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

An acetylacetone, high-efficiency and energy-saving technology is applied in the preparation field of chemical or pharmaceutical intermediates, and can solve the problems of high requirements for transfer equipment, running, running, dripping, leaking, and insufficient process continuity, and improving equipment utilization. , The effect of reducing dosage and reducing the use of conveying equipment

Active Publication Date: 2015-05-06
JILIN BEISHA PHARMA
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  • Summary
  • 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

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preparation example Construction

[0038] Schematic diagram of the preparation device of acetylacetone image 3 , cracking acid comes from cracking acid pump, through cracking acid vaporizer 1, cracking gas cooler 2 and vacuum pump 4, then enters cracking gas recooler 6 after being separated by oil anhydride separator 5, obtains ketene gas after cracking; The ketone gas is introduced into the absorption esterification kettle 7, and the absorption esterification kettle 7 is provided with an absorption primary condenser 9 and an absorption secondary condenser 8, and the absorption esterification kettle 7 is also connected with an acetone feeding flowmeter 10, an acetone spray flowmeter 11 and acetone spray tower 12, the connecting pipe section of acetone spray tower 12 and acetone feeding flowmeter 10, acetone spray flowmeter 11 is provided with acetone spray pump 19, and one side of acetone spray tower 12 is connected with acetone inlet Material flow meter 13, acetone feed flow meter 13 links to each other with ...

Embodiment 1

[0045] The schematic diagram of the preparation process is shown in figure 2 .

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

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

example 2

[0050] First add 1000kg of acetone to the absorption esterification kettle, then crack the pyrolysis acid at 750°C into ketene mixed gas and continuously feed it into the absorption esterification kettle, and at the same time add acetone continuously at a rate of 150kg / hr, and continuously draw out the esterification through the overflow port Liquid to the crude steamer, control the temperature of the crude steamer at 90°C, and continue to evaporate, so that the mixed gas continuously enters the acetone recovery tower, and at the same time turn on the reboiler steam of the acetone recovery tower, control the temperature of the tower kettle at 98±2°C, and reflux at the top of the tower , start to extract and recover acetone, control the temperature at the top of the tower to 54±2°C, then turn on the discharge pump of the acetone recovery tower kettle, control the liquid level of the tower kettle to be stable, continuously feed the isopropenyl acetate rectification tower, and then...

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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 a chemical or pharmaceutical intermediate, in particular to a high-efficiency and energy-saving preparation method of acetylacetone and a preparation device thereof. Background technique [0002] In the prior art, the preparation process route of acetylacetone is as figure 1 Shown: a certain concentration of acetic acid is cracked at high temperature to obtain vinyl ketone, and then the esterification solution of the mixture of intermediate isopropenyl acetate and acetone is obtained through the acetone absorption and esterification reaction, and then the acetone and isopropylene acetate in the esterification solution are separated by batch distillation. Esters, etc. are separated from high-boiling impurities, and then enter the rectification separation to obtain relatively pure isopropenyl acetate and recover acetone. Distillation to obtain the finished product of acetylacetone...

Claims

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Application Information

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