CN106689150A - Method for preparing cellulose ester emamectin benzoate urea micro-capsules - Google Patents
Method for preparing cellulose ester emamectin benzoate urea micro-capsules Download PDFInfo
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- CN106689150A CN106689150A CN201611000319.XA CN201611000319A CN106689150A CN 106689150 A CN106689150 A CN 106689150A CN 201611000319 A CN201611000319 A CN 201611000319A CN 106689150 A CN106689150 A CN 106689150A
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- emamectin benzoate
- urea
- cellulose esters
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- 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
- A01N25/22—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 ingredients stabilising the active ingredients
-
- 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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C9/00—Fertilisers containing urea or urea compounds
-
- 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
- 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
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
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- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Plant Pathology (AREA)
- Agronomy & Crop Science (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Soil Sciences (AREA)
- Fertilizers (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of pesticide and fertilizer preparation and particularly relates to a method for preparing cellulose ester emamectin benzoate urea micro-capsules by taking degradable natural cellulose ester as a wall material. The method for preparing the cellulose ester emamectin benzoate urea micro-capsules comprises the steps of preparing a fertilizer-containing aqueous phase, preparing a pesticide-containing oil phase, preparing w/o type primary emulsion, preparing an external water phase and preparing the cellulose ester emamectin benzoate urea micro-capsules. The cellulose ester emamectin benzoate urea micro-capsules can reduce photodegradation rate of emamectin benzoate; the generation of biuret caused by high temperature of urea in the pelletizing process is avoided, and the urea usage rate is improved. The cellulose ester emamectin benzoate urea micro-capsules make the fertilizer and the pesticide have a slow-release effect, the pesticide and the fertilizer are released slowly according to crop requirements, and the utilization efficiency is improved. The preparation process is simple, and the environmental pollution is small.
Description
Technical field
The invention belongs to medicine fertilizer preparing technical field, and in particular to a kind of with degradable native cellulose ester as wall material
Emamectin benzoate urea medicine fertilizer microcapsule preparation method.
Background technology
Emamectin-benzoate (emamectin benzoate, abbreviation emamectin benzoate) be antibioticses desinsection,
Acaricide, is also at present, to mythimna separata activity highest insecticide, have to beet armyworm, cigarette beetle and bollworm etc. remarkable anti-
Effect.The main formulation of emamectin benzoate is missible oil in the market, and missible oil need to expend a large amount of organic solvents when preparing, and be easily caused environment dirty
Dye and the wasting of resources.And emamectin benzoate is shown in photo-labile, easy decomposition failure.
Urea is a kind of high concentration nitrogenous fertilizer, the neutral quick-acting fertilizer of category, it can also be used to produce various compound fertilizers.In soil
Any harmful substance is not remained, and chronic administration does not have harmful effect.Animal husbandry can be used as the feed of ruminant.But in granulation
Temperature is too high to produce a small amount of biuret, also known as biuret, have inhibitory action to crop.China specifies fertilizer urea biuret
Content should be less than 0.5%.When Biuret Content is more than 1%, it is impossible to do seed manure, seed manure and foliar fertilizer, other apply the urea of phase
Content should not also be concentrated excessively or excessively.
Micro-capsule refers to as cyst membrane wall shell, by solid-state or liquid with natural or synthesis macromolecular material (being referred to as capsule material)
The Drug Storage type microencapsulation that state medicine parcel turns into.At present, microcapsule formulation is mainly used in the sustained release of medicine in field of medicaments.
Natural macromolecule modification material fiber element ester using biodegradability prepares environmentally friendly medicine fertilizer micro-capsule, symbol as wall material
Close study hotspot both domestic and external.
The information for being disclosed in the background section is merely intended to increase the understanding to general background of the invention, without answering
In being considered as recognizing or imply in any form that the information structure has been the prior art well known to persons skilled in the art.
The content of the invention
The present invention, with urea, emamectin benzoate as core, cellulose esters is prepared using solvent evaporation method with cellulose esters as wall material
Emamectin benzoate urea micro-capsule, the microcapsule formulation has good slow release effect to emamectin benzoate, and effectively reduces water splitting, and extension is held
The effect of effect phase;Urea is wrapped in micro-capsule, is difficult in addition to slow releasing function, in application with soil erosion, loss
It is few, improve fertilising rate;The degradation characteristic of native cellulose ester is more suitable for the release of field soil environment, to environment no pressure.
