CN109303046A - 一种可分散油悬浮助剂及其制备方法 - Google Patents
一种可分散油悬浮助剂及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003921 oil Substances 0.000 claims abstract description 18
- -1 succinic acid sorbitol ester Chemical class 0.000 claims abstract description 16
- 239000000375 suspending agent Substances 0.000 claims abstract description 15
- 239000003849 aromatic solvent Substances 0.000 claims abstract description 14
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920002367 Polyisobutene Polymers 0.000 claims abstract description 10
- OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical compound [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000004359 castor oil Substances 0.000 claims abstract description 10
- 235000019438 castor oil Nutrition 0.000 claims abstract description 10
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims abstract description 10
- 239000001384 succinic acid Substances 0.000 claims abstract description 10
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims abstract description 9
- 239000000600 sorbitol Substances 0.000 claims abstract description 9
- 239000000575 pesticide Substances 0.000 claims abstract description 7
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 5
- 235000019198 oils Nutrition 0.000 claims description 17
- 239000012752 auxiliary agent Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 10
- 230000032050 esterification Effects 0.000 claims description 9
- 238000005886 esterification reaction Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 7
- 239000008158 vegetable oil Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 235000012424 soybean oil Nutrition 0.000 claims description 6
- 239000003549 soybean oil Substances 0.000 claims description 6
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
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- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 235000019482 Palm oil Nutrition 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
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- 239000002285 corn oil Substances 0.000 claims description 2
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- 235000009566 rice Nutrition 0.000 claims description 2
- AIMMVWOEOZMVMS-UHFFFAOYSA-N cyclopropanecarboxamide Chemical compound NC(=O)C1CC1 AIMMVWOEOZMVMS-UHFFFAOYSA-N 0.000 claims 1
- 150000002085 enols Chemical class 0.000 claims 1
- 235000013311 vegetables Nutrition 0.000 claims 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
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- RTCOGUMHFFWOJV-UHFFFAOYSA-N nicosulfuron Chemical compound COC1=CC(OC)=NC(NC(=O)NS(=O)(=O)C=2C(=CC=CN=2)C(=O)N(C)C)=N1 RTCOGUMHFFWOJV-UHFFFAOYSA-N 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
