CN113749089A - 一种具有改善的稳定性的油分散组合物 - Google Patents
一种具有改善的稳定性的油分散组合物 Download PDFInfo
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- CN113749089A CN113749089A CN202010490091.7A CN202010490091A CN113749089A CN 113749089 A CN113749089 A CN 113749089A CN 202010490091 A CN202010490091 A CN 202010490091A CN 113749089 A CN113749089 A CN 113749089A
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- Prior art keywords
- fatty alcohol
- oil dispersion
- dispersion composition
- oil
- alcohol ethoxylated
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- 150000002191 fatty alcohols Chemical class 0.000 claims abstract description 63
- 230000002776 aggregation Effects 0.000 claims abstract description 29
- 239000003905 agrochemical Substances 0.000 claims abstract description 27
- 239000003495 polar organic solvent Substances 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- 238000004220 aggregation Methods 0.000 claims description 25
- 230000002363 herbicidal effect Effects 0.000 claims description 25
- YROXIXLRRCOBKF-UHFFFAOYSA-N sulfonylurea Chemical compound OC(=N)N=S(=O)=O YROXIXLRRCOBKF-UHFFFAOYSA-N 0.000 claims description 23
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
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- AIMMSOZBPYFASU-UHFFFAOYSA-N n-(4,6-dimethoxypyrimidin-2-yl)-n'-[3-(2,2,2-trifluoroethoxy)pyridin-1-ium-2-yl]sulfonylcarbamimidate Chemical compound COC1=CC(OC)=NC(NC(=O)NS(=O)(=O)C=2C(=CC=CN=2)OCC(F)(F)F)=N1 AIMMSOZBPYFASU-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 3
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- PFJJMJDEVDLPNE-UHFFFAOYSA-N Benoxacor Chemical compound C1=CC=C2N(C(=O)C(Cl)Cl)C(C)COC2=C1 PFJJMJDEVDLPNE-UHFFFAOYSA-N 0.000 claims description 2
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- TYIYMOAHACZAMQ-CQSZACIVSA-N Cyhalofop-butyl Chemical group C1=CC(O[C@H](C)C(=O)OCCCC)=CC=C1OC1=CC=C(C#N)C=C1F TYIYMOAHACZAMQ-CQSZACIVSA-N 0.000 claims description 2
- PQKBPHSEKWERTG-UHFFFAOYSA-N Fenoxaprop ethyl Chemical group C1=CC(OC(C)C(=O)OCC)=CC=C1OC1=NC2=CC=C(Cl)C=C2O1 PQKBPHSEKWERTG-UHFFFAOYSA-N 0.000 claims description 2
