CN117617241A - Coated double-carrier pesticide controlled release granule and preparation method and application thereof - Google Patents
Coated double-carrier pesticide controlled release granule and preparation method and application thereof Download PDFInfo
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- CN117617241A CN117617241A CN202311379917.2A CN202311379917A CN117617241A CN 117617241 A CN117617241 A CN 117617241A CN 202311379917 A CN202311379917 A CN 202311379917A CN 117617241 A CN117617241 A CN 117617241A
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- 239000000575 pesticide Substances 0.000 title claims abstract description 129
- 239000008187 granular material Substances 0.000 title claims abstract description 98
- 238000013270 controlled release Methods 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000012792 core layer Substances 0.000 claims abstract description 24
- 239000010410 layer Substances 0.000 claims abstract description 24
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims abstract description 17
- 229920001661 Chitosan Polymers 0.000 claims abstract description 17
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 17
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims abstract description 17
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims abstract description 17
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 50
- 239000000243 solution Substances 0.000 claims description 45
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 38
- 238000002156 mixing Methods 0.000 claims description 26
- 239000005886 Chlorantraniliprole Substances 0.000 claims description 22
- 239000004480 active ingredient Substances 0.000 claims description 20
- PSOVNZZNOMJUBI-UHFFFAOYSA-N chlorantraniliprole Chemical compound CNC(=O)C1=CC(Cl)=CC(C)=C1NC(=O)C1=CC(Br)=NN1C1=NC=CC=C1Cl PSOVNZZNOMJUBI-UHFFFAOYSA-N 0.000 claims description 20
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- 239000000843 powder Substances 0.000 claims description 20
- 238000005507 spraying Methods 0.000 claims description 18
- PGOOBECODWQEAB-UHFFFAOYSA-N (E)-clothianidin Chemical compound [O-][N+](=O)\N=C(/NC)NCC1=CN=C(Cl)S1 PGOOBECODWQEAB-UHFFFAOYSA-N 0.000 claims description 15
- 239000005888 Clothianidin Substances 0.000 claims description 15
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 13
- 229960002089 ferrous chloride Drugs 0.000 claims description 13
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 239000008188 pellet Substances 0.000 claims description 12
- 239000002917 insecticide Substances 0.000 claims description 11
- 241000196324 Embryophyta Species 0.000 claims description 10
- 241000607479 Yersinia pestis Species 0.000 claims description 10
- 235000003434 Sesamum indicum Nutrition 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000003895 organic fertilizer Substances 0.000 claims description 6
- 238000009396 hybridization Methods 0.000 claims description 5
- PXBFMLJZNCDSMP-UHFFFAOYSA-N 2-Aminobenzamide Chemical compound NC(=O)C1=CC=CC=C1N PXBFMLJZNCDSMP-UHFFFAOYSA-N 0.000 claims description 4
- WCXDHFDTOYPNIE-RIYZIHGNSA-N (E)-acetamiprid Chemical compound N#C/N=C(\C)N(C)CC1=CC=C(Cl)N=C1 WCXDHFDTOYPNIE-RIYZIHGNSA-N 0.000 claims description 3
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- NWWZPOKUUAIXIW-FLIBITNWSA-N thiamethoxam Chemical compound [O-][N+](=O)\N=C/1N(C)COCN\1CC1=CN=C(Cl)S1 NWWZPOKUUAIXIW-FLIBITNWSA-N 0.000 claims description 3
- 235000020234 walnut Nutrition 0.000 claims description 3
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- 240000002791 Brassica napus Species 0.000 claims description 2
- 235000004977 Brassica sinapistrum Nutrition 0.000 claims description 2
- 239000005906 Imidacloprid Substances 0.000 claims description 2
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- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 claims description 2
- 229940056881 imidacloprid Drugs 0.000 claims description 2
- 235000020232 peanut Nutrition 0.000 claims description 2
- 230000000361 pesticidal effect Effects 0.000 claims description 2
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- 238000007873 sieving Methods 0.000 claims description 2
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- 230000000694 effects Effects 0.000 abstract description 14
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
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- 229910052757 nitrogen Inorganic materials 0.000 description 3
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 239000003905 agrochemical Substances 0.000 description 2
- KXDAEFPNCMNJSK-UHFFFAOYSA-N benzene carboxamide Natural products NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
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- 238000001179 sorption measurement Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 241000241125 Gryllotalpa gryllotalpa Species 0.000 description 1
- 241000256259 Noctuidae Species 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
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- 150000001408 amides Chemical class 0.000 description 1
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- 239000003899 bactericide agent Substances 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
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- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000035784 germination Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003750 molluscacide Substances 0.000 description 1
- 230000002013 molluscicidal effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000005645 nematicide Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
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Classifications
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of pesticide preparation, and in particular relates to coated double-carrier pesticide controlled release granules as well as a preparation method and application thereof. The granule comprises an inner core layer and a double-network hybrid gel layer, wherein the double-network hybrid gel layer comprises a water-soluble substance and a magnetic substance, and the water-soluble substance comprises carboxymethyl cellulose and chitosan quaternary ammonium salt. The prepared granule has low cost and good pesticide controlled release performance, can still have the same effect as commercial pesticides under the condition of reduction, can promote plant growth, and provides a new technical support for the creation of efficient green pesticide preparations.
