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Preparation method of alkene epoxidation catalyst as well as catalyst prepared thereby

An epoxidation and catalyst technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve the complicated preparation process, long reaction time, harsh conditions, etc. problems, to achieve the effect of improving epoxidation selectivity, improving carbon deposition resistance, and reducing surface acidity

Active Publication Date: 2018-04-20
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both the vapor deposition method and the sol-gel method have the following disadvantages: the preparation process is cumbersome, the operation is complicated, the conditions are harsh and difficult to control, and the reaction time is long.
In addition, once the conditions are not properly controlled, the resulting catalyst is likely to generate more extra-skeletal titanium compounds (mainly free titanium dioxide), the surface of the catalyst is more acidic, and the effective utilization rate of organic peroxides is lower when used in the epoxidation of propylene.
[0008] In summary, the current conventional microporous titanium-silicon molecular sieves are too small for C 6 The above macromolecular olefin epoxidation reaction activity is very low, which limits its application in olefin epoxidation; Mesoporous molecular sieve materials such as Ti-MCM-41 and Ti-SBA-15 can be used for macromolecular olefins and EBHP Or the epoxidation reaction of CHP as the oxidant, but these catalysts have the characteristics of difficult synthesis, difficult preparation and high price of the template used, resulting in high cost and limited industrial application; SiO 2 Titanium-silicon catalyst prepared by vapor deposition method or liquid phase impregnation method as a carrier, due to the presence of acidic free TiO on the surface 2 , and the loading of titanium active centers is low, resulting in low catalyst selectivity and reactivity

Method used

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  • Preparation method of alkene epoxidation catalyst as well as catalyst prepared thereby
  • Preparation method of alkene epoxidation catalyst as well as catalyst prepared thereby
  • Preparation method of alkene epoxidation catalyst as well as catalyst prepared thereby

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The structure of the catalyst prepared in Example 1 was determined by X-ray diffractometer. The instrument is produced by PANalytical Company, the model is X’pert 3 powder.

[0057] 3. Confirmation of alkali metal modification and content

[0058] XRF analysis was carried out on the catalysts prepared in each example and comparative example to confirm whether the modification process of the alkali metal element in the step (3) was realized and the content of the alkali metal element. The instrument is produced by Shimadzu Corporation, Japan, and the model is EDX-LE.

[0059] 4. Silanization modification and confirmation of silyl content

[0060] The catalysts prepared in Example 1 and Comparative Example 3 were thermally analyzed using a scanning calorimeter to obtain a DSC curve, thereby confirming whether the silanization modification process in step (4) was realized. The scanning calorimeter is produced by Mettler-Toledo, the model is DSC1 professional.

[0061]...

Embodiment 2

[0093] Prepare titanium silica gel according to Example 1, the difference is that 20g of ethylenediamine liquid is added during the pore expansion process, and the temperature is treated at 90°C for 10h, then dried at 120°C for 3h, and roasted at 550°C for 3h to obtain a titanium-silicon composite oxide gel. material, the specific surface area determined by BET is 368m 2 / g, the average pore diameter is 10.7nm. Catalyst B was prepared by carrying out alkali metal modification and gas-phase silylation treatment under the same conditions as in Example 1.

Embodiment 3

[0095] Prepare titanium silica gel according to Example 1, the difference is that 20g of high-purity liquid ammonia is added during the pore expansion process, and the temperature is treated at 150°C for 12h, then dried at 160°C for 3h, and roasted at 550°C for 3h to obtain titanium-silicon composite oxide. material, its specific surface area is 322m as determined by BET 2 / g, the average pore diameter is 18.3nm. Catalyst C was prepared by carrying out alkali metal modification and gas-phase silylation treatment under the same conditions as in Example 1.

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Abstract

The invention relates to a preparation method of an alkene epoxidation catalyst. The preparation method of the alkene epoxidation catalyst comprises the following steps: (1) preparing titanium silicongel; (2) performing pore-enlarging treatment on the titanium silicon gel by using organic amine or liquid ammonia, drying and roasting to obtain titanium silicon composite oxide; (3) optionally performing alcohol solution treatment on organic alkali metal salt; and (4) optionally performing gas phase silanization treatment. The pore diameter of the catalyst prepared by the method is adjustable, so that the catalyst has higher activity on epoxidation reaction of olefin molecules with different kinetic diameter; and the catalyst is subjected to two-step modification, the surface acidity of thecatalyst is effectively reduced and the catalyst has higher epoxidation product selectivity.

Description

technical field [0001] The invention relates to a preparation method of an olefin epoxidation catalyst, in particular to a preparation method of a titanium-silicon composite oxide catalyst. The invention also relates to the olefin epoxidation catalyst prepared by the preparation method and its application in olefin epoxidation. Background technique [0002] For chemicals such as epoxy resins, surfactants, coatings, adhesives, and surface coating reagents that are widely used in life and industry, epoxy compounds are a class of general-purpose intermediate raw materials for the synthesis of these chemicals and have great potential. demand. The traditional production process of synthesizing epoxy compounds is generally chlorohydrin method or co-oxidation method, but this kind of method has the disadvantages of heavy pollution, large corrosion of equipment, many by-products, and high cost. [0003] Therefore, many companies at home and abroad are devoting themselves to the de...

Claims

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Application Information

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IPC IPC(8): B01J21/08B01J23/04C07D301/19C07D303/04B01J35/10
CPCC07D301/19C07D303/04B01J21/08B01J23/04B01J35/615B01J35/647B01J21/063B01J37/0201B01J37/033B01J37/0018B01J2229/32B01J37/04B01J37/088
Inventor 王同济叶飞王磊初乃波杨立超孙康黎源华卫琦
Owner WANHUA CHEM GRP
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