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- JBDHZKLJNAIJNC-LLVKDONJSA-N clodinafop-propargyl Chemical group C1=CC(O[C@H](C)C(=O)OCC#C)=CC=C1OC1=NC=C(Cl)C=C1F JBDHZKLJNAIJNC-LLVKDONJSA-N 0.000 claims description 2
- OPGCOAPTHCZZIW-UHFFFAOYSA-N diethyl 1-(2,4-dichlorophenyl)-5-methyl-4h-pyrazole-3,5-dicarboxylate Chemical group CCOC(=O)C1(C)CC(C(=O)OCC)=NN1C1=CC=C(Cl)C=C1Cl OPGCOAPTHCZZIW-UHFFFAOYSA-N 0.000 claims description 2
- COYBRKAVBMYYSF-UHFFFAOYSA-N heptan-2-yl [(5-chloroquinolin-8-yl)oxy]acetate Chemical group C1=CN=C2C(OCC(=O)OC(C)CCCCC)=CC=C(Cl)C2=C1 COYBRKAVBMYYSF-UHFFFAOYSA-N 0.000 claims description 2
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- 238000004519 manufacturing process Methods 0.000 claims description 2
- 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 claims description 2
- FOXFZRUHNHCZPX-UHFFFAOYSA-N metribuzin Chemical compound CSC1=NN=C(C(C)(C)C)C(=O)N1N FOXFZRUHNHCZPX-UHFFFAOYSA-N 0.000 claims description 2
- CHIFOSRWCNZCFN-UHFFFAOYSA-N pendimethalin Chemical compound CCC(CC)NC1=C([N+]([O-])=O)C=C(C)C(C)=C1[N+]([O-])=O CHIFOSRWCNZCFN-UHFFFAOYSA-N 0.000 claims description 2
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- NIFKBBMCXCMCAO-UHFFFAOYSA-N methyl 2-[(4,6-dimethoxypyrimidin-2-yl)carbamoylsulfamoyl]-4-(methanesulfonamidomethyl)benzoate Chemical group COC(=O)C1=CC=C(CNS(C)(=O)=O)C=C1S(=O)(=O)NC(=O)NC1=NC(OC)=CC(OC)=N1 NIFKBBMCXCMCAO-UHFFFAOYSA-N 0.000 claims 1
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Images
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
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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
- A01N25/22—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 ingredients stabilising the active ingredients
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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Abstract
本发明提供一种具有改善的稳定性的油分散组合物,其含有非极性有机溶剂、脂肪醇乙氧基化丙氧基化物、分散的农业化学活性物以及至少一种表面活性剂。本发明通过在油分散组合物中添加脂肪醇乙氧基化丙氧基化物,其能够使得农业化学活性物在非极性有机溶剂中稳定以防止发生颗粒聚集从而导致发生沉降的现象。
