CN101554179A - Mosquito killing Bacillus sphaericus leafing agent and preparation method thereof - Google Patents
Mosquito killing Bacillus sphaericus leafing agent and preparation method thereof Download PDFInfo
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- CN101554179A CN101554179A CNA2008101035411A CN200810103541A CN101554179A CN 101554179 A CN101554179 A CN 101554179A CN A2008101035411 A CNA2008101035411 A CN A2008101035411A CN 200810103541 A CN200810103541 A CN 200810103541A CN 101554179 A CN101554179 A CN 101554179A
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Abstract
The invention provides a mosquito killing Bacillus sphaericus leafing agent which is prepared by the following steps: firstly, concentrating mosquito killing Bacillus sphaericus ferment filtrate by a film concentration method; then, adsorbing the mosquito killing Bacillus sphaericus ferment filtrate by a porous carrier substance, mixing the mosquito killing Bacillus sphaericus ferment filtrate and sustained release agent and drying the mosquito killing Bacillus sphaericus ferment filtrate into a master batch at 40 DEG C-50DEG C; and finally, coating hydrophobing agent. The mosquito killing Bacillus sphaericus leafing agent is prepared by a low temperature production process, the loss rate (namely valence loss rate) of active components is only about 10 percent, and the solid recovery rate reaches about 95 percent. The technology ensures low valence loss rate, low energy consumption and low transportation cost in the production process. By measurement, the leafing agent has the effect on continuously killing Culex fatigans for more than 28 days (indoor measurement) by putting the 4mg/L leafing agent into water at one time.
Description
Technical field
The present invention relates to a kind of preparation method of biologic product, specifically, relate to a kind of mosquito Bacillus sphaericus (Bacillus sphaericus is called for short Bs) leafing agent and preparation method thereof that kills.The production technology and the preparation technology that belong to microorganism insecticide in the biopesticide.
Background technology
Killing mosquito Bacillus sphaericus (Bacillus sphaericus is called for short Bs) is the beneficial microbe that extensively is present in the natural environment, and a kind of protein companion spore body that its bacterial metabolism produces has the very high activity of killing to the larva wriggler of mosquito.Mosquito Bacillus sphaericus and bacillus thuringiensis are defined as mosquito is carried out two kinds of beneficial bacterias of biological control by The World Health Organization (WHO) with look Leah kind (being B.t.i) extremely, there are several B.s bacterial strains to be used to suitability for industrialized production and mosquito control both at home and abroad, as Bs2362 bacterial strain and the C3-41 bacterial strain of the World Health Organization to whole world recommendation.The experimental results shows, kill that the mosquito Bacillus sphaericus produced to kill the mosquito active substance very responsive to heat, being in for a long time more than 45 ℃ will inactivation, because its thermal sensitivity is too strong, so the former powder (or female powder) that suitability for industrialized production is killed mosquito Bacillus sphaericus difficulty relatively.
Relevant production process of killing the former powder of mosquito Bacillus sphaericus does not see that disclosed report is arranged abroad.Domestic relevant expert carried out the screening of mosquito Bacillus sphaericus thermal protecting agent extremely, but did not see have disclosed document to deliver and patent application always for overcoming this difficulty.
The method that the mosquito Bacillus sphaericus is killed in domestic production at present has two kinds, and a kind of is not produce pulvis, only produces aqua, avoids the heat inactivation problem thus; Another kind is to take conventional spray drying process, and it is centrifugal that disk plate centrifuge was met in fermentation afterwards, collects the bacterium slurry and produces the former powder of mosquito Bacillus sphaericus extremely with spray drying tower then.
Though it is simple to produce the method for aqua, yield is also very high, and product is tired low, and volume is big, and transportation is inconvenient, and product is easily corrupt, and the shelf-life is shorter.Killing mosquito Bacillus sphaericus product has certain international market, but seems very improper with the aqua outlet.
The way of producing former powder with spray drying process is a mature and feasible to the production of bacillus thuringiensis product, but improper to killing the mosquito Bacillus sphaericus, because spray drying process is the deactivation temperature that inlet temperature or outlet temperature all substantially exceed this product.Not only energy consumption is big so adopt spray drying process production to kill the mosquito Bacillus sphaericus, the cost height, and also the loss of tiring is also very big, and its percent of loss reaches more than 50%.
