Synthetic method of Ti-beta molecular sieve

A technology of β molecular sieve and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of molecular diffusion of unfavorable reactants, large amount of template agent, large grain size of Ti-β molecular sieve, etc., and achieve simple process flow and relative The effect of high crystallinity and high thermal stability

Active Publication Date: 2009-01-28
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0015] The direct hydrothermal method for synthesizing Ti-β molecular sieves produces a large amount of non-skeleton Ti due to the strong hydrolysis of titanium alkoxide, which will reduce the catalytic oxidation activity of the synthesized Ti-β molecular sieves; in addition, the synthesized Ti-β molecular sieves There are many defects in the unit cell structure, resulting in poor stability and hydrophobicity. The large amount of template agent makes the cost high, and the generated Ti-β molecular sieve has large grain size, which is not conducive to the diffusion of reactant molecules.

Method used

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  • Synthetic method of Ti-beta molecular sieve

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) According to SiO 2 :TiO 2 : Alcohol=1:0.0125:4.0 molar ratio Mix ethyl silicate, tetrabutyl titanate and tert-butanol evenly, and then slowly add NaOH solution dropwise to it under the condition of constant stirring, so that the molar ratio in the system For: SiO 2 :TiO 2 :Na 2 O:H 2 O=1:0.0125:0.026:6.5, and after reacting at room temperature, the mixture solution was roasted at 700°C for 3 hours, and then the sample obtained after roasting was ground into small particles, washed, filtered, and dried to obtain Ti's two-dimensional layered hydrodistalite;

[0046] (2) According to SiO 2 : templating agent: water = 1: 0.5: 6.0 molar ratio will be hydrodistalite (with SiO 2 ), the template agent TEAF was mixed with water and then crystallized at 140°C for 4 days to synthesize Ti-β molecular sieve;

[0047] (3) The titanium silicon molecular sieve raw powder obtained in step (2) and the acetic acid solution of 4mol / l are prepared into a reaction mixture accordi...

Embodiment 2

[0051] (1) According to SiO 2 :TiO 2 : Alcohol=1:0.033:4.0 molar ratio Mix ethyl silicate, tetrabutyl titanate and tert-butanol evenly, and then slowly add NaOH solution dropwise therein under constant stirring, so that the molar ratio in the system For: SiO 2 :TiO 2 :Na 2 O:H 2 O=1:0.033:0.052:13.5, and after reacting at room temperature, the mixture solution was roasted at 650°C for 5 hours, and then the sample obtained after roasting was ground into small particles, washed, filtered, and dried to obtain Ti's two-dimensional layered hydrodistalite;

[0052] (2) According to SiO 2 :TEAOH:(NH 4 ) 2 SiF 6 : Water = 1: 0.95: 0.317: 8.0 molar ratio will be hydrodisoblastite (as SiO 2 meter), templating agent (TEAOH and (NH 4 ) 2 SiF 6 ) mixed with water and crystallized at 120°C for 7 days to synthesize Ti-β molecular sieve;

[0053] (3) The titanium silicon molecular sieve raw powder obtained in step (2) and 8mol / L citric acid solution are prepared in a weight rati...

Embodiment 3

[0057] (1) According to SiO 2 :TiO 2 : Alcohol = 1:0.017:6.0 molar ratio Mix ethyl silicate, tetrabutyl titanate and tert-butanol evenly, and then slowly add NaOH solution dropwise under constant stirring, so that the molar ratio in the system For: SiO 2 :TiO 2 :Na 2 O:H 2 O=1:0.017:0.037:10.5, and after reacting at room temperature, the mixture solution was roasted at 750°C for 3 hours, and then the sample obtained after roasting was ground into small particles, washed, filtered, and dried to obtain Ti's two-dimensional layered hydrodistalite;

[0058] (2) According to SiO 2 :TEAOH:HF:Water=1:0.1:0.15:2.0

[0059] The molar ratio of hydrodistalite (as SiO 2 ), templating agents (TEAOH and HF) were mixed with water and then dynamically crystallized at 170°C for 2 days to synthesize Ti-β molecular sieves;

[0060] (3) The titanium-silicon molecular sieve raw powder obtained in step (2) and 6mol / L nitric acid solution were prepared in a weight ratio of 1:15 to prepare a...

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Abstract

A synthetic method of TI-beta zeolite comprises the steps as follows: (1) silicate ester, titanate ester and butanol are evenly mixed according to the mol ratio that SiO2: TiO2: alcohol equals 1: (0.01-0.05): (4.0-15.0), and then NaOH solution is added for reaction at the room temperature of 120 DEG C, and kanemite is obtained by roasting; (2) the kanemite (counted based on SiO2), a template agent and water are evenly mixed according to the mol ratio that the SiO2: the template agent: the water equals 1: (0.1-1.0): (2.0-8.0) at the temperature of 120-170 DEG C, and crystallized for 2-15 days to obtain raw powder of a titanium silicalite molecular sieve with BEA skeleton structure; (3) the raw powder of the titanium silicalite molecular sieve obtained in the step (2) is washed by acid; and (4) the product washed by acid is roasted to obtain a Ti-beta molecular sieve product. The Ti-beta molecular sieve synthesized by the method in the invention contains little non-skeleton Ti, contains no Al, and is characterized by high relative crystallinity, few structural defects, good thermal stability, and nano crystal grain dimension.

Description

technical field [0001] The invention relates to a synthesis method of a β molecular sieve, in particular to a synthesis method of a Ti-β molecular sieve. Background technique [0002] Mesoporous titanium-silicon molecular sieve (TS-1) is used to catalyze various oxidation reactions, especially in the selective oxidation of organic matter with the participation of hydrogen peroxide, which has excellent catalytic performance. However, its pore size is only 5.4nm, which limits the application of TS-1 in catalyzing the oxidation reaction of macromolecular reactants. The preparation of titanium-containing molecular sieves with larger pore sizes, such as Ti-β molecular sieves with a BEA framework structure, can improve the catalytic performance of epoxidation of macromolecular reactants and expand the application range of titanium-containing zeolites. For example, Ti-β zeolite with a BEA framework structure has excellent catalytic performance in the epoxidation reaction of macrom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/08
Inventor 王志光宋家庆何鸣元
Owner CHINA PETROLEUM & CHEM CORP
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