Description
技术领域
本发明属于农业化学技术领域,具体涉及一种具有改善的稳定性的油分散组合物,以及脂肪醇乙氧基化丙氧基化物在控制农业油分散制剂组合物悬浮颗粒聚集中的用途,尤其涉及通过使用C2-C20脂肪醇乙氧基化丙氧基化物抑制或防止酰胺或磺酰脲类除草剂在油分散组合物中颗粒相互聚集而形成的稳定农业化学油分散体。
背景技术
农业制剂产品必须在特定的时间内为物理和化学稳定的,从而具有商业实用性。然而其存在多种不稳定因素,例如活性物不稳定、相分离和环境因素。在现今的农业化学市场中,日益常见的是开发含有多种活性物和它们需要的溶剂、安全剂和/或助剂等的新制剂,以实现最佳谱系、效力和递送效率,而这使制剂稳定性面临越来越多的挑战。因此,能够有效地隔离、干扰或消除不相容成分之间的不利反应或不利相互作用的技术对于成功的产品而言经常是非常重要的。
农业化学组合物如除草剂、杀虫剂或杀菌剂或除草安全剂很少能按它的最初制造形成使用。农业化学物一般由两部分组成,即在制剂中组合在一起的活性物和助剂组分或惰性成分。将这两部分组合至最终产品中时会考虑到两个主要目标:①在贮存过程中维持产品的稳定性,和②为在将产品在载体如水或油中稀释后喷雾施用至待处理的区域提供容易且有效的方式。
农业化学制剂一般是基于客户的需要和活性物的物理化学性质(例如,活性成分在水或其它非水溶剂中的溶解度)而设计的。主要存在两个主要制剂种类,即固体制剂和液体制剂。液体制剂通常由于在测量、泵送、稀释和喷雾操作中容易处理而为客户所优选。
油分散体(OD)是一种液体制剂类型并定义为活性物在水不混溶溶剂中的稳定悬浮液,其可含有其它溶解的活性物并意图在使用之前用水稀释。近来,油分散体制剂在目前的制剂研究中变得更加重要。因为油分散体制剂非常适合用于以下情况:(1)水敏感的活性物,例如磺酰脲类除草剂,其极易水解降解,(2)与活性物混合物的相容问题,和(3)分子内佐剂(build-in adjuvant)的需要。
现已知道农业油分散制剂属于热力学不稳定体系,或多或少都会发生沉降现象。沉降的快慢符合斯托克斯沉速理论w=【2g(ρs-ρ)gr2】/9μ,式中:ρs为颗粒密度;ρ为水的密度;μ为流体黏度;r为颗粒半径;g为重力加速度。通常农业油分散制剂中添加流体学改性剂就是为了调节油分散流体黏度以提供制剂物理稳定性。现已有多种物质被用作流体学改性剂以使油分散制剂稳定以防止沉降,例如黏土、有机粘土、亲水性硅土和疏水性硅土、黄原胶、聚酰胺、聚乙烯吡咯烷酮、聚丙烯酸酯等。从理论公式可知油分散体中悬浮颗粒的大小也是影响沉降速率的重要因数,悬浮颗粒在贮存过程粒径的增长是加速沉降影响制剂物理稳定性的另一原因。悬浮颗粒粒径的增长一般有两种情况,一是极性溶剂对活性物或多或少的溶解作用而发生奥斯特瓦尔德熟化,二是活性物与助剂、溶剂、表面活性剂、助配方组分之间的不兼容性而发生的颗粒之间的相互聚集。
目前关于控制油分散体发生沉降分层和颗粒增长的专利也有报道,CN103118536A中主要保护的是使用粘土或硅土型流变改性剂和能够形成氢键的聚合物或低聚物的组合物,优选粘土或硅土型流变改性剂和聚乙二醇或聚丙二醇的组合物,以稳定油分散体防止发生颗粒沉降分层。CN107484767A中主要保护的是选用脂肪酸酯类溶剂作为螺虫乙酯颗粒的分散相,减少或抑制悬浮颗粒发生奥斯特瓦尔德熟化,以达到控制粒径增长稳定油分散体。然而,截止目前为止,还没有相关技术披露如何来避免油分散体中颗粒相互聚集的现象。
发明内容
为解决上述技术问题,本发明提供了具有改善的稳定性的油分散组合物,其中油分散体的悬浮颗粒在较长的贮存过程中保存相对稳定,颗粒之间不相互聚集和不相互结合,油分散体组合物的物理稳定性显著提高。这种改进是通过添加一种特定的脂肪醇乙氧基化丙氧基化物达到的。本发明意外地发现具有脂肪醇乙氧基化丙氧基化物这些化合物能显著地控制油分散体中悬浮颗粒相互聚集的现象。
为达此目的,本发明采用以下技术方案:
第一方面,本发明提供了一种具有改善的稳定性的油分散组合物,其含有以下组分:
(a)非极性有机溶剂,其相对于所述油分散组合物重量为200g/L-800g/L;
(b)脂肪醇乙氧基化丙氧基化物,其相对于所述油分散组合物重量为5g/L-150g/L;
(c)分散的农业化学活性物,其相对于所述油分散组合物重量为1g/L-300g/L;
(d)至少一种表面活性剂,其相对于所述油分散组合物重量为1g/L-300g/L。
本发明中,所述脂肪醇乙氧基化丙氧基化物与农业化学活性物的重量比为150:1到1:60,例如150:1、120:1、100:1、80:1、65:1、50:1、45:1、30:1、20:1、10:1、5:1、2:1、1:1、1:2、1:5、1:10、1:20、1:30、1:40、1:50、1:55、1:60,优选50:1到1:10,更优选10:1到1:5。
