Preparation of cyclohexanyl calcium sulfamate
A technology of calcium cyclamate and cyclohexylamine, which is applied in the field of preparation of calcium cyclamate, can solve problems such as production gaps, and achieve the effects of easy-to-obtain raw materials, high yield, and good water solubility
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Embodiment 1
[0023] Add cyclohexylamine and sulfonine into the reactor, and control the pH value of the material to 6.8, the temperature is 75° C., and react for 4 hours. The resulting mixture was heated with steam at 90°C and concentrated in vacuo for 10 hours. Add cyclohexylamine, and react for 52 hours while heating with steam to form a semi-finished product, and the heating temperature is 142°C. The remaining cyclohexylamine is recovered at around 100°C for reuse. Calcium hydroxide and water were then added to the remaining mixture, and reacted at 100° C. for 45 hours to obtain a product mixture. Add activated carbon for decolorization, remove impurities, and adjust the pH, control the pH at about 9, and keep the temperature at 50-55°C for 5 hours. Then, the obtained mixture was filtered until the transparency of the filtrate reached more than 98%. The resulting filtrate was crystallized by concentration in vacuo at about 55°C for 32 hours. The calcium cyclamate product is then sep...
Embodiment 2
[0025] Add cyclohexylamine and sulfonine into the reactor, and control the pH value of the material to 7.2, the temperature is 75° C., and react for 4 hours. The resulting mixture was heated with steam at 110°C and concentrated in vacuo for 8 hours. Add cyclohexylamine, and react for 55 hours while heating with steam to form a semi-finished product, and the heating temperature is 135°C. The remaining cyclohexylamine is recovered at around 100°C for reuse. Calcium hydroxide and water were then added to the remaining mixture, and reacted at 120° C. for 40 hours to obtain a product mixture. Add activated carbon for decolorization, remove impurities, and adjust the pH, control the pH at about 10, and keep the temperature at 50-55°C for 5 hours. Then, the obtained mixture was filtered until the transparency of the filtrate reached more than 98%. The resulting filtrate was crystallized by concentration under vacuum at about 60°C for 30 hours. The calcium cyclamate product is the...
Embodiment 3
[0027] Add cyclohexylamine and sulfonine into the reactor, and control the pH value of the material to 7.0, the temperature is 65° C., and react for 4 hours. The resulting mixture was heated with steam at 100°C and concentrated in vacuo for 9 hours. Add cyclohexylamine, and react for 53 hours while heating with steam to form a semi-finished product, and the heating temperature is 140°C. The remaining cyclohexylamine is recovered at around 100°C for reuse. Calcium hydroxide and water were then added to the remaining mixture, and reacted at 110° C. for 42 hours to obtain a product mixture. Add activated carbon for decolorization, remove impurities, and adjust the pH, control the pH at about 9.5, and keep the temperature at 52°C for 5 hours. Then, the obtained mixture was filtered until the transparency of the filtrate reached more than 98%. The resulting filtrate was crystallized by concentration in vacuo at about 58°C for 31 hours. The calcium cyclamate product is then sepa...
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Abstract
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