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Supported organic rhenium catalyst and preparation method thereof

A catalyst and a supported technology, which are applied in the field of low-loaded and high-activity supported organic rhenium catalysts and their preparation, can solve the problems of restricting large-scale production and application, difficult separation and recovery of homogeneous catalysts, etc., and achieve high selectivity, high high conversion rate

Inactive Publication Date: 2013-04-10
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, homogeneous catalysts are not easy to separate and recover, which limits the industrial application of large-scale production

Method used

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  • Supported organic rhenium catalyst and preparation method thereof
  • Supported organic rhenium catalyst and preparation method thereof
  • Supported organic rhenium catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A: Weigh 14.50125g of ZrOCl 2 ·8H 2 Dissolve O in deionized water, add 6 mL of HF solution with a mass concentration of 40%, and finally dilute to 100 mL of mixed solution I; then weigh 14.2281 g of PhPO 3 , use 1-propanol and water with a volume ratio of 1:1 to prepare 100mL alcoholic aqueous solution II; use a dual-channel constant-current peristaltic pump to inject the mixed solution I and alcoholic aqueous solution II into the high-speed rotating fully back-mixed rotating fluid at the same speed In the membrane reactor, mix quickly for 1min, adjust the slit width between the rotor and the stator of the reactor to 0.04mm, the working voltage is 100V, and the rotor speed is 4000rpm; pour the prepared colloidal slurry into a hydrothermal kettle and heat at 100°C React for 96 hours; centrifuge and wash with a large amount of deionized water for 3 times until the pH is 7, wash once with isopropanol, once with acetone, once with ether, and then dry in a vacuum oven for 2...

Embodiment 2

[0025] A: with embodiment 1;

[0026]B: Measure 10mL of dichloromethane and add it to a 25mL three-necked flask, add 1.0g of the zirconium phosphate compound prepared in step A and 0.15g of MTO in sequence, 2 Under the protection of the atmosphere, use light-proof treatment, stir at room temperature for 24 hours, and the obtained powder is the supported organic rhenium catalyst; the active component of the catalyst, methyl rhenium trioxide, is evenly dispersed on the surface of the carrier zirconium phosphate compound;

[0027] C: Under the same reaction conditions as in Example 1, the catalytic performance of the catalyst prepared in step B was tested, the reactant cyclohexene conversion rate was 41.9%, the target product epoxy cyclohexane selectivity was 100%, and the TOF value of the catalyst was 40.9h -1 .

Embodiment 3

[0029] A: with embodiment 1;

[0030] B: with embodiment 1;

[0031] C: use the catalyst prepared in step B to catalyze the epoxidation of cyclooctene to generate epoxy cyclooctane, the reaction conditions are: reaction temperature 25°C, reaction pressure normal pressure, methanol as solvent, solvent consumption 10ml / 10mmol cyclooctene, Every milliliter of cyclooctene adds the catalyst that 0.1g step B obtains, and percarbamide consumption is 1.806g / mL cyclooctene, reaction time 6h, reactant cyclooctene conversion rate 88%, target product epoxy cyclooctane selectivity 100%, the TOF value of the catalyst is 29.7h -1 .

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Abstract

The invention discloses a supported organic rhenium catalyst using a high-activity zirconium phosphate stratified material as a support and a preparation method thereof, belonging to the technical field of catalyst preparation. The zirconium phosphate compound in stratified structure is used as a support, and methylrhenium trioxide with catalytic activity is anchored to the surface of the zirconium phosphate compound, thereby obtaining the supported organic rhenium catalyst. The catalyst is used for catalyzing olefins to synthesize epoxy compounds by epoxidation, and has the advantages of high reactant conversion rate and high product selectivity.

Description

technical field [0001] The invention belongs to the field of catalysts, and in particular relates to a low-loaded high-activity loaded organic rhenium catalyst with zirconium phosphate compounds as a carrier and a preparation method thereof. Background technique [0002] The general chemical formula of zirconium phosphate compounds is Zr(O 3 P-R) 2 ·nH 2 O, where n is bound H 2 According to the number of O, it can be divided into inorganic zirconium phosphate and organic zirconium phosphonate according to the difference of R groups. Zirconium phosphate (Zr(O 3 P-OH) 2 ·nH 2 O) There are two different structural types: α-zirconium phosphate and γ-zirconium phosphate. Among them, the layers of α-zirconium phosphate are stacked together in the form of ABAB, and each layer consists of Zr atoms that are approximately in the same plane and two layers of O that sandwich Zr atoms in the middle. 3 P-OH composition. In the process of preparing zirconium phosphate, if phenylph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/38B01J31/12C07D301/03C07D303/04
Inventor 张法智赵洪月
Owner BEIJING UNIV OF CHEM TECH
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