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Method for modifying titanium-silicon zeolite material

A titanium silicalite modification technology, which is applied in the field of modification of titanium silicalite materials, can solve the problems of low activity, easy deactivation, poor selectivity and activity stability of titanium silicalite, and achieve good catalytic activity stability, Effect of Catalytic Oxidation Activity Improvement

Active Publication Date: 2012-08-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the titanium silicalite obtained by the current synthesis method generally has problems such as low activity, poor selectivity and activity stability, or easy deactivation.

Method used

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  • Method for modifying titanium-silicon zeolite material
  • Method for modifying titanium-silicon zeolite material
  • Method for modifying titanium-silicon zeolite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 20 grams of titanium silicalite TS-1 into the tetrapropyl ammonium hydroxide aqueous solution containing sucrose and stir and mix evenly, wherein titanium silicalite (gram): sucrose (mol): tetrapropyl ammonium hydroxide (mol): water (g) = 100:0.2:0.05:600. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at 100°C and autogenous pressure for 8 hours, and then hydrothermally treat it at 150°C and autogenous pressure for 48 hours, filter the resultant, wash with water, dry naturally, and heat at 580°C The modified titanium silicalite material A was obtained by calcining at low temperature for 3 hours.

[0034] The XRD crystal phase diagram of A is as follows figure 1 Shown in Curve B. The Fourier transform infrared spectrum of A is as follows figure 2 As shown in curve b, at 960cm -1 The infrared absorption peak that all-silicon molecular sieves do not have appears nearby, indicating that titanium has entered the molecular sieve f...

Embodiment 2

[0036] Add 20 grams of titanium silicalite TS-1 into the sodium hydroxide aqueous solution containing starch and stir and mix evenly, wherein titanium silicalite (gram):starch (mol):sodium hydroxide (mol):water (gram)=100: 0.01:1.2:3500. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 110°C and an autogenous pressure for 4 hours, and treat it at a temperature of 180°C and an autogenous pressure for 24 hours. Roast for 3 hours to obtain the modified titanium silicalite material B.

[0037] The XRD crystal phase diagram of B is as follows figure 1 Curve C is shown. The Fourier transform infrared spectrum of B is as follows figure 2 As shown in curve c, at 960cm -1 The infrared absorption peak that all-silicon molecular sieves do not have appears nearby, indicating that titanium has entered the molecular sieve frame, 960cm -1 Absorption peak at and 550cm -1 Absorption peak intensity ratio I 960 / I 550 The data are li...

Embodiment 3

[0039] Add 20 grams of titanium silicalite TS-1 into the tetrapropyl ammonium hydroxide aqueous solution containing furfural and stir and mix evenly, wherein titanium silicalite (gram): furfural (mol): tetrapropyl ammonium hydroxide (mol): water (gram)=100:0.04:1.0:1200. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 120°C and an autogenous pressure for 10 hours, then hydrothermally treat it at a temperature of 170°C and an autogenous pressure for 48 hours, filter the resultant, wash it with water, dry it naturally, and heat it at 480 The modified titanium silicalite material C was obtained by roasting at 8°C for 8 hours.

[0040] The XRD crystal phase diagram of C has figure 1 Characteristic of Curve A. Infrared spectrum of C 960cm -1 Absorption peak at and 550cm -1 Absorption peak intensity ratio I 960 / I 550 The data are listed in Table 1. The UV-Vis spectrum of C has image 3 The characteristics of curve ii ha...

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Abstract

The invention discloses a method for modifying a titanium-silicon zeolite material. The method comprises the following steps of: adding titanium-silicon zeolite into aqueous solution of pore-forming agent and alkali source, then treating the obtained mixture in a closed reaction kettle under a hydrothermal treatment condition, and reclaiming a product to obtain the modified titanium-silicon zeolite material. According to the modifying method, the titanium-silicon zeolite material is favorable for adsorption and diffusion of the reactants and the product, and the active center thereof is easily contacted. Compared with the prior art, in oxidation reaction, the titanium-silicon zeolite material obtained by adopting the modifying method has the advantages of shortened reaction induction period, high oxidation activity and good stability.

Description

technical field [0001] The invention relates to a modification method of a titanium silicalite material. Background technique [0002] Titanium silicalite is a new type of heteroatom zeolite developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MEL structure, MCM-22 with MWW structure and TS-48 with larger pore structure have been synthesized. Among them, the titanium silicalite TS-1 developed and synthesized by Italy Enichem Company is a new type of titanium silicalite with excellent catalytic selective oxidation performance formed by introducing transition metal element titanium into the zeolite framework with ZSM-5 structure. TS-1 not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 zeolite. Using this titanium silicalite as a catalyst can catalyze various types of organic oxidation reactions, such as epoxidation of alkenes, partial oxidation of alkanes, oxidation of alco...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/02C01B39/08
Inventor 史春风林民朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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