Propenyl ethanoate catalyst and preparation method thereof

A technology of allyl acetate and catalyst, which is applied in the directions of catalyst activation/preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of low catalyst activity and selectivity, and improve the space-time yield and selectivity. , Good technical effect, uniform grain size distribution effect

Active Publication Date: 2015-07-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One of the technical problems to be solved by this invention is the low problem of catalyst activity and selectivity existing in the prior art, and a kind of allyl acetate catalyst is provided

Method used

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  • Propenyl ethanoate catalyst and preparation method thereof
  • Propenyl ethanoate catalyst and preparation method thereof
  • Propenyl ethanoate catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Catalyst preparation

[0018] Step (a): get the liquid carbon dioxide solution 1200ml containing hexafluoroacetylacetonate palladium (II) and hexafluoroacetylacetonate copper (II) as dipping solution, the palladium content of this dipping solution is 2.75g / L, and the copper content is 0.625g / L , under the impregnation pressure of 69MPa and the impregnation temperature of 28°C, 1100ml of spherical silica support with a diameter of 4-6mm was impregnated to obtain the catalyst precursor I;

[0019] Step (b): then reduce the pressure, evaporate the liquid carbon dioxide in the catalyst precursor I at a rate of 0.3 ml (liquid carbon dioxide) / min, until the liquid carbon dioxide is evaporated to obtain the catalyst precursor II;

[0020] Step (c): reducing the catalyst precursor II in a hydrogen atmosphere, the hydrogen flow rate is 0.2 ml / min, and the reduction temperature is 75° C. to obtain the catalyst precursor III;

[0021] Step (d): infiltrate the catalyst precurs...

Embodiment 2

[0036] The steps are the same as in Example 1 except that the calcination step is added between the step (c) and the step (d). The roasting step is as follows: the catalyst precursor III is roasted in a nitrogen / acetic acid atmosphere, wherein the partial pressure of acetic acid accounts for 5% of the total pressure, the roasting temperature is 250° C., and the roasting time is 24hr. For the convenience of comparison, the preparation conditions of the catalyst are listed in Table 1, and the physical properties of the catalyst and the space-time yield and selectivity data of the catalyst are listed in Table 2.

Embodiment 3～11

[0038] Except for changing the concentration of palladium-copper in the liquid carbon dioxide dipping solution, the type of palladium-copper compound, the concentration of potassium acetate solution, the dipping pressure, the dipping temperature, the reducing gas and the reducing temperature, other operation steps are the same as in Example 2. For the convenience of comparison, the preparation conditions of the catalyst are listed in Table 1, and the physical properties of the catalyst and the space-time yield and selectivity data of the catalyst are listed in Table 2.

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Abstract

The invention relates to a propenyl ethanoate catalyst and a preparation method of the propenyl ethanoate catalyst, in order to mainly solve the problem of low space time yield and selectivity of the catalyst in the prior art. According to the invention, a catalyst for synthesizing propenyl ethanoate is adopted, and SiO2, Al2O3 or the mixture of the SiO2 and Al2O3 are taken as carriers; load active components comprises metal palladium, metal copper and alkali metal acetate; in the catalyst, the content of palladium is 1-12g/L, the content of copper is 0.1-10g/L, and the content of alkali metal acetate is 10-100g/L, wherein the average particle size of palladium copper is 4-10nm, and the number of crystalline grains within the range of -20% to 20% of the average particle size is 60-80% of all the crystalline particles. The technical scheme of the preparation method solves the problem well, and can be used for the industrial production of propenyl ethanoate.

Description

technical field [0001] The invention relates to an allyl acetate catalyst and a preparation method thereof. Background technique [0002] Allyl acetate is an important chemical raw material with a wide range of uses. The main method of producing allyl acetate in the world today is to synthesize propylene, oxygen and acetic acid through gas-phase catalytic reaction. In order to obtain catalysts with high space-time yield and high selectivity, continuous improvement has been made in the composition of active components, preparation process, and even shape of catalysts. [0003] European patent (EP0361484A2) provides a preparation method for preparing a catalyst loaded with a main catalyst noble metal, a promoter metal and an alkali metal or alkaline earth metal compound. The specific manufacturing process is as follows: the prepared mixed solution of precious metal and co-catalyst is added, dried, and then treated with an alkaline substance such as sodium silicate to convert...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J37/02C07C69/54C07C67/055
Inventor 刘军晓杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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