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Method for continuously neutralizing and extracting citric acid

An extraction method, citric acid technology, applied in the field of food chemical industry, can solve the problems of high production cost, high labor intensity of workers, unfavorable process control, etc., and achieve the goal of reducing calcium sulfate emissions, less investment in fixed assets, and low labor intensity of workers Effect

Active Publication Date: 2013-05-29
安徽丰原化工装备有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The disadvantages of the traditional calcium salt process are: first, the neutralization process is intermittently operated, the operating conditions are poor, the labor intensity of the workers is high, and the automation level is low; second, the quality of the intermediate product is unstable, which is not conducive to process control; High cost; Fourth, high consumption of auxiliary materials, about 0.86 tons of sulfuric acid and 0.86 tons of calcium carbonate per ton of citric acid; Fifth, about 2 tons of solid waste calcium sulfate per ton of citric acid
[0004] The disadvantages of the chromatography process are: first, the high investment in equipment and auxiliary facilities; second, the pre-treatment of materials is more complicated, consumes a lot of money, and costs a lot
[0005] The disadvantages of electrodialysis are: first, high investment in equipment and auxiliary facilities; second, high power consumption and high production costs
[0006] The disadvantages of the extraction method are: first, the product quality is poor; second, the product cannot be used in the food and pharmaceutical industries due to the residue of the extractant

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The production method of citric acid, comprises the steps:

[0034] 1. First put 2 cubic meters of citric acid clear liquid with an acidity of 10% into the first reaction pot, and heat the feed liquid temperature to 80°C.

[0035] 2. Slowly add calcium carbonate to carry out neutralization reaction. When the pH value is 5.0, add citric acid clear liquid and calcium carbonate at the same time, and adjust the amount of calcium carbonate added to maintain pH 5.0.

[0036] 3. After the material in the first reaction pot reaches 5 cubic meters, the material in the first reaction pot is transported to the second reaction pot, so that the feeding amount is the same as the output amount, and the liquid level of the first reaction pot is kept constant.

[0037] 4. When the volume of the material in the second reaction pot reaches 2 cubic meters, the temperature is controlled at 85°C, and calcium hydroxide is continuously added to adjust and maintain the pH to 6.0.

[0038] 5. A...

Embodiment 2

[0043] The production method of citric acid, comprises the steps:

[0044] Utilize the continuous neutralization system that embodiment 1 establishes

[0045] 1. The liquid phase produced after the separation of the fourth reaction pot material in embodiment 1 is mixed with the citric acid clear liquid in a ratio of 1:4 and then enters the first reaction pot (80° C. of temperature), and calcium carbonate is added simultaneously to maintain pH 4.5.

[0046] 2. Add calcium carbonate to the second reaction pot (temperature 80°C) to maintain pH 5.5.

[0047] 3. Add calcium carbonate and / or calcium hydroxide to the third reaction pot (temperature 85° C.) to adjust the pH to 6.

[0048] 4. Separate the materials in the third reaction pot, the solid phase calcium citrate enters the fourth reaction pot, and the liquid phase is waste water.

[0049] 5. Add the citric acid clear liquid and the solid phase material to the fourth reaction pot continuously, the reaction temperature is co...

Embodiment 3

[0052] The production method of citric acid, comprises the steps:

[0053] Utilize the continuous neutralization system that embodiment 1 establishes

[0054] 1. The liquid phase produced after the separation of the materials in the fourth reaction pot of Example 2 is mixed with the citric acid clear liquid in a ratio of 1:5 and then enters the first reaction pot (temperature 50° C.), and calcium hydroxide is added at the same time to maintain pH 4.5 .

[0055] 2. Add calcium hydroxide to the second reaction pot (temperature 55°C) to maintain pH 7.5.

[0056] 3. Add calcium hydroxide to the third reaction pot (temperature 50°C) to adjust the pH to 8.

[0057] 4. Separate the materials in the third reaction pot, the solid phase enters the fourth reaction pot, and the liquid phase is neutralized wastewater.

[0058] 5. The solid phase produced in step 4 reacts with the citric acid clear liquid in the fourth reaction pot, the reaction temperature is 75°C, and the pH value is c...

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PUM

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Abstract

The invention provides a method for continuously neutralizing and extracting citric acid, which comprises the following steps that: firstly, clear citric acid liquor and calcium carbonate and / or calcium hydroxide continuously react to gradually generate calcium citrate through segmentation control of pH value; and the generated calcium citrate reacts with the clear citric acid liquor, the liquid phase returns to the previous process after solid and liquid separation, and the solid phase is treated by acid hydrolysis, decolorization, ion exchange, concentration and crystallization to obtain the citric acid. The method has the advantages of continuous operation, high automation level, low labor intensity of worker, high equipment utilization rate, little fixed asset investment, stable intermediate product quality, low accessory consumption, little pollution, and the like.

Description

technical field [0001] The invention relates to a method for extracting citric acid, in particular to a method for extracting and separating citric acid in fermentation broth by using a calcium salt method, belonging to the field of food chemical industry. Background technique [0002] Citric acid is an organic acid widely used in beverage, food and pharmaceutical industries. my country is a major producer of citric acid, with more than 20 production plants and an output of more than 500,000 tons. The extraction methods of citric acid at home and abroad are mainly calcium salt method, chromatography, membrane separation method and extraction method. [0003] The disadvantages of the traditional calcium salt process are: first, the neutralization process is intermittently operated, the operating conditions are poor, the labor intensity of the workers is high, and the automation level is low; second, the quality of the intermediate product is unstable, which is not conducive t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C59/265C07C51/42
Inventor 李荣杰尚海涛乔华军宋加林
Owner 安徽丰原化工装备有限公司