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1. 发明授权

US5614468A Preparation of ammonium glyphosate using aqueous ammonium hydroxide in a liquid-solid reaction system 失效
标题翻译：在液 - 固反应体系中使用氢氧化铵水溶液制备草甘膦铵
公开(公告)号：US5614468A
公开(公告)日：1997-03-25
申请号：US472152
申请日：1995-06-07
申请人： Richard M. Kramer , Thomas M. Day , Ralph E. Lindemann, Jr. , Jane L. Gillespie
发明人： Richard M. Kramer , Thomas M. Day , Ralph E. Lindemann, Jr. , Jane L. Gillespie
IPC分类号： A01N57/20 , C07F9/38 , A01N57/02
CPC分类号： C07F9/3813
摘要： Solid N-phosphonomethylglycine or glyphosate acid is charged to a substantially closed system and then partially pre-dried as by continuously recirculating it through a hot air grinding/drying system. A cooled solution of ammonium hydroxide is then metered into and reacted with the partially dried glyphosate acid as it is being recirculated in a manner such that the moisture content of the reaction mass so formed is continuously decreased throughout the reaction. Following completion of the ammonium hydroxide addition, a powdered reaction mass/product having a moisture content of about 2 wt. % is formed. Significantly, at this stage, the ammonium glyphosate product is suitable for end use and it can be readily dissolved in water and immediately used as a herbicide or plant growth regulator. More importantly, however, this product is capable due to its highly sorptive character to be further formulated into a product exceptionally highly loaded with adjuvants and particularly surfactants.
摘要翻译：将固体N-膦酰基甲基甘氨酸或草甘膦酸加入到基本封闭的系统中，然后通过连续循环通过热空气研磨/干燥系统部分预干燥。然后将冷却的氢氧化铵溶液计量加入部分干燥的草甘膦酸中并与之反应，因为它被再循环，使得如此形成的反应物质的水分含量在整个反应中连续降低。完成氢氧化铵加入后，将水分含量为约2重量％的粉末状反应物质/产物％形成了。显着地，在此阶段，草甘膦铵产品适用于最终用途，并且可以容易地溶于水中并立即用作除草剂或植物生长调节剂。然而，更重要的是，该产品由于其高吸附特性而能够进一步配制成特别高负载佐剂，特别是表面活性剂的产品。

2. 发明授权

US5716903A Preparation of ammonium glyphosate using aqueous ammonium hydroxide in a liquid-solid reaction system 失效
标题翻译：在液 - 固反应体系中使用氢氧化铵水溶液制备草甘膦铵
公开(公告)号：US5716903A
公开(公告)日：1998-02-10
申请号：US778890
申请日：1997-01-03
申请人： Richard M. Kramer , Thomas M. Day , Ralph E. Lindemann, Jr. , Jane L. Gillespie
发明人： Richard M. Kramer , Thomas M. Day , Ralph E. Lindemann, Jr. , Jane L. Gillespie
IPC分类号： A01N57/20 , C07F9/38 , A01N57/02
CPC分类号： C07F9/3813
摘要： Solid N-phosphonomethylglycine or glyphosate acid is charged to a substantially closed system and then partially pre-dried as by continuously recirculating it through a hot air grinding/drying system. A cooled solution of ammonium hydroxide is then metered into and reacted with the partially dried glyphosate acid as it is being recirculated in a manner such that the moisture content of the reaction mass so formed is continuously decreased throughout the reaction. Following completion of the ammonium hydroxide addition, a powdered reaction mass/product having a moisture content of about 2 wt. % is formed. Significantly, at this stage, the ammonium glyphosate product is suitable for end use and it can be readily dissolved in water and immediately used as a herbicide or plant growth regulator. More importantly, however, this product is capable due to its highly sorptive character to be further formulated into a product exceptionally highly loaded with adjuvants and particularly surfactants.
摘要翻译：将固体N-膦酰基甲基甘氨酸或草甘膦酸加入到基本封闭的系统中，然后通过连续循环通过热空气研磨/干燥系统部分预干燥。然后将冷却的氢氧化铵溶液计量加入部分干燥的草甘膦酸中并与其反应，因为它被再循环，使得如此形成的反应物质的水分含量在整个反应中连续降低。完成氢氧化铵加入后，将水分含量为约2重量％的粉末状反应物质/产物％形成了。显着地，在此阶段，草甘膦铵产品适用于最终用途，并且可以容易地溶于水中并立即用作除草剂或植物生长调节剂。然而，更重要的是，该产品由于其高吸附特性而能够进一步配制成特别高负载佐剂，特别是表面活性剂的产品。

