Preparation method of imino-disuccinic acid and salt thereof
A technology of iminodisuccinate and iminodisuccinic acid, which is applied to the preparation of organic compounds, chemical instruments and methods, and the preparation of cyanide reactions. It can solve the problems of high equipment and management requirements, long process reaction time, In order to achieve the effects of less management difficulty, easy control of reaction conditions, and short reaction time
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[0025] The preparation method of iminodisuccinic acid and its salts of the present invention uses butenedioic acid / anhydride and aspartic acid as main raw materials, prefabricates them into reaction raw material liquid A and reaction raw material liquid B respectively, and controls the reaction process reaction liquid It is a critically saturated solution and boils at high temperature. High-concentration materials are more effective than low-concentration materials, and are also more economical. The reaction water consumption is greatly reduced, the reaction process is simplified, and the reaction time is shortened.
[0026] The method of the present invention is described in further detail below with examples.
Embodiment 1
[0028] Add 98kg (1000mol) maleic anhydride and 80kg (2000mol) NaOH into 90kg (5000mol) water and stir fully at room temperature to generate reaction solution A, the reaction time is 0.5h; mix 133kg (1000mol) L-aspartic acid with 80kg Add (2000mol) NaOH to 90kg (5000mol) water and stir fully at room temperature to generate reaction solution B. The reaction time is 0.5h; mix A and B reaction solutions in an internal mixer and react at a temperature of 120°C. Keep the reaction by distillation or adding water The liquid is in a critical saturated state and kept boiling; the reaction time is 4h, and after the reaction is completed, it is lowered to room temperature, and the tetrasodium iminodisuccinate can be obtained by CCDC method detection with a yield of 94.50%; dried at 130°C to obtain white iminodisuccinate Acid tetrasodium salt powder product, its purity does not decrease; add hydrochloric acid to obtain white iminodisuccinic acid precipitate, filter and recrystallize with et...
Embodiment 2
[0031] 116kg (1000mol) maleic acid and 116.6kg (1100mol) Na 2 CO 3 Add 135kg (7500mol) water and stir well at room temperature to generate reaction solution A, the reaction time is 0.5h; mix 139.65kg (1050mol) D-aspartic acid with 116.6kg (1100mol) Na 2 CO 3 Add 135kg (7500mol) of water and stir at room temperature to form a reaction solution B. The reaction time is 0.5h; mix the A and B reaction solutions in a reactor at a temperature of 140°C, and keep the reaction solution in a critically saturated state by distillation or adding water. And keep boiling; the reaction time is 6h, after the reaction is completed, it is cooled to room temperature, and the tetrasodium iminodisuccinate can be obtained by CCDC method with a yield of 96.71%; dried at 120°C to obtain white tetrasodium iminodisuccinate powder Product, its purity does not decrease; add hydrochloric acid to obtain white iminodisuccinic acid precipitate, filter and recrystallize with methanol to obtain high-purity im...
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