Description
Technical Field
The invention belongs to the technical field of pesticide preparation, and in particular relates to coated double-carrier pesticide controlled release granules as well as a preparation method and application thereof.
Background
At present, farmland soil often uses pesticide granules as one of means for controlling soil insects. The release characteristics of the active ingredients of the granules are divided into two types, namely a conventional type of exposure release and a controlled release, the effective utilization rate of the conventional pesticide granules is only 20-30%, and the loss rate of the conventional pesticide granules through various ways can reach 50-60%, so that the economic waste is caused, and the conventional pesticide granules are also a serious threat to the health and ecological environment of human bodies. The existing controlled release pesticide granule has the disadvantages of complicated preparation method, limited raw material sources, high preparation cost and slow release rate, can not meet the actual pest control requirements, is difficult to recycle for multiple times after field application, and is easy to cause potential pesticide residue risks.
The invention patent CN109601533A of Chinese application discloses a sustained and controlled release pesticide granule and a preparation method thereof, the sustained and controlled release pesticide granule comprises an inner core layer and an outer wrapping layer, the inner core layer and the outer wrapping layer form a spherical or ellipsoidal structure, the inner core layer comprises pesticide active ingredients, auxiliary materials and filling materials, the pesticide active ingredients are selected from one or more combinations of pesticide, bactericide, acaricide, nematicide, herbicide, molluscicide and plant growth regulator, the sustained and controlled release pesticide granule effectively prolongs the release period of pesticide, avoids the problem of waste caused by completely releasing the pesticide active ingredients at one time, and ensures that the pesticide active ingredients can be finally released into soil. The invention patent CN104829340A of the other application also discloses a microcapsule graphene composite material controlled release fertilizer granule and a preparation method thereof, wherein the granule consists of mother powder, inorganic nutrients, organic matters, an anti-hardening agent and a filler, and the granule is stable in release, and can solve the problems of fertilizer and plant diseases and insect pests in the whole season by one-time application. The release behavior of pesticides in the systems can improve the pesticide utilization rate to meet the crop growth requirement, but the control/release system still has some defects, such as the problems that carrier materials cannot be recovered, resources are wasted, environmental pollution and the like, so the further development of the green and environment-friendly control/release pesticide system becomes a research hot spot.
The pesticide control/slow release system is constructed by combining various organic and inorganic nano materials and pesticides, so as to realize the pesticide control/slow release function. Although the methods can reduce pesticide loss to a certain extent and improve the utilization rate of pesticides, the existing control/slow release system still has the following disadvantages, such as complex preparation process and high production cost; only has the function of controlling/slowly releasing, and can not provide nutrition for crops; the control/slow release system is difficult to achieve accurate release; the carrier material cannot be recovered and is easy to remain. Therefore, the sustainable development of modern agriculture health is urgent to develop new technologies to reduce production cost, control pesticide loss, and improve the effective utilization rate of pesticides.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides coated double-carrier pesticide controlled release granules and a preparation method and application thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the coated double-carrier pesticide controlled release granule comprises an inner core layer and a double-network hybridization gel layer, wherein the double-network hybridization gel layer comprises a water-soluble substance and a magnetic substance, and the water-soluble substance comprises carboxymethyl cellulose and chitosan quaternary ammonium salt.
