Novel method for synthesizing high-purity cetyl pyridinium chloride
A high-purity technology of cetylpyridinium chloride, which is applied in the field of synthesizing high-purity cetylpyridinium chloride, can solve cumbersome problems and achieve the effect of good quality, stable quality and simple process
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Embodiment 1
[0034] In the reactor connected with stirring device, heating device and reflux device, add 130 kg of acetone, 26.09 kg of hexadecane chloride, and 7.91 kg of pyridine, and start to heat and reflux, and white spots appear in the reaction system within 10 minutes to several hours. Crystallized, continued to react for 12 hours, then cooled to room temperature, filtered, and the white filter cake was washed with 13 kg of acetone. After the filter cake is dried in a blast drying oven or vacuum-dried, 26kg of finished product cetylpyridinium chloride is obtained. Analytical purity >99.5% (HPLC, area normalized method).
[0035] The combined filtrate was transferred back to the reactor, 26.09 kg of hexadecane chloride and 7.91 kg of pyridine were added, and heating and reflux was started, and the reaction was continued for 12 hours, then cooled to room temperature, filtered, and the white filter cake was washed with 13 kg of acetone. After the filter cake is dried in a blast oven o...
Embodiment 2
[0037] On the basis of Example 1, the mother liquor was applied mechanically five to six times. During the process, the molar yield of the single-pass reaction gradually increased to nearly 100%, while the purity of the product was maintained above 99%.
[0038] After applying the mother solution 6 times, it started to turn red. No longer apply mechanically, the remaining mother liquor is returned to the reaction tank, most of the solvent acetone is distilled off, the volume of the reaction solution is concentrated to 1 / 4 of the original volume, and then the stirring reaction is continued at reflux temperature for 18 to 24 hours, filtered, and used 13Kg Acetone washing, can get cetylpyridinium chloride product 33Kg again. The purity by HPLC analysis is about 99%.
[0039] The remaining mother liquor can continue to be concentrated by distillation to separate out more cetylpyridinium chloride products, but its analytical purity is lower than 99%. It can be used in environment...
Embodiment 3
[0047] In the reactor connected with a stirring device, a heating device and a reflux device, add 100 kg of ethyl acetate, 26.09 kg of hexadecane chloride, and 7.91 kg of pyridine, raise the temperature to 50 ° C, and maintain the reaction at 50 ± 5 ° C for 48 hours, then Cool down to room temperature, filter, and wash the white filter cake with 10 kg of ethyl acetate. After the filter cake is dried in a blast oven or vacuum-dried, 29kg of finished product cetylpyridinium chloride is obtained. Analytical purity >99.7% (HPLC, area normalized method).
[0048] The rest of the operations are the same as in Example 1 and Example 2. After appropriately lowering the reaction temperature and prolonging the reaction time, the crystal form of the product is better and the purity is slightly improved.
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Abstract
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