TW201620861A - 微膠囊化硝化抑制劑組成物 - Google Patents
微膠囊化硝化抑制劑組成物 Download PDFInfo
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- TW201620861A TW201620861A TW104114159A TW104114159A TW201620861A TW 201620861 A TW201620861 A TW 201620861A TW 104114159 A TW104114159 A TW 104114159A TW 104114159 A TW104114159 A TW 104114159A TW 201620861 A TW201620861 A TW 201620861A
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Abstract
本發明係關於一種改良的硝化抑制劑組成物及其在農業應用中的用途。
Description
本申請案主張2014年5月2日提出的美國暫時性專利申請案61/988,056之利益,該臨時專利申請案的揭示全文以參考之方式併入本文。
本發明係關於一種經改良的硝化抑制劑組成物及其在農業應用的用途。
(三氯甲基)吡啶化合物諸如氯啶(nitrapyrin)已經與肥料組合而使用作為硝化抑制劑,如描述在U.S.3,135,594中,其於此以參考方式併入本文。這些化合物將所施用之銨氮維持在銨形式(經穩定化的氮),此提高農作物性能。將想要的是,在播種時間廣泛地施用這些化合物與含氮肥料,但是由於潛在的揮發性損失,這些施用方法通常不令人滿意。此外,已經將氯啶加入至無水氨,預設上,其必需被注射進土壤中。
已經將其它氯啶調配物施用至土壤表面,但是其
必需在施用後8小時內機械地併入或摻水進入土壤中以克服揮發性損失。最後,亦已在U.S.4,746,513中揭示出以木質素磺酸酯密封住氯啶之快速或傾瀉釋放式膠囊調配物,其中該文獻以參考之方式併入本文。但是,雖然氯啶之釋放係藉由該密封延遲,該等膠囊在與水分接觸後會釋放出全部氯啶,此具有與先前施用方法相同的穩定性及揮發性缺點。額外的是,這些調配物的製造係困難及代價高且無法與液體尿素硝酸銨(”UAN”)肥料使用。
如在U.S.5,925,464中所揭示,已經使用縮聚密封來密封住農藝活性成份,特別是藉由使用聚胺基甲酸酯而非聚尿素密封劑來提高活性成份之處理安全性及儲存穩定性。
但是,對輸送一在田野環境中具有較大的長時間穩定性,同時能將效力程度維持在可與未密封的硝化抑制劑調配物比較之硝化抑制劑諸如(三氯甲基)吡啶類仍然有需求。
第一組具體實例包括一微膠囊懸浮調配物,其包含:(a)一懸浮相,該懸浮相包括複數個微膠囊,該微膠囊具有體積粒徑中值係約1至約10微米,其中該微膠囊包含:(1)一微膠囊壁,其係藉由在聚合性異氰酸鹽與聚胺間之界面縮聚反應製造,以形成一具有重量百分比係該微膠囊懸浮調配物的總重量之約0.2至約40百分比的聚尿素外殼,及
(2)一實質上液體核心,該實質上液體核心係密封在該聚尿素外殼內,其中該實質上液體核心包含不超過約60重量百分比的硝化抑制劑,在這些具體實例的某些中,該硝化抑制劑係2-氯-6-(三氯甲基)吡啶,及在這些具體實例中,該實質上液體核心包括不超過1.0重量百分比的固體2-氯-6-(三氯甲基)吡啶,如在溫度高於或等於15℃下決定;及(b)一水相,其中該水相包括至少約1.0重量百分比的芳香族溶劑,在某些較佳的具體實例中,該在水相中的芳香族溶劑係在微膠囊形成後加入。
第二組具體實例包括如第一組具體實例的微膠囊懸浮調配物,及進一步包括至少一種存在於水相中的離子安定劑。
第三組具體實例包括如第一或第二組具體實例的微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑係至少一種選自於由下列所組成之群的化合物:輕芳烴、貧萘輕芳烴、重芳烴及貧萘重芳烴。
第四組具體實例包括如第三組具體實例的微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑係貧萘重C10-13芳烴(naphthalene depleted heavy C10-13 aromatics)。
第五組具體實例包括如第四組具體實例的微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約1重量%至約10重量%間之貧萘重C10-13芳烴。
第六組具體實例包括如第四組具體實例的微膠
囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約2重量%至約5重量%間之貧萘重C10-13芳烴。
第七組具體實例包括如第四組具體實例的微膠囊調配物,其中該存在於水相中的芳香族溶劑包含在約2.5重量%至約3.0重量%間之貧萘重C10-13芳烴。
第八組具體實例包括如第三組具體實例的微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑係重C10-13芳烴。
第九組具體實例包括如第八組具體實例的微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約1重量%至約10重量%間之重C10-13芳烴。
第十組具體實例包括如第八組具體實例的微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約2重量%至約5重量%間之重C10-13芳烴。
第十一組具體實例包括如第八組具體實例的微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約2.5重量%至約3.0重量%間之重C10-13芳烴。
第十二組具體實例包括如第一、第二、第三、第四、第五、第六、第七、第八、第九、第十或第十一組具體實例的微膠囊懸浮調配物,其中該微膠囊具有體積粒徑中值係約1至約5微米。
第十三組具體實例包括如第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一或第十二組具體實例的微膠囊懸浮調配物,其中該懸浮相a)對
水相b)的比例係約1:0.75至約1:100。
第十四組具體實例包括如第十三組具體實例的微膠囊懸浮調配物,其中該懸浮相a)對水相b)的比例係約1:1至約1:7。
第十五組具體實例包括如第十三組具體實例的微膠囊懸浮調配物,其中該懸浮相a)對水相b)的比例係約1:1至約1:4。
第十六組具體實例包括如第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、第十二、第十三、第十四或第十五組具體實例的微膠囊懸浮調配物,其中該聚合性異氰酸鹽係聚伸甲基聚苯基異氰酸鹽。
第十七組具體實例包括如第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、第十二、第十三、第十四、第十五或第十六具體實例的微膠囊懸浮調配物,進一步包括氮肥料。
第十八組具體實例如第十七具體實例,其中該氮肥料係尿素硝酸銨。
第十九組具體實例包括一種抑制銨氮在植物生長媒質中硝化的方法,其包括一將如第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、第十二、第十三、第十四、第十五、第十六、第十七、第十八及第十九具體實例的微膠囊懸浮調配物施用至植物生長媒質的步驟。
第二十組具體實例如第十九組具體實例,其中將該調配物併入該生長媒質中。
第二十一組具體實例如第二十組具體實例,其中將該調配物施用至植物生長媒質表面。
第二十二組具體實例一種用以抑制硝化的方法,其中將如第一、第二、第三、第四、第五、第六、第七、第八、第九、第十、第十一、第十二、第十三、第十四、第十五或第十六的調配物與一殺蟲劑組合或相繼地與一殺蟲劑施用。
