Process for preparing acetylacetone by conversion of isopropenyl acetate and special-purpose equipment thereof

A technology of isopropenyl acetate and acetylacetone, which is applied in the field of preparation of acetylacetone, can solve problems such as limitations, and achieve the effects of thin boundary retention layer, high furnace temperature requirements, and reduced carbon deposition

Inactive Publication Date: 2009-04-29
SHANGHAI WUJING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in addition to the added water reacting with acetic anhydride to generate acetic acid, the excess water will enter the recovered acetone during the recovery process of the conversion liquid. When this part of acetone is reused to absorb ketene, it will affect

Method used

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  • Process for preparing acetylacetone by conversion of isopropenyl acetate and special-purpose equipment thereof
  • Process for preparing acetylacetone by conversion of isopropenyl acetate and special-purpose equipment thereof
  • Process for preparing acetylacetone by conversion of isopropenyl acetate and special-purpose equipment thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1 Process one

[0039] The feed rate of isopropenyl acetate is 0.15t / h, the temperature of the vaporizer is 110°C, nitrogen is added as the carrier gas, and the flow rate of nitrogen is 8Nm 3 / h, without using the self-heat exchanger, enter the reformer, the temperature of the reformer is 540°C, the residence time is 2.7s, and then condensed to room temperature through the condenser.

[0040] After analysis, the conversion liquid has a selectivity of 86.2%, a conversion rate of 90.3%, and a yield of 77.8%. The conversion liquid is clear and does not contain carbon particles. By adjusting the nitrogen flow rate, the residence time is further optimized, and the reaction selectivity and yield are further improved.

Embodiment 2

[0041] Embodiment 2 Process two

[0042] The feed rate of isopropenyl acetate is 0.15t / h, the temperature of the vaporizer is 110°C, no gas is loaded, a self-heat exchanger is used, and the preheating temperature at the outlet of the self-heat exchanger is 300°C, and it enters the reformer, and the temperature of the reformer is 580°C. The residence time is 2.7s. After conversion, it is condensed to 320°C through the heat exchanger, and then further condensed to room temperature of 25°C.

[0043] After analysis, the conversion liquid has a selectivity of 81.8%, a conversion rate of 95.5%, and a yield of 78.1%. The conversion liquid contains solid black particles, which are carbon particles. By precisely controlling the temperature of the transformation in stages, the selectivity and yield of the transformation are improved, and at the same time, the waste heat of the transformation gas is reused. Embodiment 3 Process three

Embodiment 3

[0043] After analysis, the conversion liquid has a selectivity of 81.8%, a conversion rate of 95.5%, and a yield of 78.1%. The conversion liquid contains solid black particles, which are carbon particles. By precisely controlling the temperature of the transformation in stages, the selectivity and yield of the transformation are improved, and at the same time, the waste heat of the transformation gas is reused. Embodiment 3 Process three

[0044] The feed rate of isopropenyl acetate is 0.15t / h, the temperature of the vaporizer is 110°C, nitrogen is added as the carrier gas, and the flow rate of nitrogen is 8Nm 3 / h, feed from the heat exchanger, the preheating temperature at the outlet of the heat exchanger is 300°C, enter the reformer, the temperature of the reformer is 530°C, the residence time is 2.7s, after the transformation, it is condensed to 320°C, and then further condensed to 20°C.

[0045] After analysis, the conversion liquid has a selectivity of 90.6%, a conversi...

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Abstract

The invention discloses a process for preparing acetylacetone by transforming acetic acid propylene and comprises the following steps of: steaming the acetic acid propylene into gas by a vaporizer; then, putting the gas to a first-way carrier gas and/or using a self heat interchanger, then leading the gas come into a reformer to get reforming gas, and finally cooling down the reforming gas. The invention also discloses a special device for the process. In the process for preparing acetylacetone by transforming acetic acidpropylene, the flow quantity of carrier gas can be adjusted according to the different inventory ratings, thereby reaching to the optimal residence time, greatly reducing carbon deposition and prolonging carbon blowing period, realizing optimal conversion rate and selectivity, and having large work condition operation window. The self heat interchanger can save energy, realize precise temperature raising in section, and raising the selectivity and yield of the transformation reaction. The combination of using the first-way carrier gas and the self heat interchanger, which are cooperated to work, can raise reaction selectivity and yield, and increase the operation flexibility in the best working conditions.

Description

technical field [0001] The invention relates to a process for preparing acetylacetone, in particular to a process for preparing acetylacetone by conversion of isopropenyl acetate. Background technique [0002] Acetylacetone is an important chemical and pharmaceutical intermediate. Its synthesis route generally adopts the acetic acid-acetone process route, that is, firstly acetone absorbs ketene under the action of a catalyst to obtain isopropenyl acetate, and then 300-600 Under the condition of ℃, acetylacetone is converted into acetylacetone. Among them, the conversion rate and the selectivity of the conversion reaction to obtain acetylacetone by converting isopropenyl acetate directly determine the difficulty of subsequent separation and the unit consumption of the product. At present, there is no simple and effective way to improve the conversion rate and selectivity. Methods. [0003] U.S. Patent 2395800 proposes a method for changing the material of the reforming furn...

Claims

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Application Information

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IPC IPC(8): C07C49/12C07C45/54
Inventor 叶小鹤曾义红陈建中胡忠
Owner SHANGHAI WUJING CHEM
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