Produce the approach that kills mosquito Bacillus sphaericus solid product (dry products in other words) in order to explore one, and the percent of loss of tiring in the assurance production process is low, energy consumption is little, cost of transportation is low, the inventor has carried out research repeatedly to killing mosquito Bacillus sphaericus fermentation post processing production technology, has finally finished the application.
Summary of the invention
The purpose of this invention is to provide a kind of mosquito Bacillus sphaericus (Bacillussphaericus) leafing agent that kills, adopt the low temperature aftertreatment technology, keep killing mosquito Bacillus sphaericus high activity, and reach lasting control efficiency.
Another object of the present invention provides a kind of preparation method of mosquito killing Bacillus sphaericus leafing agent, and this method adopts the low temperature aftertreatment technology, has avoided the bacterial classification defective of inactivation at high temperature, and the percent of loss of tiring in the assurance production process is low, energy consumption is little, and cost of transportation is low, but suitability for industrialized production.
In order to realize the object of the invention, a kind of mosquito Bacillus sphaericus (Bacillussphaericus) leafing agent that kills of the present invention, it is prepared from by following steps: adopt membrane concentration method to concentrate kill mosquito Bacillus sphaericus ferment filtrate earlier, adsorb with the porous carrier material then, mix with sustained release agent again, and be dried to master batch at 40～50 ℃, wrap up water-repelling agent at last.
For with the moisture in thalline and the zymotic fluid from, the present invention adopts miillpore filter to filter and anhydrates.The filter membrane that is adopted in the membrane concentration method of the present invention is acetyl cellulose film (CA), inorganic ceramic membrane or PVDF membrane (PVDF), best through relatively confirming inorganic ceramic membrane, according to the molecular weight size of the activated protein that kills the mosquito Bacillus sphaericus, the aperture of determining film is 50～100nm.
For realizing low temperature drying, the present invention is not according to producing former powder earlier, the back produces the process route of preparation, but directly produce the leafing agent master batch, porous carrier by leafing agent absorbs moisture content, adsorb thalline and kill the mosquito active substance, and increase the permeability of material, enlarge the porosity and the disengagement area that help water evaporates with this.
Described porous carrier material is perlite, corn cob granule, expanded white carbon, most preferably is corn cob granule.
It is good that the corn cob granule material has floatability, and adsorbing capacity is big, and material environment friendly is pollution-free, advantages such as low price.Tested the effect of the corn cob granule of different-grain diameter size, preferred result shows that the corn cob granule of 1～2mm particle diameter is best.Consumption to 1～2mm corn cob granule is tested, and when bacterium slurry solid content reached 20～25%, corncob consumption (W/W) 4.5～50% can reach the purpose of low temperature drying, and optimum is 7.5～8.5%.
The present invention selects the baking temperature of master batch, from 40～50 ℃, whenever differs from 1 ℃ a processing is set, and comparative result shows that 42 ℃ to 46 ℃ are feasible selection repeatedly, but is optimum with 45 ℃.The drying machinery of wet master batch is best with ebullated bed, and the temperature-controlled drying case of blowing-type also can be selected for use.
For the flotation time and the sustained release performance that guarantee leafing agent, the inventor superscribes sustained release agent to floating master batch.
Described sustained release agent is selected fenugreek gum, gum Arabic, cycloheptaamylose etc. for use, is preferably fenugreek gum.
The present invention has tested different fenugreek gum content, and preferred result fenugreek gum and bacterium slurry mass ratio are 0.005～0.009: 1, and optimum is 0.007: 1.Be coated with into master batch behind the ratio melt into fenugreek gum aqueous solution of fenugreek gum with 40g fenugreek gum/1L water.
Corn cob granule adsorbs thalline and kills after the mosquito active substance, can shorten greatly in the water float time, and the active substance of absorption can discharge very soon, and efficiency time only several days does not reach common requirement to the kill mosquito leafing agent.For this reason, the present invention wraps up the leafing agent master batch with the various hydrophobic agent.These water-repelling agents comprise palm oil, paraffin, and lacs etc. have also been tested individual layer parcel and multilayer parcel simultaneously.Through more selected double wrapped scheme is best, material is one deck paraffin, one deck lac, parcel paraffin layer earlier, wrap up again the lac layer and earlier parcel lac layer to wrap up two kinds of parcels orders of paraffin layer more all feasible.Lac should be used dissolve with ethanol with lac earlier during parcel, and the ratio of lac and solvent is 50ml ethanol/g lac.The parcel condition of paraffin is to add acetone under 50 ℃ the temperature, and the consumption of acetone is 3ml acetone/g paraffin.