第二十三組具體實例包括如第二十二組具體實例的方法,其中該調配物係與氮肥料一起施用。
第二十四組具體實例如第二十三組具體實例,其中該氮肥料係尿素硝酸銨。一種微膠囊懸浮調配物,其包括:一懸浮相,該懸浮相包含複數個微膠囊,該微膠囊具有體積粒徑中值係約1至約10微米,其中該微膠囊包含:(1)一微膠囊壁,其係藉由在聚合性異氰酸鹽與聚胺間之界面縮聚反應製造,以形成一具有重量百分比係該微膠囊懸浮調配物的總重量之約0.2至約40百分比的聚尿素外殼,及(2)一實質上液體核心,該實質上液體核心被密封在該聚尿素外殼內,其中該實質上液體核心包含不超過全部微膠囊的40重量百分比之2-氯-6-(三氯甲基)吡啶;及(b)一水相,其中該水相包括至少約1.0重量百分比的芳香族溶劑,其中該至少1.0百分比的芳香族溶劑係在該微膠囊形成後加入至水相。
於本文中進一步揭示出一種微膠囊懸浮調配物,其包含:一具有複數個微膠囊的懸浮相,其具有體積粒徑中值係約1至約10微米,其中該微膠囊包含:一微膠囊壁,其係藉由在聚合性異氰酸鹽與聚胺間之界面縮聚反應製造,以形成一具有重量百分比係該微膠囊懸浮調配物的總重量之約0.2至約15百分比的聚尿素外殼,及一密封在該聚尿素外殼內的化合物,其中該化合物係2-氯-6-(三氯甲基)吡啶;及一水相,其包括一離子安定劑及經分散的芳香族溶劑。
在某些具體實例中,該經分散的芳香族溶劑係至少一種選自於由下列所組成之群的化合物:輕芳烴、貧萘輕芳烴、重芳烴及貧萘重芳烴。在其它具體實例中,該經分散的芳香族溶劑係貧萘重C10-13芳烴。在又其它具體實例中,該調配物包含在約1重量%至約10重量%間之貧萘重C10-13芳烴。在更其它具體實例中,該調配物包含在約2重量%至約5重量%間之貧萘重C10-13芳烴。
在某些具體實例中,該調配物包含在約2.5重量%至約3.0重量%間之貧萘重C10-13芳烴。在又其它具體實例中,該經分散的芳香族溶劑係重C10-13芳烴。在又其它具體實例中,該調配物包含在約1重量%至約10重量%間之重C10-13芳烴。
再者,在範例性具體實例中,該調配物包含在約2重量%至約5重量%間之重C10-13芳烴。再者,該調配物包含在約2.5重量%至約3.0重量%間之重C10-13芳烴。
在進一步具體實例中,該微膠囊具有體積粒徑中
值係約1至約5微米。在其它具體實例中,該懸浮相a)對水相b)的比例係約1:0.75至約1:100。在又其它具體實例中,該懸浮相a)對水相b)係約1:1至約1:7。在進一步具體實例中,該懸浮相a)對水相b)的比例係約1:1至約1:4。
本發明亦揭示出一種微膠囊懸浮液,其中該聚合性異氰酸鹽係聚伸甲基聚苯基異氰酸鹽。在某些具體實例中,該聚胺係選自於乙二胺及二伸乙基三胺。
本發明又進一步揭示出一種肥料組成物,其包含:一氮肥料及上述的微膠囊懸浮調配物。在其它具體實例中,該氮肥料係尿素硝酸銨。
於本文中亦揭示出一種抑制銨氮在生長媒質中硝化的方法,其包括將上述的微膠囊懸浮調配物施用至該生長媒質。在進一步具體實例中,將該調配物併入該生長媒質中。在又進一步具體實例中,將該調配物施用至一生長媒質表面。在其它具體實例中,該調配物係與一殺蟲劑組合或相繼地與一殺蟲劑施用。
在又進一步具體實例中,該調配物係與氮肥料施用。該氮肥料可係尿素硝酸銨。
本發明的微膠囊懸浮調配物穩定且允許延遲氮併入農作物中,因此提供農藝及環境利益。已驚人地發現,當與未經囊封的氯啶組成物比較時,甚至當併入土壤中時,經微膠囊化的(三氯甲基)吡啶化合物諸如氯啶之組成物具有優異的性能。
在本發明之組成物中有用的(三氯甲基)吡啶化合物包括具有吡啶環的化合物及其無機酸鹽,其中該環係經至少一個三氯甲基取代。合適的化合物包括在吡啶環上除了三氯甲基外包含氯或甲基取代基的那些,及包括甲基吡啶類諸如二甲基吡啶、柯林鹼及甲基吡啶的氯化產物。合適的鹽包括鹽酸、硝酸鹽、硫酸鹽及磷酸鹽。在本發明之實行中有用的(三氯甲基)吡啶化合物典型有油狀液體或溶解在溶劑中的結晶固體。在U.S.3,135,594中描述有其它合適的化合物。較佳的(三氯甲基)吡啶有2-氯-6-(三氯甲基)吡啶,其亦已知係氯啶及N-ServeTM(Dow AgroSciences LLC的商標)產品之活性成份。
已經藉由將諸如氯啶的化合物與合適的溶劑一起密封在微膠囊中來大大地增加此化合物之用途。特別有用的微膠囊包含一氯啶/疏水性溶劑的實質上液體核心,其係由聚尿素外殼包圍。具有經選擇的適當體積及外殼厚度與組成物之微膠囊可懸浮在、儲存在水相中及以水相施用。此等有用的調配物係揭示在2009年2月26日提出的美國專利申請案序號12/393,661、2009年9月10日公告的公告案號U.S.2009-0227458 A1;2008年1月18日提出的美國專利申請案序號12/009,432、2008年7月24日公告的公告案號U.S.
2008-0176745 A1中,及在2013年2月19日發佈現在發佈為美國專利案號8,377,849;及2007年1月22日提出之美國臨時專利申請序號60/881,680中,此等全部其全文於此明確地以參考方式併入本文,如若每篇各別以參考方式併入本文般。
雖然上述指出的微膠囊水性懸浮液在某些條件下比未密封於水溶液中的氯啶更穩定,已經觀察到在儲存期間可於氯啶的微膠囊懸浮液之水相中形成氯啶的結晶。在長儲存時期期間,已顯示出於氯啶的水性微膠囊懸浮液中偏愛在約-50C至約150C之非常窄的溫度範圍內形成氯啶結晶,更特別為約00C至100C(攝氏度)。在微膠囊懸浮液的龐大水相中,氯啶結晶的重量百分比係隨著時間累積。依該微膠囊懸浮液如何處理而定,於水相中存在有可測量程度的氯啶結晶可具有些微或無關緊要或無問題。若該懸浮液係透過細點噴嘴與包含同軸篩網的噴霧器藉由噴灑該懸浮液而施用時,在微膠囊懸浮液的水相中存在有甚至約0.1重量百分比或較多的氯啶結晶可特別有問題。
為了抑制或至少明顯減慢在水相中形成氯啶結晶,於本文中揭示出一種微膠囊懸浮調配物組成物,其包括於該微膠囊懸浮液之水相中存在有至少1重量百分比的芳香族溶劑。在某些具體實例中,在水相中累積出有問題的氯啶結晶程度前,將該溶劑加入至該微膠囊懸浮液的水相。在某些具體實例中,在該懸浮液的水相中累積出有問題的氯啶結晶程度後,將該溶劑加入至該懸浮液的水相。
可使用在該微膠囊的有機相中來溶解(三氯甲基)吡啶化合物結晶的典型溶劑之實施例包括芳香族溶劑,特別是經烷基取代的苯,諸如二甲苯或丙基苯餾分;及混合的萘及烷基萘餾分;礦物油;煤油;脂肪酸的二烷基醯胺,特別是脂肪酸的二甲基醯胺,諸如辛酸的二甲基醯胺;氯化的脂肪族及芳烴,諸如1,1,1-三氯乙烷及氯苯;二醇衍生物的酯類,諸如二甘醇的正丁基、乙基或甲基醚之醋酸酯及二丙二醇的甲基醚之醋酸酯;酮類,諸如異佛爾酮及三甲基環己酮(二氫異佛爾酮);及醋酸酯產物,諸如醋酸己基或庚基酯。較佳的有機液體有二甲苯、經烷基取代的苯諸如丙基苯餾分、及烷基萘餾分。
通常來說,若須要時,所使用的溶劑量典型係約40,較佳為約50至約70,較佳為至約60重量百分比,以(三氯甲基)吡啶/溶劑溶液的總重量為基準。在該(三氯甲基)吡啶/溶劑溶液中,該(三氯甲基)吡啶的量典型為約30,較佳為約40至約60,較佳為至約50重量百分比,以該(三氯甲基)吡啶/溶劑溶液的重量為基準。
在本發明中有用的微膠囊可藉由聚合性異氰酸鹽與聚胺之縮聚反應來製備,以形成一聚尿素外殼。該微膠囊化的方法在技藝中熟知及可在本發明中使用任何此方法來提供該膠囊懸浮調配物。通常來說,可藉由首先混合聚合性異氰酸鹽與(三氯甲基)吡啶/溶劑溶液來製備該膠囊懸浮調配物。然後,將此混合物與包括乳化劑的水相結合以形成二相系統。藉由剪切將該有機相乳化進水相中直到
達成想要的顆粒尺寸。然後,逐滴加入一水性交聯聚胺溶液同時進行攪拌,以在一水性懸浮液中形成該(三氯甲基)吡啶之密封顆粒。
