CN115443990A - 含苯唑草酮钾盐的可溶液剂及其制备方法 - Google Patents
含苯唑草酮钾盐的可溶液剂及其制备方法 Download PDFInfo
- Publication number
- CN115443990A CN115443990A CN202211054645.4A CN202211054645A CN115443990A CN 115443990 A CN115443990 A CN 115443990A CN 202211054645 A CN202211054645 A CN 202211054645A CN 115443990 A CN115443990 A CN 115443990A
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- CN
- China
- Prior art keywords
- topramezone
- potassium salt
- solubles
- synergist
- soluble solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 title claims abstract description 35
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Classifications
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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
- A01N25/02—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 liquids as carriers, diluents or solvents
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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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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
本发明属于农药领域,具体涉及一种含苯唑草酮钾盐的可溶液剂及其制备方法,含苯唑草酮钾盐的可溶液剂,其中所述可溶液剂包括以下组分:以苯唑草酮表示的1‑30重量%的苯唑草酮钾盐、40‑80重量%的水分、1‑40重量%的增效剂、0.001‑0.2重量%的色素、1‑10重量%的防冻剂、0.1‑1重量%的防腐剂;本体系是真溶液体系,制剂本身稳定不会出现分层、沉淀等情况,具有更加优良的性状;将苯唑草酮做成钾盐更有利于植物的吸收,较大的提高了药效,降低了用量,易于添加环境友好的增效剂,更能发挥原药本身的优势。
Description
技术领域
本发明涉及农药领域,具体而言涉及一种含苯唑草酮钾盐的可溶液剂及其制备方法。
背景技术
苯唑草酮(topramezone)又称苯吡唑草酮,是一种高选择性苯甲酯吡唑酮类除草剂,具有高安全性、优良选择性、广谱杀草活性、时效长和兼容性强等特点,安全性高于硝磺草酮和烟嘧磺隆,是安全性最高的玉米地除草剂,也是对哺乳动物毒性最小的除草剂之一。其化学名称为4-[3-(4,5-二氢异噁唑-3-基)-2-甲基-4-甲基磺酰基]-1-甲基-5-羟基-1H-吡唑,其结构式如下:
苯唑草酮可以被植物的叶、根和茎吸收,主要用于防治玉米田一年生禾本科杂草如马唐、稗草、野稷、狗尾草、牛筋草、异型莎草等,阔叶杂草如苋、藜、田旋花、苘麻、蓼、龙葵、野芥、鸭跖草等,还能有效稳定地防治那些已经对三嗪类除草剂产生抗性的阔叶杂草。
苯唑草酮原药(97%)外观为白色粉末状,在水和有机溶剂中溶解度都比较小:水(20℃,pH 3.1)510mg/L;丙酮、乙腈、乙酸乙酯、正庚烷、异丙醇、甲醇、正辛醇、甲苯(g/L,20℃)<10mg/L。