3. 发明授权

US5633397A Preparation of ammonium glyphosate via a gas-solid reaction system 失效
标题翻译：通过气 - 固反应体系制备草甘膦铵
公开(公告)号：US5633397A
公开(公告)日：1997-05-27
申请号：US485316
申请日：1995-06-07
申请人： Jane L. Gillespie , Thomas M. Day , Richard M. Kramer
发明人： Jane L. Gillespie , Thomas M. Day , Richard M. Kramer
IPC分类号： A01N57/20 , C07F9/38 , C07F9/54
CPC分类号： A01N57/20 , C07F9/3813
摘要： Solid N-phosphonomethylglycine or glyphosate acid in "wet cake" form is charged to a suitable mixer/reactor. A stoichiometric equivalent of anhydrous ammonia gas is fed to the mixer for direct reaction with the glyphosate acid as it is agitated within the mixer. A water Jacket containing circulating water or other suitable heat transfer facilitating means readily known to those in the art is adapted to the mixer and used to remove heat from the reactor produced by the exothermic reaction. The moisture content of the glyphosate wet cake, the design of the mixer including a preferred close tolerance relation between the inner walls of the reactor and its mixing impellers together with the relative location of the ammonia gas inlet in the mixer/reactor and maintenance of a reaction temperature of about 60.degree. C. or below are all important process variables. The ammonium glyphosate thereby produced is a highly sorptive, water-soluble powder suitable for end use as a plant growth regulator or as a herbicide without further processing. Due to the highly sorptive character of the reaction product, however, it is particularly well-suited for further formulation to absorb/adsorb an exceptionally high level of adjuvants such as wetting agents, anti-foaming agents and, in particular, surfactants.
摘要翻译：以“湿饼”形式的固体N-膦酰基甲基甘氨酸或草甘膦酸加入合适的混合器/反应器中。将化学计量当量的无水氨气加入到混合器中，以便在混合器内搅拌时与草甘膦酸直接反应。含有本领域技术人员熟知的循环水或其它合适的传热促进装置的水夹克适用于混合器并用于从放热反应产生的反应器中除去热量。草甘膦湿滤饼的水分含量，混合器的设计包括反应器内壁与其混合叶轮之间的优选紧密公差关系以及氨气入口在混合器/反应器中的相对位置以及维持约60℃以下的反应温度都是重要的工艺变量。由此产生的草甘膦是一种高度吸附的水溶性粉末，适用于最终用作植物生长调节剂或作为除草剂而不进一步加工。然而，由于反应产物的高度吸附特性，特别适用于进一步配制以吸收/吸附特别高含量的助剂如润湿剂，消泡剂，特别是表面活性剂。

4. 发明授权

US06245713B1 Plant treatment compositions having enhanced biological effectiveness 有权
公开(公告)号：US06245713B1
公开(公告)日：2001-06-12
申请号：US09298136
申请日：1999-04-23
申请人： Ronald J. Brinker , Andrew D. Dyszlewski , Jane L. Gillespie , Claude R. Jones , Richard M. Kramer , Norman R. Pallas , Rodney O. Radke , Anthony J. I. Ward , Xiaodong C. Xu
发明人： Ronald J. Brinker , Andrew D. Dyszlewski , Jane L. Gillespie , Claude R. Jones , Richard M. Kramer , Norman R. Pallas , Rodney O. Radke , Anthony J. I. Ward , Xiaodong C. Xu
IPC分类号： A01N2530
CPC分类号： A01N47/24 , A01N25/28 , A01N25/30 , A01N33/22 , A01N35/06 , A01N37/22 , A01N37/40 , A01N39/04 , A01N43/40 , A01N43/50 , A01N47/36 , A01N57/20 , A01N2300/00
摘要： A composition for application to foliage of a plant to elicit a biological effect is provided. This plant treatment composition comprises, dissolved or dispersed in water, an anionic exogenous chemical substance such as the herbicide N-phosphonomethylglycine, together with (i) one or more alkylether surfactants each having the formula R12—O—(CH2CH2O)n((CHR)2O)m—R13 wherein R12 is an aliphatic saturated or unsaturated hydrocarbyl group having about 16 to about 22 carbon atoms, n is an average number of about 5 to about 100, m is an average number of 0 to about 5, one R in each —((CHR)2O)— group is hydrogen and the other R is methyl, and R13 is a hydrogen, C1-4 alkyl or C2-4 acyl group; and (ii) one or more amine surfactants each having a molecular structure that comprises (a) a hydrophobic moiety having one or a plurality of independently saturated or unsaturated, branched or unbranched, aliphatic, alicyclic or aromatic C3-20 hydrocarbyl or hydrocarbylene groups joined together by 0 to about 7 ether linkages and having in total about 8 to about 24 carbon atoms, and (b) a hydrophilic moiety comprising an amino group that is cationic or that can be protonated to become cationic, having attached directly thereto 1 to 3 oxyethylene groups or polyoxyethylene chains, these oxyethylene groups and polyoxyethylene chains comprising on average 1 to about 50 oxyethylene units per surfactant molecule, the hydrophobic moiety being attached either to the amino group or via an ether linkage to an oxyethylene unit. The weight ratio of the alkylether surfactant(s) to the amine surfactant(s) is about 1:10 to about 10:1; and the alkylether and amine surfactants are present in total in an adjuvant amount of about 0.05 to about 0.5 parts by weight per part by weight of the anionic exogenous chemical substance, expressed as acid equivalent. Also provided are solid and liquid concentrate compositions that can be diluted, dissolved or dispersed in water to form such a plant treatment composition.