Preferably, the magnetic substance comprises ferrous chloride and ferric chloride, and the molar ratio of the ferrous chloride to the ferric chloride is 1:1-6.
Preferably, the inner core layer comprises auxiliary materials, pesticide effective components and water, and the auxiliary materials comprise tea seed cake powder and organic fertilizer.
Preferably, the organic fertilizer is selected from any one of bean cake fertilizer, sesame fertilizer, rapeseed fertilizer, walnut fertilizer, plant straw, wood dust, rice bran, sugarcane powder and peanut shell.
Preferably, the tea cake powder comprises, by weight, 40-50 parts of tea cake powder, 0.5-4 parts of organic fertilizer, 2-20 parts of pesticide active ingredients and the balance of water.
Preferably, the pesticide active ingredient comprises a neonicotinoid pesticide and an anthranilamide pesticide.
Preferably, the weight part ratio of the neonicotinoid insecticide to the o-carboxamido benzamide insecticide is 3:1-1:1.
Preferably, the neonicotinoid insecticide is selected from any one of clothianidin, thiamethoxam, acetamiprid and imidacloprid.
Preferably, the o-carboxamido benzamide pesticide is selected from any one of chlorantraniliprole, tetrachlorethamide and tetrazolium-chlorantraniliprole.
The invention also provides a preparation method of the granule, which is characterized by comprising the following steps:
(1) Mixing the pesticide active ingredient, auxiliary materials and water to form a medicinal ball;
(2) Granulating and sieving the medicinal pellets to obtain an inner core layer;
(3) Dissolving water-soluble substances in water to prepare carboxymethyl cellulose water solution and chitosan quaternary ammonium salt water solution;
(4) And respectively spraying carboxymethyl cellulose aqueous solution and chitosan quaternary ammonium salt aqueous solution on the inner core layer, and reacting with a magnetic substance to obtain the granule.
Preferably, the mixing in step (1) takes about 10 to 15 minutes.
Preferably, the particle size of the inner core layer in step (2) is 2-4nm.
Preferably, in the step (3), the mass concentration of the carboxymethyl cellulose aqueous solution is 0.1-2.5%, and the mass concentration of the chitosan quaternary ammonium salt aqueous solution is 0.5-3%.
Preferably, the temperature of the reaction in step (3) is 25-35 ℃.
Preferably, sodium hydroxide solution is added during the reaction in step (3), and the reaction is followed by filtration.
Preferably, the concentration of the sodium hydroxide solution is 0.1-1mol/L.
The invention also provides application of the granule in killing underground pests.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts the double-network hybridization gel layer to coat the tea cake loaded with the pesticide, and the coated double-carrier pesticide controlled release granule with recycling is obtained.
(2) The preparation method of the granule is simple and convenient, the cost is low, and the hydrogel layer on the outer layer has the functions of water retention and heat preservation; the tea cake can be used as waste powder of tea seeds for waste utilization and high-quality utilization to serve as a pesticide carrier; the auxiliary material is an organic auxiliary fertilizer, and the medicine and fertilizer are integrated, so that nutrients can be provided for plants; meanwhile, the pesticide effect can be enhanced by compounding the pesticide, and the pesticide resistance of pests can be reduced.
(3) The invention has good pesticide controlled release performance, can still have the same effect as commercial pesticides under the condition of reduction, promotes plant growth, and provides a new technical support for the creation of efficient green pesticide preparations.
Drawings
FIG. 1 is an infrared spectrum of the pesticide controlled release granule prepared in example 1.
FIG. 2 is a nitrogen adsorption-desorption (BET) diagram of the pesticide controlled release granule prepared in example 1.