想要的顆粒尺寸及胞壁厚度將依實際的應用而定。該等微膠囊典型具有體積粒徑中值係約1至約10微米及膠囊壁厚度係約10至約125奈米。在一個具體實例中,若立即將本發明的調配物併入生長媒質中時,想要的顆粒尺寸可係約2至約10微米且胞壁係約10至約25奈米。在另一個具體實例中,若需要土壤表面穩定性時,想要的顆粒尺寸可係約1-5微米且胞壁厚度係約75至約125奈米。
亦可將其它習知的添加劑併入該調配物中,諸如乳化劑、分散劑、增稠劑、滅菌劑、殺蟲劑、鹽及膜形成聚合物。
該分散及乳化劑包括環氧烷烴與酚類及有機酸的縮合產物、磺酸烷基芳基酯類、脫水山梨糖醇酯類的聚氧基伸烷基衍生物、混合醚醇類、石油磺酸肥皂、木質素磺酸酯類、聚乙烯醇類及其類似物。該界面活性劑通常以該微膠囊懸浮調配物之約1至約20重量百分比的量使用。
在本發明的微膠囊懸浮調配物內之懸浮相對水相的比例係與在最後調配物中之想要的(三氯甲基)吡啶化合物濃度相依。典型來說,該比例將係約1:0.75至約1:100。通常來說,想要的比例係約1:1至約1:7,及較佳為約1:1至約1:4。
(三氯甲基)吡啶化合物之存在抑制銨氮在土壤
或生長媒質中硝化,因此防止源自於氮肥料、有機氮構成物或有機肥料及其類似物的銨氮快速遺失。
通常來說,以該(三氯甲基)吡啶化合物係約0.5至約1.5公斤/公頃之比例施用至土壤或生長媒質來施用本發明的微膠囊懸浮調配物,較佳比例係約0.58至約1.2公斤/公頃。可由施用偏愛考慮到諸如土壤pH、溫度、土壤型式及施用模式之因素容易地查明較佳量。
可使用將對有興趣的農作物有益之任何方式來施用本發明的微膠囊懸浮調配物。在一個具體實例中,使用帶式或列式施用將該微膠囊懸浮調配物施用至生長媒質。在另一個具體實例中,在播種或移植想要的農作物前,將該調配物施用至或遍及該生長媒質。在更另一個具體實例中,可將該調配物施用至生長植物的根區域。
額外地,該微膠囊懸浮調配物可伴隨著氮肥料之施用而施用。該調配物可在肥料施用前、後或與其同步地施用。
本發明的微膠囊懸浮調配物具有增加的利益,其可施用至土壤表面數天至數週而沒有額外的水或機械併入土壤中。再者,若須要時,本發明的調配物可在施用後直接併入土壤中。
本發明的微膠囊懸浮調配物典型具有(三氯甲基)吡啶化合物濃度量係約1,較佳為約10及更佳為約15至約50典型至約35,較佳為至約30及更佳為至約25重量百分比,以該微膠囊懸浮調配物的總重量為基準,較佳範圍係在約5
至約40重量百分比間之氯啶。然後,讓該微膠囊懸浮調配物與溶劑或水混合以獲得想要用於施用的比例。
可藉由將該微膠囊懸浮調配物分散在肥料諸如銨或有機氮肥料中來製備一土壤處理組成物。所產生的肥料組成物可就此使用或可進行修改,如藉由以額外的氮肥料或以惰性固體載劑稀釋而獲得一包含想要的活性藥劑量用於土壤處理之組成物。
該土壤可與本發明之微膠囊懸浮調配物以任何方便的方式製備,包括與土壤機械混合;施用至土壤表面,之後拖曳或切割進土壤中至想要的深度;或諸如藉由注射、噴灑、撒粉或灌溉運送進土壤中。在灌溉施用中,可將適當量的該調配物引進至灌溉水,以獲得(三氯甲基)吡啶化合物之分佈至最高6英吋(15.24公分)的想要深度。
驚人的是,一旦併入土壤中,本發明的微膠囊懸浮調配物勝過其它氯啶調配物,特別是未經囊封的形式。已認為該密封組成物將無法如非密封形式般足夠有效地釋放出氯啶,其中從膠囊擴散出將太慢而無法提供生物學效應,但是事實上觀察到相反的效應。
由於氯啶在本發明的微膠囊懸浮調配物中之控制式釋放,可達到數個優點。首先,因為其在一段延長的時間內更有效率地釋放進土壤中,可減少氯啶的量。額外的是,若須要時,本發明的微膠囊懸浮調配物可施用及遺留在表面上不需要機械併入而自然併入土壤中。
在該微膠囊懸浮調配物的某些具體實例中,將芳
香族溶劑後加入(即,在微膠囊形成後)至水相來減低在某些溫度儲存條件下於水相中的結晶形成及/或生長速率。在一個具體實例中,該後加入芳香族溶劑提供在冷溫度儲存條件下優異的減低結晶生長。在典型的具體實例中,此後加入的芳香族溶劑包括油,及其在微膠囊形成後係存在於該調配物之水相中。用語”油”於本文中將描述為通常不能與水相混合的溶劑。
在某些具體實例中,可藉由將一或多種芳香族溶劑加入至水相來處理在水相中已經包括氯啶結晶及沒有芳香族溶劑之微膠囊懸浮調配物,及可在周溫下攪拌所得的混合物一段時間大概30分鐘至5小時,以該微膠囊懸浮液的總體積為基準,直到氯啶結晶已消失。
若沒有將一或多種芳香族溶劑加入至水相,本申請案的微膠囊懸浮調配物可在約100C的中冷儲存溫度下於水相中形成氯啶結晶。該氯啶結晶可係約99%純。隨著時間,此等結晶可構成該整體微膠囊懸浮調配物的最高0.5重量百分比。但是,亦可在其它溫度下形成結晶,諸如00C、-50C及150C。溶劑基底的結晶生長抑制劑諸如芳香族溶劑可特別在約100C的中冷儲存溫度下提供優異的物理穩定性,以防止在該微膠囊懸浮液的水相中形成結晶。
可在微膠囊懸浮液形成後加入之芳香族溶劑闡明性包括:Aromatic 100 Fluid,亦已知為石油腦溶劑或輕芳烴;Aromatic 150 Fluid,亦已知為石油腦溶劑、重芳烴、高閃燃芳香族石油腦(high flash aromatic naphtha)型式II、
重芳烴溶劑石油腦、烴、C10芳烴、>1%萘、A150、S150(Solvesso 150);及Aromatic 200 Fluid,亦已知為石油腦溶劑、重芳烴、高閃燃芳香族石油腦型式II、重芳烴溶劑石油腦、烴、C10-13芳烴、>1%萘、A200及S200(Solvesso 200)。
在某些具體實例中,可在微膠囊懸浮液形成後加入至該調配物之芳香族溶劑包括貧萘或包含少於約1%的萘。該溶劑可在結晶形成前加入至該微膠囊懸浮調配物作為預防措施,或在結晶形成後加入至該微膠囊懸浮調配物作為補救措施以移除或減低結晶存在。
額外的是,本發明的微膠囊懸浮調配物可與相關連的殺蟲劑結合或使用,包括殺節肢動物劑、殺菌劑、殺真菌劑、除草劑、殺蟲劑、殺蟎劑、殺線蟲劑、硝化抑制劑諸如雙氰胺、尿素酶抑制劑諸如N-(正丁基)硫代磷酸三醯胺及其類似物、或殺蟲混合物及其協同混合物。在此施用中,本發明的微膠囊懸浮調配物可與想要的殺蟲劑槽混合或它們可相繼地施用。
範例性除草劑包括但不限於乙草胺(acetochlor)、草不綠(alachlor)、氯胺基啶酸(aminopyralid)、莠去津(atrazine)、解草酮(benoxacor)、溴苯腈、克繁草(carfentrazone)、氯磺隆(chlorsulfuron)、炔草酸(clodinafop)、克草立特(clopyralid)、麥草畏(dicamba)、二氯苯氧基丙酸-甲基、汰草滅(dimethenamid)、芬惡普(fenoxaprop)、氟唑磺隆(flucarbazone)、氟噻草胺(flufenacet)、濶草清
(flumetsulam)、氟烯草酸(flumiclorac)、氟草定(fluroxypyr)、固殺草(glufosinate-ammonium)、鎮草寧、合速隆(halosulfuron)-甲基、咪草酸(imazamethabenz)、甲氧咪草煙(imazamox)、依滅草(imazapyr)、滅草喹(imazaquin)、咪唑乙煙酸(imazethapyr)、異惡唑草酮(isoxaflutole)、快克草(quinclorac)、MCPA、MCP胺、MCP酯、高效甲霜靈(mefenoxam)、硝磺草酮(mesotrione)、莫多草(metolachlor)、左旋莫多草(s-metolachlor)、賽克津(metribuzin)、甲磺隆(metsulfuron)甲基、煙嘧磺隆(nicosulfuron)、對草快(paraquat)、施得圃(pendimethalin)、毒莠定(picloram)、氟嘧磺隆(primisulfuron)、丙苯磺隆(propoxycarbazone)、三氟丙磺隆(prosulfuron)、派芬草(pyraflufen ethyl)、玉嘧磺隆(rimsulfuron)、西瑪三、磺醯磺隆(sulfosulfuron)、噻磺隆(thifensulfuron)、苯吡唑草酮(topramezone)、三甲苯草酮(tralkoxydim)、野麥畏(triallate)、醚苯磺隆(triasulfuron)、苯磺隆(tribenuron)、三氯比(triclopyr)、氟樂靈(trifluralin)、2,4-D、2,4-D胺、2,4-D酯及其類似物。
