CN202315872U - dehydropregnenolone acetate photosensitive oxidation reaction device - Google Patents
dehydropregnenolone acetate photosensitive oxidation reaction device Download PDFInfo
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- CN202315872U CN202315872U CN2011204396809U CN201120439680U CN202315872U CN 202315872 U CN202315872 U CN 202315872U CN 2011204396809 U CN2011204396809 U CN 2011204396809U CN 201120439680 U CN201120439680 U CN 201120439680U CN 202315872 U CN202315872 U CN 202315872U
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- oxidation reaction
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Abstract
The utility model discloses a dehydropregnenolone acetate photosensitive oxidation reaction device, and relates to a chemical reaction device. The problems about pollution, complicated operation and the like of the conventional thermochemistry dehydropregnenolone acetate production are solved. The dehydropregnenolone acetate photosensitive oxidation reaction device comprises a glass container and a light generator, wherein the light generator is fixed in the glass container and consists of a filter glass tube I, a filter glass tube II, a high-voltage mercury lamp and a high-voltage mercury lamp fixing bracket. The dehydropregnenolone acetate photosensitive oxidation reaction device is convenient to operate, performs treatment at normal temperature, and is environment-friendly.
Description
Technical field
The utility model relates to a kind of chemical reaction equipment, particularly relates to a kind of diene alcohol ketone acetic ester photosensitized oxidation reaction unit.
Background technology
At present; In the traditional hot chemical production processes of diene alcohol ketone acetic ester; The false diosgenin of intermediate is that oxidation through heavy metal oxidant chromium trioxide realizes that the chromium discharging wastes that contains of initiation has caused great pollution to environment thus to the conversion of intermediate ground ketone difficult to understand; This heat chemistry oxidizing process is carried out in glacial acetic acid simultaneously, needs extracting operation times without number after reaction finishes, and causes aftertreatment technology complicated; In addition, variation of temperature has significant effects to the yield of product in this heat chemistry oxidizing process, and this brings very big difficulty for control and yield stable of reaction.
The utility model content
The purpose of the utility model is in order to overcome deficiency of the prior art, provide a kind of easy to operate, normal temperature is handled and the diene alcohol ketone acetic ester photosensitized oxidation reaction unit of environmental protection
For realizing above-mentioned purpose, the utility model provides a kind of diene alcohol ketone acetic ester photosensitized oxidation reaction unit, comprises glass container and optical generator; The lower end of institute's glass container is provided with charging aperture and air inlet; Said charging aperture is provided with the charging gate valve; Said air inlet is provided with the air inlet gate valve, and a Gas-liquid mixing valve is set between charging aperture and air inlet, and the upper end of said glass container is provided with gas-liquid mixture outlet; Said optical generator is fixed in the glass container; Said optical generator is made up of filter glass pipe one, filter glass pipe two, nitrogen tube, high-pressure sodium lamp and high-pressure sodium lamp fixed support; Said filter glass pipe two is arranged in the filter glass pipe one; Said mercury lamp fixed support is fixed on the inwall of filter glass pipe two, and said nitrogen tube is fixed in junction, filter glass Guan Yiyu filter glass pipe two top, and said high-pressure sodium lamp is fixed on the mercury lamp fixed support.
Two of said filter glass pipe one and filter glass pipes are provided with cooling fluid.
Said mercury lamp is the 10kw high-pressure sodium lamp.
Said filter glass Guan Yiwei quartz glass colour filter pipe one, said filter glass Guan Erwei quartz glass colour filter pipe two.
The utility model beneficial effect is: the diene alcohol ketone acetic ester photosensitized oxidation reaction unit of the utility model at first utilizes the light of high-pressure sodium lamp emission and airborne oxygen to realize that false diosgenin, acetone, pyridine, acetic anhydride mix back open loop under the catalytic action of sensitising agent and make ground ketone difficult to understand; Avoided the use of heavy metal oxidant chromium trioxide, made the environmental protection of diene alcohol ketone acetic ester photosensitized oxidation course of reaction; Simultaneously, the photosensitized oxidation reaction unit of the utility model utilizes photosensitized oxidation to be reflected in acetone, acetic anhydride and the pyridine solution, and the yield of ketone difficult to understand reaches more than 90% feasiblely; Secondly, the diene alcohol ketone acetic ester photosensitized oxidation in the photosensitized oxidation reaction unit of the utility model is reflected in the acetone and carries out, and need not extracting operation after the reaction, and aftertreatment technology is greatly simplified; Moreover the diene alcohol ketone acetic ester photosensitized oxidation reaction pair temperature in the photosensitized oxidation reaction unit of the utility model does not have harsh requirement, makes reaction control more easily.
Be described further below in conjunction with the diene alcohol ketone acetic ester photosensitized oxidation reaction unit of accompanying drawing the utility model.
Description of drawings
Fig. 1 is the structural representation of the utility model.
Among the figure: 1, glass container, 2, optical generator, 3, charging aperture, 4, air inlet; 5, charging gate valve, 6, the air inlet gate valve, 7, Gas-liquid mixing valve; 8, nitrogen tube, 9, gas-liquid mixture outlet, 10, quartz glass colour filter pipe one; 11, quartz glass colour filter pipe two, 12,10kw high-pressure sodium lamp, 13, the high-pressure sodium lamp fixed support.
The specific embodiment
As shown in Figure 1; The diene alcohol ketone acetic ester photosensitized oxidation reaction unit of present embodiment comprises glass container 1 and optical generator 2; The lower end of glass container 1 is provided with charging aperture 3 and air inlet 4, and charging aperture 3 is provided with charging gate valve 5, and air inlet 4 is provided with charging gate valve 6; One Gas-liquid mixing valve 7 is set between charging aperture 3 and air inlet 4, and the upper end of glass container 1 is provided with gas-liquid mixture outlet 9.Optical generator 2 is fixed in the glass container 1; Optical generator 2 is made up of quartz glass colour filter pipe 1, quartz glass colour filter pipe 2 11,10kw high-pressure sodium lamp 12 and high-pressure sodium lamp fixed support 13; Quartz glass colour filter pipe 2 11 is arranged in the quartz glass colour filter pipe 1; High-pressure sodium lamp fixed support 13 is fixed on the inwall of quartz glass colour filter pipe 2 11, and 10kw high-pressure sodium lamp 12 is fixed on the high-pressure sodium lamp fixed support 13.Nitrogen tube 8 is fixed in filter glass pipe 1 and junction, filter glass pipe 2 11 top, and 2 12 of quartz glass colour filter pipe 1 and quartz glass colour filter pipes are provided with cooling fluid.
The technological process of preparation diene alcohol ketone acetic ester: the false diosgenin of cracking diosgenin gained; In the acetone solvent of low toxicity and cheapness; Through diene alcohol ketone acetic ester photosensitized oxidation reaction unit; In the presence of sensitising agent and light, with oxygen reaction, the product that obtains is eliminated the important as precursors diene alcohol ketone acetic ester that reaction obtains synthetic other multiple steroid drugs through acidolysis again.
The diene alcohol ketone acetic ester photosensitized oxidation reaction unit of present embodiment makes the environmental protection of diene alcohol ketone acetic ester photosensitized oxidation course of reaction; Simultaneously, make the yield of diene alcohol ketone acetic ester reach more than 85%; Secondly, the photosensitized oxidation reaction unit of the utility model is simple to operate; Moreover the diene alcohol ketone acetic ester photosensitized oxidation reaction pair temperature in the photosensitized oxidation reaction unit of the utility model does not have harsh requirement, makes reaction control more easily; Continuous spectrum and quartz glass colour filter through adopting the 10kw high-pressure sodium lamp can produce 250nm to 700nm can effectively filter the useless and part stray light below the 400nm, have guaranteed that photosensitized oxidation reacts required light source, has solved the technical barrier of suitability for industrialized production.
Claims (4)
1. a diene alcohol ketone acetic ester photosensitized oxidation reaction unit is characterized in that, said diene alcohol ketone acetic ester photosensitized oxidation reaction unit comprises glass container and optical generator; The lower end of said glass container is provided with charging aperture and air inlet; Said charging aperture is provided with the charging gate valve; Said air inlet is provided with the air inlet gate valve, and a Gas-liquid mixing valve is set between charging aperture and air inlet, and the upper end of said glass container is provided with gas-liquid mixture outlet; Said optical generator is fixed in the glass container; Said optical generator is made up of filter glass pipe one, filter glass pipe two, nitrogen tube, high-pressure sodium lamp and high-pressure sodium lamp fixed support; Said filter glass pipe two is arranged in the filter glass pipe one; Said high-pressure sodium lamp fixed support is fixed on the inwall of filter glass pipe two, and said nitrogen tube is fixed in junction, filter glass Guan Yiyu filter glass pipe two top, and said high-pressure sodium lamp is fixed on the high-pressure sodium lamp fixed support.
2. diene alcohol ketone acetic ester photosensitized oxidation reaction unit according to claim 1 is characterized in that two of said filter glass pipe one and filter glass pipes are provided with cooling fluid.
3. diene alcohol ketone acetic ester photosensitized oxidation reaction unit according to claim 1 is characterized in that said mercury lamp is the 10kw high-pressure sodium lamp.
4. diene alcohol ketone acetic ester photosensitized oxidation reaction unit according to claim 1 is characterized in that, said filter glass Guan Yiwei quartz glass colour filter pipe one, said filter glass Guan Erwei quartz glass colour filter pipe two.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN2011204396809U CN202315872U (en) | 2011-11-09 | 2011-11-09 | dehydropregnenolone acetate photosensitive oxidation reaction device |
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CN2011204396809U CN202315872U (en) | 2011-11-09 | 2011-11-09 | dehydropregnenolone acetate photosensitive oxidation reaction device |
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CN202315872U true CN202315872U (en) | 2012-07-11 |
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CN2011204396809U Expired - Fee Related CN202315872U (en) | 2011-11-09 | 2011-11-09 | dehydropregnenolone acetate photosensitive oxidation reaction device |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103772464A (en) * | 2013-12-30 | 2014-05-07 | 中国科学院理化技术研究所 | Method for preparing 16-dehydropregnenolone alcohol acetate compounds by utilizing blue LED light source photosensitive oxidation |
-
2011
- 2011-11-09 CN CN2011204396809U patent/CN202315872U/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103772464A (en) * | 2013-12-30 | 2014-05-07 | 中国科学院理化技术研究所 | Method for preparing 16-dehydropregnenolone alcohol acetate compounds by utilizing blue LED light source photosensitive oxidation |
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C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
C17 | Cessation of patent right | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120711 Termination date: 20121109 |