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- KPUREKXXPHOJQT-UHFFFAOYSA-N mesotrione Chemical compound [O-][N+](=O)C1=CC(S(=O)(=O)C)=CC=C1C(=O)C1C(=O)CCCC1=O KPUREKXXPHOJQT-UHFFFAOYSA-N 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
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- 241000400644 Echinochloa oryzicola Species 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002552 dosage form Substances 0.000 description 2
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- 244000025254 Cannabis sativa Species 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
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- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
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- 150000002576 ketones Chemical class 0.000 description 1
- 239000012053 oil suspension Substances 0.000 description 1
- 239000008194 pharmaceutical composition Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000009991 scouring Methods 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
- 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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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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
- 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
- A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
- A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
- A01N41/10—Sulfones; Sulfoxides
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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
- 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
- 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
- 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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Abstract
本发明公开了一种可分散油悬浮助剂及其制备方法，其特征在于：该可分散油悬浮助剂由十二烷基苯磺酸钙、蓖麻油聚氧乙烯醚、聚异丁烯丁二酸山梨醇酯、S‑150号芳烃溶剂油组成，本发明可以有效解决农药可分散油悬剂常见的长时间存放后样品分层、变稠甚至结块的问题。
Description
技术领域
本发明属于农业技术领域，具体涉及一种可分散油悬浮助剂及其制备方法。
背景技术
2015年初，可分散油悬浮剂英文名称为Oil-basedsuspensionconcentrate,剂型英文缩写为OD。定义是：以油为介质的高分散性、稳定的悬浮体系，是一类用经过试验以不污染作物的油类作为载体的一种剂型，油类包括植物油或矿物油。同时要求油类本身具有良好的粘着性和展着性，容易粘附于蜡质或光滑的叶面，对于一些除草类农药，油悬浮剂具有粘着性和展着性好、抗雨冲刷能力强等优点。在用药时入水分散优，呈云雾状分散，而且性质稳定，贮存过程中不会出现分层及沉淀问题，热贮分解率低，成本低。特别是药液容易渗透到靶标，药效高，无不良气味。其环保特性也值得提倡，以植物油代替乳油中的芳烃溶剂，环保，贮运安全。一般来说在生产的过程中适用以水为介质的水悬浮剂的准则也适用以油为介质的油悬浮剂，然而由于还要使油基乳化，油悬浮剂对助剂的要求更高，同时也需要更多更科学配伍的表面活性剂。
发明内容
本发明的目的就是要提供一种可分散油悬浮助剂及其制备方法，它能有效解决农药可分散油悬剂常见的长时间存放后样品分层、变稠甚至结块的问题。本发明的目的是这样实现的，一种油悬浮助剂的制备方法，其特征在于：按组份由十二烷基苯磺酸钙，蓖麻油聚氧乙烯醚，聚异丁烯丁二酸山梨醇酯，S-150号芳烃溶剂油复配而成；四种组分按重量百分比为十二烷基苯磺酸钙1％～30％，蓖麻油聚氧乙烯醚5％～65％，聚异丁烯丁二酸山梨醇酯2％～40％，S-150号芳烃溶剂油1％～50％。
本发明优点：
1、根据油悬浮制剂的特点进行设计，经过科学复配及制备而成，能够适用于多数农药品种制作可油悬浮制剂。
2、入水乳化分散好，性质稳定，有效成分热贮分解率低。
3、以植物油或矿物油代替乳油中的芳烃溶剂，环保且贮运安全。
4、解决了油悬浮助剂常见的长时间存放后变稠甚至结块等问题，提高制剂入水的乳化分散能力，能够显著提高药效。
