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Method for preparing titanium silicon molecular sieve TS-1 with high framework titanium content

A technology of titanium-silicon molecular sieve and skeleton titanium, which is applied in the direction of molecular sieve compounds, molecular sieve characteristic silicates, molecular sieves and alkali exchange compounds, etc., can solve the problems of unavoidable non-skeleton titanium and low skeleton titanium content, so as to reduce cost input, Reduced synthesis cost and stable structure

Active Publication Date: 2017-08-11
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to solve the existing problems in the existing synthesis technology of titanium-silicon molecular sieve TS-1, such as the low content of skeleton titanium and the difficulty in avoiding the generation of non-skeleton titanium in the hydrothermal synthesis process.

Method used

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  • Method for preparing titanium silicon molecular sieve TS-1 with high framework titanium content
  • Method for preparing titanium silicon molecular sieve TS-1 with high framework titanium content
  • Method for preparing titanium silicon molecular sieve TS-1 with high framework titanium content

Examples

Experimental program
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Embodiment 1

[0050] Add 20.3g of methyl orthosilicate into a jacketed three-necked flask, sequentially add 0.78g of tetraethyl titanate and 42.1g of 25wt% tetrapropylammonium hydroxide solution, immerse the three-necked flask in a 40°C water bath, and hydrolyze for 1.5 h. The hydrolyzate was dealcoholized at 90°C for 1 hour, 180mL of starch solution with a concentration of 5wt% was added, stirred evenly, the mixed solution was put into a crystallization kettle, and crystallized at 160°C for 48h, the crystallized product was washed and dried, Calcined at 540°C for 6 hours to obtain TS-1, which is numbered TS-1-E.

[0051] image 3 It is the scanning electron micrograph of the titanium-silicon molecular sieve TS-1-E that embodiment 1 makes, as can be seen from the figure, the morphology of the sample that the present embodiment makes and figure 1 Very similar, ellipsoidal, particle size is about 200nm.

[0052] Depend on Figure 5 It can be seen that the sample TS-1-E synthesized accordi...

Embodiment 2

[0055] Add 29.6g of ethyl orthosilicate into a jacketed three-necked flask, sequentially add 1.60g of tetrabutyl titanate and 33.6g of 25wt% tetrapropylammonium hydroxide solution, immerse the three-necked flask in a 50°C water bath, and hydrolyze for 3 hours . The hydrolyzate was dealcoholized at 90°C for 1 hour, 100mL of starch solution with a concentration of 5wt% was added, stirred evenly, the mixed solution was put into a crystallization kettle, and crystallized at 170°C for 60h, the crystallized product was washed and dried, Calcined at 540°C for 5 hours to obtain TS-1, which is numbered TS-1-F.

[0056] Figure 4 It is the scanning electron micrograph of the titanium-silicon molecular sieve TS-1-F that embodiment 2 makes, as can be seen from the figure, the morphology of the sample that the present embodiment makes and figure 1 Very similar, ellipsoidal, particle size is about 200nm.

[0057] Depend on Figure 5 It can be seen that the sample TS-1-F synthesized acco...

Embodiment 3

[0060] Add 20.8 g of ethyl orthosilicate into a jacketed three-necked flask, sequentially add 0.96 g of tetrabutyl titanate and 9.8 g of 40 wt % tetraethylammonium hydroxide solution, immerse the three-necked flask in a 50° C. water bath, and hydrolyze for 1 h. The hydrolyzate was dealcoholized at 90°C for 0.5h, and 90mL of starch solution with a concentration of 8wt% was added, stirred evenly, and the mixed solution was put into a crystallization kettle, and crystallized at 150°C for 72h, and the crystallized product was washed and dried. Calcined at 540°C for 3 hours to obtain TS-1, which is numbered TS-1-G.

[0061] Depend on Figure 5 It can be seen that the sample TS-1-G synthesized according to Example 3 only contains framework titanium, and does not contain hexacoordinated non-framework titanium and anatase TiO 2 .

[0062] Depend on Image 6 It can be seen that the TS-1-G synthesized according to Example 1 also has a typical MFI structure, and the crystallinity of t...

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Abstract

The invention provides a method for preparing a titanium silicon molecular sieve TS-1 with high framework titanium content. The method particularly comprises the following steps: mixing a silicon source and a titanium source according to the proportion, and adding an aqueous solution of quaternary ammonium base to obtain mixed liquid; hydrolyzing the mixed liquid to remove alcohol, adding a starch solution and performing crystallization to obtain a crystallization product; and drying and roasting the crystallization product to obtain the titanium silicon molecular sieve TS-1 with high framework titanium content. According to the method, the starch solution is added in the synthesis process, the silicon source is in bridge connection with the titanium source by utilizing a large amount of hydroxyl groups in the starch, and the silicon source and the titanium source are easy to combine, so that more titanium can enter the TS-1 framework. The titanium silicon molecular sieve prepared with the method has high titanium content and hardly contains extra-framework titanium, and mother liquid can be recycled.

Description

technical field [0001] The invention relates to the technical field of catalyst synthesis, in particular to a method for synthesizing titanium-silicon molecular sieve TS-1 with high skeleton titanium content. Background technique [0002] Since the synthesis of titanium-silicon molecular sieve TS-1 was first reported in US Patent US4410501 in 1983, its oxidation system with hydrogen peroxide has shown high activity for olefin epoxidation, aromatic hydrocarbon hydroxylation, and ketone ammoxidation. Moreover, the by-product is water, which belongs to an environmentally friendly process, so it has attracted widespread attention. [0003] The main catalytic oxidation active center on the titanium-silicon molecular sieve is the four-coordinated framework titanium. However, the content of this titanium species cannot be increased arbitrarily, because the crystal lattice expands when titanium enters, thereby inhibiting more titanium from entering the framework. Titanium species e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C01B37/00
CPCC01B37/005C01B39/085C01P2002/72C01P2002/84C01P2004/03C01P2004/32C01P2004/62C01P2004/64
Inventor 左轶郭新闻刘民张廷刘准
Owner DALIAN UNIV OF TECH
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