CN104126601A - Preparation method for slow-release type imidacloprid granules - Google Patents

Preparation method for slow-release type imidacloprid granules Download PDF

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Publication number
CN104126601A
CN104126601A CN201410371228.1A CN201410371228A CN104126601A CN 104126601 A CN104126601 A CN 104126601A CN 201410371228 A CN201410371228 A CN 201410371228A CN 104126601 A CN104126601 A CN 104126601A
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imidacloprid
preparation
biomass
granule
spacetabs type
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CN201410371228.1A
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CN104126601B (en
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李建法
吕金红
李益民
徐海霞
刘森
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University of Shaoxing
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University of Shaoxing
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Abstract

A disclosed preparation method for slow-release type imidacloprid granules comprises: performing oxygen-limited pyrolysis on a biomass raw material at low-medium temperature, so as to obtain a biomass adsorption material, then grinding with imidacloprid crude drug, mixing uniformly, taking sodium alginate or carboxymethyl cellulose as a binder, and utilizing a fluidized bed spray granulation technology to prepare the imidacloprid granules. Because the biomass adsorption material obtained through pyrolysis of agricultural or forestry wastes is capable of adsorbing a part of imidacloprid active composition, the release rate of the active composition can be regulated by utilizing adsorption effect. Compared with the prior art, an adsorption carrier is low in cost and easy to obtain. Also, the biomass adsorption material is relatively light in specific gravity when being used as a pesticide carrier, is convenient for fluidized bed spray granulation, and is capable of integrally realizing granulating and drying of the imidacloprid granules. Compared with the prior art, the prepared is simple and convenient to process and good in safety. The granules have slow-release effect, are beneficial for improving the utilization rate of imidacloprid and mitigating pollution of pesticides to environment.

