Continuous acidolysis method of citrate

A technology of calcium citrate salt and acid hydrolysis, applied in the field of food chemical industry, can solve the problems of unstable quality of intermediate products, unfavorable process control, high impurity content of acid hydrolyzate, high equipment utilization rate, low labor intensity of workers, The effect of less investment in fixed assets

Active Publication Date: 2009-10-14
安徽丰原集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional calcium salt method adopts calcium citrate acid hydrolysis, and its disadvantages are: 1) It is an intermittent operation, with poor operating conditions, high labor intensity, and low automation level; 2) The quality of intermediate products i

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The continuous acid hydrolysis method of citric acid comprises the steps:

[0033] 1. First add 2 kg of calcium citrate salt with a water content of 50% and an appropriate amount of water into a main reactor with a volume of 5 liters, set the volume to 2.5 liters, and heat the temperature of the feed liquid to 80°C.

[0034] 2. Slowly add 98% concentrated sulfuric acid for reaction. When the pH value is 3.0, add calcium citrate and concentrated sulfuric acid at the same time to maintain pH 3.0 and temperature 80°C.

[0035] 3. After the material in the main reactor reaches 4 liters, the material in the main reactor is transported to the auxiliary reactor, and the feeding amount of the main reactor is kept the same as the output amount, so that the liquid level of the material in the main reactor is constant.

[0036] 4. When the volume of the secondary reactor material reaches 2 liters, the temperature is controlled at 80°C, and sulfuric acid is continuously added to ad...

Embodiment 2

[0049] Carry out the continuous acid hydrolysis reaction of citric acid by the step described in embodiment 1, difference is:

[0050] 1. Lower the temperature of the main reactor to 50°C, raise the pH to 3.5, and keep other conditions unchanged.

[0051] 2. Lower the temperature of the secondary reactor to 50° C., raise the pH to 3.0, and keep other conditions unchanged.

[0052] 3. The third reactor maintains a temperature of 80°C and a pH of 1.8.

[0053] 4. After 12 cycles of stable operation of the above system, the acid hydrolysis solution and calcium sulfate were analyzed, and the results are shown in Table 4, Table 5 and Table 6.

[0054] Table 4 acid solution quality comparison

[0055] Compare items

Intermittent acid hydrolysis acid hydrolysis solution

continuous acid hydrolysis

Citric acid concentration (%)

38

44

Ca 2+ (ppm)

2400

2000

SO4 2- (ppm)

2500

2000

[0056] Table 5 calci...

Embodiment 3

[0061] Utilize the continuous acid hydrolysis system that embodiment 1 establishes to carry out the continuous acid hydrolysis of citric acid, comprise the steps:

[0062] 1. 50% of the third reactor material discharge of embodiment 2 is returned to the main reactor, and the temperature is controlled at 80° C., and calcium citrate and sulfuric acid are added simultaneously to maintain pH 4.5.

[0063] 2. The temperature of the secondary reactor is controlled at 80°C, and sulfuric acid is added to maintain the pH at 2.5.

[0064] 3. The temperature of the third reactor is controlled at 80°C, and sulfuric acid is added to maintain the pH at 1.8.

[0065] 4. While maintaining the liquid level of the third reactor, transport the material to the solid-liquid separation equipment, and separate the material from solid-liquid. During separation, the washing water consumption is 10% of the volume of the material, and the solid phase is calcium sulfate. The liquid phase is citric acid ...

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Abstract

The invention relates to a continuous acidolysis method of citrate, comprising the following steps of: 1) first-order reaction: calcium citrate and sulphuric acid carry out acidolysis reaction in a main reactor and the pH value is 1 to 5; 2) second-order reaction: the sulphuric acid and the calcium citrate are added to control the reaction pH value to be 0.5 to 4 and acidolysis reaction is carried out in a secondary reactor; 3) third-order reaction: the sulphuric acid and the calcium citrate are added to control the reaction pH value to be 1.5 to 2.5 and acidolysis reaction is implemented in a tertiary reactor; and 4) solid-liquid separation: solid-liquid separation is implemented on products of acidolysis reaction to obtain the acidolysis solution of citrate and calcium sulphate solid. The method has the advantages of continuous operation, high automation level, stable quality of intermediate products, high concentration of acidolysis solution and low impurity ion content and the like.

Description

technical field [0001] The invention relates to the field of food chemical industry, in particular to a method for continuous acid hydrolysis of citrate. 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 the output has exceeded 700,000 tons. The extraction method of citric acid at home and abroad is mainly the calcium salt method. [0003] The traditional calcium salt method adopts calcium citrate acid hydrolysis, and its disadvantages are: 1) It is an intermittent operation, with poor operating conditions, high labor intensity, and low automation level; 2) The quality of intermediate products is unstable, which is not conducive to process control; 3) The impurity content of the acidolysis solution is high, and the ion exchange load is large; 4) the by-product calcium sulfate particles are small, the washing is diffi...

Claims

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Application Information

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IPC IPC(8): C07C59/265C07C51/02
CPCC07C51/02
Inventor 李荣杰宋家林尚海涛潘声龙崔亚放
Owner 安徽丰原集团有限公司
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