FIG. 3 is a scanning electron microscope image of the pesticide granules prepared in example 1 and comparative example 6, wherein FIG. 3 (A) is a scanning electron microscope image of the pesticide granules prepared in comparative example 6; FIG. 3 (B) is a scanning electron microscope image of the pesticide granule (magnified) prepared in comparative example 6; FIG. 3 (C) is a scanning electron microscope image of the pesticide granule prepared in example 1; fig. 3 (D) is a scanning electron microscope image of the pesticide granule (magnified) prepared in example 1.
FIG. 4 shows Fe in the controlled release granule for agricultural chemical prepared in example 1 2+ Is released.
Fig. 5 shows the cumulative release rate of clothianidin at different pH in the pesticide controlled release granule prepared in example 1.
FIG. 6 shows the cumulative release rate of chlorantraniliprole in the pesticide controlled release granule prepared in example 1 at different pH values.
FIG. 7 shows mortality of test insects (7 days) after construction of the pesticide control soil insect system in each treatment group.
FIG. 8 shows mortality (10 days) of test insects after construction of the pesticide control soil insect system in each treatment group.
FIG. 9 is the effect of each treatment group on crop growth index, wherein FIG. 9 (A) is fresh weight; FIG. 9 (B) is dry weight; FIG. 9 (C) shows chlorophyll content; fig. 9 (D) shows plant height.
Fig. 10 is the effect of each treatment group on crop morphology.
Fig. 11 shows the magnetic recovery rate and recycling effect of the pesticide controlled release granule prepared in example 1.
Fig. 12 shows the effect of each treatment group on the water retention effect.
Detailed Description
It is to be noted that the raw materials used in the present invention are all common commercial products, and the sources thereof are not particularly limited.
Example 1
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide comprises the following effective components of 8 parts of clothianidin and 3 parts of chlorantraniliprole, and the auxiliary materials of 50 parts of tea seed cake powder and 2 parts of sesame fertilizer. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 37 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the 2nm inner core layer.
(3) And (3) placing the material in the step (2) in a coating machine, spraying 50mL of carboxymethyl cellulose water solution with the mass concentration of 2%, uniformly spraying 50mL of chitosan quaternary ammonium salt water solution with the mass concentration of 1%, placing the material in 200mL of water solution containing 0.8109g of ferrous chloride and 1.6218g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the mass concentration of 0.1mol/L, stirring at 25 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled release granule with the double-network hybrid gel layer.
Example 2
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide active ingredients are 15 parts of acetamiprid and 5 parts of tetrazole-containing insect amide, the auxiliary materials are 40 parts of tea cake powder and 4 parts of plant straws, the weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 36 parts of water is added for stirring and mixing for 15min, and the medicine clusters are formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the inner core layer with the thickness of 3 nm.
(3) And (3) placing the material in the step (2) in a coating machine, spraying 50mL of carboxymethyl cellulose water solution with the mass concentration of 0.1%, uniformly spraying 50mL of chitosan quaternary ammonium salt water solution with the mass concentration of 3%, placing the material in 200mL of water solution containing 0.8109g of ferrous chloride and 2.9162g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the mass concentration of 1mol/L, stirring at 30 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled release granule with the double-network hybrid gel layer.
Example 3
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide comprises 3 parts of thiamethoxam and 1 part of chlorantraniliprole as effective components, and 50 parts of tea cake powder and 1 part of wood dust as auxiliary materials. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 45 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the inner core layer with the thickness of 4nm.
(3) And (3) placing the material in the step (2) into a coating machine, spraying 50mL of carboxymethyl cellulose water solution with the mass concentration of 2.5%, uniformly spraying 50mL of chitosan quaternary ammonium salt water solution with the mass concentration of 0.5%, placing the material into 200mL of water solution containing 0.8109g of ferrous chloride and 4.8661g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the mass concentration of 0.5mol/L, stirring at 35 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled release granule with the double-network hybrid gel layer.
Example 4
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide comprises 1 part of clothianidin and 1 part of chlorantraniliprole as effective components, and 50 parts of tea cake powder and 0.5 part of bean cake powder as auxiliary materials. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 47.5 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the 2nm inner core layer.