通常情况下将苯唑草酮加工成为悬浮剂和油悬浮剂,加工工艺复杂,成本高,而且悬浮剂体系是热力学不稳定体系容易出现分层、沉淀等现象,制剂的质量不容易保障。为保证制剂质量,我们对苯唑草酮制剂及其制备工艺进行了研究。
发明内容
根据一个方面,本发明提供一种含苯唑草酮钾盐的可溶液剂,所述可溶液剂包含以苯唑草酮表示的1-30重量%的苯唑草酮钾盐、40-80重量%的水分、以及一种或多种选自增效剂、色素、防腐剂和防冻剂的添加助剂。
根据一个具体的实施方案,本发明提供一种由苯唑草酮钾盐、色素、水分、防腐剂、防冻剂及增效剂的苯唑草酮钾盐可溶液剂,其中各组分的含量如下,以重量百分含量表示:
苯唑草酮:1%-30%
氢氧化钾:0.1%-6%
增效剂:1%-40%
色素:0.001-0.2%
防冻剂:1%-10%
防腐剂:0.1%-1%
水:40%-80%
根据另一方面,本发明提供一种制备所述含苯唑草酮钾盐的可溶液剂的方法,其包括以下步骤:
(1)根据配方加入定量的水、再加入定量的苯唑草酮原粉,开启搅拌;
(2)根据配方加入定量的氢氧化钾,搅拌至苯唑草酮原粉完全溶解,继续加入氢氧化钾调整pH7~9;
(3)根据配方加入定量的增效剂;
(4)根据配方加入定量的色素、防冻剂、防腐剂等功能助剂;
(5)根据配方加入剩余的水,充分搅拌后制成可溶液剂。
根据再一方面,本发明提供一种包装产品,在200mL、500mL、1000mL PE瓶中罐装含苯唑草酮钾盐的可溶液剂。
本发明提供一种含苯唑草酮钾盐的可溶液剂,其包含苯唑草酮表示的1-30重量%的苯唑草酮钾盐、40-80重量%的水分、1-40重量%的增效剂、0.001-0.2重量%的色素、1-10重量%的防冻剂、0.1-1重量%的防腐剂。
在本发明中,所用的增效剂是聚氧乙烯月桂醚、蓖麻油聚氧乙烯醚、牛脂氨聚氧乙烯醚、油酸聚氧乙烯脂、十二醇聚氧乙烯醚、C12-C15烷基糖苷、季胺葡萄糖苷、甲基化聚氧乙烯脂肪酸、十八烷基羧酸甜菜碱、十六烷基二甲基胺基丙基甜菜碱、十八烷基胺氧化物、C12-C15烷基醇聚氧乙烯醚硫酸盐、脂肪醇环氧乙烷加成物磺酸盐、油酰基甲基牛磺酸钠盐等增效剂中的一种或多种,以苯唑草酮钾盐的可溶液剂的总重量计,增效剂的用量可以是1-40%,优选10-30%。
在本发明中,所用的色素可以是任何农药领域中常用的能够起到区别警示作用的色素,例如是胭脂红,以苯唑草酮钾盐的可溶液剂的总重量计,色素的用量可以是0.001-0.2%,优选是0.001-0.05%。
在本发明中,所用的防冻剂可以是任何农药领域中常用的防冻剂,例如是乙二醇,以苯唑草酮钾盐的可溶液剂的总重量计,防冻剂的用量可以是1-10%,优选2-5%。
在本发明中,所用的防腐剂可以是任何农药领域中常用的防腐剂,例如是卡松,以苯唑草酮钾盐的可溶液剂的总重量计,防腐剂的用量可以是0.1-10%,优选0.1-0.5%。
下面对本发明的方法进行具体描述。
根据配方先将符合要求的定量水、再加入1-30重量%苯唑草酮原药,在反应釜中开启搅拌;
根据配方加入0.1-6重量%氢氧化钾,搅拌至苯唑草酮完全溶解,继续加入0.1~2重量%氢氧化钾调整pH7~9;
根据配方加入1-40重量%聚氧乙烯月桂醚、蓖麻油聚氧乙烯醚、牛脂氨聚氧乙烯醚、油酸聚氧乙烯脂、十二醇聚氧乙烯醚、C12-C15烷基糖苷、季胺葡萄糖苷、甲基化聚氧乙烯脂肪酸、十八烷基羧酸甜菜碱、十六烷基二甲基胺基丙基甜菜碱、十八烷基胺氧化物、C12-C15烷基醇聚氧乙烯醚硫酸盐、脂肪醇环氧乙烷加成物磺酸盐、油酰基甲基牛磺酸钠盐一种或多种增效剂;
根据配方加入0.001-0.2重量%色素、1-5重量%防冻剂、0.1-1重量%防腐剂等功能助剂;
根据配方加入剩余水,充分搅拌后制成可溶液剂。
本专利中,通过加入氢氧化钾,将不易溶于水的苯唑草酮转化成为易溶于水的苯唑草酮钾盐,再加入增效剂、防冻剂、色素、防腐剂等功能助剂,制成苯唑草酮钾盐可溶液剂。
另一方面,本发明提供一种包装产品,在200mL、500mL、1000mL PE瓶中罐装含苯唑草酮钾盐的可溶液剂。
本发明提供一种除草效果好、生产和使用安全性高的含苯唑草酮钾盐的可溶液剂。本发明的优势在于:
本体系是真溶液体系,制剂本身稳定不会出现分层、沉淀等情况,具有更加优良的性状;
将苯唑草酮做成钾盐更有利于植物的吸收,较大的提高了药效,降低了用量,符合国家的产业政策;
易于添加环境友好的增效剂,更能发挥原药本身的优势。
以下通过实施例进一步说明本发明,但本发明绝不仅限于以下实施例。除非另外指明,配方中百分比均为重量百分比。
具体实施方式
以下实施例使用的是苯唑草酮是98%苯唑草酮原粉。
实施例1:苯唑草酮钾盐溶液制备
取2800kg水加入到5000L反应釜中,开启搅拌;加入163.3kg98%苯唑草酮原粉;再加入26kg氢氧化钾,搅拌至苯唑草酮原粉完全溶解,再加入2kg氢氧化钾调整pH7~9,制得苯唑草酮溶液。
实施例2:增效剂的添加
取80kg蓖麻油聚氧乙烯醚、200kg牛脂氨聚氧乙烯醚、400kgC12-C15烷基糖苷、120kgC12-C15烷基醇聚氧乙烯醚硫酸盐加入到实施例1的反应釜中,搅拌90分钟,使增效剂完全溶解。
实施例3:功能助剂的添加
取160kg乙二醇、6kg卡松、0.4kg胭脂红加入到实施例2的反应釜中,搅拌30分钟,使功能助剂完全溶解。
实施例4:苯唑草酮钾盐可溶液剂制备
取42.3kg水加入到实施例3的反应釜中,搅拌60分钟,使成为均匀一致的溶液,制得4%苯唑草酮钾盐可溶液剂。
实施例5:苯唑草酮钾盐可溶液剂的检测
实施例4中苯唑草酮钾盐可溶液剂制备完成后,从反应釜罐口取样,进行分析。分析结果如下:
表1实施例4中苯唑草酮钾盐可溶液剂的取样分析
实施例6:苯唑草酮钾盐可溶液剂包装产品的制备
取实施例4中苯唑草酮钾盐可溶液剂,分别装入200mL、500mL、1000mL PE瓶中,热熔封口。按照农药通用标准方法GB/T 19136-2003农药热贮稳定性测定方法,进行热贮稳定性试验,结果如下:
表2实施例4中苯唑草酮钾盐可溶液剂热贮稳定性试验
以上数据表明,200mL、500mL、1000mL PE瓶可以作为施例4中苯唑草酮钾盐可溶液剂的包装材料使用。
4%苯唑草酮钾盐可溶液剂防除春玉米田杂草田间药效试验报告
试验目的:明确4%苯唑草酮钾盐可溶液剂在不同施用剂量的情况下,防除春玉米田杂草的效果、杀草谱、安全性及施用技术等项指标。
试验条件:玉米垄作,机械播种,播种量为40kg/hm2。
作物和栽培品种的选择:玉米,品种为吉单558,此品种为吉林省中部主要栽培品种,具有区域代表性。
试验对象杂草的选择:稗草(Echinochloa crus-galli(L)Beauv),狗尾草(Setaria viridis(l)Beauv),马唐(Digitaria adscendens(H.B.K.)),藜(Chenopodiumaldum L.),反枝苋(Amaranthus retroflexus L),柳叶刺蓼(Polygonum bungeanumTurcz.),铁苋菜(Acalypha australis L.),鸭跖草(Commelina communis L.),风花菜[Rorippa islandica(Oed)Borb.],猪毛菜(Salsola collinapall.),马齿苋(Portulacaoleracea L.),野西瓜苗(Hibiscus trionum L.),葎草[Humulus scandens(Lour)Merr.],荠菜(Capsella bursa-pastoris Medic.),苣荬菜(Sonchus brachyotus DC.),问荆(Equisetum arvenseL.),山苦菜[Ixeris chinensis(Thunb.)Nakai.],稀莶(Siegesbeckia orientalis L.),小蓟(Cirsium segetum Bge.),地肤[Kochia scoparia(L)Schrad.],豚草(Ambrosia artemisiifolia L.),苍耳(Xanthium sibiricumPatrin.),扁蓄(Polygonum aviculare L.),苘麻(Abutilon theophrasti Medic.),龙葵(Solanum nigrum L.),水棘针(Amethystea caerulea L.)
