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Method for extracting and separating NEO-Z (4,8-dimethylenenaphthalene-1,5(4H,8H)-dione) from pericarpium juglans

A technology of methylnaphthene and green bark, which is applied in the field of extraction and separation of 4,8-dimethylnaphthene-1,5-dione, which can solve the problems of environmental pollution, inability to be directly used as agricultural fertilizers, inedibility, etc.

Inactive Publication Date: 2015-11-11
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the green skin is highly alkaline, it cannot be eaten, nor can it be directly used as agricultural fertilizer. If it is directly discarded, it will cause certain pollution to the environment.

Method used

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  • Method for extracting and separating NEO-Z (4,8-dimethylenenaphthalene-1,5(4H,8H)-dione) from pericarpium juglans
  • Method for extracting and separating NEO-Z (4,8-dimethylenenaphthalene-1,5(4H,8H)-dione) from pericarpium juglans
  • Method for extracting and separating NEO-Z (4,8-dimethylenenaphthalene-1,5(4H,8H)-dione) from pericarpium juglans

Examples

Experimental program
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Effect test

preparation example Construction

[0029] The preparation method of compound of the present invention is as follows:

[0030] (1) Take 1kg green walnut peel and put it into water, the weight ratio of green walnut peel and water is 1:2-1:10;

[0031] (2) soaking and extracting at room temperature for 20-50 minutes; soaking can be assisted by ultrasonic waves or microwaves, so that the soaking time will be shorter than ordinary soaking time.

[0032] (3) Move the leached water phase into a round bottom flask, place it on a rotary evaporator, and evaporate under reduced pressure until the aqueous solution in the round bottom flask is almost colorless; during vacuum distillation, control the water bath temperature to 50°C-70°C , the vacuum degree is 0.06-0.08MPa. At this time, the yellow transparent aqueous solution in the receiving bottle is the aqueous solution containing the compound of the present invention.

[0033] (4) Take out the aqueous solution in the receiving bottle, add petroleum ether, and repeatedl...

Embodiment 1

[0038] (1) Put 1kg of fresh walnut green peel into 2L of water;

[0039] (2) Soak at room temperature for 30 minutes;

[0040] (3) Move the water phase after leaching into a round-bottomed flask, place it on a rotary evaporator and distill under reduced pressure until the aqueous solution in the round-bottomed flask is almost colorless, and it takes 30 minutes; The degree of vacuum is 0.07MPa. At this time, the yellow transparent aqueous solution in the receiving bottle is the aqueous solution containing the compound of the present invention.

[0041] (4) Take out the aqueous solution in the receiving bottle, add 1L of petroleum ether in three times for extraction, take the petroleum ether phase, and discard the water phase.

[0042] (5) Place the extracted petroleum ether phase on a rotary evaporator, and distill under reduced pressure under the condition that the temperature of the water bath does not exceed 30°C to obtain a yellow crude extract, weighing about 500 mg; the...

Embodiment 2

[0045] (1) Add 200g of fresh walnut green peel to 1L of water;

[0046] (2) Soak at room temperature for 20 minutes;

[0047] (3) Move the leached water phase into a round-bottomed flask, place it on a rotary evaporator, and evaporate it under reduced pressure for 20 minutes. At this time, the aqueous solution in the round-bottomed flask is almost colorless; during vacuum distillation, the temperature of the water bath is controlled to be 70 ° C. , the vacuum degree is 0.065MPa. At this time, the yellow transparent aqueous solution in the receiving bottle is the aqueous solution containing the compound of the present invention.

[0048] (4) Take out the aqueous solution in the receiving bottle, add 0.5L petroleum ether for extraction three times, take the petroleum ether phase, and discard the water phase.

[0049] (5) Place the extracted petroleum ether phase on a rotary evaporator, and distill under reduced pressure under the condition that the temperature of the water bat...

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Abstract

The invention provides a method for extracting and separating NEO-Z (4,8-dimethylenenaphthalene-1,5(4H,8H)-dione) from pericarpium juglans. The method comprises the following steps: (1) placing the pericarpium juglans into water for soaking and extracting, or soaking and extracting by using ultrasonic wave or microwave; (2) performing reduced pressure distillation on an aqueous phase subjected to soaking and extracting, and controlling the bath temperature to be 50 to 70 DEG C, and the vacuum degree to be 0.06 to 0.08MPa, so as to obtain a water solution containing the NEO-Z; the chemical structural formula of the NEO-Z is shown in the description. The applicant adopts an azeotropy preparation method to carry out extraction separation aiming at the characteristic of high symmetry of the NEO-Z, the cost is low, and the growth period is short.

Description

technical field [0001] The invention relates to a method for extracting and separating 4,8-dimethylnaphthene-1,5-dione from walnut green bark. Background technique [0002] Walnut is also called walnut, Juglandales (Juglandales), Juglandaceae (Juglandaceae), Juglans (Juglans L.), walnut (Juglansregia L.). Produced in North China, Northwest China, Southwest China, Central China, South China and East China. Distributed in Central Asia, West Asia, South Asia and Europe. Born in hillsides and hills at an altitude of 400-1800 meters, it is commonly cultivated in plains and hills in my country. It likes fertile and moist sandy loam. It is often found in places with deep soil layers on both sides of mountain valleys. The seed kernel has high oil content and is rich in nutrients. It can be eaten raw. It is a kind of nut that is beneficial to the human body and has the functions of strengthening the brain. [0003] Juglans green skin refers to the green skin of the fruit of the wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/78C07C45/84C07C45/79C07C49/447
CPCC07C45/78C07C45/79C07C45/84C07C49/447
Inventor 张峰瑞李亚高坤姜侃
Owner LANZHOU UNIVERSITY