CN110692630B - Floating carrier for floating large granules and preparation method thereof - Google Patents
Floating carrier for floating large granules and preparation method thereof Download PDFInfo
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- CN110692630B CN110692630B CN201910898153.5A CN201910898153A CN110692630B CN 110692630 B CN110692630 B CN 110692630B CN 201910898153 A CN201910898153 A CN 201910898153A CN 110692630 B CN110692630 B CN 110692630B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
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- Agricultural Chemicals And Associated Chemicals (AREA)
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Abstract
The invention discloses a floating carrier for floating large granules and a preparation method thereof. The floating carrier is prepared by the following method: (1) pulverizing cortex Corbi by pulverizer, drying, and sieving with 80-100 mesh sieve; (2) adding the sieved embolic skin powder into a ligninase solution, filtering and cleaning after the reaction is finished; (3) adding the embolic skin powder reacted in the step (2) into ammonia water with the mass concentration of 10-15%, reacting for 6-8h, filtering and cleaning after the reaction is finished; (4) and (4) adding the modified embolic cortex powder obtained in the step (3) into a solution containing EDC and NHS, mixing with a solution containing a high molecular compound, and crosslinking for 12-24h to obtain the floating carrier. According to the floating carrier, the cork is used as a carrier, the cork is crushed by a crusher to have a certain particle size, and then hydrolysis holes are formed in the cork powder through hydrolysis of ligninase, so that the loading capacity of the carrier is increased, and the floating carrier can be completely biodegraded.
Description
Technical Field
The invention relates to a floating carrier and a preparation method thereof, in particular to a floating carrier for floating large granules and a preparation method thereof.
Background
The preparation developed at the earliest is a pesticide water surface floating agent, which mainly comprises: in 1977, japanese patent JP52038095 reports that Kawasaki Masashi, Watanabe Fujinori and the like in japan first developed a powdered phytoether floating agent, which is composed of an organic pesticide, an inorganic carrier, a hydrophobic substance and a film material. The floating powder has the defects of easy drifting and easy pollution; later turned to the development of floating (granular) granules on water. The research and development of the floating granule mainly comprise the following points: firstly, the foaming tablet can float on the water surface or can foam when being immersed in the water, so that the effective ingredients can be diffused in the water; secondly, the foaming particles or powder and the like are packaged by a water-soluble packaging bag; thirdly, packaging the water surface developing agent, the water dispersible granules, the powder and the like by using a water-soluble packaging bag; fourthly, the water surface developing agent or the emulsifying liquid agent and the gel agent are packaged by a water-soluble packaging bag. The floating large granules used at present are particles which are dispersed on the water surface of a rice field by 3-8 mm, and only need to be scattered on ridges of the rice field without entering the rice field through different pesticide application modes, so that the floating large granules are a labor-saving dosage form, and the diffusivity of active ingredients in the preparation can meet the requirement of practical application in the field.
The key technology for developing the floating large particle agent is the preparation of a floating carrier, the earliest floating carrier is beaded sodium borate particles with certain granularity formed by processing sodium borate, and the carrier prepared by sodium borate particles with different granularities is used for loading pesticide active components, but the existing floating carrier has the problems of poor environmental compatibility and poor loading capacity.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problems in the prior art, the invention provides a floating carrier for floating large granules and a preparation method of the floating carrier.
The technical scheme is as follows: the invention relates to a preparation method of a floating carrier for floating large granules, which comprises the following steps:
(1) pulverizing cortex Corbi by pulverizer, drying, and sieving with 80-100 mesh sieve;
(2) adding the sieved embolic skin powder into a ligninase solution with the mass concentration of 8-10g/L, stirring for 4-5h under the condition of 200-300rmp, filtering and cleaning after the reaction is finished;
(3) adding the embolic skin powder reacted in the step (2) into ammonia water with the mass concentration of 10-15%, reacting for 6-8h at the temperature of 160-200 ℃ and the rotating speed of 200-500rmp under the condition of oxygen pressure of 2-3MPa, and filtering and cleaning after the reaction is finished;
(4) and (4) adding the modified embolic cortex powder obtained in the step (3) into a solution containing EDC and NHS, mixing with a solution containing a high molecular compound, crosslinking for 12-24h, filtering, washing and drying after crosslinking is finished, thus obtaining the floating carrier.
Preferably, in the step (4), the polymer compound is selected from one or more of chitosan, hyaluronic acid, cellulose, starch and soy protein, and the concentration of the solution of the polymer compound is 10-20 g/L.
Preferably, in the step (4), the solution of EDC and NHS has a pH of 7.2-7.4, the mass concentration of EDC is 0.5g/L, and the mass concentration of NHS is 2 g/L.
