Method for recovering acetylisovaleryltylosin tartrate from acetylisovaleryltylosin tartrate crystallization mother liquor
A technology of acetylisovaleryl tylosine tartrate and acetylisovaleryl tartrate, which is applied in the field of medicine and chemical industry, and can solve the problem that acetylisovaleryl tylosin tartrate is not heat and acid resistant, and the content of tylosin is low. , difficulties in mother liquor recovery, etc., to achieve the effect of reducing the content of pollutants, increasing the available resources, and improving the recovery rate of finished products
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Embodiment 1
[0017] 30 tons of acetylisovaleryl tylosin tartrate production, a single batch of crystallization mother liquor 55m 3 , as detected by HPLC method, the crystallization mother liquor contains 126㎎ / L acetylisovaleryl tylosin, and a large amount of impurities such as pigment, sodium ion, citrate ion, etc.
[0018] Into the mother liquor according to 8g / m 3 Add the alkylbenzene sulfonate at a certain ratio, stir at 20°C for 20 minutes, enter the air bubbler for foaming, and pump the bubble liquid film into the separation tank through the negative pressure siphon. Cool down to 5°C in the separation tank and the liquid film will break naturally, according to 200g / m 3 The proportion of polyferric sulfate (PFS) is added, and at the same time according to 13g / m 3 The proportion of polyacrylamide was added, stirred for 20 minutes, and centrifugally filtered with a centrifuge to obtain a concentrated solution of 600L. According to HPLC detection, the concentrated solution contains 110...
Embodiment 2
[0020] Production of 30 tons of acetylisovaleryl tylosin tartrate, 46m of secondary crystallization mother liquor produced in a single batch 3 , as detected by HPLC method, the crystallization mother liquor contains 52 ㎎ / L acetylisovaleryl tylosin, as well as impurities such as sodium ions and tartrate ions.
[0021] Into the mother liquor according to 10g / m 3 Add α-olefin sulfonate in the ratio of 20°C and stir for 20 minutes, enter the air bubbler for foaming, and pump the bubble liquid film into the separation tank through the negative pressure siphon. Cool down to 10°C in the separation tank and the liquid film will break naturally, according to 200g / m 3 Add a 1:3 mixture of polyalumina and polyferric sulfate (PAC:PFS=1:3) at a ratio of 12g / m 3 The proportion of polyacrylamide was added, stirred for 20 minutes, and centrifugally filtered with a centrifuge to obtain a concentrated solution of 260L. According to HPLC detection, the concentrated solution contains 9096 mg / L...
Embodiment 3
[0023] Production of 600kg grade acetylisovaleryl tylosin tartrate, 9.2m of secondary crystallization mother liquor produced in a single batch 3 According to HPLC detection, the crystallization mother liquor contains 66㎎ / L acetylisovaleryl tylosin, and impurities such as sodium ions, tartrate ions, citrate ions, etc.
[0024] Into the mother liquor according to 9g / m 3 Add α-olefin sulfonate surfactant in the ratio of 22°C and stir for 20 minutes. The mixed solution enters the air foamer for foaming, and the bubble liquid film is pumped into the separation tank through the negative pressure siphon. Cool down to 10-15°C in the separation tank and the liquid film will break naturally, at a rate of 200g / m 3 Add the 3:1 mixture of ferric chloride and aluminum sulfate (ferric chloride: aluminum sulfate = 3:1), and at the same time, according to 15g / m 3 The proportion of polyacrylamide was added, stirred for 20 minutes, and centrifugally filtered with a centrifuge to obtain 60L of ...
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