Method for adjusting pH value with oligosaccharide during synthesizing titanium silicalite molecular sieve (TS-1)

A titanium-silicon molecular sieve and synthesis process technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems that titanium-silicon molecular sieve is not easy to filter, products are easy to produce, etc., to optimize the state of titanium, facilitate aggregation, and reduce pH value. Effect

Inactive Publication Date: 2012-07-18
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems in the prior art that the prepared titanium-silicon molecular sieve is not easy to filter, and the product is easy to produce non-skeletal titanium, etc., the present invention proposes an acid-regulated titanium-silicon molecular sieve crystal that is release

Method used

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  • Method for adjusting pH value with oligosaccharide during synthesizing titanium silicalite molecular sieve (TS-1)
  • Method for adjusting pH value with oligosaccharide during synthesizing titanium silicalite molecular sieve (TS-1)
  • Method for adjusting pH value with oligosaccharide during synthesizing titanium silicalite molecular sieve (TS-1)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] (1) Prepare the synthetic serum of TS-1 according to the method of Comparative Example 1, and the molar ratio of each component is: 1TEOS:0.025TBOT:0.35TPAOH:20H 2 O, its pH is 10-11.

[0064] (2) Dissolving sucrose in water to obtain an aqueous solution of sucrose. Wherein, the molar ratio of sucrose to TEOS is 0.10, and the molar ratio of water to TEOS is 5.

[0065] (3) Add the synthetic serum of TS-1 prepared in step (1) into the aqueous solution of sucrose, and stir evenly at room temperature to obtain a clear mixed solution of titanium-silicon precursor and sucrose.

[0066] (4) The mixture of titanium silicon precursor and sucrose obtained in step (3) was statically crystallized at 185° C. for 7 days. After the reaction, the pH of the obtained mixed solution is 8-9. The product was directly filtered, washed with distilled water until the pH was about 7, and dried at 100°C to obtain the original powder of TS-1 molecular sieve.

[0067] (5) After calcining ...

Embodiment 2

[0073] (1) Prepare the synthetic serum of TS-1 according to the method of Comparative Example 1, and the molar ratio of each component is: 1TEOS:0.025TBOT:0.35TPAOH:20H 2 O.

[0074] (2) Dissolving sucrose in water to obtain an aqueous solution of sucrose. Wherein, the molar ratio of sucrose to TEOS is 0.10, and the molar ratio of water to TEOS is 5.

[0075] (3) Add the synthetic serum of TS-1 prepared in step (1) into the aqueous solution of sucrose, and stir evenly at room temperature to obtain a clear mixed solution of titanium-silicon precursor and sucrose.

[0076] (4) statically crystallize the mixture of titanium-silicon precursor and sucrose obtained in step (3) at 185° C. for 1 day, and the pH of the pre-crystallization solution is 8-9.

[0077] (5) Add a certain amount of sucrose to the pre-crystallization solution in step (4). Wherein, the molar ratio of sucrose to TEOS is 0.10.

[0078] (6) The mixed solution obtained in step (5) was statically crystallized at...

Embodiment 3

[0083] (1) Prepare the synthetic serum of TS-1 according to the method of Comparative Example 1, and the molar ratio of each component is: 1TEOS:0.025TBOT:0.35TPAOH:20H 2 O.

[0084] (2) Dissolving sucrose in water to obtain an aqueous solution of sucrose. Wherein, the molar ratio of sucrose to TEOS is 0.10, and the molar ratio of water to TEOS is 5.

[0085] (3) Add the synthetic serum of TS-1 prepared in step (1) into the aqueous solution of sucrose, and stir evenly at room temperature to obtain a clear mixed solution of titanium-silicon precursor and sucrose.

[0086] (4) statically crystallize the mixture of titanium silicon precursor and sucrose obtained in step (3) at 185° C. for 2 days, and the pH of the precrystallization solution is 8-9.

[0087] (5) Add a certain amount of sucrose to the pre-crystallization solution in step (4). Wherein, the molar ratio of sucrose to TEOS is 0.10.

[0088] (6) The mixed solution obtained in step (5) was statically crystallized at...

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Abstract

The invention discloses a method for adjusting a pH value with oligosaccharide during synthesizing TS-1. Oligosaccharide is added at the crystallization phase of a TS-1 synthesis process, and the acid released from carbonization of the oligosaccharide under a hydrothermal condition is used for adjusting the pH value. In the invention, the oligosaccharide is added in one time before crystallization of a TS-1 synthesis clear liquid, or in batches during the crystallization phase. The TS-1 synthesized by the invention is free of penetrating filtration phenomenon and is difficult to generate non-framework titanium.

Description

technical field [0001] The invention relates to a titanium-silicon molecular sieve TS-1, in particular to a method for adjusting pH value by utilizing oligosaccharide carbonization during the synthesis process of the titanium-silicon molecular sieve TS-1. Background technique [0002] Zeolite molecular sieves are widely used in petrochemical, fine chemical, environmental protection, gas separation and adsorption and many other fields due to their regular and orderly pore structure, large pore volume and specific surface area. The introduction of some catalytically active heteroatoms into the zeolite molecular sieve can make the molecular sieve have some special catalytic properties. In 1983, Taramasso et al. reported for the first time that transition metal titanium atoms could be introduced into the framework of pure silicon molecular sieve (silicalite-1) (US Patent 4410501), and this molecular sieve containing framework titanium atoms was named TS-1 (Titanium silicalite-1)...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 王一萌何建琴
Owner EAST CHINA NORMAL UNIV
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