CN114946853A - 一种飞防用控释型颗粒剂及其制备方法 - Google Patents
一种飞防用控释型颗粒剂及其制备方法 Download PDFInfo
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- A—HUMAN NECESSITIES
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- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
- A01N37/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic 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
- A01N25/08—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
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- 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
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/24—Cyanogen or compounds thereof, e.g. hydrogen cyanide, cyanic acid, cyanamide, thiocyanic acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
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Abstract
本发明涉及A01N,更具体地,本发明涉及一种飞防用控释型颗粒剂及其制备方法。所述颗粒剂的制备原料包括:有效成分、油性液体、水溶性包衣材料、载体。本发明的颗粒剂适用于飞防作业,使用无人机在滩地、沟渠等地撒施更加方便且效率更高,制备的颗粒剂外层有成膜剂包覆,强度较好,无人机飞防作业时无粉尘且不会造成药剂的浪费。本发明的颗粒剂采用湿敏性的成膜材料进行包衣,只有在目标区域有水、潮湿或湿度较大时,成膜材料溶解,药液才会释放出来,达到控释且提高药剂作用范围的作用。本发明的颗粒剂载体所吸附的药液为油性药液,遇水后会随着水的润湿面展布开来,提高药剂作用范围。
Description
技术领域
本发明涉及A01N,更具体地,本发明涉及一种飞防用控释型颗粒剂及其制备方法。
背景技术
采用含有杀灭害虫或病菌的有效成分的颗粒剂,是防止作物病害或虫害等威胁的一种方式,目前颗粒剂的使用方式主要是人工背负式喷雾喷粉机进行喷施,或者播撒机进行播撒,存在人工效率低、器械笨重,平均撒播量和撒播面积低等问题,且对于一些病害或虫害分布区域,如钉螺分布区域为江、湖洲滩的滩地和没有积水的沟、渠、塘、田的埂边等有螺环境,现有人工背负式喷施颗粒剂的方式很不方便,且费时费力故需提供一种颗粒剂,可用于飞防作业,也即使用无人机进行病虫害防治,来提高效率。
目前颗粒剂多采用载体,如细沙加粘结剂裹覆药粉的方法制备,如CN103766332A提供了一种可用于喷施的新型环保杀钉螺颗粒剂其及制备方法,包括杀钉螺有效成分、复合粘合剂、载体细沙,提供一种质量适中、对生产和施用设备影响小、长期缓释的沙基颗粒剂。但存在药粉黏结强度不够,使用无人机飞防作业时粉尘较大,污染环境且造成药剂的浪费,以及飞防作业过程流动性不佳,下料不流畅,容易堵塞且撒施不均匀的问题。