範例性殺蟲劑包括但不限於1,2-二氯丙烷、1,3-二氯丙烯、阿巴汀(abamectin)、歐殺松(acephate)、亞醌蟎(acequinocyl)、亞滅培(acetamiprid)、家蠅磷(acethion)、乙醯蟲腈(acetoprole)、阿納寧(acrinathrin)、丙烯腈、棉鈴威(alanycarb)、得滅克(aldicarb)、涕滅碸威(aldoxycarb)、阿多靈(aldrin)、丙烯除蟲菊酯、阿洛氨菌素(allosamidin)、除害威(allyxycarb)、α賽滅寧(cypermethrin)、α蛻皮激素、賽
硫磷(amidithion)、磺胺蟎酯(amidoflumet)、滅害威(aminocarb)、胺吸磷(amiton)、三亞蟎(amitraz)、毒藜鹼、氧化亞砷、乙基殺扑磷(athidathion)、茚苦楝子素、亞滅松(azamethiphos)、谷速松(azinphos)乙基、谷速松甲基、偶氮苯、三唑錫(azocyclotin)、偶氮磷(azothoate)、六氟矽酸鋇、熏蟲菊(barthrin)、異噻蟲唑(benclothiaz)、惡蟲威(bendiocarb)、免扶克(benfuracarb)、苯惡磷(benoxafos)、免速隆(bensultap)、苯蟎特(benzoximate)、苯甲酸苄酯、β賽扶寧(cyfluthrin)、β賽滅寧、聯苯阱酯(bifenazate)、畢芬寧(bifenthrin)、百蟎克(binapacryl)、反丙烯除蟲菊、苄呋烯菊酯(bioethanomethrin)、生物氯菊酯(biopermethrin)、雙三氟蟲脲(bistrifluron)、硼砂、硼酸、溴苯烯磷(bromfenvinfos)、溴DDT、溴殺烯(bromocyclen)、溴磷松(bromophos)、溴磷松乙基、新殺蟎(bromopropylate)、必克蝨(bufencarb)、布芬隆(buprofezin)、畜蟲威(butacarb)、特嘧硫磷(butathiofos)、丁酮威(butocarboxim)、布托酯(butonate)、丁酮碸威(butoxycarboxim)、克線丹(cadusafos)、砷酸鈣、聚硫醚鈣、毒殺芬(camphechlor)、氯滅殺威(carbanolate)、加保利(carbaryl)、加保扶(carbofuran)、二硫化碳、四氯化碳、加芬松(carbophenothion)、丁基加保扶、培丹(cartap)、滅蟎猛(chinomethionat)、剋安勃(chlorantraniliprole)、氯殺蟎(chlorbenside)、冰片丹(chlorbicyclen)、氯丹(chlordane)、十氯酮(chlordecone)、克死蟎(chlordimeform)、氯氧磷(chlorethoxyfos)、克凡派(chlorfenapyr)、殺蟎醇
(chlorfenethol)、殺蟎酯(chlorfenson)、敵蟎特(chlorfensulphide)、克芬松(chlorfenvinphos)、克福隆(chlorfluazuron)、氯甲磷(chlormephos)、克氯苯(chlorobenzilate)、氯仿、伊托明(chloromebuform)、滅蟲脲(chloromethiuron)、氯化苦(chloropicrin)、克氯蟎(chloropropylate)、氯辛硫磷(chlorphoxim)、氯吡唑磷(chlorprazophos)、陶斯松(chlorpyrifos)、陶斯松甲基、蟲蟎磷(chlorthiophos)、環蟲醯阱(chromafenozide)、瓜菊酯I、瓜菊酯II、順式苄呋菊酯(cismethrin)、除線威(cloethocarb)、克芬蟎(clofentezine)、氯氰碘柳胺(closantel)、可尼丁(clothianidin)、乙醯亞砷酸銅、砷酸銅、環烷酸銅、油酸銅、蠅毒磷(coumaphos)、畜蟲磷(coumithoate)、克羅他命酮(crotamiton)、賽吸磷(crotoxyphos)、苦塔冷(cruentaren)A&B、育畜磷(crufomate)、冰晶石、苯腈磷(cyanofenphos)、氰乃松(cyanophos)、果蟲磷(cyanthoate)、環蟲菊酯(cyclethrin)、乙氰菊酯(cycloprothrin)、腈吡蟎酯(cyenopyrafen)、賽芬蟎(cyflumetofen)、賽扶寧、賽洛寧(cyhalothrin)、環己錫、賽滅寧、賽酚寧(cyphenothrin)、賽滅淨(cyromazine)、賽滅磷(cythioate)、d-苧烯、邁隆(dazomet)、DBCP、DCIP、DDT、一甲呋喃丹(decarbofuran)、第滅寧(deltamethrin)、田樂磷(demephion)、田樂磷O、田樂磷S、內吸磷、內吸磷甲基、內吸磷O、內吸磷O甲基、內吸磷S、內吸磷S甲基、內吸磷S甲基碸(methylsulphon)、汰芬隆(diafenthiuron)、得拉松(dialifos)、除線特(diamidafos)、大利松(diazinon)、異氯硫
磷(dicapthon)、除線磷(dichlofenthion)、異發靈(dichlofluanid)、二氯松(dichlorvos)、開樂散(dicofol)、敵克梭(dicresyl)、雙特松(dicrotophos)、地昔尼爾(dicyclanil)、地特靈(dieldrin)、除蟎靈(dienochlor)、氟蟎(diflovidazin)、二福隆(diflubenzuron)、雙羥丙茶鹼(dilor)、四氟甲醚菊酯(dimefluthrin)、二美氟、地麥威(dimetan)、大滅松(dimethoate)、苄菊酯(dimethrin)、甲基毒蟲畏(dimethylvinphos)、敵蠅威、消蟎酚、大脫蟎(dinobuton)、白粉克(dinocap)、白粉克4、白粉克6、鄰敵蟎消(dinocton)、硝戊酯(dinopenton)、硝丙酚(dinoprop)、戊硝酚(dinosam)、硝辛酯(dinosulfon)、呋蟲胺(dinotefuran)、硝丁酯(dinoterbon)、戴芬蘭(diofenolan)、蔬果磷(dioxabenzofos)、二氧威(dioxacarb)、大克松(dioxathion)、二苯基碸、二硫龍(disulfiram)、二硫松(disulfoton)、噻喃磷(dithicrofos)、DNOC、苯氧炔蟎(dofenapyn)、得拉滅克汀(doramectin)、蛻皮甾酮(ecdysterone)、因滅汀(emamectin)、EMPC、益避寧(empenthrin)、安殺番(endosulfan)、因毒磷(endothion)、因特靈(endrin)、EPN、保幼醚(epofenonane)、依立諾克汀(eprinomectin)、益化利(esfenvalerate)、依他磷(etaphos)、愛芬克(ethiofencarb)、愛殺松(ethion)、乙蟲清(ethiprole)、益果(ethoate methyl)、普伏松(ethoprophos)、乙基DDD、甲酸乙酯、二溴化乙烯、二氯化乙烯、環氧乙烷、醚菊酯(etofenprox)、依殺(etoxazole)、益多松(etrimfos)、EXD、氨磺磷(famphur)、芬滅松(fenamiphos)、抗蟎唑(fenazaflor)、
