CN113480363A - Preparation method and application of pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid - Google Patents
Preparation method and application of pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid Download PDFInfo
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- CN113480363A CN113480363A CN202110904708.XA CN202110904708A CN113480363A CN 113480363 A CN113480363 A CN 113480363A CN 202110904708 A CN202110904708 A CN 202110904708A CN 113480363 A CN113480363 A CN 113480363A
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- imidacloprid
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- chlorantraniliprole
- fertilizer
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 45
- 239000005886 Chlorantraniliprole Substances 0.000 title claims abstract description 38
- 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 title claims abstract description 38
- 239000005906 Imidacloprid Substances 0.000 title claims abstract description 37
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229940056881 imidacloprid Drugs 0.000 title claims abstract description 37
- 239000008187 granular material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 109
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000575 pesticide Substances 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 39
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 32
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 26
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 26
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000012046 mixed solvent Substances 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 16
- 229920000742 Cotton Polymers 0.000 claims description 13
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 13
- 239000001632 sodium acetate Substances 0.000 claims description 13
- 235000017281 sodium acetate Nutrition 0.000 claims description 13
- 239000001384 succinic acid Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 6
- 241000607479 Yersinia pestis Species 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims 1
- 238000007670 refining Methods 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 abstract description 6
- 239000001913 cellulose Substances 0.000 abstract description 6
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 125000000524 functional group Chemical group 0.000 abstract description 3
- 125000004080 3-carboxypropanoyl group Chemical group O=C([*])C([H])([H])C([H])([H])C(O[H])=O 0.000 abstract 1
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 12
- 241000209140 Triticum Species 0.000 description 7
- 235000021307 Triticum Nutrition 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000000749 insecticidal effect Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- -1 nitromethylene Chemical group 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 125000002730 succinyl group Chemical group C(CCC(=O)*)(=O)* 0.000 description 4
- 238000000967 suction filtration Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000002917 insecticide Substances 0.000 description 3
- 239000000618 nitrogen fertilizer Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 description 1
- LFXSHFHOJMKZDE-UHFFFAOYSA-N 2-formamidobenzamide Chemical compound NC(=O)C1=CC=CC=C1NC=O LFXSHFHOJMKZDE-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000009863 secondary prevention Effects 0.000 description 1
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229940014800 succinic anhydride Drugs 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/60—Biocides or preservatives, e.g. disinfectants, pesticides or herbicides; Pest repellants or attractants
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
- C05G5/12—Granules or flakes
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
Abstract
The invention relates to a preparation method and application of insecticide-fertilizer granules containing chlorantraniliprole and imidacloprid, which comprises the following steps: preparing a wall material; weighing the following raw materials in parts by weight: 0.01-3 parts of chlorantraniliprole, 0.01-3 parts of imidacloprid, 0.1-5 parts of wall material, 1-4 parts of deionized water, 10-50 parts of element fertilizer and 30-50 parts of diatomite; uniformly mixing chlorantraniliprole, imidacloprid and an element fertilizer, and then carrying out air flow crushing to obtain a raw pesticide containing chlorantraniliprole, imidacloprid and the element fertilizer; uniformly mixing the raw material, wall materials, deionized water and diatomite, and granulating to obtain a medicinal fertilizer granule; mixing and esterifying the base material a, the intermediate 1 and acetic anhydride to prepare a cellulose derivative, wherein the cellulose derivative contains three functional groups of methoxyl, acetyl and succinyl, and the acetyl endows the cellulose derivative with excellent flexibility and can be used as a coating material and a wall material.
Description
Technical Field
The invention belongs to the technical field of fertilizers, and particularly relates to a preparation method and application of pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid.
Background
Chemical control is an important means of preventing and controlling pests in agriculture. However, at present, it is sometimes impossible to effectively control pests due to factors such as poor effects and developed resistance caused by the type, living characteristics, living environment, and the like of pests. In particular, it is becoming increasingly difficult to control lepidopteran, coleopteran, homopteran, and thysanopteran pests using conventional agents.