此外,现有颗粒剂到达目标后药物直接释放,药剂的浪费的同时,传统颗粒剂单个颗粒的有效作用范围很小,需使用大量的颗粒剂才能做到施药区域的覆盖,也会造成药剂过多使用。
发明内容
为了解决上述问题,本发明第一个方面提供了一种飞防用控释型颗粒剂,颗粒剂的制备原料按重量份计,包括:有效成分5~40份、油性液体5~30份、水溶性包衣材料0.5~5份、载体补足至100份。
本发明不对有效成分做具体限定,可为防治病虫害,如血防灭螺、防治朱砂叶螨、二化螟、飞虱、蚜虫等虫害,水稻恶苗病菌、落叶病、叶斑病、稻瘟病等病害的有效成分,不做具体限定。
当颗粒剂用于灭螺时,有效成分包括但不限于,五氯酚钠、氯硝柳胺乙醇胺盐、氯硝柳胺、四聚乙醛、氰氨化钙、氯乙酰胺、烟酰硫胺等。
本发明不对载体的种类做具体限定,为本领域熟知的载体,可列举的有,凹凸棒石、陶粒砂、高岭土、陶土、白炭黑、硅藻土中的一种或多种。
为了提高载体的吸附性能,所述载体可经过活化处理,如对凹凸棒石进行酸活化或热活化,当酸活化时,可通过盐酸、硫酸等活化,当热活化时,可在200~300℃加热活化,不做具体限定。
为了提高颗粒剂的流动性,减少颗粒剂的飞防过程中粉尘污染,所述载体的形状为球形或类球形,所述载体的粒径范围为1~3mm。所述载体的粒径范围为1~3mm的含义为载体的粒径在1~3mm之间(包括1mm和3mm)分布。
作为本发明一种优选的技术方案,所述油性液体选自酯类液体、矿物油、植物油、酯化植物油中的一种或多种。
作为本发明一种优选的技术方案,所述酯类液体选自油酸甲酯、乙酸乙酯、油酸丁酯、月桂酸乙酯、月桂酸甲酯、月桂酸丁酯、棕榈酸甲酯、棕榈酸乙酯、棕榈酸丁酯、酯化植物油中的一种或多种。优选为所述酯类液体为链状酯类液体,所述酯类液体的碳原子数为10~25,可列举的有,10、11、12、13、14、15、16、17、18、19、20、21、22、23、24、25。
作为本发明一种优选的技术方案,所述酯化植物油为植物油与醇反应得到酯类物质,根据反应的醇的类型,可分为甲酯化植物油、丁酯化植物油、辛酯化植物油等,可列举的有,甲酯化大豆油、甲酯化椰子油等,不做具体限定。
作为本发明一种优选的技术方案,所述植物油选自玉米油、菜籽油、大豆油、椰子油、葵花籽油中的一种或多种。
作为本发明一种优选的技术方案,所述油性液体包括酯类液体和植物油,重量比为1:(0.2~0.4)。
作为本发明一种优选的技术方案,所述颗粒剂的制备原料按重量份计,还包括扩散剂1~5份、分散剂0.1~3份。
作为本发明一种优选的技术方案,所述扩散剂包括有机硅聚氧乙烯醚,有机硅聚氧乙烯醚为聚醚与二甲基硅氧烷接枝共聚得到的,作为有机硅聚氧乙烯醚的实例,包括但不限于,青岛美斯得有机硅有限公司的DM-MSD9196(HLB为7.8)、DM-MSD9113(HLB为8.1)、MSD9103(HLB为11.8)、MSD9101(HLB为13.4)。
作为本发明一种优选的技术方案,所述有机硅聚氧乙烯醚的HLB为7~10,可列举的有,7、8、9、10。
作为本发明一种优选的技术方案,所述分散剂包括木质素磺酸盐、聚羧酸盐中的至少一种,作为木质素磺酸盐的实例,包括但不限于,木质素磺酸钠、木质素磺酸钾、木质素磺酸钙、木质素磺酸镁。优选为木质素磺酸钙、木质素磺酸镁。
