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Preparation method of anhydrous citric acid with specific granularity

A technology of anhydrous citric acid and citric acid, applied in organic chemical methods, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problem that citric acid cannot be effectively controlled in the crystallization process, increase the cost of citric acid preparation, and increase the production workshop Energy consumption and other issues, to achieve the effect of eliminating adverse effects, avoiding uneven crystal particle size, and improving enterprise production efficiency

Active Publication Date: 2016-11-09
RIZHAO JINHE BOYUAN BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the particle size of the citric acid product prepared by the existing continuous crystallization technology is not uniform enough, and there are particles in various mesh ranges. In order to meet the customer's requirements for the product particle size, the company needs to dry the product and then sieve it, which does not meet the particle size requirements. The products are used as waste materials and re-materialized into the citric acid preparation process, which will undoubtedly increase the energy consumption of the production workshop and increase the cost of citric acid preparation
And the citric acid product purity that makes is low, and moisture is high, and bulk density is little, makes product quality be affected
For a long time, citric acid preparation technology has been unable to effectively control the crystallization process according to the requirements of product particle size and appearance shape

Method used

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  • Preparation method of anhydrous citric acid with specific granularity
  • Preparation method of anhydrous citric acid with specific granularity
  • Preparation method of anhydrous citric acid with specific granularity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Prepare the anhydrous citric acid product with a particle size of 20-40 meshes required by the customer.

[0045] The citric acid acid solution obtained after calcium salt neutralization and sulfuric acid acid hydrolysis is subjected to ion exchange through continuous separation equipment to remove various pigments and anion and cation impurities. After separation treatment, the permeability of the separation solution Luminosity is 99.6%, Cl - , SO 4 2- , Fe 3+ The content is less than 0.5mg / L, and the acidity is 55%.

[0046] Concentrating and evaporating the off-transaction liquid to obtain a multi-effect concentrate, the relative density of the multi-effect concentrate is 1360kg / m 3 , with an acidity of 104%.

[0047] will be 5m 3 The multi-effect concentrate is added to the crystallizer for concentrated crystallization. The initial temperature of the concentrate is 55°C, the crystallization vacuum is 0.092MPa, and the evaporation temperature is 61°C. When the...

Embodiment 2

[0052] Prepare the anhydrous citric acid product with a particle size of 30-60 meshes required by the customer.

[0053] The citric acid acid solution obtained after calcium salt neutralization and sulfuric acid acid hydrolysis is subjected to ion exchange through continuous separation equipment to remove various pigments and anion and cation impurities. After separation treatment, the permeability of the separation solution Luminosity is 99.8%, Cl - , SO 4 2- , Fe 3+ The content is less than 0.4mg / L, and the acidity is 53%.

[0054] Concentrating and evaporating the off-transaction liquid to obtain a multi-effect concentrated liquid with a relative density of 1370kg / m 3 , with an acidity of 106%.

[0055] will be 6.4m 3 The multi-effect concentrate is added to the crystallizer for concentrated crystallization. The initial temperature of the concentrate is 53°C, the crystallization vacuum is 0.091MPa, and the evaporation temperature is 62°C. When the solution supersatur...

Embodiment 3

[0060] Prepare the anhydrous citric acid product with a particle size of 40-60 meshes required by the customer.

[0061] The citric acid acid solution obtained after calcium salt neutralization and sulfuric acid acid hydrolysis is subjected to ion exchange through continuous separation equipment to remove various pigments and anion and cation impurities. After separation treatment, the permeability of the separation solution Luminosity is 99.8%, Cl - , SO 4 2- , Fe 3+ The content is less than 0.3mg / L, and the acidity is 58%.

[0062] Concentrating and evaporating the off-transaction liquid to obtain a multi-effect concentrate, the relative density of the multi-effect concentrate is 1385kg / m 3 , with an acidity of 105%.

[0063] will be 6m 3 The multi-effect concentrate is added to the crystallizer for concentrated crystallization. The initial temperature of the concentrate is 53°C, the crystallization vacuum is 0.090MPa, and the evaporation temperature is 63°C. When the...

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Abstract

The invention discloses a preparation method of anhydrous citric acid with specific granularity. The method comprises the following steps: carrying out multiple-effect evaporative concentration on an ion exchange treated citric acid acidolysis liquid, feeding the obtained multiple-effect concentrate to a crystallizer, carrying out continuous evaporative crystallization, and adding crystal seeds when the concentrate reaches certain supersaturation degree in order to induce crystal formation; adjusting the evaporation rate of a feed liquid and the addition rate of the multiple-effect concentrate in the crystallization process to control the supersaturation degree in order to stabilize the crystallization rate; arranging an online particle size determinator on the crystallizer, and discharging the obtained material when the granularity of crystals reaches required granularity; and centrifuging the obtained crystal slurry, and drying the centrifuged crystal slurry to obtain the anhydrous citric acid product with high purity, low water, uniform particles, concentrated granularity distribution, high bulk density and good anti-agglomeration capability. The anhydrous citric acid product obtained in the invention can meet different clients' requirements for the product granularity without screening, avoids the step of recovering and converting products with unsatisfactory granularity, reduces the energy consumption and improves the citric acid production efficiency.

Description

technical field [0001] The invention relates to a method for preparing anhydrous citric acid, in particular to a method for preparing anhydrous citric acid with a specific particle size. Background technique [0002] Citric acid is a very important organic acid, which is widely used in food, medicine, chemical industry and other industries. The preparation method is generally as follows: liquefy and ferment corn, potato, molasses and other starchy raw materials, neutralize the fermented clear liquid by calcium salt method or hydrogen calcium method, acidolysis with concentrated sulfuric acid, and filter, decolorize, ion exchange, etc. The operation is to obtain the ionotropic liquid, which is concentrated by evaporation and then added to the crystallizer for evaporation and crystallization, and then the citric acid product is obtained through subsequent processes such as centrifugation and drying. [0003] In the production process of citric acid, the quality of crystalliza...

Claims

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Application Information

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IPC IPC(8): C07C51/43C07C59/265
CPCC07B2200/13C07C51/43C07C59/265
Inventor 寇光智李昌涛马菲菲孔玉蒋水星刘长静
Owner RIZHAO JINHE BOYUAN BIOCHEM
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