CN1313004C - Granular agent containing chlorpysifos and its preparation method - Google Patents
Granular agent containing chlorpysifos and its preparation method Download PDFInfo
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- CN1313004C CN1313004C CNB031473121A CN03147312A CN1313004C CN 1313004 C CN1313004 C CN 1313004C CN B031473121 A CNB031473121 A CN B031473121A CN 03147312 A CN03147312 A CN 03147312A CN 1313004 C CN1313004 C CN 1313004C
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Abstract
Description
技术领域Technical field
本发明涉及一种有效成份为毒死蜱、主要用于防治地下害虫的农药制剂颗粒剂的制备方法。The invention relates to a preparation method of a pesticide preparation granule whose active ingredient is chlorpyrifos and is mainly used for preventing and controlling underground pests.
背景技术 Background technique
毒死蜱(英文名chlorpyrifos),化学名称O,O-二乙基-O(3,5,6-三氯-2-吡啶基)硫逐磷酸酯,又名乐斯本(美国陶氏益农公司商品名)、安民乐、克乐死等,是美国DOW化学公司于1965年首先开发的产品,是一种高效、广谱、毒性低的有机磷杀虫杀螨剂。20多年应用证明,使用浓度没有增加,害虫对它基本无抗药性。毒死蜱主要通过触杀、胃毒及熏蒸3种作用方式控制害虫。杀虫谱可与甲胺磷相比,但毒性比甲胺磷低很多,属中等毒性,在有机磷杀虫剂中属低毒。可广泛用于水稻、小麦、棉花、蔬菜、果树、茶树、卫生等诸多领域,对防治水稻螟虫、纵卷叶螟、飞虱、棉花叶螨、蚜虫、菜青虫、小菜蛾、豆野螟、红蜘蛛、茶尺蠖、孑孓、蟑螂等害虫都有效,在国内外涉及的应用领域广泛,是替代高毒农药较理想的大吨位品种。其结构式为:Chlorpyrifos (English name chlorpyrifos), chemical name O, O-diethyl-O (3,5,6-trichloro-2-pyridyl) phosphorothioate, also known as Lesben (Dow AgroSciences, Inc. Product name), Anminle, Keleshi, etc., were first developed by DOW Chemical Company of the United States in 1965. It is an organophosphorus insecticide and acaricide with high efficiency, broad spectrum and low toxicity. More than 20 years of application have proved that the use concentration has not increased, and pests have basically no resistance to it. Chlorpyrifos mainly controls pests through three modes of action: contact killing, stomach poisoning and fumigation. The insecticidal spectrum can be compared with methamidophos, but the toxicity is much lower than that of methamidophos, which belongs to moderate toxicity and is low toxicity among organophosphorus insecticides. It can be widely used in many fields such as rice, wheat, cotton, vegetables, fruit trees, tea trees, and hygiene. Red spider mite, tea inchworm, larvae, cockroach and other pests are all effective, and they are widely used in domestic and foreign applications, and are ideal large-tonnage varieties to replace highly toxic pesticides. Its structural formula is:
R为甲基或乙基R is methyl or ethyl
R为乙基则称为乙基毒死蜱(简称毒死蜱),R为甲基称为甲基毒死蜱,在我国广泛使用的是乙基毒死蜱。If R is ethyl, it is called chlorpyrifos ethyl (chlorpyrifos for short), if R is methyl, it is called chlorpyrifos methyl, and chlorpyrifos ethyl is widely used in my country.
