CN1416710A - Fast barbasco extracting and purifying process - Google Patents
Fast barbasco extracting and purifying process Download PDFInfo
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- CN1416710A CN1416710A CN 02153008 CN02153008A CN1416710A CN 1416710 A CN1416710 A CN 1416710A CN 02153008 CN02153008 CN 02153008 CN 02153008 A CN02153008 A CN 02153008A CN 1416710 A CN1416710 A CN 1416710A
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- rotenone
- extraction
- former medicine
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- dimethyl formamide
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Abstract
The fast barbasco extracting and purifying process mainly includes crushing derris root, leaching in leaching solvent benzene or vinyl trichloride with water-displacing agent N, N-dimethyl formamide in 2.5-10 times the derris root volume, filtering, submicron suction filtering, depression concentration, washing in methanol, and ethanol, mixture, discharging, crystallization and stoving. The said process features fast extracting speed, high production efficiency, low cost, high barbasco yield and less environmental pollution and can be used in industrial production.
Description
Technical field
The present invention relates to the insecticide technical field.
Technical background
A large amount of uses of chemical pesticide for a long time, human Pest Control has been played important function, but the residue of pesticide on crop, the vegetables Lay mankind itself's health has also been constituted the serious danger side of body, so the exploitation of biological source insecticide become an important channel of environmental protection type agricultural.The application of rotenone in insecticide can effectively address the above problem, and is characterized in not having poisoning, is difficult for residually, do not influence food quality, and insect is difficult for producing resistance and wildness again.The applicant had once applied for " process for extracting raw rotenone " patent, efficiently solve the industrial production problem of rotenone, but its extraction rate is still slower, production efficiency need improve, owing to used the carbon tetrachloride toxic solvent in the technology, had problem of environmental pollution and former medicine loss waste problem.
Summary of the invention
The purpose of this invention is to provide the former medicine fast purification of a kind of rotenone extraction method, not only extraction rate is fast for it, can improve its production efficiency greatly, reduces cost, and can effectively reduce the loss waste of environmental pollution and active ingredient, be particularly suitable for commercial Application.
One of technical scheme of the present invention is:, the former medicine fast purification of a kind of rotenone extraction method, comprise derris root is pulverized, stirring and leaching in the lixiviate still, with the leaching liquor coarse filtration, after handling, the sub-micron suction strainer enters concentrating under reduced pressure in the anti-still, air-dry or chemical method shrink, the weight proportion that it is characterized in that derris root and extraction solvent is 10-40: 100, extraction solvent is for being purified petroleum benzin, and aqua NN dimethyl formamide is caught up with in adding, its weight proportion is NN dimethyl formamide: purified petroleum benzin=2-40: 98-60, and extraction temperature is 70-80 ℃; Coarse filtration, fine filtering enter in the washer after concentrating, and wash under high pressure blowback condition, wash qualified post crystallization, release liquid, and it is qualified that clout enters the dried bath of drier, gets product; The paste rotenone after it concentrates and the weight ratio of cleaning solvent are 10-50: 90-50, and cleaning solvent is an alcohols material.
Be good with NN dimethyl formamide: purified petroleum benzin=4-20: 96-80 in the above-mentioned extraction solvent.
For making effect better, above-mentioned derris root preferably is crushed to 2.0-2.5mm sawdust shape.
Above-mentioned the most handy ethanol of cleaning solvent and methyl alcohol mixed liquor, its weight proportion are ethanol: methyl alcohol=1: 2-25.
Two of technical scheme of the present invention is: the former medicine fast purification of a kind of rotenone extraction method, comprise derris root is pulverized, stirring and leaching in the lixiviate still, with the leaching liquor coarse filtration, after handling, the sub-micron suction strainer enters concentrating under reduced pressure in the anti-still, air-dry or chemical method shrink, the weight proportion that it is characterized in that derris root and extraction solvent is 10-40: 100, extraction solvent is a trichloro-ethylene, and aqua NN dimethyl formamide is caught up with in adding, its weight proportion is NN dimethyl formamide: trichloro-ethylene=8-30: 92-70, and extraction temperature is 70-85 ℃; Coarse filtration, fine filtering enter in the washer after concentrating, and wash under high pressure blowback condition, wash qualified post crystallization, release liquid, and clout enters that to do bath in the drier qualified, gets product; The paste rotenone after it concentrates and the weight ratio of cleaning solvent are 10-50: 90-50, and cleaning solvent is an alcohols material.
Be good with NN dimethyl formamide: trichloro-ethylene=10-20: 90-80 in the above-mentioned extraction solvent.
For making effect better, above-mentioned derris root preferably is crushed to the sawdust shape of 2.0-2.5mm.
Above-mentioned alcohols cleaning solvent can be used ethanol and methyl alcohol mixed liquor, and its weight proportion is an ethanol: methyl alcohol=1: 2-25.
Good effect of the present invention is as follows: extraction rate is fast, the production efficiency height, and cost reduces greatly, and because without carbon tetrachloride Xian Di agent, so rotenone loss less wastage, the output capacity height, the availability height can effectively reduce environmental pollution, is particularly suitable for industry and applies.Be described further below in conjunction with embodiment, but not as a limitation of the invention.
Embodiment
Scheme one embodiment: get derris root and pulverize, extract, shrink gained rotenone cream is put into washer pressurization blowback Xian Di by scheme one described technology, qualified back blowing, drying is up to the standards, and gets product.Extract proportioning and temperature in the kettle such as following table 1:
Rotenone cream and washing agent proportioning such as following table 2:
Pure proportioning such as following table 3 in the washing agent:
Annotate: 10-15 ℃ commonly used of wash temperature, under crystallization temperature, to be advisable.