芬殺蟎(fenazaquin)、芬布賜(fenbutatin oxide)、皮蠅磷(fenchlorphos)、乙苯威(fenethacarb)、五氟苯菊酯(fenfluthrin)、撲滅松(fenitrothion)、丁基滅必蝨(fenobucarb)、芬硫克(fenothiocarb)、芬納克瑞(fenoxacrim)、芬諾克(fenoxycarb)、吡氯氰菊酯(fenpirithrin)、芬普寧(fenpropathrin)、芬普蟎(fenpyroximate)、芬蟎酯(fenson)、繁福松(densulfothion)、芬殺松(fenthion)、芬殺松乙基、氟硝二苯胺(fentrifanil)、芬化利(fenvalerate)、芬普尼(fipronil)、氟尼胺(flonicamid)、嘧蟎酯(fluacrypyrim)、氟佐隆(fluazuron)、氟大滅(flubendiamide)、弗卞敏(flubenzimine)、伏康脲(flucofuron)、氟環脲(flucycloxuron)、護賽寧(flucythrinate)、聯氟蟎(fluenetil)、嘧蟲胺(flufenerim)、氟芬隆(flufenoxuron)、弗芬克斯(flufenprox)、氟氯苯氰菊酯(flumethrin)、氟殺蟎(fluorbenside)、福化利(fluvalinate)、大福松(fonofos)、覆滅蟎(formetanate)、福木松(formothion)、胺甲威(formparanate)、丁苯硫磷(fosmethilan)、福司吡酯(fospirate)、福賽絕(fosthiazate)、丁硫環磷(fosthietan)、丁硫環磷、呋線威(furathiocarb)、糠醛菊酯(furethrin)、糠醛、γ賽洛寧、γHCH、合芬寧(halfenprox)、氯醯阱(halofenozide)、HCH、HEOD、七氯(heptachlor)、飛達松(heptenophos)、速殺硫磷(heterophos)、六伏隆(hexaflumuron)、合賽多(hexythiazox)、HHDN、愛美松(hydramethylnon)、氰化氫、烯蟲乙酯(hydroprene)、喹啉威(hyquincarb)、依米賽福司(imicyafos)、益達胺(imidacloprid)、依普寧(imiprothrin)、
因得克(indoxacarb)、碘甲烷、IPSP、抑滅伏(isamidofos)、氯唑磷(isazofos)、碳氯靈(isobenzan)、水胺硫磷(isocarbophos)、異艾氏劑(isodrin)、亞芬松(isofenphos)、滅必蝨(isoprocarb)、亞賜圃(isoprothiolane)、獲賜松(isothioate)、加福松(isoxathion)、伊維菌素茉莉菊酯(jasmolin)I、茉莉菊酯II、碘硫磷(jodfenphos)、青春激素I、青春激素II、青春激素III、克來范(kelevan)、丙諾保幼素(kinoprene)、λ賽洛寧、砷酸鉛、雷皮菌素(lepimectin)、對溴磷(leptophos)、靈丹(lindane)、啶蟲磷(lirimfos)、祿芬隆(lufenuron)、噻唑磷(lythidathion)、馬拉松(malathion)、特蟎腈(malonoben)、疊氮磷(mazidox)、滅加松(mecarbam)、甲基滅蚜磷(mecarphon)、滅蚜松(menazon)、地胺磷(mephosfolan)、氯化亞汞、甲硫酚(mesulfen)、倍硫磷亞碸(mesulfenfos)、美氟綜(metaflumizone)、威百畝(metam)、蟲蟎畏(methacrifos)、達馬松(methamidophos)、滅大松(methidathion)、滅賜克(methiocarb)、殺蟲乙烯磷(methocrotophos)、納乃得(methomyl)、美賜平(methoprene)、甲氧滴滴涕、甲氧蟲醯阱(methoxyfenozide)、溴甲烷、異硫代氰酸甲酯、甲氯仿、二氯甲烷、美特寧、治滅蝨(metolcarb)、惡蟲酮(metoxadiazone)、美文松(mevinphos)、茲克威(mexacarbate)、密滅汀(milbemectin)、米貝黴素(milbemycin)肟、丙胺氟(mipafox)、滅蟻靈(mirex)、MNAF、亞素靈(monocrotophos)、茂果(morphothion)、摩西達克汀(moxidectin)、萘酞磷(naftalofos)、乃力松(naled)、萘、尼古丁、氟蟻靈(nifluridide)、
尼可黴素(nikkomycins)、烯啶蟲胺(nitenpyram)、硝蟲噻(nithiazine)、戊氰威(nitrilacarb)、諾魯隆(novaluron)、諾福隆(noviflumuron)、歐滅松(omethoate)、歐殺滅(oxamyl)、滅多松(oxydemeton methyl)、異亞碸磷(oxydeprofos)、碸撲磷(oxydisulfoton)、對二氯苯、巴拉松(parathion)、巴拉松甲基、氟幼脲(penfluron)、五氯苯酚、百滅寧(permethrin)、芬硫磷(phenkapton)、酚丁滅寧(phenothrin)、賽達松(phenthoate)、福瑞松(phorate)、裕必松(phosalone)、硫環磷(phosfolan)、益滅松(phosmet)、對氯硫磷(phosnichlor)、福賜米松(phosphamidon)、膦、弗弗松(phosphocarb)、巴賽松(phoxim)、巴賽松甲基、甲胺嘧磷(pirimetaphos)、比加普(pirimicarb)、亞特松(pirimiphos)乙基、亞特松甲基、亞砷酸鉀、硫氰酸鉀、pp’DDT、普亞滅寧(prallethrin)、早熟素(precocene)I、早熟素II、早熟素III、醯胺嘧啶磷(primidophos)、丙氯醇(proclonol)、佈飛松(profenofos)、丙氟菊酯(profluthrin)、蜱虱威(promacyl)、猛殺威(promecarb)、加護松(propaphos)、歐蟎多(propargite)、胺丙畏(propetamphos)、安丹(propoxur)、乙噻唑磷(prothidathion)、普硫松(prothiofos)、飛克松(prothoate)、羅芬布(protrifenbute)、白克松(pyraclofos)、吡氟蟲腈(pyrafluprole)、定菌磷(pyrazophos)、派瑞美辛(pyresmethrin)、除蟲菊酯I、除蟲菊酯II、畢達本(pyridaben)、啶蟲丙醚(pyridalyl)、必芬松(pyridaphenthion)、派夫昆松(pyrifluquinazon)、畢汰芬(pyrimidifen)、嘧硫磷(pyrimitate)、皮瑞普(pyriprole)、百
