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Method for directly producing sodium citrate, potassium citrate and ammonium citrate from citric acid fermentation broth by melamine compound salt crystallization

A technology of citric acid fermentation broth and sodium citrate, which is applied in carboxylate preparation, separation/purification of carboxylic acid compounds, organic chemistry, etc., and can solve the problems of high cost and low yield of citric acid

Inactive Publication Date: 2017-08-25
姚鼎文
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Everyone who is engaged in the chemical industry knows that the production method of sodium citrate, potassium and ammonium salts is the simplest and most feasible method is the neutralization reaction of citric acid with sodium alkali, potassium alkali and ammonia water. The product quality of this method is good, but the cost is relatively high , the yield of citric acid is low, and there are many innovations in domestic processing technology at present. In summary, there are ion exchange resins that exchange citric acid in the fermentation broth with resin, and then rinse the resin with sodium hydroxide solution to produce sodium citrate solution. Concentrate, crystallize, and dry to obtain sodium citrate; first add citric acid in the fermentation broth to calcium carbonate to form calcium citrate, and then react with sodium carbonate under the action of a quaternary ammonium citrate surfactant to produce sodium citrate And calcium carbonate, the latter returns to the front to precipitate citric acid; there is a reaction between citric acid mother liquor and sodium hydroxide in the presence of ethanol to generate sodium citrate

Method used

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  • Method for directly producing sodium citrate, potassium citrate and ammonium citrate from citric acid fermentation broth by melamine compound salt crystallization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Take some fermentation slurry from the fermentation workshop of a domestic citric acid factory, press and filter, take 100 grams of mycelia, mix with 20 grams of sweet potato dry powder and 20 grams of feed sodium calcium phosphate, and extrude into granular form at 85-95 degrees Celsius Dried, ready-made compound feed sodium-calcium phosphate, get 1000 grams of fermented liquid that filters mycelium, measure citric acid content and be 17.8%, add the industrial melamine 238 grams that purity is 98%, stir 1 hour at 25 degrees centigrade, pump Filtration, rinsing, return of filtrate and washing water for the submerged culture of sweet potato dry powder, add 25% sodium hydroxide solution to the wet solid phase, adjust to the amount of trisodium salt, stir for half an hour, suction filter and wash, wet The solid phase is regenerated melamine, which is returned to extract the citric acid in the next cycle of fermentation broth, the filtrate and washing water are concentrated,...

Embodiment 2

[0014] Take 1000 grams of the fermented liquid filtered above, add 238 grams of industrial melamine with a purity of 98%, stir for 1 hour at 25 degrees Celsius, filter with suction, rinse, and return the filtrate and washing water for the submerged culture of sweet potato dry powder, wet solid phase Add potassium hydroxide with a concentration of 25%, adjust to the amount of tripotassium salt, stir at 25 degrees Celsius for half an hour, filter with suction, rinse, the wet solid phase is regenerated melamine, return to extract the lemon in the fermentation broth The acid, filtrate and washing water were concentrated, crystallized, separated, and dried at 100-110 degrees Celsius to obtain 275 grams of anhydrous potassium citrate with a purity of 98.1%. It was learned that the national standard would not be promulgated until several months later, and currently it can only be used by root users The required quality is manufactured. Since this process does not add chemical raw mate...

Embodiment 3

[0016] Take 1000 grams of the above-filtered fermented liquid, add 238 grams of melamine with a purity of 98%, stir for 1 hour at 26 degrees Celsius, filter with suction, wash, and return the filtrate and washing water to the submerged cultivation of sweet potato dry powder, and add concentration to the wet solid phase It is 25% ammonia water, adjusted to the amount of triammonium salt generated, stirred at 26 degrees Celsius for half an hour, filtered, washed, and the wet solid phase is returned to extract citric acid in the fermentation broth, the filtrate and washing water are concentrated, crystallized, separated, Dried at 100-110 degree Celsius to obtain 218 grams of ammonium citrate with a purity of 98.2%.

[0017] Table 1, trisodium citrate anhydrous analysis, weight (%)

[0018] standard name BP2000 This craft product content ≥99％ 99.3％ acidity and alkalinity meet the requirements meet the requirements Sulfate ≤0.03％ 0％ Heavy m...

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Abstract

Provided is a method for using melamine and citric acid in a citric acid fermentation broth to react to form citric acid-melamine compound salt crystals used for producing sodium citrate, potassium citrate and ammonium citrate. The method includes the steps of putting the melamine into a starch fermentation broth and stirring at normal temperature to make the mixture react; filtering and washing to obtain the citric acid-melamine compound salt crystals; making sodium alkali and potash react with ammonium hydroxide respectively to form the sodium citrate, potassium citrate and ammonium citrate solutions and the solid melamine, wherein the melamine is returned to the next cycle to extract citric acid from the fermentation broth; blending the mycelium obtained by filtering with sodium phosphate calcium fodder and sweet potato powder; extruding the blending for moulding, and drying to obtain sodium phosphate calcium composite fodder; conducting concentrated crystallization on the sodium citrate, potassium citrate and ammonium citrate solutions and washing water respectively, and drying to obtain the sodium citrate, potassium citrate and ammonium citrate products.

Description

technical field [0001] The invention belongs to the production technology of citrate, and is a technical category of directly producing citrate from starch fermentation liquid by utilizing the performance of forming double salt crystals with melamine and citric acid. Background technique [0002] Everyone who is engaged in the chemical industry knows that the production method of sodium citrate, potassium and ammonium salts is the simplest and most feasible method is the neutralization reaction of citric acid with sodium alkali, potassium alkali and ammonia water. The product quality of this method is good, but the cost is relatively high , the yield of citric acid is low, and there are many innovations in domestic processing technology at present. In summary, there are ion exchange resins that exchange citric acid in the fermentation broth with resin, and then rinse the resin with sodium hydroxide solution to produce sodium citrate solution. Concentrate, crystallize, and dr...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C51/43C07C59/265
CPCC07C51/41C07C51/43C07C59/265
Inventor 姚鼎文姚宁雷硤
Owner 姚鼎文
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