Preferably, in the step (4), the solution of the polymer compound is a mixed solution of chitosan and hyaluronic acid.
Preferably, in the step (4), the mass ratio of the modified embolic powder to the high molecular compound is 10-15: 1-2.
Preferably, in the step (4), the mass ratio of the chitosan to the hyaluronic acid is 1: 1.
The floating carrier obtained by the preparation method.
Has the advantages that: (1) according to the invention, the cork is used as a carrier, the cork is crushed by a crusher to have a certain particle size, and then hydrolysis holes are formed in the cork powder through hydrolysis of ligninase, so that the loading capacity of the carrier is increased; (2) the surface of the embolic powder is aminated and modified by a macromolecular compound, so that the bonding firmness of an active substance and a carrier is improved; (3) the floating carrier of the present invention is completely biodegradable.
Detailed Description
Example 1: step 1: preparation of enzymolysis embolus skin powder
Crushing 100g of cork by a crusher, drying and sieving by a 100-mesh sieve; adding sieved cortex Cinnamomi Japonici powder into 500mL ligninase solution with mass concentration of 10g/L, stirring for 5h under 300rmp, filtering after reaction, washing with distilled water for 3 times, and drying for use.
Step 2: and (2) adding 100g of the dried cork powder prepared in the step (1) into a reaction kettle, reacting for 8 hours at 190 ℃ and under the conditions of the rotating speed of 300rmp and the oxygen pressure of 3MPa, wherein the reaction kettle contains 500mL of ammonia water with the mass concentration of 10%, filtering after the reaction is finished, washing for 3 times by using distilled water, and drying for later use.
And step 3: adding 5g of chitosan with average molecular weight of 15KDa and 5g of hyaluronic acid with average molecular weight of 20KDa into 100mL of acetic acid aqueous solution containing 0.02mol/L to obtain macromolecular compound mixed solution.
And 4, step 4: adding 0.5g EDC and 2g NHS solid into 1000mL of acetic acid-ammonium acetate buffer solution with pH of 7.4, stirring, dissolving to obtain solution with mass concentration of 0.5g/L EDC and mass concentration of 2g/L NHS, adding 100g of the embolic powder prepared in the step 2, slowly dripping 100mL of the macromolecular compound mixed solution prepared in the step 3, crosslinking for 12h, filtering after crosslinking, washing with distilled water for 3 times, and drying at 60 ℃ to obtain the floating carrier.
Example 2: steps 1-4 are the same as example 1, 0.5g EDC and 2g NHS solids by weight are added to 1000mL acetic acid-ammonium acetate buffer solution with pH 7.4, stirred and dissolved to obtain solution with mass concentration of 0.5g/L EDC and 2g/L NHS, then 100g of the embolic powder prepared in step 2 is added, 200mL of the polymer compound mixed solution in step 3 is slowly dropped, cross-linked for 24h, after cross-linking is finished, filtered, washed with distilled water for 3 times, and dried at 60 ℃ to obtain the floating carrier.
Example 3: steps 1-4 are the same as example 1, 0.5g EDC and 2g NHS solid are added into 1000mL acetic acid-ammonium acetate buffer solution with pH 7.4 according to the amount, stirred and dissolved to obtain solution with mass concentration of 0.5g/L EDC and 2g/L NHS, then 100g of the embolic powder prepared in step 2 is added, 67mL of the macromolecular compound mixed solution in step 3 is slowly dripped, crosslinking is carried out for 12-24h, after the crosslinking is finished, filtration is carried out, washing is carried out for 3 times by distilled water, and drying is carried out at 60 ℃ to obtain the floating carrier.
Comparative example 1: the floating carrier is obtained without enzymolysis in the step 1 and the rest steps are the same as the step 1.
Comparative example 2: the floating carrier was obtained in the same manner as in example 1 without ammonification in step 2.
Comparative example 3: step 1 and step 2 were the same as in example 1 to obtain a floating carrier.
And step 3: adding 5g of chitosan with average molecular weight of 15KDa and 5g of hyaluronic acid with average molecular weight of 20KDa into 100mL of acetic acid aqueous solution containing 0.02mol/L to obtain macromolecular compound mixed solution.
And 4, step 4: and (3) mixing 100g of the embolic skin powder prepared in the step 2 with 100mL of the macromolecular compound mixed solution prepared in the step 3, distilling under reduced pressure, and drying at 60 ℃ to obtain the floating carrier.