利普芬(pyriproxyfen)、夸西亞(quassia)、拜裕松(quinalphos)、拜裕松、拜裕松甲基、喹塞昂(quinothion)、匡替飛斯(quantifies)、碘醚柳胺(rafoxanide)、列滅寧(resmethrin)、魚藤酮、魚尼丁(ryania)、沙巴藜蘆(sabadilla)、八甲磷(schradan)、西拉滅汀(selamectin)、矽護芬(silafluofen)、亞砷酸鈉、氟化鈉、六氟矽酸鈉、硫氰酸鈉、蘇硫磷(sophamide)、賜諾特(spinetoram)、賜諾殺(spinosad)、螺蟎酯(spirodiclofen)、螺甲蟎酯(spiromesifen)、螺蟲乙酯(spirotetramat)、磺苯醚隆(sulcofuron)、舒非侖(sulfiram)、氟蟲胺(sulfluramid)、治螟磷(sulfotep)、硫、氟化硫醯、硫丙磷(sulprofos)、τ福化利(fluvalinate)、噻蟎威(tazimcarb)、TDE、得芬諾(tebufenozide)、吡蟎胺(tebufenpyrad)、嘧丙磷(tebupirimfos)、得福隆(teflubenzuron)、泰氟菊酯、亞培松(temephos)、TEPP、環戊烯丙菊酯(terallethrin)、托福松(terbufos)、四氯乙烷、殺蟲畏、得脫蟎(tetradifon)、治滅寧(etramethrin)、四抗霉素(tetranactin)、殺蟎好(tetrasul)、θ賽滅寧、噻蟲啉(thiacloprid)、賽速安(thiamethoxam)、噻氯磷(thicrofos)、抗蟲威(thiocarboxime)、硫賜安(thiocyclam)、硫敵克(thiodicarb)、硫伐隆(thiofanox)、甲基乙拌磷、蟲線磷(thionazin)、克殺蟎(thioquinox)、硫殺塔(thiosultap)、蘇力菌素(thuringiensin)、脫派雷(tolfenpyrad)、泰滅寧(tralomethrin)、拜富寧(transfluthrin)、反氯菊酯(transpermethrin)、苯蟎噻(triarathene)、唑蚜威(triazamate)、三落松(triazophos)、三氯松(trichlorfon)、異皮蠅磷
(trichlormetaphos)3、毒壤膦(trichloronat)、三氯丙氧磷(trifenofos)、三福隆(triflumuron)、混滅威(trimethacarb)、烯蟲硫酯(triprene)、繁米松(vamidothion)、繁米松、氟吡唑蟲(vaniliprole)、氟吡唑蟲、XMC、滅殺威(xylylcarb)、ζ賽滅寧及丙硫惡唑磷(zolaprofos)。
可額外使用上述殺蟲劑之任何組合。
可額外使用在防除標的害蟲上具有效力來自DuPont之Rynaxypyr(TM),一種新的農作物保護化學物質。
如遍及本專利說明書所使用,用語”約”指為所描述的值加或減10%,例如用語”約1.0”包括0.9至1.1的值。
提供下列實施例來闡明本發明。該等實施例不想要限制本發明的範圍及它們應該不如此解釋。量係以重量份或重量百分比計,除非其它方面有指示出。
表I總整理出用於膠囊懸浮液製備的組分之重量百分比。總配料的大小係以所使用的氯啶之重量為基準,其典型為大約25克。以所指示出的濃度加入乳化劑及交聯胺之水溶液。微膠囊懸浮調配物技術在技藝中知曉。額外在技藝中亦熟知的是,用以製造微膠囊懸浮調配物的加入順序及相應程序可製造出具有不同物理特徵(諸如黏性)的調配物。下列製備程序係製備程序的一個闡明性具體實例,及應該不視為本發明之限制。
將油可溶性單體PAPI 27(聚伸甲基聚苯基異氰
酸鹽)(Dow Chemical)加入至寬嘴廣口瓶。然後,加入呈50%氯啶儲存溶液形式的氯啶(Dow AgroSciences)及Aromatic 200(Exxon)。讓所產生的有機相與如在表I中指示出的乳化劑水溶液結合。使用安裝有¾英吋混合管及一般目的乳化頭之Silverson L4RT-A高速混合器來乳化所產生的二相混合物。藉由首先使用位於水相中的混合管末端吸入有機相,以相對低速度(~1000rpm)混合直到充分乳化來達成乳化。然後,以離散式增量來增加速度,在每次增加後測量顆粒尺寸。繼續此方法直到獲得想要的顆粒尺寸。然後,逐滴加入可溶於水的胺(二伸乙基三胺(DETA,Aldrich)或乙二胺(EDA,Aldrich)溶液(10重量%在水中),同時以減低的速率攪拌。在完全加入後,攪拌所產生的膠囊懸浮液額外一分鐘。在膠囊形成後,如在表I中指示出般加入Kelzan S(如為1.5%水溶液)、矽酸鎂鋁(如為5%水溶液)、Proxel GXL及剩餘部分的水,及使用Silverson混合器進行最後均化。
使用安裝有小體積樣品單元的Malvern Mastersizer 2000光散射顆粒尺寸器來決定膠囊懸浮液顆粒尺寸分佈。表II報導出每種調配物的體積中點分佈(”VMD”)。
以球形體積相關於其半徑的幾何公式為基準來計算達成標的壁厚度所需要之膠囊壁組分的量。若假設一核殼型形態且該核心包含非壁形成、不溶於水的組分(氯啶、溶劑)及該外殼由可聚合材料(可溶於油及水的單體)構成時,則核心體積(Vc)與核心體積加上外殼體積(Vs)的比例相關於其各別半徑之方程式(1)可適用,其中rs係包括外殼的膠囊半徑及ls係外殼厚度。
對外殼體積求解方程式(1)產生:
以質量(mi)及密度(di)取代其各別體積(ms/ds=Vs
及mc/dc=Vc,其中下標s或c各別指為外殼或核心),及對外殼質量求解提供:
藉由比較方程式(2)及(3)可看見,當使用質量來
計算製造出具有想要的尺寸及壁厚度之膠囊所需要的壁組分之量時,密度比例ds/dc的效應為施用一常數修正因子。
因此,為了精確計算ms,核心及外殼的密度必需已知或至少從每種組分的密度之加權平均估計。但是,這些計算的主要目的為使用膠囊壁厚度作為方便的概念工具,其將有希望地有助於了解膠囊性能行為,因此,設計出新的膠囊調配物。對此目的來說,大約值感覺係足夠。考慮到這一點,將ds/dc值設定為1來進行簡化,此產生方程式(4)。
進行下列取代:mc=mo-mOSM,ms=mo+(fWSM/OSM))mOSM-mc,及fWSM/OSM=mWSM/mOSM(可溶於水的單體對可溶於油的單體之比例),其中mo係油組分(氯啶、溶劑、可溶於油的單體)之總質量,mOSM係可溶於油的單體之質量,及mWSM係可溶於水的單體之質量,及對mOSM求解產生:
對決定mOSM來說,在計算時使用全部量的mWSM。在本研究中,對全部膠囊懸浮液製備來說,該可溶於水的
單體相對於該可溶於油的單體係以1:1當量使用。
相反地,對每種膠囊懸浮液製劑來說,對rs值及方程式(6)使用VMD顆粒尺寸來計算膠囊壁厚度ls。表II包括這些值。
收集、風乾及壓碎Drummer粉砂黏壤土(sicl)土壤的大批樣品,通過2毫米篩網。在土壤製備後,將大約25克經處理的土壤放進燒杯中,及使用實施例調配物1-5每種,以7.5毫升包含10毫克N(如為(NH4)2SO4)及0.0、0.25或0.50ppm氯啶(以土壤樣品之重量為基準)的水處理。然後,將該經處理的土壤均勻地分佈在土壤表面上且立即以另外25克土壤覆蓋。每種比例提供三個複製品,和三個50克沒有加入肥料或抑制劑的土壤樣品,及三個經N-Serve 24(Dow AgroSciences)處理的土壤複製品。一旦液體被吸收進土壤中,混合該等材料以獲得該肥料/實施例調配物的均勻分佈。在混合後,加入水使得土壤達到田間容水量。燒杯不密封,但是進行覆蓋以減少蒸發及維持在大約25℃的室溫下。以5天的區間測量從每個燒杯損失的水量,及若損失超過2.5毫升時進行置換。
在開始育成後的第7,14,21,28,35,42,49及56天時,乾燥、研磨及混合包含在每個各別燒杯中的土壤。分析次樣品的NH4-N,如由Mulvaney,R.L.1996;”Nitrogen-Inorganic Forms”,pp.1123-1184描述。在D.L.Sparks(ed.)Methods of soil analysis:Part 3/SSSA Book Ser.5.SSSA,Madison,WI中。若少於30%的N以銨餘留在任何處理之全部複製品中時,停止該處理之分析。表III及表IV提供複製品的平均。
在相同比例下,比較該微膠囊化調配物與氯啶N-Serve 24(可從Dow AgroSciences獲得)調配物。在第5週時,進行測試之全部五個經密封使用0.5ppm氯啶的調配物皆勝過N-Serve 24,此闡明在相同比例下,它們提供優異的剩餘氮穩定性能。
範例性組成物6及7的水相進一步包括一離子安定劑。在這些組成物中,使用係二辛基磺基琥珀酸鈉(Geropon SDS,可從Rhodia獲得)的離子安定劑。取代或除了二辛基磺基琥珀酸鈉外,可使用任何其它合適的離子安定劑。