In order to realize another object of the present invention, a kind of preparation method who kills mosquito Bacillus sphaericus (Bacillus sphaericus) leafing agent of the present invention, it comprises the steps: to adopt membrane concentration method to concentrate kill mosquito Bacillus sphaericus ferment filtrate earlier, adsorb with the porous carrier material then, mix with sustained release agent again, and be dried to master batch at 40～50 ℃, wrap up water-repelling agent at last and form.
Wherein, the filter membrane that is adopted in the described membrane concentration method is acetyl cellulose film (CA), inorganic ceramic membrane and PVDF membrane (PVDF), is preferably inorganic ceramic membrane, and the aperture of film is 50～100nm.
Described porous carrier material is perlite, corn cob granule, expanded white carbon, most preferably is corn cob granule, and particle diameter is 1～2mm.
When bacterium slurry solid content reached 20～25%, corncob consumption (W/W) 4.5～50% can reach the purpose of low temperature drying, and optimum is 7.5～8.5%.
Baking temperature of the present invention is preferably 45 ℃.The drying machinery of wet master batch is best with ebullated bed, and the temperature-controlled drying case of blowing-type also can be selected for use.
Described sustained release agent is selected fenugreek gum, gum Arabic, cycloheptaamylose etc. for use, is preferably fenugreek gum.
The present invention has tested different fenugreek gum content, and preferred result fenugreek gum and bacterium slurry mass ratio are 0.005～0.009: 1, and optimum is 0.007: 1.Be coated with into master batch behind the ratio melt into fenugreek gum aqueous solution of fenugreek gum with 40g fenugreek gum/1L water.
Described water-repelling agent comprises palm oil, paraffin, and lacs etc. can be adopted individual layer parcel and multilayer parcel.Through more selected double wrapped scheme is best, material is one deck paraffin, one deck lac, parcel paraffin layer earlier, wrap up again the lac layer and earlier parcel lac layer to wrap up two kinds of parcels orders of paraffin layer more all feasible.Lac should be used dissolve with ethanol with lac earlier during parcel, and the ratio of lac and solvent is 50ml ethanol/g lac.The parcel condition of paraffin is to add acetone under 50 ℃ the temperature, and the consumption of acetone is 3ml acetone/g paraffin.
The mosquito Bacillus sphaericus master batch low-temperature production process that kills of the present invention can be produced mosquito killing Bacillus sphaericus leafing agent, the percent of loss of active ingredient (percent of loss of promptly tiring) only about 10%, and solid recovery rate reaches about 95%.And the percent of loss of tiring in this technology assurance production process is low, and energy consumption is little, and cost of transportation is low.After measured, leafing agent dosing time 4mg/L of the present invention continues to kill culex pipiens fatigans (Culex fatigans) effect and is (indoor measurement) more than 28 days in water.
Description of drawings
Fig. 1 is mosquito Bacillus sphaericus master batch low-temperature production process and the leafing agent production process route schematic diagram of killing of the present invention.
Embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
Add hydrochloric acid after the kill mosquito Bacillus sphaericus ferments successfully and transfer pH5.0, through link-suspended basket centrifuge remove slag (the screen cloth mesh is 60 orders, and centrifuge speed is 1000rpm).Getting the 75kg ferment filtrate, is 45w at power, and membrane area is 0.3m
2, membrane aperture is to concentrate 35 ℃ of running temperatures in the inorganic ceramic membrane module of 100nm, 6 hours 25 minutes running time, discharge clear liquid 66.3kg through concentrating, emit the bacterium slurry, and the bacterium slurry in remaining in film and the pipeline with a little flushing with clean water, collect bacterium slurry 8.6kg, transfer pH value 4.8 with watery hydrochloric acid simultaneously.It is the dry corn cob granule 0.67kg of 1-2mm that this bacterium slurry is added particle diameter by weight 7.8%, in trough-type mixture machine with the two abundant mixing, again the 60.2g fenugreek gum is dissolved in the 1.4L clear water and becomes the fenugreek gum aqueous solution, the fenugreek gum aqueous solution is poured in the trough-type mixture machine, with the abundant mixing of carrier that adheres to the bacterium slurry, material is the bean dregs shape.Place 45 ℃ of air dry oven inner dryings, the master batch 2.71kg that obtained parching through 12 hours.
