CN102219820A - Method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening - Google Patents
Method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening Download PDFInfo
- Publication number
- CN102219820A CN102219820A CN 201110111114 CN201110111114A CN102219820A CN 102219820 A CN102219820 A CN 102219820A CN 201110111114 CN201110111114 CN 201110111114 CN 201110111114 A CN201110111114 A CN 201110111114A CN 102219820 A CN102219820 A CN 102219820A
- Authority
- CN
- China
- Prior art keywords
- infrared heating
- heating
- acetic ester
- open loop
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening comprises the steps of ring-opening cracking, extraction and refining, wherein infrared heating is carried out on a reaction kettle during ring-opening cracking process. In the invention, as a silicon carbide far infrared heating and radiation heating device and a tank body are assembled together, the reaction kettle is heated by controlling the voltage and current of a heating device, so that temperature and voltage can be automatically controlled, power can be automatically adjusted and randomly set, the temperature control is precise, heat buffer is small, personal errors are reduced, the stability of infrared heating ring-opening reaction is ensured, and further the reaction is more sufficient.
Description
Technical field
The invention belongs to the steroid hormone pharmaceutical intermediate and clean production technical field, be specially the processing method that relates to a kind of silicon carbide far-infrared heating open loop manufacture order, diene alcohol ketone acetic ester.
Background technology
Diene alcohol ketone acetic ester (abbreviation diene) chemical name: 5.16-pregnen diethylene-3 β-alcohol-20-ketone acetic ester, molecular formula is C
23H
32O
3, have the parent nucleus of pentamethylene a pair of horses going side by side perhydro phenanthrene, belong to typical steroidal compounds.Diene is the important intermediate of synthetic various steroid hormone class medicines, can produce progestogens medicine (Progesterone as raw material, Zytron, sour progesterone), the adrenocortical hormone medicine is (as hydrocortisone, Prednisolone Acetate, Betamethasone Valerate) sexual hormoue and protein anabolic hormone medicine (methyltestosterone, medroxyprogestrone Acetate, Synasteron, stanozolol) etc.
The open loop scission reaction is one of crucial chemical reaction in the diene alcohol ketone acetic ester production process.This is reflected in the ring-opening reaction still and carries out, and what material carried out in the still is the gas-liquid-solid phase reaction of High Temperature High Pressure, so the open loop still is one of key equipment of products production.Traditional open loop heating means are to utilize electric heating oil bath heating, promptly inject an amount of thermal oil in the chuck of open loop still, insert several electric heating tubes in the oil, and energising post-heating thermal oil makes the reactor heat temperature raising indirectly.
Mainly there is following defective in tradition reactor equipment:
1, open loop scission reaction processing condition are very harsh to temperature, pressure, time requirement.When using legacy equipment, temperature of reaction in the production process, pressure, time are wayward, careless slightlyly very easily cause failure of open loop scission reaction or reaction not exclusively, cause yield reduce, off quality.
What 2, material carried out in the still is high-temperature high-voltage reaction, and its temperature of reaction is 210 ℃, and pressure is 0.6Mpa, and heat-conducting oil heating temperature height uses the electrothermal tube heating in addition, in case reveal, accident such as easily cause fire or scald, burn, potential safety hazard is big.
3, thermal oil is for a long time under high-temperature condition, and the carbonization fouling needs periodic replacement thermal oil and electrothermal tube, cleans chuck, has increased production man-hour, has prolonged the production cycle.
4, the deep fat heat transfer coefficient is little, and thermo-efficiency is low, and power consumption increases.
Above reason increases the enterprise product cost expense, and security risk increases.Therefore, the problem that otherwise substitutes the traditional heating method is being studied always by domestic diene alcohol ketone acetic ester manufacturer.
Summary of the invention
The object of the present invention is achieved like this: a kind of method of utilizing far-infrared heating open loop manufacture order, diene alcohol ketone acetic ester, comprise open loop cracking, extraction and refining, and in the open loop scission reaction process reactor is adopted far-infrared heating.
