CN1156479C - Process for extracting raw rotenone - Google Patents
Process for extracting raw rotenone Download PDFInfo
- Publication number
- CN1156479C CN1156479C CNB001071416A CN00107141A CN1156479C CN 1156479 C CN1156479 C CN 1156479C CN B001071416 A CNB001071416 A CN B001071416A CN 00107141 A CN00107141 A CN 00107141A CN 1156479 C CN1156479 C CN 1156479C
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- CN
- China
- Prior art keywords
- rotenone
- derris root
- tubatoxin
- acetone
- benzene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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Abstract
The present invention relates to an extraction method of a rotenone original drug, which is a method of directly extracting rotenone from derris root. The present invention comprises the technologies that the milled derris root is added in a leaching kettle to extract by benzene and acetone, stirred, tapped, put in a reaction kettle after being processed by a submicron technology, and stirred, the temperature is kept from 76 to 80 DEG C, the mixture is decompressed and concentrated, and the rotenone original drug mixture is obtained. The method of directly extracting the rotenone from the derris root, is an origination at home and abroad, has the advantages of reasonable technology, low cost, high efficiency, easy guaranteed quality, mass production and wide range of application, and has higher industrial applicable value.
Description
The present invention relates to the sterilant technical field.
A large amount of uses of chemical pesticide for a long time though human Pest Control has been played vital role, have constituted serious threat to mankind itself's health.Environment is subjected to pollution in various degree, and the chemical pesticide of getaway makes the eubiosis lose control.The research report that tissues such as NAS are delivered is pointed out: the present pesticide residues thing severe overweight in the food, be the safe capacity normal value accepted of children 100-500 doubly, children are just suffering harm such as cancer and neurotoxic.In addition, fruit tree and vegetables are the dosage maximum in farm crop, wherein the dosage of vegetables accounts for about 28% of world's sterilant market sale, the recall rate of riskiest pesticide acephatemet is the highest, account for 71.3% of the total intake of organophosphorus, only Shenzhen 1985-1990 just reaches 166 because of edible vegetable causes poisoning (acute) incident, and 5211 people rank first in the whole country.The World Health Organization estimates that annual global pesticide intoxication number reaches more than 100000 people, dead about 20000 people.Because being extensive use of of chemical pesticide makes the resistance of insect constantly increase, working concentration also increases thereupon, also makes the pesticide residue of agricultural byproducts increase year by year, has formed the vicious cycle state year after year.Ecology is damaged, and beneficial insect (bird) is out of control.Countries in the world all with environmental protection type agricultural as the agricultural development direction, the Application and Development of biological source insecticide will be a kind of important channel of realizing environmental protection type agricultural.Tubatoxin is applied in agricultural chemicals, is used for pest control, and its maximum characteristics are: " being difficult for residual ", no poisoning does not influence the food quality, and insect is difficult for producing resistance and rampant again problem.Can only from derris root, extracting at present of tubatoxin, method falls behind, and content is low, and efficient is low, not can manufacture, and turnout is little, and the manufacturing cost height can not satisfy actual needs far away.
The purpose of this invention is to provide a kind of process for extracting raw rotenone, it is to adopt scientific process method directly to extract tubatoxin from derris root, and its cost is low, and the efficient height is easy to operate, and quality easy to control has higher industrial application value.
The present invention is achieved in that a kind of process for extracting raw rotenone, earlier derris root is pulverized, and puts it in the lixiviate still with benzene and acetone extraction again, its ratio is: 100 parts in derris root powder, benzene 80-160 part, acetone 0-50 part, stir, the blowing coarse filtration enters in the reactor after handling with the submicron suction strainer again and stirs, and temperature in the kettle remains on 76-80 ℃, concentrating under reduced pressure, catch up with water, measure blowing, obtain the former medicine of tubatoxin of rotenone content＞30%.
The sawdust meal that derris root is crushed to 1.5-2.0mm is good.
Withdrawal ratio is: 100 parts in derris root powder, and benzene 80-100 part, acetone 15-35 part is preferable.
Use above-mentioned processing method, can wash through tetracol phenixin behind the blowing, freezing and crystallizing, air-dry and make the former medicine of tubatoxin, containing the tubatoxin amount during measurement is 35-98%.