栽培条件:试验地设在吉林省农业科学院公主岭试验地,土壤为黑壤土,pH值为7.0左右,有机质含量2.2%左右。前茬作物为玉米,没有使用除草剂。
其他条件:玉米垄作,垄距65cm,秋翻春起垄,为东北主要栽培方式。
试验设计和安排
试验药剂:苯唑草酮钾盐;含量:4%;剂型:可溶液剂;生产厂家:济南绿霸农药有限公司。
对照药剂:苯唑草酮;含量:30%;剂型:悬浮剂;生产厂家:巴斯夫欧洲公司。设人工除草和空白对照处理。
供试药剂试验设计,如下表:
表3供试药剂试验设计
小区排列,如下表:
表4小区排列情况
1 | 2 | 3 | 4 | 5 | 6 | 7 |
6 | 7 | 1 | 2 | 3 | 4 | 5 |
4 | 5 | 6 | 7 | 1 | 2 | 3 |
3 | 4 | 5 | 6 | 7 | 1 | 2 |
小区面积和重复:小区面积:20m2;重复次数:4次。
使用方法:按实验设计准确量取药剂(精确至0.05mL),加入试验用喷雾器中,每个处理加水3L,采用扇形喷头,喷头垂直地面,距作物25-30㎝,均匀喷雾处理,将全部药液喷完。
施药器械:“利农HD400”背负式喷雾器为新加坡利农私人有限公司生产的除草剂专用喷雾器,药液箱容量为16L,聚丙烯材料活塞式泵,扁扇型喷头,喷杆与胶管总长度为1.95m,喷射速率每分钟810mL,工作压力5Kg/cm2,处理时喷头距离作物约25cm,喷幅80cm。
施药时间和次数:施药日期是2021年6月1日,玉米3-5片叶,杂草2-5叶。
使用量:每亩实际用水量是25L,制剂实际亩用量分别为40、50、60、100g。
防治病虫和非靶标杂草药剂资料:无
气象资料:2021年6月1日,晴,8~22℃,无持续风向≤3级,天气情况有利于药效正常发挥作用。
田间管理资料:施肥:播种时一次性施足底肥,不追肥,整个栽培过程未灌溉。人工除草时间为6月7日,6月24日,二次。
杂草调查时间和次数:调查3次,时间是2021年6月16日,7月1日,7月16日。
调查方法:采用绝对值调查法,用人工制作的0.25m2铁框,每小区调查3点,随机取点,调查记载心叶没有死亡的杂草种类、数量。并对所调查的不同种类杂草数量进行方差分析,添加到防效后。小区杂草群落主要由稗草、藜、鸭趾草、风花菜、蓼、龙葵、苘麻、猪毛菜、小蓟组成。
药效计算方法:防治效果(%)=[1-PT/CK]×100
作物调查时间和次数:调查四次,时间是2021年6月1日,6月11日,6月21日,7月1日。
调查方法:药后10、20、30、40d目测玉米出苗、拔节、抽雄、生长、株高等生物性状,是否有药害发生并做记录,秋后每小区20㎡测实产。
药害的分级方法按GB/T17980.42-2000进行,具体如下:
1级:作物生长正常,无任何受害症状;
2级:作物轻微药害,药害少于10%;
3级:作物中等药害,以后能恢复,不影响产量;
4级:作物药害较重,难以恢复,造成减产。
5级:作物药害严重,不能恢复,造成明显减产或绝产。
对其他生物影响
作物产量和质量,如下表:
表5作物产量和质量情况
处理 | 产量kg/h㎡ | 增产(%) | 药害等级 |
1 | 5425 | -4.41 | 1 |
2 | 5720 | 0.79 | 1 |
3 | 5915 | 4.23 | 1 |
4 | 5825 | 2.64 | 2 |
5 | 5730 | 0.97 | 1 |
6 | 5675 | - | - |
7ck | 3050 | -46.26 | - |
结果与分析,如下表:
表6对各种杂草防效%及差异显著性情况
注:1、其它包括龙葵、苘麻、猪毛菜、小蓟等阔叶杂草。2、表中差异显著性为试验田小区内
调查的杂草株数或鲜重所做的方差分析,5%差异显著性,下表同。
4%苯唑草酮钾盐SL防治效果(%)——施药后30d,结果如下表:
表7施药后30d 4%苯唑草酮钾盐SL防治效
4%苯唑草酮钾盐SL防治效果(%)——施药后45d,结果如下表:
表8施药后45d4%苯唑草酮钾盐SL防治效果
