Background and Overview
Food-grade fumaric acid is a pure souring agent with pure taste. It is used as souring agent in drinks, wine, cakes and pickles, etc. It also acts as food preservative, antioxidant and PH regulator. Fumaric acid is an important basic chemical raw material and fine chemical products, widely used in coating, resin, medicine, plasticizer and other fields. It can be used in industry to produce unsaturated resin and alkyd resin, and as a raw material for producing electrophoretic paint.
The preparation of
Reported 1,
(1) Catalytic reaction: maleic acid wastewater with a mass fraction of 100 was added with a mass fraction of 5.5~6 thiourea catalyst, and stirred for 12h at room temperature to obtain crude fumarate; The catalytic reaction is carried out in the isomerism reaction kettle, the isomerism reaction kettle is cylindrical reaction kettle, the volume is 10~12 cubic meters, 10 cubic meters is used in this embodiment;
(2) washing, take crude fumaric acid, wash with distilled water, and then add distilled water, heat to 95~100℃ to dissolve, then add activated carbon decolorization, get pure fumaric acid; In the washing step, the crude fumaric acid is washed with distilled water and sent into a centrifuge for centrifuge separation, and then the crude fumaric acid after washing is added to the distilled water treatment; The washing wastewater produced after fumaric acid crude product is washed with distilled water is used as circulating cooling water to continue to be put into the production process.
(3) Purification reaction, take a certain amount of pure fumaric acid, wash it with distilled water, then add activated activated carbon, decolorization reflux reaction 2h, get food grade fumaric acid; In this purification reaction, after decolorization reflux reaction, the material is sent to a continuous crystallizer for crystallization, and the temperature is controlled below 25℃. The crystallized fumaric acid was sent into a centrifuge for centrifuge and dried at low temperature to obtain food-grade fumaric acid.
Reported 2,
The invention relates to a method for preparing fumaric acid fermentation liquid by fermentation, and the technological steps are as follows:
(1) Selection of strain: Rhizopus Oryzae CICC40506 was selected.
(2) Culture medium preparation:
Medium Components Seed medium (g/L)
Glucose 10 to 30, 40 to 120
Potassium dihydrogen phosphate 0.6~1.0 0.6~1.0
Ammonium sulfate is 1.0 ~ 3.0
Magnesium sulfate 0.5~0.6 0.5~0.6
Zinc sulfate 0.1~0.15 0.1~0.15
Ferrous sulfate 0.0088~0.01 0.0088~0.01
Urea is 0.1 ~ 0.3
Calcium carbonate 40 ~ 50
(3) Seed culture: 500ml triangular flask, liquid volume (seed medium) of 50~100ml, culture temperature of 30~35℃, spore strain inoculation amount of 1.0~8.0×107/100 mL seed solution, shaking speed of 180~220RPm, culture for 12h, this is the first grade seed solution. The primary seed solution was inoculated in a new sterile medium with 10% inoculation amount for 12h, which was the secondary seed solution. Similarly, the secondary seed solution was inoculated in a new sterile medium with 10% inoculation amount for 12-16h, which was the tertiary seed solution. The secondary and tertiary seed media and their technological parameters were cultured in the same primary seed solution.
(4) Fermentation culture: A 300L fermentator was used with 250L of liquid (fermentation medium), and the seed liquid was inserted into the fermentation medium at a volume ratio of 10%. The strategy of intermittent air ventilation was adopted in the whole fermentation process with different time periods. The ventilation volume was maintained at 1.0-1.2 VVM for the first 24 hours and 0.5-0.6 VVM for 24-36 hours. The ventilation rate was 0 VVM for 36 to 48 hours, 0.5 to 0.6 VVM for 48 to 60 hours, 1.0 to 1.2 VVM for 60 to 72 hours, and 1.0 to 1.2 VVM for 72 hours. The fermentation temperature was controlled within the range of 30 to 35℃, and the stirring speed was 150 RPm. Sterile glucose solution was added to maintain the glucose concentration of 20-30g /L in the ferment tank. The fermentation lasted for 100h, and fumaric acid fermentation liquid was obtained. The fumaric acid concentration in the fermentation broth is ≥40 g/L.
Reported 3,
CN200810243712.0 reported a separation and purification method of phthalic acid water and fumaric acid production process, the phthalic acid water was cooled and stood before solid-liquid separation, and then the solid-liquid separation clarification solution was put into the series decolorization system and purification system under the condition of 0~40℃, and pure butenic acid solution was separated. The purification system was regenerated with the regenerating agent, and the pH value of the regenerating agent was lowered. The separated butenic acid solution was driven into a conversion reaction kettle and catalyst was added. The solution was heated at 40~150℃ for 0.1~10h and cooled to 0~50℃. Fumaric acid was obtained after solid-liquid separation and washing and drying. The invention not only obtains high quality butenedioic acid solution, but also produces organic by-products such as phthalic acid with high yield, removes impurities such as pigment, reduces downstream wastewater treatment load, and achieves the effect of food-grade fumaric acid in one conversion crystallization.
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