CN1985598A - Natural pyrethrin water emulsion and its preparation - Google Patents

Natural pyrethrin water emulsion and its preparation Download PDF

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Publication number
CN1985598A
CN1985598A CN 200510048737 CN200510048737A CN1985598A CN 1985598 A CN1985598 A CN 1985598A CN 200510048737 CN200510048737 CN 200510048737 CN 200510048737 A CN200510048737 A CN 200510048737A CN 1985598 A CN1985598 A CN 1985598A
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pyrethrin
water emulsion
sodium
water
mixing
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CN1985598B (en
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李定中
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Yunnan Nanbao Biotechnology Co., Ltd.
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YUXI YALINJIE PLANT CHEMICAL CO Ltd YUNNAN
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Abstract

The pyrethrin water emulsion consists of pyrethrin 1 weight portions, synergist 1-30 weight portions, sodium benzene sulfonate 10-95 weight portions, and water 0-95 weight portions. It is water soluble, light stable and water stable. When used, it can form one air isolating layer in the surface of pest and has high pesticidal effect. It is used in killing pest in vegetable, fruit, flower, tea, Chinese medicine plant, etc. and may be also used for other purpose. It has high pesticidal effect, low residue and other advantages.

Description

Aqueous emulsion of natural pyrethrum and preparation method thereof
Technical field
The present invention relates to a kind of Dalmatian chrysanthemum preparation, especially a kind of pyrethrin water emulsion and preparation method thereof.
Technical background
China's agricultural production midium or long term is used chemical pesticide and chemical fertilizer, the use of a large amount of organic nitrogens, organic phosphor, carbamates chemical synthetic pesticide, cause the residual of a large amount of agricultural chemicals, thereby cause the pollution of soil, natural water, agricultural product, even more serious is that residue of pesticide are passed through directly to endanger human and livestock health after the food chain enrichment, use chemical pesticide in addition too much insect is developed immunity to drugs, cause dosage to increase year by year, further increase the weight of the harm of chemical synthetic pesticide.Natural pyrethrum is a kind of inhibition nerve fiber, come from the tagging property plant insecticide of feverfew Dalmatian chrysanthemum, it has the insecticidal activity height, insecticidal spectrum is wide, and multiple sanitary insect pest, stored grain insects and pest are had good control efficiency, simultaneously in occurring in nature decomposition and residual low easily, wait the homoiothermy animal safer to people and animals, therefore, enjoying the extensive concern of countries in the world, is that one of safest plant insecticide is recommended to closing ball by FAO (Food and Agriculture Organization of the United Nation).But for a long time, since Dalmatian chrysanthemum see the easy resolution characteristic of light and with the immiscible characteristics of water, the formulation development of pyrethrin is restricted always, as application number is the cream preparation that 01145597.7 Chinese patent discloses a kind of pyrethrin, solve the problem of the former pharmaceutically dosage formization of domestic Dalmatian chrysanthemum, also developed formulations such as pulvis, wetting powder, microcapsule formulations afterwards.But there is following problem in existing formulation: 1, organic solvents such as the toluene of equivalent, dimethylbenzene are arranged in the emulsifiable concentrate, not only waste petroleum resources but also can cause the pollution of environment, and because low, the easy firing of burning-point of solvent is restricted on links such as production, storing, use.Organic solvent has the medicament of promotion to crop epidermis, zoodermic osmosis, has increased the chance of agricultural chemicals to chemical injury of crops and person poultry poisoning; Organic solvent constantly is dispersed in the atmosphere in the agricultural chemicals use, causes atmospheric pollution.The environment-friendly advantage of the botanical pesticide that these harm have weakened is restricted its use in high-end organic food desinsection field.2, existing formulation be difficult to take into account the stability of insecticide efficiency and formulation, and use cost is higher, and large-scale promotion application is caused certain obstacle when solving the Dalmatian chrysanthemum formulationization.
Summary of the invention
