Method for recovering fumaric acid from tiamulin production mother solution
A technology of tiamulin and fumaric acid, which is applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, water/sludge/sewage treatment, etc., can solve the problem of increasing the production cost of tiamulin. Wastewater treatment load, waste of resources and other issues, to achieve the effect of saving treatment costs, reducing production costs, and high recovery rate
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Embodiment 1
[0026] Put 500ml of Taimiao salt mother liquor whose content has been detected in a 1000ml reaction bottle (the content of fumaric acid is 7.1%, the content of tiamiaoline is 5%, remove methanol under the pressure of -0.08Mpa, add 320ml of water and 160ml of butyl acetate , add about 120ml of 40% NaOH to adjust the pH>10, stir for 10min, and let stand to separate layers. The oil layer is recovered and treated separately. The water layer is adjusted to PH at 1-2 with 15% sulfuric acid, stirred for 30min, and filtered after fumaric acid is completely precipitated. Wash the fumaric acid crystals with dilute sulfuric acid, and then dry the crystals to obtain 30 g of fumaric acid with a purity of 98.1% and a yield of 82.6%.
Embodiment 2
[0028] Put 500ml of Taimiao salt mother liquor with detected content in a 1000ml reaction bottle (the content of fumaric acid is 8%, the content of tiamiaoline is 5.5%, remove methanol under the pressure of -0.08Mpa, add 400ml of water and 200mlMIBK, add about 150ml of 40% NaOH to adjust the pH to > 10, stir for 30 minutes, and let stand to separate layers. The oil layer is recovered and treated separately. The water layer is adjusted to a pH of 1-2 with 15% hydrochloric acid, and stirred for 30 minutes. After all the fumaric acid is precipitated, filter and wash with dilute hydrochloric acid Fumaric acid crystals were then dried to obtain 33 g of fumaric acid with a purity of 99.2% and a yield of 81.1%.
Embodiment 3
[0030] Put 500ml of Taimiao salt mother liquor with detected content in a 1000ml reaction bottle (the content of fumaric acid is 6.2%, the content of tiamiaoline is 4.5%, remove methanol under the pressure of -0.08Mpa, add 280ml of water and 350mlMIBK, add about 105ml of 40% NaOH to adjust the pH to > 10, stir for 30 minutes, and let stand to separate layers. The oil layer is recovered and treated separately. The water layer is adjusted to a pH of 1-2 with 15% hydrochloric acid, stirred for 30 minutes, and after fumaric acid is completely precipitated, filter and wash with dilute hydrochloric acid Fumaric acid crystals were then dried to obtain 27g of fumaric acid with a purity of 98.9% and a yield of 86.1%.
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