目前颗粒剂一般使用载体和粘结剂包覆药粉的方法制备,存在包覆强度弱,得到的颗粒流动性不好等问题,若用于飞防作用,容易出现堵塞出口、粉尘飞扬等问题,本发明通过将有效成分粉体配成药液,并采用较大粒径,且形状类球形或球形的载体进行吸附的方式,得到的颗粒剂,具有较均匀的形状和合适的重力,可减少飞防作业时的粉尘飞扬等问题。
但发明人也发现,本发明使用较大粒径的载体,使得难以完全吸附药液,残留在表面的药液因为和包衣材料的性质不同,会造成部分药液暴露在包衣表面,造成堵塞出口,长期放置容易出现粘结,发明人发现,通过添加合适的游行液体和分散剂、扩散剂,可减少药液暴露在包衣表面,避免飞防堵塞和放置粘结等问题。
这可能是因为,通过添加一定长度的链状酯类液体,和含有一定链长的脂肪酸的植物油,并添加低HLB的有机硅聚氧乙烯醚、木质素磺酸盐,和和有效成分作用时,可在有机成分表面形成内部为木质素磺酸盐和植物油,外部为有机硅聚氧乙烯醚和酯类液体的结构,当和载体,如活化的凹凸棒石混合过程中,利用有机成分表面的阴离子磺酸盐和凹凸棒石表面的吸附,和阳离子交换,带动有机成分和有机成分外部的酯类液体和有机硅聚氧乙烯醚和凹凸棒石作用,又因为有机硅聚氧乙烯醚的有机硅的低分子间作用力,以及柔性聚氧乙烯醚的作用,促进了有机成分、油性液体和扩散剂、分散剂等进入载体内部,减少载体外部的药液残留,从而避免药液暴露在表面造成的堵塞和粘结等。
作为本发明一种优选的技术方案,所述水溶性包衣材料选自羟丙基甲基纤维素、羟基丙基纤维素、聚乙烯吡咯烷酮、聚维酮、聚乙烯醇中的一种或多种。
作为聚乙烯醇的实例,可列举的有,中石化川维的PVA 1788(平均聚合度为1700,醇解度为87~89%)、PVA 2088(平均聚合度为2000,醇解度为87~89%),PVA2488(平均聚合度为2400、醇解度为87~89%)、PVA0588(平均聚合度为500,醇解度为87~89%),聚乙烯醇是通过聚醋酸乙烯酯醇解得到的,醇解度为醇解的官能团占总官能团的百分数,聚合度为大分子中单体的数目。
为了达到在含水环境中的控释效果,发明人发现,聚乙烯醇的醇解度不能太高,当太高时,不利于在水中溶解。所述聚乙烯醇的平均聚合度为500~3000,优选为1000~3000,更优选为1500~3000。所述醇解度小于90%,优选为70~90%,更优选为80~90%。
作为聚乙烯吡咯烷酮的实例,可列举的有,山东广申电子科技有限公司的PVPK17、PVP K30、PVP K60、PVP K90。所述聚乙烯吡咯烷酮的K值为15~30。
作为本发明一种优选的技术方案,所述聚乙烯醇和聚乙烯吡咯烷酮的重量比为1:(0.1~0.3)。
目前颗粒剂达到目标区域后直接释放,容易造成药液的浪费,本发明通过在颗粒剂表面进行包衣,如使用水溶性材料,如聚乙烯醇进行包衣,可控制颗粒剂释放的条件,当在接触水,或者湿度较大时,使得包衣材料溶解,才会释放药液,达到控释的作用,尤其适用于潮湿或者有水环境下虫害或病害的控制,减少粉尘产生。
但发明人也发现,因为本发明使用的水溶性材料,如聚乙烯醇等形成较软的包衣膜,且受到药液的油性液体相互排斥使得水溶性材料,如聚乙烯醇等吸附性较差,增加脱落的产生,而包衣的脱落,也会造成药液的损失,而发明人发现,通过添加较低分子量的聚乙烯吡咯烷酮,和合适分子量的聚乙烯醇共同作为包衣材料,并在油性液体中添加植物油,可促进包衣的稳定,减少脱落。
