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Citric acid waste production citric acid technology
The first step involves the processing of solid residue obtained after crushing oranges. The citrus residue is pressed to separate the juice, while the solid fraction is dried to produce dried orange peel. The extracted juice is then heated and concentrated into molasses.
In the second step, fermentation takes place. A mixture of 50 grams of orange peel and more than 500 ml of molasses is placed in a flask. The mixture is sterilized at 121°C for 30 minutes, followed by inoculation with yeast spores. Then, 50 times the volume of distilled water is added for extraction. The solution is filtered, and calcium carbonate is added to the filtrate. After filtering out the solids, sulfuric acid is introduced to treat the mixture. This reaction produces calcium sulfate, which is removed through filtration. The remaining filtrate is concentrated and crystallized to obtain the final product.
Processing steps include:
(1) Raw Material Preparation: Citrus processing residues are used as the main material. The residue is squeezed to extract juice, which is then heated and concentrated into molasses. The solid residue is dried to produce orange peel. The tangerine is processed using a 0.25 cm mesh screen.
(2) Fermentation: The prepared tangerine peel and molasses are placed in a container, and yeast is added for fermentation. The optimal temperature for spore growth and mycelium development is 35°C, while the post-fermentation acid production occurs at 30°C. The ideal fermentation time is 4 days, with a humidity level of 50%, and a 2% methanol solution is added to enhance citric acid yield.
(3) Calcium Carbonate Addition: After fermentation, 2% activated carbon is added to adsorb impurities and filter the mixture. Then, calcium carbonate is added to the filtrate while stirring. This causes the formation of insoluble calcium citrate, which precipitates from the broth and is separated by filtration.
(4) Acid Hydrolysis: The calcium citrate is diluted with water to form a paste and heated to 85°C. Sulfuric acid is slowly added based on the amount of calcium carbonate used (92–95% of the input). To determine the endpoint, two test tubes are used. One contains 1 ml of 20% sulfuric acid, and the other has 2 ml of calcium chloride mixed with 1 ml of the filtered acid solution. Both are boiled, cooled, and observed. If no turbidity appears, 1 ml of 95% alcohol is added. If both remain clear, the reaction is complete. If turbidity appears, more sulfuric acid or additional calcium citrate may be needed.
(5) Concentration and Crystallization: The resulting clear solution is filtered and decanted. It is then heated to a concentration of 36.5–37°Bé before being canned. After cooling, citric acid crystals form. The mother liquor is removed using a centrifuge, and the crystals are washed with cold water. They are then dried in a cool place to remove surface moisture.
Important Notes:
(1) Calcium citrate should be treated with an acidic solution promptly to prevent mold and degradation.
(2) Citric acid becomes more corrosive when concentrated, so it is commonly handled in enameled containers. If the concentration is too high, the product may turn into powder; if too low, it can result in large crystal sizes and leftover citric acid in the mother liquor, reducing overall yield.
Author: Liaoning Liaozhong County Chemical Factory