CN1356873A - 二硝基苯胺和氧乙酰胺的除草可乳化浓缩组合物 - Google Patents
二硝基苯胺和氧乙酰胺的除草可乳化浓缩组合物 Download PDFInfo
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- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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Abstract
本发明提供了二硝基苯胺除草剂和氧乙酰胺除草剂的除草可乳化浓缩组合物。该组合物使用磷酸作为稳定剂以防氧乙酰胺除草剂组分在储存过程中的分解。
Description
本发明的背景
二硝基苯胺除草剂如二甲戊乐灵和氟乐灵、和氧乙酰胺除草剂如氟噻草胺(fluthiamid)是本领域熟知的。使用这些种类除草剂的组合处理公开于美国专利4968342和5759955、以及德国专利№19720367。但包含二硝基苯胺和氧乙酰胺除草剂的可乳化浓缩组合物(emulsifiable concentrate compositions)不为本领域已知。
美国专利3898075涉及包含m-双氨基甲酸酯和有机酸的稳定化液体组合物。美国专利2954396描述了一种用某些水解抑制剂稳定化氨基甲酸酯的方法。但美国专利3898075或美国专利2954396均没有描述任何稳定化氧乙酰胺除草剂的方法。
因此,本发明的一个目的是提供二硝基苯胺除草剂和氧乙酰胺除草剂的稳定的可乳化浓缩组合物。
本领域熟练技术人员由以下描述和所附权利要求书显然得出本发明的其它目的和优点。
本发明的综述
本发明涉及一种除草可乳化浓缩组合物,以重量/重量计,包含约15-40%的二硝基苯胺除草剂、约1-10%的氧乙酰胺除草剂、约0.01-1%的磷酸、至多约30%的乳化剂或乳化剂混合物、至多约1%的消泡剂、和有机溶剂或有机溶剂混合物。
本发明的详细描述
以重量/重量计,本发明的除草可乳化浓缩组合物包含约15-40%的二硝基苯胺除草剂、约1-10%的氧乙酰胺除草剂、约0.01-1%的磷酸、至多约30%的乳化剂或乳化剂混合物、至多约1%的消泡剂、和有机溶剂或有机溶剂混合物。
本发明优选的除草可乳化浓缩组合物以重量/重量计,包含约15-40%的二硝基苯胺除草剂、约1-10%的氧乙酰胺除草剂、约0.01-1%的磷酸、约2-10%的烷基芳基磺酸盐、约0.5-5%的聚亚烷基二醇醚、约1%-5%的乙氧基化脂肪醇、至多约1%的消泡剂、和馏程为约135-305℃的芳烃溶剂。
本发明更优选的可乳化浓缩组合物以重量/重量计,包含约25-35%的二甲戊乐灵、约4-8%的氟噻草胺、约0.05-0.2%的磷酸、约2-6%的十二烷基苯磺酸盐、约1-3%的烷基封端氧化乙烯/氧化丙烯嵌段共聚物、约1-5%的每分子具有约8-12摩尔氧化乙烯的乙氧基化C10-C16脂肪醇、至多约1%的消泡剂、和馏程为约135-305℃的芳烃溶剂。
磷酸是本发明组合物的一种特别重要的成分,因为已经发现,氧乙酰胺除草剂在本发明的含磷酸的可乳化浓缩组合物中比在不含磷酸的相应可乳化浓缩组合物中更加稳定。在本发明的一个优选实施方案中,氧乙酰胺除草剂与磷酸的比率(以重量计)优选为约30∶1-100∶1,更优选为约40∶1-70∶1。
其中:
R是氢原子、C2-C4烷基或氯乙基;
R1是C2-C5烷基、氯乙基、2-甲代烯丙基或环丙基甲基;
R2是氢原子、甲基或氨基;和
R3是三氟甲基、C1-C3烷基、SO2NH2或SO2CH3。
优选用于本发明的二硝基苯胺除草剂包括二甲戊乐灵和氟乐灵,其中二甲戊乐灵更优选。适用于本发明组合物的氧乙酰胺除草剂是描述于以下的那些:
U.S.专利Nos.4,408,055;4,509,971;4,540,430;4,549,899;4,585,471;4,645,525;4,756,741;4,784,682;4,788,291;4,833,243;4,968,342;4,988,380;5,090,991和5,234,896;EP申请 Nos.300344-A和500934-A1;和WO 97/08160.优选用于本发明组合物的氧乙酰胺除草剂具有结构式II:
