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Solid acid catalyst as well as preparation method and application of solid acid catalyst

A solid acid catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of low utilization rate of active sites, difficulty in bare leakage, etc., and achieve cycle stability and utilization The effect of high yield and simple preparation method

Inactive Publication Date: 2015-05-06
NANJING UNIV OF INFORMATION SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, different types of solid acids such as Amberlyst, Nafion, USY, HBEA, HMOR, and HZSM-5 have been used to catalyze the oxidation of cyclopentanone, but the active sites of these solid acids are often wrapped, which is difficult to expose and the utilization rate of active sites is low.

Method used

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  • Solid acid catalyst as well as preparation method and application of solid acid catalyst
  • Solid acid catalyst as well as preparation method and application of solid acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 0.3 g of zirconium hydrogen phosphate and disperse it in 20 mL of deionized water, ultrasonically stir for 3 hours, then add 10 mL of 0.1 mol / L 1-propylamine, and ultrasonically treat for 3 hours in an ice bath to obtain exfoliated zirconium hydrogen phosphate nanosheets. Then drop 10mL of 0.1mol / L HCl into it, and wash by centrifugation until there is no Cl in the filtrate. - In the presence of protonated zirconium hydrogen phosphate nanosheets.

[0032] (2) Preparation of solid acid catalyst

[0033] Using ion exchange method, 0.3655g Zn(AC) 2 Dissolve in 50mL deionized water, add the above-mentioned protonated zirconium hydrogen phosphate nanosheets, wherein Zn(AC) 2 The molar ratio of zinc ions to zirconium hydrogen phosphate is 2:1. Stir and sonicate for 2 hours, then reflux at 80°C for 12 hours. After the reaction is finished, let it stand for 12 hours, set the centrifugal speed to 20000r / min, centrifuge for 2 minutes, wash with deionized water until th...

Embodiment 2

[0036] When the solid acid catalyst prepared in Examples 1-2 is applied to the Baeyer-Villiger oxidation reaction, the specific method can be: weigh 0.05g of solid acid, add 0.3951g of cyclohexanone, 2.2391g of 30wt.% hydrogen peroxide, at 70°C React for 12 hours, the reaction chemical formula is as figure 1 shown. After the reaction, the catalyst was centrifugally separated, and the catalyst was washed with hydrogen peroxide to carry out the next round of reaction. A total of 5 catalytic reactions were performed. After the reaction solution was filtered, the gas-mass spectrometer was used to analyze the yield of the product caprolactone. The results are shown in Table 1.

[0037] Example 3

Embodiment 3

[0039] Weigh 1.2 g of zirconium hydrogen phosphate and disperse it in 50 mL of deionized water, ultrasonically stir for 5 hours, then add 4 mL of 1 mol / L 1-propylamine, and then ultrasonically treat for 5 hours in an ice bath to obtain exfoliated zirconium hydrogen phosphate nanosheets . Then drop 4 mL of 1 mol / L HCl into it, and wash by centrifugation until there is no Cl in the filtrate. - In the presence of protonated zirconium hydrogen phosphate nanosheets.

[0040] (2) Preparation of solid acid catalyst

[0041] In this example, the ion exchange method is adopted, and the molar ratio of yttrium ion to zirconium hydrogen phosphate is 3:1, and 1.7684g C 2 h 3 o2 Y was dissolved in 60 mL of deionized water, and then 1.2 g of the above-mentioned protonated zirconium hydrogen phosphate nanosheets were added, and stirred at 90° C. for 12 hours. After the reaction was completed, let it stand for 5 hours, set the centrifugal speed to 10000 r / min, centrifuged for 15 minutes to...

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Abstract

The invention provides a solid acid catalyst as well as a preparation method and an application of the solid acid catalyst. The catalyst is applied to the Baeyer-Villiger oxidation reaction to catalyze the conversion of cyclic ketones into lactones; the catalyst has the advantages of high active site utilization rate, good selectivity, good stability, and easy recycling. The solid acid catalyst is composed of two parts, namely the active ingredient of the catalyst and a carrier, wherein the carrier is zirconium hydrogen phosphate nanosheet; the active ingredient is one or the combination of several of lanthanum, yttrium, aluminum, neodymium, cerium, chromium, zinc, indium, tin, scandium, praseodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium metal ions; the molar ratio of the metal component to the zirconium hydrogen phosphate in the solid acid catalyst is (1: 5) to (5: 1).

Description

technical field [0001] The invention belongs to the technical field of catalysts in organic synthesis, and in particular relates to a solid acid catalyst and a preparation method thereof. Background technique [0002] Baeyer-Villiger oxidation is a basic organic chemical reaction that oxidizes cyclic ketones to corresponding lactones. It is of great significance to functional group conversion and ring expansion in organic synthesis, and has a wide range of application values. The oxidation product obtained by using this reaction is an important intermediate of many drugs, pesticides and dyes. At present, the catalysts widely used in the oxidation of ketones mainly include trifluoroperoxyacetic acid, monoperoxymaleic acid, monoperoxyphthalic acid, 3,5-dinitroperoxyformic acid, p-nitroperoxybenzoic acid, m-chloroperoxybenzoic acid, peroxybenzoic acid, peracetic acid, etc., but these oxides have many dangers in transportation and handling, and the post-treatment process is c...

Claims

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Application Information

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IPC IPC(8): B01J27/18C07D313/04C07D313/10
CPCY02P20/584
Inventor 周莹杰王卫李南
Owner NANJING UNIV OF INFORMATION SCI & TECH
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