Description

The preparation method of spacetabs type Imidacloprid granule
Technical field
The present invention relates to pesticidal preparations field, relate in particular to a kind of preparation method of spacetabs type Imidacloprid granule.
Background technology
Imidacloprid is Nitromethylene insecticides, have tag, the multiple drug effect such as stomach toxicity and interior suction, be mainly used in preventing and treating sucking pest and resistant strain thereof.Imidacloprid is nicotinoids super-high-efficient insecticide, there is wide spectrum, efficient, low toxicity, low-residual, insect is difficult for producing resistance, to plurality of advantages such as people, animal, plant and natural enemies securities, can be used for the various crop such as paddy rice, wheat, corn, cotton, potato, vegetables, beet, fruit tree.Due to its good interior absorption, be specially adapted to seed treatment and spread the dispenser of granule mode.At present, Imidacloprid preparation common on market mainly contains missible oil, suspending agent, wetting powder, water dispersible granules etc., and the defending insect and killing effect of these formulations is better, but the lasting period is generally shorter, often need to repeatedly repeat dispenser.
This be because, active component in the Traditional Agricultural pharmaceutically dosage forms such as Imidacloprid missible oil discharges very fast, easily with the loss of surface runoff, or with the soil moisture leaching loss that moves both vertically, thereby cause agricultural chemicals availability lower, the lasting period is shorter, need to repeatedly repeats dispenser and just can reach insect killing and preventing effect, meanwhile, the active component of leaching loss or loss also can polluted surface or underground water.
Summary of the invention
Problem for above-mentioned existence, the invention provides a kind of preparation method of spacetabs type Imidacloprid granule, to overcome Imidacloprid active component of the prior art, discharge and comparatively fast cause that agricultural chemicals availability is lower and active component runs off or leaching loss causes the problem of earth's surface or groundwater contamination, thereby both improved drug effect, extended the lasting period, reduce again the migration of agricultural chemicals in environment, from source, control pesticide pollution, and then can reduce Imidacloprid spraying times, improve dispenser safety.
To achieve these goals, the technical scheme that the present invention takes is:
A preparation method for spacetabs type Imidacloprid granule, comprising:
Preparation biomass material and the former medicine of Imidacloprid;
Biomass material is limit oxygen pyrolysis under the temperature condition of 200 ℃~500 ℃, obtains biomass absorbent material;
The ratio that is 2~10:1 according to mass ratio by described biomass absorbent material and the former medicine of described Imidacloprid is evenly mixed, and mixed mixed material is ground to granularity is less than 0.15mm, obtains medicine carrying powder;
Described medicine carrying powder is added in fluidized bed spray granulation machine; adopt sodium alginate or carboxymethyl cellulose aqueous solution as binding agent liquid; regulate fluidizing gas velocity, fluidized-bed layer temperature and atomization air pressure; to after the atomization of described binding agent liquid, evenly be sprayed on fluidised medicine carrying powder; carry out fluidized drying simultaneously and process 0.3~1.5h, thereby make the Imidacloprid granule that particle diameter is 0.2~1.5mm.
The preparation method of above-mentioned spacetabs type Imidacloprid granule, wherein, described biomass material is discarded living beings in straw, wood chip, these agriculturals of leaf or production of forestry.
The preparation method of above-mentioned spacetabs type Imidacloprid granule, wherein, described biomass absorbent material is the carbide that has pore structure and hydrophobicity and Imidacloprid is had to higher adsorption capacity.
The preparation method of above-mentioned spacetabs type Imidacloprid granule, wherein, described binding agent liquid adopts sodium alginate or the carboxymethyl cellulose aqueous solution that mass concentration is 0.2%~2.0%.
The preparation method of above-mentioned spacetabs type Imidacloprid granule, wherein, described fluidizing gas velocity is controlled between 0.5~2.5m/s.
The preparation method of above-mentioned spacetabs type Imidacloprid granule, wherein, described fluidized-bed layer temperature is controlled between 50~80 ℃.
The preparation method of above-mentioned spacetabs type Imidacloprid granule, wherein, described atomization air pressure is controlled between 0.1~0.5MPa.
Technique scheme tool has the following advantages or beneficial effect:
The preparation method of spacetabs type Imidacloprid granule provided by the invention, by biomass material is obtained to biomass absorbent material in the pyrolysis of middle low temperature limits oxygen, then grind together with the former medicine of Imidacloprid, after evenly mixing, take sodium alginate or carboxymethyl cellulose as binding agent, utilize fluidized bed spray granulation technology to prepare Imidacloprid granule.The biomass absorbent material obtaining due to agricultural or forestry waste pyrolysis can adsorb a part of Imidacloprid active component, thereby can utilize the rate of release of suction-operated regulation activity composition, and compared with prior art, absorption carrier is with low cost, be easy to get; Meanwhile, biomass absorbent material is lighter as farm chemical carrier proportion, is convenient to fluidized bed spray granulation, can integratedly realize the granulation of Imidacloprid granule and be dried, and compared with prior art, preparation processing is easy, safety good; And this granule has slow releasing function, be conducive to improve Imidacloprid availability, alleviate the pollution of agricultural chemicals to environment.
Accompanying drawing explanation
By reading the detailed description of non-limiting example being done with reference to the following drawings, the present invention and feature thereof, profile and advantage will become more apparent.In whole accompanying drawings, identical mark is indicated identical part.Deliberately proportionally do not draw accompanying drawing, focus on illustrating purport of the present invention.
Fig. 1 is the preparation method's of the spacetabs type Imidacloprid granule that provides of the embodiment of the present invention 1 schematic flow sheet;
Fig. 2 is the releasing curve diagram of the Imidacloprid granule that makes of the preparation method who utilizes the embodiment of the present invention 1 to provide that the embodiment of the present invention 2 provides.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, the present invention is further illustrated, but not as limiting to the invention.