其中:
R4是氢原子、F、Cl、Br、C1-C4烷基、C1-C4卤代烷基、C1-C4烷氧基、C1-C4卤代烷氧基、C1-C4烷基磺酰基或C1-C4卤代烷基磺酰基;
R5是氢原子或C1-C6烷基;和
R6是任选被1-3个F、Cl、Br、CN、NO2、C1-C4烷基、C1-C4卤代烷基、C1-C4烷氧基或C1-C4卤代烷氧基的任何组合所取代的苯基。
更优选用于本发明可乳化浓缩组合物的氧乙酰胺除草剂是这些,其中:
R4是C1-C4卤代烷基;
R5是C1-C4烷基;和
R6是任选被一个或两个F、Cl、或C1-C4烷基的任何组合所取代的苯基。
最优选的氧乙酰胺除草剂是具有结构式II的这些,其中:
R4是CF3、CHF2或CFCl2;
R5是异丙基;和
R6选自苯基、3-氯苯基、4-氯苯基、2-氟苯基、4-氟苯基、2-甲基苯基、3-甲基苯基、4-甲基苯基和3,4-二甲基苯基。
特别适用于本发明组合物的氧乙酰胺除草剂是4’-氟-N-异丙基-2-{[5-(三氟甲基)-1,3,4-噻二唑-2-基]氧基}乙酰苯胺(氟噻草胺)。
适用于本发明组合物的乳化剂包括但不限于:烷基芳基磺酸盐,包括C8-C18烷基苯磺酸盐如十二烷基苯磺酸钙;聚亚烷基二醇醚,包括烷基封端氧化乙烯/氧化丙烯嵌段共聚物如丁基封端氧化乙烯/氧化丙烯嵌段共聚物;和乙氧基化脂肪醇,包括每分子具有约8-12摩尔氧化乙烯的乙氧基化C10-C16脂肪醇;及其混合物。优选的乳化剂包括十二烷基苯磺酸的碱金属或碱土金属盐,如十二烷基苯磺酸钙,包括可得自Rhodia,Milan,意大利的SOPROPHOR70,一种十二烷基苯磺酸钙在异丁醇中的60%溶液;丁基封端氧化乙烯/氧化丙烯嵌段共聚物,包括可得自Witco SA,Saint-Pierre Les Elbeuf,法国的WITCONOLNS 500K,一种丁基封端氧化乙烯/氧化丙烯嵌段共聚物;和每分子具有约8-12摩尔氧化乙烯的乙氧基化C10-C16脂肪醇,包括可得自Rhodia,Milan,Italy的RHODASURF870,一种每分子包含10摩尔氧化乙烯的C13乙氧基化脂肪醇;及其混合物。
适用于本发明组合物的有机溶剂包括芳烃溶剂如甲苯、二甲苯、多核芳烃如萘和烷基萘及其混合物,其中许多可得自原油分馏且馏程一般为135-305℃,其中最优选馏程为约183-290℃。这些溶剂可以各种商品名购得,如都购自Exxon,Fareham,Hants,英国的SOLVESSO200和AROMATIC200。
适用于本发明组合物的消泡剂包括常规的消泡剂,其中硅氧烷基消泡剂如以商品名SILICOLAPSE购自Rhodia,Lyon,法国的那些是优选的。在本发明的一个优选实施方案中,消泡剂的用量足以防止在使用本发明乳液浓缩物制备罐混合物(tank mixes)时的非所需发泡。通常,低于1%重量的消泡剂是足够的,其中约0.01-0.1%重量的量是优选的。
本发明除草可乳化浓缩组合物可通过将所有成分在有机溶剂中进行混合而制成。在本发明的一个优选实施方案中,该组合物制备如下:
(a)将烷基芳基磺酸盐、乙氧基化脂肪醇、消泡剂和有机溶剂混合得到第一均匀混合物;
(b)在搅拌下向步骤(a)的第一均匀混合物中加入熔融二硝基苯胺和熔融聚亚烷基二醇醚,得到第二均匀混合物;
(c)在搅拌下向步骤(b)的第二均匀混合物中加入氧乙酰胺除草剂,得到第三均匀混合物;和
(d)在搅拌下向步骤(c)的第三均匀混合物中加入磷酸。
本发明的可乳化浓缩组合物用水稀释并以稀水乳液施用到需要进行杂草控制的场所。典型的稀释比率为约1升浓缩物/400升水至4升浓缩物/100升水。尽管本发明组合物在单独使用时可有效地用于控制杂草,但它们也可与包括其它除草剂的其它生物化学品结合或组合使用。
为了便于进一步理解本发明,以下所给出的实施例主要用于举例说明其具体细节。本发明的范围不应视为局限于这些实施例,而是包括在权利要求书中所定义的整个主题。
