CN1170828C - Process for preparing matrine water aque and powder agent by CO2 super critical extraction technology - Google Patents
Process for preparing matrine water aque and powder agent by CO2 super critical extraction technology Download PDFInfo
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- CN1170828C CN1170828C CNB021037574A CN02103757A CN1170828C CN 1170828 C CN1170828 C CN 1170828C CN B021037574 A CNB021037574 A CN B021037574A CN 02103757 A CN02103757 A CN 02103757A CN 1170828 C CN1170828 C CN 1170828C
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- matrine
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The present invention relates to a method for preparing a matrine solution and matrine powder by a CO2 supercritical extraction technique. The dry products of flavescent sophora roots are sliced and pulverized and are loaded in an extraction kettle, a CO2 medium is supplied, the pressure is controlled to be 20 to 30MPa, the temperature is controlled to be 30 to 40 DEG C, and the time is from 40 minutes to 1 hour; matrine initial powder with the content of less than 50% is made by separation by a separator twice and spray drying. The matrine solution with the content of 0.01 to 50% and the matrine powder is prepared by the matrine initial powder. The present invention which is adopted to prepare the grass pesticide matrine solution and the matrine powder has the advantages of simple process, low cost, easy operation and greatly enhanced purity of the chemical ingredients of natural plants; the purity of the chemical ingredients of the natural plants is approximate to the purity of the chemical ingredients made by industrial synthesis; because of the improvement of the purity, the disinsection is accelerated, the shelf life is prolonged, and the present invention is favorable to the commercial production of pesticides.
Description
Technical field
The invention belongs to agricultural chemicals, be specifically related to a kind of employing CO
2Supercritical extraction technique prepares the method for medicinal herb pesticide aqueous matrine solution and matrine pulvis.
Background technology
China is used for nearly 600,000 tons of the chemical pesticide of farm crop every year, and is more stable because of its chemical property, is difficult for degraded, long-term accumulation year after year, caused the severe contamination to soil, some toxic substances enter human body with biologic chain, are threatening human health and life.
Chemical pesticide is in prevention and elimination of disease and pests, also do not have and selectively injure a large amount of pest natural enemies---beneficial insect and beneficial bird, destroyed the natural control between the nature biotechnology population, cause disturbed ecological balance, pest resistance to insecticide strengthens, and insect pest is rampant more, even pesticide dosage is increasing, sick, insect pest prevents and treats more difficult and more difficult, and is more and more serious to the pollution of environment.More external scientific research institutions propose to use the biological pesticide substituting chemical pesticide, and this has become the effective way that solves the agricultural chemicals environmental pollution.The pertinent literature of domestic existing matrine sterilant is reported at present, and its preparation method generally adopts decoction water to carry, and this method technology falls behind, and active constituent content is low, and the quality guaranteed period is short, and desinsection speed is slow.If will improve content of matrine and purity, complex process, technical difficulty is big, cost height, not easy to operate and grasp.
Summary of the invention
The technical problem that the present invention mainly solves is to adopt CO
2Supercritical extraction technique prepares aqueous matrine solution and matrine pulvis, to improve matrine content and purity, prolongs the agricultural chemicals quality guaranteed period, improves desinsection speed.
Technical solution of the present invention is: the kuh-seng dry product is cut into slices, is crushed to 40～80 orders, in the extraction kettle of packing into, feed CO
2Medium, pressure-controlling are at 20～30MPa, and temperature is controlled at 30～40 ℃, time is 40 minutes to 1 hour, then through separator 2 times separate, spraying drying, make content for less than the former powder of 50% matrine, preparing content by the former powder of above-mentioned matrine is 0.01%～50% aqueous matrine solution.
The processing method of preparation aqueous matrine solution is: add double solvents in the reactor, then content is joined in the reactor less than the former powder of 50% matrine, make its dissolving, add emulsifying agent again, mix, promptly make aqueous matrine solution.
The emulsifying agent add-on is 5%～8% of an aqueous matrine solution total amount in the aqueous matrine solution: the add-on sum of double solvents and the former powder of matrine is 92%～95% of an aqueous matrine solution total amount.
For example: when matrine content was 5%, the former grain weight amount of matrine was 10% in its aqueous matrine solution, and double solvents weight is 85%, and emulsifying agent weight is 5%.
Above-mentioned double solvents adopts industrial spirit, anion surfactant, Virahol and water; Emulsifying agent is OP-10, TX-10 or peregal.
The kuh-seng dry product is cut into slices, is crushed to 40～80 orders, in the extraction kettle of packing into, feed CO
2Medium, pressure-controlling are at 20～30MPa, and temperature is controlled at 30～40 ℃, time is 40 minutes to 1 hour, then through separator 2 times separate, spraying drying, make content for less than the former powder of 50% matrine, preparing content by the former powder of above-mentioned matrine is 0.01%～50% matrine pulvis.