For solving the water-soluble and stability problem of Dalmatian chrysanthemum, the invention provides a kind of novel pyrethrin water emulsion and preparation method thereof, be difficult to the barrier realized to break through pyrethrin water emulsion type for a long time always, when keeping its safety, reduce the usage amount of pyrethrin and increase insecticidal effect.
Difficult point of the present invention is to solve Dalmatian chrysanthemum and the immiscible problem of water, and keeps it to have stability preferably, improves insecticidal effect.The present invention is by being dispersed in liquid or semi-solid pesticide active ingredient in the water, effective ingredient wherein can be stablized in the medium-term and long-term maintenance of water, and under the stirring of fierceness, by emulsifier former medicine is scattered in the water, adds emulsus or transparency liquid that auxiliary agents such as stabilizing agent, antifreezing agent are modulated into then.It can reduce the pollution to environment, and is little to eyes, skin irritation, has improved the safety of production, storing and use.
Pyrethrin water emulsion provided by the invention is made up of the raw material of following mass parts:
1 part of pyrethrin
Synergist 1-30 part
Benzene sulfonic acid is received 10-95 part
Water 0-95 part.
It is the natural pyrethrin product of 1-85% that described pyrethrin adopts its net content.
Described synergist adopts one or more in piperonyl butoxide, sesamin, Octacide 264, synergy alcohol, synergy phosphorus, eucalyptus oil and the peppermint oil.
Described benzene sulfonic acid sodium salt adopts one or more in sodium alkyl sulfonate, sodium alkyl benzene sulfonate, sodium n-alkylbenzenesulfonate, a nitro paratoluenesulfonic acid sodium salt, sodium alkylamidosulfonate, calcium dodecyl benzene sulfonate, lauryl sodium sulfate, alkyl phosphate salt and the sodium alkylamidosulfonate.
Pyrethrin water emulsion provided by the invention makes by following method:
A, under 20-25 ℃ of temperature, get 1 part of pyrethrin, add 1-30 part synergist stirring and evenly mixing therein;
B, add 10-95 part benzene sulfonic acid in the thing and receive, stirred 10-30 minute with the mixing speed of 800-1000 rev/min of kind as emulsifier above-mentioned all mixing;
C, add water 0-50 part above-mentioned all mixing in the thing, making the pyrethrin effective component content is 1.5-15%, stirs 10-30 minute with the mixing speed of 800-1000 rev/min of kind, promptly makes pyrethrin water emulsion.
The present invention compared with prior art has following advantage and effect: adopt such scheme, can solve pyrethrin and the molten problem of water preferably, and can form air barrier at the insect body surface when using, drug effect is given full play to, improved insecticidal effect, help reducing pesticide dosage, in addition, the present invention can solve that natural pyrethrum is met photo-labile and problem such as instability in water, especially after benzene sulfonic acid sodium salt being allocated into as the emulsifier of pyrethrin, make product have the auxiliary insecticidal function of superior physics, can be widely used in vegetables, fruit, flowers, tealeaves, kill aphid in organic food such as Chinese herbal medicine and the pollution-free food production, plant hopper, caterpillar, cabbage caterpillar, but insects such as two spotted spider mite are other purposes insecticide of double as also outward, as: prevent and treat common sanitary insect pest indoor, as mosquito, fly, cockroach etc.; Plant is used for livestock body surface deinsectization etc.The present invention compares with existing Dalmatian chrysanthemum preparation technique and has following characteristics in addition:
1, desinsection is efficient, and under the prerequisite that keeps equal drug effect, consumption has only the 1/2-1/4 of missible oil formulation consumption, has reduced drug cost, makes its large-scale promotion application become possibility.
2, residual quantity is low, and the solvent of this formulation is a water, does not have other chemical solvent, and easily decompose in environment the use back, residual toxicity is low.
3, have tagging property more by force, the invention enables the characteristic of tagging of Dalmatian chrysanthemum to be given full play to, after the dispenser onset very fast, can control the expansion of insect pest scope fast.
Be the superiority that shows that the present invention possesses, the present invention is through field control effectiveness test, and its result is reported as follows:
1 materials and methods
1.1 reagent agent
Reagent agent 1.5% pyrethrin water emulsion is that Yuxi Yalinjie Plant Chemical Co., Ltd., Yunnan produces; Contrast medicament 20% is killed the chrysanthemum emulsifiable concentrate, and (it is that Red Sun Group Co.,Ltd. Nanjing first insecticide factory produces that active ingredient contains sumicidin 20%M/M.
1.2 for studying thing and controlling object