It is that silicon carbide far-infrared heating radiant heating device and tank body are fitted together that reactor is adopted far-infrared heating, finishes heating to reactor by the electric current and voltage of controlling heating unit.
Through silicon carbide far-infrared heating open loop manufacture order or diene alcohol ketone acetic ester, be example with the diene alcohol ketone acetic ester that obtains: content is more than 99%, and main impure point is below 1.0%, fusing point: more than 168 ℃, and alcohol insoluble solids: clarification.Yield: more than 67%.
Major advantage of the present invention:
1, because the present invention adopts silicon carbide far-infrared heating radiant heating device and tank body to fit together, electric current and voltage by the control heating unit is finished heating to reactor, can temperature automatically controlled pressure control, power can be regulated any setting, temperature control accurately automatically, the heat buffering is little, the minimizing personal errors, guaranteed the stability of far-infrared heating ring-opening reaction, made reaction more complete.
2, eliminated potential safety hazard, safety anti-explosive, environmentally safe, far-infrared heating mode belong to and clean production technique, meet the requirement of ISO14001 environment management system.
3. far-infrared heating mode electric conversion efficiency height, obvious energy conservation is compared energy-conservationly 20% with heat-conducting oil heating, owing to do not need to change thermal oil and heat pipe, can reduce advantages such as running cost about 4.5%.
4, after system comes into operation, improved labor strength to the full extent and reduced operator's technical requirements, error rate reduces greatly, has guaranteed product percent of pass.
Embodiment
Through the method that diene alcohol ketone acetic ester is produced in the open loop of silicon carbide far-infrared heating, throw diosgenin 160kg, add Glacial acetic acid 88kg, aceticanhydride 252kg, mother liquor 96kg imports the set(ting)value of processing requirement on request, open silicon carbide far-infrared heating housing autocontrol switch, carry out the open loop scission reaction.When interior temperature rise to 196 ℃, when interior pressure reaches 0.44MPa, the instrument timing of cutting off the power supply automatically.Open loop scission reaction 60 minutes, last interior temperature is reaching 208 ℃, and pressure 0.58MPa open loop finishes.Be pressed in the oxydrolysis jar of getting acid at the bottom of the 90kg ready, begin cooling, when temperature in the jar is reduced to 10～12 ℃, both closed salt solution, oxygenant is added in the oxidation tank, carry out oxidizing reaction at once.When temperature rises to 98 ℃ of clock reactions 30 minutes, chuck feeds the steam heating temperature reaction then, and air distillation was reclaimed acetic acid 50 minutes, and the reclaim under reduced pressure Glacial acetic acid is 30 minutes again.Reaction finishes, generation based on the compound feed liquid of diene alcohol ketone acetic ester after filtration to extractor, adding hexanaphthene 1520L extracts, add hot water 640L, stirred after 30 minutes static 1 hour, begin branch acid then, can begin to add hot water (50～60 ℃) after dividing acid to finish and wash material, add at every turn and control about 55 ℃ of interior temperature about water 400L, stirred 30 minutes, the static extremely neutrality of repeatedly washing more than 40 minutes.The flush away water-soluble impurity, static 4～6 hours branch vibration layers, to treatment tank, the filtrate heating concentrates reclaims hexanaphthene to doing through filter, add ethanol 100L, the gradation band adds 100L ethanol after doing again, is pressed into the centrifugal crude product that gets of crystallizer decrease temperature crystalline after the reflux, and it is anti-refining that crude product drops into treatment tank again, the same crystallizer of process is cooled to that centrifuging gets finished product below 10 ℃, oven dry is pulverized, packing.
The present invention also is applicable to the production of monoene alcohol ketone acetic ester.