The processing method of preparation matrine pulvis is: composite assistant, caking agent and content are joined in the stirrer less than the former powder of 50% matrine, and stirring gets final product.
The caking agent add-on is 5%～8% of a matrine pulvis total amount in the matrine pulvis; The add-on sum of composite assistant and the former powder of matrine is 92%～95% of a matrine pulvis total amount.
For example: when matrine content was 5%, the former grain weight amount of matrine was 10% in its matrine pulvis, and composite assistant weight is 85%, and caking agent weight is 5%.
Above-mentioned composite assistant adopts wilkinite and anion surfactant; Caking agent adopts spaonin powder, tea saponin powder or starch.
In sum, adopt CO
2Supercritical extraction technique prepares the method for medicinal herb pesticide aqueous matrine solution and matrine pulvis, and technology is simple, and cost is low, and is easy and simple to handle, improved the purity of chemical ingredients in the natural phant greatly, and it is synthetic to be similar to industry.Because the raising of purity speeds up desinsection, the quality guaranteed period prolongs, and is convenient to the suitability for industrialized production of agricultural chemicals.
Embodiment
A. the embodiment for preparing aqueous matrine solution: the kuh-seng dry product is cut into slices, is crushed to 50 orders, in the extraction kettle of packing into, feed CO
2Medium, pressure-controlling are at 25～28MPa, and temperature is controlled at 30～35 ℃, and the time is 40 minutes to 1 hour, then through separator 2 times separate, spraying drying, make content and be 40%～50% the former powder of matrine.In reactor, add 944 kilograms of the double solventss formed by industrial spirit, anion surfactant, Virahol and water, be that 40%～50% the former powder of matrine joins in the reactor for 6 kilograms then with content, make its dissolving, add 50 kilograms of OP-10 emulsifying agents again, mix, make content and be 1000 kilograms of 0.26% aqueous matrine solutions.
The weight ratio of contained material is in the above-mentioned double solvents: industrial spirit accounts for 60%, anion surfactant accounts for 10%, Virahol accounts for 5%, and all the other are water.
Adopt the field control effectiveness test of the aqueous matrine solution control Chinese cabbage cabbage caterpillar of the present invention's preparation:
1, test medicine and source: 0.26% aqueous matrine solution (the present invention's preparation); 50% Volaton (Lianyun Harbour second insecticide factory produces, and is commercially available).
2, test conditions: the experimental plot is located at Yangchuan village, Xia County, and crop is an autumn cabbage, tests each sub-district cultivation management term harmonization, and cabbage caterpillar is laid particular stress on generation in being, can satisfy test conditions.
3, test method: 0.26% aqueous matrine solution, with commodity amount 30ml, three processing of 40ml, 50ml, the contrast medicament is established 50% Volaton, single processing, other establishes clear water contrast, totally 5 processing, 20 sub-districts, sub-district area 30m
2, arrange in the district at random.
Carry out the routine spraying in the cabbage caterpillar occurance peak, mu sprays medicine once with 50 kilograms of soups.Investigation insect pest situation radix before the medicine was investigated residual worm amount in 1 day, 3 days, 7 days respectively after the medication.Adopt fixed 5 points in every sub-district, every fixed 5, investigate the cabbage caterpillar quantity for totally 25, preventive effect is proofreaied and correct in statistical computation.
4, result and analysis:
From investigation result, 0.26% aqueous matrine solution control cabbage caterpillar mu 30ml, 40ml, 50ml, the average one day after preventive effect of medication is respectively 88.8%, 88.2% and 93.7%; 3 days average preventive effects are respectively 92.3%, 93.7%, 97.58% behind the medicine; 7 days average preventive effects are respectively 88.5%, 89.3% and 93.6% behind the medicine; Wherein mu all is significantly higher than the preventive effect of the Volaton (86.8%, 92.32% and 86%) of contrast medicine 50% with the preventive effect of 30～40ml.Simultaneously also as can be seen, 0.26% aqueous matrine solution control cabbage caterpillar has the advantages that speed is fast, the lasting period is long, can effectively control the harm of cabbage caterpillar.
Duration of test is not found the poisoning phenomenon.
Adopt the field control effectiveness test of the aqueous matrine solution of the present invention's preparation control spinach root knot nematode:
1, test medicine and source: 0.26% aqueous matrine solution (the present invention's preparation); 50% phoxim emulsifiable concentrate (Lianyun Harbour second insecticide factory produces, and is commercially available); 50% thiophos missible oil (Danyang, Jiangsu insecticide factory produces, and is commercially available).
