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Method for synthesizing crotonic acid by using byproduct of croton aldehyde

A technology for by-producing crotonaldehyde and crotonic acid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate and other directions, can solve the problems of low yield of crotonic acid, complicated pretreatment method of salt-added rectification, and equipment with Corrosion and other problems, to achieve the effect of high reactivity, simple pretreatment method and high recovery rate

Inactive Publication Date: 2009-07-08
SINOPEC YANGZI PETROCHEM
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  • Summary
  • Abstract
  • Description
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AI Technical Summary

Problems solved by technology

The yield of crotonic acid synthesized by this method is low, and the salting and rectifying pretreatment method used is complicated and corrosive to equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 800g of crotonaldehyde with a content of 23.37% in a 1000ml three-necked flask of a distillation tower with a diameter of 23.37%. The by-product crotonaldehyde in the acetaldehyde plant is distilled without reflux until the tower top temperature reaches 65°C and stops. The remaining liquid in the flask weighs 371g , The kettle liquid was analyzed by gas chromatography, the mass content of crotonaldehyde was 45.75%, and the recovery rate of crotonaldehyde was 90.79%.

Embodiment 2

[0022] Add 800g of crotonaldehyde with 33.54% crotonaldehyde content in a 1000ml three-necked flask of a distillation tower with a diameter of 33.54%. Distill without reflux until the tower top temperature reaches 65°C and stop. The remaining liquid in the flask weighs 443g , The kettle liquid was analyzed by gas chromatography, the mass content of crotonaldehyde was 55.01%, and the recovery rate of crotonaldehyde was 90.82%.

Embodiment 3

[0024] Add 800g of crotonaldehyde with a 23.37% crotonaldehyde content in a 1000ml three-neck flask of a distillation tower with a diameter of 23.37%. , The kettle liquid was analyzed by gas chromatography, the mass content of crotonaldehyde was 26.50%, and the recovery rate of crotonaldehyde was 98.95%.

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Abstract

The invention relates to a method for synthesizing crotonic acid by using the by-product crotonaldehyde. The by-product crotonaldehyde with a content of 20-40% is subjected to atmospheric distillation to control the boiling point of the overhead distillate at 25°C-65°C to remove light Components, the content of crotonaldehyde in the still liquid can be increased to 45-60%. With the still liquid as the raw material, acetone, acetic acid, benzene or toluene as the solvent, phosphomolybdic acid as the main catalyst, and vanadium pentoxide as the The co-catalyst is used to synthesize crotonic acid through oxygen reaction at a reaction temperature of 30-100°C and a pressure of 0.3-0.9 MPa. Phosphomolybdic acid can also be loaded on activated carbon, SiO2, γ-Al2O3, molecular sieve and other carriers to make a supported catalyst, and the catalyst can be separated from the reaction solution by filtration, and dried in the air at 120°C for 3 hours can be used recycle. After the reaction product is separated from the catalyst, the solvent is distilled off, recrystallized twice with deionized water, and vacuum-dried to obtain a crotonic acid product with a mass content of more than 99%. The method of the invention is simple and effective, and the yield of crotonic acid is high.

Description

technical field [0001] The invention relates to a comprehensive utilization method of chemical by-products, in particular to a method for synthesizing crotonic acid by utilizing the by-product crotonaldehyde. Background technique [0002] Acetaldehyde is an important raw material for the synthesis of acetic acid, pyridine, pentaerythritol and sorbic acid, and its main industrial production methods include ethanol oxidation and ethylene direct oxidation. Due to the active nature of acetaldehyde, in the production process of acetaldehyde, two molecules of acetaldehyde undergo condensation and dehydration reaction to form crotonaldehyde, and the by-product crotonaldehyde is extracted from the side line at the 8th tray in the upper part of the acetaldehyde refining tower. The chemical components include crotonaldehyde, acetaldehyde, water and paraldehyde, etc. Crotonaldehyde and water also form a binary azeotrope, and crotonaldehyde is chemically active and easy to polymerize, s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/235C07C57/08B01J27/199
Inventor 乔旭李维新汤吉海温从科崔咪芬秦建元赵宝明
Owner SINOPEC YANGZI PETROCHEM
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