为达到上述目的，本发明的技术方案为：
一种可分散油悬浮助剂及其制备方法，按照重量百分比，将十二烷基苯磺酸钙1％～30％，蓖麻油聚氧乙烯醚5％～65％，聚异丁烯丁二酸山梨醇酯2％～40％，S-150号芳烃溶剂油1％～50％。四种组分加入到反应釜中，混合搅拌均匀至淡黄色均相液体，即得到本发明组合物。
上述可分散油悬浮助剂，可以用于生产多种有效成分的可分散油悬浮剂产品，其具体方法为，加入0.1％～50％农药有效成分，1％～30％本发明助剂，0.1％～5％的增粘剂，0％～30％溶剂，30％～98.8％植物油，将上述各组分加入到混配釜，搅拌均匀，用高剪切机剪切30分钟到60分钟，再将物料通过砂磨机研磨，至物料粒径D50小于2微米，即得到可以适合使用的农药可分散油悬浮剂。
上述可分散油悬浮助剂，所述增粘剂可以是白炭黑，膨润土，聚乙烯醇等一种或几种。
上述可分散油悬浮助剂，所述溶剂可以是二甲苯、S-150号芳烃溶剂油等芳烃类溶剂或甲醇、乙醇等醇类或其混合物。
上述可分散油悬浮助剂，所述植物油可以是大豆油、玉米油、菜籽油、甲酯化大豆油、甲酯化棕榈油、甲酯化菜籽油、稻米油中的一种或几种。
具体实施方式
为验证本发明可分散油悬浮助剂的使用方法，申请人通过具体实例用以进一步详细说明本发明，但本发明绝非仅仅限于以下这些实施例。配方中百分比均为重量百分比，具体实施例如下：
配方一：
以质量百分数计，在30℃磁力搅拌下，加入十二烷基苯磺酸钙5％，蓖麻油聚氧乙烯醚15％，聚异丁烯丁二酸山梨醇酯30％，S-150号芳烃溶剂油50％，混合搅拌均匀至淡黄色均相液体。
配方二：
以质量百分数计，在30℃磁力搅拌下，加入十二烷基苯磺酸钙15％，蓖麻油聚氧乙烯醚15％，聚异丁烯丁二酸山梨醇酯30％，S-150号芳烃溶剂油40％，混合搅拌均匀至淡黄色均相液体。
配方三：
以质量百分数计，在30℃磁力搅拌下，加入十二烷基苯磺酸钙15％，蓖麻油聚氧乙烯醚30％，聚异丁烯丁二酸山梨醇酯30％，S-150号芳烃溶剂油25％，混合搅拌均匀至淡黄色均相液体。
配方四：
以质量百分数计，在30℃磁力搅拌下，加入十二烷基苯磺酸钙30％，蓖麻油聚氧乙烯醚25％，聚异丁烯丁二酸山梨醇酯30％，S-150号芳烃溶剂油15％，混合搅拌均匀至淡黄色均相液体。
配方五：
以质量百分数计，在30℃磁力搅拌下，加入十二烷基苯磺酸钙20％，蓖麻油聚氧乙烯醚50％，聚异丁烯丁二酸山梨醇酯20％，S-150号芳烃溶剂油10％，混合搅拌均匀至淡黄色均相液体。
助剂应用的性能测试：采用以上配方的助剂，选用五氟磺草胺，烟嘧磺隆，硝磺草酮三种有效成分，配制成如下可分散油悬浮剂，测试制剂的性能及药效情况。
2.5％五氟磺草胺OD的配制：将2.5％五氟磺草胺原药(折百)，配方一助剂15％，膨润土2％，白炭黑1％，甲酯化大豆油补足至100％，S-150号芳烃溶剂油10％，加入到反应釜，搅拌均匀，高速剪切30分钟，将物料加入到砂磨机研磨，至物料粒径D50小于2微米时，得到该制剂产品。
4％烟嘧磺隆OD的配制：将4％烟嘧磺隆原药(折百)，配方二助剂15％，膨润土2％，白炭黑1％，甲酯化大豆油补足至100％，S-150号芳烃溶剂油10％，加入到反应釜，搅拌均匀，高速剪切30分钟，将物料加入到砂磨机研磨，至物料粒径D50小于2微米时，得到该制剂产品。
10％硝磺草酮OD的配制:将10％硝磺草酮原药(折百)，配方二助剂15％，膨润土2％，白炭黑1％，甲酯化大豆油补足至100％，S-150号芳烃溶剂油10％，加入到反应釜，搅拌均匀，高速剪切30分钟，将物料加入到砂磨机研磨，至物料粒径D50小于2微米时，得到该制剂产品。
按照可分散油悬浮剂的质量指标，三种可分散油悬浮剂性能测试如下表：
由上表可以看出，采用本发明助剂，配制不同成分的可分散油悬浮剂，其制剂各项性能指标都很好，悬浮率显著高于标准值，入水自发分散性能良好，产品经过冷贮试验，流动性能良好，热贮试验，产品析油量也小于5％，一般可分散油悬浮剂经过热贮后析油量多大于10％，说明此制剂各项指标均比较稳定。
为了验证以上三个制剂配方使用的药效情况，我们进行了三个制剂与市售同类制剂的药效对比试验，具体情况见下表。
| 制剂 | 试验作物 | 防治对象 | 亩用制剂量mL | 7天防效，％ | 14天防效，％ |
| 2.5％五氟磺草胺OD | 水稻 | 稗草 | 100 | 87.3 | 98.7 |
| 市售2.5％五氟磺草胺OD | 水稻 | 稗草 | 100 | 83.2 | 95.7 |
| 4％烟嘧磺隆OD | 玉米 | 一年生杂草 | 100 | 82.1 | 93.7 |
| 市售4％烟嘧磺隆OD | 玉米 | 一年生杂草 | 100 | 78.6 | 88.7 |
| 10％硝磺草酮OD | 玉米 | 一年生杂草 | 100 | 83.4 | 92.1 |
| 市售10％硝磺草酮OD | 玉米 | 一年生杂草 | 100 | 81.6 | 90.8 |
田间药效试验表明，采用本发明助剂配制的三种有效成分的制剂，与市售同类制剂对比，其药效略优于对照药剂。
综上所述，采用本发明可分散油悬浮剂助剂，配制成多种有效成分的可分散油悬浮剂制剂，各项性能指标合格，田间药效表现良好，具有很好的应用前景。
Claims (5)
1.一种可分散油悬浮助剂及其制备方法，其特征在于：所述可分散油悬浮助剂以质量百分数计，包括：十二烷基苯磺酸钙1%～30%，蓖麻油聚氧乙烯醚5%～65%，聚异丁烯丁二酸山梨醇酯2%～40%，S-150号芳烃溶剂油1%～50%。
2.根据权利要求1所述的可分散油悬浮助剂，其使用方法为，加入0.1%-50%农药有效成分，1%～30%本发明助剂，0.1%～5%的增粘剂，0%～30%溶剂，30%～98.8%植物油，将上述各组分加入到混配釜，搅拌均匀，用高剪切机剪切30分钟到60分钟，再将物料通过砂磨机研磨，至物料粒径D50小于2微米，即得到可以适合使用的农药可分散油悬浮剂。
3.根据权利要求1所述的可分散油悬浮助剂，所述增粘剂可以是白炭黑，膨润土，聚乙烯醇等一种或几种。
4.根据权利要求1所述的可分散油悬浮助剂，所述溶剂可以是二甲苯、S-150号芳烃溶剂油等芳烃类溶剂或甲醇、乙醇等醇类或其混合物。
5.根据权利要求1所述的可分散油悬浮助剂，所述植物油可以是大豆油、玉米油、菜籽油、甲酯化大豆油、甲酯化棕榈油、甲酯化菜籽油、稻米油中的一种或几种。
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