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Synthesis method of hollow titanium silicalite molecular sieve TS-1

A titanium-silicon molecular sieve, TS-1 technology, applied in molecular sieve catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve the problems of difficult to achieve meso-microporous composite, two-phase separation, unfavorable selective oxidation reaction, etc. High catalytic activity and stability, good stability, and the effect of improving diffusion performance

Active Publication Date: 2020-07-31
DALIAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The post-treatment method is to synthesize the TS-1 matrix first, and then treat it with an alkali solution to form a mesoporous or macroporous structure (Appl.Catal., A 2013,453,272), but during the alkali treatment, TS-1 Part of the active center framework titanium will be converted into non-framework titanium or anatase TiO 2 , which is unfavorable for the selective oxidation reaction
The one-step method is to add mesoporous and microporous templates to the synthesis system at the same time to synthesize mesoporous composite titanium-silicon molecular sieves (Ind. Eng. Chem. Res. 2017, 57, 512). Phase separation, it is difficult to achieve the purpose of mesoporous composite

Method used

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  • Synthesis method of hollow titanium silicalite molecular sieve TS-1
  • Synthesis method of hollow titanium silicalite molecular sieve TS-1
  • Synthesis method of hollow titanium silicalite molecular sieve TS-1

Examples

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Effect test

Embodiment 1

[0034] According to the method provided by the Chinese patent (CN95105343.4), weigh 22g of CaO into a three-necked flask, digest with 200g of water to form a lime emulsion, heat the water bath to 40℃, and under strong mechanical stirring, 500mL / min The flow rate passes into CO 2 , CO 2 With Ca(OH) 2 It reacts under highly turbulent conditions to produce ultrafine calcium carbonate particles. After reacting for 20 minutes, the pH of the suspension is 7-8. The suspension is filtered and the solid is dried to obtain ultrafine CaCO 3 , Its average particle size is about 70nm, denoted as CaCO 3 -A.

Embodiment 2

[0036] According to the method provided by the Chinese patent (CN01145312.5), weigh 50g of CaO into a three-necked flask, add 500mL of water at 95℃, stir evenly, and cool to obtain Ca(OH) 2 Raw material liquid. Roughly mix the raw material liquid with water to contain Ca 2+ 0.8mol / L Ca(OH) 2 Suspension, using EDTA complexometric titration to determine Ca(OH) 2 Ca in suspension 2+ The exact concentration. Take 200mL 0.8mol / L Ca(OH) 2 Suspension, add 8mL ammonia water, mix well, and pass CO at a flow rate of 50mL / min 2 The reaction temperature was 30°C, and the reaction was completed when the pH of the suspension reached 8.5. The morphology of the obtained calcium carbonate is spherical and the average particle size is about 150nm, which is recorded as CaCO 3 -B.

Embodiment 3

[0038] According to the method provided by the Chinese patent (CN104291366A), nano-magnesium carbonate is prepared. Prepare an ammonia solution with a concentration of 1mol / L and pass in a certain amount of CO 2 Gas to make NH 3 With CO 2 The molar ratio of is 2:1, then add 0.1g / L of nano-magnesium oxide crystal grains with an average particle size of 15nm, stir slowly, and get A solution; prepare MgCl with a concentration of 3mol / L 2 Solution, and add 1.4g / L ethylenediamine polyoxyethylene block polyether, 2.3g / L alkyl alcohol amide polyoxyethylene ether, 1.8g / L hydroxypropyl methylcellulose, and stir slowly Evenly, get B solution; at 65℃, slowly drop a certain amount of B solution into A solution, and finally maintain Mg 2+ :NH 4 + :CO 2 The molar ratio is 1:4:2. After the addition is completed, slowly stir for 10min, let stand for 45min, then filter under reduced pressure and repeatedly wash 5 times with absolute ethanol, and finally dry at 120℃ for 5h to obtain the average of...

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Abstract

The invention provides a preparation method of a hollow titanium silicalite molecular sieve TS-1. The preparation method comprises the following steps: firstly, preparing carbonate which can be dissolved in an acid solution but cannot be dissolved in water or an alkaline solution; then adding the carbonate into a synthesis system of the titanium silicalite molecular sieve TS-1, and preparing a molecular sieve MCO3@TS-1 with a core-shell structure by taking tetrapropylammonium hydroxide as a template agent, and adopting a dry glue conversion method; finally, carrying out acid treatment on the MCO3@TS-1 to remove the carbonate; washing, drying and roasting to obtain the hollow titanium silicalite molecular sieve TS-1. The hollow structure of the molecular sieve prepared by the method is morebeneficial to diffusion of macromolecules, so that the limitation of intrinsic micropore channels of the TS-1 molecular sieve on catalytic reaction is overcome, and non-framework titanium can be removed and the removal of the framework titanium is inhibited through acid treatment.

Description

Technical field [0001] The present invention relates to a preparation method of hollow titanium silicon molecular sieve TS-1. Background technique [0002] Zeolite molecular sieve is a crystalline porous material with uniform pores. It has the characteristics of high specific surface, flexible framework and controllable synthesis, making it widely used in catalysis, purification, adsorption, separation and other industrial fields. Titanium silicate molecular sieve TS-1 introduces transition metal titanium atoms into the molecular sieve framework with MFI topological structure to form a heteroatom molecular sieve with catalytic oxidation activity. Since the first report of the synthesis of titanium silicon molecular sieve TS-1 in 1983, US patent US4410501 has used titanium silicon molecular sieve as catalyst and H 2 O 2 It is a mild reaction system formed by oxidants. It exhibits high activity and high selectivity in the selective oxidation of olefin epoxidation, aromatic hydroxyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J37/00B01J37/02C07D301/12C07D303/04
CPCB01J29/89B01J37/0018B01J37/0221B01J37/0228B01J37/00C07D303/04C07D301/12B01J35/396Y02P20/52
Inventor 左轶李同辉郭新闻刘民
Owner DALIAN UNIV OF TECH