Embodiment 1:
Fig. 1 is the preparation method's of the spacetabs type Imidacloprid granule that provides of the embodiment of the present invention 1 schematic flow sheet; The preparation method of the spacetabs type Imidacloprid granule that as shown in the figure, the embodiment of the present invention 1 provides comprises:
First, preparation biomass material and the former medicine of Imidacloprid, this biomass material is discarded living beings in straw, wood chip, these agriculturals of leaf or production of forestry;
Then, biomass material is limit under the temperature condition of 200 ℃~500 ℃ to oxygen pyrolysis (that is: starvation carries out pyrolysis), obtain biomass absorbent material, this biomass absorbent material is the carbide that has pore structure and hydrophobicity and Imidacloprid is had to higher adsorption capacity;
The ratio that is 2~10:1 by biomass absorbent material and the former medicine of Imidacloprid according to mass ratio is more evenly mixed, as 2:1,3:1,4:1,5:1,6:1,7:1,8:1,9:1,10:1 etc., and mixed mixed material is ground to granularity is less than 0.15mm, obtain medicine carrying powder;
Finally medicine carrying powder is added in fluidized bed spray granulation machine; the sodium alginate that employing mass concentration is 0.2%~2.0% or carboxymethyl cellulose aqueous solution are as binding agent liquid; regulate fluidizing gas velocity between 0.5~2.5m/s, fluidized-bed layer temperature between 50~80 ℃ and atomization air pressure between 0.1~0.5MPa; to after the atomization of binding agent liquid, evenly be sprayed on fluidised medicine carrying powder; carry out fluidized drying simultaneously and process 0.3~1.5h, thereby make the Imidacloprid granule that particle diameter is 0.2~1.5mm.
Embodiment 2:
Take the dry leaf of 300g, put into several crucibles in batches, cover after crucible cover, put into Muffle furnace, be warming up to after 300 ℃, insulation 3h, cooling, after crucible is cooled to room temperature, is taken out residual carbide in crucible, wash and regulate pH=6.5, solids after suction filtration is dried, and pulverizes, and obtains biomass absorbent material 72g.
Above-mentioned biomass absorbent material is ground and mixed together with the former medicine of Imidacloprid (purity 95%) 15g, and porphyrize sieves (aperture is 0.15mm), obtains medicine carrying powder.Then; medicine carrying powder is added in fluidized bed spray granulation machine; adopting 0.5% (mass concentration) sodium alginate aqueous solution is binding agent; adjusting fluidizing gas velocity is that 1.5m/s, fluidized-bed layer temperature are 60, atomization air pressure is 0.3MPa; to after the atomization of binding agent liquid, evenly be sprayed on fluidised medicine carrying powder; fluidized drying is processed after 0.5h, and obtaining average grain diameter is the Imidacloprid granule 88g of 0.6mm.
The Imidacloprid active component content that sampling records in granule is 16%.
Fig. 2 is the releasing curve diagram of the Imidacloprid granule that makes of the preparation method who utilizes the embodiment of the present invention 1 to provide that the embodiment of the present invention 2 provides.Release experiment method is as follows: get Imidacloprid granule 40mg, put into the tool plug conical flask that fills 300mL distilled water, conical flask is put into 25 ℃ of water-bath constant temperature oscillations, and water sampling analysis Imidacloprid concentration wherein after the certain hour of interval, calculates and is discharged into the Imidacloprid mass M in water t, accordingly, calculate the Imidacloprid release rate (M under different time t/ M 0* 100%), draw the time dependent release profiles of release rate.
In order to verify the sustained release performance of gained Imidacloprid granule in above-described embodiment 2, get commercially available 20% imidacloprid wettable powder 32mg, put into the tool plug conical flask that fills 300mL distilled water.Do as mentioned above release experiment in water, draw release profiles.
According to Fig. 2, can find out, compare with pulvis, after same time, the release rate of granule obviously declines, and has embodied gained granule of the present invention slower to the release of Imidacloprid active component, has obvious sustained release performance.
In sum, the preparation method of the spacetabs type Imidacloprid granule that the embodiment of the present invention provides, by biomass material is obtained to biomass absorbent material in the pyrolysis of middle low temperature limits oxygen, then grind together with the former medicine of Imidacloprid, after evenly mixing, take sodium alginate or carboxymethyl cellulose as binding agent, utilize fluidized bed spray granulation technology to prepare Imidacloprid granule.The biomass absorbent material obtaining due to agricultural or forestry waste pyrolysis can adsorb a part of Imidacloprid active component, thereby can utilize the rate of release of suction-operated regulation activity composition, and compared with prior art, absorption carrier is with low cost, be easy to get; Meanwhile, biomass absorbent material is lighter as farm chemical carrier proportion, is convenient to fluidized bed spray granulation, can integratedly realize the granulation of Imidacloprid granule and be dried, and compared with prior art, preparation processing is easy, safety good; And this granule has slow releasing function, be conducive to improve Imidacloprid availability, alleviate the pollution of agricultural chemicals to environment.
It should be appreciated by those skilled in the art that those skilled in the art can realize described variation example in conjunction with prior art and above-described embodiment, do not repeat them here.Such variation example does not affect flesh and blood of the present invention, does not repeat them here.
Above preferred embodiment of the present invention is described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and the equipment of wherein not describing in detail to the greatest extent and structure are construed as with the common mode in this area to be implemented; Any those of ordinary skill in the art, make many possible changes and modification not departing from technical solution of the present invention, or are revised as the equivalent embodiment of equivalent variations, and this does not affect flesh and blood of the present invention.Therefore, every content that does not depart from technical solution of the present invention,, all still belongs in the scope of technical solution of the present invention protection any simple modification made for any of the above embodiments, equivalent variations and modification according to technical spirit of the present invention.

