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A kind of modification method of 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, physical/chemical process catalysts, etc., can solve the problems of poor stability, low effective utilization rate, low catalyst activity, etc., and achieve good stability, The effect of increasing the total titanium content and high selectivity

Active Publication Date: 2011-12-21
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 (can reach more than 95%). The main problems at present are low catalyst activity, poor stability, H 2 Low effective utilization

Method used

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  • A kind of modification method of titanium silicon molecular sieve

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preparation example Construction

[0022] In the preparation method provided by the present invention, the reducing agent described in step (1) is selected from one or more of hydrazine, borohydride, sodium citrate, wherein hydrazine can be hydrazine hydrate, hydrazine hydrochloride, hydrazine sulfate, The borohydride can be sodium borohydride, potassium borohydride.

[0023] In the modification method provided by the present invention, the order of adding titanium-silicon molecular sieve, titanium source, protective agent, palladium source, reducing agent and alkali source is preferably mixed with titanium-silicon molecular sieve, titanium source, protective agent, palladium source, A reducing agent is added to the solution of the alkali source.

[0024]In the modification method provided by the present invention, the hydrothermal treatment described in step (2) is carried out according to the existing hydrothermal treatment method in the synthesis of titanium-silicon molecular sieves or the modification of ti...

Embodiment 1

[0032] Take 20 grams of titanium-silicon molecular sieve TS-1, concentration of 0.01g / mL (calculated as palladium atom) ammonium nitrate palladium complex solution, TiCl 4 , hydrazine hydrate and cetyltrimethylammonium bromide are added to the aqueous solution (mass percentage concentration 10%) of tetrapropylammonium hydroxide and stirred evenly, wherein titanium silicon molecular sieve (gram): TiCl 4 (mol): hexadecyltrimethylammonium bromide (mol): tetrapropyl ammonium hydroxide (mol): ammonium nitrate palladium complex (gram, in palladium): hydrazine hydrate (mol): water ( mol)=100:0.1:0.005:0.5:2.0:3.0:1000. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 150°C and autogenous pressure for 48h, filter, wash, dry at room temperature, and then roast it in a nitrogen atmosphere at 550°C for 5h to obtain a modified microporous titanium-silicon molecular sieve, which is denoted as a.

Embodiment 2

[0034] Take 20 grams of titanium-silicon molecular sieve TS-1, a palladium chloride solution with a concentration of 0.01g / mL (calculated as palladium atoms), Ti(SO 4 ) 2 , hydrazine hydrochloride and polyacrylate are added to the aqueous solution of sodium hydroxide (mass percentage concentration 15%) and stirred evenly, wherein titanium silicon molecular sieve (gram): Ti(SO 4 ) 2 (mol): polyacrylate (mol): sodium hydroxide (mol): palladium chloride (gram, calculated as palladium): hydrazine hydrochloride (mol): water (mol) = 100: 0.5: 0.9: 1.0: 0.15: 0.1:1600. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at 180°C and autogenous pressure for 24h, filter, wash, dry at 110°C for 3h, and roast at 450°C for 5h in a nitrogen atmosphere to obtain the modified microporous titanium-silicon molecular sieve B .

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Abstract

A method for modifying titanium-silicon molecular sieves, comprising: mixing titanium-silicon molecular sieves, titanium sources, protective agents, alkali sources, precious metal sources, reducing agents, and water according to the ratio of 100: (0.001-1): (0.0001-5): (0.005-5 ): (0.005~10): (0.005~20): (500~10000) ratio mixing, and then the step of hydrothermal treatment; wherein the protective agent is selected from polybenzimidazole, polypropylene, polyethylene glycol, polyethylene One or more of styrene, polyvinyl chloride, polyethylene and their derivatives, anionic surfactants, cationic surfactants, nonionic surfactants, glucose and cyclodextrin, the reducing agent is selected from One or more of hydrazine, borohydride, sodium citrate. The modified molecular sieve obtained by the method has high skeleton titanium content, high oxidation activity and selectivity, and good 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 Patents(China)
IPC IPC(8): B01J29/89
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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