A kind of preparation method of sec-butyl acetate

A technology of sec-butyl acetate and acetic acid, which is applied in the field of preparation of sec-butyl acetate, can solve problems such as equipment corrosion, environmental pollution, and short service life of catalysts, and achieve the effects of improving quality, reducing separation difficulty, and improving stability

Active Publication Date: 2016-01-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The reaction of acetic acid and butene to prepare sec-butyl acetate will be accompanied by the side reaction of butene polymerization, and generate C which is difficult to separate. 8 Olefins, and the boiling point of this type of olefin impurity is very close to the boiling point of the target product, it is difficult to separate, which greatly increases the difficulty of refining sec-butyl acetate, and also seriously affects the purity of the product
[0005] CN1844076A takes sulfuric acid as catalyzer, produces butyl acetate with reactive distillation method, uses sulfuric acid as catalyzer, will inevitably cause corrosion to equipment, and discharge a large amount of acid-containing waste water, serious environmental pollution problem
CN184187C discloses with superacid SO 4 2- / Fe 2 o 3 -ZrO 2 -SiO 2 As a catalyst to catalyze the reaction of acetic acid and butanol, due to the superacid in the reaction process, especially in the presence of water, SO 4 2- It is easy to lose, causing the catalyst to be deactivated, and the deactivated catalyst is difficult to regenerate, and the service life of the catalyst is short
The sulfonic acid group of the resin catalyst is easy to lose during the reaction, resulting in catalyst deactivation, and the metal ions carried by the reaction raw materials during transportation and storage will also poison the catalyst
"Chemical Engineer" 2007 No. 3 reported the use of SnCl 4 Modified cation exchange resin catalyst to solve the problem of catalyst deactivation, but its conversion rate only reached 70%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] D005 type resin catalyst is used in the reaction of acetic acid and 1-butene to synthesize sec-butyl acetate. The reaction is carried out on a fixed-bed continuous reaction device, the reaction temperature is 100°C, the reaction pressure is 3.0MPa, the molar ratio of enoic acid is 3, and the acetic acid to The volume space velocity of the catalyst is 0.8h -1 , and the reaction results are shown in Table 1.

Embodiment 2

[0025] DNWⅡ type resin catalyst is used in the reaction of acetic acid and 1-butene to synthesize sec-butyl acetate. The reaction is carried out on a fixed-bed continuous reaction device, the reaction temperature is 100°C, the reaction pressure is 3.0MPa, the molar ratio of enoic acid is 3, and the acetic acid to The volume space velocity of the catalyst is 0.8h -1 , and the reaction results are shown in Table 1.

Embodiment 3

[0027] 1. Preparation of metal-modified ion-exchange resin catalyst: a: Wash 70 grams of hydrogen-type styrene-based strongly acidic cation-exchange resin with deionized water for 5 times, each time for 20 minutes, and dry in a vacuum oven at 90°C for 20 hours ; B: the dried hydrogen-type strongly acidic cation exchange resin and 350g mass percent are 15% FeCl 3 The ethanol solution was modified under stirring for 7.5 hours, washed 5 times with absolute ethanol, 5 minutes each time, and dried in a vacuum oven at 90°C for 20 hours; c: The dried hydrogen-form cation exchange resin was washed with 0.5 % of SnCl 4 300 g of ethanol solution was reacted under stirring for 8 hours; d: Washed 5 times with absolute ethanol for 20 minutes each time, and dried in a vacuum oven at 90° C. for 20 hours to obtain a metal-modified ion exchange resin catalyst.

[0028] 2. Use this catalyst in the reaction of acetic acid and 1-butene to synthesize sec-butyl acetate. The reaction is carried out...

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Abstract

The invention discloses a preparation method of alcohol sec-butyl acetate. According to the method, acetic acid and butylene are used as raw materials, ion-exchange resin is used as a catalyzer, reaction is performed under the action of nitrogen and hydrogen mixture, the mol ratio of hydrogen to nitrogen in the nitrogen and hydrogen mixture is 1:1 to 10:1, and the hydrogen partial pressure of the hydrogen in a reaction system is 0.4 to 2.4 MPa. The method can not only reduce the generation of C8 olefin which is difficult to separate, but also be operated stably during a long period.

Description

technical field [0001] The present invention relates to a kind of preparation method of sec-butyl acetate, specifically relate to a kind of method that is raw material preparation sec-butyl acetate with acetic acid and butene. Background technique [0002] Second-butyl acetate is one of the four isomers of butyl acetate. It is a colorless, flammable liquid with a fruity aroma. It is insoluble in water and miscible with ethanol and ether. Second-butyl acetate is widely used in nitrocellulose, paint, artificial leather, medicine, paint, fragrance, ink and plastic industries. At the same time, it can also be used as extractant, dehydrating agent and metal cleaning agent and other components. [0003] There are two process routes for the production of sec-butyl acetate: one is to use acetic acid and sec-butanol as raw materials, and sulfuric acid or other strong acids are used as catalysts to obtain sec-butyl acetate through esterification reaction; the other is to use acetic a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/14C07C67/04B01J31/08
CPCB01J31/08C07C67/04C07C69/14
Inventor 刘野霍稳周李花伊魏晓霞田丹
Owner CHINA PETROLEUM & CHEM CORP
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