Method for preparing isophorone by acetone liquid condensation with alkali catalyst

A technology of isophorone and catalyst, applied in the field of preparation of isophorone, can solve the problems of low single-pass conversion rate of acetone, low effective selectivity of isophorone, high process cost, etc.

Active Publication Date: 2014-01-01
WANHUA CHEM GRP CO LTD +1
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0011] The object of the present invention is to overcome the disadvantages such as low conversion rate of acetone per pass, low effective selectivity of isophorone, high process cost and the like in the previous liquid-phase method for synthesizing isophorone, and provide a kind of acetone that can be synthesized under the condition of alkaline catalyst. A new method for preparing isophorone by liquid phase condensation can significantly enhance the mass transfer and heat transfer effects of the reaction system, improve the single-pass conversion rate of acetone and the effective selectivity of isophorone, and is simple and reliable, with economic advantages

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  • Method for preparing isophorone by acetone liquid condensation with alkali catalyst

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Experimental program
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Effect test

Embodiment 1

[0032] according to figure 1 The technological process, under continuous steady-state operating conditions, fresh acetone is heated to 230 ℃ through heat exchanger 9 with the flow rate of 100kg / h and the reclaimed acetone (mainly acetone, other about 18wt%) of rectification step from the back , and then preheated to the same temperature, flow rate 38kg / h, KOH aqueous solution with a concentration of 1.8% enters the mixer 7 and mixes fully. After mixing, the mass flow ratio of acetone and water is about 4: 1, and KOH is in the total mixture. The mass fraction is about 0.1%. The mixer adopts SV-type high-efficiency static mixer with a pipe diameter of 20mm and a length of 1m. The residence time of the reaction liquid in the mixer is 15s. The acetone conversion rate is 2% through gas chromatography analysis. Then the reaction solution enters the microchannel reactor 6 produced by Wanhua Polyurethane Company to react. The channel cross section is circular, the inner diameter of t...

Embodiment 2

[0034] according to figure 1 The technological process, under continuous steady-state operating conditions, after fresh acetone is mixed with the reclaimed acetone (mainly acetone, about 18wt% of water) from the rectification step behind with the flow rate of 100kg / h, it is pre-heated by heat exchanger 9 Heat to 280°C, and then fully mix with the KOH solution with a flow rate of 12kg / h and a concentration of 5.0% that is preheated to the same temperature through the mixer 7. At this time, the mass ratio of acetone and water is about 5:1, and KOH is in the total mixture. The mass fraction in is 0.12%. The mixer adopts SV type high-efficiency static mixer with a pipe diameter of 20mm and a length of 1m, and the residence time of the reaction liquid in the mixer is 3s. Then the reaction solution enters the microchannel reactor 6 produced by Wanhua Polyurethane Company for reaction. The inner diameter of the microchannel is 1.5 mm, the number of channels is 1200, the reaction tem...

Embodiment 3

[0036] according to figure 1 The technical process, under continuous steady-state operating conditions, fresh acetone is mixed with reclaimed acetone (mainly acetone, about 18% by weight of water) from the rectification step behind with the flow rate of 100kg / h after fresh acetone is preheated through heat exchanger 9 Heat to 250°C, then fully mix with the KOH solution that is preheated to the same temperature and have a flow rate of 13kg / h and a concentration of 3.2% through the mixer 7. The mass ratio of the mixed acetone and KOH solution is about 5: 1, and KOH is in the The mass fraction in the total mixture is about 0.08%. The mixer adopts SV-type high-efficiency static mixer, with a pipe diameter of 10mm, a pipe number of 30, and a length of 10m. The residence time of the reaction solution in the mixer is 1min. The acetone conversion rate is 6% through gas chromatography analysis, and then the reaction solution is mixed with a 120kg Enter the microchannel reactor 6 that ...

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Abstract

The invention discloses a method for preparing isophorone by acetone liquid condensation with an alkali catalyst. The method comprises steps of: heating an aqueous solution of acetone and the alkali catalyst to 230-280 DEG C under continuous stable operation conditions; controlling the pressure to maintain the acetone and water in liquid phase state; then introducing the two together through a mixer and a micro channel reactor with a total staying time of 3-15 min; carrying out a condensation reaction on the acetone with catalysis effect of the alkali catalyst to generate isophorone; and sending the reaction products into a reaction rectifying tower, removing unreacted acetone and hydrolyzing high boiling products with carbon atom number higher than 12, so as to obtain the isophorone crude product in a column bottom. A acetone one-way conversion rate exceeds 20%, and isophorone effective selectivity reaches higher than 90%. The method of the invention generates good mass transfer and heat transfer effects and has accurately controlled reaction time, high one-way conversion rate and good effective selectivity.

Description

technical field [0001] The invention relates to a method for preparing isophorone, in particular to a method for preparing isophorone by liquid-phase condensation of acetone under an alkaline catalyst. Background technique [0002] Isophorone, chemical name: 3,5,5-trimethyl-2-cyclohexen-1-one, molecular formula C9H14O. Isophorone is one of the important products of deep processing of acetone. It has strong dissolving ability, good dispersibility and good leveling property, and it is a good solvent for various polymer materials. Because of its structure of conjugated unsaturated ketone, it can be further reacted to obtain important products such as alcohols, acids, amines, esters and isocyanates, which are widely used in industrial fields such as polyurethane elastomers, medicine, coatings, and adhesives. [0003] As an important fine chemical raw material, isophorone has developed rapidly in developed countries since the 1990s, and is currently widely used in industrially d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/603C07C45/74
Inventor 何岩员玫李浩丁建生黎源杜永顺罗务习赵文娟张志合于学丽
Owner WANHUA CHEM GRP CO LTD
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