本发明使用的非极性有机溶剂优选一种或多种与水不混溶的非极性溶剂,一般在水中溶解度小于0.5重量%,包括一种或多种石油馏出物如衍生自苯的芳族烃,例如甲苯、二甲苯、混三甲苯等,脂肪族烃如己烷、辛烷、环己烷等,植物油、种子油或动物油如大豆油、菜籽油、橄榄油、蓖麻油、葵花籽油、椰子油、玉米油、棉籽油、亚麻籽油、棕榈油、花生油、红花油、芝麻油等,以及植物油或动物油的C1-C6的酯如油酸甲酯、环氧大豆油、棕榈酸甲酯、蓖麻油乙酯、C6-C20饱和和不饱和脂肪族羧酸的C1-C6烷基酯。
在本发明中强极性有机溶剂不被优先考虑,例如醚类如四氢呋喃等、亚烷基二醇二烷基醚如乙二醇二乙醚等,酰胺如二甲基乙酰胺或N-甲基吡咯烷酮等,酮如甲基乙基酮等,腈如丁腈等,亚砜或砜如二甲亚砜或环丁砜等,和亚烃基碳酸酯如碳酸丙基酯或碳酸丁基酯等。这些强极性有机溶剂有很好的溶解性能,对大多数农业活性物,例如磺胺、磺酰脲类除草剂有一定的溶解能力。在这类强极性有机溶剂中分散的活性物颗粒很容易出现奥斯特瓦尔德熟化现象。质子性溶剂,例如水、醇、聚多元醇有时可与一些存在于油分散体制剂中的活性成分或者除草安全剂不相容。具体地,在水的存在下,一些磺酰脲除草剂具有经在磺酰脲桥处断裂而水解的降解现象。上述类别的有机溶剂都不是被本发明所选用的。
本发明中非极性有机溶剂相对于所述油分散组合物重量为200g/L-800g/L,例如200g/L、250g/L、300g/L、350g/L、400g/L、450g/L、500g/L、550g/L、600g/L、650g/L、700g/L、750g/L或800g/L,优选300g/L-750g/L。
本发明所述的脂肪醇乙氧基化丙氧基化物是由饱和和/或不饱和的直链和/或支链的一元醇与乙二醇和丙二醇按一定摩尔比共聚而生的醚,其中所述的脂肪醇选自C2-C20的醇,例如C2、C6、C8、C9、C11、C14、C16或C20,优选C4-C16的饱和一元醇;所述的脂肪醇乙氧基化丙氧基化物的数均分子量范围在100-1,000,000,例如数均分子量为100、200、1000、2200、2500、3000、4500、5200、6300、7000、8600、9500、10,000、30,000、50,000、100,000、500,000或1,000,000,优选200-100,000。
本发明中所述的脂肪醇乙氧基化丙氧基化物,具体可以选自商品名为TOXIMUL8320(C4)、EMULSOGEN MTP 070(C16-18)、EMULSOGEN 3510(C4)、ATLAS G-5000(C4)或Atplus 245(C9-C11)等。
本发明的脂肪醇乙氧基化丙氧基化物相对于所述油分散组合物重量为5g/L-150g/L,例如5g/L、10g/L、20g/L、30g/L、40g/L、50g/L、60g/L、80g/L、90g/L、100g/L、120g/L或150g/L,优选10g/L-120g/L。
发明人出乎意料的发现,脂肪醇乙氧基化丙氧基化物这类化合物在油分散体中能很好地阻止农业化学活性物,尤其是除草活性物,特别是除草的磺胺、磺酰脲类活性物,悬浮颗粒之间相互作用而发生聚集的现象,以起到稳定油分散体中悬浮颗粒的用途。
本发明适合的分散的农业化学活性成分可包括来自以下种类的一种或多种除草剂,尤其是磺胺类、磺酰脲类除草剂。
可适于分散在本发明非极性有机溶剂中的除草剂包括但不限于醚苯磺隆(triasulfuron)、苯磺隆(tribenuron)、甲磺隆(metasulfuron)、噻吩磺隆(thifensulfuron)、氟啶磺隆(flupyrsulfuron)、碘磺隆(iodosulfuron)、玉嘧磺隆(rimsulfuron)、烟嘧磺隆(nicosulfuron)、醚磺隆(cinosulfuron)、苄嘧磺隆(bensulfuron)、三氟啶磺隆(trifloxysulfuron)、甲酰胺磺隆(foramsulphuron)、甲基二磺隆(mesosulphuron)、磺酰磺隆(sulphosulphuron)、氟唑磺隆(flucarbazone-sodium)三氟甲磺隆(tritosulphuron)和衍生物,以及氟唑啶草(flumetsulam)、唑草磺胺(metosulam)、氯酯磺草胺(chloransulam)、双氟磺草胺(florasulam)、唑嘧磺胺(diclosulam)、五氟磺草胺(penoxsulam)、甲氧磺草胺(pyroxsulam)、吡氟酰草胺(diflufenican)、氟吡菌酰胺(thifluzamide)和衍生物等。