(3) And (3) placing the material in the step (2) in a coating machine, spraying 50mL of carboxymethyl cellulose water solution with the mass concentration of 1%, uniformly spraying 50mL of chitosan quaternary ammonium salt solution with the mass concentration of 2%, placing the material in 200mL of water solution containing 0.8109g of ferrous chloride and 5.8393g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the mass concentration of 0.1mol/L, stirring at 25 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled release granule with the double-network hybrid gel layer.
Comparative example 1
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide comprises, by weight, 8 parts of clothianidin and 3 parts of chlorantraniliprole as effective components, and 50 parts of walnut shell powder and 2 parts of sesame fertilizer as auxiliary materials. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 37 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the 2nm inner core layer.
(3) And (3) placing the material in the step (2) in a coating machine, spraying 50mL of carboxymethyl cellulose water solution with the mass concentration of 2%, uniformly spraying 50mL of chitosan quaternary ammonium salt water solution with the mass concentration of 1%, placing the material in 200mL of water solution containing 0.8109g of ferrous chloride and 1.6218g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the mass concentration of 0.1mol/L, stirring at 25 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled release granule with the double-network hybrid gel layer.
Comparative example 2
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide comprises the following effective components of 8 parts of clothianidin and 3 parts of chlorantraniliprole, and the auxiliary materials of 50 parts of tea seed cake powder and 2 parts of sesame fertilizer. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 37 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the 2nm inner core layer.
(3) And (3) putting the material in the step (2) into a coating machine, spraying 100mL of carboxymethyl cellulose water solution with the mass concentration of 3%, putting the material into 200mL of water solution containing 0.8109g of ferrous chloride and 1.6218g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the concentration of 0.1mol/L, stirring at 25 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled-release granule with the double-network hybrid gel layer.
Comparative example 3
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide comprises the following effective components of 8 parts of clothianidin and 3 parts of chlorantraniliprole, and the auxiliary materials of 50 parts of tea seed cake powder and 2 parts of sesame fertilizer. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 37 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the 2nm inner core layer.
(3) And (3) putting the material in the step (2) into a coating machine, spraying 100mL of chitosan quaternary ammonium salt aqueous solution with the mass concentration of 3%, putting the material into 200mL of aqueous solution containing 0.8109g of ferrous chloride and 1.6218g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the concentration of 0.1mol/L, stirring at 25 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled-release granule with the double-network hybrid gel layer.
Comparative example 4
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide comprises the following effective components of 8 parts of clothianidin and 3 parts of chlorantraniliprole, and the auxiliary materials of 25 parts of tea seed cake powder and 4 parts of sesame fertilizer. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 60 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the 2nm inner core layer.
(3) And (3) placing the material in the step (2) in a coating machine, spraying 50mL of carboxymethyl cellulose water solution with the mass concentration of 2%, uniformly spraying 50mL of chitosan quaternary ammonium salt water solution with the mass concentration of 1%, placing the material in 200mL of water solution containing 0.8109g of ferrous chloride and 1.6218g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the mass concentration of 0.1mol/L, stirring at 25 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled release granule with the double-network hybrid gel layer.
Comparative example 5
The preparation method of the coated double-carrier pesticide controlled release granule comprises the following steps:
(1) The pesticide comprises the following effective components of 8 parts of clothianidin and 3 parts of chlorantraniliprole, and the auxiliary materials of 50 parts of tea seed cake powder and 2 parts of sesame fertilizer. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 37 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the 2nm inner core layer.
(3) And (3) placing the material in the step (2) in a coating machine, spraying 50mL of carboxymethyl cellulose water solution with the mass concentration of 2%, uniformly spraying 50mL of chitosan quaternary ammonium salt water solution with the mass concentration of 1%, placing the material in 200mL of water solution containing 0.8109g of ferrous chloride and 9.7322g of ferric chloride, dropwise adding 2mL of sodium hydroxide solution with the mass concentration of 0.1mol/L, stirring at 25 ℃ for reacting for 1min, and filtering to obtain the pesticide controlled release granule with the double-network hybrid gel layer.