Method through silicon carbide far-infrared heating open loop manufacture order enol ketone acetic ester, throw tigogenin 160kg, add Glacial acetic acid 88kg, aceticanhydride 252kg, mother liquor 96kg, the temperature and pressure set(ting)value of input processing requirement is opened silicon carbide far-infrared heating housing autocontrol switch, carries out the open loop scission reaction.When interior temperature rise to 196 ℃, when interior pressure reaches 0.44MPa, the timing of cutting off the power supply automatically.Open loop 60 minutes, last interior temperature is reaching 208～210 ℃, and pressure 0.60MPa open loop finishes.Be pressed in the oxydrolysis jar of getting acid at the bottom of the 90kg ready, begin cooling, when temperature in the jar is reduced to 10～12 ℃, both closed salt solution, oxygenant is added in the oxidation tank, carry out oxidizing reaction at once.When temperature rises to 98 ℃ of clock reactions 30 minutes, chuck feeds the steam heating temperature reaction then, and air distillation was reclaimed acetic acid 50 minutes, and the reclaim under reduced pressure Glacial acetic acid is 30 minutes again.Reaction finishes, generation based on the compound feed liquid of monoene alcohol ketone acetic ester after filtration to extractor, adding hexanaphthene 1520L extracts, add hot water 640L, stirred after 30 minutes static 1 hour, begin branch acid then, can begin to add hot water (50～60 ℃) after dividing acid to finish and wash material, add at every turn and control about 55 ℃ of interior temperature about water 400L, stirred 30 minutes, the static extremely neutrality of repeatedly washing more than 40 minutes.The flush away water-soluble impurity, static 4～6 hours branch vibration layers, to treatment tank, the filtrate heating concentrates reclaims hexanaphthene to doing through filter, add ethanol 100L, the gradation band adds 100L ethanol after doing again, is pressed into the centrifugal crude product that gets of crystallizer decrease temperature crystalline after the reflux, and it is anti-refining that crude product drops into treatment tank again, the same crystallizer of process is cooled to that centrifuging gets finished product below 10 ℃, oven dry is pulverized, packing.
Claims (2)
1. a method of utilizing far-infrared heating open loop manufacture order, diene alcohol ketone acetic ester comprises open loop cracking, extraction and refining, it is characterized in that: in the open loop scission reaction process reactor is adopted far-infrared heating.
2. the method for utilizing far-infrared heating open loop manufacture order, diene alcohol ketone acetic ester according to claim 1, it is characterized in that: it is that silicon carbide far-infrared heating radiant heating device and tank body are fitted together that reactor is adopted far-infrared heating, finishes heating to reactor by the electric current and voltage of controlling heating unit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110111114 CN102219820A (en) | 2011-05-02 | 2011-05-02 | Method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110111114 CN102219820A (en) | 2011-05-02 | 2011-05-02 | Method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102219820A true CN102219820A (en) | 2011-10-19 |
Family
ID=44776546
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110111114 Pending CN102219820A (en) | 2011-05-02 | 2011-05-02 | Method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102219820A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044513A (en) * | 2012-12-20 | 2013-04-17 | 湖北省丹江口开泰激素有限责任公司 | Method for manufacturing dehydropregnenolone acetate by using mixed solvent |
| CN103113448A (en) * | 2013-02-04 | 2013-05-22 | 湖北民生生物医药有限公司 | Production method for synthesizing pregnenolone acetate from ticogenin |
| CN108212055A (en) * | 2017-09-27 | 2018-06-29 | 湖北民生生物医药有限公司 | A kind of diene oxidation technology automatic control system and method |
