2: 0.005: 0.5: 1000. At room temperature, ethyl orthosilicate, butylenediamine and water were stirred for 50 minutes according to the ratio of ethyl orthosilicate (mol): butylenediamine (mol): water (mol) = 1: 4.5: 200, and mixed For liquid 2, mix liquid 1 and liquid 2 according to the ratio of molecular sieve (g): Si (mol) = 200: 1, put them into a stainless steel reactor, seal them, and conduct hydrothermal treatment at a tempera...

Embodiment 2

[0035] Take 10 grams of titanium-silicon molecular sieve TS-1, a palladium chloride solution with a concentration of 0.01 g / mL (calculated as palladium atoms) and polyacrylate, and add it to an aqueous solution of hexamethylenediamine (15% by mass) and stir evenly to obtain a mixture. Liquid 1, wherein titanium-silicon molecular sieve (gram): polyacrylate (mol): sodium hydroxide (mol): palladium chloride (gram, calculated as palladium): water (mol) = 100: 0.9: 1.0: 0.15: 1600 . At 45°C, methyl orthosilicate, tetrapropylammonium hydroxide and water were mixed according to the ratio of methylorthosilicate (mol): tetrapropylammonium hydroxide (mol): water (mol) = 1: 1.8: 300 Proportionally stirred for 30 minutes to obtain mixed solution 2, then mixed solution 1 and mixed solution 2 according to the ratio of molecular sieve (gram): Si (mol) = 500: 1 and then put into a stainless steel reactor to seal, at a temperature of 180 ° C Hydrothermal treatment under autogenous pressure fo...

Embodiment 3

[0037] Get 10 grams of titanium-silicon molecular sieve TS-1, a concentration of 0.01g / mL (in terms of palladium atoms) palladium nitrate solution and Tween 80 to join the aqueous solution of tetrapropylammonium hydroxide and n-butylamine (mass percentage concentration 10%) Mixed solution 1 was obtained by stirring in the medium, wherein titanium-silicon molecular sieve (gram): protective agent (mole): organic amine (mole): palladium source (gram, calculated as palladium): water (mole) = 100: 0.03: 0.1: 0.05 : 550; At room temperature, silica sol, butylenediamine and water are mixed according to silica sol (mole, as SiO 2 (meter): butyldiamine (mol): water (mol) = 1: 1.2: 450 ratio and stirred for 80 minutes to obtain mixed solution 2; : 1 ratio and put into a stainless steel reactor and seal it, hydrothermally treat 120h at a temperature of 120°C and autogenous pressure, filter, wash, then dry at 150°C for 3h, and roast in a nitrogen atmosphere at 350°C for 5h to obtain Modi...

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Abstract

The invention provides a method for modifying a titanium-silicon molecular sieve, and belongs to the technical field of inorganic chemicals and the synthesis of inorganic chemicals. The method comprises the following steps of: adding the titanium-silicon molecular sieve, a protective agent and a noble metal source in a solution containing organic amine, evenly mixing the mixture, adding a hydrating solution of silicon in the mixing solution and evenly mixing the mixed solution, putting the mixedsolution in a reaction kettle for hydro-thermal treatment, and recycling the sieve. The titanium-silicon molecular sieve modified by the method has obviously high catalytic oxidation activity, selectivity and stability.

Description

technical field [0001] The invention relates to a method for modifying a titanium-silicon molecular sieve. Background technique [0002] Titanium silicate 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 silicate molecular sieves can be used to catalyze a variety of organic oxidation reactions, such as olefin epoxidation, alkane partial oxidation, alcohol oxidation, phenol hydroxylation, cyclic ketone ammoxidation, and in the reaction, non-polluting low-concentration peroxidation can be used As an oxidizing agent, hydrogen has high reaction selectivity and has the incomparable advantages of energy saving, economy and environmental friendliness compared with traditional oxidation systems. As a catalyst for the selective oxidation of organic matter, titanium-silicon molecular siev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J37/02C07D301/04C07D303/04
Inventor 史春风林民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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