Ultrasonic-assisted coenzyme Q10 crystallizing method

An ultrasound and coenzyme technology, applied in organic chemistry, quinone separation/purification, etc., can solve the problems of small number of crystal seeds, no description of product crystal shape indicators, and insufficient elimination of explosive nucleation, etc., to achieve uniform distribution, easy filtration and The effect of shortening the drying and crystallization time

Active Publication Date: 2015-03-11
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is simple to operate, but the number of seed crystals is small, which is not enough to eliminate explosive nucleation, and there is no description of the crystal form index of the product

Method used

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  • Ultrasonic-assisted coenzyme Q10 crystallizing method
  • Ultrasonic-assisted coenzyme Q10 crystallizing method
  • Ultrasonic-assisted coenzyme Q10 crystallizing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Take 95% pure coenzyme Q 10 200g of the crude product and 600g of isopropanol were stirred and heated to 60°C under the protection of nitrogen and protected from light to form a uniform solution. Then cooling crystallization was carried out, and the temperature of the solution was lowered to 38° C. at a cooling rate of 20° C. / hour. At this time, 30kHz 800W (1000W / kg solution) ultrasonic waves were used to assist crystallization for 10 minutes, and then the temperature was lowered to 20°C at a rate of 10°C / hour. After filtering, washing with 95% ethanol and drying, the coenzyme Q 10 The crystal product is 173.01g, the yield is 91.0%, the purity is 99.2%, and the main particle size is 80.2μm. The product has large particle size, good fluidity, no agglomeration phenomenon, and is easy to use.

Embodiment 2

[0024] Take 90% pure coenzyme Q 10 150 g of the crude product, 600 g of 95% ethanol, stirred and heated to 55° C. under the protection of nitrogen and protected from light, completely dissolved to form a uniform solution. Then cooling crystallization was carried out, and the temperature of the solution was lowered to 36° C. at a cooling rate of 10° C. / hour. At this time, 20kHz 150W (200W / kg solution) ultrasonic waves were used for 30 seconds to assist crystallization for 5 minutes, and then the temperature of the solution was lowered to 13° C. at a cooling rate of 8° C. / hour. After filtering, washing with n-propanol and drying, the coenzyme Q 10 The crystal product is 124.68g, the yield is 92.3%, the purity is 99.6%, and the main particle size is 62.7μm. The product has large particle size, good fluidity, no agglomeration phenomenon, and is easy to use.

Embodiment 3

[0026] Take 92% pure coenzyme Q 10 200g of the crude product and 500g of ethyl acetate were stirred and heated to 60°C under the protection of nitrogen and protected from light to form a uniform solution. Then cooling crystallization was carried out, and the temperature of the solution was lowered to 40° C. at a cooling rate of 15° C. / hour. At this time, 40kHz 350W (500W / kg solution) ultrasonic waves were used for 15 seconds to assist crystallization for 20 minutes, and then the temperature of the solution was lowered to 15° C. at a cooling rate of 15° C. / hour and maintained for 1 hour. After filtering, washing with absolute ethanol and drying, the coenzyme Q 10 The crystal product is 171.02g, the yield is 92.9%, the purity is 99.3%, and the main particle size is 55.3μm. The product has large particle size, good fluidity, no agglomeration phenomenon, and is easy to use.

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Abstract

The invention relates to an ultrasonic-assisted coenzyme Q10 crystallizing method which comprises following steps: adding coenzyme Q10 with a purity being 90-95% to an organic solvent, wherein a mass ratio of the raw material to the organic solvent is 20-40:100; stirring the mixture and increasing the temperature to 50-60 DEG C for completely dissolving the coenzyme Q10 to form a uniform solution; performing a cooling crystallization process; decreasing the temperature of the solution to 36-40 DEG C with the ultrasonic-assisted crystallization being carried out for 5-20 min; decreasing the temperature of the solution to 13-20 DEG C; and performing filtration, a washing operation and a drying operating to obtain a coenzyme Q10 crystal product. The method is short in crystallization time. The coenzyme Q10 crystal product has a large granularity of about 70 [mu]m and is uniform in distribution. The solution is easy to filter and dry, is good in flowability and is free of coalescence. A single-way crystallization yield is higher than 90%. The purity of the coenzyme Q10 crystal product is higher than 99.0%. The method is convenient to operate, is low in cost, is less in energy consumption, is free of generation of harmful wastes and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering crystallization, in particular to a coenzyme Q aided by ultrasonic waves 10 method of crystallization. Background technique [0002] Ubiquinone (UQ for short), also known as coenzyme Q (Coenzyme Q), is a general term for a class of fat-soluble quinones widely found in nature, and its structure is similar to vitamin E and vitamin K. The ubiquinone molecule contains a side chain composed of multiple isoprene units connected to the p-benzoquinone core. The length of the side chain varies with the source of ubiquinone. In mammals, the coenzyme generally contains 10 isoprene units, so it is also called coenzyme Q 10 (Ubidecarenone), which is orange-yellow or light yellow solid powder, chemical name 2-(3,7,11,15,19,23,27,31,35,39-decylmethyl-2,6,10,14 ,18,22,26,30,34,38-tetradecenyl)-5,6-dimethoxy-3-methyl-p-benzoquinone, the molecular formula is C 59 h 90 o 4 , with a molecular weigh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/28C07C46/10
CPCC07C46/10C07C50/28
Inventor 陈巍朱培培侯宝红尹秋响张美景谢闯龚俊波郝红勋王永莉鲍颖
Owner TIANJIN UNIV
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