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Preparation method of iron-tartaric acid-sodium complex

A tartaric acid and complex technology, which is applied in the field of complex preparation, can solve problems such as waste of raw materials and influence on the stability of complexes, and achieve the effects of small raw material consumption, simple preparation method, and mild reaction conditions

Active Publication Date: 2013-11-06
HUNAN XUETIAN FINE CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After the racemization is completed, if it is to be adjusted to neutral or acidic for complexation, due to the buffering effect of sodium tartrate, it needs to consume a large amount of inorganic or organic acid to adjust to a suitable pH value, which will cause waste of raw materials ; if Fe is introduced in the alkaline range of pH>9 3+ or Fe 2+ Form a complex solution, the stability of the complex formed by sodium tartrate and iron will be affected, Fe 3+ or Fe 2+ It is easy to precipitate in the form of hydroxide and break the network
[0022] In summary, the prior art has realized the mesization reaction of sodium tartrate, and simultaneously prepared iron-tartrate complexes with certain stability, but there are still some unsatisfactory situations, so there is still room for improvement

Method used

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  • Preparation method of iron-tartaric acid-sodium complex
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  • Preparation method of iron-tartaric acid-sodium complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Add 3 kg of L-TA to the autoclave, H 2 O 3kg, heat up to 165°C, keep warm for 40h. Stop heating, stir and release the feed liquid after gradually cooling down. Detected content, meso form accounted for 45.6%, racemate accounted for 54.4%. Add 50% FeCl with stirring 3 Solution 6.5kg, after the complexation is uniform, add 50% NaOH solution 4.8kg under the condition of reflux with condensation. Stir evenly until a light green uniform iron-tartrate-sodium complex is formed, with a pH value of 2.2.

Embodiment 2

[0053] Add 4 kg of L-TA to the autoclave, H 2 O 2kg, heat up to 170°C, keep warm for 40h. Stop heating, stir and release the feed liquid after gradually cooling down. In the detection content, the meso form accounted for 51.7%, and the racemate accounted for 48.3%. Add 50% FeCl with stirring 3 Solution 9kg, after the complexation is uniform, add 50% NaOH solution 7.5kg under the condition of reflux with condensation. Stir evenly until a yellow-green uniform iron-tartrate-sodium complex is formed, with a pH value of 4.5.

Embodiment 3

[0055] Add 4 kg of L-TA to the autoclave, H 2 O 2kg, HCl (36% content) 0.5kg, heat up to 165°C, keep warm for 24h. Stop heating, stir and release the feed liquid after gradually cooling down. Detected content, meso form accounted for 58.4%, racemate accounted for 41.6%. Add 50% FeCl with stirring 3 Solution 9kg, after the complexation is uniform, add 50% NaOH solution 8.5kg under the condition of reflux with condensation. Stir evenly until a dark green uniform iron-tartrate-sodium complex is formed, with a pH value of 6.8.

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Abstract

The invention discloses a preparation method of an iron-tartaric acid-sodium complex. The preparation method comprises following steps: (1) water and dextrotartaric acid are added into a high-pressure reaction vessel, wherein the dextrotartaric acid concentration of the solution is more than 5 wt%; the solution is stirred, heated to 155 to 175 DEG C, and reacted for 8 to 48h at the temperature of 155 to 175 DEG C; (2) the contents of the ingredients in the high-pressure reaction vessel are determined, and the reaction is stopped when more than 30 wt% of dextrotartaric acid is converted to mesotartaric acid; (3) the ingredients in the high-pressure reaction vessel are cooled to room temperature, and then the solution is discharged; (4) a solution containing Fe3<+> is added into the solution with stirring; and (5) a solution containing Na<+> is added into the solution with stirring, the mixture is stirred until appearance is clear, color is uniform, no precipitate is generated and no stratification is causes, and then the iron-tartaric acid-sodium complex is obtained. Reaction conditions of the preparation method are mild; the preparation method is simple; consumption of raw materials is less; no pollution is caused; the preparation method is suitable for industrial production; and the stability of the iron-tartaric acid-sodium complex is much higher than that of complex prepared by existing methods.

Description

technical field [0001] The invention relates to the technical field of preparation of complexes, in particular to a preparation method of an iron-tartrate-sodium complex. Background technique [0002] The molecular structure of tartaric acid (LA) contains two chiral carbon atoms. The product has three configurations. The structural formula is as follows: figure 1 shown. [0003] Equal amounts of L-tartaric acid and D-tartaric acid combine to form the fourth substance, the optically inactive racemic tartaric acid (DL-TA). Due to the small differences in the structures of these several substances, there are certain difficulties in the synthesis and separation of pure products. The natural tartaric acid in plants is mainly L-TA, while the synthetic tartaric acid is mainly DL-TA. Meso-tartaric acid can be produced by fermenting and decomposing plant starch, but this method is difficult to be used in industrial applications due to the low conversion rate and the difficulty of ...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C59/255
Inventor 谢维跃曾平冯章明蒋佑清胡良页汤志球佘光前聂晖许筠
Owner HUNAN XUETIAN FINE CHEM IND
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