Mother liquor pretreatment and recycling method in the synthesis of chain glycine ferrous complex

A ferrous glycinate and complex technology, which is applied in the preparation of organic compounds, chemical instruments and methods, and cyanide reaction preparation, can solve the problems of unfavorable product quality, affecting mother liquor circulation, and large nitrogen consumption, and achieve anti-oxidation The process is simple, the product quality is improved, and the effect of less iron filings

Inactive Publication Date: 2017-12-01
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the production process and the mother liquor storage process of intermittent production, there is not only the problem that ferrous iron is easily oxidized by air, but also the problem of accumulation of impurities due to repeated circulation of the mother liquor, which affects the color and quality of the product
[0004] In order to realize the recycling of mother liquor and ensure the color and quality of the product, some are protected by nitrogen gas during the production process and the mother liquor storage process, but a large amount of nitrogen is consumed; some are protected by reducing agents such as reduced iron powder, but reduced iron powder The price of other reducing agents is high, and excessive reduced iron powder also affects the circulation of the mother liquor, which needs to be filtered
In short, no matter it is nitrogen protection or reduced iron powder protection, it is difficult to completely prevent ferrous iron from being oxidized by air during the mother liquor storage and repeated cycle production process. Heavy metal ion impurities, which gradually adversely affect product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Using ferrous sulfate and glycine as the main raw materials, at 60°C-80°C, control the molar ratio of ingredients to about 1:1, stir and mix for 0.5-1h for hydrothermal synthesis. Cool to 25°C, and directly cool and crystallize to obtain the product. The mother liquor obtained by centrifugation is adjusted to a pH of 1.5-3.5 with sulfuric acid, and stored in a storage tank. In the mother liquor stored for 1 day, add 4% by weight of the mother liquor, scrap iron chips from iron ball processing, heat to 50°C-90°C, react and hydrolyze for 5min-1h, and suction filter into a synthesis tank. Control the molar ratio of ingredients to about 1:1, add ferrous sulfate, glycine and other raw materials, stir and mix at 60°C-80°C for 0.5-1h for hydrothermal synthesis. Cool to 25°C, and directly cool and crystallize to obtain the product. The product quality has been tested to meet the GB / T 21996-2008 national standard.

Embodiment 2

[0020] The pH of the mother liquor in Example 1 was adjusted to 1.5-3.5 with sulfuric acid, and stored in a storage tank for 5 days. In the mother liquor stored for 5 days, 2% by weight of the mother liquor is added with waste iron chips from mechanical processing of iron materials, heated to 50°C-90°C, reacted and hydrolyzed for 5min-1h, and suction filtered into a synthesis tank. Control the molar ratio of ingredients to about 1:1, add ferrous sulfate, glycine and other raw materials, stir and mix at 60°C-80°C for 0.5-1h for hydrothermal synthesis. Cool to 25°C, and directly cool and crystallize to obtain the product. The product quality has been tested to meet the GB / T 21996-2008 national standard.

Embodiment 3

[0022] With the mother liquor in the embodiment 2, according to the method of the present invention, the mother liquor is pretreated and recycled 8 times (that is, circulated 10 times in total), and the mother liquor is stored for 12 hours each time. The mother liquor obtained in the tenth production was adjusted to a pH of 1.5-3.5 with sulfuric acid, and stored in a storage tank for 2 days. In the mother liquor that has been circulated 10 times and stored for 2 days, add 3% by weight of the mother liquor, scrap iron scraps in iron ball processing, heat to 50°C-90°C, react and hydrolyze for 5min-1h, and suction filter to Synthesis tank. Control the molar ratio of ingredients to about 1:1, add ferrous sulfate, glycine and other raw materials, stir and mix at 60°C-80°C for 0.5-1h for hydrothermal synthesis. Cool to 25°C, and directly cool and crystallize to obtain the product. The product quality has been tested to meet the GB / T 21996-2008 national standard.

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Abstract

The invention provides a method for pretreatment and recycling of mother liquor in the synthesis of ferrous chain glycine complex, which belongs to the technical field of preparation of third-generation trace element feed additive-ferrous chain glycine complex. The main process of the method of the present invention is as follows: the synthesis mother liquor of ferrous glycosidic acid complex is stored under strong acidity; when the mother liquor is recycled, waste iron filings are used as reducing agent, reacted and hydrolyzed and precipitated under high temperature and strong acidity, and pumped while hot Filter into the reaction tank to realize the pretreatment and recycling of the mother liquor. The advantages and positive effects of the present invention are: there is no need to care about the storage time of the mother liquor and the degree of oxidation, and the low-cost waste iron filings are used instead of the high-cost reduced iron powder as the reducing agent, and the mother liquor can be guaranteed in the synthesis process. The required pH can also flocculate and co-precipitate the impurities accumulated in the circulating mother liquor, improve the product quality, and the operation is simple and convenient.

Description

technical field [0001] The invention belongs to the technical field of preparation of the third-generation trace element feed additive-chain ferrous glycosine complex, and in particular relates to a mother liquor pretreatment and recycling method in the synthesis of the chain ferrous glycinate complex. Background technique [0002] Water-soluble chain glycine ferrous complex is the third-generation trace element iron feed additive that has developed rapidly at home and abroad in recent years. It uses ferrous sulfate and glycine as the main raw materials. It is stirred and mixed at 60°C-80°C with a molar ratio of about 1:1. After hydrothermal synthesis for 0.5-1h, it is cooled to a certain temperature to directly crystallize and precipitate the product. Its production process is simple, the yield is high, and the cost is low. [0003] Since the ferrous glycoside complex is water-soluble, the mother liquor after cooling and crystallization always contains a considerable amoun...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/76C07C227/18
Inventor 余润兰黄逸强杨佳余肇璟曾伟民刘学端
Owner CENT SOUTH UNIV
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