对于本发明的油分散组合物,可分散的农业化学活性物相对于所述油分散组合物重量为1g/L-300g/L,例如1g/L、10g/L、30g/L、40g/L、50g/L、60g/L、70g/L、80g/L、100g/L、150g/L、180g/L、220g/L、250g/L或300g/L,优选10g/L-250g/L。公知的是,可根据各除草剂的亩使用量将这种油分散体制剂在使用时稀释1-2000倍。
本发明中,所述农业化学活性物在所述非极性有机溶剂中的溶解度小于10g/L,例如0.1g/L、0.3g/L、0.5g/L、1g/L、2g/L、3g/L、4g/L、5g/L、6g/L、7g/L、8g/L或9g/L,优选小于5g/L,更优选小于1g/L。
本发明的油分散组合物还可以存在可溶于或分散油相的合适的第二活性成分,包括一种或多种非磺胺或磺酰脲类除草剂,例如炔草酯(clodinafop-propargyl)、氰氟草酯(cyhalofop-butyl)、噁唑禾草灵(fenoxaprop-ethyl)、乙草胺(acetochlor)、丙草胺(pretilachlor)、精异丙甲草胺(S-metolachlor)、氯氟吡氧乙酸异辛酯(fluroxypyr)、精喹禾灵(quizalofop-P)、氨氯吡啶酸(picloram)、二氯喹啉酸(quinclorac)、二甲戊灵(pendimethalin)、2,4-D、硝磺草酮(mesotrione)、丙草胺(pretilachlor)、精喹禾灵(quizalofop-P)、丁草胺(butachlor)、莠去津(atrazine)、嗪草酮(metribuzin)、唑啉草酯(pinoxaden)、苯唑草酮(topramezone)等。
本发明的油分散组合物还可以存在溶解或分散的除草安全剂。合适的除草剂安全剂可包括解草酯(cloquintocet-mexyl)、解草嗪(benoxacor)、解草胺腈(cyometrinil)、双苯噁唑酸乙酯(isoxadifen ethyl)、吡唑解草酯(mefenpyrdiethyl)、解草腈(oxabetrinil)及它们的衍生物和类似物。
本发明所述的至少一种表面活性剂是合适的功能性表面活性剂在油分散体配制剂中常用于该目的的表面活性剂,例如乳化剂、分散剂、润湿剂、消泡剂、pH调节剂、增稠剂、防腐剂等。
合适的乳化剂为在农业化学配制剂中用于该目的的任何物质,优选烷基酚与环氧乙烷和/或环氧丙烷的反应物、乙氧基化的壬基酚、蓖麻油乙氧基化物、多烷氧基化的醇的混合物(Atlox 4894)、烷基钙盐、烷基苯磺酸钙盐、脱水山梨醇衍生物或聚环氧乙烷-脱水山梨醇脂肪酸酯中任意一种或至少两种的组合,其中典型但非限制性的组合为:乙氧基化的壬基酚和蓖麻油乙氧基化物的组合,乙氧基化的壬基酚和烷基钙盐的组合,乙氧基化的壬基酚和烷基苯磺酸钙盐的组合,蓖麻油乙氧基化物和烷基钙盐的组合,烷基苯磺酸钙盐和脱水山梨醇衍生物的组合,烷基钙盐和脱水山梨醇衍生物的一种或多种。
合适的分散剂为在农业化学配制剂中用于该目的的任何物质,例如非离子型、两性型、阳离子型和阴离子型(聚合物)表面活性剂。优选如萘磺酸盐、萘磺酸盐-甲醛缩聚物、烷基磺酸盐、木质素磺酸盐、聚羧酸盐、脂肪醇乙氧基化物、脂肪醇乙氧基化物、脂肪醇烷氧基化物、EO/PO嵌段共聚物、乙氧基化醇的磺酸,磺基琥珀酸盐,脂肪酸甲基牛磺酸盐,三苯乙烯基苯酚乙氧基化物和烷氧基化物,三仲丁基苯酚乙氧基化物,硫酸化甲酚-甲醛缩合物、萘和烷基萘的硫酸化缩合物,乙氧基化脂肪醇、三苯乙烯基苯酚和三仲丁基苯酚的磷酸酯,以及乙氧基化脂肪醇、聚丙烯酸、聚甲基丙烯酸和丙烯酸酯共聚物、三苯乙烯基苯酚和三仲丁基苯酚的醚硫酸盐和聚合物分散剂中的一种或多种。
合适的润湿剂为在农业化学配制剂中用于该目的的任何物质,优选阴离子润湿剂,例如阴离子润湿剂的碱金属、碱土金属或铵盐。合适的润湿剂为萘磺酸盐(例如亚甲基二萘磺酸二钠盐,萘磺酸钠-甲醛缩合物,萘磺酸铵-甲醛缩合物),烷基萘磺酸盐(例如烷基萘磺酸钠),苯磺酸盐,烷基苯磺酸盐(例如枯烯磺酸钠、枯烯磺酸钾、二甲苯磺酸钠、甲苯磺酸钠),烷烃磺酸盐(例如十四碳烯磺酸钠),α-烯烃磺酸盐(例如α-烯烃磺酸钠),磺基琥珀酸盐(例如二辛基磺基琥珀酸钠),烷基磷酸盐(例如月桂基肉豆蔻基磷酸盐),烷基硫酸盐(例如月桂基硫酸钠、鲸蜡基硬脂基硫酸钠、鲸蜡基硫酸钠、肉豆蔻基硫酸钠、鲸蜡基硬脂基硫酸钠)。
合适的消泡剂为在农业化学配制剂中用于该目的的任何物质,例如硅酮、长链醇和脂肪酸的盐。
合适的pH调节剂为在农业化学配制剂中用于该目的的任何物质,例如磷酸、醋酸、柠檬酸、碳酸钠、碳酸氢钠、磷酸钾、磷酸一氢钾、磷酸二氢钾等能提供质子酸或质子碱的物质。
合适的增稠剂为在农业化学配制剂中用于该目的的任何物质,例如硅酸镁铝、白炭黑、硅藻土、聚乙烯醇、聚乙烯吡咯烷酮。
合适的防腐剂为在农业化学配制剂中用于该目的的任何物质,例如烷基异噻唑啉酮类和苯并异噻唑啉酮类。