Comparative example 6
The preparation method of the pesticide granule comprises the following steps:
(1) The pesticide comprises the following effective components of 8 parts of clothianidin and 3 parts of chlorantraniliprole, and the auxiliary materials of 50 parts of tea seed cake powder and 2 parts of sesame fertilizer. The weighed raw materials are sequentially placed into a disc mixer for stirring and mixing, 37 parts of water is added for stirring and mixing for 10min, and a medicine cluster is formed.
(2) Extruding and granulating the medicinal pellets, putting into a coating machine, polishing, drying, screening and preparing the 2nm inner core layer.
(3) And (3) placing the material in the step (2) into 200mL of aqueous solution containing 0.8109g of ferrous chloride and 1.6218g of ferric chloride, dropwise adding 2mL of 0.1mol/L sodium hydroxide solution, stirring at 25 ℃ for reacting for 1min, and filtering to obtain the pesticide granules.
Characterization of controlled release granule of pesticide and cumulative release rate of pesticide were determined in experiment
1. The experimental method comprises the following steps:
the characterization method comprises the following steps: the pesticide controlled release granules prepared in example 1 were subjected to nitrogen adsorption and desorption (BET) and infrared (FTIR) characterization, and the pesticide granules prepared in example 1 and comparative example 6 were subjected to Scanning Electron Microscopy (SEM) characterization. The infrared spectrum of the pesticide controlled release granule prepared in example 1 is shown in fig. 1, the nitrogen adsorption and desorption (BET) diagram is shown in fig. 2, and the scanning electron microscope diagrams are shown in fig. 3 (C) and 3 (D). The sem images of the pesticide granules prepared in comparative example 6 are shown in fig. 3 (a) and 3 (B).
The method for measuring the accumulated release rate of the pesticide active ingredient comprises the following steps: 0.1g of the pesticide controlled release granules prepared in examples 1 to 4 and comparative examples 1 to 5 were weighed respectively, 10mL of 90% acetonitrile aqueous solution was added, 100. Mu.L of the solution was taken at fixed intervals and diluted to 1mL with acetonitrile, and the solution was passed through an organic filter membrane of 0.22 μm, and the cumulative release rate of the pesticide active ingredient was detected under the above-mentioned detection conditions. Each set of experiments was run in triplicate. Fe in the pesticide controlled release granule prepared in example 1 2+ The release amount of clothianidin in the controlled-release granule of pesticide prepared in example 1 is shown in FIG. 4, the cumulative release rate of clothianidin at different pH values in the controlled-release granule of pesticide prepared in example 1 is shown in FIG. 5The cumulative release rates of chlorantraniliprole in the release granule at different pH values are shown in figure 6.
The calculation formula of the accumulated release rate of the pesticide active ingredient is shown as follows:
wherein: c (C) t The concentration of the sample taken at time t, (mg/mL); v (V) t The volume of sample taken at time t, (100 μl); v (V) total To total volume of release medium, (10 mL); m is m 0 The mass of the gel sphere (10 mg).
2. Data analysis:
it can be seen from figures 1, 2, 3 (C) and 3 (D) that clothianidin, chlorantraniliprole and dual network hybrid gel layers have all been successfully loaded.
As can be seen from FIGS. 4 to 6, the controlled release granule for agricultural chemical prepared in example 1 contains Fe 2+ The release amount reaches the maximum value at the 7 th day, and the release rate of the pesticide active ingredients clothianidin and chlorantraniliprole is continuously increased under different pH values.
The measurement results of the cumulative release rates of the pesticide active ingredients prepared in examples 1 to 4 and comparative examples 1 to 5 are shown in Table 2.
TABLE 2
Experiment three for determining mortality of pesticide controlled release granules on underground pests
1. The experimental method comprises the following steps: 10 grubs and mole cricket are taken and put into a box (10 cm x 8cm x 5 cm) filled with soil insect-cultivating, wherein the soil is wetted by a proper amount of water, and the following treatments are respectively carried out: (1) a blank group (distilled water treatment); (2) 11.9mg of 1.6% chlorantraniliprole insecticide (commercial agent) was added; (3) 9.5mg of the pesticide controlled release granule prepared in example 1 (20% reduction) was added; (4) 11.9mg of the pesticide controlled release granule prepared in example 1 was added. The tested pests are supplemented after the death rate is counted on the 7 th day, so that the number of the pests in the system is maintained at 10, and the death rate is counted again on the 10 th day. Mortality (7 days) of the test insects in each treatment group is shown in fig. 7.
