Method for synthesizing vitamin D3 in segmented and fixed spectrum band manner
A vitamin and spectral band technology, applied in the field of photoreaction, can solve the problems of prone to conformational inversion, low yield, low purity and content, etc., to improve the conversion rate of raw materials and product quality, and improve the dissolved concentration of substrates. Effect
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Embodiment 1
[0018] (1) Dissolution of 7-dehydrocholesterol
[0019] In the batching kettle, add 237.5kg methanol, 712.5kg n-hexane, add 50kg 7-dehydrocholesterol (content: 96%) under stirring, add 1kg 2,6-tert-butyl p-cresol, stir and heat up to 30°C , to dissolve it;
[0020] (2) First-level fixed-band illumination
[0021] Firstly, pass the first-level fixed-band ultraviolet lamp (the light source is a 10KW LED lamp, wavelength: 290nm) through nitrogen for 30 minutes, turn it on, and preheat it for 30 minutes. Then filter the solution in step (1), pass it through a rotameter and a temperature control device, and pass it into a first-order fixed-spectrum band ultraviolet lamp to control the material flow rate to 400L / hr, control the material inlet temperature to 32°C, and the outlet temperature to 18°C. ℃;
[0022] (3) Second-level fixed-band illumination
[0023] First, pass nitrogen gas through the secondary fixed-band ultraviolet lamp (15KW LED lamp, wavelength: 250nm) for 25 minu...
Embodiment 2
[0027] (1) Dissolution of 7-dehydrocholesterol
[0028] In the batching kettle, add 135.7kg isopropanol, 542.8kg isoheptane, add 50kg 7-dehydrocholesterol (content: 97%) under stirring, add 0.5kg 2,6-tert-butyl p-methylphenol, stir Raise the temperature to 28°C to dissolve it;
[0029] (2) First-level fixed-band illumination
[0030] First pass the first-level fixed-spectrum ultraviolet lamp (the light source is an 8KW LED lamp, wavelength: 300nm) through nitrogen for 25 minutes, turn it on, and preheat it for 20 minutes, then filter the solution in step (1), and pass it through the rotameter and The temperature control device is connected to a first-level fixed-spectrum band ultraviolet lamp to control the material flow rate to 500L / hr, and to control the material inlet temperature to 33°C and the outlet temperature to 20°C;
[0031] (3) Second-level fixed-band illumination
[0032] First, pass the nitrogen gas through the secondary fixed-spectrum ultraviolet lamp (18KW LE...
Embodiment 3
[0036] (1) Dissolution of 7-dehydrocholesterol
[0037] In the batching kettle, add 127.2kg of absolute ethanol, 763.4kg of isopentane, add 75kg of 7-dehydrocholesterol (content: 98%) under stirring, add 2,6-tert-butyl-p-methoxyphenol, stir and heat up to 32°C to make it dissolve;
[0038] (2) First-level fixed-band illumination
[0039] First pass the first-level fixed-spectrum ultraviolet lamp (15KW LED lamp, wavelength: 320nm) with nitrogen gas for 28 minutes, turn it on, and preheat it for 25 minutes, then filter the solution in step (1), and pass it through the rotameter and The temperature control device is connected to a first-level fixed-spectrum band ultraviolet lamp to control the material flow rate to 420L / hr, and to control the material inlet temperature to 29°C and the outlet temperature to 18°C;
[0040] (3) Second-level fixed-band illumination
[0041] First pass the nitrogen gas through the secondary fixed-spectrum ultraviolet lamp (the light source is a 15K...
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