本发明的表面活性剂相对于所述油分散组合物重量为1g/L-300g/L,例如1g/L、10g/L、30g/L、40g/L、50g/L、60g/L、70g/L、80g/L、100g/L、150g/L、180g/L、220g/L、250g/L或300g/L,优选为10g/L-200g/L。
进一步优选地,本发明中所述的油分散组合物由以下组分组成:
(a)非极性有机溶剂,其相对所述油分散组合物重量为300g/L-750g/L;
(b)脂肪醇乙氧基化丙氧基化物,其相对所述油分散组合物重量为10g/L-120g/L;
(c)分散的农业化学活性物,其相对于所述油分散组合物重量为10g/L-250g/L;
(d)至少一种表面活性剂,其相对于所述油分散组合物重量为10g/L-200g/L。
根据本发明制备得到的农业油分散组合物,即使在高温或者寒冷条件下存放,仍可保存稳定,未发现任何颗粒相互聚集的现象,更未发现因为颗粒聚集而导致加速沉降的现象,通过显微镜观察未发现有聚集的现象,马尔文粒径仪测试也未发现粒径显著增长,制剂产品显示很好的物理稳定性,长期贮存后不会对使用产生质量问题。
本发明所述的“聚集”是指分散在油分散体中的颗粒之间相互吸引、靠拢、聚拢、堆积的现象,更有甚者颗粒与颗粒之间相互作用结合形成大颗粒,而不能轻易的被再次离散开来。本发明所述的粒径“增长”是指悬浮颗粒因为颗粒之间的聚集而形成大的颗粒,从程度而言,粒径增长是颗粒聚集在热力学上进一步的形态。所述的“沉降”是由于颗粒聚集使得颗粒粒径增大到一定程度而引起油分散体发生固液分离的现象。
本发明出人意料的发现添加脂肪醇乙氧基化丙氧基化物可解决农业油分散体组合物在贮存过程中的悬浮颗粒聚集的问题,同时也有效的避免了颗粒增长、沉降而引起制剂质量不稳定、不方便使用的问题。脂肪醇乙氧基化丙氧基化物对控制农业油分散组合物中颗粒聚集是不可预期的,有着出乎本技术领域技术人员意料之外控制效果。
第二方面,本发明还提供了制备前述油分散组合物的方法,其包括以下步骤:
步骤1:将农业化学活性物和表面活性剂加入到非极性有机溶剂中,搅拌使之均匀;
步骤2:将步骤1的混合物经充分研磨得到油基浓缩液;
步骤3:将脂肪醇乙氧基化物按比例加入到油基浓缩液中,搅拌直至混合均匀,即得本发明的油分散组合物。
优选地,步骤2所述的研磨在0-50℃的温度下进行,例如0℃、10℃、15℃、20℃、25℃、30℃、35℃、40℃、45℃或50℃,优选15-45℃。
优选地,步骤2所述研磨得到油基浓缩液中农业化学活性物的颗粒粒径D50≤5μm,例如0.4μm、0.8μm、1μm、2μm、3μm、4μm、4.5μm、4.8μm、5μm,优选D50≤3μm。
第三方面,本发明还提供了一种防止农业油分散制剂组合物中磺胺或磺酰脲类除草活性物的悬浮颗粒互相聚集的方法。
所述方法包括加入足够量的脂肪醇乙氧基化丙氧基化物来减少磺胺或磺酰脲类除草活性物的悬浮颗粒相互聚集;所述脂肪醇乙氧基化丙氧基化物选自数均分子量在100-1,000,000的C2-C20脂肪醇乙氧基化丙氧基化物,优选数均分子量在200-100,000的C4-C16脂肪醇乙氧基化丙氧基化物;
优选地,所述足够量的脂肪醇乙氧基化丙氧基化物和磺胺或磺酰脲类除草活性物的重量比为150:1到1:60,优选50:1到1:10,更优选10:1到1:5。
在防止农业油分散体组合物悬浮颗粒聚集的方法中,脂肪醇乙氧基化丙氧基化物加入到农业油分散体组合物中,其形成的农业油分散体组合物含有以下组分:
(I)非极性有机溶剂;
(II)脂肪醇乙氧基化丙氧基化物;
(III)分散的磺胺或磺酰脲类化学活性物;
(IV)至少一种表面活性剂。
在防止农业油分散体组合物的悬浮颗粒聚集时,所述脂肪醇乙氧基化丙氧基化物的选择以及各组分的选择和配比等均与前面第一方面中是一致的,在此不做赘述。
第四方面,本发明还提供了脂肪醇乙氧基化丙氧基化物在抑制或防止第一方面所述的油分散组合物中磺胺或磺酰脲类除草活性物的悬浮颗粒相互聚集中的用途。
所述脂肪醇乙氧基化丙氧基化物选自数均分子量在100-1,000,000的C2-C20脂肪醇乙氧基化丙氧基化物,优选数均分子量在200-100,000的C4-C16脂肪醇乙氧基化丙氧基化物;所述脂肪醇乙氧基化丙氧基化物和磺胺或磺酰脲类除草活性物的重量比为150:1到1:60,优选50:1到1:10,更优选10:1到1:5。
在抑制或防止所述油分散组合物悬浮颗粒聚集时,脂肪醇乙氧基化丙氧基化物加入到农业油分散体组合物中,其形成的农业油分散体组合物含有以下组分:
(I)非极性有机溶剂;
(II)脂肪醇乙氧基化丙氧基化物;
(III)分散的磺胺或磺酰脲类化学活性物;
(IV)至少一种表面活性剂。
在抑制或防止农业油分散体组合物的悬浮颗粒聚集时,所述脂肪醇乙氧基化丙氧基化物的选择以及各组分的选择和配比等均与前面第一方面中是一致的,在此不做赘述。