10 pieces of cutworms are taken and placed in a culture dish (diameter is 9 cm), filter paper moistened by distilled water is paved on the bottom of the culture dish, and the following treatments are respectively carried out: (1) a blank group (distilled water treatment); (2) 9.45mg of 1.6% chlorantraniliprole insecticide (commercial agent) was added; (3) 7.56mg of the pesticide controlled release granule prepared in example 1 (20% reduction) was added; (4) 9.45mg of the pesticide controlled release granule prepared in example 1 was added. The tested pests are supplemented after the death rate is counted on the 7 th day, so that the number of the pests in the system is maintained at 10, and the death rate is counted again on the 10 th day. Mortality (10 days) of the test insects in each treatment group is shown in fig. 8.
2. Data analysis: as can be seen from fig. 7 to 8, the pesticide controlled release granule of the present invention has a good effect of killing soil insects compared with a general commercial agent.
Experiment four to determine the influence of pesticide controlled release granule on crop growth and morphology
1. The experimental method comprises the following steps: the pesticide controlled release granule containing the double-network hybrid gel layer is directly applied to soil surfaces, colonization holes and transplanting furrows, or is applied along with fertilizer, seeds and the like, and is used for root and seedling increase in crop growth. The specific application method is that when crops are cultivated in soil (the diameter of the used flowerpot is 16cm, 10 plants are planted in each group of flowerpots), small furrows are dug around the basal part, and the treatment group A is respectively: blank control (distilled water treatment); treatment group B: 30.1mg of 1.6% chlorantraniliprole insecticide is added; treatment group C: 24.1mg of the pesticide controlled release granule prepared in example 1 (20% reduction) was added; treatment group D: 30.1mg of the pesticide controlled release granule prepared in example 1 is added, four groups of treated fine sand-mixed soil are spread in a small ditch, and covered by a soil layer. After experimental treatment, conventional management is carried out, the germination rate of the granules along with the plant after planting is observed, and the root length and root weight of the plant are measured by a chlorophyll meter after the granules grow to 3 weeks. The effect of each treatment group on the fresh weight, dry weight, chlorophyll content and plant height of the crop growth is shown in fig. 9 (a), fig. 9 (B), fig. 9 (C) and fig. 9 (D), and the effect of each treatment group on the crop morphology is shown in fig. 10.
2. Data analysis: as can be seen from fig. 9 (a), 9 (B), 9 (C), 9 (D) and 10, the pesticide controlled release granule prepared by the present invention has the effect of promoting the growth of crops.
Experiment five to determine magnetic recovery rate, cyclic utilization and water retention rate of pesticide controlled release granule
1. The experimental method comprises the following steps:
the method for measuring the magnetic recovery rate and recycling of the pesticide controlled release granule comprises the following steps: mixing 0.5g of the pesticide controlled release granule prepared in example 1 into a certain amount of soil, uniformly mixing, recovering the active ingredient in the granule by using a 0.2T magnet in the fourth day of release in the soil, and adding and releasing the active ingredient to evaluate the recycling performance of the carrier. The magnetic recovery rate and recycling effect of the pesticide controlled release granule prepared in example 1 are shown in fig. 11.
The method for measuring the water retention rate of the pesticide controlled release granule comprises the following steps: 0.2g of chlorantraniliprole is weighed as a treatment group A (the double-network hybridized gel layer coating is C1) and 0.2g of a commodity agent (1.6% chlorantraniliprole insecticide is C2) is weighed as a treatment group B. Samples C1 and C2 were mixed with 10g of dry sand (150-200 mesh) in a petri dish (diameter 9 cm), respectively, and 15mL of deionized water was slowly added to the system, which was covered with 10g of dry sand; in addition, no sample was added as blank group C. The initial weights of C1 and C2 and CK were designated as W C1 ，W C2 And W is CK . Standing at 30deg.C for 10 hr, and recording the weight of the obtained system as W C1＇ ，W C2＇ And W is CK＇ . The effect of each treatment group on the water retention effect is shown in fig. 12.