Scheme two embodiment: get derris root and pulverize, extract by scheme two technologies.
Extract solvent burden ratio and temperature in the kettle such as following table 4:
Annotate: rotenone cream and washing agent proportioning are with table 2, table 3.Rotenone cream water content generally is not more than 5 ‰ herein.
The rotenone that the foregoing description can make is former in index parameter such as following table 5:
| Project | Index | ||
| The top grade product | Primes | Qualified | |
| The rotenone mass fraction 〉= | ????75.0 | ????50.0 | ????35.0 |
| The water quality mark, acid (with sulfuric acid) mass fraction, | ????1.5 ????0.3 | ||
Its extraction time, comparable above-mentioned prior art shortened 1/2 to more than 2/3, as being 3h originally, now can reach 1h, so improved productivity ratio greatly, cost can reduce more than 1/3, and pollutes and lack, and because of make the Xian Di solvent without carbon tetrachloride, the rotenone dissolving is run off and reduced.
Claims (8)
1, the former medicine fast purification of a kind of rotenone extraction method, comprise derris root is pulverized, stirring and leaching in the lixiviate still, with the leaching liquor coarse filtration, enter concentrating under reduced pressure in the anti-still, air-dry or chemical method shrink after the sub-micron suction strainer is handled, the weight proportion that it is characterized in that derris root and extraction solvent is 10-40: 100; Extraction solvent is a purified petroleum benzin, and adds and to catch up with aqua NN dimethyl formamide, and its weight proportion is NN dimethyl formamide: purified petroleum benzin=2-40: 98-60, and extraction temperature is 70-85 ℃; Coarse filtration, fine filtering enter in the washer after concentrating again, wash under high pressure blowback condition, wash qualified post crystallization, release liquid, and clout enters that to do bath in the drier qualified, gets product; The paste rotenone after it concentrates and the weight ratio of cleaning solvent are 10-50: 90-50, and cleaning solvent is an alcohols material.
2, the former medicine fast purification of rotenone according to claim 1 extraction method is characterized in that N.N dimethyl formamide in the extraction solvent: purified petroleum benzin=4-20: 96-80.
3, the former medicine fast purification of rotenone according to claim 1 extraction method is characterized in that derris root is crushed to the sawdust shape of 2.0-2.5mm.
4, according to claim 1, the former medicine fast purification of 2 or 3 described rotenone extraction method, it is characterized in that cleaning solvent ethanol and methyl alcohol mixed liquor, its weight proportion is an ethanol: methyl alcohol=1: 2-25.
5, the former medicine fast purification of a kind of rotenone extraction method, comprise derris root is pulverized, stirring and leaching in the lixiviate still, with the leaching liquor coarse filtration, enter concentrating under reduced pressure in the anti-still, air-dry or chemical method shrink after the sub-micron suction strainer is handled, the weight proportion that it is characterized in that derris root and extraction solvent is 10-40: 100; Extraction solvent is a trichloro-ethylene, and adds and to catch up with aqua NN dimethyl formamide, and its weight proportion is NN dimethyl formamide: trichloro-ethylene=8-30: 92-70, and extraction temperature is 70-85 ℃; Coarse filtration, fine filtering enter in the washer after concentrating, and wash under high pressure blowback condition, wash qualified post crystallization, release liquid, and it is qualified that clout enters the dried bath of drier, gets product; The paste rotenone after it concentrates and the weight ratio of cleaning solvent are 10-50: 90-50, and cleaning solvent is an alcohols material.
6, the former medicine fast purification of rotenone according to claim 5 extraction method is characterized in that in the extraction solvent, N.N dimethyl formamide: trichloro-ethylene=10-20: 90-80.
7, the former medicine fast purification of rotenone according to claim 5 extraction method is characterized in that derris root is crushed to the sawdust shape of 2.0-2.5mm.
8, according to claim 5, the former medicine fast purification of 6 or 7 described rotenone extraction method, it is characterized in that cleaning solution ethanol and methyl alcohol mixed liquor, its weight proportion is an ethanol: methyl alcohol=1: 2-25.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02153008 CN1202727C (en) | 2002-11-25 | 2002-11-25 | Fast barbasco extracting and purifying process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02153008 CN1202727C (en) | 2002-11-25 | 2002-11-25 | Fast barbasco extracting and purifying process |
Publications (2)
| Publication Number | Publication Date |
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| CN1416710A true CN1416710A (en) | 2003-05-14 |
| CN1202727C CN1202727C (en) | 2005-05-25 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 02153008 Expired - Fee Related CN1202727C (en) | 2002-11-25 | 2002-11-25 | Fast barbasco extracting and purifying process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044440A (en) * | 2012-12-31 | 2013-04-17 | 深圳市华农生物工程有限公司 | Critical extraction method for rotenone |
-
2002
- 2002-11-25 CN CN 02153008 patent/CN1202727C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044440A (en) * | 2012-12-31 | 2013-04-17 | 深圳市华农生物工程有限公司 | Critical extraction method for rotenone |
| CN103044440B (en) * | 2012-12-31 | 2015-11-18 | 深圳市华农生物工程有限公司 | A kind of Critical extraction method for rotenone |
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| Publication number | Publication date |
|---|---|
| CN1202727C (en) | 2005-05-25 |
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Granted publication date: 20050525 |