毒死蜱通常以乳油或水乳剂的形式应用于农业及非农业,但由于其常用乳油制剂在使用过程中,药物释放快,加上喷雾时的飘移,往往只能发挥60~70%的药效,不能很好的利用,为了克服这些不足,人们纷纷对毒死蜱的制剂加以创新,出现了大批的毒死复配剂,都是以提高渗透、吸附等作用,从而减少用量,来达到充分利用、提高药效的目的,目前市场上存在着多种毒死蜱单剂或者是复配制剂,如申请号为01100515的发明专利申请公开了吡虫啉与毒死蜱的复配,对苹果绵蚜有特殊防效;申请号为01100511的发明专利申请公开了阿维菌素与毒死蜱的复配,对梨木虱有特殊防效;申请号为00128287的发明专利申请公开了三唑磷与毒死蜱的复配,主要用于防治水稻螟虫;申请号为98111820的发明专利申请公开了菊酯类杀虫剂与毒死蜱的复配以提高药效;申请号为98122085的发明专利申请公开了硫丹与毒死蜱的复配而成的乳油,主要目的是提高持效性;申请号为98122084的发明专利申请公开了敌敌畏与毒死蜱的复配而成的乳油,主要目的是增效;申请号为93120345的发明专利申请公开了甲基对硫磷和辛硫磷与毒死蜱的复配,主要用于棉铃虫的防除。Chlorpyrifos is usually used in agriculture and non-agriculture in the form of emulsifiable concentrate or water emulsion. However, due to the rapid release of the drug during the use of its commonly used emulsifiable concentrate preparation, and the drift during spraying, it often only exerts 60-70% of the drug effect. It cannot be well utilized. In order to overcome these shortcomings, people have innovated the preparations of chlorpyrifos one after another. A large number of chlorpyrifos compound agents have appeared, all of which are to improve penetration, adsorption, etc., thereby reducing the dosage, so as to achieve full utilization and improve For the purpose of drug efficacy, there are many kinds of chlorpyrifos single agent or compound preparations on the market. For example, the invention patent application with application number 01100515 discloses the compound of imidacloprid and chlorpyrifos, which has special control effect on apple aphid; application number The invention patent application of No. 01100511 discloses the compounding of abamectin and chlorpyrifos, which has special control effect on pear psyllid; the invention patent application of application number 00128287 discloses the compounding of triazophos and chlorpyrifos, which is mainly used to control rice borers; application number 98111820 patent application for invention discloses the compounding of pyrethroid insecticides and chlorpyrifos to improve efficacy; The main purpose is to improve the long-lasting effect; the invention patent application with the application number 98122084 discloses the compounded emulsifiable concentrate of dichlorvos and chlorpyrifos, and the main purpose is to increase the efficiency; the invention patent application with the application number 93120345 discloses methyl parathion The combination with phoxim and chlorpyrifos is mainly used for the control of cotton bollworm.
而颗粒剂的撒施方便,几乎无飘移现象,因此,现越来越多地被广泛应用于各领域上,颗粒剂可以缓慢控制药释放,因此还可以以准确的最佳剂量施用,而达到长期防治的目的,而这是人们所希望的。Granules are easy to spread and have almost no drift phenomenon. Therefore, they are now more and more widely used in various fields. Granules can slowly control drug release, so they can also be administered at an accurate and optimal dose to achieve The purpose of long-term prevention and control, and this is what people hope.
为了抑制农药过快地释放,人们将许多农药都制成颗粒剂,如呋喃丹、杀虫单。但大多颗粒剂以碎石、细沙等高堆积密度的材料作载体,这种方法制造成本不高,但其缺点是颗粒比重大,比表面积小,与防治对象接触面小,撒施不均匀,吸附性差。过去也曾建议过在制备颗粒剂时使用石蜡,但这方法的缺点是与水的表面张力大,活性成分不能充分被释放,加上需将石蜡熔融并将之与其它组分不易均匀混合,因此,制备这些颗粒剂的方法复杂。In order to inhibit the rapid release of pesticides, many pesticides are made into granules, such as carbofuran and monosultap. However, most granules use materials with high bulk density such as crushed stones and fine sand as carriers. This method has low manufacturing cost, but its disadvantages are that the specific surface area of the particles is large, the contact surface with the control object is small, and the application is uneven. , poor adsorption. It has also been suggested to use paraffin wax in the preparation of granules in the past, but the disadvantage of this method is that the surface tension with water is high, the active ingredient cannot be fully released, and it is necessary to melt the paraffin wax and mix it with other components. Therefore, the methods for preparing these granules are complicated.
本发明的目的是提供了一种以毒死蜱为活性组份的颗粒剂及其制备方法,主要用于防治地下害虫。The object of the present invention is to provide a granule with chlorpyrifos as an active component and a preparation method thereof, which are mainly used for preventing and controlling underground pests.
发明内容Contents of the invention
本发明以毒死蜱为活性成份,并将其均匀分散在一或多种载体和吸附剂中,通过挤出造粒机造粒,干燥后即成。The invention uses chlorpyrifos as the active ingredient, uniformly disperses it in one or more carriers and adsorbents, granulates through an extruding granulator, and is ready after drying.
所述的载体为酸性自土、凹凸棒土、硅藻土、高岭土、膨润土、滑石、淀粉中的一种或一种以上的混合。其用量占总重的50-80%。The carrier is one or a mixture of acidic clay, attapulgite, diatomite, kaolin, bentonite, talc and starch. Its consumption accounts for 50-80% of total weight.
