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Preparation method of propenyl ethanoate catalyst and synthesis method of propenyl ethanoate

A technology of allyl acetate and a synthesis method, which is applied in the directions of catalyst activation/preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of low activity and selectivity of allyl acetate catalysts, and achieves improved activity and selective effect

Active Publication Date: 2015-03-25
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 the present invention is the low problem of allyl acetate catalyst activity and selectivity synthesized in the prior art

Method used

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  • Preparation method of propenyl ethanoate catalyst and synthesis method of propenyl ethanoate
  • Preparation method of propenyl ethanoate catalyst and synthesis method of propenyl ethanoate
  • Preparation method of propenyl ethanoate catalyst and synthesis method of propenyl ethanoate

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Preparation of modified carrier: Spray 350ml of 110g / L potassium oxalate aqueous solution evenly on 1.1L spherical SiO2 with a diameter of 5.6mm 2 on the carrier and dried to obtain a modified carrier (X), wherein the alkali metal carboxylate accounted for 8.3 wt% of the modified carrier.

[0027] The preparation of supported catalyst: use sodium bicarbonate pH regulator and water as solvent preparation pH to be 1.05, containing 3.50gPd and 0.40gCu chloropalladic acid, cupric chloride aqueous solution, obtain impregnating liquid 560ml, it is mixed in the pot impregnated on the carrier (X), dried at 80°C, and 105ml contains 21.5g Na 2 SiO 3 9H 2 The solution of O is fully mixed, aged for 24h, and then used with a solubility of 10% (in the form of N 2 h 4 ·H 2 (2 in weight ratio) was reduced with 550ml of hydrazine hydrate, washed with water, and dried at 90°C to obtain B, and 335ml of a solution containing 33g of potassium acetate was weighed, impregnated on B, and...

Embodiment 2

[0030] for 【Example 1】 comparative example.

[0031] Preparation of modified carrier: Spray 350ml of 110g / L potassium oxalate aqueous solution evenly on 1.1L spherical SiO2 with a diameter of 5.6mm 2 on the carrier and dried to obtain a modified carrier (X), wherein the alkali metal carboxylate accounted for 8.3 wt% of the modified carrier.

[0032]Preparation of supported catalyst: Weigh 3.50g of metal palladium and 0.40g of metal copper into a crucible fixed between the electrodes of Knotes-927500 static metal atom reactor, evacuate the system to 0.002Pa, and cool with liquid nitrogen Reaction flask to -200°C; introduce 10ml of toluene into the reaction flask to fill the inner wall of the reaction flask, increase the current to evaporate Pd and Cu, and continuously introduce toluene to co-condense gaseous Pd and Cu atoms with toluene in the reaction flask Wall; the temperature is raised to -80°C, the coacervate melts and falls to the bottom of the reaction bottle to obtai...

Embodiment 3

[0041] for [Comparative Example 1] comparative example.

[0042] Preparation of the supported catalyst: Weigh 3.50g of metal palladium and 0.40g of metal copper and put them into a stationary Knotes-927500

[0043] In the crucible between the electrodes of the type metal atom reactor, the system is evacuated to 0.002Pa, and the reaction bottle is cooled to -200°C with liquid nitrogen; 10ml of toluene is introduced into the reaction bottle to fill the inner wall of the reaction bottle, and the current is increased. , to evaporate Pd and Cu, and continuously introduce toluene, so that gaseous Pd, Cu atoms and toluene co-condense on the wall of the reaction bottle; when the temperature is raised to -80°C, the co-condensates melt and fall into the bottom of the reaction bottle to obtain a solution, and the obtained solution is immersed in 1.1L spherical SiO with a diameter of 5.6mm 2 On the support (X), the temperature is raised to 30°C, and the catalyst precursor A is obtained...

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Abstract

The invention relates to a preparation method of a propenyl ethanoate catalyst, a catalyst obtained by the method and a synthesis method of propenyl ethanoate, and mainly solves the problem that the catalysts are not high in activity and selectivity in the prior art. According to the preparation method of the propenyl ethanoate catalyst, the catalyst comprises a carrier, an active component and a co-catalyst, wherein the carrier is selected from at least one of SiO2 or Al2O3; the active component comprises a metal Pd and a metal Cu; the co-catalyst is potassium acetate. The preparation method comprises the following steps: (1) loading alkali metal carboxylate on the carrier to obtain an alkali metal carboxylate modified carrier, wherein the alkali metal carboxylate accounts for 1.0-15wt% of the modified carrier; and (2) loading the metal Pd and the metal Cu with required quantity by using a solvated metal atom impregnation method (SMAI). The problem can be better solved and the propenyl ethanoate catalyst can be used for industrial production of propenyl ethanoate.

Description

technical field [0001] The invention relates to a preparation method of an allyl acetate catalyst, the obtained catalyst, and a synthesis method of allyl acetate. Background technique [0002] In the reaction of preparing allyl acetate by fixed bed gas phase reaction using propylene, oxygen and acetic acid as raw materials, SiO 2 、Al 2 o 3 or SiO 2 and Al 2 o 3 The composed mixture is used as a carrier, loaded with Pd, Cu and potassium acetate, and the catalysts in which Pd and Cu are distributed in an eggshell shape are well known to those skilled in the art. The preparation method of the catalyst has been disclosed by US3,917,676 (titled: Process for producing ally acetate), that is, the mixture containing noble metal Pd and Cu is impregnated on the carrier, and after drying, the free Pd and Cu are solidified The active metal Pd and Cu are formed on the surface of the carrier, and then the catalyst is obtained after being treated with co-catalyst KOAc and dried. The...

Claims

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Application Information

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IPC IPC(8): B01J37/02B01J31/04C07C67/055C07C69/155
Inventor 查晓钟杨运信张丽斌
Owner CHINA PETROLEUM & CHEM CORP
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