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Method for preparing titanium silicon molecular sieve

A technology of titanium-silicon molecular sieve and titanium source, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolite, etc., can solve the problem of long crystallization time of titanium-silicon molecular sieve, unsatisfactory effect, long pre-synthesis time, etc. problem, achieve the effect of improving synthesis efficiency and benefit, reducing preparation cost, and shortening crystallization time

Active Publication Date: 2012-12-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] In the existing technology for preparing titanium-silicon molecular sieves (such as GB 2071071A, USP 4410501, and Zeolites, 1992, Vol.12: 943), it is necessary to heat and remove alcohol during the early synthesis, so that the early synthesis time is relatively long; at the same time, due to The crystallization ability of Ti itself is weak, which makes the crystallization time for preparing titanium silicon molecular sieves longer
In recent years, although through certain improvement (as CN101134575A, CN1247771A), effect is not very satisfactory

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preparation example Construction

[0009] The preparation method of the titanium-silicon molecular sieve provided by the present invention is to add an accelerator to the synthetic mother liquor of the titanium-silicon molecular sieve, and then introduce an alkali source template agent to hydrolyze the organic silicate and the titanium source, and finally hydrothermally crystallize the mixture, and recover the product.

[0010] In the method provided by the invention, its general formula of said organosilicate is R 1 4 SiO 4 , where R 1 Preferably an alkyl group with 1 to 4 carbon atoms, more preferably R 1 For ethyl.

[0011] In the method provided by the present invention, the titanium source is an inorganic titanium salt or an organic titanate, preferably an organic titanate. Said inorganic titanium salt can be TiCl 4 , Ti(SO 4 ) 2 or TiOCl 2 ; Its general formula of said organic titanate is Ti(OR 2 ) 4 , where R 2 is an alkyl group having 1 to 6 carbon atoms, preferred R 2 is an alkyl group hav...

Embodiment 1

[0027] At 60°C, firstly mix tetraethyl orthosilicate and tetrabutyl titanate evenly, then add accelerator Keggin phosphotungstic heteropoly acid to the resulting mixture, then add tetrapropylammonium hydroxide aqueous solution, wait The mixed solution is hydrolyzed to obtain the molar composition of tetraethyl orthosilicate in the reaction system: tetrabutyl titanate: tetrapropyl ammonium hydroxide: accelerator: water = 100: 5: 10: 0.005: 200, wherein orthosilicate Acid Tetraethyl Ester as SiO 2 In terms of tetrabutyl titanate as TiO 2 Then put the mixed solution into a stainless steel sealed reaction kettle, and crystallize it at a temperature of 170°C and an autogenous pressure for 12 hours, filter the resulting crystallized product, wash it with water, and dry it at 110°C for 120 minutes, then heat it at 550°C Calcined at high temperature for 3 hours to obtain molecular sieves. Its XRD crystal phase diagram is consistent with the comparative example, indicating that the T...

Embodiment 2

[0029] At a temperature of 80°C, firstly mix tetraethyl orthosilicate and tetrabutyl titanate evenly, then add accelerator Keggin molybdotungstic heteropolyacid to the resulting mixture, and then add tetrapropylammonium hydroxide aqueous solution, The mixed solution is to be hydrolyzed so that the molar composition of the reaction system is tetraethyl orthosilicate: tetrabutyl titanate: tetrapropylammonium hydroxide: accelerator: water = 100: 2: 15: 0.001: 100, wherein orthosilicate Acid Tetraethyl Ester as SiO 2 In terms of tetrabutyl titanate as TiO 2 Then the mixed solution was put into a stainless steel sealed reaction vessel, and crystallized at a temperature of 170° C. and autogenous pressure for 6 hours, and then the crystallized product was recovered according to the method of Example 1 to obtain a molecular sieve. Its XRD crystal phase diagram is consistent with the comparative example, indicating that what is obtained is a TS-1 molecular sieve with MFI structure; -...

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Abstract

The invention relates to a method for preparing a titanium silicon molecular sieve. The method is characterized by comprising the following steps of: within a temperature range from 40 DEG C to 90 DEG C, mixing an organic silicate ester with a titanium source, adding an accelerating agent and introducing an alkali source template to hydrolyze the organic silicate ester and the titanium source so as to obtain a mixture; hydrothermally crystallizing the mixture in a reaction kettle for 6-36 hours at 120-200 DEG C; and taking a product out and recycling to obtain a TS-1 titanium silicon molecular sieve, wherein the mole ratio of the organic silicate ester to the titanium source to the alkali source template to the accelerating agent to the water in the mixture is 100:(0.005-50.0):(0.005-20.0):(0.0005-5.0):(20-1,000); the organic silicate ester is counted in terms of SiO2; the titanium source is counted in terms of TiO2; and the accelerating agent is polymetallic oxyacid or salt thereof. According to the method, the amount of the used accelerating agent is reduced, the amount of the used template is reduced and the preparation cost is lowered; besides, the time for hydrolyzing and crystallizing the silicon source and the titanium source is shortened, and generally the crystallization can be completed within 6 to 12 hours.

Description

technical field [0001] The invention relates to a preparation method of a titanium silicalite molecular sieve, in particular to a preparation method of a titanium silicalite molecular sieve (TS-1) with an MFI structure. Background technique [0002] Titanium silicalite molecular sieve is a new heteroatom molecular sieve developed in the early 1980s. TS-1 with MFI structure, TS-2 with MEL structure, and TS-48 with larger pore structure have been synthesized so far. This type of molecular sieve has excellent selective oxidation performance and high catalytic activity for many organic oxidation reactions, such as epoxidation of olefins, hydroxylation of aromatic hydrocarbons, oximation of cyclohexanone, and oxidation of alcohols. -ox) type molecular sieve catalysts have good application prospects. [0003] TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transition metal eleme...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08B01J29/89
Inventor 史春风林民朱斌慕旭宏罗一斌龙立华汝迎春
Owner CHINA PETROLEUM & CHEM CORP