这可能是因为包衣过程中,通过使用聚乙烯吡咯烷酮和聚乙烯醇共同进行包衣,可在形成的聚乙烯醇包衣膜上均匀交叉聚乙烯吡咯烷酮的结构,使得一方面在聚乙烯醇羟基和载体羟基作用的同时,聚乙烯吡咯烷酮的环状结构在进一步支撑包衣膜的同时,其相对极性的环状结构也减少了和油性液体的排斥,从而进一步增加包衣膜的吸附性,避免脱落。
作为本发明一种优选的技术方案,所述扩散剂还包括烷基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚中的至少一种,所述有机硅聚氧乙烯醚,和烷基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚中的至少一种的重量比为(2~4):1。
作为烷基酚聚氧乙烯醚的实例,包括但不限于,辛基酚聚氧乙烯醚,如海石花的OP-4(HLB为8~8.6)、OP-7(HLB为11.5~12.5)、OP-9(HLB为12.7~13.4)、OP-10(HLB为13.3~14)、OP-13(HLB为14)、OP-15(HLB为15)、OP-20(HLB为16)、OP-30(HLB为17)、OP-40(HLB为18)、OP-50(HLB为19)。所述烷基酚聚氧乙烯醚的HLB为11~16。
作为脂肪醇聚氧乙烯醚的实例,包括但不限于,油醇聚氧乙烯醚,如海石花的OV-3(HLB为6)、OV-5(HLB为8)、OV-10(HLB为12.4)、OV-15、OV-20(HLB为15.4)、OV-24,异癸醇聚氧乙烯醚,如海石花的E-1007、E-1009,C16-18脂肪醇聚氧乙烯醚,如海石花的O-8(HLB为11~12)、O-9(HLB为12~12.5)、O-10(HLB为12.5~13)、O-15(HLB为14~15)、O-20(HLB为15~16),C12-14脂肪醇聚氧乙烯醚,如海石花的MOA-7(HLB为12~13)、MOA-19(HLB为13~14)、MOA-15(HLB为15~16)。所述脂肪醇聚氧乙烯醚的HLB为11~16。
作为本发明一种优选的技术方案,所述分散剂还包括EO-PO嵌段共聚物,所述木质素磺酸盐、聚羧酸盐中的至少一种,和EO-PO嵌段共聚物的重量比为(2~4):1。
作为EO-PO嵌段共聚物的实例,包括但不限于,巴斯夫的RPE1740(EO含量为40%)、RPE1720(EO含量为20%)、RPE2520(EO含量为20%)、RPE3110(EO含量为10%)、RPE 2035(EO含量为35%)、RPE 2520(EO含量为20%)、RPE 2525(EO含量为25%)。所述EO含量为EO-PO嵌段共聚物中的EO占EO和PO的摩尔百分数。所述EO-PO嵌段共聚物的EO含量为20~50%,优选为25~50%,更优选为30~50%。
且发明人发现,当采用聚乙烯醇和聚乙烯吡咯烷酮共同作为包衣材料,在提高包衣吸附和强度的同时,因为聚乙烯吡咯烷酮中极性环状结构的作用,长期放置或者较高温度下,可能和内部药液产生一定的溶解,造成部分黏附。而发明人发现,通过使用较长链油性液体,并添加合适的扩散剂和分散剂,可减少对包衣膜的溶解,提高高温流动性。
这可能是因为当添加较长链油性液体,如酯类液体的链长,并控制植物油的用量时,控制药液的极性,可减少和包衣膜中聚乙烯吡咯烷酮相容的同时,添加较高HLB的羟基聚氧乙烯醚和较高EO值得EO-PO嵌段共聚物,利用羟基聚氧乙烯醚和嵌段聚醚的亲油性差异,使得药液外层主要为聚氧乙烯醚和嵌段聚醚的EO嵌段,减少药液中油性液体和包衣材料的接触,进一步减少油性液体对包衣的排斥,提高高温流动性的同时,减少脱落的产生。
本发明第二个方面提供了一种所述的飞防用控释型颗粒剂的制备方法,包括:
吸附性药液制备:将有效成分、油性液体、润湿剂、分散剂共混,研磨,得到粒径D90小于3μm的吸附性药液;
载体吸附:将吸附性药液和载体搅拌吸附,得到负载药液;本发明混合搅拌的时间不做具体限定,将吸附性药液吸附进载体中即可;
包衣:将负载药液放入包衣机中,加入水溶性包衣材料包衣,得到所述颗粒剂。
发明人发现,通过控制药液的粒径,在促进药液和载体吸附的同时,在控释过程中,随着包衣的溶解,合适粒径的药液释放到水中或潮湿环境中时,利用药液的油性液体、分散剂和扩散剂的展布作用,可促进小粒径有效成分均匀的扩散,提高药液作用范围。
本发明与现有技术相比具有以下有益效果:
(1)本发明的颗粒剂适用于飞防作业,使用无人机在滩地、沟渠等地撒施更加方便且效率更高,省时省力。
(2)本发明采用的制备方法为:吸附载体对药液进行吸附后,使用成膜剂对载体进行包衣。此种方法制备的颗粒剂外层有成膜剂包覆,强度较好,无人机飞防作业时无粉尘且不会造成药剂的浪费。
(3)本发明采用的颗粒剂载体为球状、近球状的规则载体颗粒,且粒径分布范围窄,大小均一,流动性佳,下料流畅,方便无人机撒施且撒施更为均匀。
(4)本发明的颗粒剂采用湿敏性的成膜材料进行包衣,只有在目标区域有水、潮湿或湿度较大时,成膜材料溶解,药液才会释放出来,达到控释且提高药剂作用范围的作用。
(5)本发明的颗粒剂载体所吸附的药液为油性药液,遇水后会随着水的润湿面展布开来,提高药剂作用范围。
附图说明
图1为实施例1提供的颗粒剂飞防撒施到土壤上的图。
具体实施方式
实施例
实施例1
本例提供一种颗粒剂,颗粒剂的制备原料按重量份计,包括:有效成分8份、油性液体10份、水溶性包衣材料4份、扩散剂3份、分散剂1份、载体补足至100份;所述有效成分为氯硝柳胺乙醇胺盐,所述载体为热活化凹凸棒石,当热活化时,在250℃加热活化,所述载体的形状为类球形,所述载体的粒径范围为1~3mm,所述油性液体选自酯类液体和植物油,重量比为1:0.3,所述酯类液体选自油酸甲酯,所述植物油选自大豆油,所述扩散剂包括有机硅聚氧乙烯醚DM-MSD9196和烷基酚聚氧乙烯醚OP-9,重量比为3:1,所述分散剂包括木质素磺酸钙和EO-PO嵌段共聚物RPE1740,重量比为3:1,所述水溶性包衣材料选自聚乙烯醇PVA2088和聚乙烯吡咯烷酮PVP K17,重量比为1:0.2。
本例还提供如上所述的颗粒剂的制备方法,包括:
吸附性药液制备:将有效成分、油性液体、润湿剂、分散剂共混,研磨,得到粒径D90小于3μm的吸附性药液;
载体吸附:将载体放入搅拌机中,喷洒吸附性药液,搅拌吸附,得到负载药液;
包衣:将负载药液放入包衣机中,将水溶性包衣材料溶于无水乙醇后喷入包衣机包衣、烘干,得到所述颗粒剂。
实施例2
本例提供一种颗粒剂,颗粒剂的制备原料按重量份计,包括:有效成分10份、油性液体14份、水溶性包衣材料5份、扩散剂5份、分散剂2份、载体补足至100份;所述有效成分为氯硝柳胺,所述载体为热活化凹凸棒石,当热活化时,在300℃加热活化,所述载体的形状为类球形,所述载体的粒径范围为1~3mm,所述油性液体选自酯类液体和植物油,重量比为1:0.4,所述酯类液体选自油酸丁酯,所述植物油选自椰子油,所述扩散剂包括有机硅聚氧乙烯醚DM-MSD9113和脂肪醇聚氧乙烯醚OV-10,重量比为4:1,所述分散剂包括木质素磺酸镁和EO-PO嵌段共聚物RPE 2035,重量比为4:1,所述水溶性包衣材料选自聚乙烯醇PVA2488和聚乙烯吡咯烷酮PVP K30,重量比为1:0.3。
