Clean production process for amino acids such as iminodiacetic acid

A technology of iminodiacetic acid and calcium iminodiacetate is applied in the fields of chemical fertilizers, fine chemicals, and pesticides, and can solve the problems of complicated refining process, poor salt quality, and many times of solid-liquid separation, so as to simplify process steps and reduce production. cost and the effect of cleaner production

Active Publication Date: 2016-10-05
BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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  • Application Information

AI Technical Summary

Problems solved by technology

This method has the problems of loss of alkali hydrolysis yield and easy production of colored substances. The yield of diacid is only about 90%. A large amount of diacid wastewater containing salt is concentrated and desalinated, and the method of regeneration of evaporative condensate is used. The energy consumption is high, and the salt Poor quality, difficult to use
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  • Clean production process for amino acids such as iminodiacetic acid
  • Clean production process for amino acids such as iminodiacetic acid
  • Clean production process for amino acids such as iminodiacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1 Preparation of calcium iminodiacetate by hydrolyzing iminodiacetonitrile with milk of lime

[0040] Lime (31.4 g, 98%, 0.55 mol) was added to water (200 g), and stirred for 15 min. Keep the temperature of the solution at about 50°C, add iminodiacetonitrile (50 g, 95%, 0.5 mol) in portions, and complete the addition in about half an hour. Stir at 50-55°C for 0.5-1 h, raise the temperature to about 90-100°C, deamination under reduced pressure, and replenish water in due time. When the pH of the evaporated water vapor is 8-9, stop the deamination. The solution was filtered and washed.

[0041] The crude product of calcium iminodiacetic acid (113 g, containing iminodiacetic acid: 58 g, 1 No other impurities were found on H-NMR), the filtrate was combined with washing liquid (containing iminodiacetic acid: 5.2 g), and the total yield of iminodiacetic acid calcium was 95.0%.

Embodiment 2

[0042] Example 2 Calcium iminodiacetate prepared by hydrolyzing iminodiacetonitrile with lime milk, mother liquor applied mechanically

[0043] Put lime (31.4 g, 98%, 0.55 mol) into water (60 g), stir and react for 15 min, and then add the mother liquor from the previous batch of calcium salt separation. Keep the temperature of the solution at about 50°C, add iminodiacetonitrile (50 g, 95%, 0.5 mol) in portions, and complete the addition in about half an hour. Stir at 50-55°C for 0.5-1 h, raise the temperature to about 90-100°C, deamination under reduced pressure, and replenish water in due time. When the pH of the evaporated water vapor is 8-9, stop the deamination. The calcium iminodiacetic acid was filtered out, washed, washed with water and combined with mother liquor for the next batch of reactions.

[0044] The experimental results are as follows, the total yield of iminodiacetic acid in the crude product of 7 batches of reaction iminodiacetic acid calcium is 93.10...

Embodiment 3

[0046] Example 3 Patent (publication number: CN101619077A ) method to prepare iminodiacetic acid calcium

[0047] Add 872 mL of water to the reactor, evacuate to 0.1 Mpa, raise the temperature to 45-50°C, add lime (70%, 143 g) and iminodiacetonitrile (95%, 151 g) into the water several times evenly, each Add once every 5 minutes, finish adding in 3 hours, keep warm for 1 hour, then raise the temperature to 75°C, keep warm for 2 hours, then raise the temperature to 100°C, keep warm for reaction, stop the reaction when the pH of the water vapor is 7, cool, filter, The filtrate and filter cake were collected separately.

[0048] The crude product of calcium iminodiacetic acid (117 g, containing iminodiacetic acid: 58.8 g, impurities: nitrilotriacetic acid: 3.8 g, glycine: 0.1 g) was obtained in the experiment, and the filtrate was combined with washing liquid (containing iminodiacetic acid: 3.53 g ), the total yield of iminodiacetic acid was 93.8%.

[0049] Compared wi...

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Abstract

The invention relates to a clean production method for amino acids such as iminodiacetic acid. The method comprises the steps: carrying out alkaline hydrolysis on amino-nitrile by adopting cheap lime cream, and carrying out deamination, so as to obtain an iminodiacetic acid calcium salt crude product; suspending the obtained iminodiacetic acid calcium salt crude product into water or mother liquor, adding sulfuric acid or other inorganic acid into the water or mother liquor for acidification, and filtering out an inorganic calcium salt filter cake with low water solubility; and subjecting the filter liquor to cooling and crystallization, carrying out separation so as to obtain iminodiacetic acid solids, and applying the crystallization mother liquor to an acidification reaction of next batch mechanically. During the acidification by the sulfuric acid, gypsum can be converted into calcium carbonate and ammonium sulfate by further using a byproduct, i.e., ammonia water of an alkaline hydrolysis process and carbon dioxide in flue gas, so as to directly generate compound fertilizers; the calcium carbonate can also be separated, and ammonium sulfate crystals can also be concentrated; and the calcium carbonate can be sold as a byproduct or be subjected to heated decomposition so as to obtain a quicklime raw material which can be applied mechanically. According to the novel process, the complete utilization of resources can be realized, the reaction selectivity is higher, the production of colored byproducts is reduced, and a concentrating process for removing waste salts such as sodium sulfate and sodium chloride and a wastewater treatment link are avoided; and due to concentration, the use level of a decolorant can be greatly lowered, the energy saving and consumption lowering effects are remarkable, and the production cost is reduced remarkably.

Description

technical field [0001] The invention relates to a clean production process for amino acids such as iminodiacetic acid, and belongs to the technical fields of pesticides, fertilizers and fine chemicals. Background technique [0002] Iminodiacetic acid, CAS No. 142-73-4, alias iminodiacetic acid, N-(carboxymethyl) glycine, aminodiacetic acid, referred to as IDA. Iminodiacetic acid is mainly used as an intermediate in the synthesis of glyphosate and other pesticides, and can also be used as a phosphorus-releasing organic double-effect fertilizer, a raw material for ion exchange resins, rubber, electroplating, and food additives. [0003] Iminodiacetic acid has the following synthetic routes: [0004] 1. Chloroacetic acid method Chloroacetic acid reacts with ammonia water or sodium hydroxide to produce sodium chloroacetate, then reacts with hydrazine hydrate to form hydrazinodiacetic acid, and then acidifies with hydrochloric acid under the action of sodium nitrite to form imin...

Claims

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Application Information

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IPC IPC(8): C07C229/16C07C227/26
Inventor 尹应武李宇航杨少梅孙响响韩田田孙瑞崔建斌师雪琴张海双
Owner BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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