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A kind of preparation method of iminodisuccinic acid and salt thereof

A technology of iminodisuccinate and iminodisuccinic acid is applied in the preparation of organic compounds, cyanide reaction preparation, chemical instruments and methods, etc. In order to achieve the effect of less management difficulty, easy control of reaction conditions, and short reaction time

Active Publication Date: 2019-04-02
SHIJIAZHUANG TIEDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The synthesis and preparation method of IDS is mainly prepared by closed high-pressure reaction of maleic anhydride and ammonia water under alkaline conditions. The disadvantages are: the yield of the product iminodisuccinate is less than 80%, there is ammonia gas residue in the reaction process, and It requires high temperature and high pressure operation, high potential safety hazards, high requirements for equipment and management, large investment and high energy consumption
[0004] There is another preparation method of iminodisuccinate chelating agent reported in the literature, adopting raw material is maleic anhydride / salt or derivative thereof and aspartic acid / salt or derivative thereof in the presence of alkali metal hydroxide The reaction preparation realizes the reaction under normal pressure, and provides a relatively simple method for the industrial preparation of iminodisuccinate, but there are still the following disadvantages: the reaction time of the process is relatively long, which is 6h~30h, and the yield is relatively low. The low is 70%~85%, and because 15~30% of the raw materials are unreacted or side-reacted, it is easy to form salt and precipitate under alkaline conditions, and because iminodisuccinate and reaction raw materials or by-products The cost of separation is high, so it is generally provided to users in the form of a mixture generated by the final reaction. The higher the residual rate of raw materials or the more by-products, the effect in practical applications will be reduced, such as weakened chelation effect, unreacted Precipitation of raw materials or by-products, etc.

Method used

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Examples

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preparation example Construction

[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) of water and stir fully at room temperature to generate reaction solution A, the reaction time is 0.5h; 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 iminodisuccinic acid white crystals, its purity is >99.5% detec...

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Abstract

The invention relates to the technical field of preparation of organic compounds, in particular to the technical field of preparation of a metal chelating agent, and specifically discloses a preparation method of iminodisuccinic acid and its salts: the basic raw material solution containing butenedioic acid A is mixed and reacted with the alkaline raw material solution B containing aspartic acid radicals, the reaction solution is in a critical saturated state and kept boiling, and the reaction is completed to obtain iminodisuccinate. Continue to add inorganic acid to the product to obtain iminodisuccinic acid precipitate, filter and recrystallize to obtain iminodisuccinic acid white crystals. The method of the invention has the advantages of short reaction time, high reaction yield, low energy consumption and low cost, and the obtained product has high purity and good performance, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to the technical field of preparation of organic compounds, in particular to the technical field of preparation of a metal chelating agent. Background technique [0002] Iminodisuccinic acid and its salts (chemical abbreviation: IDS or IDHA) is a new type of green chelating agent, which has a strong ability to chelate metal ions. Compared with traditional polycarboxylic acid chelating agents (such as EDTA ), also has excellent degradability, is environmentally friendly, and can solve the problem of environmental pollution that is difficult to degrade when heavy metal ions are combined with traditional chelating agents. It can be widely used in many fields such as petrochemical industry, textile industry, and heavy metal extraction. [0003] The synthesis and preparation method of IDS is mainly prepared by closed high-pressure reaction of maleic anhydride and ammonia water under alkaline conditions. The disadvantages are: the yield...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/24C07C227/18C07C227/40
CPCC07C227/18C07C227/40C07C229/24Y02P20/54
Inventor 杨晋辉陈艳雪彭玲徐亢亢唐康康陈秉翼王紫璇
Owner SHIJIAZHUANG TIEDAO UNIV