Construction of a Citric Acid Production Line with an Annual Output of 10, 000 Tons of Bioreactor Fermentation

The main method of obtaining citric acid today is microbial fermentation, especially the fermentation of Aspergillus niger. Citric acid is an important chemical raw material necessary for the food and chemical industries. In the food industry, citric acid has a refreshing sour taste, is non-toxic, and has high safety. Because citric acid has good solubility and strong chelating power, Therefore, it is widely used in various food processing. In the production of various beverages and sweets, adding an appropriate amount of citric acid can increase the acidity of the food and make the food more refreshing.
In the pharmaceutical industry, acid radicals are often used as synthetic raw materials for certain medicines due to their direct absorption characteristics. Citrates synthesized in medicine, such as sodium citrate, potassium citrate, etc., are widely used in clinical medicine. In the chemical industry, citric acid is an important part of the regulator. It is used in the preparation of buffers, catalysts, and activators. As a chelating agent, sodium citrate can replace sodium tripolyphosphate. It is environmentally friendly and can be used as an important raw material for non-phosphorus washing powder. Many fats and oils contain certain metal ions, which affect the stability of the fats. When producing various edible oils, the presence of metal ions will cause certain harm to the human body.
The world's annual output of citric acid exceeds 2 million tons, 62% is used as food additives, 12% is detergent, 11% is used in medicine and chemical industry, and the proportion of other industries is not small, about 15%. However, the demand for citric acid is increasing rapidly year by year, and it still cannot meet people's increasing material needs. The country with the largest consumption of citric acid is the United States, with an annual demand of nearly 700,000 tons. As a food additive, about 45% of citric acid is used in the beverage industry, while the detergent industry consumes 20%, and 10% is used in medicine and chemicals. The output of citric acid in my country has reached 500,000 tons, and the total export volume of citric acid and citrate is about 400,000 tons, with an average annual export growth of 20% to 30%.
With the development of the world economy and the improvement of people's living standards, the market demand for citric acid is also growing rapidly. Therefore, the citric acid market has great development potential in the world.
 

