CN106689150B - A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule - Google Patents
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule Download PDFInfo
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- CN106689150B CN106689150B CN201611000319.XA CN201611000319A CN106689150B CN 106689150 B CN106689150 B CN 106689150B CN 201611000319 A CN201611000319 A CN 201611000319A CN 106689150 B CN106689150 B CN 106689150B
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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
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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
- A01N25/22—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 medicine fertilizer preparation technical fields, and in particular to a kind of using degradable native cellulose ester as the emamectin benzoate urea medicine fertilizer microcapsule preparation method of wall material.A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule includes the following steps: the preparation of the preparation of the water phase containing chemical fertilizer, the preparation of the phase containing medicine oil, the preparation of w/o type colostric fluid, the preparation of outer aqueous phase and cellulose esters emamectin benzoate urea micro-capsule.Cellulose esters emamectin benzoate urea micro-capsule of the invention can reduce the photodegradation rate of emamectin benzoate；It avoids urea from generating biuret in pelletization high temperature, improves the utilization rate of urea；Cellulose esters emamectin benzoate urea micro-capsule of the invention makes chemical fertilizer and pesticide all have slow release effect, and pesticide and fertilizer is made to need slow release according to crop, improves utilization efficiency；Its preparation process is simple, environmental pollution is small.
Description
Technical field
The invention belongs to medicine fertilizer preparation technical fields, and in particular to a kind of using degradable native cellulose ester as wall material
Emamectin benzoate urea medicine fertilizer microcapsule preparation method.
Background technique
Emamectin-benzoate (emamectin benzoate, abbreviation emamectin benzoate) be antibiotics desinsection,
Acaricide, and have at present to beet armyworm, cigarette beetle and bollworm etc. brilliant anti-to the highest insecticide of mythimna separata activity
Effect.The main dosage form of emamectin benzoate is missible oil currently on the market, and missible oil need to expend a large amount of organic solvents when preparing, and easily leads to environment dirt
Dye and the wasting of resources.And emamectin benzoate is light-exposed unstable, easy decomposition failure.
Urea is a kind of high concentration nitrogenous fertilizer, belongs to neutral quick-acting fertilizer, it can also be used to produce a variety of compound fertilizers.In the soil
Any harmful substance is not remained, and chronic administration does not have adverse effect.Animal husbandry can be used as the feed of ruminant.But in granulation
Temperature is excessively high to generate a small amount of biuret, also known as biuret, have inhibiting effect to crop.China provides fertilizer urea biuret
Content should be less than 0.5%.When Biuret Content is more than 1%, seed manure, seed manure and foliar fertilizer cannot be done, the urea of other application phases
Content also excessively or should not be concentrated excessively.
Micro-capsule, which refers to, uses natural or synthesis high molecular material (being referred to as capsule material) as cyst membrane wall shell, by solid-state or liquid
State drug wraps up the Drug Storage type microencapsulation become.Currently, microcapsule formulation is mainly used in the sustained release of drug in field of medicaments.
Using the natural macromolecule modification material fiber element ester of biodegradability as wall material, environmentally friendly medicine fertilizer micro-capsule is prepared, is accorded with
Close research hotspot both domestic and external.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
The present invention, using urea, emamectin benzoate as core material, prepares cellulose esters using solvent evaporation method using cellulose esters as wall material
Emamectin benzoate urea micro-capsule, which has good slow release effect to emamectin benzoate, and water splitting is effectively reduced, and extension is held
The effect of effect phase；Urea is wrapped in micro-capsule, is not easy other than with 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.
The technical solution provided by the present invention is:
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, its step are as follows:
(1) preparation of the water phase containing chemical fertilizer: urea and 15% Arabic gum are uniformly mixed, water phase containing chemical fertilizer is obtained；
(2) preparation of the phase containing medicine oil: emamectin benzoate and cellulose esters are dissolved in chloroform, phase containing medicine oil is obtained；
(3) preparation of w/o type colostric fluid: the phase containing medicine oil that water phase containing chemical fertilizer that step (1) obtains, step (2) are obtained
It is mixed with surfactant, stirs 0.5-2min at revolving speed 1500-3000r/min, obtain w/o type colostric fluid；
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.25-0.5mL organic silicone oil, is uniformly mixed, obtains outer water
Phase；
(5) at room temperature, the mixing speed for controlling 400-800r/min w/o type colostric fluid is added dropwise in outer aqueous phase, room
Temperature is lower to stir 30min, is warming up to 55 DEG C and continues to stir 60min, then filters, gained filter residue is placed at 50 DEG C and is dried in vacuo,
Up to cellulose esters emamectin benzoate urea micro-capsule.
Preferably, the mass ratio of urea and 15% Arabic gum is 1:1-5 in step (1).
Preferably, the mass ratio of emamectin benzoate and cellulose esters is 1:1-5 in step (2).
Preferably, the ratio that the volume that chloroform is added in step (2) is the gross mass of emamectin benzoate and cellulose esters is 5-
10:1.
Preferably, surfactant is the 0-20% of water phase containing chemical fertilizer and the quality of phase containing medicine oil in step (3).
Preferably, the ratio that the quality that 1% poly-vinyl alcohol solution is added in step (4) is organic silicone oil volume is 1:
250-300。
Compared with prior art, the invention has the following beneficial effects:
(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 generates biuret, improves the utilization rate of urea.
(2) cellulose esters emamectin benzoate urea micro-capsule of the invention can discharge chemical fertilizer and pesticide simultaneously, to realize at one stroke
Two effects obtained.
(3) cellulose esters emamectin benzoate urea micro-capsule of the invention obtains chemical fertilizer and pesticide all has slow release effect, makes pesticide
Slow release is needed according to crop with fertilizer, improves utilization efficiency.
(4) cellulose esters emamectin benzoate urea micro-capsule of the invention have biodegradability, its preparation process it is simple, to ring
Border pollution is small.
Specific embodiment
Below with reference to concrete example, the present invention is described in further detail.
Embodiment 1:
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, its step are as follows:
(1) preparation of the water phase containing chemical fertilizer: urea and 15% Arabic gum are uniformly mixed, water phase containing chemical fertilizer is obtained；Urea
Mass ratio with 15% Arabic gum is 1:1；
(2) preparation of the phase containing medicine oil: emamectin benzoate and acetylbutyrylcellulose are dissolved in chloroform, phase containing medicine oil is obtained；
The mass ratio of emamectin benzoate and cellulose esters is 1:1；The volume of chloroform is added as the ratio of the gross mass of emamectin benzoate and cellulose esters
For 5:1；
(3) preparation of w/o type colostric fluid: the phase containing medicine oil that water phase containing chemical fertilizer that step (1) obtains, step (2) are obtained
It is mixed with surfactant, stirs 0.5min at revolving speed 1500r/min, obtain w/o type colostric fluid；Surfactant is added
Quality is the 0% of water phase containing chemical fertilizer and the quality of phase containing medicine oil；
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.25mL organic silicone oil, is uniformly mixed, obtains outer aqueous phase；
It is 1:250 that the quality that 1% poly-vinyl alcohol solution is added, which is the ratio of organic silicone oil volume,；
(5) at room temperature, the mixing speed for controlling 400r/min w/o type colostric fluid is added dropwise in outer aqueous phase, at room temperature
Stir 30min, be warming up to 55 DEG C continue stir 60min, then filter, by gained filter residue be placed at 50 DEG C be dried in vacuo to get
Cellulose esters emamectin benzoate urea micro-capsule.
Embodiment 2:
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, its step are as follows:
(1) preparation of the water phase containing chemical fertilizer: urea and 15% Arabic gum are uniformly mixed, water phase containing chemical fertilizer is obtained；Urea
Mass ratio with 15% Arabic gum is 1:5；
(2) it the preparation of the phase containing medicine oil: by emamectin benzoate and acetic acid lauric acid cellulose dissolution in chloroform, obtains containing medicine oil
Phase；The mass ratio of emamectin benzoate and cellulose esters is 1:5；The volume of chloroform is added as the ratio of the gross mass of emamectin benzoate and cellulose esters
Example is 10:1；
(3) preparation of w/o type colostric fluid: the phase containing medicine oil that water phase containing chemical fertilizer that step (1) obtains, step (2) are obtained
It is mixed with surfactant, stirs 2min at revolving speed 3000r/min, obtain w/o type colostric fluid；The matter of surfactant is added
Amount is the 20% of water phase containing chemical fertilizer and the quality of phase containing medicine oil；
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.5mL organic silicone oil, is uniformly mixed, obtains outer aqueous phase；Add
It is 1:300 that the quality for entering 1% poly-vinyl alcohol solution, which is the ratio of organic silicone oil volume,；
(5) at room temperature, the mixing speed for controlling 800r/min w/o type colostric fluid is added dropwise in outer aqueous phase, at room temperature
Stir 30min, be warming up to 55 DEG C continue stir 60min, then filter, by gained filter residue be placed at 50 DEG C be dried in vacuo to get
Cellulose esters emamectin benzoate urea micro-capsule.
Embodiment 3:
A kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, its step are as follows:
(1) preparation of the water phase containing chemical fertilizer: urea and 15% Arabic gum are uniformly mixed, water phase containing chemical fertilizer is obtained；Urea
Mass ratio with 15% Arabic gum is 1:3；
(2) preparation of the phase containing medicine oil: by emamectin benzoate and laurate cellulose dissolution in chloroform, phase containing medicine oil is obtained；
The mass ratio of emamectin benzoate and cellulose esters is 1:2；The volume of chloroform is added as the ratio of the gross mass of emamectin benzoate and cellulose esters
For 8:1；
(3) preparation of w/o type colostric fluid: the phase containing medicine oil that water phase containing chemical fertilizer that step (1) obtains, step (2) are obtained
It is mixed with surfactant, stirs 1min at revolving speed 2000r/min, obtain w/o type colostric fluid；The matter of surfactant is added
Amount is the 10% of water phase containing chemical fertilizer and the quality of phase containing medicine oil；
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.4mL organic silicone oil, is uniformly mixed, obtains outer aqueous phase；Add
It is 1:280 that the quality for entering 1% poly-vinyl alcohol solution, which is the ratio of organic silicone oil volume,；
(5) at room temperature, the mixing speed for controlling 600r/min w/o type colostric fluid is added dropwise in outer aqueous phase, at room temperature
Stir 30min, be warming up to 55 DEG C continue stir 60min, then filter, by gained filter residue be placed at 50 DEG C be dried in vacuo to get
Cellulose esters emamectin benzoate urea micro-capsule.
Cellulose esters emamectin benzoate urea micro-capsule will be obtained in embodiment 1-3, to the embedding rate of emamectin benzoate in micro-capsule and urea
It is measured, see Table 1 for details.
The performance measurement of cellulose esters emamectin benzoate urea micro-capsule is prepared using method of the invention for table 1
As shown in Table 1, the embedding of cellulose esters emamectin benzoate urea micro-capsule emamectin benzoate is prepared using method of the invention
Rate is 90% or more, and the embedding rate of urea is 75% or more, it is seen then that cellulose esters first dimension is prepared in method of the invention
Salt urea micro-capsule it is functional.
The aforementioned description to specific exemplary embodiment of the invention is 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 the above instruction, can much be changed
And variation.The purpose of selecting and describing the exemplary embodiment is that explaining specific principle of the invention and its actually answering
With so that those skilled in the art can be realized and utilize a variety of different exemplary implementation schemes of the invention and
Various chooses and changes.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (3)
1. a kind of preparation method of cellulose esters emamectin benzoate urea micro-capsule, which is characterized in that its step are as follows:
(1) preparation of the water phase containing chemical fertilizer: urea and 15% Arabic gum are uniformly mixed, water phase containing chemical fertilizer is obtained；
(2) preparation of the phase containing medicine oil: emamectin benzoate and cellulose esters are dissolved in chloroform, phase containing medicine oil is obtained；
(3) preparation of w/o type colostric fluid: the phase containing medicine oil and table that water phase containing chemical fertilizer that step (1) obtains, step (2) are obtained
The mixing of face activating agent, stirs 0.5-2min at revolving speed 1500-3000r/min, obtains w/o type colostric fluid；
(4) 1% poly-vinyl alcohol solution is taken, is added into 0.25-0.5mL organic silicone oil, is uniformly mixed, obtains outer aqueous phase；
(5) at room temperature, the mixing speed for controlling 400-800r/min w/o type colostric fluid is added dropwise in outer aqueous phase, at room temperature
Stir 30min, be warming up to 55 DEG C continue stir 60min, then filter, by gained filter residue be placed at 50 DEG C be dried in vacuo to get
Cellulose esters emamectin benzoate urea micro-capsule；
The mass ratio of urea and 15% Arabic gum is 1:1-5 in step (1)；
The mass ratio of emamectin benzoate and cellulose esters is 1:1-5 in step (2)；
It is 5-10:1 that the volume of addition chloroform, which is the ratio of the gross mass of emamectin benzoate and cellulose esters, in step (2).
2. the preparation method of cellulose esters emamectin benzoate urea micro-capsule according to claim 1, which is characterized in that step (3)
Middle surfactant is the 0-20% of water phase containing chemical fertilizer and the quality of phase containing medicine oil.
3. the preparation method of cellulose esters emamectin benzoate urea micro-capsule according to claim 1, which is characterized in that step (4)
The middle quality that 1% poly-vinyl alcohol solution is added is that 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 |
|---|
| 国内功能性肥料—药肥的生产方法;冯德学等;《磷肥与复肥》;20161015;第31卷(第10期);第16-18页 |
| 浅谈溶剂蒸发法制备微胶囊与农药微胶囊的开发;冯建国等;《农药学学报》;20111231;第13卷(第6期);第568-575页 |
| 溶剂挥发法制备甲氨基阿维菌素苯甲酸盐微球;郑海瑛等;《农药学学报》;20121231;第14卷(第5期);第557-564页 |
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