The chlorantraniliprole is an o-formylaminobenzamide pesticide, the imidacloprid is a nitromethylene pesticide, belongs to a chloronicotinyl pesticide, is also called a neonicotinoid pesticide, has broad spectrum, high efficiency, low toxicity and low residue, is not easy to generate resistance by pests, and has multiple functions of contact poisoning, stomach toxicity, systemic absorption and the like.
At present, the effects of fertilization and insecticidal control are poor through pesticide fertilizer granules, and the traditional means is only to add insecticides in pesticide fertilizers and the like, so that the insecticides are killed while the fertilizers are fertilized, but the insecticide is one-time insecticidal, and the staged control on crops cannot be realized.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method and application of pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid.
The purpose of the invention can be realized by the following technical scheme:
the preparation method of the pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid comprises the following steps:
step S1, preparing a wall material;
step S2, weighing the following raw materials in parts by weight: 0.01-3 parts of chlorantraniliprole, 0.01-3 parts of imidacloprid, 0.1-5 parts of wall material, 1-4 parts of deionized water, 10-50 parts of element fertilizer and 30-50 parts of diatomite;
step S3, uniformly mixing chlorantraniliprole, imidacloprid and the element fertilizer, and then performing air flow crushing to obtain a raw pesticide containing chlorantraniliprole, imidacloprid and the element fertilizer;
and step S4, uniformly mixing the raw medicine, the wall material, the deionized water and the diatomite, and granulating to obtain the medicinal fertilizer granules.
Further, the wall material is prepared by the following steps:
step S11, crushing cotton fibers into fine materials of 0.1-0.3mm, placing the fine materials into a reaction kettle, vacuumizing, introducing nitrogen, adding a mixed solvent for treatment for 30min to obtain a primary material, adding a treatment solution into the primary material, heating to 40-45 ℃, keeping the temperature for reaction for 1h, heating to 80 ℃, continuing the reaction for 1h to obtain a base material a, wherein the weight ratio of the cotton fibers to the mixed solvent to the treatment solution is 1: 3: 10;
in step S11, the base material a, i.e., the modified cellulose, is prepared by treating the cotton fiber;
step S12, adding succinic acid and phosphorus oxychloride into a reaction kettle, heating to 230 ℃, preserving heat at the temperature, and reacting for 4 hours to obtain an intermediate 1, wherein the dosage of the phosphorus oxychloride is controlled to be 5-10% of the weight of the succinic acid;
in the step S12, phosphorus oxychloride is used as a dehydrating agent, succinic acid is dehydrated to prepare an intermediate 1, and the intermediate 1 is succinic anhydride;
step S13, adding the base material a into a reaction kettle, then sequentially adding acetic acid and sodium acetate, stirring at a constant speed for 30min, then adding the intermediate 1 and acetic anhydride, heating to 100-.
Step S13, adding acetic acid and sodium acetate, taking the acetic acid as a solvent and the sodium acetate as a catalyst, constructing an acetic acid-sodium acetate system, mixing and reacting a base material a, an intermediate 1 and acetic anhydride to prepare a wall material, and mixing and esterifying the base material a, the intermediate 1 and the acetic anhydride to prepare the wall material, namely the cellulose derivative, wherein the wall material contains three functional groups of methoxy, acetyl and succinyl, the acetyl groups endow the wall material with excellent flexibility, can be used as a coating material and a wall material, and has excellent processing performance, and the succinyl groups endow the wall material with excellent solubility.
Further, in step S11, the mixed solvent is a mixture of 70% by mass aqueous sodium hydroxide solution, toluene and isopropanol in a weight ratio of 100: 150: 30.
Further, in step S11, the treating fluid is prepared by mixing toluene, isopropanol, chloromethane and propylene oxide according to the weight ratio of 20: 4: 6: 1.