The Water Retention Ratio (WRR) is calculated as follows:
water Retention Ratio (WRR) = [ (W) c1 -W c1′ )-(W CK -W CK )]/(W c1 -W c1′ )×100％
Wherein: w (W) CK Initial weight for blank treatment group, (g);
W C1 (W C2 ) To the initial weight of treatment group a (treatment group B), (g);
W CK＇ post-reaction weight for blank treatment group, (g);
W C1＇ (W C2＇ ) The weight after reaction of treatment group A (treatment group B), and (g).
2. Data analysis: as can be seen from fig. 11, the pesticide controlled release granule prepared by the present invention has good magnetic recovery rate and excellent recyclability. As can be seen from fig. 12, the pesticide controlled release granule prepared by the invention has good water retention performance.
Finally, it should be noted that the above description is only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and that the simple modification and equivalent substitution of the technical solution of the present invention can be made by those skilled in the art without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The coated double-carrier pesticide controlled release granule is characterized by comprising an inner core layer and a double-network hybridization gel layer, wherein the double-network hybridization gel layer comprises a water-soluble substance and a magnetic substance, and the water-soluble substance comprises carboxymethyl cellulose and chitosan quaternary ammonium salt.
2. The granule of claim 1, wherein the magnetic substance comprises ferrous chloride and ferric chloride in a molar ratio of 1:1-6.
3. The granule of claim 1, wherein the inner core layer comprises an auxiliary material, a pesticide active ingredient and water, the auxiliary material comprises tea cake powder and an organic fertilizer, and the organic fertilizer is selected from any one of bean cake fertilizer, sesame fertilizer, rapeseed fertilizer, walnut fertilizer, plant straw, wood dust, rice bran, sugarcane powder and peanut shell.
4. The granule as claimed in claim 3, wherein the tea cake powder is 40-50 parts by weight, the organic fertilizer is 0.5-4 parts by weight, the pesticide active ingredient is 2-20 parts by weight, and the balance is water.
5. A granule as claimed in claim 3, characterized in that the pesticidal active ingredient comprises a neonicotinoid insecticide selected from any one of clothianidin, thiamethoxam, acetamiprid and imidacloprid and an o-carboxamidobenzamide insecticide selected from any one of chlorantraniliprole, tetrachlorethamide and tetrazolium-chlorantraniliprole.
6. The granule of claim 5, wherein the weight ratio of the neonicotinoid insecticide to the anthranilamide insecticide is 3:1-1:1.
7. A process for the preparation of granules as claimed in any of claims 3 to 6, comprising the steps of:
(1) Mixing the pesticide active ingredient, auxiliary materials and water to form a medicinal ball;
(2) Granulating and sieving the medicinal pellets to obtain an inner core layer;
(3) Dissolving water-soluble substances in water to prepare carboxymethyl cellulose water solution and chitosan quaternary ammonium salt water solution;
(4) And respectively spraying carboxymethyl cellulose aqueous solution and chitosan quaternary ammonium salt aqueous solution on the inner core layer, and reacting with a magnetic substance to obtain the granule.
8. The method according to claim 7, wherein the mixing time in step (1) is 10 to 15 minutes; the grain diameter of the inner core layer in the step (2) is 2-4nm; the mass concentration of the carboxymethyl cellulose aqueous solution in the step (3) is 0.1-2.5%, and the mass concentration of the chitosan quaternary ammonium salt aqueous solution is 0.5-3%; the temperature of the reaction in step (4) is 25-35 ℃.
9. The process according to claim 7, wherein a sodium hydroxide solution is added during the reaction in the step (4), and the concentration of the sodium hydroxide solution is 0.1 to 1mol/L.
10. Use of a granule according to any one of claims 1 to 6 or a granule prepared by a method according to any one of claims 7 to 9 for combating subterranean pests.
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