Claims (7)

1. a preparation method for spacetabs type Imidacloprid granule, is characterized in that, comprising:
Preparation biomass material and the former medicine of Imidacloprid;
Biomass material is limit to oxygen pyrolysis under the temperature condition of 200 ℃~500 ℃, obtain biomass absorbent material;
The ratio that is 2~10:1 according to mass ratio by described biomass absorbent material and the former medicine of Imidacloprid is evenly mixed, and mixed mixed material is ground to granularity is less than 0.15mm, obtains medicine carrying powder;
Described medicine carrying powder is added in fluidized bed spray granulation machine; adopt sodium alginate or carboxymethyl cellulose aqueous solution as binding agent liquid; regulate fluidizing gas velocity, fluidized-bed layer temperature and atomization air pressure; to after the atomization of described binding agent liquid, evenly be sprayed on fluidised medicine carrying powder; carry out fluidized drying simultaneously and process 0.3~1.5h, thereby make the Imidacloprid granule that particle diameter is 0.2~1.5mm.
2. the preparation method of spacetabs type Imidacloprid granule as claimed in claim 1, is characterized in that, described biomass material is discarded living beings in straw, wood chip, these agriculturals of leaf or production of forestry.
3. the preparation method of spacetabs type Imidacloprid granule as claimed in claim 1, is characterized in that, described biomass absorbent material is the carbide that has pore structure and hydrophobicity and Imidacloprid is had to higher adsorption capacity.
4. the preparation method of spacetabs type Imidacloprid granule as claimed in claim 1, is characterized in that, described binding agent liquid adopts sodium alginate or the carboxymethyl cellulose aqueous solution that mass concentration is 0.2%~2.0%.
5. the preparation method of spacetabs type Imidacloprid granule as claimed in claim 1, is characterized in that, described fluidizing gas velocity is controlled between 0.5~2.5m/s.
6. the preparation method of spacetabs type Imidacloprid granule as claimed in claim 1, is characterized in that, described fluidized-bed layer temperature is controlled between 50~80 ℃.
7. the preparation method of spacetabs type Imidacloprid granule as claimed in claim 1, is characterized in that, described atomization air pressure is controlled between 0.1~0.5MPa.
CN201410371228.1A 2014-07-31 2014-07-31 The preparation method of spacetabs type imidacloprid granule Expired - Fee Related CN104126601B (en)

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Cited By (6)

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CN104430323A (en) * 2014-11-26 2015-03-25 北京农学院 Controlled-release pesticide granules
CN105854798A (en) * 2016-04-14 2016-08-17 中国农业科学院植物保护研究所 Preparing method for biochar and method for loading imidacloprid on biochar
CN106508898A (en) * 2015-09-11 2017-03-22 沈阳化工研究院有限公司 Biomass-based slow-release pesticide and preparation method thereof
CN106831207A (en) * 2017-04-11 2017-06-13 叶集区华农种植专业合作社 A kind of pear tree can prevent and treat slow release fertilizer of anthracnose and preparation method thereof
CN107324954A (en) * 2017-07-29 2017-11-07 山西省农业科学院植物保护研究所 A kind of sheet bacterial manure granule that subterranean pest-insect is prevented and treated by carrier of chicken manure and preparation method thereof
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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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104430323A (en) * 2014-11-26 2015-03-25 北京农学院 Controlled-release pesticide granules
CN106508898A (en) * 2015-09-11 2017-03-22 沈阳化工研究院有限公司 Biomass-based slow-release pesticide and preparation method thereof
CN106508898B (en) * 2015-09-11 2020-04-24 沈阳化工研究院有限公司 Biomass-based slow-release pesticide and preparation method thereof
CN105854798A (en) * 2016-04-14 2016-08-17 中国农业科学院植物保护研究所 Preparing method for biochar and method for loading imidacloprid on biochar
CN106831207A (en) * 2017-04-11 2017-06-13 叶集区华农种植专业合作社 A kind of pear tree can prevent and treat slow release fertilizer of anthracnose and preparation method thereof
CN107324954A (en) * 2017-07-29 2017-11-07 山西省农业科学院植物保护研究所 A kind of sheet bacterial manure granule that subterranean pest-insect is prevented and treated by carrier of chicken manure and preparation method thereof
CN107324954B (en) * 2017-07-29 2023-10-03 山西农业大学 Flaky bacterial fertilizer granule taking chicken manure as carrier for controlling soil insects and preparation method thereof
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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