本例还提供如上所述的颗粒剂的制备方法,包括:
吸附性药液制备:将有效成分、油性液体、润湿剂、分散剂共混,研磨,得到粒径D90小于3μm的吸附性药液;
载体吸附:将载体放入搅拌机中,喷洒吸附性药液,搅拌吸附,得到负载药液;
包衣:将负载药液放入包衣机中,将水溶性包衣材料溶于无水乙醇后喷入包衣机包衣、烘干,得到所述颗粒剂。
实施例3
本例提供一种颗粒剂,颗粒剂的制备原料按重量份计,包括:有效成分5份、油性液体7份、水溶性包衣材料3份、扩散剂2份、分散剂0.8份、载体补足至100份;所述有效成分为氰氨化钙,所述载体为热活化凹凸棒石,当热活化时,在230℃加热活化,所述载体的形状为类球形,所述载体的粒径范围为1~3mm,所述油性液体选自酯类液体和植物油,重量比为1:0.2,所述酯类液体选自棕榈酸甲酯,所述植物油选自玉米油,所述扩散剂包括有机硅聚氧乙烯醚DM-MSD9113和脂肪醇聚氧乙烯醚MOA-15,重量比为2:1,所述分散剂包括木质素磺酸镁和EO-PO嵌段共聚物RPE 2035,重量比为2:1,所述水溶性包衣材料选自聚乙烯醇PVA1788和聚乙烯吡咯烷酮PVP K17,重量比为1:0.1。
本例还提供如上所述的颗粒剂的制备方法,包括:
吸附性药液制备:将有效成分、油性液体、润湿剂、分散剂共混,研磨,得到粒径D90小于3μm的吸附性药液;
载体吸附:将载体放入搅拌机中,喷洒吸附性药液,搅拌吸附,得到负载药液;
包衣:将负载药液放入包衣机中,将水溶性包衣材料溶于无水乙醇后喷入包衣机包衣、烘干,得到所述颗粒剂。
实施例4
本例提供一种颗粒剂,颗粒剂的制备原料按重量份计,包括:有效成分8份、油性液体10份、水溶性包衣材料4份、扩散剂3份、分散剂1份、载体补足至100份;所述有效成分为氯硝柳胺乙醇胺盐,所述载体为热活化凹凸棒石,当热活化时,在250℃加热活化,所述载体的形状为类球形,所述载体的粒径范围为1~3mm,所述油性液体选自酯类液体,所述酯类液体选自油酸甲酯,所述扩散剂包括有机硅聚氧乙烯醚DM-MSD9196和烷基酚聚氧乙烯醚OP-9,重量比为3:1,所述分散剂包括木质素磺酸钙和EO-PO嵌段共聚物RPE1740,重量比为3:1,所述水溶性包衣材料选自聚乙烯醇PVA 2088和聚乙烯吡咯烷酮PVP K17,重量比为1:0.2。
本例还提供如上所述的颗粒剂的制备方法,包括:
吸附性药液制备:将有效成分、油性液体、润湿剂、分散剂共混,研磨,得到粒径D90小于3μm的吸附性药液;
载体吸附:将载体放入搅拌机中,喷洒吸附性药液,搅拌吸附,得到负载药液;
包衣:将负载药液放入包衣机中,将水溶性包衣材料溶于无水乙醇后喷入包衣机包衣、烘干,得到所述颗粒剂。
实施例5
本例提供一种颗粒剂,颗粒剂的制备原料按重量份计,包括:有效成分8份、油性液体10份、水溶性包衣材料4份、扩散剂3份、分散剂1份、载体补足至100份;所述有效成分为氯硝柳胺乙醇胺盐,所述载体为热活化凹凸棒石,当热活化时,在250℃加热活化,所述载体的形状为类球形,所述载体的粒径范围为1~3mm,所述油性液体选自酯类液体和植物油,重量比为1:0.3,所述酯类液体选自油酸甲酯,所述植物油选自大豆油,所述扩散剂包括有机硅聚氧乙烯醚DM-MSD9196,所述分散剂包括木质素磺酸钙,所述水溶性包衣材料选自聚乙烯醇PVA 2088和聚乙烯吡咯烷酮PVP K17,重量比为1:0.2。
本例还提供如上所述的颗粒剂的制备方法,包括:
吸附性药液制备:将有效成分、油性液体、润湿剂、分散剂共混,研磨,得到粒径D90小于3μm的吸附性药液;