For to study thing is head cabbage, kind be in sweet 17.Controlling object is cabbage aphid (Brevicorynebrassicae Linnaeus).
1.3 test method
1.3.1 experimental scheme
Experimental field be located at Shang Tan village, Honggu District safety town, Lanzhou, select the heavier field piece of aphid damage, crop is on the occasion of the rosette stage.Test is carried out in the middle of the piece of field, and the outside is provided with guard row, the cultivation condition uniformity of all experimental plots.Duration of test did not have precipitation in 24 hours, poured water once in the test back on the 3rd day.750 times of liquid of 1.5% Dalmatian chrysanthemum rope aqueous emulsion, 1000 times of liquid, 3 concentration of 1250 times of liquid are established in test; Killing 1500 times of liquid of chrysanthemum emulsifiable concentrate (being 30ml/ mu) with 20% is the medicament contrast, is blank with the clear water.Sub-district area 20m 2, every processing repeats 4 times, randomized arrangement.
1.3.2 application method and time
Adopt Singapore to produce agricultural sharp HD one 400 type knapsack hand sprayer even spraying afternoon April 27, use amount of liquid medicine soup 675kg/hm 22~moderate breeze power is arranged during the dispenser.
1.3.3 investigation method
5 points are fixedly looked in every sub-district, every 2 strain totally 10 strains, and the aphid number alives of each sub-district of investigation before the dispenser, 1d, 7d investigate remaining aphid number alive respectively after the dispenser, according to the aphid number calculating insect population alive of insect population radix and each day investigation before the dispenser go down rate and control efficiency.
(DMRT) analyzes test data with the Deng Kenshi duncan's new multiple range method.Experimental scheme, investigation method, insect pest situation and preventive effect computational methods are all carried out with reference to People's Republic of China's " pesticide field efficacy medicine test criterion ".
1.4 test site reaches experimental field condition
Test site is located at Shang Tan village, Honggu District safety town, Lanzhou, and environmental condition is average temperature of the whole year 8, average temperature difference per day 13.0, and 146~173 days frost-free seasons,>0 accumulated temperature 258 days, accumulated temperature are 3410;>5 accumulated temperature 215 days, accumulated temperature 3259;>10 accumulated temperature 173 days, accumulated temperature 2904.Annual with according to the time several 2610 hours to 2350 hours, the total solar radiation amount is 125.8 kilocalories/cm 2Annual precipitation 290~360mm mainly was distributed in for 7,8,9 March, and 12~January, precipitation was minimum.
Experimental field physical features is smooth, cauliflower growing way uniformity, and aphid damage is heavier.Last earth belongs to red clay, soil-ripening degree height, and soil property is fertile, and organic matter and essential nutrient contents are higher, and the preserve moisture and fertility performance is good, organic average content 1.15%, full nitrogen 0.107%, full phosphorus 0.199%, rapid available phosphorus 11.5mg/100g, available potassium 178mg/100g.Experimental field preceding crop is multiple cropping in an autumn mulch film Chinese cabbage, is middle canopy wild cabbage studying thing, kind be in sweet 17.Ridging overlay film on the 2nd duplicate rows field planting in March, the high 15cm in ridge, spacing in the rows 33cm waters field planting water after the field planting.Spread fertilizer over the fields farmyard manure 4000kg/667m before the ridging 2, ridge central authorities ditch spread phosphorus two ammoniums.40kg/667m 2。Irrigated through furrow 1 time studying thing, be the rosette stage breeding time.Test and poured water once in the 3rd day.
2 results and analysis
2.1 result of the test
By following table as can be seen, 1 day preventive effect is respectively 92.88%, 90.82% and 88.33% after 750 times of liquid of 1.5% pyrethrin water emulsion, 1000 times of liquid, the dispenser of 1250 times of liquid control cabbage aphids: 7 days preventive effect is respectively 93.20%, 90.41% and 87.98% behind the medicine; Each preventive effect of handling of 1.5% pyrethrin water emulsion all is lower than the contrast medicament, and with contrast pharmacy control efficacy significant difference, contrast medicament 20% kill chrysanthemum emulsifiable concentrate preventive effect the 1st day be 93.25%, the 7 day be 95.68%.
2.2 influence to crop and other biology
Duration of test is through irregularly observing, and reagent agent is respectively handled cabbage plant and grown normally, the leaf look, leafly is as good as with contrast, illustrates that 1.5% pyrethrin water emulsion supplies the amount of reagent scope interior to wild cabbage safety, no poisoning.