2, test is handled: 1000 times of 0.26% aqueous matrine solutions; 500 times of 0.26% aqueous matrine solutions; 1000 times of 50% phoxim emulsifiable concentrates; 1000 times of 50% thiophos missible oil; Clear water is handled.
Filling root (200～250kg/ mu pouring amount) is adopted in every processing, and the sub-district area is 200m
2, do not establish repetition, the sub-district random alignment.
3, test conditions: the experimental plot is located at vegetables field, Yangchuan village, Xia County, 2 mu of areas, and the spinach root knot nematode is taken place serious.September 15 sowing, October 1 neat seedling, duration of test is not poured water, October 10 root irrigation.
Sickness rate of investigation and unit surface root knot nematode insect gall number before irritating root; 5 samplings of every processing sub-district zigzag, every some investigation area 1 * 1m
2Investigation 1m
2The spinach death rate is got 50 * 50cm at every simultaneously, degree of depth 30cm, the sampling of cutting the earth, the insect gall number of investigation root knot nematode; Irritate behind the root 10 days, investigated the sickness rate of secondary spinach and the insect gall number of unit surface in 20 days more as stated above.
4, result and analysis:
Test-results shows that 0.26% aqueous matrine solution is remarkable to spinach root knot nematode preventive effect, and preventive effect all reaches more than 84%, and 10 days, 20 days preventive effect is respectively 88.27% and 89.69% behind its Chinese medicine; 1000 times of preventive effects of handling behind the medicines 10 days, 20 days are respectively 84.76% and 86.89; It is suitable substantially that 1000 times of the Volaton of contrast medicament 50%, 50% thiophos and 0.26% aqueous matrine solutions are handled preventive effect; All reach more than 80% in 10 days preventive effects behind the medicine, all reaching more than 84% in 20 days behind the medicine.
Duration of test in the working concentration scope, does not produce detrimentally affect to the land for growing field crops spinach growth for medicament.
B. the embodiment for preparing the matrine pulvis is: make content according to the method described above and be 40%～50% the former powder of matrine.In weight ratio, 949 kilograms of the composite assistants that wilkinite with 60% and 40% anion surfactant are formed, with 50 kilograms of 5% caking agent spaonin powders and content be that 40%～50% the former powder of matrine joins in the stirrer for 1 kilogram, stirring and promptly can be made into content is 1000 kilograms in 0.05% matrine pulvis.
Adopt the field control effectiveness test of the matrine pulvis of the present invention's preparation control leek root maggot:
1, test medicine and source: 0.05% matrine pulvis (the present invention's preparation); 50% phoxim emulsifiable concentrate (Lianyun Harbour second insecticide factory produces, and is commercially available); 50% thiophos missible oil (Danyang, Jiangsu insecticide factory produces, and is commercially available).
2, test conditions: the experimental plot is located at Yangchuan village, Xia County fragrant-flowered garlic maggot and often sends out ground, and crop is a Hankow winter fragrant-flowered garlic, 2.5 mu of areas, and it is general to test each sub-district cultivation management condition, and the fragrant-flowered garlic maggot is taken place serious.
3, test is handled and method:
0.05% matrine pulvis 2kg/ mu; 0.05% matrine pulvis 4kg/ mu; 50% phoxim emulsifiable concentrate is irritated root amount 200kg/ mu for 1000 times; 50% thiophos missible oil is irritated root amount 200kg/ mu for 1000 times; Root amount 250kg/ mu is irritated in the clear water contrast.Handle the filling root July 10 calendar year 2001 at each, the sub-district area is 100m
2, do not establish repetition, the sub-district random alignment.
Before the medicine and behind the medicine 10,15 days three times, each every sub-district Z font, 5 samplings, every the 20 * 20cm that cuts the earth
2, degree of depth 10cm takes back indoor stripping and looks into record each point fragrant-flowered garlic maggot quantity, and worm tiller rate is calculated the insect population rate that goes down, and proofreaies and correct preventive effect.
5 samplings of 10 days, 15 days every sub-district Z fonts behind the medicine, the death rate of observation unit's area, every some investigation area 0.5 * 0.5m
2, to calculate the diseased plant preventive effect.
4, result and analysis:
Field experiment result shows, content is that 0.05% matrine pulvis has significant preventive effect to leek because of the fragrant-flowered garlic maggot causes dead seedling, particularly 0.05% matrine pulvis 4kg/ mu filling root preventive effect is more outstanding, its behind medicine 10 days, 20 days preventive effect respectively up to 78.9% and 86.88%, far above the preventive effect of other medicaments.