Technical scheme provided by the present invention is:
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, its step is as follows:
(1) preparation of the phase of water containing chemical fertilizer:Urea and 15% Arabic gum are well mixed, the phase of water containing chemical fertilizer is obtained;
(2) preparation of pastille oil phase:Emamectin benzoate and cellulose esters are dissolved in chloroform, pastille oil phase is obtained;
(3) preparation of w/o types colostric fluid:The pastille oil phase that the phase of water containing chemical fertilizer that step (1) is obtained, step (2) are obtained
With surfactant mixing, 0.5-2min is stirred under rotating speed 1500-3000r/min, obtain w/o type colostric fluids;
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.25-0.5mL organic silicone oils, be well mixed, obtain outer water
Phase;
(5) at room temperature, the mixing speed of 400-800r/min is controlled, w/o type colostric fluids is added dropwise in outer water phase, room
The lower stirring 30min of temperature, is warming up to 55 DEG C and continues to stir 60min, and then suction filtration, is vacuum dried at gained filter residue is placed in into 50 DEG C,
Obtain final product cellulose esters emamectin benzoate urea micro-capsule.
Preferably, the mass ratio of urea and 15% Arabic gum is 1 in step (1):1-5.
Preferably, the mass ratio of emamectin benzoate and cellulose esters is 1 in step (2):1-5.
Preferably, adding the volume of chloroform in step (2) for the ratio of emamectin benzoate and the gross mass of cellulose esters is 5-
10:1.
Preferably, surfactant is the 0-20% of the phase of water containing chemical fertilizer and pastille oil phase quality in step (3).
Preferably, adding the quality of 1% poly-vinyl alcohol solution in step (4) for the ratio of organic silicone oil volume is 1:
250-300。
Compared with prior art, the present invention has the advantages that:
(1) cellulose esters emamectin benzoate urea micro-capsule of the invention can reduce the photodegradation rate of emamectin benzoate;Urea is avoided to exist
Pelletization high temperature produces biuret, improves the utilization rate of urea.
(2) cellulose esters emamectin benzoate urea micro-capsule of the invention can simultaneously discharge chemical fertilizer and agricultural chemicals, so as to realize at one stroke
Two effects for obtaining.
(3) cellulose esters emamectin benzoate urea micro-capsule of the invention obtains chemical fertilizer and agricultural chemicals is respectively provided with slow release effect, makes agricultural chemicals
Slow release is needed according to crop with fertilizer, utilization ratio is improved.
(4) cellulose esters emamectin benzoate urea micro-capsule of the invention there is biodegradability, its preparation process is simple, to ring
Border pollution is small.
Specific embodiment
With reference to concrete example, the present invention is further detailed explanation.
Embodiment 1:
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, its step is as follows:
(1) preparation of the phase of water containing chemical fertilizer:Urea and 15% Arabic gum are well mixed, the phase of water containing chemical fertilizer is obtained;Urea
It is 1 with the mass ratio of 15% Arabic gum:1;
(2) preparation of pastille oil phase:Emamectin benzoate and acetylbutyrylcellulose are dissolved in chloroform, pastille oil phase is obtained;
The mass ratio of emamectin benzoate and cellulose esters is 1:1;It is emamectin benzoate and the ratio of the gross mass of cellulose esters to add the volume of chloroform
It is 5:1;
(3) preparation of w/o types colostric fluid:The pastille oil phase that the phase of water containing chemical fertilizer that step (1) is obtained, step (2) are obtained
With surfactant mixing, 0.5min is stirred under rotating speed 1500r/min, obtain w/o type colostric fluids;Add surfactant
Quality is the 0% of the phase of water containing chemical fertilizer and pastille oil phase quality;
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.25mL organic silicone oils, be well mixed, obtain outer water phase;
It is 1 for the ratio of organic silicone oil volume to add the quality of 1% poly-vinyl alcohol solution:250;
(5) at room temperature, the mixing speed of 400r/min is controlled, w/o type colostric fluids is added dropwise in outer water phase, at room temperature
Stirring 30min, is warming up to 55 DEG C and continues to stir 60min, and then suction filtration, is vacuum dried at gained filter residue is placed in into 50 DEG C, obtains final product
Cellulose esters emamectin benzoate urea micro-capsule.