5. 发明授权

US06605568B1 Process for making a downstream processable ammonium glyphosate paste 有权
标题翻译：制备下游可加工的草甘膦浆料的方法
公开(公告)号：US06605568B1
公开(公告)日：2003-08-12
申请号：US09627078
申请日：2000-07-27
申请人： Brent D. Massmann , Richard M. Kramer , John T. Wang , Marc Emile Toussaint
发明人： Brent D. Massmann , Richard M. Kramer , John T. Wang , Marc Emile Toussaint
IPC分类号： A01N5702
CPC分类号： A01N57/20 , A01N25/14 , A01N25/04 , A01N2300/00
摘要： A process is provided for preparing a downstream processable ammonium glyphosate paste, comprising mixing in a suitable vessel (i) particulate glyphosate acid, (ii) ammonia in an amount of about 0.8 to about 1.25 moles per mole of the glyphosate acid, and (iii) water in an amount of about 10% to about 25% by weight of all materials being mixed in the vessel, thereby causing a reaction of the glyphosate acid and ammonia that generates heat causing partial evaporation of the water, and forms an ammonium glyphosate paste having a moisture content of about 5% to about 20% by weight. A process is also provided for preparing a dry granular herbicidal composition, comprising (a) forming an ammonium glyphosate paste as described above and thereafter, if the moisture content of the paste is greater than about 15% by weight, applying heat and/or vacuum to reduce the moisture content to about 5% to about 15% by weight; (b) thereafter adding to the paste, with mixing, one or more surfactants in a weight ratio of total surfactant to ammonium glyphosate of about 1:9 to about 1:3 to form an extrudable wet mix; (c) extruding the wet mix to form extrudate strands that break to form moist coherent granules; and (d) drying the granules to produce the dry granular composition.
摘要翻译：提供了一种制备可下游可加工的草甘膦草浆的方法，包括在合适的容器中混合（i）草甘膦颗粒酸，（ii）每摩尔草甘膦酸约0.8至约1.25摩尔的氨和（iii ）水的量为所有材料在容器中混合的约10％至约25％重量，从而导致产生热量的草甘膦酸和氨的反应，导致水的部分蒸发，并形成草甘膦铵水分含量为约5％至约20％重量。还提供了制备干燥颗粒除草组合物的方法，其包括（a）如上所述形成草甘膦铵盐，此后如果糊剂的水分含量大于约15重量％，施加热和/或真空以将水分含量降低至约5重量％至约15重量％; （b）此后，通过混合将一种或多种表面活性剂与草甘膦铵的重量比为约1:9至约1:3的一种或多种表面活性剂加入到糊中以形成可挤出的湿混合物; （c）挤出湿混合物以形成破裂以形成潮湿的粘结颗粒的挤出物链; 和（d）干燥颗粒以产生干燥颗粒组合物。

6. 发明授权

US06448434B1 Process for making ammonium glyphosate powder 有权
标题翻译：制备草甘膦铵粉的方法
公开(公告)号：US06448434B1
公开(公告)日：2002-09-10
申请号：US09624949
申请日：2000-07-25
申请人： Richard M. Kramer
发明人： Richard M. Kramer
IPC分类号： C07F938
CPC分类号： C07F9/3813 , A01N57/20 , A01N25/14 , A01N2300/00
摘要： A process is provided for preparing ammonium glyphosate powder suitable for downstream processing by extrusion to make a granular formulation comprising ammonium glyphosate and surfactant. The process comprises (a) mixing (i) solid particulate glyphosate acid, (ii) water in an amount of about 0.5 to about 3 parts by weight per part by weight of glyphosate acid, and (iii) a base that supplies ammonium cations, in an amount of about 0.8 to about 1.25 mole equivalents of ammonia per mole of glyphosate acid, to form an aqueous reaction medium; (b) allowing the glyphosate acid to react with the base in the reaction medium to form a reaction product comprising a concentrated aqueous solution of ammonium glyphosate; (c) drying the reaction product, for example with a drum dryer, to recover a particulate solid; and (d) accelerating the particulate solid in a turbulent high-velocity gas stream, for example in a jet mill, to form by particle-particle attrition an ammonium glyphosate powder having a mean particle size of about 5 to about 20 &mgr;m.
摘要翻译：提供了一种通过挤出制备适于下游加工的草甘膦铵粉末以制备包含草甘膦和表面活性剂的颗粒制剂的方法。该方法包括（i）混合（i）固体颗粒草甘膦酸，（ii）约0.5至约3重量份的量的草甘膦酸，和（iii）提供铵阳离子的碱，其量为每摩尔草甘膦酸约0.8至约1.25摩尔当量的氨，以形成水性反应介质; （b）使草甘膦酸与反应介质中的碱反应形成包含浓缩的草甘膦铵水溶液的反应产物; （c）干燥反应产物，例如用滚筒式干燥器回收颗粒状固体; 和（d）加速湍流高速气流中的颗粒状固体，例如在喷射式研磨机中，通过粒子颗粒磨损形成平均粒度约5至约20微米的草甘膦粉末。

