Production method of 1-octen-3-one

A production method and technology of octene, which is applied in the production field of 1-octen-3-one, can solve the problems of unreasonable post-treatment process design, complex product components, and increased operation difficulty, so as to improve the aroma quality and simplify operation Steps, the effect of shortening the reaction time

Pending Publication Date: 2021-12-31
TENGZHOU TIANSHUI BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It not only wastes raw materials, but also causes environmental pollution. In addition, after the chlorination reaction is completed, the excess thionyl chloride in the reaction system is all hydrolyzed and neutralized, which wastes raw materials and increases the difficulty of operation.
[0010] 2) In the existing 1-octen-3-one production process, the design of the post-treatment process is unreasonable, the composition of the product is relatively complicated, the product purity is low, and the aroma of the product is poor

Method used

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  • Production method of 1-octen-3-one
  • Production method of 1-octen-3-one
  • Production method of 1-octen-3-one

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0036] Synthesis of 1-octen-3-ol;

[0037] 100L enamel reaction kettle, with a material dropping pipe (connected to a metering pump), add 52kg of solvent methyl tert-butyl ether, 2.32kg of magnesium chips, 1.5kg of chloropentane into the reaction kettle and start stirring, heat up to 40°C, When the liquid in the kettle starts to turn, it means that it has been started. When the temperature rises to 58°C, the water can be passed to cool down until the heat release is slow, and the start-up is completed. Then begin to beat with the speed of 4kg / h with metering pump, remaining 10kg chloropentane, reaction exotherm is obvious, control reaction temperature at 55 ± 2 ℃, when temperature is higher than 57 ℃, automatically cut off feeding system (if necessary, also can Manually control the flow of water to cool down), about 2.5 hours to complete the beating, control the temperature at 55±2°C and react for 2 to 3 hours, let the magnesium react completely, and observe the phenomenon to ...

Embodiment 2

[0041] Synthesis of 1-octen-3-ol;

[0042] 100L enamel reaction kettle, equipped with a material dropping pipe (connected to the metering pump), add 52kg of solvent methyl tert-butyl ether, 2.62kg of magnesium chips, 1.5kg of chloropentane into the reaction kettle and start stirring, heat up to 40°C, When the liquid in the kettle starts to turn, it means that it has been started. When the temperature rises to 58°C, the water can be passed to cool down until the heat release is slow, and the start-up is completed. Then begin to beat with the speed of 4kg / h with metering pump, remaining 10kg chloropentane, reaction exotherm is obvious, control reaction temperature at 55 ± 2 ℃, when temperature is higher than 57 ℃, automatically cut off feeding system (if necessary, also can Manually control the flow of water to cool down), about 2.5 hours to complete the beating, control the temperature at 55±2°C and react for 2 to 3 hours, let the magnesium react completely, and observe the phe...

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Abstract

The invention discloses a production method of 1-octen-3-one. The production method comprises the following steps: adding a solvent methyl tert-butyl ether and magnesium chips into a reaction kettle, sealing the reaction kettle, replacing air in the kettle with nitrogen, pumping chloropentane into the reaction kettle by using a metering pump according to regulations, controlling the temperature to be 55 + / -2 DEG C, reacting, transferring reaction liquid in the kettle into a condensation kettle after the reaction is finished, performing condensation, adding water to hydrolyze after condensation, neutralizing, layering, and concentrating a water phase by using methyl tert-butyl ether to obtain crude 1-octen-3-ol; and adding a catalyst into the crude 1-octen-3-ol, introducing oxygen for 5-8 hours, cooling cooling, and carrying out reduced pressure rectification on a reaction liquid which is crude 1-octen-3-one to obtain the product.The aroma quality of the obtained product is greatly improved, the product grade is improved, and the whole production process is safe and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of food additive production, in particular to a production method of 1-octen-3-one. Background technique [0002] 1-octen-3-one is an aliphatic fragrance. It has a fresh earthy, mushroom, and vegetable aroma, and is a food flavor that can be used to prepare vegetables, fish, dairy products, and mushrooms. 1-octen-3-one can also be used as a raw material for the synthesis of butyl-decalactone. [0003] 1-octen-3-one, the molecular formula is C 8 h 14 0, the structural formula is as follows. CAS: 4312-99-6 [0004] [0005] At present, there are relatively few reports on the synthesis of 1-octen-3-one. The current synthesis method is: react thionyl chloride with n-hexanoic acid under normal pressure to form hexanoic acid chloride, and then add vinyl ether to form The β-chloroketone was hydrolyzed in an alkaline environment, neutralized with hydrochloric acid after hydrolysis, extracted, concentrated, ...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07C45/39C07C49/203C07C29/40C07C33/03
CPCC07C29/40C07C45/39C07C33/03C07C49/203
Inventor张翔洲张士金李兴华马兆锋
OwnerTENGZHOU TIANSHUI BIO TECH CO LTD