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Granular titanium-silicon molecular sieve catalyst and preparation method thereof

A titanium-silicon molecular sieve and catalyst technology, applied in molecular sieve catalysts, catalyst activation/preparation, chemical instruments and methods, etc., can solve the problems of difficult separation, easy breakage, low strength, etc., and achieve easy separation, difficult to crush, and large particle size. Effect

Inactive Publication Date: 2009-12-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In summary, due to the low strength of the granular titanium-silicon molecular sieve catalyst prepared by the existing method for preparing granular titanium-silicon molecular sieve, it is easy to break when used in a slurry reactor due to stirring, and it is not easy to separate after the reaction; or because the titanium-silicon molecular sieve Some of the active centers are covered, resulting in a decline in catalytic performance, unable to meet the application requirements

Method used

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  • Granular titanium-silicon molecular sieve catalyst and preparation method thereof
  • Granular titanium-silicon molecular sieve catalyst and preparation method thereof
  • Granular titanium-silicon molecular sieve catalyst and preparation method thereof

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Embodiment 1

[0031] A method for preparing a granular titanium-silicon molecular sieve catalyst, comprising the following steps:

[0032] (1) According to the mass ratio of 1:1:0.5:0.5:1: titanium silicon molecular sieve (TS-1) fine powder, tetraethyl silicate (TEOS), ethylene glycol-propylene glycol-ethylene glycol copolymer Compound (P123, average molecular weight 5800), mass percent concentration are 36% hydrochloric acid and water;

[0033] (2) Add hydrochloric acid into water, add P123 under stirring, after P123 dissolves, add TEOS dropwise, after TEOS is completely hydrolyzed (from milky to transparent), add TS-1 fine powder and mix to form a slurry;

[0034] (3) Calcining the slurry in air at 550° C. for 30 hours to obtain a granular titanium-silicon molecular sieve catalyst.

[0035] The particle diameter of the granular titanium-silicon molecular sieve catalyst is 5 μm to 75 μm. Nitrogen physical adsorption and desorption isotherms (see figure 1 ) shows a hysteresis loop, which...

Embodiment 2

[0037] The granular titanium-silicon molecular sieve catalyst prepared by Example 1 is used to catalyze the epoxidation reaction of propylene, and the experimental steps are as follows: the reaction is carried out at 120 cm 3 in a high-pressure reactor. Water bath heating, magnetic stirring, the reaction kettle is equipped with a water cooling device. Add 32cm to the reactor 3 Methanol, the granular titanium silicon molecular sieve catalyst that 0.40g prepares with embodiment 1, the hydrogen peroxide (H of 3.60g (30wt.%) 2 o 2 ) and 1.30 g of methyl tert-butyl ether (MTBE), heated to 40° C. in a water bath, passed through propylene to maintain the reaction pressure at 0.4 MPa, and the stirring speed was 1000 rpm, and the reaction was carried out for 1.5 h.

[0038] After the reaction, the product is separated from the catalyst with a centrifuge, analyzed by HP4890 gas chromatography, the FID detector, the chromatographic column is SE-54 (30m × 0.25mm × 0.33 μm), and the met...

Embodiment 3

[0044] A method for preparing a granular titanium-silicon molecular sieve catalyst, comprising the following steps:

[0045] (1) According to the mass ratio of 1:1:1.4:0.2:1: TS-1 fine powder, TEOS, P123 (average molecular weight 5800), hydrochloric acid and water with a mass percentage concentration of 36%;

[0046] (2) Add hydrochloric acid into water, add P123 under stirring, after P123 dissolves, add TEOS dropwise, after TEOS is completely hydrolyzed (from milky to transparent), add TS-1 fine powder and mix to form a slurry;

[0047](3) Calcining the slurry in air at 500° C. for 30 hours to obtain a granular titanium-silicon molecular sieve catalyst.

[0048] The particle diameter of the granular titanium-silicon molecular sieve catalyst is 5 μm to 70 μm. Nitrogen physical adsorption and desorption isotherms (see image 3 ) shows a hysteresis ring, indicating that the silica gel except TS-1 fine powder exists in the form of mesopores.

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Abstract

The invention discloses a granular titanium-silicon molecular sieve catalyst and a preparation method thereof. The granular titanium-silicon molecular sieve catalyst is prepared by using the following method: hydrochloric acid is added into water, the mixture is stirred and added with a glycol-propylene glycol-glycol copolymer, ethyl orthosilicate is dropped after the glycol-propylene glycol-glycol copolymer is dissolved, titanium-silicon molecular sieve fine powder is added into the mixture after the ethyl orthosilicate is completely hydrolyzed to be evenly mixed into a slurry state substance; and the slurry state substance is calcined for 5 to 30 hours in the air at 500 to 950 DEG C to obtain the granular titanium-silicon molecular sieve catalyst which has a middle hole, is covered with a silica gel layer and has a particle diameter of 5mu m to 75mu m. The granular titanium-silicon molecular sieve catalyst prepared by the invention has large particle diameter and high strength, is not easy to pulverize, is easy to separate after catalyzed reaction is completed, keeps the catalysis property of the titanium-silicon molecular sieve fine powder and is used for preparing propylene oxide by catalyzing propylene ring oxidation, and the oxydol conversion rate and the propylene oxide selectivity of the granular titanium-silicon molecular sieve catalyst approach to those of titanium-silicon molecular sieve fine powder.

Description

technical field [0001] The invention relates to a titanium-silicon molecular sieve catalyst and a preparation method, in particular to a granular titanium-silicon molecular sieve catalyst and a preparation method. Background technique [0002] Titanium silicate molecular sieve (TS-1) is a new type of catalytic oxidation catalyst, which can be used to catalyze the epoxidation of olefins to prepare olefin epoxides, catalyze the ammoximation of ketones to prepare the corresponding ketoximes, and catalyze the oxidation of phenols to prepare the corresponding quinone etc. The oxidation reaction catalyzed by titanium-silicon molecular sieve has high product selectivity and few by-products. [0003] Titanium-silicon molecular sieve fine powder is synthesized by using tetrapropylammonium hydroxide as template, titanate as titanium source, and tetraethyl silicate as silicon source, with a particle size of 0.1-0.3 μm (US4410501A, CN1191125C, CN1234683C). The catalytic performance of...

Claims

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Application Information

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IPC IPC(8): B01J29/89B01J35/02B01J37/00C07D303/04C07D301/12
CPCY02P20/52
Inventor 王亚权孟凡会张宇王磊
Owner TIANJIN UNIV
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