Embodiment 2:
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, its step is as follows:
(1) preparation of the phase of water containing chemical fertilizer:Urea and 15% Arabic gum are well mixed, the phase of water containing chemical fertilizer is obtained;Urea
It is 1 with the mass ratio of 15% Arabic gum:5;
(2) preparation of pastille oil phase:By emamectin benzoate and acetic acid laurate cellulose dissolution in chloroform, obtain containing medicine oil
Phase;The mass ratio of emamectin benzoate and cellulose esters is 1:5;It is emamectin benzoate and the ratio of the gross mass of cellulose esters to add the volume of chloroform
Example is 10:1;
(3) preparation of w/o types colostric fluid:The pastille oil phase that the phase of water containing chemical fertilizer that step (1) is obtained, step (2) are obtained
With surfactant mixing, 2min is stirred under rotating speed 3000r/min, obtain w/o type colostric fluids;Add the matter of surfactant
Amount is the 20% of the phase of water containing chemical fertilizer and pastille oil phase quality;
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.5mL organic silicone oils, be well mixed, obtain outer water phase;Plus
Enter the quality of 1% poly-vinyl alcohol solution for the ratio of organic silicone oil volume is 1:300;
(5) at room temperature, the mixing speed of 800r/min is controlled, w/o type colostric fluids is added dropwise in outer water phase, at room temperature
Stirring 30min, is warming up to 55 DEG C and continues to stir 60min, and then suction filtration, is vacuum dried at gained filter residue is placed in into 50 DEG C, obtains final product
Cellulose esters emamectin benzoate urea micro-capsule.
Embodiment 3:
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, its step is as follows:
(1) preparation of the phase of water containing chemical fertilizer:Urea and 15% Arabic gum are well mixed, the phase of water containing chemical fertilizer is obtained;Urea
It is 1 with the mass ratio of 15% Arabic gum:3;
(2) preparation of pastille oil phase:By emamectin benzoate and laurate cellulose dissolution in chloroform, pastille oil phase is obtained;
The mass ratio of emamectin benzoate and cellulose esters is 1:2;It is emamectin benzoate and the ratio of the gross mass of cellulose esters to add the volume of chloroform
It is 8:1;
(3) preparation of w/o types colostric fluid:The pastille oil phase that the phase of water containing chemical fertilizer that step (1) is obtained, step (2) are obtained
With surfactant mixing, 1min is stirred under rotating speed 2000r/min, obtain w/o type colostric fluids;Add the matter of surfactant
Amount is the 10% of the phase of water containing chemical fertilizer and pastille oil phase quality;
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.4mL organic silicone oils, be well mixed, obtain outer water phase;Plus
Enter the quality of 1% poly-vinyl alcohol solution for the ratio of organic silicone oil volume is 1:280;
(5) at room temperature, the mixing speed of 600r/min is controlled, w/o type colostric fluids is added dropwise in outer water phase, at room temperature
Stirring 30min, is warming up to 55 DEG C and continues to stir 60min, and then suction filtration, is vacuum dried at gained filter residue is placed in into 50 DEG C, obtains final product
Cellulose esters emamectin benzoate urea micro-capsule.
Cellulose esters emamectin benzoate urea micro-capsule will be obtained in embodiment 1-3, to emamectin benzoate in micro-capsule and the embedding rate of urea
It is measured, refers to table 1.
Table 1 prepares the performance measurement of cellulose esters emamectin benzoate urea micro-capsule using the method for the present invention
As shown in Table 1, the embedding of cellulose esters emamectin benzoate urea micro-capsule emamectin benzoate is prepared using the method for the present invention
More than 90%, the embedding rate of urea is more than 75% for rate, it is seen then that the method for the present invention prepares cellulose esters first dimension
Salt urea micro-capsule it is functional.
