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Synthesis method of titanium silicalite TS-1

A titanium-silicon molecular sieve and a synthesis method technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of increasing the content of amorphous six-coordinate non-framework titanium, increasing the cost of TS-1 molecular sieve, poor effect of post-modification methods, etc. , to achieve the effect of inhibiting the formation of amorphous six-coordinate non-framework titanium, reducing acid centers, and relaxing purity requirements

Active Publication Date: 2012-01-18
DALIAN UNIV OF TECH
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  • Abstract
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  • Application Information

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Problems solved by technology

[0068] In conclusion, although the research on the synthesis of TS-1 has been carried out for nearly thirty years, the synthesis of high-quality TS-1 molecular sieves is still a major challenge. These challenges are mainly manifested in: tetrapropylammonium hydroxide as template The synthesis cost of molecular sieves in the synthesis system is high; the synthesis of TS-1 molecular sieves by replacing tetrapropylammonium hydroxide with other templates will increase the content of amorphous six-coordinated non-skeleton titanium, which is not conducive to catalytic applications; the effect of post-modification methods is poor And increase the cost of TS-1 molecular sieve

Method used

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  • Synthesis method of titanium silicalite TS-1
  • Synthesis method of titanium silicalite TS-1
  • Synthesis method of titanium silicalite TS-1

Examples

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Embodiment 1

[0109] Get 220ml deionized water and join in 225g silica sol (20%wt), and add 5.3g sodium sulfate, after stirring for 10 minutes, add 20.4g tetrapropylammonium bromide in the glue solution, continue to stir for 20 minutes, obtained Raw silicon solution; mix tetrabutyl titanate and acetylacetone at a mass ratio of 1:0.9, and stir for 15 minutes to obtain raw titanium; take 14.7ml of the prepared raw titanium solution and add it to the raw silicon solution, and stir for 30 minutes Finally, add 54ml of n-butylamine, continue to stir for 15 minutes to obtain a uniform gel; then add the resulting gel to a 2L stainless steel reactor, and crystallize for 48 hours under autogenous pressure at 170°C; the product is filtered by conventional methods, Wash until neutral, dry at 110°C, and bake at 540°C for 6 hours to remove the templating agent to obtain molecular sieve sample B.

[0110] Its Fourier transform infrared spectrum and figure 1 Similarly, in the infrared spectrum at 960cm -...

Embodiment 2

[0112] Take 220ml of deionized water and add it to 225g of silica sol (20%wt), and after stirring for 10 minutes, add 20.4g of tetrapropylammonium bromide to the glue solution, and continue stirring for 20 minutes to obtain a raw silicon solution; Tetrabutyl ester and acetylacetone were mixed at a mass ratio of 1:0.9 and stirred for 15 minutes to obtain raw titanium; 14.7ml of the prepared raw titanium solution was added to the raw silicon solution, and after stirring for 30 minutes, 5.3g of sodium sulfate was added , stirred for 5 minutes, added 54ml of n-butylamine, and continued to stir for 10 minutes to obtain a uniform gel; then the resulting gel was added to a 2L stainless steel reactor, and crystallized for 48 hours under autogenous pressure and 170°C; the product was purified by conventional methods Filter, wash until neutral, dry at 110°C, and bake at 540°C for 6 hours to remove the template agent to obtain a molecular sieve sample. The propylene epoxidation propertie...

Embodiment 3

[0115] Repeat embodiment 1, but wherein the add-on of sodium sulfate becomes 10.6g, 2.65g, 0.53g. That is, c=0.2, 0.05, 0.01, then molecular sieve samples C, D, E are obtained in sequence.

[0116] Its Fourier transform infrared spectrum is consistent with figure 1 Similarly, the UV-Vis spectrum and figure 2 (b) Similarly, the amorphous hexacoordinated non-skeleton content is significantly reduced. There is no absorption band of anatase at 330nm.

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Abstract

The invention belongs to the field of preparation of molecular sieve material, and discloses a synthesis method of a titanium silicalite TS-1. The method is characterized by comprising the following steps of: preparing a titanium-silicon gel with a silicon source, a titanium source, a template agent, an alkaline mineralizing agent and water according to certain proportion, and introducing right amount of alkali metal salt in the gel preparation process through a direction method or an indirection method; then, executing hydrothermal crystallization at 160-180 DEG C; and obtaining the titanium silicalite TS-1 after filtering, washing, drying and roasting. With the synthesis method provided by the invention, depolymerization of the silicon source can be promoted in the gel preparation process, so that titanium can enter into a skeleton smoothly and generation of amorphous six-coordinate non-skeleton titanium can be restrained. Based on the action of alkaline metal ions and an acid site of the molecular sieve non-skeleton titanium, the acid site of the cheap titanium silicalite TS-1 is removed, and selectivity of propylene epoxide is greatly improved while taking the titanium silicalite TS-1 as the catalyst for the propylene epoxidation.

Description

technical field [0001] The invention belongs to the field of molecular sieve material preparation, and relates to a method for synthesizing a titanium-silicon molecular sieve (TS-1) with an MFI structure. Background technique [0002] Titanium silicate molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. Among them, titanium silicalite-1 with MFI structure is referred to as TS-1. The catalytic system composed of TS-1 molecular sieve and dilute hydrogen peroxide is widely used in the field of selective oxidation, and has excellent selective oxidation reaction performance. The use of TS-1 molecular sieve in the oxidation reaction of organic matter avoids the problems of complex oxidation process and environmental pollution. It has the unparalleled advantages of energy saving, economy and environmental friendliness compared with traditional oxidation systems. It is considered as a milestone in zeolite catalysis in the 1980s . Therefore, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/06
Inventor 郭洪臣张蕾李海龙贾玉华刘春燕
Owner DALIAN UNIV OF TECH
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