The invention has the beneficial effects that:
the pesticide-fertilizer granules are prepared by taking chlorantraniliprole and imidacloprid as insecticidal base materials, and a wall material is prepared by mixing and esterifying a base material a, an intermediate 1 and acetic anhydride in the preparation process, namely the wall material is a cellulose derivative which contains three functional groups of methoxyl group, acetyl group and succinyl group, wherein the acetyl group endows the wall material with excellent flexibility, the wall material can be used as a coating material and a wall material, and has excellent processing performance, the succinyl group endows the wall material with excellent solubility, the wall material can be dissolved when meeting a manually sprayed solvent when being used as the wall material, so that an internal insecticidal composition is released, a long-term effective treatment effect is achieved, the treatment efficiency is improved, the first insecticidal control is carried out when the fertilizer is applied, and then the chlorantraniliprole and the imidacloprid which are wrapped by the wall material can be released again when the solvent is manually sprayed, and (5) performing secondary prevention and control.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The wall material is prepared by the following steps:
step S11, crushing cotton fibers into fine materials of 0.1mm, placing the fine materials in a reaction kettle, vacuumizing, introducing nitrogen, adding a mixed solvent for treatment for 30min to obtain a primary material, then adding a treatment solution into the primary material, heating to 40 ℃, carrying out heat preservation reaction for 1h, heating to 80 ℃, and continuing the reaction for 1h to obtain a base material a, wherein the weight ratio of the cotton fibers to the mixed solvent to the treatment solution is 1: 3: 10;
the mixed solvent is formed by mixing 70 percent of sodium hydroxide aqueous solution, toluene and isopropanol according to the weight ratio of 100: 150: 30.
The treating fluid is prepared by mixing toluene, isopropanol, chloromethane and propylene oxide according to the weight ratio of 20: 4: 6: 1.
Step S12, adding succinic acid and phosphorus oxychloride into a reaction kettle, heating to 230 ℃, preserving heat at the temperature, and reacting for 4 hours to obtain an intermediate 1, wherein the dosage of the phosphorus oxychloride is controlled to be 5% of the weight of the succinic acid;
step S13, adding the base material a into a reaction kettle, then sequentially adding acetic acid and sodium acetate, stirring at a constant speed for 30min, then adding the intermediate 1 and acetic anhydride, heating to 100 ℃, stirring at a constant speed, reacting for 2h, cooling to room temperature after the reaction is finished, adding deionized water, forming a precipitate at a rotation speed of 800r/min, performing suction filtration, washing and drying to obtain the wall material, controlling the dosage ratio of the base material a, the acetic acid and the sodium acetate to be 10 g: 70 mL: 9g, controlling the dosage of the intermediate 1 to be 5 weight of the base material a, and controlling the dosage of the acetic anhydride to be 7 weight of the base material a.
Example 2
The wall material is prepared by the following steps:
step S11, crushing cotton fibers into fine materials of 0.2mm, placing the fine materials in a reaction kettle, vacuumizing, introducing nitrogen, adding a mixed solvent for treatment for 30min to obtain a primary material, then adding a treatment solution into the primary material, heating to 40 ℃, carrying out heat preservation reaction for 1h, heating to 80 ℃, and continuing the reaction for 1h to obtain a base material a, wherein the weight ratio of the cotton fibers to the mixed solvent to the treatment solution is 1: 3: 10;
the mixed solvent is formed by mixing 70 percent of sodium hydroxide aqueous solution, toluene and isopropanol according to the weight ratio of 100: 150: 30.
The treating fluid is prepared by mixing toluene, isopropanol, chloromethane and propylene oxide according to the weight ratio of 20: 4: 6: 1.
Step S12, adding succinic acid and phosphorus oxychloride into a reaction kettle, heating to 230 ℃, preserving heat at the temperature, and reacting for 4 hours to obtain an intermediate 1, wherein the dosage of the phosphorus oxychloride is controlled to be 6% of the weight of the succinic acid;
step S13, adding the base material a into a reaction kettle, then sequentially adding acetic acid and sodium acetate, stirring at a constant speed for 30min, then adding the intermediate 1 and acetic anhydride, heating to 100 ℃, stirring at a constant speed, reacting for 2h, cooling to room temperature after the reaction is finished, adding deionized water, forming a precipitate at a rotation speed of 800r/min, performing suction filtration, washing and drying to obtain the wall material, wherein the dosage ratio of the base material a, the acetic acid and the sodium acetate is controlled to be 10 g: 70 mL: 9g, the dosage of the intermediate 1 is 6% of the weight of the base material a, and the dosage of the acetic anhydride is 8% of the weight of the base material a.
