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A method and device for preparing tea aroma ketone

A technology of tea aroma ketone and isophorone, which is applied in the field of direct catalytic oxidation of α-isophorone to prepare tea aroma ketone, can solve the problems of low conversion rate and large amount of catalyst, and achieve high conversion rate, conversion rate and No reduction in selectivity and small amount of catalyst

Inactive Publication Date: 2019-10-25
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention aims at the problems existing in the above-mentioned prior art, and provides a method for preparing tea aroma ketone, which solves the problems of large amount of catalyst and low conversion rate in the prior art

Method used

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  • A method and device for preparing tea aroma ketone

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Comparison scheme
Effect test

Embodiment 1

[0024] Add 100 kg of α-isophorone, 3.5 kg of N-hydroxyphthalimide (or 3,4,5,6-tetrachloro-N-hydroxyphthalimide) into the reaction kettle (1) imine 6.5 kg or N-hydroxysuccinimide 2.5 kg), open the condenser, pass oxygen to remove the air in the reactor and pipeline. Close the exhaust valve (6), open the ventilation valve (7), and turn on the air pump (4) to circulate oxygen. The temperature of the reactor was raised to 65°C, and the reaction was carried out for 10 hours. During this period, when the pressure of the pressure gauge (8) decreases, oxygen is supplemented intermittently through the oxygen source (9) to maintain the atmospheric pressure at about 1.0 MPa, and the drain valve (5) is intermittently opened to release the water generated by the reaction to prevent the water level from being too high And return to the reactor (1). After the reaction is completed, the conversion rate of α-isophorone in the reaction kettle is 34-38% according to gas phase analysis, and the...

Embodiment 2

[0026] Add 100 kg of α-isophorone and 12 kg of N-hydroxyphthalimide into the reaction kettle (1), open the condenser, and ventilate the air in the reaction kettle and the pipeline through oxygen. Close the exhaust valve (6), open the ventilation valve (7), and turn on the air pump (4) to circulate oxygen. The temperature of the reaction kettle was raised to 95° C., and the reaction was carried out for 5 hours. During this period, when the pressure of the pressure gauge (8) decreases, oxygen is supplemented intermittently through the oxygen source (9) to maintain the atmospheric pressure at about 1.0 MPa, and the drain valve (5) is intermittently opened to drain water to prevent water from flowing back into the reactor (1) . After the reaction was completed, the conversion rate of α-isophorone in the reaction kettle was analyzed by gas phase to be 45%, and the selectivity of tea aroma ketone was 81%.

Embodiment 3

[0028] Add 100 kg of α-isophorone and 6 kg of N-hydroxyphthalimide into the reaction kettle (1), open the condenser, open the exhaust valve (6), close the vent valve (7), and open Air pump (4) feeds air. The temperature of the reaction kettle was raised to 55° C., and the reaction was carried out for 15 hours. Open the drain valve (5) intermittently to release the water generated by the reaction, so as to prevent the water level from returning to the reactor (1) due to excessive water level. After the reaction was completed, the conversion rate of α-isophorone in the reaction kettle by gas phase analysis was 35%, and the selectivity of tea aroma ketone was 91%.

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Abstract

The present invention relates to a method and an apparatus for preparing 4-ketoisophorone through catalytic oxidation of alpha-isophorone, and further provides the process conditions and the reaction device of the catalytic oxidation reaction, wherein the process conditions of the reaction comprise that 4-ketoisophorone is prepared through direct catalytic oxidation of alpha-isophorone at a temperature of 30-120 DEG C under a solvent-free condition by adopting air or oxygen as an oxidizing agent and adopting N-hydroxy phthalimide and an analog thereof as a catalyst. Compared to the method and the apparatus in the prior art, the method and the apparatus of the present invention have advantages of no solvent, low catalyst consumption, mild reaction condition, high conversion rate, good selectivity, production efficiency improving, and good practical prospect.

Description

technical field [0001] The invention relates to a method and a device for directly catalyzing and oxidizing α-isophorone to prepare tea aroma ketone. Background technique [0002] Tea aroma ketone, also known as oxyisophorone, is a natural compound present in a variety of plants. Tea aroma ketone is a light yellow liquid or solid at room temperature. Its pure product has a strong aroma and a long-lasting aroma. The aroma is slightly sour and honey-sweet woody and dried fruit. Tea aroma ketone is not only a seasoning or spice in food or cosmetic preparations, but also an intermediate for the preparation of various carotenoids, vitamins and spices. [0003] The content of tea aroma ketone in natural products is very low. At present, it mainly comes from artificial synthesis and is obtained by catalytic oxidation of α-isophorone or β-isophorone. Due to the high activity of β-isophorone oxidation reaction and the high selectivity of tea aroma ketone, most of the current resear...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/603C07C45/34
CPCC07C45/34C07C49/603
Inventor 盛学斌钱佳琦冯长瑞肖航
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY