CN116686831A - 一种含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂及其制备方法和应用 - Google Patents
一种含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂及其制备方法和应用 Download PDFInfo
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- SYJGKVOENHZYMQ-UHFFFAOYSA-N Penoxsulam Chemical compound N1=C2C(OC)=CN=C(OC)N2N=C1NS(=O)(=O)C1=C(OCC(F)F)C=CC=C1C(F)(F)F SYJGKVOENHZYMQ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- YLPGTOIOYRQOHV-UHFFFAOYSA-N Pretilachlor Chemical compound CCCOCCN(C(=O)CCl)C1=C(CC)C=CC=C1CC YLPGTOIOYRQOHV-UHFFFAOYSA-N 0.000 title claims abstract description 26
- BGNQYGRXEXDAIQ-UHFFFAOYSA-N Pyrazosulfuron-ethyl Chemical group C1=NN(C)C(S(=O)(=O)NC(=O)NC=2N=C(OC)C=C(OC)N=2)=C1C(=O)OCC BGNQYGRXEXDAIQ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title abstract description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 36
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- MQKXWEJVDDRQKK-UHFFFAOYSA-N bis(6-methylheptyl) butanedioate Chemical compound CC(C)CCCCCOC(=O)CCC(=O)OCCCCCC(C)C MQKXWEJVDDRQKK-UHFFFAOYSA-N 0.000 description 1
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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
- 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
- A01N37/18—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/22—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G22/00—Cultivation of specific crops or plants not otherwise provided for
- A01G22/20—Cereals
- A01G22/22—Rice
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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
- A01N25/30—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 characterised by the surfactants
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- A—HUMAN NECESSITIES
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- 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
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
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- A—HUMAN NECESSITIES
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- 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
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- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
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- A—HUMAN NECESSITIES
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- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
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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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Abstract
本发明涉及农业领域,具体涉及一种含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂及其制备方法和应用。所述水分散片剂包括丙草胺原药、吡嘧磺隆原药、五氟磺草胺原药、聚羧酸钠盐分散剂、硫酸盐类润湿剂、白炭黑、腰果酚聚氧乙烯醚乳化剂、柠檬酸、碳酸氢钠、粘结剂、润滑剂和载体。本发明还涉及所述水分散片剂的制备方法和防除水稻田杂草的用途。
Description
技术领域
本发明涉及农业领域,具体涉及一种含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂及其制备方法和应用。
背景技术
稻田除草是水稻种植的一大难题,化学除草是目前控制杂草的主要手段。近年来,由于一些除草剂品种大面积使用,已经导致很多杂草产生了抗药性。现有技术中的除草剂已不能有效解决稻田杂草。
吡嘧磺隆属于磺酰脲类除草剂,为选择性内吸传导型除草剂,主要通过根系被吸收,在杂草植株体内迅速转移,抑制生长,杂草逐渐死亡。水稻能分解该药剂,对水稻生长几乎没有影响,可以防除一年生和多年生阔叶杂草和莎草科杂草。
丙草胺是选择性芽前除草剂,细胞分裂抑制剂。用于土壤处理,可防除稻田稗草、异型莎草、牛毛毡、鸭舌草、窄叶泽泻等。其作用机理为杂草通过中下胚轴和胚芽鞘吸收药剂,干扰蛋白质合成,对杂草的光合作用和呼吸作用也有间接影响。
五氟磺草胺为传导型除草剂,经茎叶、幼芽及根系吸收,通过木质部和韧皮部传导至分生组织,抑制植株生长。五氟磺草胺为稻田用广谱除草剂,适用于水稻的旱直播田、水直播田、秧田以及抛秧、插秧栽培田。
在先发明CN109526975A公开了含有吡嘧磺隆、丙草胺和五氟磺草胺的水分散片剂,但是该水分散片剂在入水的分散性、崩解性等方面还有待进一步改善。从省力化考虑,本领域持续存在制备分散性等制剂性能优异的水分散片剂的客观需求。
发明内容
为解决现有技术存在的问题,本发明人在前期研究的基础上,通过进一步的配方筛选,主要是表面活性成分的筛选,获得了在分散性、悬浮性等各方面性能优异的水分散片剂制剂配方,基于此完成了本发明。
本发明一方面涉及一种含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂,所述水分散片剂由如下组分及其重量百分含量组成:
丙草胺原药 15%
吡嘧磺隆原药 2%
五氟磺草胺原药1%
聚羧酸钠盐分散剂2.0%
硫酸盐类润湿剂1.5%
白炭黑15%
腰果酚聚氧乙烯醚乳化剂10%
柠檬酸20%
碳酸氢钠20%
粘结剂 5%
润滑剂2%
载体补足100%
其中,
所述聚羧酸钠盐分散剂为Geropon T/36;
所述硫酸盐类润湿剂为Geropon L-WET/P;
所述腰果酚聚氧乙烯醚乳化剂为NSAE-10。
在本发明所述的水分散片剂中,所述粘结剂选自淀粉、糊精、羧甲基纤维素、羧乙基纤维素、明胶、阿拉伯胶、黄原胶中的一种或多种,优选糊精。
在本发明所述的水分散片剂中,所述润滑剂选自滑石粉或硬脂酸镁,优选硬脂酸镁。
在本发明所述的水分散片剂中,所述载体选自无水硫酸钠、尿素、高岭土中的一种或多种,优选无水硫酸钠。
在本发明中,通过选用合适的表面活性成分,如乳化剂、分散剂、润湿剂配伍及其用量配比,辅以其他助剂,使得制备的水分散片剂在悬浮率等各方面方面性能优异。
本发明另一方面涉及本发明所述的一种含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂的制备方法,其包含如下步骤:
将丙草胺原药与腰果酚聚氧乙烯醚乳化剂混合均匀,然后加入吸附剂白炭黑进行吸附;然后,向其中加入吡嘧磺隆原药、五氟磺草胺原药、聚羧酸钠盐分散剂、硫酸盐类润湿剂、载体,混合均匀并气流粉碎;然后,依次加入柠檬酸、润滑剂、碳酸氢钠混合均匀,加入粘结剂造粒、筛分、压片、干燥,即得。
本发明另一方面涉及本发明所述的一种含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂用于防除水稻田杂草的用途。