Example 3
The wall material is prepared by the following steps:
step S11, crushing cotton fibers into fine materials of 0.3mm, placing the fine materials in a reaction kettle, vacuumizing, introducing nitrogen, adding a mixed solvent for treatment for 30min to obtain a primary material, then adding a treatment solution into the primary material, heating to 45 ℃, carrying out heat preservation reaction for 1h, heating to 80 ℃, and continuing the reaction for 1h to obtain a base material a, wherein the weight ratio of the cotton fibers to the mixed solvent to the treatment solution is 1: 3: 10;
the mixed solvent is formed by mixing 70 percent of sodium hydroxide aqueous solution, toluene and isopropanol according to the weight ratio of 100: 150: 30.
The treating fluid is prepared by mixing toluene, isopropanol, chloromethane and propylene oxide according to the weight ratio of 20: 4: 6: 1.
Step S12, adding succinic acid and phosphorus oxychloride into a reaction kettle, heating to 230 ℃, preserving heat at the temperature, and reacting for 4 hours to obtain an intermediate 1, wherein the dosage of the phosphorus oxychloride is controlled to be 8% of the weight of the succinic acid;
step S13, adding the base material a into a reaction kettle, then sequentially adding acetic acid and sodium acetate, stirring at a constant speed for 30min, then adding the intermediate 1 and acetic anhydride, heating to 110 ℃, stirring at a constant speed, reacting for 2h, cooling to room temperature after the reaction is finished, adding deionized water, forming a precipitate at a rotation speed of 800r/min, performing suction filtration, washing and drying to obtain the wall material, wherein the dosage ratio of the base material a, the acetic acid and the sodium acetate is controlled to be 10 g: 70 mL: 9g, the dosage of the intermediate 1 is 8% of the weight of the base material a, and the dosage of the acetic anhydride is 9% of the weight of the base material a.
Example 4
The wall material is prepared by the following steps:
step S11, crushing cotton fibers into fine materials of 0.3mm, placing the fine materials in a reaction kettle, vacuumizing, introducing nitrogen, adding a mixed solvent for treatment for 30min to obtain a primary material, then adding a treatment solution into the primary material, heating to 45 ℃, carrying out heat preservation reaction for 1h, heating to 80 ℃, and continuing the reaction for 1h to obtain a base material a, wherein the weight ratio of the cotton fibers to the mixed solvent to the treatment solution is 1: 3: 10;
the mixed solvent is formed by mixing 70 percent of sodium hydroxide aqueous solution, toluene and isopropanol according to the weight ratio of 100: 150: 30.
The treating fluid is prepared by mixing toluene, isopropanol, chloromethane and propylene oxide according to the weight ratio of 20: 4: 6: 1.
Step S12, adding succinic acid and phosphorus oxychloride into a reaction kettle, heating to 230 ℃, preserving heat at the temperature, and reacting for 4 hours to obtain an intermediate 1, wherein the dosage of the phosphorus oxychloride is controlled to be 10% of the weight of the succinic acid;
step S13, adding the base material a into a reaction kettle, then sequentially adding acetic acid and sodium acetate, stirring at a constant speed for 30min, then adding the intermediate 1 and acetic anhydride, heating to 110 ℃, stirring at a constant speed, reacting for 2h, cooling to room temperature after the reaction is finished, adding deionized water, forming a precipitate at a rotation speed of 800r/min, performing suction filtration, washing and drying to obtain the wall material, wherein the dosage ratio of the base material a, the acetic acid and the sodium acetate is controlled to be 10 g: 70 mL: 9g, the dosage of the intermediate 1 is 10% of the weight of the base material a, and the dosage of the acetic anhydride is 10% of the weight of the base material a.