One: Production plan
This project uses corn as the raw material. After the corn is crushed and adjusted, the corn steep liquor is liquefied by the jet liquefaction process. The liquefied mash is filtered to remove residue to obtain the liquefied clear liquid, and the liquefied clear liquid enters the fermentation section. In the extraction section, this project adopts the domestic advanced "absorption method" to extract citric acid.:
two: technological process
Using corn as the raw material, the finished product is obtained after crushing, slurrying, liquefaction, filtration, fermentation, anion exchange, decolorization, cation exchange, secondary decolorization, evaporation and concentration, crystallization, centrifugal separation, and drying.
Three: Basic steps
1. Raw material pretreatment
After removing impurities, the raw corn is crushed and sieved through 60 mesh to obtain qualified corn flour.
2. Corn flour mixing and liquefaction
Convey corn flour to the mixing tank through the material conveyor; add water at 65°C at a mass ratio (corn flour: water) of 1:4.5, and adjust the slurry pH within the range of 5.0 to 7.0 by using alkaline salt Na2CO3 solution. And add 0.1% calcium chloride as a protectant and activator of amylase. Finally, add powder high temperature resistant α-amylase (enzyme activity 20000U/g, adding amount is 10U/g corn flour), mix evenly, and feed the material into a high-pressure ejector, where the slurry and steam can directly and instantaneously contact. The discharge temperature is 105°C. The liquid material sprayed from the ejector is cooled down to 97°C through the cooling system, and poured into a laminar flow tank for 30 minutes, and the temperature of the heat preservation tank is maintained at 95°C [23-25]. Then perform a secondary injection. In the second ejector, the liquid material and steam are in direct contact to make the temperature rise rapidly to 130°C, and the maintenance in the tank is maintained for about 8 minutes.
Kill high-temperature resistant α-amylase, further coagulate and coagulate protein, filter the bored after treatment, and cool the filtrate through a vacuum flash cooling system, and then pump the liquid material into the secondary liquefaction tank to lower the temperature of the liquid material At 95°C, add high-temperature-resistant α-amylase (enzyme activity of 20000U/g, adding amount of 8U/g corn flour) into the secondary liquefaction tank, liquefy for 30 minutes, and complete the liquefaction after passing the iodine test.
3. Fermentation
The liquefied mash is filtered to remove the corn residue to obtain the liquefied clear liquid. After the temperature is lowered to 37ºC, it is pumped into the fermenter. At the same time, the sterilized 0.9% urea, 0.1% KH3PO4, 0.25% MgSO4 and 10 are added to the fermenter according to the following mass-volume ratio % Seed liquid. The fermentation temperature is controlled at 34°C, pH is about 6.7, and the fermentation cycle is about 72 hours. End of fermentation
Afterwards, the fermentation broth is removed by the vacuum drum filter to remove the mycelium to obtain the fermentation clear liquid. The mycelium is the raw material of high-quality feed, and the fermentation clear liquid enters the extraction and refining section [24-25].
4. Extraction and refining
The fermented liquid passes through 8310# anion exchange adsorption resin to separate citric acid from other impurities (in the exchange process, change the pressure in the adsorption exchange column, adjust the pressure to 4.9×106Pa to vent, repeat 2 to 3 times), and then use 10% NH4OH is freed to get a freeing liquid. Add lye to the liberation solution to adjust the pH 9.0, heat and boil under normal pressure for 10 minutes, take it out, add powdered activated carbon (5g activated carbon/L of the solution), filter to remove organic impurities and some pigments and other residues to obtain a clear liquid [26 -32]. The clear liquid is subjected to cation exchange resin to remove ammonia ions, and then subjected to a second decolorization to obtain 18% citric acid solution. The pure citric acid solution is evaporated and concentrated and then crystallized, and then the mother liquor and crystals are separated by a centrifuge, the mother liquor is returned for adsorption and exchange again, and the crystals are dried to obtain qualified citric acid.
5. Finished product packaging
The dried and qualified citric acid crystals are packaged and transported to the finished product warehouse.
Four: Process characteristics
In this process, corn is used as a raw material, and the corn meal is liquefied and the clear liquid is taken for fermentation. Compared with traditional dried potato raw materials, the original strains can be used to maintain the current fermentation level. Under the condition that the fermentation index remains unchanged, the total yield can be increased by at least 5 percentage points, which promotes the consumption of citric acid. Significant decline. Use corn as  Raw material, corn residue with more than 30% crude protein can be obtained, which can be used as feed additive to produce nutritious feed. 1t corn can produce about 130kg of commercial feed, which can reduce the raw material purchase price of citric acid, which has a great cost advantage over dried potato raw materials. Using corn syrup as raw material for fermentation production can make waste water discharge
The amount is drastically reduced. The amount of waste water produced per ton of acid is reduced from the conventional 30m3-50m3 to 20m3-25m3, and the concentration of organic pollutants is also greatly reduced, from more than 20000mgCOD/L to about 5000mg COD/L, and the color changes from sauce black to yellow . Two consecutive enzymatic injection liquefaction process liquefaction treatment of corn starch. Due to the high protein content of raw corn and the large raw material particles, the continuous jet liquefaction method with two enzyme additions is adopted. The method is to spray high-pressure steam directly into the thin layer of starch slurry, the slurry is heated to the required temperature instantaneously, and after holding for a certain period of time, the gelatinization and liquefaction of corn starch are completed. It can be seen from the production situation that the effect of this method on liquefying corn starch is better, and the protein impurities are condensed together, so that the liquefied liquid has good filterability. At the same time, the equipment is simple and convenient for continuous operation. In the corn liquefaction process, a laminar flow tank is used instead of the traditional heat preservation tank. This requires that the substrate molecule to be acted on has a certain size range to facilitate the formation of this complex with the glucoamylase. In order to ensure that the size of the substrate molecule is within a certain range, the corn slurry must be evenly liquefied. With the traditional liquefaction insulation tank, the liquid material that enters first cannot be guaranteed to go out first, resulting in excessive liquefaction of the advanced material liquid, and incomplete liquefaction of the subsequent material liquid, resulting in uneven liquefaction before and after. For this reason, a one-layer flow tank is designed. This tank is thin and tall. The material liquid is fed tangentially from the upper part to prevent the material liquid from short-circuiting, and the material liquid is discharged from the lower part, thus ensuring that the material liquid is first in, first out, and the final liquefaction is uniform.
Adopt rapid temperature rise to kill enzyme, flash and instantaneous cooling method. During high temperature treatment, the temperature is increased to 120~145ºC by the ejector. The rapid heating produces less "insoluble starch granules" than the gradual heating. The resulting liquefied liquid is transparent and easy to filter, and the starch yield rate is high. At the same time, the rapid heating is adopted. Method, shorten the production cycle. In addition, after spray heating to 120-145°C, keep it in the holding tank for about 5-10 minutes to disperse the formed "insoluble starch granules" under the action of high temperature, and at the same time, the protein is denatured and the protein is further coagulated. Using vacuum flash cooling, the concentration of the liquefied liquid can be increased, and the starch will be further dispersed by using the high pressure difference, and the sugar yield can be increased. During the adsorption exchange process, the adsorbent constantly "jitters", eliminating the need for batch regeneration. Using a weakly basic anion exchanger with large absorption capacity and strong anti-pollution ability, the fermentation broth is directly absorbed without decolorization. At the same time, the pressure in the adsorption exchange column is changed, and the pressure is adjusted to 4.9×106Pa to emptying, repeated 2 to 3 times. This "shake" process can fully agitate the adsorption exchange resin, so there is no need to regenerate the resin in batches after the rubber washing process like the separation method, which reduces the consumption of water, acid, and alkali. Adjust the pH of the release solution to improve the effect of separating impurities. Alkali is added to the liberation liquid flowing out of the anion exchange resin. Adjusting the pH to 8-10 can destroy the colloidal stability of the citric acid solution, thereby flocculating and separating a small amount of soluble proteins, sugars, colloids, miscellaneous acids and other impurities from the solution. The "absorption method" [33-36] adopts the alkali-free method to avoid the disadvantages of the original acid-free method that the reducing sugars are too high and the easy-to-carbon compounds are not up to standard. Compared with the traditional calcium salt method, the extraction yield has increased from about 75% to
80%, improved product quality and reduced production costs. Compared with the original "calcium salt method", the "absorption method" increases the benefit by 1,000 yuan/ton of citric acid. The production realizes automatic program control and eliminates the production waste residue. CaSO4 generates only a small amount of waste water, which saves energy and is beneficial to environmental protection

