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 cataly

Method used

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  • Method for preparing alpha-isophorone

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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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