Still can between deceiving, observe natural enemies such as a large amount of Chrysopas, ladybug in 7 days behind the medicine, show that 1.5% pyrethrin water emulsion is safer to natural enemy.
Aphid field control effectiveness test result (Lanzhou 2005) on the 1.5% pyrethrin water emulsion control wild cabbage
Medicament Multiple Radix (head) before the medicine Behind the medicine 1 day Behind the medicine 7 days
Residual borer population (%) The rate that goes down (%) Preventive effect (%) Residual borer population The rate that goes down (%) Preventive effect (%)
1.5% pyrethrin water emulsion is killed chrysanthemum ester blank 750 1000 1250 1500 / 1879.75 1606.75 1579.00 1723.00 1726.50 137.25 151.00 189.00 119.25 1768.75 92.71 90.60 88.04 93.08 -2.45 92.88b 90.82c 88.33 93.25a 306.75 370.00 455.75 179.00 4146.25 83.68 76.97 71.14 89.62 -140.15 93.20b 90.41c 87.98d 95.68a
Annotate: data are the mean value of 4 repetitions in the table; Letter representation difference shows material property (0.05 level)
3 brief summaries
1.5% pyrethrin water emulsion has comparatively desirable control efficiency to cabbage aphid (Brevicoryne brassicae Linnaeus), and quick-acting is better, all more than 90%, the lasting period is more than 7 days in the preventive effect of 1d, 7d after the medication for its 750~1000 times of liquid.Reagent agent in test dose to crop safety.Therefore, suggestion is applied on producing.
Embodiment:
Embodiment 1
Get the raw materials ready by following proportioning:
1 part of pyrethrin
5 parts of piperonyl butoxides
10 parts of sodium alkyl sulfonates
84 parts in water
The following method of process:
A, under 20 ℃ of temperature, get 1 part of pyrethrin, add 3 parts of synergist piperonyl butoxide stirring and evenly mixings therein;
B, add 10 parts of sodium alkyl sulfonates in the thing as emulsifier above-mentioned all mixing, with the emulsification pretreatment machine with the speed emulsification of 800 rev/mins of kinds 30 minutes;
C, mix all above-mentioned that to add water to the pyrethrin effective component content in the thing be 1.5%, stirred 30 minutes, promptly make pyrethrin water emulsion with the mixing speed of 800 rev/mins of kinds.
Embodiment 2
Get the raw materials ready by following proportioning:
1 part of pyrethrin
3 parts of sesamins
90 parts of sodium alkylamidosulfonates
6 parts in water
The following method of process:
A, under 25 ℃ of temperature, get 1 part of pyrethrin, add 3 parts of synergist sesamin stirring and evenly mixings therein;
B, add 90 parts of sodium alkylamidosulfonates in the thing as emulsifier above-mentioned all mixing, with the emulsification pretreatment machine with the speed emulsification of 1000 rev/mins of kinds 10 minutes;
C, mix all above-mentioned that to add water to the pyrethrin effective component content in the thing be 15%, stirred 10 minutes, promptly make pyrethrin water emulsion with the mixing speed of 1000 rev/mins of kinds.
Embodiment 3
Get the raw materials ready by following proportioning:
1 part of pyrethrin
3 parts of peppermint oils
70 parts of sodium n-alkylbenzenesulfonates
26 parts in water
The following method of process:
A, under 23 ℃ of temperature, get 1 part of pyrethrin, add 3 parts of synergist peppermint oil stirring and evenly mixings therein;
B, add 70 parts of sodium n-alkylbenzenesulfonates in the thing as emulsifier above-mentioned all mixing, with the emulsification pretreatment machine with the speed emulsification of 900 rev/mins of kinds 20 minutes;
C, mix all above-mentioned that to add water to the pyrethrin effective component content in the thing be 8%, stirred 20 minutes, promptly make pyrethrin water emulsion with the mixing speed of 900 rev/mins of kinds.
Embodiment 4
Get the raw materials ready by following proportioning:
1 part of pyrethrin
2 parts of eucalyptus oils
Between 77 parts of nitro paratoluenesulfonic acid sodium salts
Method with embodiment 1 makes pyrethrin water emulsion.
Embodiment 5
Get the raw materials ready by following proportioning:
1 part of pyrethrin
1 part of Octacide 264
3 parts of synergy alcohol
Between 95 parts of nitro paratoluenesulfonic acid sodium salts
Method with embodiment 2 makes pyrethrin water emulsion.
Embodiment 6
Get the raw materials ready by following proportioning:
1 part of pyrethrin
3 parts in synergy phosphorus
50 parts of sodium alkylamidosulfonates
47 parts of calcium dodecyl benzene sulfonates
Method with embodiment 3 makes pyrethrin water emulsion.
Embodiment 7
Get the raw materials ready by following proportioning:
1 part of pyrethrin
3 parts of peppermint oils
1 part in synergy phosphorus
10 parts of calcium dodecyl benzene sulfonates
80 parts of lauryl sodium sulfate
3 parts of alkyl phosphate salts
Method with embodiment 3 makes pyrethrin water emulsion.