Comparative example 1
This comparative example is base a after being subjected to step S11.
Comparative example 2
This comparative example is cross-linked starch as the wall material.
Referring to the preparation method of the granules of the present invention, the wall materials prepared in examples 1 to 4 and comparative examples 1 to 2 were used to prepare granules, the dosage of chlorantraniliprole was controlled to be 0.5% of the weight of the granules, 5g of the granules were placed in 1L of deionized water for a release test, 5mL of liquid was taken out after 30min, the concentration a of chlorantraniliprole in the solution was measured by using a high performance liquid chromatograph, then the residual granules were placed in an aqueous ethanol solution with a volume fraction of 15%, 5mL of liquid was taken out after 30min, and the concentration B of chlorantraniliprole in the solution was measured, and the results are shown in table 1 below:
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | Comparative example 2 | |
| The concentration is A% | 53.2 | 55.3 | 53.1 | 52.8 | 53.0 | 98 |
| Concentration B% | 42.6 | 41.5 | 42.1 | 40.5 | 3.5 | 0.2 |
As can be seen from Table 1 above, examples 1-4 had 30min release concentrations of 52.8-55.3% in deionized water, 30min release concentrations of 40.5-42.6% in aqueous ethanol, comparative examples 1-2 had 30min release concentrations of 53.0-98% in deionized water, and 30min release concentrations of 0.2-3.5% in aqueous ethanol; therefore, the granules prepared by the wall material prepared by the invention have excellent slow release effect;
example 5
The preparation method of the pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid comprises the following steps:
step S1, preparing wall material as in example 1;
step S2, weighing the following raw materials in parts by weight: 0.01 part of chlorantraniliprole, 0.01 part of imidacloprid, 0.1 part of wall material, 1 part of deionized water, 10 parts of ammoniacal nitrogen fertilizer and 30 parts of diatomite;
step S3, uniformly mixing chlorantraniliprole, imidacloprid and the element fertilizer, and then performing air flow crushing to obtain a raw pesticide containing chlorantraniliprole, imidacloprid and the element fertilizer;
and step S4, uniformly mixing the raw medicine, the wall material, the deionized water and the diatomite, and granulating to obtain the medicinal fertilizer granules.
Example 6
The preparation method of the pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid comprises the following steps:
step S1, preparing wall material as in example 1;
step S2, weighing the following raw materials in parts by weight: 1.5 parts of chlorantraniliprole, 1.5 parts of imidacloprid, 3 parts of wall materials, 2 parts of deionized water, 30 parts of ammoniacal nitrogen fertilizer and 40 parts of diatomite;
step S3, uniformly mixing chlorantraniliprole, imidacloprid and the element fertilizer, and then performing air flow crushing to obtain a raw pesticide containing chlorantraniliprole, imidacloprid and the element fertilizer;
and step S4, uniformly mixing the raw medicine, the wall material, the deionized water and the diatomite, and granulating to obtain the medicinal fertilizer granules.
Example 7
The preparation method of the pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid comprises the following steps:
step S1, preparing wall material as in example 1;
step S2, weighing the following raw materials in parts by weight: 3 parts of chlorantraniliprole, 3 parts of imidacloprid, 5 parts of wall materials, 4 parts of deionized water, 50 parts of ammoniacal nitrogen fertilizer and 50 parts of diatomite;
step S3, uniformly mixing chlorantraniliprole, imidacloprid and the element fertilizer, and then performing air flow crushing to obtain a raw pesticide containing chlorantraniliprole, imidacloprid and the element fertilizer;
and step S4, uniformly mixing the raw medicine, the wall material, the deionized water and the diatomite, and granulating to obtain the medicinal fertilizer granules.
Comparative example 3
The comparative example is a fertilizer granule containing imidacloprid in the market.
