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Titanium dioxide microspheres@all silicon silica-1 molecular sieve core-shell catalyst, preparation method and application

Active Publication Date: 2019-09-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst is used to prepare diphenyl carbonate by transesterification, which overcomes the problems of low activity, low selectivity and easy deactivation of heterogeneous catalysts in the prior art, and has the characteristics of high activity, high selectivity and not easy deactivation

Method used

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  • Titanium dioxide microspheres@all silicon silica-1 molecular sieve core-shell catalyst, preparation method and application
  • Titanium dioxide microspheres@all silicon silica-1 molecular sieve core-shell catalyst, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of titanium dioxide microspheres: add 10mL 0.4mmol / L KCl solution to 1000mL absolute ethanol, stir for 10min, then under vigorous stirring, add 42.5g n-butyl titanate dropwise to the above KCl solution, dropwise After the addition is completed, continue to stir for 30 minutes, stand at room temperature for 2 hours, then centrifuge, wash with deionized water 3 times, dry in an oven at 120°C for 12 hours, and calcinate at 400°C to obtain nuclear phase titanium dioxide microspheres C1. The average diameter of the prepared C1 was 800 nm.

[0028] Preparation of titanium dioxide microspheres@全siliconSilica-1 molecular sieve core-shell catalyst: add 7.2g of tetrapropylammonium hydroxide (25wt% aqueous solution) and 1.0g of NaOH into 50mL of deionized water, mix well, add 5.0g of the above-prepared Titanium dioxide microspheres C1, ultrasonically dispersed for 30 minutes, stirred at 80°C for 3 hours, then slowly added 6.62g of ethyl orthosilicate, aged at 25°C for 3 h...

Embodiment 2

[0030] Preparation of titanium dioxide microspheres: add 10 mL of 0.1 mol / L KBr solution to 1000 mL of absolute ethanol, stir for 10 minutes, and then under vigorous stirring, add 42.5 g of n-butyl titanate dropwise to the above KBr solution. After the addition is complete, continue to stir for 30 minutes, stand for 2 hours at room temperature, then centrifuge, wash with deionized water three times, dry in an oven at 120°C for 12 hours, and calcinate at 300°C to obtain nuclear phase titanium dioxide microspheres C2. The average diameter of the prepared C2 was 310 nm.

[0031] Preparation of titanium dioxide microspheres@全siliconSilica-1 molecular sieve core-shell catalyst: tetrapropylammonium bromide is made into a 50mL, 0.2mol / L solution, and ammonia is added to adjust the pH to 13.5. After mixing evenly, add 5.0g of titanium dioxide Microsphere C2, ultrasonically dispersed for 30 minutes, stirred at 80°C for 3 hours, then slowly added 201.3g of tetraethyl orthosilicate, aged at...

Embodiment 3

[0033] Preparation of titanium dioxide microspheres: add 10 mL of 1.0 mol / L KCl solution to 1000 mL of absolute ethanol, stir for 10 minutes, and then under vigorous stirring, add 35.5 g of isopropyl titanate dropwise to the above KCl solution. After the addition is complete, continue to stir for 30 minutes, let stand at room temperature for 2 hours, then centrifuge, wash with deionized water for 3 times, dry in an oven at 120°C for 12 hours, and calcinate at 400°C to obtain nuclear phase titanium dioxide microspheres C3. The average diameter of C3 is 150 nm.

[0034] Preparation of titanium dioxide microsphere@全siliconSilica-1 molecular sieve core-shell catalyst: tetraethylammonium hydroxide was made into a 50mL, 0.2mol / L solution, and ammonia was added to adjust the pH to 13.5. After mixing, add 5.0g of titanium dioxide Microsphere C3, ultrasonically dispersed for 30 minutes, stirred at 80°C for 3 hours, then slowly added 90.3g of methyl orthosilicate, aged at 50°C for 1 hour, ...

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Abstract

The invention relates to a titanium dioxide microsphere@all-silicon silica-1 molecular sieve core-shell-structured catalyst, and a preparation method and application thereof. The nuclear phase of the catalyst is a titanium dioxide microsphere, and the shell layer of the catalyst is an all-silicon silica-1 molecular sieve; and the catalyst is applicable to industrial production for diphenyl carbonate through transesterification of dimethyl carbonate and phenyl acetate.

Description

Technical field [0001] The invention relates to a titanium dioxide microsphere@全silicon Silica-1 molecular sieve core-shell catalyst, preparation method and application. Background technique [0002] Diphenyl carbonate is the raw material for the preparation of polycarbonate by non-phosgene method. Its traditional preparation method is phosgene method. Due to the potential harm of highly toxic phosgene to the environment and safety production, it is restricted by policy. The synthesis of diphenyl carbonate (DPC) by transesterification of phenol (PhOH) and dimethyl carbonate (DMC) under the action of a catalyst is currently the only industrialized non-phosgene synthesis route of diphenyl carbonate. However, this route has the problems of low equilibrium conversion rate and high energy consumption for separation of DMC and methanol azeotrope. The route of transesterification of dimethyl carbonate and phenyl acetate (PA) to produce diphenyl carbonate has the advantages of high equi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/035C07C68/06C07C69/96
Inventor 陈梁锋戈军伟何文军
Owner CHINA PETROLEUM & CHEM CORP
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