实施例1
可乳化类似物组合物的制备
将以SOPROPHOR70购自Rhodia,Milan,意大利的60%十二烷基苯磺酸钙异丁醇溶液(53.0克,5.00%重量)、以RHODASURF870购自Rhodia,Milan,意大利的每分子包含10摩尔氧化乙烯的C13乙氧基化脂肪醇(32.0克,3.00%重量)、以SILICOLAPSE431购自Rhodia,Lyon,法国的硅氧烷消泡剂(0.1克,0.01%重量)、和以SOLVESSO200购自Exxon,Fareham,Hants,英国的馏程为约226-279℃的芳烃混合(C10-C13)芳香族化合物(557.0克,52.29%重量)的混合物搅拌至均匀。将熔融二甲戊乐灵(333.3克,90%实际,31.33%重量)和以WITCONOLNS 500K购自Witco SA,Saint-Pierre LesElbeuf,法国的熔融丁基封端氧化乙烯/氧化丙烯嵌段共聚物(21.0克,2.00%重量)在搅拌下加入该混合物。固体氟噻草胺(66.7克,90%实际,6.27%重量)随后加入该混合物并将该混合物搅拌至所有固体物质溶解。将85%磷酸溶液(1.0克,0.10%重量)加入该混合物,搅拌直至均匀,得到在表I中称作组合物№1的可乳化浓缩组合物。
使用基本上相同的步骤,得到在表I中称作组合物№2-14的可乳化浓缩组合物。
表1
可乳化浓缩组合物
成分-%重量/重量化合物№ 二甲戊乐灵 氟噻草胺 85%磷酸溶液 SOPROPHOR RHODASURF WITCONOL SILCOLAPSE SOLVESSO 70 NS 500K 431 200
870
1 31.331 6.271 0.10 5.00 3.00 2.00 0.01 52.29
2 28.202 5.642 0.10 5.00 3.00 2.00 0.01 56.05
3 32.001 6.401 0.05 3.84 2 60 1.06 0.01 54.04
4 32.001 6.401 0.10 3.84 2.60 1.06 0.01 53.99
5 32.001 6.401 0.15 3.84 2.60 1.06 0.01 53.94
6 32.001 6.401 0.20 3.84 2.60 1.06 0.01 53.89
7 32.001 6.401 0.25 3.84 2.60 1.06 0.01 53.84
8 32.001 6.401 0.50 3.84 2.60 1.06 0.01 53.59
9 28.802 5.762 0.05 3.84 2.60 1.06 0.01 57.8810 28.802 5.762 0.10 3.84 2.60 1.06 0.01 57.8311 28.802 5.762 0.15 3.84 2.60 1.06 0.01 57.7812 28.802 5.762 0.20 3.84 2.60 1.06 0.01 57.7313 28.802 5.762 0.25 3.84 2.60 1.06 0.01 57.6814 28.802 5.762 0.50 3.84 2.60 1.06 0.01 57.43190%实际2100%实际
实施例2
试验组合物的储存稳定性的评估
将在表l中确定的试验组合物和以下确定的对比组合物的样品放在玻璃瓶中。将瓶盖上并放在温控储存孵化箱中。在完成所需的储存周期之后,取出样品并分析二甲戊乐灵和氟噻草胺的含量。活性成分含量表示为相对储存之前活性成分含量的百分数(%起始含量)。结果汇总于表II。
由表II数据可以看出,氟噻草胺在含磷酸的本发明可乳化浓缩组合物中比在不含磷酸的对比可乳化浓缩组合物中更加稳定。
对比组合物1
成分 %重量/重量二甲戊乐灵(90%实际) 32.00氟噻草胺(90%实际) 6.40SOPROPHOR70 3.84RHODASURF870 2.60WITCONOLNS 500K 1.06SILCOLAPSE431 0.01SOLVESSO200 54.091按照实施例1所述的步骤来制备,只是没有加入85%磷酸溶液。