The experiment is carried out in a farmer wheat field at the periphery of the south of Henan, each group is treated for 4 times, and the treatment area is 30m2. The experimental groups respectively apply the pesticide-fertilizer granules prepared in examples 5 to 7, and the application mode is that the pesticide-fertilizer slow-release preparation is spread in soil; comparative example 3 the application of 2% imidacloprid sustained release granules and the application of each control group were the same as the application of the experimental group. After wheat is matureAnd collecting wheat, counting the wheat yield of each group, and inspecting the economic state of the wheat field of each group. The application rates of the test samples for each group, and the wheat yields for each group are shown in Table 2.
TABLE 2
As can be seen from Table 2 above, the control effect on wheat planting of examples 5 to 7 is superior to that of comparative example 3.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (6)
1. The preparation method of the pesticide-fertilizer granules containing chlorantraniliprole and imidacloprid is characterized by comprising the following steps: the method comprises the following steps:
step S1, preparing a wall material;
step S2, weighing the following raw materials in parts by weight: 0.01-3 parts of chlorantraniliprole, 0.01-3 parts of imidacloprid, 0.1-5 parts of wall material, 1-4 parts of deionized water, 10-50 parts of element fertilizer and 30-50 parts of diatomite;
step S3, uniformly mixing chlorantraniliprole, imidacloprid and the element fertilizer, and then performing air flow crushing to obtain a raw pesticide containing chlorantraniliprole, imidacloprid and the element fertilizer;
and step S4, uniformly mixing the raw medicine, the wall material, the deionized water and the diatomite, and granulating to obtain the medicinal fertilizer granules.
2. The preparation method of the insecticide-fertilizer granules containing the chlorantraniliprole and the imidacloprid according to claim 1, which is characterized by comprising the following steps of: the wall material is prepared by the following steps:
step S11, crushing cotton fibers into fine materials, placing the fine materials into a reaction kettle, vacuumizing, introducing nitrogen, adding a mixed solvent, treating for 30min to obtain a primary material, adding a treatment solution into the primary material, heating to 40-45 ℃, keeping the temperature, reacting for 1h, heating to 80 ℃, continuing to react for 1h, and refining to obtain a base material a;
step S12, adding succinic acid and phosphorus oxychloride into a reaction kettle, heating to 230 ℃, preserving heat at the temperature, and reacting for 4 hours to obtain an intermediate 1;
and step S13, adding the base material a into a reaction kettle, then sequentially adding acetic acid and sodium acetate, stirring at a constant speed for 30min, then adding the intermediate 1 and acetic anhydride, heating to 100-.
3. The preparation method of the insecticide-fertilizer granules containing the chlorantraniliprole and the imidacloprid according to claim 2, which is characterized by comprising the following steps of: in step S11, the mixed solvent is prepared by mixing 70% by mass of sodium hydroxide aqueous solution, toluene and isopropanol according to the weight ratio of 100: 150: 30.
4. The preparation method of the insecticide-fertilizer granules containing the chlorantraniliprole and the imidacloprid according to claim 2, which is characterized by comprising the following steps of: in step S11, the treating fluid is formed by mixing toluene, isopropanol, chloromethane and propylene oxide according to the weight ratio of 20: 4: 6: 1.
5. The preparation method of the insecticide-fertilizer granules containing the chlorantraniliprole and the imidacloprid according to claim 2, which is characterized by comprising the following steps of: in the step S11, the weight ratio of the cotton fiber, the mixed solvent and the treatment liquid is 1: 3: 10, the dosage of the phosphorus oxychloride is controlled to be 5-10% of the weight of the succinic acid in the step S12, the dosage ratio of the base material a, the acetic acid and the sodium acetate is controlled to be 10 g: 70 mL: 9g in the step S13, the dosage of the intermediate 1 is 5-10% of the weight of the base material a, and the dosage of the acetic anhydride is 7-10% of the weight of the base material a.
6. The application of the pesticide fertilizer granules prepared by the preparation method according to claim 1 in farmland pest control.
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