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Method for preparing alpha-isophorone

A technology of isophorone and acetone, applied in the field of compound preparation, can solve the problems of easy deactivation of gas-phase catalysts, low reaction efficiency per unit volume reactor, etc.

Active Publication Date: 2010-01-27
ZHEJIANG UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0023] From the above literature reports, it can be seen that although the synthesis of α-isophorone by the gas phase method is improved compared with the liquid phase method, the catalyst of the gas phase method is easily deactivated, and the reaction efficiency per unit volume of the reactor is low, thus limiting its large-scale application. Application in production

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  • Method for preparing alpha-isophorone

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Experimental program
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Effect test

Embodiment 1

[0030] according to figure 1 In the process flow shown, acetone is pressurized to 3.2MPa through pump 1 at a flow rate of 100Kg / hour under continuous steady-state operating conditions, and then mixed with the recovered acetone mixture, and then pressurized to 8.0MPa through pump 2. After being preheated to 280°C by preheater 4, it is mixed with 2Kg / hour 10% NaOH solution pressurized to the same pressure, and then enters pipeline reactor 5 for supercritical reaction, and the reaction residence time is 3 minutes. The reaction liquid is decompressed to 3.0MPa through the pressure reducing valve 6 and then enters the flash tower 7 with 4m AX packing, and the mixture of unreacted acetone and intermediate mesityl oxide evaporated from the top of the tower is condensed and recovered by the condenser 8 Acetone mixture. The top reflux ratio of the flash tower is controlled to be 0.3, and the continuously recovered acetone mixture is boosted by the pump 3 and recycled for reaction. Th...

Embodiment 2

[0032] according to figure 1In the process flow shown, under continuous steady-state operating conditions, acetone is pressurized to 4.2MPa through pump 1 at a flow rate of 100Kg / hour, then mixed with the recovered acetone mixture, and then pressurized to 20.0MPa through pump 2. After being preheated to 320°C by preheater 4, it is mixed with 0.5Kg / hour 10% NaOH solution pressurized to the same pressure, and then enters pipeline reactor 5 for supercritical reaction, and the reaction residence time is 2 minutes. The reaction liquid is decompressed to 4.0 MPa by the pressure reducing valve 6 and then enters the flash tower 7 with 2 meters of CY packing, and the mixture of unreacted acetone and intermediate mesityl oxide evaporated from the top of the tower is condensed and recovered by the condenser 8 Acetone mixture. The top reflux ratio of the flash tower is controlled to be 0.3, and the continuously recovered acetone mixture is boosted by the pump 3 and recycled for reaction....

Embodiment 3

[0034] according to figure 1 In the process flow shown, acetone is pressurized to 3.7MPa through pump 1 at a flow rate of 100Kg / hour, and then mixed with the recovered acetone mixture, and then pressurized to 15.0MPa through pump 2. After being preheated to 300°C by preheater 4, it is mixed with 5Kg / hour 10% KOH solution pressurized to the same pressure, and then enters pipeline reactor 5 for supercritical reaction, and the reaction residence time is 1 minute. The reaction liquid is decompressed to 3.5 MPa by the pressure reducing valve 6 and enters the flash tower 7 with 3 meters of BX packing, and the mixture of unreacted acetone and intermediate mesityl oxide evaporated from the top of the tower is condensed and recovered by the condenser 8 Acetone mixture. The top reflux ratio of the flash tower is controlled to be 0.3, and the continuously recovered acetone mixture is boosted by the pump 3 and recycled for reaction. The liquid in the flash tower enters the hydrolysis to...

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Abstract

The invention discloses a method for preparing alpha-isophorone, which comprises the following steps: pressurizing a mixture of acetone and recycled acetone to 8.0-20.0MPa under the condition of continuous steady state operation and preheating to 280 DEG C-320 DEG C; then mixing the mixture with 10 percent of NaOH solution or 10 percent of KOH solution pressurized to the same pressure; carrying out super-critical reaction for 1-3 min in a pipe type reaction vessel; decompressing the reaction liquid to 3.0-4.0MPa and entering a flashing steam tower; obtaining the recycled acetone mixture from the top of the tower; leading tower kettle liquid to enter a hydrolyzing tower to hydrolyze polymers (C12 and C15); continuously extracting hydrolyzed reaction liquid from a tower kettle of the hydrolyzing tower, cooling, decompressing to normal pressure and layering in a layering device to obtain an alpha-isophorone rough product layer and a byproduct water layer. The method for synthesizing the alpha-isophorone has short needed reaction time, few byproducts and high reaction yield and is suitable for industrialized production.

Description

technical field [0001] The present invention relates to a preparation method of compounds, in particular to a preparation method of α-isophorone. Background technique [0002] α-isophorone (3,5,5-trimethyl-2-cyclohexen-1-one) is an important fine chemical product, it has strong dissolving ability, good dispersion and leveling property, and is used by many An excellent solvent for polymer resins; in addition, it is also an important raw material for organic synthesis, which can be used to synthesize fine chemical products such as 3,5-dimethylphenol, isophorone diisocyanate, and tea aroma ketone. [0003] α-isophorone is usually synthesized by acetone liquid phase or gas phase condensation. [0004] The liquid-phase condensation method is usually carried out in a liquid state below the critical point of acetone. The liquid-phase condensation reaction requires an alkaline catalyst, which was calcium oxide or sodium amide (US2,399,976, DE134,982) in the early stage, but the ca...

Claims

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Application Information

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IPC IPC(8): C07C49/603C07C45/74
Inventor 陈志荣李浩然尹红徐勇王纯超
Owner ZHEJIANG UNIV
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