其中,所述水稻田杂草包括稗草、千金子、双穗雀稗、稻李氏禾、鸭舌草、水竹叶、耳叶水苋、丁香蓼、水花生,陌上菜、慈姑、雨久花、泽泻、节节菜、异型莎草、萤蔺、水三棱、牛毛毡、日照漂浮草等多种稻常见杂草。优选稗草、雨久花、异型莎草。
本发明的有益效果
本发明通过选用合适的表面活性成分,如乳化剂、分散剂、润湿剂配伍及其用量配比,辅以其他助剂,使得制备的水分散片剂在悬浮率等各方面方面性能优异。
另外,本发明水分散片剂在稻田杂草防治中表现出优异的效果。
具体实施方式
下面结合具体实施方式对本发明的技术方案进行说明,但本发明并不限制于此。
一、助剂配伍筛选
通过下述正交试验筛选乳化剂、润湿剂、分散剂的最佳配伍。其中,所供筛选的助剂如下:
乳化剂:十二烷基苯磺酸钙; NSAE-10(腰果酚聚氧乙烯醚), Genapol X080(脂肪醇聚氧乙烯醚);
润湿剂:十二烷基硫酸钠;丁二酸二异辛酯磺酸钠;Geropon L-WET/P(硫酸盐类);
分散剂:Geropon T/36(聚羧酸钠盐);木质素磺酸钠;拉开粉BX(烷基萘基硫酸钠盐);
具体为:将15g丙草胺原药与2g乳化剂混合均匀,然后加入15g白炭黑进行吸附;然后,向其中加入2g吡嘧磺隆原药、1g五氟磺草胺原药、2g分散剂、2g润湿剂、无水硫酸钠补足100g,混合均匀并气流粉碎得粉状物,测定其悬浮率。
其中,悬浮率的测定方法为:取样品2g,加入盛有100 mL 标准硬水(342mg/L)的烧杯中用玻璃棒搅匀,然后用标准硬水全部洗入250 mL量筒中,并稀释至刻度,盖上塞子,以量筒底部为轴心,将量筒在1 min内上下颠倒30次。打开塞子,垂直放入30℃ 的恒温水浴中,放置30 min。然后用吸管将内容物的9/10(225 mL)移除,抽液时吸管沿量筒内壁随液面下降而下移,避免下部沉淀物搅动。测定试样和留在量筒底部25 mL悬浮液中有效成分的含量。试验设3次重复。按照下式计算样品悬浮率:
悬浮率 = [(m1-m2)/m1] × (10/9)
式中:
m1代表悬浮液试样中有效成分质量;
m2代表留在量筒底部25 mL悬浮液中有效成分质量;
测定结果如下表所示。
表1 乳化剂、润湿剂、分散剂最佳配伍筛选结果
上述结果显示,当乳化剂选择NSAE-10,润湿剂选择Geropon L-WET/P,以及分散剂选择Geropon T/36时,悬浮率最大,为76.5%。因此,确定其为最佳配伍。
二、乳化剂、润湿剂、分散剂最佳用量筛选
将15g丙草胺原药与不同用量的NSAE-10混合均匀,然后加入15g白炭黑进行吸附;然后,向其中加入2g吡嘧磺隆原药、1g五氟磺草胺原药、不同用量的Geropon L-WET/P、不同用量的Geropon T/36、无水硫酸钠补足100g,混合均匀并气流粉碎得粉状物,测定其悬浮率。其中,NSAE-10、Geropon L-WET/P、Geropon T/36的用量如下表2所示。
其中,悬浮率的测定方法同上。结果如下表所示。
表2最佳用量筛选结果
序号 | NSAE-10(g) | Geropon L-WET/P(g) | Geropon T/36(g) | 悬浮率(%) |
1 | 9 | 1.5 | 3 | 84.2 |
2 | 9 | 2.5 | 2 | 88.0 |
3 | 10 | 0.5 | 3 | 78.9 |
4 | 10 | 1.5 | 2 | 93.6 |
5 | 11 | 0.5 | 2 | 86.7 |
6 | 11 | 1.5 | 1 | 81.3 |
上述结果显示,当乳化剂NSAE-10的用量为10%,润湿剂Geropon L-WET/P的用量为1.5%,分散剂Geropon T/36的用量为2%时,配方的悬浮率最大,为93.6%。因此,NSAE-10的用量为10%,润湿剂Geropon L-WET/P的用量为1.5%,分散剂Geropon T/36的用量为2%是优选的。
三、制剂实施例
实施例1
水分散片剂配方为:丙草胺原药150g、吡嘧磺隆原药20g、五氟磺草胺原药10g、Geropon T/36为20g、Geropon L-WET/P 15g、白炭黑150g、NSAE-10为100g、柠檬酸200g、碳酸氢钠200g、糊精 50g、硬脂酸镁20g、无水硫酸钠 补足1000g。
制备方法为:将丙草胺原药与NSAE-10混合均匀,然后加入吸附剂白炭黑进行吸附;然后,向其中加入吡嘧磺隆原药、五氟磺草胺原药、Geropon T/36、Geropon L-WET/P、无水硫酸钠,混合均匀并气流粉碎;然后,依次加入柠檬酸、硬脂酸镁、碳酸氢钠混合均匀,加入糊精水溶液造粒、筛分、压片、干燥,即得。
实施例2:
水分散片剂配方为:丙草胺原药150g、吡嘧磺隆原药20g、五氟磺草胺原药10g、Geropon T/36为20g、Geropon L-WET/P 15g、白炭黑150g、NSAE-10为100g、柠檬酸200g、碳酸氢钠200g、羧甲基纤维素50g、滑石粉20g、无水硫酸钠 补足1000g。
制备方法同实施例1。
实施例3:
水分散片剂配方为:丙草胺原药150g、吡嘧磺隆原药20g、五氟磺草胺原药10g、Geropon T/36为20g、Geropon L-WET/P 15g、白炭黑150g、NSAE-10为100g、柠檬酸200g、碳酸氢钠200g、阿拉伯胶50g、硬脂酸镁20g、高岭土 补足1000g。
制备方法同实施例1。
对比例1:
水分散片剂配方为:丙草胺原药150g、吡嘧磺隆原药20g、五氟磺草胺原药10g、Geropon T/36为20g、十二烷基硫酸钠15g、白炭黑150g、Genapol X080为100g、柠檬酸200g、碳酸氢钠200g、糊精 50g、硬脂酸镁20g、无水硫酸钠 补足1000g。
制备方法同实施例1。
对比例2:
水分散片剂配方为:丙草胺原药150g、吡嘧磺隆原药20g、五氟磺草胺原药10g、拉开粉BX为20g、丁二酸二异辛酯磺酸钠15g、白炭黑150g、NSAE-10为100g、柠檬酸200g、碳酸氢钠200g、糊精 50g、硬脂酸镁20g、无水硫酸钠 补足1000g。
制备方法同实施例1。
对比例3
水分散片剂配方为:丙草胺原药150g、吡嘧磺隆原药20g、五氟磺草胺原药10g、Geropon T/36为20g、十二烷基硫酸钠7.5g、脂肪醇硫酸钠7.5g、白炭黑150g、Genapol X080为50g、十二烷基苯磺酸钙50g、柠檬酸200g、碳酸氢钠200g、糊精 50g、硬脂酸镁20g、无水硫酸钠 补足1000g。
制备方法同实施例1。
测定本发明实施例1-3制备的制剂与对比例1-3制剂的悬浮率和崩解时间。
其中,悬浮率的测定方法如上所述。
崩解时间的测定方法为:将制备的水分散片剂投入装有水的水槽中,从片剂接触水面开始计时,直到药剂完全分散时结束计时。
结果如下表所示。
表3 崩解时间、悬浮率测定结果
上述结果显示,本发明实施例1-3所制备的水分散片剂在崩解时间、悬浮率等方面优于对比例1-3。其中,实施例1的崩解时间最短,悬浮率最大,是最优选的配方。
四、田间试验
试验作物:水稻田,品种为哈粳稻2号;
试验田中的主要杂草种类为:稗草(Echinochloa crusgalli(L.)Beauv.),雨久花(Monochoria korsakowii Regel et Maack),异型莎草(Cyperus difformis L.);
供试药剂:实施例1-3药剂;
对照药剂:对比例1-3药剂;
施药方法及用量:5月22日插秧,5月28日施药,一次施药,撒施,施药量如下表所示。
小区安排和重复:小区面积为25 m2, 四次重复。各小区随机排列。
调查方法:处理后15天调查株数防效。每小区随机定3点,每点0.25m2。药效计算方法为:
试验结果如下。
表4田间药效试验结果
上述结果显示,本发明实施例1-3的防效优于对比例1-3。其中,实施例1的防效最优。
最后应说明的是:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。
Claims (10)
1.一种含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂,其特征在于,所述水分散片剂由如下组分及其重量百分含量组成:
丙草胺原药 15%
吡嘧磺隆原药 2%
五氟磺草胺原药1%
聚羧酸钠盐分散剂2.0%
硫酸盐类润湿剂1.5%
白炭黑15%
腰果酚聚氧乙烯醚乳化剂10%
柠檬酸20%
碳酸氢钠20%
粘结剂 5%
润滑剂2%
载体补足100%
其中,
所述聚羧酸钠盐分散剂为Geropon T/36;所述硫酸盐类润湿剂为Geropon L-WET/P;所述腰果酚聚氧乙烯醚乳化剂为NSAE-10。
2.根据权利要求1所述的水分散片剂,其特征在于,所述粘结剂选自淀粉、糊精、羧甲基纤维素、羧乙基纤维素、明胶、阿拉伯胶、黄原胶中的一种或多种。
3.根据权利要求2所述的水分散片剂,其特征在于,所述粘结剂为糊精。
4.根据权利要求1所述的水分散片剂,其特征在于,所述润滑剂选自滑石粉或硬脂酸镁。
5.根据权利要求4所述的水分散片剂,其特征在于,所述润滑剂为硬脂酸镁。
6.根据权利要求1所述的水分散片剂,其特征在于,所述载体选自无水硫酸钠、尿素、高岭土中的一种或多种。
7.根据权利要求6所述的水分散片剂,其特征在于,所述载体为无水硫酸钠。
8.权利要求1所述的含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂的制备方法,其特征在于,包含如下步骤:
将丙草胺原药与腰果酚聚氧乙烯醚乳化剂混合均匀,然后加入吸附剂白炭黑进行吸附;然后,向其中加入吡嘧磺隆原药、五氟磺草胺原药、聚羧酸钠盐分散剂、硫酸盐类润湿剂、载体,混合均匀并气流粉碎;然后,依次加入柠檬酸、润滑剂、碳酸氢钠混合均匀,加入粘结剂造粒、筛分、压片、干燥,即得。
9.权利要求1所述的含有丙草胺、吡嘧磺隆与五氟磺草胺的水分散片剂用于防除水稻田杂草的用途。
10.根据权利要求9所述的用途,其特征在于,所述杂草为稗草、雨久花、异型莎草。
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