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A kind of preparation method of sodium iron edetate

A technology of sodium ferric edetate and ethylenediaminetetraacetic acid, which is applied in the field of preparation of sodium ferric edetate, and can solve the problems of difficult filtration and washing of colloids, low reactivity of iron oxide, and increased industrial production costs, etc. problems, to achieve the effects of short reaction time, high product yield, and improved crop quality

Active Publication Date: 2017-11-28
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℃-50℃, stir to dissolve, then weigh 2.11kg of ammonium bicarbonate and slowly add it to the ferrous sulfate solution under stirring, wait for 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. The filter cake is quickly air-dried and pulverized to obtain high-activity iron hydroxide reaction raw materials. 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 iron hydroxide raw material prepared above under stirring, and use sodium hydroxide Adjust the pH to 6.0, heat to 80°C, react for 30 minutes, filter the reaction solution to evaporate and concentrate, cool to crystallize, and smash the crystals to obtain the finished product. Th...

Embodiment 2

[0020] Weigh 4.38kg of ferrous sulfate heptahydrate and add it to 9L of deionized water, heat to 40℃-50℃, stir to dissolve, then weigh 1.31kg of sodium carbonate and slowly add it to the ferrous sulfate solution under stirring. Filter the reaction solution until the bubbles emerge. Wash the filter cake with deionized water for 2-3 times until there is no sulfate ion. The filter cake is quickly air-dried and crushed to obtain high-activity iron hydroxide reaction raw materials. The yield of iron hydroxide It is more than 98%.

[0021] Add 10L of deionized water to a 20L reactor, slowly add 4.10kg of ethylenediaminetetraacetic acid and 0.56kg of sodium hydroxide into it, and continue to add 1.65kg of the iron hydroxide raw material prepared above under stirring, and use sodium hydroxide Adjust the pH to 5.5, heat to 70°C, react for 50 minutes, filter the reaction solution to evaporate and concentrate, cool to crystallize, and crush the crystals to obtain the finished product. The ...

Embodiment 3

[0023] Weigh 3.71kg of ferrous sulfate heptahydrate and add it to 9.6L of deionized water, heat to 40℃-50℃, stir to dissolve, then weigh 1.06kg of ammonium bicarbonate and 0.55kg of sodium carbonate and slowly add to the subsulfite under stirring In the iron solution, after the reaction has no bubbles, filter the reaction solution and wash the filter cake with deionized water for 2-3 times until there is no sulfate ion. The filter cake is quickly air-dried and crushed to obtain highly active iron hydroxide. The raw material, iron hydroxide yield is 98% or more.

[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 ferric hydroxide prepared above under stirring, and adjust the pH to 5.0. Heat to 60°C, react for 50 minutes, filter the reaction solution to evaporate and concentrate, cool to crystallize, and crush the crystals to obtain the finished product. The pro...

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Abstract

The invention discloses a preparation method of sodium ferric EDTA, comprising the following steps: (1) weighing a predetermined amount of ferrous sulfate heptahydrate and adding it to deionized water; weighing a predetermined amount of bicarbonate, carbonic acid The mixture of salt or bicarbonate and carbonate is added in the ferrous sulfate solution, and the reaction obtains large particle ferrous hydroxide precipitation; Bubbling air is fully oxidized to ferrous hydroxide powder for subsequent use; ( 2) Weigh a predetermined amount of EDTA and sodium hydroxide, add deionized water; (3) according to a predetermined molar ratio, add ferric hydroxide to the solution obtained in the step (2) under agitation powder, adjust the pH to 4.5-6.0, heat to 60 ℃-80 ℃, stir and react for 30min-50min, the solution is filtered and crystallized to obtain the finished product of sodium iron ethylenediaminetetraacetate. The ferric hydroxide prepared by the on-site oxidation of ferrous hydroxide in the method of the invention has high reaction activity, short subsequent chelation reaction time, high product yield and greatly improved production efficiency.

Description

Technical field [0001] The invention relates to a chelated trace element fertilizer, in particular to a preparation method of sodium ferric ethylenediaminetetraacetate. Background technique [0002] Although iron is low in crops, it has two important functions: first, it is an important part of certain enzymes and many electron transport proteins; second, it can regulate the synthesis of chloroplast protein and chlorophyll. Iron deficiency in plants will cause chlorosis between leaf veins, which will affect plant photosynthesis and respiration, resulting in reduced crop yields and quality. The main supplements to iron are inorganic iron fertilizers, such as ferrous sulfate, iron sulfate, ferric chloride, etc., and chelated iron fertilizers, such as sodium iron ethylenediaminetetraacetate, sodium iron diethylenetriaminepentaacetate, Ethylenediamine di-o-hydroxyphenyl sodium iron acetate and so on. Inorganic iron fertilizer is easy to precipitate, has low utilization rate, and is...

Claims

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Application Information

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Patent Type & Authority Patents(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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