Gained fundatrix grain is detected, its water content 3.16%, the 4582ITU/mg that tires, active component yield (rate of recovery of tiring) is 91.02%, solid recovery rate 96.07%.
Embodiment 2
Add hydrochloric acid after the kill mosquito Bacillus sphaericus ferments successfully and transfer pH5.0, through link-suspended basket centrifuge remove slag (the screen cloth mesh is 40 orders, and centrifuge speed is 1000rpm).Getting the 75kg ferment filtrate, is 45w at power, and membrane area is 0.3m
2, membrane aperture is to concentrate 36 ℃ of running temperatures in the inorganic ceramic membrane module of 100nm, 6 hours 20 minutes running time, discharge stillness of night 66.6kg through concentrating, emit the bacterium slurry, and the bacterium slurry in remaining in film and the pipeline with a little flushing with clean water, collect bacterium slurry 8.5kg, transfer pH value 4.8 with watery hydrochloric acid simultaneously.This bacterium slurry is added perlite particle 2.0124kg by weight 23.4%, in trough-type mixture machine with the two abundant mixing, again the 68.8g fenugreek gum is dissolved in the 1.4L clear water and becomes the fenugreek gum aqueous solution, the fenugreek gum aqueous solution is poured in the trough-type mixture machine, with the abundant mixing of carrier that adheres to the bacterium slurry, material is the bean dregs shape.Place 45 ℃ of air dry oven inner dryings, the master batch 3.846kg that obtained parching through 13.5 hours.
Gained fundatrix grain is detected, its water content 3.23%, the 3760ITU/mg that tires, active component yield (rate of recovery of tiring) is 89.86%, solid recovery rate 96.39%.
Embodiment 3
Add hydrochloric acid after the kill mosquito Bacillus sphaericus ferments successfully and transfer pH5.0, through link-suspended basket centrifuge remove slag (the screen cloth mesh is 60 orders, and centrifuge speed is 1000rpm).Getting the 75kg ferment filtrate, is 45w at power, and membrane area is 0.3m
2, membrane aperture is to concentrate 37 ℃ of running temperatures in the inorganic ceramic membrane module of 100nm, 6 hours 18 minutes running time, discharge stillness of night 66.5kg through concentrating, emit the bacterium slurry, and the bacterium slurry in remaining in film and the pipeline with a little flushing with clean water, collect bacterium slurry 8.6kg, transfer pH value 4.8 with watery hydrochloric acid simultaneously.It is the dry corn cob granule 0.7432kg of 1-2mm that this bacterium slurry is added particle diameter by weight 9.0%, in trough-type mixture machine with the two abundant mixing, again the 68.8g fenugreek gum is dissolved in the 1.4L clear water and becomes the fenugreek gum aqueous solution, the fenugreek gum aqueous solution is poured in the trough-type mixture machine, with the abundant mixing of carrier that adheres to the bacterium slurry, material is the bean dregs shape.Place 45 ℃ of air dry oven inner dryings, the master batch 2.83kg that obtained parching through 12 hours.
Gained fundatrix grain is detected, its water content 3.07%, the 4496ITU/mg that tires, active component yield (rate of recovery of tiring) is 90.86%, solid recovery rate 95.98%.
Embodiment 4
According to this process route, adopt two hydrophobic layer structures.Fundatrix grain: lac: paraffin=3.5: 0.02: 0.2 (mass ratio).One: the fundatrix grain 350g that gets embodiment 1 pours in the trough-type mixture machine.Two: the 2g lac is dissolved in the 100ml ethanolic solution earlier, the ethanolic solution of lac is poured into fully be mixed into a in the trough-type mixture machine again.Three: under 50 ℃,, pour in the trough-type mixture machine and fully be mixed into b with a with adding 60ml acetone in the 20g paraffin.Four: b is moved in the temperature control air dry oven under 45 ℃ of conditions dry 0.5 hour become leafing agent product c.
Gained c is carried out Performance Detection, its water content 3.65%.4286ITU/mg tires.
