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Vitamin D3 production process

A production process, vitamin technology, applied in the direction of sustainable manufacturing/processing, chemical industry, climate sustainability, etc., can solve the problems of low product purity, serious environmental pollution, inability to react, etc., to improve process conditions and simplify processes Steps, the effect of reducing occupational health hazards

Active Publication Date: 2017-03-08
SICHUAN YUXIN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the removal of 7-dehydrocholesterol in the light reaction to generate pre-vitamin D 3 In addition, it is very easy to generate toxic by-product tachysterol, so pyridine and 3,5-dinitrobenzoyl chloride and other reagents are often used in the production process of vitamin D3 to separate and purify vitamin D through esterification and crystallization. 3 , the steps involved in the esterification crystallization method are numerous, need to use chemical reagents such as pyridine, 3,5-dinitrobenzoyl chloride or butyryl chloride and other reagents to carry out additional reactions, which seriously pollutes the environment and cannot be completely reacted, and the purity of the obtained product is not high. high and low yield

Method used

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  • Vitamin D3 production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 10 kg of 7-dehydrocholesterol and 300 L of methanol were added to the batching tank, the temperature was raised to 32° C. with stirring, and a photoreaction solution with a concentration of 3wt% was prepared. The photochemical reaction is carried out by an ultraviolet irradiator with a light source power of 20kw, the temperature of the photoreaction solution is controlled to be 65°C, and the flow rate of the photoreaction solution is controlled at 120L / h, and then the irradiated reaction solution is concentrated under reduced pressure in a concentration pot, and the concentrated The filtrate was transferred to a refrigerated stirring tank at -16°C for freezing and crystallization for 10h, and the unreacted raw materials were recovered by filtration. The filtrate was reacted at 60°C and -0.08Mpa for 2 hours to obtain 1.5 kg of converted oil. The converted oil was detected by liquid phase. of which vitamin D 3 The content is 80wt%; 1.5 kilograms of transformed oil and 3 t...

Embodiment 2

[0029] 15 kg of 7-dehydrocholesterol, 350 L of methanol and 280 L of cyclohexane were added to the batching tank, the stirring was turned on and the temperature was raised to 30° C. to prepare a light reaction solution with a concentration of 2 wt %, and the light reaction solution was incubated for 2 hours. The photochemical reaction is carried out by an ultraviolet irradiator with a light source power of 30kw that is passing through nitrogen, the temperature of the photoreaction solution is controlled to 60°C, and the flow rate of the photoreaction solution is controlled to 110L / h, and then the irradiated reaction solution is reduced in the concentration pot. Pressure and concentration, transfer the concentrate into a refrigerated stirring tank and freeze and crystallize at -15°C for 8h, filter and recover unreacted raw materials, and react the filtrate at 65°C and -0.09Mpa for 1.5 hours to obtain 1.8 kg of transformed oil. Oil tested by liquid phase for vitamin D 3 The cont...

Embodiment 3

[0031] 12 kg of 7-dehydrocholesterol and 260 L of ethanol were added to the batching tank, the temperature was raised to 35° C. with stirring, and a photoreaction solution with a concentration of 4wt% was prepared. The photochemical reaction is carried out by an ultraviolet irradiator with a light source power of 25kw, the temperature of the photoreaction solution is controlled to be 70°C, and the flow rate of the photoreaction solution is controlled at 130L / h, and then the irradiated reaction solution is concentrated under reduced pressure in a concentration pot, and the concentrated The filtrate was transferred to a refrigerated stirring tank at -20°C for freezing and crystallization for 5h, the unreacted raw materials were recovered by filtration, and the filtrate was reacted at 70°C and -0.095Mpa for 1 hour to obtain 1.68 kg of transformed oil, which was detected by liquid phase. of which vitamin D 3 The content of ethyl acetate is 83wt%; the conversion oil and 2 times the...

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Abstract

The invention discloses a vitamin D3 production process, which comprises: S1, light irradiation and thermal isomerization reaction; S2, chromatography elution separation; S3, refrigeration crystallization separation; and S4, drying mixing sub-packing. Compared to the process in the prior art, the process of the present invention has the following characteristics that the synthesis process conditions are improved, such that the productivity of the process is improved, and the total yield of the product is more than 90%; the thermal isomerization reaction of the vitamin D3 and the pressure reducing concentration are combined so as to simplify the process steps and save the process energy consumption; the synthesis reaction zone and the purification separation zone are completely separated so as to easily perform process maintenance and process management; in the purification process, the chromatography crystallization method is directly used to replace the original process of chromatography, esterification and hydrolysis crystallization, such that the use of the toxic organic reagent is avoided, and the effects of energy saving, consumption reducing and environmental protection are achieved; and the tail oil tailings generated during the vitamin D3 series production process can be adopted as the feed additive resource so as to be used.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a vitamin D that meets pharmacopoeia standards 3 production process. Background technique [0002] Vitamin D 3 (Vitamin D 3 ), also known as cholecalciferol, is a colorless crystal with a melting point of 84-85 °C. It is a fat-soluble substance, insoluble in water, soluble in alcohol, ether, acetone, chloroform, vegetable oil and other solvents. Vitamin D 3 It is easy to be oxidized and deactivated in humid air, and can withstand high temperature and oxidation in neutral and alkaline solutions. Therefore, it should be stored in a cold environment with nitrogen, no light and no acid. [0003] Vitamins are found in human and most animal tissues. Human skin contains its precursor dehydrocholesterol, which can be converted into vitamins under sunlight or ultraviolet irradiation. Foods such as cod liver oil, liver, roe, butter, milk, and egg yolk are also rich in vitamins. Vitamin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C401/00
CPCC07C401/00Y02P20/10
Inventor 冷莉
Owner SICHUAN YUXIN PHARM CO LTD
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