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Preparation method and application of titanium-silicon composite oxide catalyst

A composite oxide and catalyst technology, which is applied in the direction of catalyst activation/preparation, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc. It can solve the complicated preparation process, long reaction time, difficult control, etc. problems, to achieve the effect of good catalytic activity, fast decomposition process and easy operation

Active Publication Date: 2017-01-18
WANHUA CHEM GRP CO LTD
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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.
However, there is no report on the example of using low temperature plasma for the preparation of epoxidation catalysts

Method used

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  • Preparation method and application of titanium-silicon composite oxide catalyst
  • Preparation method and application of titanium-silicon composite oxide catalyst
  • Preparation method and application of titanium-silicon composite oxide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Under stirring, 5g TiCl 4 with 3g Mg(NO 3 ) 2 Dissolve in 80 mL of isopropanol. Add 25g of macroporous type C silica gel to the above solution, and soak at 40°C for 12 hours. The above mixture was then passed through an oil bath at 100°C for 3 hours. The obtained catalyst precursor was treated in a flat-plate dielectric barrier discharge plasma discharger for 1 hour using a plasma generator power supply with a power of 50 W and using air as the discharge medium. Then, at 250° C., with high-purity nitrogen as the carrier gas, 3 g of hexamethyldisilazane was passed through for reaction for 1 hour to obtain catalyst B. It was used in reaction kettle and fixed bed propylene epoxidation reaction respectively, and its reaction performance was evaluated. The results are shown in Table 2.

Embodiment 2

[0057] Under stirring, 10g TiCl 4 with 4g Zn(NO 3 ) 2 Dissolve in 100mL ethanol. Add 60g of SBA-15 (Nankai University Catalyst Factory, calculated according to the silicon dioxide content as 100%) to the above solution, and soak at 20°C for 2 hours. The above mixture was then passed through an oil bath at 80 °C for 2 hours. The obtained catalyst precursor was treated in a flat-plate dielectric barrier discharge plasma discharger for 0.5 hours using a plasma generator power supply with a power of 40W and using air as the discharge medium. Afterwards, at 120° C., 1 g of hexamethyldisilazane was passed through with high-purity nitrogen as the carrier gas for 0.5 hour reaction to obtain catalyst C. It was used in reaction kettle and fixed bed propylene epoxidation reaction respectively, and its reaction performance was evaluated. The results are shown in Table 2.

Embodiment 3

[0059] Under stirring, mix 18g tetrabutyl titanate with 3g ZnCl 2 Dissolve in 80mL ethanol. Add 40 g of HMS (Nankai University Catalyst Factory, calculated according to the silicon dioxide content as 100%) to the above solution, and soak at 20° C. for 20 hours. The above mixture was then passed through an oil bath at 80 °C for 1 hour. The obtained catalyst precursor was treated in a flat-plate dielectric barrier discharge plasma discharger for 1.5 hours using a plasma generator power supply with a power of 80W and using air as the discharge medium. Then, at 300° C., with high-purity nitrogen as the carrier gas, 8 g of hexamethyldisilazane was passed through for reaction for 8 hours to obtain catalyst D. It was used in reaction kettle and fixed bed propylene epoxidation reaction respectively, and its reaction performance was evaluated. The results are shown in Table 2.

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Abstract

The invention relates to a preparation method of a titanium-silicon composite oxide catalyst. The method comprises the following steps: 1, simultaneously impregnating a silica carrier with a titanium source and a soluble alkaline metal salt; 2, carrying out low temperature plasma treatment; and 3, modifying by using an organosilane reagent. Alkaline oxide is introduced to modify the catalyst when the impregnation process titanium source loading is carried out, and the low temperature plasma treatment is carried out, so the production of a titanium compound outside a framework and the surface acidity of the catalyst are effectively reduced, thereby the catalyst substantially improves the selectivity and the yield of epoxides in the olefin epoxidation reaction.

Description

technical field [0001] The invention relates to a preparation method of an epoxidation catalyst, in particular to a preparation method of a titanium-silicon composite oxide catalyst and its application in olefin epoxidation. Background technique [0002] Propylene oxide is an important basic organic chemical raw material and the third largest derivative of propylene. It is mainly used in the production of chemical products such as polyether polyols, propylene glycol and nonionic surfactants, and its annual demand is increasing year by year. At present, the technologies for industrial production of propylene oxide mainly include chlorohydrin method and organic peroxide co-oxidation method, the latter includes tert-butyl hydroperoxide oxidation method (PO / MTBE) and ethylbenzene hydroperoxide oxidation method (PO / SM). The advantages of the chlorohydrin method are that the process is short, the process is mature, the operation is flexible, the purity of the raw material propyl...

Claims

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Application Information

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IPC IPC(8): B01J31/38B01J37/34C07D301/19C07D303/04
CPCB01J31/38B01J37/349B01J2231/72C07D301/19C07D303/04
Inventor 周游初乃波王磊王同济叶飞崔娇英张礼昌黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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