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A kind of production technology of vitamin d3

A production process and vitamin technology, applied in the chemical industry, sustainable manufacturing/processing, climate sustainability, etc., can solve problems such as low product purity, serious environmental pollution, and numerous steps, and achieve improved process conditions and simplified processes Steps, Effects of Improving Purity

Active Publication Date: 2018-08-07
SICHUAN YUXIN PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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. Therefore, in the production process of vitamin D3, reagents such as pyridine and 3,5-dinitrobenzoyl chloride are often used to separate and purify vitamin D through esterification and crystallization. 3 , the steps involved in the esterification crystallization method are numerous, and chemical reagents such as pyridine, 3,5-dinitrobenzoyl chloride or butyryl chloride need to be used for additional reactions, which seriously pollute 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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  • A kind of production technology of vitamin d3

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Experimental program
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Effect test

Embodiment 1

[0027] Add 10kg of 7-dehydrocholesterol and 300L of methanol into the batching tank, start stirring and heat up to 32°C to prepare a photoreaction solution with a concentration of 3wt%, and keep it warm for 1.5 hours. 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 at 65°C, 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. The material was transferred to a refrigerated and stirred tank at -16°C for freezing and crystallization for 10 hours, unreacted raw materials were recovered by filtration, and the filtrate was reacted at 60°C and -0.08Mpa for 2 hours to obtain 1.5 kg of converted oil, which was detected by liquid phase of which vitamin D 3 The content is 80wt%; 1.5 kg of converted oil and 3 times the amount of ethyl acetate are sent in...

Embodiment 2

[0029] Add 15kg of 7-dehydrocholesterol, 350L of methanol and 280L of cyclohexane into the batching tank, start stirring and raise the temperature to 30°C to prepare a photoreaction solution with a concentration of 2wt%, keep it warm for 2 hours, and then pass the photoreaction solution through flow The photochemical reaction is carried out by the ultraviolet irradiator with a light source power of 30kw, the temperature of the photoreaction solution is controlled at 60°C, the flow rate of the photoreaction solution is controlled at 110L / h, and then the irradiated reaction solution is reduced in the concentration pot. Concentrate under pressure, transfer the concentrate to a refrigerated stirring tank and freeze and crystallize at -15°C for 8 hours, filter and recover unreacted raw materials, react the filtrate at 65°C and -0.09Mpa for 1.5 hours to obtain 1.8 kg of transformed oil, transform Vitamin D in oil detected by liquid phase 3 The content is 83wt%; the converted oil and...

Embodiment 3

[0031] Add 12kg of 7-dehydrocholesterol and 260L of ethanol into the batching tank, start stirring and heat up to 35°C to prepare a photoreaction solution with a concentration of 4wt%, keep it warm for 1 hour, and then pass the photoreaction solution through the flowmeter through the nitrogen The ultraviolet irradiator with the light source power of 25kw carries out the photochemical reaction, the temperature of the photoreaction solution is controlled at 70°C, 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 material was transferred to a refrigerated and stirred tank and frozen and crystallized at -20°C for 5 hours, 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 converted oil, which was detected by liquid phase of which vitamin D 3 The cont...

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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 chemical industry, in particular to a kind of vitamin D conforming to the standard of Pharmacopoeia 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, but soluble in solvents such as alcohol, ether, acetone, chloroform, and vegetable oil. Vitamin D 3 It is easy to oxidize and deactivate in humid air, but it can withstand high temperature and oxidation in neutral and alkaline solutions. Therefore, it should be stored in nitrogen, light-free and acid-free cold environment. [0003] Vitamins are found in human and most animal tissues. Human skin contains its precursor dehydrocholesterol, which can be transformed into vitamins under sunlight or ultraviolet radiation. Foods such as cod liver oil, liver, roe, butter, milk, and egg yolk are also r...

Claims

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Application Information

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