將範例性組成物6及7及N-Serve 24(0.5磅活性成份/英畝;0.58公斤/公頃)與尿素硝酸銨(UAN)(160磅/英畝;181.5公斤/公頃)組合的四個複製品、和尿素硝酸銨(160磅N/英畝;181.5公斤/公頃)與0硝化抑制劑處理之四個複製品施用至掃除植被的Drummer sicl樣品。
在施用實施例調配物後,讓該調配物立即與水分併合。一旦併合發生,將處理開放至天然下雨及環境影響。
在併合後第21,28,35,42,49及56天時,從每個處理收集土壤樣品及對NH4-N分析,如由Mulvaney所描述般,如參照先前。收集深度0-3英吋(0-7.6公分)的樣品8週,在併入第一處理後7及8週時,額外收集深度3-6英吋(7.6公分-15.2公分)的樣品。在施用當天,收集深度0-3英吋
(0-7.6公分)的樣品用於NH4-N分析。
藉由分析土壤樣品之銨分子(NH4)存在來測量硝化抑制劑將氮保持在氨形式的效率。表V報導出複製品的平均。
在進一步分析中,實施例6及7的硝化抑制係與那些調配物的表面穩定性耦合。UAN單獨及UAN+N-Serve處理係在施用當天以水分併合至土壤,同時在併合前一週將二個實施例調配物鋪在土壤表面上。當預示有下雨事件時,保護等待水分併入的土地免受水分。結果列在表VI中。
現在參照表V及VI。範例性組成物6及7二者係比
N-Serve 24更有效的硝化抑制劑。
表VII列出使用於範例性組成物的膠囊懸浮液製備之組分的重量百分比。總配料的大小係2.1公斤(範例性組成物8)或185克(範例性組成物9)。將可溶於油的單體PAPI 27(聚伸甲基聚苯基異氰酸鹽,Dow Chemical)加入至寬嘴廣口瓶。然後,以氯啶工藝濃縮儲存溶液的形式加入N-Serve TG(Dow AgroSciences;90重量%氯啶)及Aromatic 200(Exxon)。將所產生的均勻有機相與由Kraftsperse 25M、Tergitol 15-S-7、Geropon SDS及Proxcel GXL構成的水溶液結合。
使用安裝有%英吋混合管及一般目的乳化頭之Silverson L4RT-A高速混合器來乳化所產生的二相混合物。藉由首先使用位於水相中的混合管末端吸入有機相,以相當低的速度(-1000rpm)混合直到充分乳化來達成乳化。然後,以離散式增量增加速度,在每次增加後測量顆粒尺寸。繼續此方法直到獲得想要的顆粒尺寸(2.5微米)。
其次,逐滴加入可溶於水的胺乙二胺水溶液(在實施例8中係20重量%;在範例性組成物9、10及11中係30重量%),同時以減低的速率攪拌該混合物。在加入可溶於水的胺後,攪拌所產生的膠囊懸浮液額外的時間以允許該聚尿素外殼形成反應進一步朝向完成進行。在膠囊形成後,該完成相包括加入的Avicel(如為5重量%水溶液)、
Kelzan(如為1.5重量%水溶液)、Proxel GXL及剩餘部分的水,如在表VII中指示出般,及使用Silverson混合器進行最後均化。該分散相包括氯啶、Aromatic 200、PAPI 27及乙二胺,其係49.55重量%(實施例8)或55.94重量%(實施例9)。
表VII列出用於膠囊懸浮液製備的組分之重量百分比。總配料的大小係100公斤。藉由熔化N-Serve TG及將其加入至該溶劑來製備一均勻的N-Serve TG(Dow AgroSciences,90重量%氯啶)及Aromatic 200(Exxon)溶液。至此,加入可溶於油的單體PAPI 27及一起混合以產生油相。藉由將Kraftsperse 25M、Tergitol 15-S-7、Geropon SDS、Proxel GXL、抗發泡劑100 IND及水混合進一均勻的溶液中來製備水相。
經由轉子/定子均化器槽,以1.25:1.0比例一起計量供給該油相及水相,以產生具有想要的顆粒尺寸(2.5微米)之乳液。繼續此方法直到油相耗盡。在加入胺之前,將該配料冷卻至低於15℃。在攪動下將30重量%胺加入該配料中。在加入黏性組分前,攪拌該反應容器最少2小時。該黏性相由5w/w% A vicel、1.5w/w% Kelzan S、1% Proxel GXL及水組成。若需要的話,加入額外的水以達成標的試驗,然後包裝該配料用於最後使用。
表VII列出使用來製備在範例性組成物中的膠囊懸浮液之組分的重量百分比。總配料的大小係400公斤。藉由熔化N-Serve TG及將其加入至溶劑來製備一均勻的N-Serve TG(Dow AgroSciences,90重量%氯啶)及Aromatic 200(Exxon)溶液。將可溶於油的單體PAPI 27加入至此,及一起混合以產生油相。藉由將Kraftsperse 25M、Tergitol 15-S-7、Geropon SDS、Proxel GXL、抗發泡劑100 IND及水混合進一均勻的溶液中來製備水相。
經由轉子/定子均化器槽,以1.25:1.0比例一起計量供給該油相及水相,以產生一具有想要的顆粒尺寸(2.5微米)之乳液。繼續此方法直到油相耗盡。在加入胺之前,將該配料冷卻至低於15℃。藉由使用側流循環流,以每分鐘100升之速率泵取該乳液,將30重量%胺加入該配料中。在少於10分鐘內加入該胺,較佳為少於5分鐘,以定型該膠囊壁。在加入該黏性組分前,攪拌該反應容器最少2小時。該黏性相由5w/w% A vicel、1.5w/w% Kelzan S、1% Proxel GXL及水組成。若需要的話,加入額外的水以達成標的試驗,然後包裝該配料用於最後使用。
決定在懸浮液中形成微膠囊後將芳香族溶劑加入至該懸浮液的水相之效應
將數部分之本揭示的微膠囊懸浮調配物(~195克懸浮調配物)稱重進250毫升玻璃瓶中。將特定量(以重量百分比為基準)的多種芳香族溶劑直接加入該包含微膠囊懸浮調配物的玻璃瓶。
在線性搖動器上攪拌該等瓶30-45分鐘以製備一均勻的微膠囊懸浮調配物,即,將該後加入的芳香族溶劑
遍及該微膠囊懸浮調配物溶解或分散。一旦達成均勻的調配物,將樣品瓶放置在約0℃或約10℃的冰箱中。在不同時間點處對每個瓶子進行取樣及測試該樣品之存在於水相中的結晶。
在10℃及0℃儲存樣品中進行溼式篩選程序,以決定該結晶形成如為該總微膠囊懸浮調配物的重量百分比。將大約20克的每個各別微膠囊懸浮調配物樣品加入至包含在100至200克的自來水間之玻璃燒杯。使用玻璃攪拌棒攪拌該溶液,然後傾倒通過75微米篩孔篩。以額外的水沖洗燒杯及該沖洗液亦傾倒通過該篩。將自來水傾倒在篩中的樣品上大約30秒以將弱團聚物沖洗通過該過濾器。將遺留在篩網上的殘餘物沖洗到經稱重的濾紙上及真空過濾。允許此濾紙與樣品在真空抽風櫃中乾燥至少四小時,然後再稱重。使用如下的方程式來計算殘餘物百分比:殘餘物百分比(%)=(在乾燥後之濾紙及殘餘物重量(克)-濾紙重量(克))/(經篩選的總樣品(克))。藉由氣相層析法,使用內部標準技術分析從微膠囊懸浮調配物分離出的氯啶結晶用於化學鑑別及純度。
在2週及4週時間區間處,對儲存在10℃及0℃下的每個樣品重覆該方法,及記錄殘餘物重量百分比,如在下列表VIII中列出。顯示在表VIII中的篩選結果顯示出在儲存於10℃及0℃下4週後,Aromatic 200ND(貧萘)明顯減低結晶形成及改良結晶穩定性,如與無加入結晶抑制劑的對照比較。
參照表VIII。如由在水相中缺乏結晶明瞭,在儲存於0℃及10℃下儲存4週後,Aromatic 200ND顯示出最好的結果。環己酮及Hallcomid M-8-10無法和Aromatic 200ND一樣。實際上,表VIII顯示出在儲存於0℃下4週後,相對於不包含將額外的溶劑加入至懸浮液的水相之對照組,在使用推定的結晶抑制劑環己酮及Hallcomid M-8-10所製備之樣品中的氯啶結晶量(以重量百分比為基準)增加。
這些結果驚人地提供知曉環己酮係氯啶之特別
有效的溶劑(在周溫(24℃)下溶解約60重量%氯啶)。亦知曉環己酮在周溫(24℃)下比Aromatic 100溶解更多氯啶,其中Aromatic 100在周溫(24℃)下僅溶解約51重量百分比氯啶。