第五方面,本发明还提供了一种有害生物的防治方法,所述方法为使用如第一方面所述的油分散组合物于有害生物生长的场所。
所述油分散组合物应用时以水喷雾稀释液的形式使用。
所述油分散组合物包含磺胺或磺酰脲类除草活性物,以防治有害杂草的生长。
本发明提供了如第一方面所述油分散组合物的施用方法,具体地有效施用量经常取决于例如,植物类型、植物生长阶段、环境条件的恶劣程度、待防治的杂草、昆虫或真菌病原体和施用条件。通常,将需要进行保护以防杂草或昆虫,或需要防治或消除病害或病原体的植物与一定量的在载体如水中稀释的油分散体制剂接触,所述制剂将提供1-40,000ppm,优选10-20,000ppm量的活性成分。公知的是,可将这种浓缩制剂根据农业实践在使用时稀释1-2000倍。所述接触可为任何有效方式。例如,可用与适当量的稀释剂或载体如水混合的活性成分喷洒到植物的任何暴露部分,例如:叶或茎。
可将本发明的前述组合物施用至植物叶子或与植物相邻的土壤或区域。另外,可将本发明组合物与农业活性成分如除草剂、杀昆虫剂、杀菌剂、杀线虫剂、杀螨剂、杀生物剂、杀白蚁剂、杀啮齿动物剂、杀软体动物剂、杀节肢动物剂、肥料、生长调节剂和信息素的任何组合混合或与所述组合一起施用。
与现有技术相比,本发明至少具有以下有益效果:
本发明中通过添加脂肪醇乙氧基化丙氧基化物,可解决农业油分散体组合物在贮存过程中的悬浮颗粒聚集的问题,同时也有效的避免了颗粒增长、沉降而引起制剂质量不稳定、不方便使用的问题;通过将添加有脂肪醇乙氧基化丙氧基化物的油分散组合物置于54℃热贮14天后,其粒径增长率可控制在3.10-5.50%,颗粒间几乎不聚集。
附图说明
图1是常温3个月后实施例1样品在400倍显微镜下的观察结果;
图2是常温3个月后实施例4样品在400倍显微镜下的观察结果;
图3是常温3个月后对比实施例1样品在400倍显微镜下的观察结果;
图4是常温3个月后对比实施例4样品在400倍显微镜下的观察结果。
下面对本发明进一步详细说明。但下述的实例仅仅是本发明的简易例子,并不代表或限制本发明的权利保护范围,本发明的保护范围以权利要求书为准。
具体实施方式
下面结合附图并通过具体实施方式来进一步说明本发明的技术方案。
为便于理解本发明,本发明列举实施例如下。本领域技术人员应该明了,所述实施例仅仅是帮助理解本发明,不应视为对本发明的具体限制。
本发明中所用到的脂肪醇乙氧基化丙氧基化物,均可通过市场购买获得。以下各实施例中用到的脂肪醇乙氧基化丙氧基化物对应商品名如表1所示。
表1
脂肪醇乙氧基化丙氧基化物 | 商品名 | |
实施例1 | C4脂肪醇乙氧基化丙氧基化物 | TOXIMUL 8320 |
实施例2 | C4脂肪醇乙氧基化丙氧基化物 | EMULSOGEN 3510 |
实施例3 | C4脂肪醇乙氧基化丙氧基化物 | ATLAS G-5000 |
实施例4 | 混合C9-C11脂肪醇乙氧基化丙氧基化物 | Atplus 245 |
实施例5 | 混合C9-C11脂肪醇乙氧基化丙氧基化物 | Atplus 245 |
实施例6 | 混合C16-18脂肪醇乙氧基化丙氧基化物 | EMULSOGEN MTP 070 |
实施例1
实施例2
实施例3
实施例4
实施例5
实施例6
对比实施例1
对比实施例2
对比实施例3
对比实施例4
对比实施例5
对比实施例6
将上述实施例1-6和对比实施例1-6的样品进行加速贮存实验,将各样品装入量筒中放入54℃的烘箱热贮14天后进行样品外观显微镜观察和通过马尔文激光粒径仪测试粒径大小,并与热贮前样品进行对比,测试结果如下表2。
表2
注:根据显微镜肉眼观察结合粒径测试增长率大于10%和大于20%为界限判断聚集程度,其中“-”表示颗粒不聚集或不明显;“+”表示颗粒聚集;“++”表示颗粒严重聚集。
从表2所示结果可以看出,本发明的农业油分散组合物,热贮后的样品不聚集或不明显,粒径相对于对比实施例1-6增长较小。
本发明所述的粒径增长主要是因为颗粒聚集造成的。常温贮存3个月后将实施例1和实施例4样品在400倍显微镜下观察,如图1和图2所示,明显发现添加了本发明所述的脂肪醇乙氧基化丙氧基化物这类物质的油分散体具有较好的颗粒分散性,仍均匀地分布在油分散体中,而未添加本发明所述脂肪醇乙氧基化丙氧基化物这类物质的油分散体,将对比实施例1和对比实施例4样本在400倍显微镜下观察,如图3和图4所示,原分散的颗粒发生了相互聚集、团结,已不能均匀地分布在油分散体中。
综上所述,本发明中通过添加脂肪醇乙氧基化丙氧基化物,可解决农业油分散体组合物在贮存过程中的悬浮颗粒聚集的问题,同时也有效的避免了颗粒增长、沉降而引起制剂质量不稳定、不方便使用的问题。
Claims (19)
1.具有改善的稳定性的油分散组合物,其特征在于,含有以下组分:
(a)非极性有机溶剂,其相对于所述油分散组合物重量为200g/L-800g/L;
