Method for preparation of high purity and high yield metformin hydrochloride by two-component solvent
A high-purity metformin hydrochloride technology, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve problems such as long reaction time, side reactions, and poor fluidity, and achieve shortened crystallization process time, The effect of ensuring crystal particle distribution and improving production safety
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Embodiment 1
[0051] A method for preparing metformin hydrochloride with high purity and high yield by a two-component solvent, comprising the following steps:
[0052] (1) Preparation of dimethylamine hydrochloride
[0053] 1. Add part of hydrochloric acid and dimethylamine gas
[0054] Measure 920kg of hydrochloric acid with a concentration of 31% into the head tank, then put 560Kg of hydrochloric acid in the head tank into the salt-forming reaction kettle first, start stirring, and feed frozen brine into the jacket of the reaction kettle, and wait until the temperature of the kettle drops to 10 ℃, feed frozen brine to the shell side of the cooler, start feeding dimethylamine gas into the salt-forming reactor, adjust the feeding speed of dimethylamine gas, the amount of dimethylamine gas added is about 200Kg, and keep the temperature of the kettle at 20°C.
[0055] 2. The material enters the vent pipe
[0056] Turn on the circulation pump, and open the valve leading to the high end of t...
Embodiment 2
[0094] Through test, adopt the step of embodiment 1, adopt following process parameter:
[0095] (1) Preparation of dimethylamine hydrochloride
[0096] 1. Add part of hydrochloric acid and dimethylamine gas
[0097] Measure 31% hydrochloric acid into the high-level tank, put about 60% of the total amount of hydrochloric acid into the salt-forming reactor first, start stirring, feed frozen brine into the jacket of the reactor, wait until the temperature of the kettle drops to 10-20°C, Feed frozen brine into the shell side of the cooler, and start feeding dimethylamine gas into the salt-forming reaction kettle. The amount of dimethylamine gas added is about two-thirds of the total amount, and the feeding speed of dimethylamine gas is adjusted to keep the temperature of the kettle at 15 ~25°C.
[0098] Dimethylamine: 31% industrial hydrochloric acid (weight ratio) = 1: 2.75 to 2.98.
[0099] 2. The material enters the vent pipe
[0100] Turn on the circulation pump, and ope...
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