Vinyl acetate preparation method

A vinyl acetate and ethylene technology, applied in the field of vinyl acetate preparation, can solve the problems of low space-time yield and selectivity, and achieve the effects of improving space-time yield and selectivity, good technical effect, and improved selectivity

Active 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 the present invention is the problem of low space-time yield and selectivity existing in the prior art, and a new preparation method of vinyl acetate is provided, which has the characteristics of high space-time yield and selectivity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] (1) Catalyst preparation

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

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 in the liquid carbon dioxide impregnating solution, the type of palladium-gold compound, the concentration of potassium acetate solution, impregnating pressure, impregnating temperature, reducing gas, reducing 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 vinyl acetate preparation method which 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 ethylene, 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 gold and alkali metal acetate; and the catalyst comprises 1-12g/L of palladium, 0.1-9g/L of gold and 10-90g/L of alkali metal acetate. The method is characterized in that the average crystal grain diameters of palladium and gold are between 4 and 9nm, and crystal grains with the average crystal grain diameters within a scope of plus or minus 20% account for 60-81% 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 vinyl acetate. Background technique [0002] Vinyl acetate is an important chemical raw material, widely used in the manufacture of polyvinyl alcohol, vinyl copolymer resins, adhesives, coatings, textile processing, paper coating, etc. The main method of producing vinyl acetate in the world today is to take ethylene, oxygen and acetic acid as raw materials, use palladium-gold-potassium acetate / silicon dioxide as a catalyst, and synthesize through a gas-phase catalytic reaction. 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] The patent (CN1226188A) of Herchester Rayon Company provides a preparation method for preparing a catalyst loaded with a main catalyst noble metal, a promoter metal and an alkali metal ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/15C07C67/055B01J31/28B01J37/02
Inventor 刘军晓杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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