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Preparation method of EDDHA chelated ferric salt

A technology for chelating iron and salt solution is applied in the field of preparation of EDDHA chelated iron salt, and can solve the problems affecting the purity of EDDHA chelated iron salt, large impurities and the like

Active Publication Date: 2021-05-11
HEBEI CHENGXIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no relatively suitable production method to avoid the participation of the phenolic hydroxyl para-H in the reaction.
The current method for preparing EDDHA chelated iron salt still inevitably has a large amount of phenolic hydroxyl para-H to participate in the reaction, and produces a large amount of corresponding impurities, which seriously affects the purity of EDDHA chelated iron salt

Method used

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  • Preparation method of EDDHA chelated ferric salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A preparation method of EDDHA chelated iron salt, the concrete processing steps are:

[0030] Add 564.66g of phenol into a 2000ml four-necked bottle, stir and heat to 40°C, start to drop 71.07g of 50wt% glyoxylic acid and 36g of ethylenediamine at the same time at a constant speed, and the dropping time is 1.5h. After the dropwise addition, 71.07g of 50wt% glyoxylic acid and 75g of 32% lye (sodium hydroxide solution) were added dropwise at a constant speed for 1.5 hours. After the dropwise addition was completed, the temperature was raised to 60° C. and kept for 5 hours to obtain the reaction product. The temperature of the reaction product was lowered to 42° C., 540 g of water was added, and then 67.89 g of toluene was added to extract the reaction product, stirred for 10 min, and separated after standing for 10 min to obtain an aqueous phase. This extraction process was repeated twice (33.95 g of toluene each time), and the aqueous phases obtained by the three extrac...

Embodiment 2

[0034] A preparation method of EDDHA chelated iron salt, the concrete processing steps are:

[0035] Add 847g of phenol into a 2000ml four-neck flask, stir and heat to 50°C, start to drop 88.84g of 50wt% glyoxylic acid and 36g of ethylenediamine at the same time at a constant speed, and the dropping time is 1.5h. After the dropwise addition, 88.84g of 50wt% glyoxylic acid and 76.5g of 32% lye (sodium hydroxide solution) were added dropwise at a constant speed for 1.5 hours. After the dropwise addition was completed, the temperature was raised to 75° C. and kept for 3 hours to obtain the reaction product. The temperature of the reaction product was lowered to 42° C., 540 g of water was added, and 167.72 g of butyl acetate was added to extract the reaction product, stirred for 15 min, left to stand for 15 min, and separated to obtain an aqueous phase. The extraction process was repeated twice more (the amount of butyl acetate was 86.86g), and the aqueous phases obtained by the ...

Embodiment 3

[0039]A preparation method of EDDHA chelated iron salt, the concrete processing steps are:

[0040] Add 1242g of phenol into a 2000ml four-necked bottle, stir and heat to 70°C, and start to dropwise add 106.6g of 50wt% glyoxylic acid and 36g of ethylenediamine simultaneously at a constant speed for 1.5h. After the dropwise addition, 106.6g of 50wt% glyoxylic acid and 78.75g of 32% lye (sodium hydroxide solution) were added dropwise at a constant speed for 1.5 hours. After the dropwise addition was completed, the temperature was raised to 90° C. and kept for 1 hour to obtain the reaction product. The temperature of the reaction product was lowered to 42° C., 540 g of water was added, and 316.5 g of carbon tetrachloride was added to extract the reaction product, stirred for 20 min, and separated after standing for 20 min to obtain an aqueous phase. This extraction process was repeated twice (the amount of carbon tetrachloride each time was 158.25g), and the aqueous phases obtai...

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Abstract

The invention relates to the technical field of chemical synthesis, and particularly discloses a preparation method of EDDHA chelated ferric salt. The preparation method of the EDDHA chelated ferric salt comprises the following process steps of: a, heating phenol to 40-70 DEG C, adding ethylenediamine and glyoxylic acid, and uniformly mixing to obtain an initial mixed material; b, adding glyoxylic acid and an alkaline aqueous solution into the initial mixed material to obtain a reaction raw material mixture; c, heating the reaction raw material mixture to 60-90 DEG C for reaction, and extracting a reaction product by using an extracting solvent to obtain an EDDHA salt solution; d, carrying out chelation reaction on the EDDHA salt solution and inorganic ferric salt to obtain an EDDHA chelated ferric salt solution; and e, carrying out concentration, centrifugal separation and drying treatment on the EDDHA chelated ferric salt solution to obtain the EDDHA chelated ferric salt. According to the preparation method of the EDDHA chelated ferric salt, provided by the invention, the EDDHA chelated ferric salt with high purity and high quality can be obtained.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of EDDHA chelated iron salt. Background technique [0002] Iron is one of the seven trace elements needed for plant growth, and is the main preparation for curing plant leaflets and yellow leaves. The properties of traditionally applied iron-containing inorganic salt fertilizers are unstable, resulting in low use functions and destructive effects on the soil, which is not conducive to green agriculture and sustainable development. Therefore, the agricultural demand for soluble high-purity organic chelated iron fertilizers has become a top priority. [0003] EDDHA chelated iron salt is a high-efficiency, high-quality, super-active chelated iron, which is used as a trace element fertilizer in agriculture and is one of the most effective products for treating plant iron deficiency and yellow leaf disease. But because the production method of EDDHA c...

Claims

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Application Information

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IPC IPC(8): C07C227/18C07C229/76C07C227/10C07C227/40C07C229/36
CPCC07C227/18C07C227/10C07C227/40C07C229/36C07C229/76Y02E60/10
Inventor 程雪莲袁志文李成果李娟张伟渠永娟闫成会
Owner HEBEI CHENGXIN
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