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Method for preparing 2-propenyl ethanoate by using propylene gas phase oxidation method

A gas-phase oxidation and allyl acetate technology, which is applied in the preparation of carboxylic acid esters, preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low space-time yield and selectivity, low single-pass conversion rate of propylene and acetic acid, etc. , to achieve the effect of improving space-time yield and selectivity, and improving single-pass conversion rate

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

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Problems solved by technology

[0003] The technical problem to be solved by this invention is the problem that the one-pass conversion rate of propylene and acetic acid exists in the prior art is low, the space-time yield of reaction and the low selectivity problem, provide a kind of preparation method of allyl acetate of propylene gas-phase oxidation method, The method has the characteristics of high single-pass conversion of propylene and acetic acid, high reaction space-time yield and high selectivity.

Method used

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  • Method for preparing 2-propenyl ethanoate by using propylene gas phase oxidation method
  • Method for preparing 2-propenyl ethanoate by using propylene gas phase oxidation method
  • Method for preparing 2-propenyl ethanoate by using propylene gas phase oxidation method

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Embodiment 1

[0018] use as figure 1 The shown propylene gas-phase oxidation method prepares the fixed-bed vertical pipe reactor of allyl acetate, the diameter of the reactor is 32mm, the height is 800mm, the catalyst loading capacity is 6L, the catalyst particle diameter is 3-6 millimeters, and the palladium content in the catalyst is 3.36 g / L, the copper content is 0.48g / L, and the potassium acetate content is 48g / L. The feed ratio of raw materials is: propylene / acetic acid / oxygen / water=72.0 / 6.0 / 6.0 / 16.0 (molar ratio), and the space velocity is 2000hr -1 . During the reaction process, the catalyst reaction temperature was controlled to be 160° C., and the reactor inlet pressure was 0.7 MPa. Propylene, acetic acid, oxygen and water are fed after being mixed in the preheater. According to the oxygen content analysis result of the online analysis port, supplement the oxygen content to 4% through the oxygen supplement port. The composition of the reaction product was analyzed by gas chrom...

Embodiment 2

[0020] The palladium content in the catalyst is 9.12g / L, the copper content is 1.92g / L, and the potassium acetate content is 72g / L. The feed ratio of raw materials is: propylene / acetic acid / oxygen / water=69.0 / 8.0 / 5.0 / 18.0 (molar ratio), and the space velocity is 2500hr -1 . During the reaction process, the catalyst reaction temperature was controlled to be 170° C., and the reactor inlet pressure was 0.8 MPa. Propylene, acetic acid, oxygen and water are fed after being mixed in the preheater. According to the oxygen content analysis result of the online analysis port, supplement the oxygen content to 3% through the oxygen supplement port. Other conditions are with embodiment 1.

Embodiment 3

[0022] According to the oxygen content analysis result of the online analysis port, supplement the oxygen content to 6% through the oxygen supplement port. Reactor, reaction conditions and catalyzer are with embodiment 1. Due to the large amount of oxygen supplementation, the side reactions increase and the selectivity decreases significantly, so the supplementation of oxygen should not be too much.

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Abstract

The invention relates to a method for preparing 2-propenyl ethanoate by using a propylene gas phase oxidation method and mainly aims to solve the problems of low per-pass conversion between propylene and acetic acid, low space time yield and selectivity of reaction in the prior art. The problems are better solved by using the technical scheme that raw material mixing gas and a catalyst bed (1) are in contact for reaction in a fixed bed vertical tubular reactor to obtain a reaction product containing 2-propenyl ethanoate, wherein the fixed bed vertical tubular reactor is provided with at least one oxygen replenishing port (4) at the position which is 1 / 5 to 4 / 5 of the height of the catalyst bed, an online analysis port (5) corresponding to the oxygen replenishing port (4) is arranged near the upstream of the oxygen replenishing port (4), and oxygen is replenished through the oxygen replenishing port (4) according to an online analysis result so that the concentration of the oxygen is kept 3-4% of reaction mixed gas in molar percentage. The method can be used for industrial production of the 2-propenyl ethanoate prepared by using the propylene gas phase oxidation method.

Description

technical field [0001] The invention relates to a method for preparing allyl acetate by gas-phase oxidation of propylene, using propylene, acetic acid, water and oxygen or an oxygen-containing gas as raw materials. Background technique [0002] Propylene acetate is an important organic chemical raw material. Propyl acetate is hydrolyzed to produce allyl alcohol, dichloropropanol is synthesized, and dichloropropanol is saponified to produce epichlorohydrin. Allyl acetate is industrially mainly reacted with propylene and oxygen under the action of palladium and co-catalyst in the presence of acetic acid to produce allyl acetate. This reaction is carried out in a reaction tube equipped with a catalyst, the reaction temperature is about 150-190°C, the reaction pressure is 0.6-1.0MPa, and the space velocity is about 2000-4000hr -1 . Section 2.1 on page 9 of the "Jinshan Oil Chemical Fiber" periodical, Volume 19, No. 4, 2000, introduces the existing fixed-bed standpipe reactor f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/54C07C67/055
Inventor 张丽斌杨运信
Owner CHINA PETROLEUM & CHEM CORP