7. 发明授权

US07008904B2 Herbicidal compositions containing glyphosate and bipyridilium 有权
标题翻译：含有草甘膦和联吡啶的除草组合物
公开(公告)号：US07008904B2
公开(公告)日：2006-03-07
申请号：US10204094
申请日：2001-02-13
申请人： Ron P. Crockett , Andrew Dyszlewski , Richard M. Kramer , Domingo C. Riego , Joseph J. Sandbrink , Donald L. Suttner , Dennis H. Williamson , Daniel R. Wright
发明人： Ron P. Crockett , Andrew Dyszlewski , Richard M. Kramer , Domingo C. Riego , Joseph J. Sandbrink , Donald L. Suttner , Dennis H. Williamson , Daniel R. Wright
IPC分类号： A01N43/40 , A01N43/90 , A01N57/02
CPC分类号： A01N57/20 , A01N43/90 , A01N43/40 , A01N25/30 , A01N2300/00
摘要： Herbicidal compositions are provided which cause rapid symptomology while delivering long term control of regrowth of plants. The herbicidal compositions comprise N-phosphonomethylglycine or a herbicidal derivative thereof, a bipyridilium or a herbicidal derivative thereof, and at least one surfactant. A herbicidal spray composition is preparable from a particulate solid concentrate or a liquid concentrate. Also provided is a method for killing or controlling the growth of plants comprising the step of contacting the foliage of said plants with an aqueous herbicidal composition of the invention.
摘要翻译：提供除草剂组合物，其引起快速症状，同时长期控制植物的再生长。除草组合物包含N-膦酰甲基甘氨酸或其除草衍生物，联吡啶或其除草衍生物和至少一种表面活性剂。可以从颗粒状固体浓缩物或液体浓缩物制备除草喷雾组合物。还提供了杀死或控制植物生长的方法，包括使所述植物的叶与本发明的水性除草组合物接触的步骤。

8. 发明授权

US06599858B1 Process for making ammonium glyphosate flakes 失效
标题翻译：制备草甘膦片的方法
公开(公告)号：US06599858B1
公开(公告)日：2003-07-29
申请号：US09703077
申请日：2000-07-25
申请人： Richard M. Kramer
发明人： Richard M. Kramer
IPC分类号： A01N5718
CPC分类号： A01N57/20 , A01N25/34 , A01N25/14 , A01N25/16 , A01N2300/00
摘要： A process is provided for preparing ammonium glyphosate flakes, comprising (a) mixing (i) solid particulate glyphosate acid, (ii) water in an amount of about 0.5 to about 3 parts by weight per part by weight of glyphosate acid, and (iii) a base that supplies ammonium cations, in an amount of about 0.8 to about 1.25 mole equivalents of ammonia per mole of glyphosate acid, to form an aqueous reaction medium; (b) allowing the glyphosate acid to react with the base in the reaction medium to form a reaction product comprising a concentrated aqueous solution of ammonium glyphosate; (c) drying the reaction product by contact thereof with a heated surface to form, primarily by evaporation of water, a solid deposit on the heated surface; and (d) scraping the solid deposit off the heated surface to recover dry flakes of ammonium glyphosate.
摘要翻译：提供用于制备草甘膦铵片的方法，其包括（i）混合（i）固体颗粒草甘膦酸，（ii）约0.5至约3重量份的草甘膦酸重量的水和（iii ）提供铵阳离子的碱，其量为每摩尔草甘膦酸约0.8至约1.25摩尔当量的氨，以形成水性反应介质; （b）使草甘膦酸与反应介质中的碱反应形成包含浓缩的草甘膦铵水溶液的反应产物; （c）通过与加热表面的接触来干燥反应产物，主要通过蒸发水以在加热的表面上形成固体沉积物; 和（d）将固体沉积物刮掉加热的表面以回收草甘膦的干燥薄片。

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