Claims (5)

1, a kind of pyrethrin water emulsion is characterized in that being made up of the raw material of following mass parts:
1 part of pyrethrin
Synergist 1-30 part
Benzene sulfonic acid is received 10-95 part
Water 0-95 part.
2, pyrethrin water emulsion according to claim 1 is characterized in that it is the natural pyrethrin product of 1-85% that described pyrethrin adopts its net content.
3, pyrethrin water emulsion according to claim 1 is characterized in that described synergist adopts one or more in piperonyl butoxide, sesamin, Octacide 264, synergy alcohol, synergy phosphorus, eucalyptus oil and the peppermint oil.
4, pyrethrin water emulsion according to claim 1 is characterized in that described benzene sulfonic acid sodium salt adopts one or more in sodium alkyl sulfonate, sodium alkyl benzene sulfonate, sodium n-alkylbenzenesulfonate, a nitro paratoluenesulfonic acid sodium salt, sodium alkylamidosulfonate, calcium dodecyl benzene sulfonate, lauryl sodium sulfate, alkyl phosphate salt and the sodium alkylamidosulfonate.
5, a kind of preparation method of pyrethrin water emulsion as claimed in claim 1 is characterized in that by following method:
A, under 20-25 ℃ of temperature, get 1 part of pyrethrin, add 1-30 part synergist stirring and evenly mixing therein;
B, add 10-95 part benzene sulfonic acid in the thing and receive, stirred 10-30 minute with the mixing speed of 800-1000 rev/min of kind as emulsifier above-mentioned all mixing;
C, add water 0-50 part above-mentioned all mixing in the thing, making the pyrethrin effective component content is 1.5-15%, stirs 10-30 minute with the mixing speed of 800-1000 rev/min of kind, promptly makes pyrethrin water emulsion.
CN2005100487371A 2005-12-22 2005-12-22 Natural pyrethrin water emulsion and its preparation Active CN1985598B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101341875B (en) * 2008-08-25 2011-06-08 严兵 Water-based natural pyrethrin sanitary insecticide and preparation method thereof
CN103190397A (en) * 2013-04-02 2013-07-10 红云红河烟草(集团)有限责任公司 Tobacco axillary bud inhibitor additive and application thereof
CN103329943A (en) * 2013-04-22 2013-10-02 河南省科高植物天然产物开发工程技术有限公司 Insecticide composition containing natural celastrus angulatus and natural pyrethrin
CN103651592A (en) * 2013-12-27 2014-03-26 成都新朝阳作物科学有限公司 Pesticide composition containing pyrethrum and lantana camara extracts, and preparation method and application thereof
CN114145315A (en) * 2021-12-29 2022-03-08 成都绿金生物科技有限责任公司 Pyrethrum extract emulsion in water and preparation method thereof
CN116868996A (en) * 2023-09-04 2023-10-13 成都绿金高新技术股份有限公司 Pyrethrin emulsion with high stability and preparation method thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4421471A1 (en) * 1994-06-20 1996-01-25 Temmen Gmbh Insecticidal agent based on natural pyrethrum
CN1206919C (en) * 2003-05-01 2005-06-22 红河森菊生物有限责任公司 Slow releasing agent of pyrethrin and its preparing method

