Method for preparing allyl acetate

A technology of allyl acetate and acetic acid, which is applied in the field of preparation of allyl acetate, can solve the problems of low space-time yield and selectivity, and achieve improved space-time yield and selectivity, good technical effects, and selectivity Improved effect

Inactive Publication Date: 2013-05-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by this invention is the problem of low space-time yield and selectivity in the prior art, and a new preparation method of allyl acetate is provided, which has high space-time yield and selectivity specialty

Method used

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  • Method for preparing allyl acetate
  • Method for preparing allyl acetate
  • Method for preparing allyl acetate

Examples

Experimental program
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Effect test

Embodiment 1

[0010] (1) Catalyst preparation

[0011] Step (a): Take 1200ml of liquid carbon dioxide solution containing palladium(II) hexafluoroacetylacetonate and copper(II) hexafluoroacetylacetonate as the impregnating solution, the palladium content of the impregnating solution is 2.75g / L, and the copper content is 0.625g / L , impregnating 1100 ml of spherical silica carriers with a diameter of 4 to 6 mm at an impregnation pressure of 69 MPa and an impregnation temperature of 28° C. to obtain a catalyst precursor I;

[0012] Step (b): Then reduce the pressure and evaporate the liquid carbon dioxide in the catalyst precursor I at a rate of 0.3ml (liquid carbon dioxide) / min until the liquid carbon dioxide evaporates completely to obtain the catalyst precursor II;

[0013] Step (c): reducing the catalyst precursor II in a hydrogen atmosphere, the hydrogen flow rate is 0.2ml / min, and the reduction temperature is 75°C to obtain the catalyst precursor III;

[0014] Step (d): soak the catalys...

Embodiment 2

[0029] Except that the roasting step is added between step (c) and step (d), other steps are all the same as in Example 1. Wherein the roasting step is: the catalyst precursor III is roasted under 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, the physical property data of the catalyst are listed in Table 2, and the evaluation conditions, space-time yield and selectivity data of the catalyst are listed in Table 3.

Embodiment 3～14

[0031] In addition to changing the concentration of palladium copper in the liquid carbon dioxide impregnation solution, the type of palladium copper compound, the concentration of potassium acetate solution, impregnation pressure, impregnation temperature, reducing gas, reduction temperature, molar ratio of reaction raw materials, space velocity of raw material gas, reaction pressure and reaction Except temperature, other operation steps are all identical with embodiment 2. For the convenience of comparison, the preparation conditions of the catalyst are listed in Table 1, the physical property data of the catalyst are listed in Table 2, and the evaluation conditions, space-time yield and selectivity data of the catalyst are listed in Table 3.

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Abstract

The invention relates to a method for preparing allyl acetate, and the method is mainly used for solving the problems of space time yield and low selectivity of the prior art. The method for preparing allyl acetate is adopted, reaction raw materials which consist of propylene, acetic acid, oxygen and water are contacted with a catalyst so as to obtain a reaction product containing allyl acetate, wherein the catalyst takes SiO2, Al2O3 or a mixture thereof as a carrier, and load active components comprise metal palladium, metal copper and alkali metal acetate; and the catalyst comprises 1-12g / L of palladium, 0.1-10g / L of copper and 10-100g / L of alkali metal acetate, wherein the average crystal grain diameters of palladium and copper are between 4 and 10nm, and crystal grains with the average crystal grain diameters within a scope of plus or minus 20% account for 60-80% of the whole crystal grains. The method can be utilized for better solving the problems and used for allyl acetate industrial production.

Description

technical field [0001] The present invention relates to a kind of preparation method of allyl acetate. 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 as raw materials. In order to obtain catalysts with high space-time yield and high selectivity, continuous improvements have been made in the composition of the active components of the catalyst, the preparation process, and even the shape. [0003] European patent (EP0361484A2) provides a method for preparing a catalyst loaded with a main catalyst noble metal, a promoter metal and an alkali metal or alkaline earth metal compound. Its specific manufacturing process is as follows: (1) In the rotating dipping tank, add the mixed solution of the precious metal and the co-catalyst, and pass it into hot air to dry; (2) Tak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/155C07C67/055B01J31/04
Inventor 刘军晓杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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