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Production process for synthetizing EDDHA (Ethylenediamine-N,N'-bis(2-hydroxyphenylacetic acid) ferric-sodium complex) Ferrochel with one-step method

A production process, chelated iron technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of unfavorable environmental protection, high production cost, long process, etc., and achieve low production cost and no pollution Effect of energy consumption and low energy consumption

Inactive Publication Date: 2013-09-25
SICHUAN TONGFENG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process method not only has a long flow process and low yield, but also requires a large amount of organic solvent carbon tetrachloride (carcinogenic risk), high production cost, and unfavorable environmental protection

Method used

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  • Production process for synthetizing EDDHA (Ethylenediamine-N,N'-bis(2-hydroxyphenylacetic acid) ferric-sodium complex) Ferrochel with one-step method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1) Raw material ratio (molar ratio)

[0017] Phenol 1.0

[0018] Ethylenediamine 0.4

[0019] Sodium hydroxide 3.0

[0020] Glyoxylic acid 0.8

[0021] Iron ion (ferrous sulfate) 0.5

[0022] water 20

[0023] 2) Dissolve phenol with 10 moles of water, add ethylenediamine and sodium hydroxide solution dropwise to the phenol solution at a temperature of 100°C, mix well, then add glyoxylic acid dropwise, and react at this temperature for 2 hours, Get EDDHA aqueous solution, wherein the weight percent concentration of sodium hydroxide aqueous solution is 40%;

[0024] 3) Dissolve the iron salt in the remaining 10 moles of water, and when the temperature of the EDDHA aqueous solution in step 2) is lowered to 40°C, add the iron salt aqueous solution, adjust the pH to 7.0, stir and react for 15 minutes, and obtain the EDDHA chelated iron solution, which is dried Obtain 233g of EDDHA chelated iron of the present invention, yield 91%.

Embodiment 2

[0026] 1) Raw material ratio (molar ratio)

[0027] Phenol 1.0

[0028] Ethylenediamine 0.5

[0029] Sodium hydroxide 4.0

[0030] Glyoxylic acid 1.0

[0031] Iron ion (ferric chloride) 0.5

[0032] water 20

[0033] 2) Dissolve phenol with 10 moles of water, add ethylenediamine and sodium hydroxide solution dropwise to the phenol solution at 50°C, mix well, then add glyoxylic acid dropwise, and react at this temperature for 3 hours, Get EDDHA aqueous solution, wherein the weight percent concentration of sodium hydroxide aqueous solution is 40%;

[0034] 3) Dissolve the iron salt in the remaining 10 moles of water, and when the temperature of the EDDHA aqueous solution in step 2) is lowered to 40°C, add the iron salt aqueous solution, adjust the pH to 7.5, stir and react for 30 minutes to obtain the EDDHA chelated iron solution, and after drying Obtain 240.5 g of EDDHA chelated iron of the present invention, yield 94%.

Embodiment 3

[0036] 1) Raw material ratio (molar ratio)

[0037] Phenol 1.0

[0038] Ethylenediamine 0.6

[0039] Sodium Hydroxide 2.0

[0040] Glyoxylic acid 1.2

[0041] Iron ion (ferrous ammonium sulfate) 0.5

[0042] water 20

[0043] 2) Dissolve phenol with 10 moles of water, add ethylenediamine and sodium hydroxide solution dropwise to the phenol solution at 70°C, mix well, then add glyoxylic acid dropwise, and react at this temperature for 2.5 hours , to get EDDHA aqueous solution, wherein the weight percent concentration of sodium hydroxide aqueous solution is 40%;

[0044] 3) Dissolve the salt in the remaining 10 moles of water, and add the iron salt solution when the temperature of the EDDHA aqueous solution in step 2) is lowered to 40° C., and adjust the pH to 6.5, and stir and react for 20 minutes to obtain the EDDHA chelated iron solution, which is obtained after drying. The EDDHA chelated iron of the present invention is 248g, and the yield is 97.5%.

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Abstract

The invention provides a production process for synthetizing EDDHA Ferrochel with a one-step method, comprising the following process steps of: weighing the following raw material components in the molar ratio: 1.0% of phenol, 0.4-0.6% of quadrol, 2.0-4.0% of sodium hydroxide, 0.8-1.2% of glyoxylic acid, 0.5% of iron ion and 20% of water; firstly, synthetizing EDDHA aqueous solution; then reacting with ferric salt to synthetizing EDDHA Ferrochel solution; and drying to finally obtain the EDDHA Ferrochel. The production process has the advantages of short process flow, high yield, low production cost, no pollution and low energy consumption and does not need organic solvent. The iron content of the EDDHA Ferrochel is more than 7%, when the EDDHA Ferrochel is dissolved in water, the content of the water insoluble is less than 0.1%, and EDDHA Ferrochel is stable when PH is between 3 and 10. The EDDHA Ferrochel is mainly used as fertilizer.

Description

Technical field [0001] The invention relates to a fertilizer synthesis process, in particular to a one-step production process for synthesizing EDDHA chelated iron. technical background [0002] Iron, as one of the essential trace elements that affects plant growth and development, has been widely recognized. If fruit trees are deficient in iron, they will cause dwarf plants, shrunken stems, and white stripes and necrotic spots between leaf veins, resulting in yellowing of young tillers, complete yellowing and whitening of young leaves, and necrosis from top to bottom, seriously affecting the yield of fruit trees. , until death. On the other hand, although iron is abundant in soil, it is water-insoluble ferric oxide and has no activity. If ordinary inorganic iron salts are used, the ferrous iron ions are easily oxidized to ferric iron in soil with pH > 5, and eventually become inactive ferric oxide. EDDHA chelated iron (chemical name: ethylenediamine-N, N'hydroxyphenyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/76C07C229/36C07C227/10
Inventor 韩瑜王金梅龙章富许建光
Owner SICHUAN TONGFENG TECH
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