Preparation method for iron sodium ethylene diamine tetraacetate

A technology of sodium ferric EDTA and EDTA, applied in the field of preparation of sodium ferric EDTA, can solve the problem that colloids are difficult to filter and wash, the reactivity of iron oxide is low, and industrial production costs are increased, etc. problems, to achieve the effect of short reaction time, high product yield and improved crop quality

Active Publication Date: 2016-02-03
上海永通生态工程股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. When ferric chloride or ferric sulfate is used as raw material for direct preparation in the process, the product will contain a large amount of inorganic salt by-products such as sodium chloride and sodium sulfate, which will be difficult to separate later and increase the cost of industrial production
[0005] 2. When disodium edetate is used as raw material in the process, there will also be a large amount of sodium ions in the product, which will reduce the purity of the product
[0006] 3. When iron oxide is used to prepare chelated iron, due to the low reactivity of iron oxide, high reaction temperature is required, and the reaction time will be greatly extended at the same time, resulting in high energy consumption and low efficiency.
Colloids are difficult to filter and wash, which will bring difficulties to subsequent production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Weigh 3.71kg of ferrous sulfate heptahydrate and add it to 8L of deionized water, heat to 40°C-50°C, stir to dissolve, then weigh 2.11kg of ammonium bicarbonate and slowly add it to the ferrous sulfate solution while stirring, and wait for the reaction Filter the reaction solution until no bubbles emerge, wash the filter cake with deionized water for 2-3 times until there is no sulfate ion, quickly air-dry and crush the filter cake to obtain the high-activity ferric hydroxide reaction raw material, and collect the ferric hydroxide The rate is above 98%.

[0018] Add 10L of deionized water to a 20L reaction kettle, slowly add 3.12kg of ethylenediaminetetraacetic acid and 0.43kg of sodium hydroxide into it, continue to add 1.37kg of the above-mentioned ferric hydroxide raw material under stirring, and use sodium hydroxide Adjust the pH to 6.0, heat to 80°C, and react for 30 minutes. The reaction solution is filtered, evaporated, concentrated, cooled and crystallized, and ...

Embodiment 2

[0020] Weigh 4.38kg of ferrous sulfate heptahydrate and add it to 9L of deionized water, heat to 40°C-50°C, stir to dissolve, then weigh 1.31kg of sodium carbonate and slowly add it to the ferrous sulfate solution under stirring, until no reaction occurs Filter the reaction solution until bubbles emerge, wash the filter cake with deionized water for 2-3 times until there are no sulfate ions, quickly air-dry and crush the filter cake to obtain the high-activity ferric hydroxide reaction raw material, and the yield of ferric hydroxide is It is more than 98%.

[0021] Add 10L of deionized water to a 20L reaction kettle, slowly add 4.10kg of ethylenediaminetetraacetic acid and 0.56kg of sodium hydroxide into it, continue to add 1.65kg of the above-mentioned ferric hydroxide raw material under stirring, and use sodium hydroxide Adjust the pH to 5.5, heat to 70°C, and react for 50 minutes. The reaction solution is filtered, evaporated, concentrated, cooled and crystallized, and the ...

Embodiment 3

[0023] Weigh 3.71kg of ferrous sulfate heptahydrate and add it to 9.6L of deionized water, heat to 40°C-50°C, stir to dissolve, then weigh 1.06kg of ammonium bicarbonate and 0.55kg of sodium carbonate and slowly add it to the sulfurous acid In the iron solution, filter the reaction solution until no bubbles emerge from the reaction, wash the filter cake 2-3 times with deionized water until there is no sulfate ion, quickly air-dry the filter cake and crush it to obtain a high-activity ferric hydroxide reaction Raw material, ferric hydroxide yield is more than 98%.

[0024] Add 10L of deionized water to a 20L reactor, slowly add 3.82kg of ethylenediaminetetraacetic acid and 0.52kg of sodium hydroxide into it, continue to add 1.40kg of the above-mentioned ferric hydroxide under stirring, and adjust the pH to 5.0, Heating to 60°C, reacting for 50 minutes, filtering the reaction solution, evaporating and concentrating, cooling and crystallizing, and crushing the crystals to obtain ...

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PUM

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Abstract

The invention discloses a preparation method for iron sodium ethylene diamine tetraacetate. The preparation method comprises the following steps: (1) weighing a predetermined amount of ferrous sulfate heptahydrate, adding ferrous sulfate heptahydrate into deionized water, weighing a predetermined amount of bicarbonate, carbonate or a mixture of bicarbonate and carbonate, adding the weighed bicarbonate, carbonate or mixture into a ferrous sulphate solution, carrying out a reaction so as to obtain large-grain ferrous hydroxide precipitate and introducing air to completely oxidize ferrous hydroxide into reddish brown iron hydroxide powder for subsequent usage; (2) weighing a predetermined amount of ethylene diamine tetraacetic acid and sodium hydroxide and adding ethylene diamine tetraacetic acid and sodium hydroxide into deionized water; and (3) addin gthe iron hydroxide powder into the solution obtained in the step (2) under stirring according to a predetermined mol ratio, adjusting a pH value to 4.5 to 6.0, heating the solution to 60 to 80 DEG C, carrying out stirring reaction for 30 to 50 min and subjecting the solution to filtering and crystallization so as to obtain finished iron sodium ethylene diamine tetraacetate. The method provided by the invention prepares iron hydroxide through on-site oxidation of ferrous hydroxide, and the prepared iron hydroxide has high reaction activity, needs short time for subsequent chelation reaction and enables product yield to be high and production efficiency to be greatly improved.

Description

technical field [0001] The invention relates to a chelated trace element fertilizer, in particular to a preparation method of sodium ferric edetate. Background technique [0002] Although the content of iron in crops is small, it has two important functions: first, it is an important part of some enzymes and many electron transfer proteins; second, it can regulate the synthesis of chloroplast protein and chlorophyll. If the plant is deficient in iron, it will cause chlorosis between the leaf veins, which will affect the photosynthesis and respiration of the plant, resulting in reduced yield and quality of crops. The supplement of iron mainly includes inorganic iron fertilizers, such as ferrous sulfate, ferric sulfate, ferric chloride, etc., and chelated iron fertilizers, such as sodium ferric ethylenediamine tetraacetate, sodium ferric diethylenetriamine pentaacetate, Sodium ferric ethylenediamine di-o-hydroxyphenylacetate, etc. Inorganic iron fertilizer is easy to precipi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C229/16C07C227/18
Inventor 石称华连晓敏周芳钱志红
Owner 上海永通生态工程股份有限公司
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