4%苯唑草酮钾盐SL是一种能够抑制羟基苯基丙酮酸酯双氧化酶(HPPD)的芽前和苗后广谱选择性除草剂,其酮容易在植物木质部和韧皮部传导,具有触杀作用和持效性,可被植物的根和茎叶吸收,导致酪氨酸的积累,使质体醌和生育酚的生物合成受阻,进而影响到类胡萝卜素的生物合成,杂草茎叶白化后死亡,可有效防治主要的阔叶草和一些禾本科杂草,玉米能快速地将苯唑草酮降解为无活性化合物。
使用方法:玉米苗后3-5叶期,杂草出齐,一般杂草2-5叶期施药,适宜用量为:杂草基数低的田块为24g/hm2(有效成分用量),一般田块施用30g/hm2(有效成分用量),杂草基数大的可施用36g/hm2(有效成分用量)。,选择风力小于3级的天气,每公顷对水375L,茎叶喷雾处理,喷雾要求均匀一致,不得漏喷和重喷。可有效防除稗草、藜、鸭趾草、风花菜、蓼等杂草,对其它阔叶杂草(龙葵、苘麻、猪毛菜、小蓟)亦有较好防效;对稗草有一定防效,但明显低于对阔叶杂草防效。本年度试验中,药后15d调查,试验药剂不同梯度处理对各种杂草的综合防效幅度为90.2%~98.7%;药后30d调查,对各种杂草的株数综合防效幅度为89.6%~100.0%,鲜重防效幅度为94.1%~100.0%;药后45d调查,对各种杂草的株数综合防效幅度为82.9%~99.5%。
安全性:倍剂量区部分玉米叶片出现淡紫色斑点,10-15d恢复,其它未见对玉米生长发育及产量有不良影响,测产结果表明,试验各处理与人工除草相比较增产幅度为-4.41%~4.23%。
Claims (10)
1.一种含苯唑草酮钾盐的可溶液剂,其特征在于,所述可溶液剂包含以苯唑草酮表示的1-30重量%的苯唑草酮钾盐、40-80重量%的水分、以及一种或多种选自增效剂、色素、防腐剂和防冻剂的添加助剂。
2.根据权利要求1所述的含苯唑草酮钾盐的可溶液剂,其特征在于,其中所述可溶液剂包括以下组分:以苯唑草酮表示的1-30重量%的苯唑草酮钾盐、40-80重量%的水分、1-40重量%的增效剂、0.001-0.2重量%的色素、1-10重量%的防冻剂、0.1-1重量%的防腐剂。
3.根据权利要求1或2所述的含苯唑草酮钾盐的可溶液剂,其特征在于,其中所述增效剂包含聚氧乙烯月桂醚、蓖麻油聚氧乙烯醚、牛脂氨聚氧乙烯醚、油酸聚氧乙烯脂、十二醇聚氧乙烯醚、C12-C15烷基糖苷、季胺葡萄糖苷、甲基化聚氧乙烯脂肪酸、十八烷基羧酸甜菜碱、十六烷基二甲基胺基丙基甜菜碱、十八烷基胺氧化物、C12-C15烷基醇聚氧乙烯醚硫酸盐、脂肪醇环氧乙烷加成物磺酸盐、油酰基甲基牛磺酸钠盐的一种或多种;其中所述增效剂含量为1-40重量%。
4.根据权利要求1或2所述的含苯唑草酮钾盐的可溶液剂,其特征在于,其中所述色素含量为0.001-0.2重量%。
5.根据权利要求1或2所述的含苯唑草酮钾盐的可溶液剂,其特征在于,其中所述防冻剂含量为1-10重量%。
6.根据权利要求1或2所述的含苯唑草酮钾盐的可溶液剂,其特征在于,其中所述防腐剂含量为0.1-1重量%。
7.制备根据权利要求1所述的含苯唑草酮钾盐的可溶液剂的方法,其特征在于,所述方法包括以下步骤:
(1)将苯唑草酮原粉在水中均匀分散;
(2)加入氢氧化钾,使苯唑草酮原粉完全溶解,并调整pH7~9;
(3)加入增效剂、色素、防冻剂、防腐剂等功能助剂,充分搅拌后制成可溶液剂。
8.制备根据权利要求7所述的含苯唑草酮钾盐的可溶液剂的方法,其特征在于,所述方法包括以下步骤:
(1)根据配方加入定量的水、再加入定量的苯唑草酮原粉,开启搅拌;
(2)根据配方加入定量的氢氧化钾,搅拌至苯唑草酮原粉完全溶解,继续加入氢氧化钾调整pH7~9;
(3)根据配方加入定量的增效剂;
(4)根据配方加入定量的色素、防冻剂、防腐剂等功能助剂;
(5)根据配方加入剩余的水,充分搅拌后制成可溶液剂。
9.根据权利要求7或8所述方法,其特征在于,其所述制备过程在反应釜中进行。
10.一种包装产品,其在200mL、500mL、1000mLPE瓶中罐装包括根据权利1-6之一所述的含苯唑草酮钾盐的可溶液剂或者根据权利7-8所述方法制备的含苯唑草酮钾盐的可溶液剂。
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