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101341875B (en) * 2008-08-25 2011-06-08 严兵 Water-based natural pyrethrin sanitary insecticide and preparation method thereof
CN103190397A (en) * 2013-04-02 2013-07-10 红云红河烟草(集团)有限责任公司 Tobacco axillary bud inhibitor additive and application thereof
CN103329943A (en) * 2013-04-22 2013-10-02 河南省科高植物天然产物开发工程技术有限公司 Insecticide composition containing natural celastrus angulatus and natural pyrethrin
CN103651592A (en) * 2013-12-27 2014-03-26 成都新朝阳作物科学有限公司 Pesticide composition containing pyrethrum and lantana camara extracts, and preparation method and application thereof
CN103651592B (en) * 2013-12-27 2016-02-17 成都新朝阳作物科学有限公司 Containing composition pesticide and the preparation method and application of Dalmatian chrysanthemum and extract from Lantana camara
CN114145315A (en) * 2021-12-29 2022-03-08 成都绿金生物科技有限责任公司 Pyrethrum extract emulsion in water and preparation method thereof
CN116868996A (en) * 2023-09-04 2023-10-13 成都绿金高新技术股份有限公司 Pyrethrin emulsion with high stability and preparation method thereof
CN116868996B (en) * 2023-09-04 2024-01-02 成都绿金高新技术股份有限公司 Pyrethrin emulsion with high stability and preparation method thereof

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Application publication date: 20070627

Assignee: Yunnan Nanbao Biotechnology Co., Ltd.

Assignor: Yunnan Nanbao Phytochemical Engineering Co., Ltd.

Contract record no.: 2012530000045

Denomination of invention: Natural pyrethrin water emulsion and its preparation

Granted publication date: 20100428

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Record date: 20120815

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Address after: 653100 5 Tengxiao Road, Yuxi hi tech Development Zone, Yunnan

Patentee after: Yunnan Nanbao Biotechnology Co., Ltd.

Address before: 653201 Xiaojie Town, ALSHAN County, Yuxi, Yunnan

Patentee before: Yunnan Nanbao Phytochemical Engineering Co., Ltd.

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