Content is that 0.05% matrine pulvis is remarkable to the prevention effect of fragrant-flowered garlic maggot, and particularly 0.05% matrine pulvis 4kg/ mu preventive effect is more remarkable, and 10 days, 15 days preventive effects are respectively 79.81% and 86.57% behind the medicine; The preventive effect that 2kg/ mu handle to be irritated root was respectively 74.77%, 83.1% in 10 days, 15 days behind medicine, suitable with the preventive effect of 1000 times of 50% thiophos, the better prevention effect is arranged, and 50% Volaton preventive effect is lower slightly, and 10 days, 15 days preventive effect is respectively 67.86% and 79.99% behind its medicine.Its efficiency time is suitable substantially with the contrast medicament, can reach fragrant-flowered garlic maggot prevention effect preferably.
The duration of test observations shows, reagent agent in the working concentration scope not the growth to leek produce detrimentally affect, and can impel the leek leaf dark green, the stem tiller is straight and upright, growing way is prosperous, and leek is had tangible stimulating growth effect.
Claims (6)
1, a kind of employing CO
2Supercritical extraction technique prepares the method for aqueous matrine solution, it is characterized in that the section of kuh-seng dry product, is crushed to 40～80 orders, in the extraction kettle of packing into, feeds CO
2Medium, pressure-controlling are at 20～30MPa, and temperature is controlled at 30～40 ℃, time is 40 minutes to 1 hour, then through separator 2 times separate, spraying drying, make content for less than the former powder of 50% matrine, preparing content by the former powder of above-mentioned matrine is 0.01%～50% aqueous matrine solution;
The processing method of preparation aqueous matrine solution is: add double solvents in the reactor, then content is joined in the reactor less than the former powder of 50% matrine, make its dissolving, add emulsifying agent again, mix, promptly make aqueous matrine solution; The emulsifying agent add-on is 5%～8% of an aqueous matrine solution total amount in the aqueous matrine solution, and the add-on sum of double solvents and the former powder of matrine is 92%～95% of an aqueous matrine solution total amount; Above-mentioned double solvents adopts industrial spirit, anion surfactant, Virahol and water.
2, a kind of employing CO
2Supercritical extraction technique prepares the method for matrine pulvis, it is characterized in that the section of kuh-seng dry product, is crushed to 40～80 orders, in the extraction kettle of packing into, feeds CO
2Medium, pressure-controlling are at 20～30MPa, and temperature is controlled at 30～40 ℃, time is 40 minutes to 1 hour, then through separator 2 times separate, spraying drying, make content for less than the former powder of 50% matrine, preparing content by the former powder of above-mentioned matrine is 0.01%～50% matrine pulvis;
The processing method of preparation matrine pulvis is: composite assistant, caking agent and content are joined in the stirrer less than the former powder of 50% matrine, and stirring gets final product; The caking agent add-on is 5%～8% of a matrine pulvis total amount in the matrine pulvis, and the add-on sum of composite assistant and the former powder of matrine is 92%～95% of a matrine pulvis total amount.
3, the method for preparing aqueous matrine solution according to claim 1 is characterized in that in the above-mentioned double solvents that industrial spirit accounts for 60%, anion surfactant accounts for 10%, Virahol accounts for 5%, and all the other are water.
4, the method for preparing aqueous matrine solution according to claim 1 is characterized in that mentioned emulsifier is OP-10, TX-10 or peregal.
5, the method for preparing the matrine pulvis according to claim 2 is characterized in that above-mentioned composite assistant adopts wilkinite and anion surfactant.
6, the method for preparing the matrine pulvis according to claim 2 is characterized in that above-mentioned caking agent adopts spaonin powder, tea saponin powder or starch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021037574A CN1170828C (en) | 2002-03-20 | 2002-03-20 | Process for preparing matrine water aque and powder agent by CO2 super critical extraction technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021037574A CN1170828C (en) | 2002-03-20 | 2002-03-20 | Process for preparing matrine water aque and powder agent by CO2 super critical extraction technology |
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| Publication Number | Publication Date |
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| CN1385228A CN1385228A (en) | 2002-12-18 |
| CN1170828C true CN1170828C (en) | 2004-10-13 |
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| CNB021037574A Expired - Fee Related CN1170828C (en) | 2002-03-20 | 2002-03-20 | Process for preparing matrine water aque and powder agent by CO2 super critical extraction technology |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101130541B (en) * | 2007-09-11 | 2010-09-29 | 重庆大学 | Method for extracting and separating matrine and oxymatrine from trialkyl phosphine oxide inverse micellar solution |
| CN101720791B (en) * | 2008-10-24 | 2014-05-28 | 沈阳东大迪克化工药业有限公司 | Matrine pure plant source pesticide |
| CN108658988A (en) * | 2017-04-01 | 2018-10-16 | 南京泽朗生物科技有限公司 | A kind of preparation method of matrine |
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