Application example 1: the floating granules were obtained by replacing the glass floating beads with the floating carriers prepared in examples 1-3 according to the method of example 1 of the applicant's patent 2017101184557. The preparation method comprises the following steps: adsorbing 8 parts by weight of thifluzamide by 8 parts by weight of white carbon black, uniformly mixing with 9 parts by weight of sulfonate lignin, 9 parts by weight of phenyl phenol polyoxyethylene ether and 12 parts by weight of KCl, and performing superfine grinding by using a jet mill to obtain mother powder; uniformly mixing the mother powder with 7.5 parts by weight of mineral oil, 7.5 parts by weight of vegetable oil and the balance of floating carrier, wherein the total weight is 100 parts by weight, transferring the mixture into extrusion granulation equipment for granulation to obtain irregular cylindrical particles, and drying and screening the obtained particles to obtain the finished thifluzamide bactericidal macro-particles with the effective component content of 8%.
Second, measurement method
Water surface diffusion velocity test
(1) Solution and apparatus
Tap water: drinking grade;
a water tank: the length is 120cm, the width is 20cm, and the height is 10 cm; and (3) constant-temperature water bath: (30 + -2) deg.C;
and a stopwatch.
(2) Determination of water surface diffusion velocity
Putting tap water into a water tank with the length multiplied by the width multiplied by the height multiplied by 120cm multiplied by 20cm multiplied by 10cm, wherein the height of a water layer is more than or equal to 2 cm; 20mg of the sample was weighed and placed in the water surface area at the top of the tank to allow self-diffusion, and the time required for the sample to diffuse to just 1m on the water surface was measured using a stopwatch, and the measurements were performed in parallel three times and averaged. Measuring the diffusion speed V (m/min) of the sample on the water surface;
(3) determination of the loss Rate of active ingredient
Since the floating macrogranules only play a role in preventing or treating diseases after reaching the target, and the part of the floating macrogranules which cannot reach the target or near the target for a long time or immediately sinks to the water bottom after application is regarded as a part without effect, the percentage of active substances reaching the diameter range of 8 centimeters of plants and more than 2cm of a water layer after 5 minutes and 10 minutes after application in the total amount of the original active substances is tested in the experiment.
The measurement results are shown in table 1:
as can be seen from examples 1 to 3, the floating carriers of examples 1 to 3 prepared by the present invention have similar diffusion rate and drug release effect to those of the existing carriers, and as can be seen from comparative example 1, the floating carrier without enzymatic hydrolysis has poor diffusion rate and drug release effect. It can be seen from comparative examples 2-3 that the diffusion rate of the floating carrier subjected to enzymatic hydrolysis in the present invention does not change significantly, but the release effect on the drug is poor because the adsorption effect of the floating carrier subjected to surface modification on the drug is increased and the release effect of the prior art is obtained, and the floating carrier prepared by the present invention can be completely biodegraded and is environmentally friendly.
Claims (3)
1. A preparation method of a floating carrier for floating large granules is characterized by comprising the following steps:
(1) pulverizing cortex Corbi by pulverizer, drying, and sieving with 80-100 mesh sieve;
(2) adding the sieved embolic skin powder into a ligninase solution with the mass concentration of 8-10g/L, stirring for 4-5h under the condition of 200-300rmp, filtering and cleaning after the reaction is finished;
(3) adding the embolic skin powder reacted in the step (2) into ammonia water with the mass concentration of 10-15%, reacting for 6-8h at the temperature of 160-200 ℃ and the rotating speed of 200-500rmp under the condition of oxygen pressure of 2-3MPa, and filtering and cleaning after the reaction is finished;
(4) adding the modified embolic skin powder obtained in the step (3) into a solution containing EDC and NHS, mixing with a solution containing a high molecular compound, crosslinking for 12-24h, filtering, washing and drying after crosslinking is finished to obtain a floating carrier; the solution of the high molecular compound is a mixed solution of chitosan and hyaluronic acid; the mass ratio of the chitosan to the hyaluronic acid is 1: 1; the mass ratio of the modified embolic powder to the high molecular compound is 10-15: 1-2.
2. The method for preparing a floating carrier for floating granules according to claim 1, wherein in step (4), the solution of EDC and NHS has a pH of 7.2-7.4, the mass concentration of EDC is 0.5g/L, and the mass concentration of NHS is 2 g/L.
3. A floating carrier obtained by the production method according to any one of claims 1 to 2.
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| CN201910898153.5A CN110692630B (en) | 2019-09-23 | 2019-09-23 | Floating carrier for floating large granules and preparation method thereof |
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| CN201910898153.5A CN110692630B (en) | 2019-09-23 | 2019-09-23 | Floating carrier for floating large granules and preparation method thereof |
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| CN110692630B true CN110692630B (en) | 2021-05-07 |
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| CN115530163B (en) * | 2022-09-22 | 2023-08-08 | 华南农业大学 | Enzyme response nano pesticide and preparation method and application thereof |
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