此外,知曉Hallcomid M-8-10在周溫下溶解約50重量百分比氯啶,在0℃下約40重量百分比,及在-10℃下約35重量百分比。同時,Aromatic 150在周溫下僅溶解約43重量百分比氯啶,在0℃下約25重量百分比及在-10℃下約29重量百分比。
以其對Aromatic 100及150的類似性為基準,就溶解或減低氯啶結晶來說,預計Aromatic 200ND的表現程度與其它芳香族溶劑約相同(即,比環己酮或Hallcomid M-8-10較不成功)。如總整理在表VIII中的結果指示出,Aromatic 200ND經証明係一種意外較好的抑制劑或結晶形成及在此實驗中所測試的其它溶劑。
製備具有在Aromatic 200中包含44.7%、47.1%及49.1%氯啶的油相之微膠囊懸浮調配物。參見表IX,其表列出在每種調配物中的組分。將來自每種調配物的樣品放置在瓶中及將該等瓶子儲存在冰箱中,將該冰箱維持在約10℃。在不同時間點對每個瓶子進行取樣,及使用溼式篩選測試來測試每個樣品之結晶形成存在。
以額外的Aromatic 200在油相微膠囊中所製備之微膠囊調配物(44.7%氯啶在油相中,2%額外的Aromatic 200,與以47.1%氯啶在油相中所製備之調配物比較)在儲存於10℃下6週後產生氯啶結晶。比較上,以47.1%氯啶在油相中及2.00%密封後加入的Aromatic 200所製備之微膠囊調配物顯示出在儲存於10℃下12週後無氯啶結晶形成。
藉由將約2重量%Aromatic 200加入至水相來處理一微膠囊懸浮調配物,其中該懸浮調配物若非相同則類似於可商業購得的調配物InstinctTM(可從Dow AgroSciences獲得),其可與類似於藉由反應表IX的第3或5行之組分所形成而顯示出在水相中包括氯啶結晶的調配物比較。在周溫下攪拌所得的混合物30分鐘至5小時。在混合後,無氯啶結晶存在於該調配物的水相中。這些結果指示出將小部分的Aromatic 200加入至已微膠囊化的氯啶懸浮液諸如InstinctTM之水相可防止在水相中形成氯啶結晶,亦可使用來明顯減低或甚至消除預先形成存在於此懸浮液的水相中之氯啶結晶二者。
雖然已經在圖形及前述描述中詳細地闡明及描述出新穎的技術,其係視為闡明性及不在特徵上限制,要了解的是,已經顯示及描述出者僅有較佳的具體實例及想
要保護在該新穎技術的精神內所達到的全部改變及修改。同樣地,雖然使用特定實施例、理論上的論點、記述及闡明來闡明該新穎技術,這些闡明及伴隨的討論決不應該解釋為技術限制。在此申請案中所參照的全部專利、專利申請案及對教科書、科學專題著作、公告及其類似文獻之參照其全文係以參考之方式併入本文。
Claims (24)
- 一種微膠囊懸浮調配物,其包含:(a)一懸浮相,該懸浮相包括複數個微膠囊,該等微膠囊具有一約1至約10微米之體積粒徑中值,其中該等微膠囊包含:(1)一微膠囊壁,其係藉由在聚合性異氰酸鹽與聚胺間之界面縮聚反應產生,以形成一具有重量百分比係該微膠囊懸浮調配物的總重量之約0.2至約40百分比的聚尿素外殼;及(2)一實質上液體核心,該實質上液體核心係密封在該聚尿素外殼內,其中該實質上液體核心包括不超過全部微膠囊的約60重量百分比之2-氯-6-(三氯甲基)吡啶,及其中在溫度至少15℃下,該實質上液體核心包括不超過1.0重量百分比的固體2-氯-6-(三氯甲基)吡啶;及(b)一水相,其中該水相包括該微膠囊懸浮調配物的總重量之至少約1.0重量百分比的芳香族溶劑。
- 如請求項1之微膠囊懸浮調配物,進一步包括至少一種離子安定劑存在於該水相中。
- 如請求項1之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑係至少一種選自於由下列所組成之群的化合物:輕芳烴、貧萘輕芳烴、重芳烴及貧萘重芳烴。
- 如請求項3之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑係貧萘重C10-13芳烴。
- 如請求項4之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約1重量%至約10重量%間之貧萘重C10-13芳烴。
- 如請求項4之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約2重量%至約5重量%間之貧萘重C10-13芳烴。
- 如請求項4之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約2.5重量%至約3.0重量%間之貧萘重C10-13芳烴。
- 如請求項3之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑係重C10-13芳烴。
- 如請求項8之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約1重量%至約10重量%間之重C10-13芳烴。
- 如請求項8之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約2重量%至約5重量%間之重C10-13芳烴。
- 如請求項8之微膠囊懸浮調配物,其中該存在於水相中的芳香族溶劑包含在約2.5重量%至約3.0重量%間之重C10-13芳烴。
- 如請求項1之微膠囊懸浮調配物,其中該等微膠囊具有一約1至約5微米之體積粒徑中值。
- 如請求項1之微膠囊懸浮調配物,其中該懸浮相a)對水相b)的比例係約1:0.75至約1:100。
- 如請求項1之微膠囊懸浮調配物,其中該懸浮相a)對水相b)的比例係約1:1至約1:7。
- 如請求項1之微膠囊懸浮調配物,其中該懸浮相a)對水相b)的比例係約1:1至約1:4。
- 如請求項1之微膠囊懸浮調配物,其中該聚合性異氰酸鹽係聚伸甲基聚苯基異氰酸鹽。
- 一種肥料組成物,其包含一氮肥料及該如請求項1之微膠囊懸浮調配物。
- 如請求項17之肥料組成物,其中該氮肥料係尿素硝酸銨。
- 一種抑制銨氮在生長媒質中硝化的方法,其步驟包括將如請求項1之微膠囊懸浮調配物施用至一植物生長媒質。
- 如請求項19之方法,其中將該調配物被併入該生長媒質中。
- 如請求項19之方法,其中將該調配物被施用至該生長媒質表面。
- 如請求項19之方法,其中該調配物係與一殺蟲劑組合或相繼地與一殺蟲劑被施用。
- 如請求項19之方法,其中該調配物係與氮肥料被施用。
- 如請求項23之方法,其中該氮肥料係尿素硝酸銨。
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CN102249817B (zh) * | 2011-04-21 | 2013-08-28 | 浙江奥复托化工有限公司 | 一种抑制土壤氮流失的制剂、制备方法及其应用 |
BR102012027933A2 (pt) * | 2011-11-01 | 2015-11-17 | Dow Agrosciences Llc | composições pesticidas estáveis |
CN103044137B (zh) * | 2012-12-26 | 2014-11-12 | 南通联农农药制剂研究开发有限公司 | 一种氮肥稳定剂组合物及其制备方法 |
CN103202298A (zh) * | 2013-03-21 | 2013-07-17 | 江苏三迪化学有限公司 | 一种2-氯-6-三氯甲基吡啶微胶囊悬浮剂的制作方法 |
BR112017013770B1 (pt) * | 2014-12-31 | 2022-05-17 | Dow Agrosciences Llc | Formulação de suspensão de microcápsula, e seu método de fabricação |
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