Method for preparing methyl heptenone from waste liquid of dehydrogenated linalool production

A technology of dehydrolinalool and methyl heptenone, which is applied in the field of manufacturing methyl heptenone, can solve the problems of waste of petroleum resources, difficulty in separation, adverse effects on environmental protection, etc., and achieve the effect of easy operation and simple process

Active Publication Date: 2010-11-03
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 dark black with high viscosity and cannot be discharged directly to the environment. It usually needs to be incinerated. Not only is it difficult to separate, 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

[0017] Add a certain amount of dehydrolinalool production waste liquid into a reaction kettle with a reflux condenser, a heating device and a stirring device, and then add a required amount of alkali aqueous solution. 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 depolymerization reaction conditions of each embodiment are shown in Table 1.

[0018] The material liquid of the depolymerization reaction product is cooled to room temperature, and the oil phase material is 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, which is the crude product of methyl heptenone.

Embodiment 11～18

[0020] 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 1300mm. There is an annular expansion tube at the bottom of the rectification column, which is filled with stainless steel packing. The vacuum of the system is obtained by a 2ZX-4 rotary vane vacuum pump. Collect the overhead fraction at 72-74°C to obtain the refined product of methyl heptenone. The main rectification process conditions of each embodiment and the purity of the product are shown in Table 2.

[0021] The total raw material feeding amount of Examples 1-10 and the total product amount obtained in Examples 11-18 were measured, and the product yield was calculated to be 79.5%.

[0022] Table 1.

[0023]

alkaline solution

Waste liquid / alkaline aqueous solution (volume ratio)

Reaction temperature (°C)

Response time (hr)

...

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Abstract

The invention relates to a method to produce methyl heptenone from the production waste liquid produced by dehydrogenated linalool, and the waste liquid contains dehydrogenated linalool dimmer which is produced during the synthesizing process of the dehydrogenated linalool through ethynylation reaction of the methyl heptenone. The method comprises the processes that: the waste liquid is depolymerized in alkaline solution, the depolymerization reacting resultants is carried out oil-water phase separation, and the alkaline solution is recovered and recycled; the oil-water phase materials is distilled by steam, the oil phase materials in the gas phase condensate are collected, and the methyl heptenone is obtained. The obtained rough methyl heptenone is decompression rectified and purified, the tower top distillates between 72 to 74 DEG C are collected, and therefore the refined product is obtained. 75 to 80kg of the refined methyl heptenone products can be prepared from 100kg waste liquid. The beneficial effects of the invention is that: a green utilization method with high economic value is supplied for the waste liquid, so this part of petroleum resource can be fully used, and the exhaust of contaminants arising from the production process of the dehydrogenated linalool through the ethynylation reaction of the methyl heptenone is reduced.

Description

technical field [0001] The present invention relates to a method for producing methylheptenone from dehydrolinalool production waste liquid, the waste liquid contains dimerized dehydrolinalool and dehydrolinalool, and is produced in the acetylation reaction of methylheptenone Production process for the synthesis of dehydrolinalool. Background technique [0002] Methylheptenone is an important raw material for the preparation of dehydrolinalool, which can further 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 during the process, which contains...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/51C07C49/203
Inventor 翁羽飞郭世卓丁仙华奚军王帅
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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