The foregoing description to specific illustrative embodiment of the invention be in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to above-mentioned teaching, can be much changed
And change.The purpose of selecting and describing the exemplary embodiment is that explaining that certain principles of the invention and its reality should
With so that those skilled in the art can realize and using a variety of exemplaries of the invention and
A variety of selections and change.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (6)
1. a kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, it is characterised in that its step is as follows:
(1) preparation of the phase of water containing chemical fertilizer:Urea and 15% Arabic gum are well mixed, the phase of water containing chemical fertilizer is obtained;
(2) preparation of pastille oil phase:Emamectin benzoate and cellulose esters are dissolved in chloroform, pastille oil phase is obtained;
(3) preparation of w/o types colostric fluid:Pastille oil phase and table that the phase of water containing chemical fertilizer that step (1) is obtained, step (2) are obtained
Face activating agent mixing, 0.5-2min is stirred under rotating speed 1500-3000r/min, obtains w/o type colostric fluids;
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.25-0.5mL organic silicone oils, be well mixed, obtain outer water phase;
(5) at room temperature, the mixing speed of 400-800r/min is controlled, w/o type colostric fluids is added dropwise in outer water phase, at room temperature
Stirring 30min, is warming up to 55 DEG C and continues to stir 60min, and then suction filtration, is vacuum dried at gained filter residue is placed in into 50 DEG C, obtains final product
Cellulose esters emamectin benzoate urea micro-capsule.
2. the preparation method of cellulose esters emamectin benzoate urea micro-capsule according to claim 1, it is characterised in that step (1)
The mass ratio of middle urea and 15% Arabic gum is 1:1-5.
3. the preparation method of cellulose esters emamectin benzoate urea micro-capsule according to claim 1, it is characterised in that step (2)
The mass ratio of middle emamectin benzoate and cellulose esters is 1:1-5.
4. the preparation method of cellulose esters emamectin benzoate urea micro-capsule according to claim 1, it is characterised in that step (2)
The middle volume for adding chloroform is for the ratio of emamectin benzoate and the gross mass of cellulose esters is 5-10:1.
5. the preparation method of cellulose esters emamectin benzoate urea micro-capsule according to claim 1, it is characterised in that step (3)
Middle surfactant is the 0-20% of the phase of water containing chemical fertilizer and pastille oil phase quality.
6. the preparation method of cellulose esters emamectin benzoate urea micro-capsule according to claim 1, it is characterised in that step (4)
The middle quality for adding 1% poly-vinyl alcohol solution is for the ratio of organic silicone oil volume is 1:250-300.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2000048465A1 (en) * | 1999-02-19 | 2000-08-24 | Thies Technology | Pest controlling |
CN102696640A (en) * | 2012-06-15 | 2012-10-03 | 福建农林大学 | Emamectin benzoate polylactic acid microsphere suspension and preparation method thereof |
CN103798232A (en) * | 2012-11-14 | 2014-05-21 | 中国农业科学院植物保护研究所 | Emamectin benzoate microsphere and preparation method thereof |
CN104886091A (en) * | 2015-06-30 | 2015-09-09 | 福建农林大学 | Biodegradable emamectin benzoate microsphere |
-
2016
- 2016-11-14 CN CN201611000319.XA patent/CN106689150B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2000048465A1 (en) * | 1999-02-19 | 2000-08-24 | Thies Technology | Pest controlling |
CN102696640A (en) * | 2012-06-15 | 2012-10-03 | 福建农林大学 | Emamectin benzoate polylactic acid microsphere suspension and preparation method thereof |
CN103798232A (en) * | 2012-11-14 | 2014-05-21 | 中国农业科学院植物保护研究所 | Emamectin benzoate microsphere and preparation method thereof |
CN104886091A (en) * | 2015-06-30 | 2015-09-09 | 福建农林大学 | Biodegradable emamectin benzoate microsphere |
Non-Patent Citations (3)
Title |
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冯建国等: "浅谈溶剂蒸发法制备微胶囊与农药微胶囊的开发", 《农药学学报》 * |
冯德学等: "国内功能性肥料—药肥的生产方法", 《磷肥与复肥》 * |
郑海瑛等: "溶剂挥发法制备甲氨基阿维菌素苯甲酸盐微球", 《农药学学报》 * |
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