A kind of preparation method of lysine acetate bulk drug
A technology of lysine acetate and lysine hydrochloride, which is applied in the field of amino acid preparation, can solve the problems of insufficient environmental protection of ammonia gas, high energy consumption of ammonia, and environmental pollution, and facilitate industrial scale-up, reduce water consumption, and shorten concentration time Effect
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Embodiment 1
[0042] The preparation of embodiment 1 lysine acetate
[0043] (1) After dissolving 10kg of lysine hydrochloride in water, the diluted solubility is 20% (g / 100ml water). The aqueous solution of lysine hydrochloride is electrodialyzed with a special heterogeneous metal film (EPL4016C of Hangzhou Lanran Environmental Technology Co., Ltd. ) Dechlorination, the volume of the clear solution after dechlorination is twice the volume of the concentrated solution, the conductivity of the clear solution after dechlorination is ≤400μs / cm, and the yield is ≥99%;
[0044] (2) Add the concentrated lysine solution into a 100L reaction kettle, add glacial acetic acid with the same number of moles as lysine, adjust the pH value to 7.0, and react at 70-80°C for 2 hours to obtain a lysine acetate solution ;
[0045] (3) Regulate the pH of the lysine acetate aqueous solution to be 4.0 to obtain the lysine acetate feed liquid;
[0046] (4) Ammonium acetate is first added to the lysine acetate fe...
Embodiment 2
[0051] The preparation of embodiment 2 lysine acetate
[0052](1) After lysine hydrochloride 10kg is dissolved in water, the solubility after dilution is 20%. The aqueous solution of lysine hydrochloride is dechlorinated by electrodialysis special heterogeneous metal membrane. 2 times, the clear night conductivity after dechlorination is ≤350μs / cm, and the yield is ≥98%;
[0053] (2) Add the lysine solution into a 100L reaction kettle, add glacial acetic acid with 1.1 times the molar number of lysine, and adjust the pH value to 7.0, and react at 70-80°C for 2 hours to obtain a lysine acetate solution;
[0054] (3) Regulate the pH of the lysine acetate aqueous solution to be 3.0 to obtain the lysine acetate feed liquid;
[0055] (4) Ammonium acetate is first added in the lysine acetate feed solution, so that the mass ratio of the inorganic salt to the final concentration is 20%, and then ethanol is added so that the mass ratio of the organic solvent to the final concentration ...
Embodiment 3
[0060] The preparation of embodiment 3 lysine acetate
[0061] (1) After lysine hydrochloride 10kg is dissolved in water, the solubility after dilution is 20%. The lysine hydrochloride aqueous solution is dechlorinated by electrodialysis special heterogeneous metal membrane. The clear volume after dechlorination is 2% of the dope volume times, the clear night conductivity after dechlorination is ≤300μs / cm, and the yield is ≥97%;
[0062] (2) Add the lysine solution into a 100L reaction kettle, add glacial acetic acid with 1.2 times the molar number of lysine, and adjust the pH value to 7.0, and react at 70-80°C for 2 hours to obtain a lysine acetate solution;
[0063] (3) Regulate the pH of the lysine acetate aqueous solution to be 5.0 to obtain the lysine acetate feed liquid;
[0064] (4) Ammonium acetate is first added in the lysine acetate feed solution, so that the mass ratio of the inorganic salt to the final concentration is 20%, and then ethanol is added so that the ma...
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