表II
储存稳定性的评估
储存温度 储存周期(周) 85%磷酸溶液 %起始含量组合物№
(℃) (%重量/重量) 二甲戊乐灵 氟噻草胺对比组合物 54 2 0 100 95组合物
3 54 2 0.05 100 100
4 54 2 0.10 100 99
5 54 2 0.15 101 99
6 54 2 0.20 100 98
6 37 12 0.20 99 98
7 54 2 0.25 103 103
8 54 2 0.50 102 102对比组合物 37 12 0 101 94组合物
3 37 12 0.05 100 99
4 37 12 0.10 99 101
5 37 12 0.15 99 99
6 37 12 0.20 99 98
Claims (18)
1.一种除草可乳化浓缩组合物,以重量/重量计,它包含约15-40%的二硝基苯胺除草剂、约1-10%的氧乙酰胺除草剂、约0.01-1%的磷酸、至多约30%的乳化剂或乳化剂混合物、至多约1%的消泡剂、和有机溶剂或有机溶剂混合物。
2.根据权利要求1的组合物,其中所述乳化剂或乳化剂混合物包含约2-10%的烷基芳基磺酸盐、约0.5-5%的聚亚烷基二醇醚和约1-5%的乙氧基化脂肪醇,且所述有机溶剂或有机溶剂混合物是馏程为约135-305℃的芳烃溶剂。
3.根据权利要求1的组合物,以重量/重量计,它包含约25-35%的二甲戊乐灵、约4-8%的氟噻草胺、约0.05-0.2%的磷酸、约2-6%的十二烷基苯磺酸盐、约1-3%的烷基封端氧化乙烯/氧化丙烯嵌段共聚物、约1-5%的每分子具有约8-12摩尔氧化乙烯的乙氧基化C10-C16脂肪醇、至多约1%的消泡剂、和馏程为约135-305℃的芳烃溶剂。
4.根据权利要求1的组合物,其中氧乙酰胺除草剂与磷酸的比率以重量计为约30∶1-100∶1。
5.根据权利要求4的组合物,其中所述比率为约40∶1-70∶1。
6.根据权利要求1的组合物,其中所述乳化剂选自烷基芳基磺酸盐、聚亚烷基二醇醚、和乙氧基化脂肪醇、及其混合物。
7.根据权利要求6的组合物,其中所述烷基芳基磺酸盐是C8-C18烷基苯磺酸盐;所述聚亚烷基二醇醚是烷基封端氧化乙烯/氧化丙烯嵌段共聚物;且所述乙氧基化脂肪醇是每分子具有约8-12摩尔氧化乙烯的乙氧基化C10-C16脂肪醇。
8.根据权利要求1的组合物,其中存在消泡剂。
10.根据权利要求1的组合物,其中所述二硝基苯胺除草剂选自二甲戊乐灵和氟乐灵。
11.根据权利要求1的组合物,其中所述二硝基苯胺除草剂是二甲戊乐灵。
12.根据权利要求1的组合物,其中所述氧乙酰胺除草剂具有结构式II:
其中:
R4是氢原子、F、Cl、Br、C1-C4烷基、C1-C4卤代烷基、C1-C4烷氧基、C1-C4卤代烷氧基、C1-C4烷基磺酰基或C1-C4卤代烷基磺酰基;
R5是氢原子或C1-C6烷基;和
R6是任选被1-3个F、Cl、Br、CN、NO2、C1-C4烷基、C1-C4卤代烷基、C1-C4烷氧基或C1-C4卤代烷氧基的任何组合所取代的苯基。
13.根据权利要求12的组合物,其中:
R4是C1-C4卤代烷基;
R5是C1-C4烷基;和
R6是任选被一个或两个F、Cl、或C1-C4烷基的任何组合所取代的苯基。
14.根据权利要求13的组合物,其中:
R4是CF3、CHF2或CFCl2;
R5是异丙基;和
R6选自苯基、3-氯苯基、4-氯苯基、2-氟苯基、4-氟苯基、2-甲基苯基、3-甲基苯基、4-甲基苯基和3,4-二甲基苯基。
15.根据权利要求1的组合物,其中所述氧乙酰胺除草剂是氟噻草胺。
16.根据权利要求1的组合物,其中所述有机溶剂是馏程为约135-305℃的芳烃溶剂。
17.根据权利要求16的组合物,其中所述馏程为约183-290℃。
18.一种包含水和如权利要求1所述的组合物的含水罐混合物。
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