                                     List of main equipment of a citric acid plant with an annual output of 10,000 tons

Fuzhou FUL Fluid Equipment & Pharmaceutical Co., Ltd is a comprehensive enterprise which integrates R & D, production and construction of pharmaceutical production equipments, development and transfer of biotechnology, and cooperative production and sales of drugs and vaccines. The self-developed pharmaceutical production equipment branded FUL has been put into operation in many well-known pharmaceutical enterprises such as SINOPHARM, CSPC and also cooperates with many well-known pharmaceutical enterprises in production and sales, including pharmaceutical intermediates, APIs and finished drug preparations.

Fuzhou FUL Fluid Equipment & Pharmaceutical Co., Ltd business radiates to all levels, including direct supply cooperation with government departments and industry representatives, as well as establishing supply cooperation relationship with retail industry. We supply high quality, safe and effective medicines and medical equipment to governments, hospitals, clinics and licensed pharmacies in different countries with timely and effective services at reasonable prices.

At present Fuzhou FUL Fluid Equipment & Pharmaceutical Co., Ltd has the SINOPHARM authorization to sell its intermediates and APIs,and has the authorizations of CSPC & HUABEI PHARM sell its finished drug preparations;then FUL is the only manufacture in China which can supply the complete service from pharmaceutical produciton lines,intermediates and APIs to finished drug preparations and vaccines.Then we are seeking the professional pharmaceutical enterprices to work together for further cooperations.

 

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