(b)脂肪醇乙氧基化丙氧基化物,其相对于所述油分散组合物重量为5g/L-150g/L;
(c)分散的农业化学活性物,其相对于所述油分散组合物重量为1g/L-300g/L;
(d)至少一种表面活性剂,其相对于所述油分散组合物重量为1g/L-300g/L。
2.根据权利要求1所述的油分散组合物,其特征在于,所述脂肪醇乙氧基化丙氧基化物与农业化学活性物的重量比为150:1到1:60,优选50:1到1:10,更优选10:1到1:5。
3.根据权利要求1所述的油分散组合物,其特征在于,所述非极性有机溶剂为芳烃、脂肪族烃、植物油或植物油酯化物中的任意一种或至少两种的混合物。
4.根据权利要求1所述的油分散组合物,其特征在于,所述脂肪醇乙氧基化丙氧基化物为数均分子量在100-1,000,000的C2-C20脂肪醇乙氧基化丙氧基化物,优选数均分子量在200-100,000的C4-C16脂肪醇乙氧基化丙氧基化物。
5.根据权利要求1所述的油分散组合物,其特征在于,所述农业化学活性物包含选自以下除草剂中的至少一种:磺胺、磺酰脲以及它们的衍生物。
6.根据权利要求5所述的油分散组合物,其特征在于,所述除草剂选自以下中的至少一种:苯磺隆、甲磺隆、噻吩磺隆、氟啶磺隆、碘磺隆、玉嘧磺隆、烟嘧磺隆、醚磺隆、苄嘧磺隆、三氟啶磺隆、甲酰胺磺隆、甲基二磺隆、氟唑磺隆、唑草磺胺、氯酯磺草胺、双氟磺草胺、唑嘧磺胺、五氟磺草胺、甲氧磺草胺或吡氟酰草胺。
7.根据权利要求1所述的油分散组合物,其特征在于,所述农业化学活性物在所述非极性有机溶剂中的溶解度小于10g/L,优选小于5g/L,更优选小于1g/L。
8.根据权利要求1所述的油分散组合物,其特征在于,所述油分散组合物还可以包含分散或溶解在所述非极性有机溶剂中的非磺胺或磺酰脲类除草剂或除草安全剂。
9.根据权利要求8所述的油分散组合物,其特征在于,所述非磺胺或磺酰脲类除草剂包括炔草酯、氰氟草酯、噁唑禾草灵、乙草胺、丙草胺、精异丙甲草胺、氯氟吡氧乙酸异辛酯、精喹禾灵、氨氯吡啶酸、二氯喹啉酸、二甲戊灵、2,4-D、硝磺草酮、丙草胺、精喹禾灵、丁草胺、莠去津、嗪草酮、唑啉草酯或苯唑草酮中的任意一种或至少两种的混合物。
10.根据权利要求8所述的油分散组合物,其特征在于,所述除草安全剂包括解草酯、解草嗪、解草胺腈、双苯噁唑酸乙酯、吡唑解草酯或解草腈中的任意一种或至少两种的混合物。
11.根据权利要求1所述的油分散组合物,其特征在于,所述表面活性剂包含乳化剂、分散剂、润湿剂、消泡剂、pH调节剂、增稠剂或防腐剂中的至少一种。
12.一种制备如权利要求1所述的油分散组合物的方法,其特征在于,包括以下步骤:
步骤1:将农业化学活性物和表面活性剂加入到非极性有机溶剂中,搅拌使之均匀;
步骤2:将步骤1的混合物经充分研磨得到油基浓缩液;
步骤3:将脂肪醇乙氧基化物按比例加入到油基浓缩液中,搅拌直至混合均匀,得到所述油分散组合物。
13.根据权利要求12所述的方法,其特征在于,步骤2所述研磨在0-50℃的温度下进行,优选15-45℃。
14.根据权利要求12所述的方法,其特征在于,步骤2所述研磨得到油基浓缩液的颗粒粒径D50≤5μm,优选D50≤3μm。
15.一种防止农业油分散制剂组合物中磺胺或磺酰脲类除草活性物的悬浮颗粒互相聚集的方法,其特征在于,所述方法包括加入足够量的脂肪醇乙氧基化丙氧基化物来减少磺胺或磺酰脲类除草活性物的悬浮颗粒相互聚集;所述脂肪醇乙氧基化丙氧基化物选自数均分子量在100-1,000,000的C2-C20脂肪醇乙氧基化丙氧基化物,优选数均分子量在200-100,000的C4-C16脂肪醇乙氧基化丙氧基化物;
优选地,所述足够量的脂肪醇乙氧基化丙氧基化物和磺胺或磺酰脲类除草活性物的重量比为150:1到1:60,优选50:1到1:10,更优选10:1到1:5。
16.脂肪醇乙氧基化丙氧基化物在抑制或防止权利要求1所述的油分散组合物中磺胺或磺酰脲类除草活性物的悬浮颗粒互相聚集中的用途,其特征在于,所述脂肪醇乙氧基化丙氧基化物选自数均分子量在100-1,000,000的C2-C20脂肪醇乙氧基化丙氧基化物,优选数均分子量在200-100,000的C4-C16脂肪醇乙氧基化丙氧基化物;所述脂肪醇乙氧基化丙氧基化物和磺胺或磺酰脲类除草活性物的重量比为150:1到1:60,优选50:1到1:10,更优选10:1到1:5。
17.一种有害生物的防治方法,其特征在于,所述方法为使用根据权利要求1到11任一项所述的油分散组合物于有害生物生长的场所。
18.根据权利要求17所述的防治方法,其特征在于,所述油分散组合物应用时以水喷雾稀释液的形式使用。
19.根据权利要求17或18所述的防治方法,其特征在于,所述油分散组合物包含磺胺或磺酰脲类除草活性物,以防治有害杂草的生长。
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