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Method for producing methyl heptenone from dehydrogenated linalool production waste liquor

A technology for dehydrolinalool and methylheptenone, which is applied in chemical instruments and methods, separation/purification of carbonyl compounds, preparation of carbonyl compounds, etc., can solve the waste of petroleum resources, difficulty in separation of waste liquid, and poor environmental protection impact, etc.

Inactive Publication Date: 2006-12-20
SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The waste liquid is difficult to separate, it is dark black, and has a high viscosity. It cannot be discharged directly to the environment. It usually needs to be incinerated, and it is even difficult to use it as a fuel. So far, there have been no literature reports on recovery, separation, etc. of economic value.
This not only causes a certain waste of oil resources, but also has adverse effects on environmental protection.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～10

[0015] Add 200g dehydrolinalool production waste liquid in the glass reactor with reflux condenser, heating device and stirring device 1500ml, then add the alkali aqueous solution of required amount. While stirring, heat to the required reaction temperature, and the reaction pressure is normal pressure. The reaction was terminated after the desired reaction time. The main reaction conditions of each embodiment are shown in Table 1. The reaction material liquid was cooled to room temperature, and the oil phase material was obtained by standing and separating. The pressure for oil phase material is 1kg / cm 2 The water vapor is distilled, and the steamed gas phase material is condensed and separated to obtain the oil phase material as the crude product of methyl heptenone.

Embodiment 11～18

[0017] The crude methyl heptenone products obtained in Examples 1-10 were mixed and purified by rectification under reduced pressure. The inner diameter of the rectification column is 25mm, and the length of the column is 1200mm. There is an annular expansion tube at the bottom of the rectification column, which is filled with stainless steel packing. The vacuum is obtained by a ZX-4 rotary vane vacuum pump. Collect the overhead fraction at 75-78°C to obtain the refined product of methyl heptenone. The main rectification process conditions of each embodiment are shown in Table 2, and the yield of the product and the purity of the product are shown in Table 3.

[0018]

[0019] System pressure

[0020] product yield

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PUM

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Abstract

This invention relates to a method for producing methylheptenone from dehydrolinalool production waste solution, which uses didehydrolinalool produced during the methylheptenone ethynylation reaction to synthesize dehydrolinalool, comprising: 1) the waste solution performs depolymerizing reaction in NaOH or KOH solution; 2) the reaction products perform oil-water separation and NaOH or KOH solution is recovered to be used again; 3) distill the oil-phase material with steam, and collect the gas-phase cooling liquid oil-phase material so as to obtain the crude methylheptenone; 4) purify the crude methylheptenone by depression distillation and collect the top fraction at 75-78Deg C so as to produce the refined product. This invention is characterized in that it provides a green and economic method to utilize the waste solution and make full use of this petroleum resource.

Description

technical field [0001] The invention relates to a method for producing methylheptenone from dehydrolinalool production waste liquid, the waste liquid contains dimerized dehydrolinalool, which is produced from the acetylation reaction of methylheptenone to synthesize dehydrolinalyl Alcohol production process. Background technique [0002] Methylheptenone, scientific name 6-methyl-5-hepten-2-one, is an important raw material for the preparation of dehydrolinalool, which can be further used to prepare vitamin A, vitamin E, vitamin K and various spices and flavors . In the prior art, dehydrolinalool is mainly synthesized from methyl heptenone through ethynylation reaction, and the main by-product of the synthesis reaction is dimerized dehydrolinalool. Usually in the crude dehydrolinalool, there will always be 2-8 wt% dimerized dehydrolinalool. The crude product of dehydrolinalool must be processed by distillation, and a certain amount of distillation raffinate is produced dur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/203C07C45/52C07C45/82
Inventor 翁羽飞郭世卓奚军丁仙华殷慧
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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