所述的吸附剂为木屑、秸杆粉、米皮糠、自炭黑中的一种或一种以上的混合,优选为秸杆粉、米皮糠。其用量占总重的5-40%。The adsorbent is a mixture of one or more of wood chips, straw powder, rice bran, and self-carbon black, preferably straw powder and rice bran. Its consumption accounts for 5-40% of total weight.
本发明所用的活性成份为毒死蜱,可以为含量在85%以上的原药,也可以为直接从生产过程中取得的未经提纯及还含有甲苯等有机溶剂半成品(称为油苯),其中含有15-84%的毒死蜱。当采用高含量的原药时,由于毒死蜱在室温下是固体,为了使其混合均匀,尚需将其熔化成液态再与载体和吸附剂采用机械搅拌方式混合。若采用低含量的油苯来配制,由于已经为液态,则不必熔化。该制剂主要施用于土壤中,用于地下害虫的防除,较低的含量有利于施用时的分散均匀,因此本发明优选活性成份毒死蜱的含量为1-20%。The active ingredient used in the present invention is chlorpyrifos, which can be the original drug with a content of more than 85%, or can be directly obtained from the production process without purification and also contains organic solvent semi-finished products such as toluene (called oil benzene), which contains 15-84% chlorpyrifos. When high content of the original drug is used, since chlorpyrifos is solid at room temperature, in order to mix it evenly, it needs to be melted into a liquid state and then mixed with the carrier and adsorbent by mechanical stirring. If a low content of benzene is used to prepare, since it is already in a liquid state, it does not need to be melted. The preparation is mainly applied in the soil for the prevention and control of underground pests, and the lower content is conducive to uniform dispersion during application. Therefore, the content of the active ingredient chlorpyrifos is preferably 1-20% in the present invention.
本发明颗粒剂的制备方法:(1)将含有毒死蜱的物质与载体、吸附剂与水混合均匀,得到湿料I;(2)将I通过挤出造粒机造粒,得粒状物II;(3)将II干燥。The preparation method of the granule of the present invention: (1) uniformly mix the material containing chlorpyrifos with the carrier, the adsorbent and water to obtain the wet material I; (2) granulate the I through an extrusion granulator to obtain the granule II; (3) Dry II.
为了方便造粒,应控制湿料I中挥发组份(主要为水、原药中带入的甲苯等)的含量为1-20%,优选为5-8%。In order to facilitate granulation, the content of volatile components (mainly water, toluene, etc. carried in the original drug) in the wet material I should be controlled to be 1-20%, preferably 5-8%.
烘干后,可任选地调整颗粒剂的颗粒大小,经过筛分选取粒径为0.2-3mm的范围,粒径过大颗粒可以集中后粉碎再过筛,剩余的粉未可以返回造粒系统。当然也可以通过调整造粒机来达到其它粒径范围的产品。After drying, the particle size of the granules can be adjusted optionally, and the particle size range of 0.2-3mm can be selected after sieving. The particles with too large particle size can be concentrated, crushed and then sieved, and the remaining powder can be returned to the granulation system. . Of course, products in other particle size ranges can also be obtained by adjusting the granulator.
本发明颗粒剂有许多优点:(1)制备简单、方便;(2)能控制有效成分的缓慢释放;(3)堆积密度小,比一般颗粒剂的堆积密度小一倍左右;(4)比表面积增大,有利于均匀撒施,能有效发挥其活性成分的作用,降低用量;(5)采用环保型吸附剂,对环境安全,而且分解后可作有机肥使用,与现有颗粒剂相比较,本发明的颗粒剂更适合于地下害虫的防治,以及施用于阴沟、水田、杂草丛等蚊蝇孽生场所,防治蚊蝇幼虫等的孳生。The granules of the present invention have many advantages: (1) preparation is simple and convenient; (2) can control the slow release of active ingredients; (3) the bulk density is small, about one time less than that of general granules; The surface area increases, which is conducive to uniform spreading, can effectively play the role of its active ingredients, and reduce the dosage; (5) the use of environmentally friendly adsorbents is environmentally safe, and can be used as organic fertilizers after decomposition, which is comparable to existing granules. In comparison, the granules of the present invention are more suitable for the prevention and control of underground pests, and are applied to places where mosquitoes and flies live, such as gutters, paddy fields, and weeds, to prevent the breeding of mosquito and fly larvae.
具体实施方式 Detailed ways
现具体的实施例来描述本发明,实施例所采用的配方只是可以实现本发明的一部分,不能理解为对本发明的限制。The present invention will be described by specific examples. The formulations used in the examples are only part of the present invention and should not be construed as a limitation of the present invention.
