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    • 1. 发明授权
    • Process for the production of aminoguanidine bicarbonate
    • 生产氨基胍二碳酸酯的方法
    • US3673253A
    • 1972-06-27
    • US3673253D
    • 1968-02-21
    • BAYER AG
    • SIMONS PETER
    • C07C281/16C07C133/10
    • C07C281/16
    • Production of aminoguanidine bicarbonate by reacting finely divided solid calcium cyanamide with hydrazine, in the form of mono or dihydrazine sulfate or hydrazine hydrate and sulfuric acid in admixture, in neutral to alkaline aqueous medium, e.g. at pH 7 to about 9.5 and about 15*-90* C, using sulfuric acid for pH adjustment to form aminoguanidine, cooling the reaction mixture, e.g. to about 60*-40* C, to precipitate the resultant calcium sulfate sludge, and treating the sludge-free resultant reaction mixture, e.g. at 25*-50* C, with a bicarbonate precipitating agent, e.g. alkali metal or ammonium bicarbonate or carbon dioxide and alkali metal or ammonium hydroxide, to precipitate the aminoguanidine bicarbonate therefrom; OPTIONALLY AVOIDING IRON CONTAMINATION OF THE DESIRED PRODUCT BY EITHER ADJUSTING TO ACID PH, e.g. pH 3-4, the reaction mixture prior to bicarbonate agent treatment to maintain such iron in soluble form, e.g. when Fe content low, or adjusting to about pH 7.5-8.5 the reaction mixture prior to bicarbonate agent treatment followed by air introduction, e.g. at 60*-45* C, to remove the iron content, e.g. when Fe content high-up to about 5 percent, as ferric hydroxide precipitate, the latter alternative being optionally carried out prior to calcium sulfate sludge precipitation (i.e. removal) to effect joint precipitation of such ferric hydroxide and sludge prior to bicarbonate treatment.
    • 在中性至碱性水性介质例如中性至碱性水性介质中,使细分散的固体氰氨腈与肼反应生成氨基胍碳酸氢盐,其形式为硫酸单或二肼硫酸盐或水合肼和硫酸。 在pH7至约9.5和约15-90℃下,使用硫酸进行pH调节以形成氨基胍,冷却反应混合物,例如 至约60°-40℃,以沉淀所得的硫酸钙污泥,并处理无污泥的所得反应混合物,例如 在25℃-50℃下,用碳酸氢盐沉淀剂, 碱金属或碳酸氢铵或二氧化碳和碱金属或氢氧化铵,以从其中沉淀氨基胍碳酸氢盐; 通过调节酸性pH可以避免所有产品的铁污染,例如 pH 3-4,在碳酸氢钠试剂处理之前的反应混合物保持这种可溶形式的铁,例如 当Fe含量低时,或者在碳酸氢盐处理之前,随后空气引入,例如,将反应混合物调节至约pH 7.5-8.5。 在60°-45℃下,除去铁含量,例如 当Fe含量高达约5%时,随着氢氧化铁沉淀,后一种替代方案任选在硫酸钙污泥沉淀(即除去)之前进行,以在碳酸氢盐处理之前进行这种氢氧化铁和污泥的联合沉淀。