Embodiment 5
According to this process route, adopt two hydrophobic layer structures.Fundatrix grain: paraffin: lac=3.5: 0.2: 0.02 (mass ratio).One: the fundatrix grain 350g that gets embodiment 1 pours in the trough-type mixture machine.Two: under 50 ℃,, pour trough-type mixture machine into and fully be mixed into a1 with adding 60ml acetone in the 20g paraffin.Three: the 2g lac is dissolved in the 100ml ethanolic solution earlier, again the ethanolic solution of lac is poured in the trough-type mixture machine, fully be mixed into b1, four: b1 is moved in the temperature control air dry oven under 45 ℃ of conditions dry 0.5 hour become leafing agent product c1 with a1.
Gained c1 is carried out Performance Detection, its water content 3.61%.4259ITU/mg tires.
Experimental example 1
According to the technology of embodiment 4, change proportioning into the fundatrix grain: paraffin: lac=3.5: 0.1: 0.01 (mass ratio) is prepared into leafing agent C2; Fundatrix grain: paraffin=3.5: 0.3 (mass ratio) preparation leafing agent C3.With C, C2, C3 kill the mosquito determination of activity, and select for use and tire to the aqueous suspension of 200ITU/mg is contrast 1, and the pulvis of tiring to 700ITU/mg is contrast 2, and clear water is contrast 3.With the 4L Plastic Drum is container, and every barreled is gone into the 3L running water that spends the night.Flotation time is that its floatability is the fate more than 50%, and preventive effect is for adding the lethality of mosquito larvae after 48 hours.
The result adds up as table 1:
Table 1 BS leafing agent of the present invention and BS aqueous suspension (contrast 2) lasting effect relatively
| Product to be measured | Flotation time (my god) | Preventive effect (%) |
| c | 28-30 | Preventive effect was 69.7-100 in preceding 21 days, and the preventive effect after 28 days is 53.3 |
| c2 | 18-20 | Preventive effect was 73.0-100 in preceding 14 days, and the preventive effect after 21 days is 51.7 |
| c3 | 16-18 | Preventive effect was 72.7-100 in preceding 14 days, and the preventive effect after 21 days is 46.3 |
| Contrast 1 | —— | Preventive effect was 76.0-100 in preceding 7 days, and the preventive effect after 14 days is 20.3 |
| Contrast 2 | —— | Preventive effect was 73.7-100 in preceding 7 days, and the preventive effect after 14 days is 31.0 |
| Contrast 3 | —— | 0 |
By last table as can be seen, the longest in the flotation time by the leafing agent c of this technology preparation, control efficiency and other products and contrast are similar, but the lasting period obviously is longer than other products and contrast.
Experimental example 2
Get membrane process respectively, powder injection process, flocculation centrifuging process products obtained therefrom are tired yield and cost relatively.
Powder injection process processing method: the 25kg zymotic fluid through the processing of directly dusting, is obtained 0.52kg dry powder.
Membrane process processing method: the same batch fermentation liquid of 25kg is concentrated drying through technology of the present invention.Obtain the female powder of leafing agent that 0.81kg does.
This experiment adopts the method for biologicall test to come testing result, the product of considering film concentrate drying technology is that dry bacterial powder is attached on the carrier, directly measuring can be because slowly-releasing and interference measurement result, and therefore, the product of this test after with the membrane process processing carries out wet-milling and become powder to measure later on.The active ingredient loss that produces heat in the process that the purpose of wet-milling is to avoid grinding and cause.
The centrifugal concentration method of flocculating: add 3 ‰ flocculant aluminium chloride in the zymotic fluid with same batch of 1kg and above-mentioned zymotic fluid, handled 5 minutes with 3000r/min.Collect supernatant and precipitation respectively.Collect supernatant 880g, precipitation 120g, 8.33 times of cycles of concentration.
Above-mentioned three kinds of methods are concentrated the test products of producing measure its concentration multiple respectively, the gross activity recovery rate, comparative result is listed in the table 2.
Three kinds of method for concentration pluses and minuses of table 2BS zymotic fluid relatively
By last table as can be seen, technology of the present invention obviously is better than traditional processing technology on activity yield and operating cost.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. one kind is killed mosquito Bacillus sphaericus (Bacillus sphaericus) leafing agent, it is characterized in that, it is prepared from by following steps: adopt membrane concentration method to concentrate kill mosquito Bacillus sphaericus ferment filtrate earlier, adsorb with the porous carrier material then, mix with sustained release agent again, and be dried to master batch at 40～50 ℃, wrap up water-repelling agent at last.