载体吸附:将载体放入搅拌机中,喷洒吸附性药液,搅拌吸附,得到负载药液;
包衣:将负载药液放入包衣机中,将水溶性包衣材料溶于无水乙醇后喷入包衣机包衣、烘干,得到所述颗粒剂。
性能评价
1、飞防测试:将实施例1提供的颗粒剂进行飞防测试,其中飞行高度为3.5米-4米,速度为5米/秒进行颗粒剂的喷洒,其中喷洒到地面的颗粒剂如图1颗粒所示,其中从图1可知,本发明颗粒剂喷洒均匀,且颗粒剂之间彼此不粘结,且喷洒8h过程中,喷洒口未发生堵塞等问题,运行良好。
2、流动性:观察实施例1~5提供的颗粒剂分别在23℃,和54℃存储14天后的流动性,其中优为流动性好,无粘结,良为流动性较好,有小于2%颗粒剂粘结,中为流动性一般,有2~5%颗粒剂粘结,差为流动性差,有大于5%颗粒剂粘结,结果见表1。
3、脱落率:将实施例1~5提供的颗粒剂在振动频率150次/min条件下振动30min后,测试振动前后的质量为m0和m1,则脱落率为(m0-m1)/m0*100%,结果见表1。
4、性能测试:测试实施例1~3的水分和堆积密度,发现水分<3%,堆积密度为1.1~1.5g/mL。
表1性能表征测试
由表1测试结果可知,本发明提供的颗粒剂具有好的控释性能,当用于飞防作业时,可避免堵塞开口以及粉尘飞扬等问题,可提高颗粒剂撒施的效率,减少人工成本。
应理解,本文中描述的实施方式应仅在描述的意义上考虑且不用于限制的目的。各实施方式内的特征、优点或方面的描述应被认为可用于其它实施方式中的其它类似特征、优点或方面。
Claims (10)
1.一种飞防用控释型颗粒剂,其特征在于,所述颗粒剂的制备原料按重量份计,包括:有效成分5~40份、油性液体5~30份、水溶性包衣材料0.5~5份、载体补足至100份。
2.根据权利要求1所述的飞防用控释型颗粒剂,其特征在于,所述载体的形状为球形或类球形。
3.根据权利要求1所述的飞防用控释型颗粒剂,其特征在于,所述载体的粒径范围为1~3mm。
4.根据权利要求1所述的飞防用控释型颗粒剂,其特征在于,所述油性液体选自酯类液体、矿物油、植物油、酯化植物油中的一种或多种。
5.根据权利要求4所述的飞防用控释型颗粒剂,其特征在于,所述酯类液体为链状酯类液体,所述酯类液体的碳原子数为10~25。
6.根据权利要求1所述的飞防用控释型颗粒剂,其特征在于,所述植物油选自玉米油、菜籽油、大豆油、椰子油、葵花籽油中的一种或多种。
7.根据权利要求1所述的飞防用控释型颗粒剂,其特征在于,所述水溶性包衣材料选自羟丙基甲基纤维素、羟基丙基纤维素、聚乙烯吡咯烷酮、聚维酮、聚乙烯醇中的一种或多种。
8.根据权利要求1~7任意一项所述的飞防用控释型颗粒剂,其特征在于,所述颗粒剂的制备原料按重量份计,还包括扩散剂1~5份、分散剂0.1~3份。
9.根据权利要求8所述的飞防用控释型颗粒剂,其特征在于,所述扩散剂包括有机硅聚氧乙烯醚、烷基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚中的至少一种。
10.一种根据权利要求8或9所述的飞防用控释型颗粒剂的制备方法,其特征在于,包括:
吸附性药液制备:将有效成分、油性液体、润湿剂、分散剂共混,研磨,得到粒径D90小于3μm的吸附性药液;
载体吸附:将吸附性药液和载体搅拌吸附,得到负载药液;
包衣:将负载药液放入包衣机中,加入水溶性包衣材料包衣,得到所述颗粒剂。
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