Preparation method of diammonium hydrogen citrate

A technology of diammonium hydrogen citrate and citric acid, applied in the field of food additives, can solve the problems of exhaust gas emission, many materials, large energy consumption, etc., and achieve the effect of avoiding decomposition

Inactive Publication Date: 2015-03-25
NANTONG FEIYU FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The diammonium hydrogen citrate product is usually prepared by reacting citric acid and ammonium salt, and then decolorizing with activated carbon, filtering, removing impurities, concentrating, crystallizing, drying and other processes. This method has a long process, low yield, and exhaust gas emissions , causing environmental pollution
[0003] Among the existing published patents, the patent name is: Synthetic method of ammonium citrate, and the application number is:

Method used

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  • Preparation method of diammonium hydrogen citrate

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specific Embodiment 1

[0029] A preparation method of diammonium hydrogen citrate, comprising the steps of:

[0030] Step (1), using edible citric acid and liquid ammonia as raw materials;

[0031] Step (2), dissolving edible citric acid in water to prepare a solution with a concentration of 39%;

[0032] In step (3), the liquid ammonia is passed into the citric acid aqueous solution, and the liquid ammonia is slowly added to control the pH value of the solution to be within the range of 4.5;

[0033] Step (4), air-cool the above materials to 19°C, until a large amount of diammonium hydrogen citrate crystallizes out, and separates from the mother liquor through a centrifuge to obtain crystals of diammonium hydrogen citrate;

[0034] In step (5), send the crystals of diammonium hydrogen citrate to a drying oven at 62°C for 45 minutes to obtain diammonium hydrogen citrate;

[0035] In step (6), continue to dissolve the remaining mother liquor in edible citric acid for recycling.

specific Embodiment 2

[0036] A preparation method of diammonium hydrogen citrate, comprising the steps of:

[0037] Step (1), using edible citric acid and liquid ammonia as raw materials;

[0038] Step (2), dissolving edible citric acid in water to prepare a solution with a concentration of 51%;

[0039] In step (3), the liquid ammonia is passed into the citric acid aqueous solution, and the liquid ammonia is slowly added to control the pH value of the solution to be within the range of 5.5;

[0040] Step (4), air-cool the above materials to 27°C until a large amount of diammonium hydrogen citrate crystallizes, and separate from the mother liquor through a centrifuge to obtain crystals of diammonium hydrogen citrate;

[0041] Step (5), sending the diammonium hydrogen citrate crystals to a drying oven at 70°C for 60 minutes to obtain diammonium hydrogen citrate;

[0042] In step (6), continue to dissolve the remaining mother liquor in edible citric acid for recycling.

specific Embodiment 3

[0043] A preparation method of diammonium hydrogen citrate, comprising the steps of:

[0044] Step (1), using edible citric acid and liquid ammonia as raw materials;

[0045] Step (2), dissolving edible citric acid in water to prepare a solution with a concentration of 47%;

[0046] In step (3), the liquid ammonia is passed into the citric acid aqueous solution, and the liquid ammonia is slowly added to control the pH value of the solution to be within the range of 5.1;

[0047] Step (4), air-cool the above materials to 23°C until a large amount of diammonium hydrogen citrate crystallizes out, and separates from the mother liquor through a centrifuge to obtain crystals of diammonium hydrogen citrate;

[0048] Step (5), sending the diammonium hydrogen citrate crystals to a drying oven at 64°C for 56 minutes to obtain diammonium hydrogen citrate;

[0049] In step (6), continue to dissolve the remaining mother liquor in edible citric acid for recycling.

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Abstract

The invention discloses a preparation method of diammonium hydrogen citrate. The preparation method comprises the following steps: by taking edible citric acid and liquid ammonia as raw materials, dissolving the edible citric acid into water to prepare a 39%-51% solution; introducing liquid ammonia into the citric acid solution, slowly adding liquid ammonia, and controlling the pH value of the solution to be within 4.5-5.5; performing air cooling on the materials to room temperature until a great amount of diammonium hydrogen citrate is crystalized and separated out, and separating mother liquor through a centrifugal machine to obtain diammonium hydrogen citrate crystals; conveying the diammonium hydrogen citrate crystals to a drying oven at 62DEG C-70DEG C, and drying for 45-60 minutes, to obtain diammonium hydrogen citrate; continuously dissolving edible citric acid with the remaining mother liquor and recycling. The high-concentration citric acid is prepared, so that the usage amount of water is less, the citric acid is cooled, crystalized and separated out through the ammonina introduction and reaction, centrifugal is performed, dehydrated mother liquor can be continuously used for dissolving citric acid, and no energy consumption, no emission and no environment pollution exist during the overall process.

Description

technical field [0001] The invention belongs to the field of food additives, in particular to a preparation method of diammonium hydrogen citrate. Background technique [0002] Diammonium hydrogen citrate is a white granule or crystalline powder, soluble in about 1 part of water, the aqueous solution is weakly acidic, slightly soluble in ethanol, and decomposes upon high heat, with a density of 1.48. In addition to the same role as ammonium citrate, it can also be used in probiotics and yogurt starters. The diammonium hydrogen citrate product is usually prepared by reacting citric acid and ammonium salt, and then decolorizing with activated carbon, filtering, removing impurities, concentrating, crystallizing, drying and other processes. This method has a long process, low yield, and exhaust gas emissions , causing environmental pollution. [0003] Among the existing published patents, the patent name is: Synthetic method of ammonium citrate, and the application number is: ...

Claims

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Application Information

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IPC IPC(8): C07C59/265C07C51/41
CPCC07C51/412C07C51/43C07C59/265
Inventor 姚建飞朱碧君姚佼
Owner NANTONG FEIYU FINE CHEM
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