The empirical formula of tubatoxin is C
23H
22O
6, structural formula is:
Above-mentioned benzene and acetone are solvent, add acetone and can improve extracted amount, only with acetone also can, but cost is too high.
Advantage of the present invention is: raw material extensively is easy to get, and extraction process is scientific and reasonable, quality easy to control, and cost is low, efficient height, but mass production, purposes is wide, and higher industrial application value is arranged.
Be described further below in conjunction with embodiment, but not as a limitation of the invention.
Embodiment:
Get derris root and pulverize, extract, obtain its material of the former medicine of tubatoxin and extracting solution proportioning and temperature in the kettle such as following table after the air-dry or chemical method of concentrating under reduced pressure is caught up with water by above-mentioned Process.
As embodiment 3, can obtain 50% the former medicine of pale brown chromatic dispersion shape solid tubatoxin, it again through the washing of four carbonoxides, freezing, crystallization, can be made 70% the former medicine of tubatoxin.
The index parameter such as the following table of the former medicine of tubatoxin that the foregoing description makes:
| Project | Index | ||
| The top grade product | First grade | Salable product | |
| The tubatoxin massfraction, % 〉= | 70.0 | 50.0 | 40.0 |
| The quality mark, %≤ | 1.5 | ||
| Benzene is not tolerant, %≤ | 0.5 | ||
| Acid (with H2SO4) massfraction, %≤ | 0.3 | ||
Above product can be used as single agent use or puts into and use after agricultural chemicals adds other solvents, auxiliary agent, emulsifying agent.Can be widely used in the sterilant of various vegetables, fruit tree and farm crop, and medicine and other fields.
Claims (4)
1, a kind of process for extracting raw rotenone is characterized in that earlier derris root being pulverized, and puts it in the lixiviate still with benzene and acetone extraction again, its ratio is: 100 parts in derris root powder, benzene 80-160 part, acetone 0-50 part, stir, the blowing coarse filtration enters in the reactor after handling with the submicron suction strainer again and stirs, temperature in the kettle remains on 76-80 ℃, concentrating under reduced pressure, air-dry or chemical method is caught up with water, measures, blowing obtains the former medicine of tubatoxin of rotenone content＞30%.
2, extraction method according to claim 1 is characterized in that derris root is crushed to the sawdust meal of 1.5-2.0mm.
3, extraction method according to claim 1 is characterized in that withdrawal ratio is: 100 parts in derris root powder, benzene 80-100 part, acetone 15-35 part.
4, according to claim 1,2 or 3 described extraction methods, it is characterized in that behind the blowing again through the tetracol phenixin washing, freezing and crystallizing, air-dry and make the former medicine of tubatoxin, containing the tubatoxin amount in the former medicine is 35-98%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001071416A CN1156479C (en) | 2000-04-21 | 2000-04-21 | Process for extracting raw rotenone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB001071416A CN1156479C (en) | 2000-04-21 | 2000-04-21 | Process for extracting raw rotenone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1273972A CN1273972A (en) | 2000-11-22 |
| CN1156479C true CN1156479C (en) | 2004-07-07 |
Family
ID=4578491
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB001071416A Expired - Fee Related CN1156479C (en) | 2000-04-21 | 2000-04-21 | Process for extracting raw rotenone |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1156479C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1319448C (en) * | 2006-01-05 | 2007-06-06 | 厦门大学 | Tubatoxin antifoulant |
| CN102669026A (en) * | 2012-05-18 | 2012-09-19 | 中国水产科学研究院淡水渔业研究中心 | Quick-acting environment-friendly pool cleaning method for procambarus clarkii |
| CN110240602B (en) * | 2019-06-21 | 2024-02-13 | 广西施乐农化科技开发有限责任公司 | Production equipment and production process of rotenone |
| CN110903297B (en) * | 2019-12-20 | 2020-10-13 | 海南省林业科学研究所 | Macroporous resin extraction method of rotenone and analogue |
| CN113336766A (en) * | 2021-06-29 | 2021-09-03 | 李群生 | Process for producing rotenone raw medicine |
-
2000
- 2000-04-21 CN CNB001071416A patent/CN1156479C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1273972A (en) | 2000-11-22 |
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|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20040707 Termination date: 20160421 |