实施例1:取95%毒死蜱原药10.526kg,凹凸棒土60kg,米皮糠29.474kg,水10kg,将毒死蜱原药加热熔化,加入凹凸棒土、米皮糠、水,搅拌混合均匀,再转入挤出造粒机进行造粒,最后烘干,过筛得10%毒死蜱颗粒剂。Embodiment 1: get 95% chlorpyrifos former medicine 10.526kg, attapulgite 60kg, rice bran 29.474kg, water 10kg, the former medicine of chlorpyrifos is heated and melted, add attapulgite, rice bran, water, stir and mix, and then Transfer to an extrusion granulator for granulation, finally dry, and sieve to obtain 10% chlorpyrifos granules.
实施例2:取含毒死蜱80%的油苯6.25kg,酸性白土30kg,高岭土40kg,秸杆粉25kg,水5kg,实施方案同实施例1,得5%毒死蜱颗粒剂。Embodiment 2: get 6.25kg of benzene containing chlorpyrifos 80%, acid white clay 30kg, kaolin 40kg, straw powder 25kg, water 5kg, embodiment is the same as embodiment 1, gets 5% chlorpyrifos granule.
实施例3:取95%毒死蜱原药21.05kg,硅藻土30kg、膨润土30kg,木屑18.95kg,水10kg,实施方案同实施例1,得20%毒死蜱颗粒剂。Embodiment 3: get 21.05kg of 95% chlorpyrifos technical material, 30kg of diatomite, 30kg of bentonite, 18.95kg of sawdust, 10kg of water, embodiment is the same as embodiment 1, obtains 20% chlorpyrifos granule.
实施例4:采用实施例1制得的10%毒死蜱颗粒剂,分别在广东和山东用于防治甘蔗蔗龟和韭蛆,对于地下害虫药效好于相同有效成份的乳油,田间药效试验结果如下:Embodiment 4: Adopt the 10% chlorpyrifos granule that embodiment 1 makes, be used for preventing and treating sugarcane tortoise and leek maggot respectively in Guangdong and Shandong, for underground pest drug effect is better than the emulsifiable concentrate of the same active ingredient, field efficacy test result as follows:
10%毒死蜱颗粒剂防治甘蔗蔗龟田间药效试验
10%毒死蜱颗粒剂防治韭蛆保苗效果试验
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|---|---|---|---|---|
| CN100508755C (en) * | 2007-04-11 | 2009-07-08 | 江苏省农业科学院 | Granules for controlling Laodelphax striatella in wheat fields |
| CN102047876A (en) * | 2009-11-05 | 2011-05-11 | 甘肃省农业科学院植物保护研究所 | Formula and preparation method of granular pesticide |
| CN101953383B (en) * | 2010-05-27 | 2011-09-21 | 江苏点金石凹土研究开发有限公司 | Attapulgite fly spray |
| CN101953385B (en) * | 2010-05-27 | 2011-09-21 | 江苏点金石凹土研究开发有限公司 | Suspension for killing mosquito eggs |
| CN101953380B (en) * | 2010-05-27 | 2012-04-18 | 江苏点金石凹土研究开发有限公司 | Attapulgite maggot killing powder |
| CN101953375A (en) * | 2010-05-27 | 2011-01-26 | 江苏点金石凹土研究开发有限公司 | Attapulgite mosquito-killing powder |
| CN101953382B (en) * | 2010-05-27 | 2012-04-18 | 江苏点金石凹土研究开发有限公司 | Attapulgite fly-killing powder |
| CN102657155B (en) * | 2012-05-10 | 2013-11-06 | 肇庆市真格生物科技有限公司 | Nematicide granules with sawdust as carrier and preparation method thereof |
| CN103461325A (en) * | 2013-06-06 | 2013-12-25 | 黄山市迎客松生物科技有限公司 | Straw-based drug liquid controlled release agent and preparation method thereof |
| CN103636660B (en) * | 2013-11-26 | 2016-05-25 | 肇庆市真格生物科技有限公司 | A kind of for preventing and treating the Environmental-protection particle agent of Sugarcane Pests |
| CN106259423A (en) * | 2016-08-15 | 2017-01-04 | 河南省莱恩坪安园林植保有限公司 | Spacetabs type subterranean pest-insect insecticide used by a kind of ornamental plant |
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| US4380537A (en) * | 1977-11-21 | 1983-04-19 | The Dow Chemical Company | Stabilized insecticide formulations |
| EP0110157A1 (en) * | 1982-10-28 | 1984-06-13 | Pennwalt Corporation | Granular pesticide composition |
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