2. mosquito killing Bacillus sphaericus leafing agent according to claim 1 is characterized in that the filter membrane that is adopted in the described membrane concentration method is acetyl cellulose film, inorganic ceramic membrane or PVDF membrane.
3. mosquito killing Bacillus sphaericus leafing agent according to claim 1 and 2 is characterized in that, described filter membrane is an inorganic ceramic membrane.
4. according to any described mosquito killing Bacillus sphaericus leafing agent of claim 1-3, it is characterized in that described porous carrier material is perlite, corn cob granule, expanded white carbon.
5. according to any described mosquito killing Bacillus sphaericus leafing agent of claim 1-4, it is characterized in that described corn cob granule consumption (W/W) 4.5～50%.
6. according to any described mosquito killing Bacillus sphaericus leafing agent of claim 1-5, it is characterized in that described sustained release agent is selected fenugreek gum, gum Arabic or cycloheptaamylose for use.
7. according to the described mosquito killing Bacillus sphaericus leafing agent of claim 6, it is characterized in that described fenugreek gum and bacterium slurry mass ratio are 0.009～0.005: 1.
8, according to any described mosquito killing Bacillus sphaericus leafing agent of claim 1-7, it is characterized in that described water-repelling agent is selected one or more in palm oil, paraffin or the lac for use.
9, according to any described mosquito killing Bacillus sphaericus leafing agent of claim 1-8, it is characterized in that, adopt individual layer parcel or multilayer parcel when described water-repelling agent wraps up.
10. the method for preparing any described mosquito killing Bacillus sphaericus leafing agent of claim 1-9, it is characterized in that, it comprises the steps: to adopt membrane concentration method to concentrate kill mosquito Bacillus sphaericus ferment filtrate earlier, adsorb with the porous carrier material then, mix with sustained release agent again, and be dried to master batch at 40～50 ℃, wrap up water-repelling agent at last and form.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102669185A (en) * | 2012-03-27 | 2012-09-19 | 泰山医学院 | Water release method of culex larva bio-control bacteria |
| CN103141530A (en) * | 2013-02-06 | 2013-06-12 | 深圳馥稷生物科技有限公司 | Plant essential oil-containing mosquito repellent |
| CN104430542A (en) * | 2014-11-10 | 2015-03-25 | 中国科学院武汉病毒研究所 | Method for preparing bacillus sphaericus wettable powder |
| CN107282014A (en) * | 2017-07-17 | 2017-10-24 | 黄建社 | The Bacillus thuringiensis subsp. israelensis floatation pad of toxic chemical substance in water can be adsorbed |
| CN108925586A (en) * | 2018-08-24 | 2018-12-04 | 成都特普生物科技股份有限公司 | A kind of antimicrobial composition preparation improving plant pest management effect |
| CN113040137A (en) * | 2019-12-26 | 2021-06-29 | 武汉科诺生物科技股份有限公司 | Application of biomass puffed particles as mosquito killing drug carrier |
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2008
- 2008-04-08 CN CNA2008101035411A patent/CN101554179A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102669185A (en) * | 2012-03-27 | 2012-09-19 | 泰山医学院 | Water release method of culex larva bio-control bacteria |
| CN103141530A (en) * | 2013-02-06 | 2013-06-12 | 深圳馥稷生物科技有限公司 | Plant essential oil-containing mosquito repellent |
| CN103141530B (en) * | 2013-02-06 | 2014-10-22 | 深圳馥稷生物科技有限公司 | Plant essential oil-containing mosquito repellent |
| CN104430542A (en) * | 2014-11-10 | 2015-03-25 | 中国科学院武汉病毒研究所 | Method for preparing bacillus sphaericus wettable powder |
| CN107282014A (en) * | 2017-07-17 | 2017-10-24 | 黄建社 | The Bacillus thuringiensis subsp. israelensis floatation pad of toxic chemical substance in water can be adsorbed |
| CN108925586A (en) * | 2018-08-24 | 2018-12-04 | 成都特普生物科技股份有限公司 | A kind of antimicrobial composition preparation improving plant pest management effect |
| CN113040137A (en) * | 2019-12-26 | 2021-06-29 | 武汉科诺生物科技股份有限公司 | Application of biomass puffed particles as mosquito killing drug carrier |
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| AD01 | Patent right deemed abandoned |
Effective date of abandoning: 20091014 |
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| C20 | Patent right or utility model deemed to be abandoned or is abandoned |