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Titanium-silicon material with core-shell structure and its preparation method and method for producing epoxy compound by oxidation reaction of macromolecular olefin

A core-shell structure, titanium-silicon molecular sieve technology, applied in molecular sieves and alkali exchange compounds, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of reducing the number of catalytic active centers, low catalytic activity, waste of raw materials, etc. Conversion rate and target product selectivity, high catalytic activity, and the effect of improving utilization

Active Publication Date: 2022-03-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this process, there are many factors that affect the insertion of titanium into the framework, the conditions of hydrolysis, crystallization nucleation, and crystal growth are not easy to control, and there is a certain amount of titanium that cannot be effectively inserted into the molecular sieve framework and stays in the channel in the form of non-skeleton titanium. The production of non-skeletal titanium not only reduces the number of catalytic active centers, but also non-skeletal titanium-silicon species will promote the ineffective decomposition of hydrogen peroxide, resulting in waste of raw materials. Therefore, the TS-1 molecular sieve synthesized by this method has low catalytic activity, poor stability, and difficult to reproduce.

Method used

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  • Titanium-silicon material with core-shell structure and its preparation method and method for producing epoxy compound by oxidation reaction of macromolecular olefin
  • Titanium-silicon material with core-shell structure and its preparation method and method for producing epoxy compound by oxidation reaction of macromolecular olefin
  • Titanium-silicon material with core-shell structure and its preparation method and method for producing epoxy compound by oxidation reaction of macromolecular olefin

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Embodiment approach

[0083] A specific embodiment, the macromolecular olefin may be cyclohexene, cyclooctene, styrene or limonene.

[0084] The present disclosure is further illustrated by the following examples, but the present disclosure is not limited thereby.

[0085] In the examples and comparative examples, the surface titanium-silicon ratio and the bulk phase titanium-silicon ratio of the titanium-silicon molecular sieve are measured by the transmission electron microscope-energy dispersive X-ray spectroscopic elemental analysis (TEM-EDX) method (photo as figure 2 shown). First, the samples were dispersed with ethanol to ensure that the crystal grains do not overlap, and then loaded on the copper grid. When dispersing, the amount of sample should be as small as possible so that the particles do not overlap together, and then observe the shape of the sample through a transmission electron microscope (TEM), randomly select a single isolated particle in the field of view and make a straight...

Embodiment 1

[0095] Titanium silicate molecular sieves were prepared as follows, marked as RTTS-1:

[0096] a. The first structure directing agent A (C 22-6-6-1-1-1-1 Oh 2 ), tetraethyl orthosilicate (TEOS) and deionized water, according to the first structure-directing agent A: TEOS: H 2 O=0.3:1:800 molar ratio Weigh the raw materials, add them to the beaker one by one, put them on a magnetic stirrer with heating and stirring functions, mix evenly, and stir at 80°C for 3 hours, replenish the evaporated water at any time , to obtain a colorless transparent hydrolyzed solution, that is, the first hydrolyzed mixture.

[0097] b. Transfer the first hydrolysis mixture to a closed stainless steel reaction kettle, and crystallize at a constant temperature of 170°C for 15 days. The crystallized product is filtered and washed 10 times with deionized water. The water consumption is 10 times the molecular sieve weight each time. The filter cake is dried at 110°C for 24 hours, and then roasted at ...

Embodiment 2-16

[0103] Titanium-silicon molecular sieves were prepared according to the steps in Example 1 and the raw material ratios and synthesis conditions in Tables 1 to 4, respectively marked as RTTS-2 to RTTS-16. The most probable diameter of mesopores, the ratio of surface Ti-Si ratio to bulk Ti-Si ratio are listed in Table 5.

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Abstract

The disclosure relates to a titanium-silicon material with a core-shell structure and its preparation method and a method for producing epoxy compounds by oxidizing macromolecular olefins. The material includes an inner core and an outer shell. Titanium-silicon molecular sieves, in terms of oxides and in molar quantities, TiO of core-shell structure titanium-silicon materials 2 with SiO 2 The molar ratio is 1: (30-100); the ratio of the surface titanium-silicon ratio of the core-shell structure titanium-silicon material to the bulk titanium-silicon ratio is 2.0-4.4, and the titanium-silicon ratio refers to TiO 2 with SiO 2 The molar ratio; the most probable pore diameter of the mesopore of the core-shell structure titanium silicon material is 14-34nm. The shell surface of the titanium-silicon core-shell structure material of the present disclosure is rich and has a suitable most probable pore size, and its use in the process of producing epoxy compounds by the oxidation reaction of macromolecular olefins is conducive to improving the conversion rate of raw materials and the selectivity of target products, and Improve the utilization rate of oxidant in oxidation reaction.

Description

technical field [0001] The disclosure relates to a titanium-silicon material with a core-shell structure, a preparation method thereof, and a method for producing epoxy compounds by oxidizing macromolecular olefins. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s, which refers to a type of heteroatom molecular sieve containing titanium skeleton. The currently synthesized microporous titanium silicate molecular sieves include TS-1 (MFI structure), TS-2 (MEL structure), Ti-Beta (BEA structure), Ti-ZSM-12 (MTW structure) and Ti-MCM-22 ( MWW structure), etc. Mesoporous titanium-silicon molecular sieves include Ti-MCM-41 and Ti-SBA-15, etc. The development and application of titanium-silicon molecular sieves has successfully expanded zeolite molecular sieves from the field of acid catalysis to the field of catalytic oxidation, which is a milestone. Among them, the Italian Enichem company fir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89B01J35/10C01B39/08C01B39/00C07D301/12C07D303/04
CPCB01J29/89C01B39/08C01B39/00C07D301/12C07D303/04C01P2004/80C01P2004/04C01P2006/17B01J2229/18B01J35/615B01J35/617B01J35/635B01J35/633B01J35/647
Inventor 杨永佳林民夏长久朱斌彭欣欣刘聿嘉罗一斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP