KR20040069831A - Preparation Method for Microcapsule Insecticides - Google Patents
Preparation Method for Microcapsule Insecticides Download PDFInfo
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- KR20040069831A KR20040069831A KR1020030006379A KR20030006379A KR20040069831A KR 20040069831 A KR20040069831 A KR 20040069831A KR 1020030006379 A KR1020030006379 A KR 1020030006379A KR 20030006379 A KR20030006379 A KR 20030006379A KR 20040069831 A KR20040069831 A KR 20040069831A
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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
- A01N25/26—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
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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
- 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
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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
- A01N53/00—Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
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Abstract
Description
본 발명은 마이크로캡슐 살충제의 제조방법 및 동 방법에 의해 제조한 마이크로캡슐 살충제에 대한 것이다.The present invention relates to a method for producing a microcapsule insecticide and a microcapsule insecticide prepared by the same method.
일반적으로 캡슐이란 천연 고분자 또는 합성 고분자를 원료로 하는 미소한 용기를 의미하며, 보통 크기에 따라 나노캡슐, 마이크로캡슐, 알갱이(bead)로 나뉘어져 부르고 있다. 캡슐은 보호하고자 하는 물질을 주위로부터 보호하는 것을 주된 역할을 한다. 또한 캡슐은 고농도, 고활성 물질에 대하여 농도 및 활성을 일정하게 하며 요구되는 조건에서 서서히 방출시킬 수도 있는 막 투과 제어기능을 할 수 있어서 이러한 기능을 이용하여 휘발성 물질의 장기보관, 맛과 냄새의 마스킹(masking)도 시킬 수 있고, 내부 물질의 방출제어 기능이 있으므로 물질의독성을 감소시킬 수도 있다. 따라서 이와 같은 여러 가지 장점을 가지는 캡슐은 산업계의 기술 개발에 미치는 바가 크며, 특히 내용물의 대상물질이 화학물질 뿐만 아니라 생명체나 미 생명체에 대해서도 가능하다. 즉 살아있는 세포나 조직, 유산균등에도 적용되어서 생명공학 분야에서는 눈부신 고도의 기술을 시도하고 있다.In general, a capsule refers to a small container made of a natural polymer or a synthetic polymer as a raw material, and is generally divided into nanocapsules, microcapsules, and beads according to sizes. Capsules play a major role in protecting the material to be protected from the environment. In addition, the capsule can control the permeability of the membrane to maintain a constant concentration and activity for high concentrations and highly active substances, and may be released slowly under the required conditions. It can also mask and reduce the toxicity of the material, as it has a controlled release of the internal material. Therefore, the capsule having such various advantages has a great impact on the development of technology in the industry, and particularly the target substance of the contents is possible not only for chemical substances but also for living or non-living organisms. In other words, it is applied to living cells, tissues, lactic acid bacteria, etc., and is attempting a dazzling high technology in biotechnology.
캡슐을 제조하는 방법에는 계면중합법, In-Situ 중합법, 분무캡슐중합법, 다중에멀전중합법, 유화-확산 중합법등이 있다.Methods for preparing capsules include interfacial polymerization, in-situ polymerization, spray capsule polymerization, multi-emulsion polymerization, emulsion-diffusion polymerization, and the like.
살충제는 사람에게 해로운 벌레나 곤충을 없애는 것으로서 이러한 살충제는 현재 에어로졸 형태, 플라스틱 캡 안에 적당한 먹이와 살충제를 배합한 독먹이법 형태, 그리고 조그마한 캔에 살충제를 넣고 연막에 의해 살충효과를 나타내는 훈연법 형태 등이 있다.Insecticides are used to eliminate harmful bees and insects that are harmful to humans. These insecticides are currently in aerosol form, poisonous form with proper food and pesticides in a plastic cap, and smoked form with insecticides in small cans and smoked by smoke. Etc.
그러나 상기와 같은 살충제는 적용할 수 있는 범위가 한정되고, 한 번 살포 후 약효의 지속성이 오래 가지 않으며, 살포시 유해한 유기용매의 불쾌한 냄새로 인하여 불편한 점이 많은 문제가 있다.However, the pesticides as described above are limited to the range that can be applied, there is a problem that there is a lot of inconvenience due to the unpleasant smell of harmful organic solvent during spraying does not last long after the spraying.
본 발명은 상기한 종래 기술의 문제점을 해결하기 위해 제안된 것으로써, 본 발명은 캡슐 제조시에 섞이지 않는 두 상(O/W)을 강제 유화시킨 후 농도 차에 의해 활성물질과 함께 섞여 있던 액이 수상으로 분산되어 고분자 캡슐이 형성되는 유화-확산 중합법을 이용하여 마이크로캡슐 살충제의 제조방법 제공을 목적으로 한다.The present invention has been proposed to solve the above problems of the prior art, the present invention is a liquid mixed with the active material by the concentration difference after the forced emulsification of the two phases (O / W) that is not mixed at the time of capsule preparation An object of the present invention is to provide a method for producing a microcapsule insecticide by using an emulsion-diffusion polymerization method in which a water-dispersed polymer capsule is dispersed in the aqueous phase.
본 발명에 의한 마이크로캡슐 살충제의 제조방법에 의한 마이크로캡슐 살충제는 살충제오일의 유해하고, 불쾌한 냄새를 마스킹 하면서 약효의 효과가 오래 지속되도록 할 수 있다. 또한 생분해성 고분자를 캡슐화제로 사용하고, 물을 용매로 사용하기 때문에 환경 친화적인 살충제 캡슐을 제조할 수 있어 환경문제 해결에도 일조할 수 있다. 한편 일반적으로 살충제로서 사용의 폭이 한정되었던 에어로졸 형태, 매트 형태, 독먹이법 형태 그리고 훈연법 형태의 단점을 보완하여 그 응용 범위를 확대시킬 수 있는 마이크로캡슐 살충제를 제조할 수 있다.The microcapsule insecticide according to the method for preparing a microcapsule insecticide according to the present invention may allow a long-lasting effect of the drug while masking harmful and unpleasant odors of the pesticide oil. In addition, since the biodegradable polymer is used as the encapsulating agent, and water is used as the solvent, an environmentally friendly insecticide capsule can be prepared, which can help solve environmental problems. Meanwhile, microcapsule insecticides can be prepared to supplement the disadvantages of aerosol form, mat form, poisoning form, and fume form, which have generally been used as a pesticide, to extend the application range.
도 1은 본 발명의 마이크로캡슐 살충제를 나타낸 사진이다.1 is a photograph showing a microcapsule insecticide of the present invention.
본 발명은 유화-확산법을 이용하여 마이크로캡슐 살충제를 제조한다. 본 발명에서 유화-확산법을 이용하여 마이크로캡슐 살충제를 제조하는 이유는 생체에 무해에 용매의 사용으로 인체에 해가 거의 없으며, 마이크로 크기의 미세캡슐을 제조할 수 있기 때문이다.The present invention uses the emulsion-diffusion method to prepare a microcapsule insecticide. The reason for producing the microcapsule insecticide using the emulsion-diffusion method in the present invention is that it is almost harmless to the human body by using a solvent, which is harmless to a living body, and can produce microcapsules having a micro size.
이러한 유화-확산법은 생분해성 고분자 또는 약제를 함유한 용매상과 안정화제를 함유한 수상이 상호 포화 후 열역학적으로 안정한 상태에 있다가 교반에 의해 용매상은 연속상인 수상에 액적의 형태로 평형을 이룬다. 이 때 안정화제는 새로 생성된 계면의 액적에 흡착하며 용매가 자발적으로 물에 유화하지 못하기 때문에 교반이 필수적이다. 용매가 물에 완전히 녹을 수 있을 만큼의 충분한 양의 물을 첨가하면 열역학적 불안정에 의해 용매가 수상으로 확산되며 용질의 이동에 의해 마이크로 크기의 미세 캡슐을 제조할 수 있다.In this emulsion-diffusion method, a solvent phase containing a biodegradable polymer or drug and a water phase containing a stabilizer are in a thermodynamically stable state after mutual saturation, and by stirring, the solvent phase equilibrates in the form of droplets to the continuous water phase. At this time, the stabilizing agent is adsorbed on the droplets of the newly formed interface and stirring is essential because the solvent does not spontaneously emulsify in water. Adding a sufficient amount of water so that the solvent is completely soluble in water causes the solvent to diffuse into the aqueous phase due to thermodynamic instability and to produce micro-sized microcapsules by solute migration.
상기에서 언급한 유화-확산법을 이용한 본 발명의 마이크로캡슐 살충제의 제조방법은The preparation method of the microcapsule insecticide of the present invention using the above-mentioned emulsion-diffusion method
생분해성 고분자 0.1∼1.0 중량부를 용매 10∼20 중량부에 용해시키는 단계와,Dissolving 0.1 to 1.0 parts by weight of the biodegradable polymer in 10 to 20 parts by weight of the solvent,
전기의 생분해성 고분자가 용해된 용해액에 살충성물질 0.001∼0.01 중량부를 혼합하는 단계와,Mixing 0.001 to 0.01 parts by weight of an insecticidal substance in a solution in which the biodegradable polymer is dissolved;
전기의 생분해성 고분자, 용매 및 살충성물질의 혼합용액을 안정화제 0.5∼5 중량부가 용해되어 있는 수용액 20∼30 중량부에 포화시키는 단계와,Saturating the mixed solution of the biodegradable polymer, the solvent, and the insecticidal substance in an amount of 20 to 30 parts by weight of an aqueous solution in which 0.5 to 5 parts by weight of a stabilizer is dissolved;
전기의 포화용액을 유화시키는 단계와,Emulsifying the saturated solution of electricity,
전기의 유화된 포화용액에 물 43.99∼69.399 중량부를 첨가하여 용매를 수상으로 확산시킨 후 용매를 제거하는 단계를 포함한다.43.99 to 69.399 parts by weight of water is added to the emulsified saturated solution, and the solvent is diffused into an aqueous phase and then the solvent is removed.
본 발명에서 생분해성 고분자, 용매, 살충성물질, 안정화제에 대하여 다양한 사용량으로 마이크로캡슐 살충제를 제조시 생분해성 고분자 0.1∼1.0 중량부, 용매 10∼20 중량부, 살충성물질 0.001∼0.01 중량부, 안정화제 0.5∼5 중량부를 사용시 최적의 마이크로캡슐 살충제를 제조할 수 있다.In the present invention, when preparing microcapsule insecticides in various amounts with respect to biodegradable polymers, solvents, insecticides, and stabilizers, 0.1 to 1.0 parts by weight of biodegradable polymers, 10 to 20 parts by weight of solvents, and 0.001 to 0.01 parts by weight of pesticides When using 0.5 to 5 parts by weight of stabilizer, an optimal microcapsule insecticide can be prepared.
상기에서 생분해성 고분자는 본 발명의 마이크로캡슐 살충제에 있어서, 캡슐화제의 역할을 하는 것으로서 물에 부분적으로 용해하는 분해성이 있는 고분자를 사용할 수 있다. 이러한 생분해성 고분자의 일예로서 본 발명에서는 폴리카프로락톤(polycaprolactone, PCL), 폴리락틱에시드(polylactic acid, PLA), 또는 폴리글리콜라이드(polyglycollide, PGA) 중에서 선택된 어느 하나를 사용한다.In the biodegradable polymer as described above, in the microcapsule insecticide of the present invention, a degradable polymer partially dissolved in water may be used as the encapsulating agent. As one example of such a biodegradable polymer, the present invention uses any one selected from polycaprolactone (PCL), polylactic acid (PLA), or polyglycollide (PGA).
본 발명에서 생분해성 고분자를 용해시키는 용매는 인체에 해가 없으며, 화학적 및 물리적으로 안정하고, 물에 부분적으로 용해되며, 고분자에 대해서 용해도가 큰 용매이면 어떠한 것이라도 사용할 수 있다. 본 발명에서 이러한 용매로 프로필렌카보네이트(propylene carbonate, PC), 에틸아세테이트(ethyl acetate, EA), 메틸렌클로라이드(methylene chloride, MC) 중에서 선택된 어느 하나를 사용한다. 전기의 용매중 프로필렌카보네이트는 물 1g당 약 0.25ml, 에틸아세테이트는 물 1g당 약 0.1ml, 메틸렌클로라이드는 물 1g당 약 0.5ml가 용해된다.The solvent for dissolving the biodegradable polymer in the present invention may be any solvent as long as it is harmless to the human body, chemically and physically stable, partially soluble in water, and high in solubility with respect to the polymer. In the present invention, any one selected from propylene carbonate (PC), ethyl acetate (EA), and methylene chloride (MC) is used as the solvent. In the former solvent, about 0.25 ml of propylene carbonate per 1 g of water, about 0.1 ml of ethyl acetate per 1 g of water, and about 0.5 ml of methylene chloride per 1 g of water are dissolved.
본 발명에서 살충제물질은 오일(oil) 형태의 피레스로이드계 살충물질 보다 상세하게는 퍼메쓰린(permethrin), 델타메쓰린(deltamethrin), 사이퍼메쓰린 (cypermethrin) 중에서 선택된 어느 하나를 사용할 수 있다.In the present invention, the pesticide material may be any one selected from permethrin, permethrin, deltamethrin, and cypermethrin.
생분해성 고분자와 살충성물질의 안정성을 위해 사용하는 안정화제는 폴리옥시에틸렌 소르비탄 모노라우레이트(Polyoxyethylene sorbitan monolaurate), 플루오닉에프-68(pluronic F-68), 소듐라우릴설페이트(Sodium Lauryl Sulfate, CH3(CH2)10CH2OSO3Na), 오디움 도데실 디페닐오삭이드 디설포네이트(odium dodecyl diphenyloxide disulfonate), 폴리비닐알코올(polyvinyl alcohol, PVA) 중에서 선택된 어느 하나를 수용액에 용해된 형태로 사용한다.Stabilizers used to stabilize biodegradable polymers and pesticides include polyoxyethylene sorbitan monolaurate, fluoric F-68 and sodium lauryl sulfate , Any one selected from CH 3 (CH 2 ) 10 CH 2 OSO 3 Na), sodium dodecyl diphenyloxide disulfonate, and polyvinyl alcohol (PVA) in an aqueous solution Use in the form of.
상기에서 생분해성 고분자, 용매 및 살충성물질의 혼합용액을 안정화제가 용해되어 있는 수용액에 포화시킨 후 이 포화용액을 균질화기로 교반하여 유화시킨다. 균질화기는 용매가 물에 유화하기 않기 때문에 포화 수용액을 강제적으로 교반시킴으로써 포화용액을 유화시키기 위해 사용한다. 이때 균질화기에 의한 유화단계는 5분∼15분 동안 3000∼20000rpm의 교반속도로 유화시킨다. 균질화기의 교반속도가 3000rpm 미만이면 충분한 유화가 이루어지지 않고, 20000rpm을 초과하면 미세입자간에 응집이 발생할 수 있는 문제가 있어 유화시 교반속도는 3000∼20000rpm이 바람직하다.The saturated solution of the biodegradable polymer, the solvent and the insecticide is saturated in an aqueous solution in which the stabilizer is dissolved, and then the saturated solution is stirred with a homogenizer and emulsified. The homogenizer is used to emulsify the saturated solution by forcibly stirring the saturated aqueous solution because the solvent is not emulsified in water. At this time, the emulsifying step by the homogenizer is emulsified at a stirring speed of 3000 to 20000 rpm for 5 to 15 minutes. If the agitation speed of the homogenizer is less than 3000rpm, sufficient emulsification is not achieved. If the agitation speed exceeds 20000rpm, there is a problem that aggregation may occur between fine particles. The stirring speed during emulsification is preferably 3000-20000rpm.
전기의 유화단계를 거친 유화용액은 과량의 물을 첨가하여 용매를 수상으로 확산시킨다. 첨가하는 물의 양은 용매의 중량에 대해 3∼4배의 물을 첨가하고, 물의 온도는 20∼60℃가 바람직하다. 용매를 확산시키기 위해 첨가하는 물의 온도가 20℃ 미만이면 용매가 수상으로 확산되는 속도가 늦어 살충제 제조시간이 오래 소요되며, 물의 온도가 60℃ 초과하면 용매가 수상으로의 확산속도에 대한 차이가 없이 물의 온도를 올리는데 비용이 소요되므로 용매를 수상으로 확산시키기 위해 사용하는 물의 온도는 20∼60℃가 바람직하다.The emulsion solution, which has undergone the previous emulsification step, is added with excess water to diffuse the solvent into the water phase. As for the quantity of water to add, 3-4 times of water is added with respect to the weight of a solvent, and 20-60 degreeC of the temperature of water is preferable. If the temperature of the water added to diffuse the solvent is less than 20 ℃, the diffusion rate of the solvent into the aqueous phase is slow, it takes a long time to prepare the pesticide, if the temperature of the water exceeds 60 ℃, the solvent does not have a difference in the rate of diffusion into the water phase Since cost is required to raise the temperature of the water, the temperature of the water used for diffusing the solvent into the water phase is preferably 20 to 60 ° C.
용매가 수상으로 확산되면 수상을 증류함으로써 용매를 제거한다. 이때 수상을 제거하는 방법으로는 로터리증류법을 포함하는 공지의 증류방법을 이용할 수 있다. 용매를 제거하기 위한 수상의 증류방법은 본 발명의 핵심적인 구성사항이 아니므로 이하 자세한 내용의 기재는 생략하기로 한다.If the solvent diffuses into the aqueous phase, the solvent is removed by distilling the aqueous phase. At this time, a known distillation method including a rotary distillation method can be used as a method of removing the aqueous phase. Since the distillation method of the aqueous phase for removing the solvent is not a key component of the present invention, description of the following detailed description will be omitted.
한편 본 발명은 상기에서 언급한 제조방법에 의해 제조된 마이크로캡슐 살충제를 포함한다.Meanwhile, the present invention includes a microcapsule insecticide prepared by the above-mentioned manufacturing method.
이하 본 발명을 하기의 실시예에 의하여 설명하고자 한다. 그러나 이들은 본 발명의 일실시예에 불과한 것으로 이들에 의해 본 발명의 권리범위가 한정되는 것은 아니다.Hereinafter, the present invention will be described by the following examples. However, these are only examples of the present invention, and the scope of the present invention is not limited thereto.
<실시예 1><Example 1>
상온에서 용매인 에틸아세테이트 10g에 생분해성 고분자인 폴리카프로락톤 0.2g을 용해시킨 후 살충성물질로서 퍼메쓰린 0.02g을 혼합하였다.0.2 g of polycaprolactone, a biodegradable polymer, was dissolved in 10 g of ethyl acetate as a solvent at room temperature, followed by mixing 0.02 g of permethrin as an insecticide.
전기의 용매, 생분해성 고분자 및 살충성물질의 혼합과는 별도로 안정화제로서 플루오닉에프-68(pluronic F-68, BASF) 1g을 물 20g에 용해시켰다.Apart from the mixing of the solvent, biodegradable polymer and pesticide, 1 g of pluronic F-68 (BASF) was dissolved in 20 g of water as a stabilizer.
전기의 용매, 생분해성 고분자 및 살충제물질의 혼합용액을 안정화제가 포함되어 있는 수용액에 첨가하여 포화시켰다. 이 포화용액을 균질화기를 이용하여 6000rpm∼12000rpm으로 5분∼10분 동안 유화시켰다.The mixed solution of the solvent, biodegradable polymer and pesticide material was added to the aqueous solution containing the stabilizer and saturated. This saturated solution was emulsified at 6000 rpm to 12000 rpm for 5 to 10 minutes using a homogenizer.
유화된 용액에 25℃ 온도의 물을 80g∼100g 첨가하여 용매를 수상으로 확산시키고 로터리증류기를 이용하여 수상으로 확산된 용매를 제거함으로써 도 2와 같이 지름이 2∼15㎛인 마이크로캡슐 살충제를 제조하였다.80 g to 100 g of water at 25 ° C. was added to the emulsified solution to diffuse the solvent into the aqueous phase, and a microcapsule insecticide having a diameter of 2 to 15 μm was prepared as shown in FIG. 2 by removing the solvent diffused into the aqueous phase using a rotary distillation machine. It was.
<실시예 2><Example 2>
상온에서 용매인 메틸렌클로라이드 20g에 폴리카프로락톤 2.5g을 용해시킨후 퍼메쓰린 6.5g를 혼합하였다.After dissolving 2.5 g of polycaprolactone in 20 g of methylene chloride as a solvent at room temperature, 6.5 g of permethrin was mixed.
전기의 용매, 폴리카프로락톤 및 퍼메쓰린의 혼합과는 별도로 안정화제로서 플루오닉에프-68 0.6g을 물 30g에 용해시켰다.Apart from the mixing of the former solvent, polycaprolactone and permethrin, 0.6 g of fluoronic-68 as a stabilizer was dissolved in 30 g of water.
전기의 용매, 폴리카프로락톤 및 퍼메쓰린의 혼합용액을 안정화제가 포함되어 있는 수용액에 첨가하여 포화시켰다. 이 포화용액을 균질화기를 이용하여 6000rpm∼12000rpm으로 5분∼10분 동안 유화시켰다.The mixed solution of the solvent, polycaprolactone and permethrin was added to the aqueous solution containing a stabilizer and saturated. This saturated solution was emulsified at 6000 rpm to 12000 rpm for 5 to 10 minutes using a homogenizer.
유화한 용액에 25℃ 온도의 물을 50g∼100g 첨가하여 용매를 수상으로 확산시키고 로터리증류기를 이용하여 수상으로 확산된 용매를 제거함으로서 지름이 2∼15㎛인 마이크로캡슐 살충제를 제조하였다.50 g to 100 g of water at 25 ° C. was added to the emulsified solution to diffuse the solvent into the aqueous phase, and a microcapsule insecticide having a diameter of 2 to 15 μm was prepared by removing the solvent diffused into the aqueous phase using a rotary distillation machine.
<실시예 3><Example 3>
안정화제인 플루오닉에프-68의 사용량을 하기의 표 1과 같이 달리 사용하는 것을 제외하고는 상기 실시예 1과 동일한 방법으로 마이크로캡슐 살충제를 제조하였다. 한편 마이크로캡슐 살충제의 평균입자 크기는 광산란 장치(Zeta plus, 미국 Brookhaven사)를 사용하여 측정하고 그 결과를 하기의 표 1에 나타내었다.A microcapsule insecticide was prepared in the same manner as in Example 1 except that the amount of the fluoric F-68 stabilizer was used differently as shown in Table 1 below. Meanwhile, the average particle size of the microcapsule insecticide was measured using a light scattering apparatus (Zeta plus, Brookhaven, USA) and the results are shown in Table 1 below.
<표 1> 안정화제의 첨가량에 따른 마이크로캡슐의 크기Table 1 Size of microcapsules according to the amount of stabilizer added
상기 표 1에서와 같이 안정화제의 함량이 증가함에 따라 캡슐의 크기가 감소하였다. 이것은 임계 마이셀 농도하에서 더 많은 마이셀의 수를 형성하기 때문이다. 그러나 유화제의 함량이 계속 증가함에 따라 캡슐의 크기가 항상 감소하는 것은 아니다.As shown in Table 1, the size of the capsule decreased as the stabilizer content increased. This is because it forms more micelle numbers under the critical micelle concentration. However, the capsule size does not always decrease as the amount of emulsifier continues to increase.
<실시예 4><Example 4>
균질화기의 교반속도를 하기의 표 2와 같이 변화시키는 것을 제외하고는 상기 실시예 1과 동일한 방법으로 마이크로캡슐 살충제를 제조하였다. 제조한 마이크로캡슐 살충제의 평균입자 크기를 실시예 3에서 언급한 광산란 장치로 측정하고 그 결과를 표 2에 나타내었다.A microcapsule insecticide was prepared in the same manner as in Example 1, except that the stirring speed of the homogenizer was changed as shown in Table 2 below. The average particle size of the prepared microcapsule insecticide was measured by the light scattering apparatus mentioned in Example 3 and the results are shown in Table 2.
하기의 표 2에 나타난 결과로부터 교반속도가 증가할수록 마이크로캡슐의 입자크기가 감소함을 알 수 있다. 이것은 균질화기의 회전속도가 증가할수록 일정한 시간동안 더 많은 전단력이 에멀젼 액적에 가해지므로 액적의 크기가 감소하며 액적으로부터 생성되는 미세 입자의 크기도 감소하기 때문이다.From the results shown in Table 2 below, it can be seen that as the stirring speed increases, the particle size of the microcapsules decreases. This is because as the speed of the homogenizer increases, more shear force is applied to the emulsion droplets for a certain time, so that the size of the droplets decreases and the size of the fine particles generated from the droplets also decreases.
<표 2> 교반속도에 따른 마이크로캡슐의 크기<Table 2> Size of microcapsules according to stirring speed
본 발명은 유화-확산공정을 이용하여 캡슐화제로서 생분해성 고분자를 포함하고, 캡슐화제의 중심물질로서 살충성물질을 함유하는 마이크로캡슐 살충제의 제법을 제공할 수 있다.The present invention can provide a preparation method of a microcapsule insecticide comprising a biodegradable polymer as an encapsulating agent and an insecticide as a central substance of the encapsulant using an emulsification-diffusion process.
본 발명에 의해 제조된 마이크로캡슐 살충제는 한 번의 살포시 캡슐화제인 생분생성 고분자를 통해 살충성물질이 서서히 용출되므로 약효의 지속성이 우수하고 적은 양을 사용하게 되어 경제적이다. 또한 본 발명의 마이크로캡슐 살충제는 물을 매질로 하여 제조하였기 때문에 용매로 인한 냄새에 대한 단점을 극복할 수 있다.The microcapsule insecticide prepared by the present invention is economical because the pesticide is slowly eluted through the bioproducible polymer which is an encapsulating agent in one spraying, and thus it is economical because it has excellent sustainability and uses a small amount. In addition, since the microcapsule insecticide of the present invention was prepared using water as a medium, it can overcome the disadvantage of the odor caused by the solvent.
Claims (7)
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| CN100372461C (en) * | 2005-07-20 | 2008-03-05 | 吴学民 | Method for producing pesticide micro capsule |
| US9861096B2 (en) | 2008-10-01 | 2018-01-09 | Cornell University | Biodegradable chemical delivery system |
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| KR102278422B1 (en) * | 2019-10-02 | 2021-07-19 | 안호영 | Pesticide composition comprising nanoscale encapsulation formulation of active ingredient chemicals using multicomponent polymer system |
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