High-efficiency energy-saving preparation method and preparation device of acetylacetone

An acetylacetone, high-efficiency and energy-saving technology, applied in the field of chemical or pharmaceutical intermediate preparation, can solve the problems of high requirements on transfer equipment, insufficient process continuity, running, running, dripping, leaking, etc., to improve equipment utilization. , The effect of reducing the use of conveying equipment and reducing the amount of consumption

Active Publication Date: 2013-10-02
JILIN BEISHA PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The specific preparation method is to use acetone to absorb the ketene cracked by acetic acid to obtain an esterification solution containing about 70% isopropenyl acetate, which also has a small amount of solids, and then distill isopropenyl acetate, acetone, etc. The boiling point is separated from the high boiling point acetic anhydride and a small amount of solids, and then the isopropenyl acetate and acetone are condensed and collected, and then enter the acetone recovery tower to recover acetone, and then enter the isopropenyl acetate rectification tower to purify the isopropenyl acetate, and then The isopropenyl acetate liquid is gasified and enters the indexing furnace for isomerization to obtain a mixed gas containing about 80% acetylacetone. After cooling and condensing to wait for the indexing liquid, and then rectifying to obtain the finished product of acetylacetone. The process of repeated evaporation, condensation, re-evaporation, and re-condensation has high energy requirements, and consumes a large amount of steam and cooling water, which is not conducive to energy saving, and the liquid material also needs to be transferred multiple times, and the material is corroded during the production of acetylacetone. It is highly resistant, so the requirements for transfer equipment are high, and repeated evaporation and condensation will easily cause loss of materials, and it is easy to cause losses such as running, popping, dripping, and leaking. At the same time, the amount of equipment maintenance is large, which is not conducive to the improvement of system efficiency. Improvement, process continuity is not enough
[0003] CN101514151B (2012-7-18) discloses a process for preparing acetylacetone from isopropenyl acetate. The steps include steaming isopropenyl acetate into gas through a vaporizer, and then connecting the gas to a carrier gas and / or using self-heat exchange Then enter the reformer to convert the reformed gas and cool it down. However, this process is to vaporize the liquid and then transfer it. In this process, the transferred gas needs to be cooled into a liquid, which consumes a lot of energy and costs a lot.

Method used

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  • High-efficiency energy-saving preparation method and preparation device of acetylacetone
  • High-efficiency energy-saving preparation method and preparation device of acetylacetone
  • High-efficiency energy-saving preparation method and preparation device of acetylacetone

Examples

Experimental program
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preparation example Construction

[0038] Schematic diagram of acetylacetone preparation device image 3 The pyrolysis acid comes from the pyrolysis acid pump, passes through the pyrolysis acid vaporizer 1, the pyrolysis gas cooler 2, and the vacuum pump 4, and then is separated by the oil anhydride separator 5 and then enters the pyrolysis gas recooler 6, to obtain the cracked ketene gas; The ketone gas is introduced into the absorption esterification tank 7, and the absorption esterification tank 7 is provided with an absorption primary condenser 9 and an absorption secondary condenser 8. The absorption esterification tank 7 is also connected with an acetone feeding flow meter 10 and an acetone spray flow meter 11 and acetone spray tower 12, acetone spray tower 12 and acetone feeding flow meter 10, acetone spray flow meter 11 is provided with an acetone spray pump 19 on the connecting pipe section, and one side of acetone spray tower 12 is connected with acetone inlet The material flow meter 13, the acetone fe...

Embodiment 1

[0045] See the schematic diagram of the preparation process figure 2 .

[0046] First, 1000kg of acetone is added to the absorption esterification kettle, and then the pyrolysis acid is cracked at 700°C into ketene mixed gas and continuously passed into the absorption esterification kettle, and at the same time, acetone is continuously added at a rate of 120kg / hr.

[0047] Continuously lead the esterification liquid to the crude steamer through the overflow port, control the temperature of the crude steamer to 90℃, and continuously evaporate, so that the mixed gas continuously enters the acetone recovery tower, at the same time, open the reboiler steam of the acetone recovery tower, and control the temperature of the tower and kettle to 98± 2℃, after the reflux at the top of the tower, start to produce and recover acetone, control the temperature at the top of the tower to 54±2℃, and then turn on the acetone recovery tower kettle discharge pump to control the tower kettle liquid le...

example 2

[0050] First add 1000kg of acetone to the absorption esterification kettle, then the pyrolysis acid is cracked into ketene mixed gas at 750℃ to continuously pass into the absorption esterification kettle, at the same time, acetone is continuously added at the rate of 150kg / hr, and the esterification is continuously drawn through the overflow port Liquid to the crude steaming kettle, control the temperature of the crude steaming kettle to 90℃, continuously evaporate, make the mixed gas continuously enter the acetone recovery tower, and open the reboiler steam of the acetone recovery tower at the same time, control the temperature of the tower kettle to 98±2℃, and reflux at the top of the tower , Start to produce and recover acetone, control the temperature of the top of the tower to 54±2℃, then turn on the acetone recovery tower bottom discharge pump to control the level of the tower bottom to stabilize, and continuously feed the isopropenyl acetate distillation tower, and then tu...

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Abstract

The invention relates to a preparation method of a chemical or medical intermediate, and in particular relates to a high-efficiency energy-saving preparation method and preparation device of acetylacetone. The method sequentially comprises the steps of: adding acetone and introducing ketene simultaneously, proceeding with the reaction through continuously introducing isopropenyl acetate esterification liquid, continuously discharging the isopropenyl acetate esterification liquid to a simple distillation still, continuously distilling off mixed vapor containing the acetone and isopropenyl acetate, enabling the simply distilled mixed gas to enter an acetone recycling tower, carrying out rectification, recycling the acetone, enabling tower bottoms of the acetone recycling tower to enter an isopropenyl acetate rectifying tower, carrying out rectification, enabling the isopropenyl acetate gas from the tower top to enter into a transposition process after passing through a heat exchanger, carry out an isomerization reaction, enabling the produced transposition mixed gas to enter an end product rectifying tower after exchanging heat with the isopropenyl acetate gas, carrying out rectification and obtaining end products of the acetylacetone. The method has the advantages of realizing the continuous production, greatly reducing the energy consumption, reducing the production cost and achieving the effects of energy conservation and emission reduction.

Description

Technical field [0001] The invention relates to a preparation method and a preparation device of chemical or pharmaceutical intermediates, in particular to a preparation method and a preparation device of high-efficiency and energy-saving acetylacetone. Background technique [0002] In the prior art, the preparation process of acetylacetone is as follows figure 1 Shown: A certain concentration of acetic acid is pyrolyzed to obtain ketene, and then an esterified mixture of isopropenyl acetate and acetone is obtained by acetone absorption and esterification reaction, and then the acetone and isopropenyl acetate in the esterified liquid are obtained by batch distillation Esters are separated from high-boiling impurities, and then they are separated by distillation to obtain relatively pure isopropenyl acetate and recovered acetone. Isopropenyl acetate is isomerized to obtain crude acetylacetone transposition liquid, and then the transposition liquid is passed through the refined Dis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/14C07C45/54B01D3/02
CPCY02P20/10
Inventor 黄升刘斌
Owner JILIN BEISHA PHARMA
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