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    • 4. 发明申请
    • CONTINUOUS PROCESS FOR THE PREPARATION OF N-(PHOSPHONOMETHYL) IMINODIACETIC ACID
    • N-(磷酸基乙基)亚氨基二乙酸的连续制备方法
    • WO0009520A9
    • 2000-09-28
    • PCT/US9918501
    • 1999-08-12
    • MONSANTO COSTERN MICHAEL KJOHNSON TODD JJORGENSON AMY LROGERS MICHAEL DFRANCZYK THADDEUS S III
    • STERN MICHAEL KJOHNSON TODD JJORGENSON AMY LROGERS MICHAEL DFRANCZYK THADDEUS S III
    • B01J20/26B01J20/34B01J31/20B01J31/40B01J38/00C07B61/00C07C233/47C07D241/08C07F9/38
    • C07D241/08C07C233/47C07F9/3808
    • In the process of the present invention, N-acetyliminodiacetic acid is formed via a continuous amidocarboxymethylation reaction. In this reaction, N-(acetyl)iminodiacetic acid is formed in an amidocarboxymethylation reactor system, into which a source of each of the following is continuously fed: (1) acetamide or an acetamide derivative (2) formaldehyde or a formaldehyde generator or derivative (3) a carbonylation catalyst (4) carbon monoxide and optionally (5) hydrogen. In turn, an amidocarboxymethylation reaction product stream, which contains N-(acetyl)iminodiacetic acid and the carbonylation catalyst, is withdrawn from the amidocarboxymethylation reactor system. The carbonylation catalyst is separated from the amidocarboxymethylation reaction product stream to recover the carbonylation catalyst and form a catalyst depleted product stream which contains N-(acetyl)iminodiacetic acid. The separated carbonylation catalyst is returned to the amidocarboxymethylation reactor system, and the N-(acetyl)iminodiacetic acid in the catalyst depleted product stream is either: (1) reacted with a source of phosphorous and a source of formaldehyde in the presence of an acid to form a phosphonomethylation reaction product stream containing N-(phosphonomethyl)iminodiacetic acid and acetic acid; or (2) deacylated and cyclized to form a 2,5-diketopiperazine, and then reacted with a source of phosphorous and a source of formaldehyde in the presence of an acid to form a phosphonomethylation reaction product stream containing N-(phosphonomethyl)iminodiacetic acid and acetic acid. Either way, the N-(phosphonomethyl)iminodiacetic acid is precipitated from the phosphonomethylation reaction product stream in the presence of acetic acid, and the precipitate is recovered to form a filtrate stream. The filtrate stream is separated into an acetic acid enriched stream and an acetic acid depleted stream. At least a portion of the acetic acid enriched stream is fed to an acetamide synthesis reactor into which ammonia is simultaneously fed to form an acetamide product stream, which is fed (directly or indirectly) back to the amidocarboxymethylation reactor system.
    • 在本发明的方法中,N-乙酰基二乙酸通过连续的酰胺基羧甲基化反应形成。 在该反应中,在酰氨基羧甲基化反应器系统中形成N-(乙酰基)亚氨基二乙酸,连续进料以下每一种来源:(1)乙酰胺或乙酰胺衍生物(2)甲醛或甲醛产生剂或衍生物 (3)羰基化催化剂(4)一氧化碳和任选(5)氢。 接着,将含有N-(乙酰基)亚氨基二乙酸和羰基化催化剂的酰胺基羧甲基化反应产物流从酰胺基羧甲基化反应器系统中排出。 羰基化催化剂与酰氨基羧甲基化反应产物流分离以回收羰基化催化剂并形成含有N-(乙酰基)亚氨基二乙酸的催化剂耗尽产物流。 将分离出的羰基化催化剂返回到酰氨基羧甲基化反应器体系中,并且催化剂去除产物流中的N-(乙酰基)亚氨基二乙酸或者:(1)在酸存在下与磷来源和甲醛来源反应 以形成含有N-(膦酰基甲基)亚氨基二乙酸和乙酸的膦酰甲基化反应产物流; 或(2)脱酰并环化形成2,5-二酮哌嗪,然后在酸存在下与磷源和甲醛源反应,形成含N-(膦酰基甲基)亚氨基二乙酸的膦酰甲基化反应产物流 和乙酸。 不管怎样,在乙酸存在下N-膦酰基甲基化亚氨基二乙酸从膦酰基甲基化反应产物流中沉淀出来,沉淀物被回收形成滤液流。 将滤液流分离成富含乙酸的物流和贫含乙酸的物流。 将至少一部分富含乙酸的物流进料到乙酰胺合成反应器中,其中氨同时进料到乙酰胺合成反应器中以形成乙酰胺产物物流,将其(直接或间接)进料到酰胺基羧甲基化反应器体系中。