| CN112587953A (en) * | 2020-12-18 | 2021-04-02 | 湖北民生生物医药有限公司 | Automatic extraction element of dehydropregnenolone face ketone acetate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1763066A (en) * | 2005-11-17 | 2006-04-26 | 台州百大药业有限公司 | Methylprednisolone chemical synthesis method |
| CN101712712A (en) * | 2009-11-11 | 2010-05-26 | 湖北民生工贸有限公司 | Method for preparing 16-dehydropregnenolone acetate by multistage filtration and recrystallization |
| CN201807359U (en) * | 2010-09-07 | 2011-04-27 | 天津科技大学 | Reaction kettle capable of heating by adopting far infrared radiation |
-
2011
- 2011-05-02 CN CN 201110111114 patent/CN102219820A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1763066A (en) * | 2005-11-17 | 2006-04-26 | 台州百大药业有限公司 | Methylprednisolone chemical synthesis method |
| CN101712712A (en) * | 2009-11-11 | 2010-05-26 | 湖北民生工贸有限公司 | Method for preparing 16-dehydropregnenolone acetate by multistage filtration and recrystallization |
| CN201807359U (en) * | 2010-09-07 | 2011-04-27 | 天津科技大学 | Reaction kettle capable of heating by adopting far infrared radiation |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103044513A (en) * | 2012-12-20 | 2013-04-17 | 湖北省丹江口开泰激素有限责任公司 | Method for manufacturing dehydropregnenolone acetate by using mixed solvent |
| CN103113448A (en) * | 2013-02-04 | 2013-05-22 | 湖北民生生物医药有限公司 | Production method for synthesizing pregnenolone acetate from ticogenin |
| CN103113448B (en) * | 2013-02-04 | 2016-05-11 | 湖北民生生物医药有限公司 | A kind of production method by the synthetic pregnenolone acetate of tigogenin |
| CN108212055A (en) * | 2017-09-27 | 2018-06-29 | 湖北民生生物医药有限公司 | A kind of diene oxidation technology automatic control system and method |
| CN112587953A (en) * | 2020-12-18 | 2021-04-02 | 湖北民生生物医药有限公司 | Automatic extraction element of dehydropregnenolone face ketone acetate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102219820A (en) | Method for producing pregnenolone acetic ester and 16-dehydropregnenolone acetate by utilizing infrared heating ring opening | |
| CN102304094B (en) | Preparation method of sulfadoxine and intermediate thereof | |
| CN101712712A (en) | Method for preparing 16-dehydropregnenolone acetate by multistage filtration and recrystallization | |
| US20170355657A1 (en) | Device and process for producing undecylenic acid methyl ester using methyl ricinoleate as raw material | |
| CN105004192B (en) | Gas filter system and a kind of yellow phosphorus furnace gas filter method | |
| CN112479847B (en) | Method for preparing diketene by cracking acetic acid | |
| CN102746356B (en) | Process for producing dehydroepiandrosterone acetate through homogeneous phase method | |
| CN102391136B (en) | Method and device for producing 4,4-diaminodiphenyl ethers by using catalytic hydrogenation process | |
| CN106008232A (en) | Recycling device of amitraz prepared product | |
| CN1026181C (en) | Cracking of disgenin and new art of mother liquor recovery therefrom | |
| CN204529786U (en) | Utilize the device of regenerating waste oil lubricating base oils | |
| CN104098638A (en) | Dehydroepiandrosterone acetate preparation method | |
| CN106928300A (en) | A kind of new technology of the acetic acid Lipase absobed epiandrosterone of 3 β monohydric pregnants, 16 alkene, 20 ketone 3 | |
| CN103396309A (en) | Method for producing high-purity propylgallate by virtue of pressurization process | |
| CN109369760B (en) | Method for preparing dehydromethyltestosterone | |
| CN103773832B (en) | Method and the technique of 4-AD is extracted from plant sterol aqueous phase fermentation liquid | |
| CN210496408U (en) | 2-chlorine-5-chloromethyl pyridine apparatus for producing | |
| CN104496950B (en) | Method for upgrading quality of industrial o-phthalic anhydride | |
| CN104818106A (en) | Preparation method for basic lubricating oil | |
| CN204529787U (en) | The equipment of regenerating waste oil lubricating base oils | |
| CN105177313B (en) | A kind of magnesium metal reduction heating means of interior external heat | |
| CN109851654A (en) | The method of pipeline reactor saponification extracting cholesterin from lanolin | |
| CN109456378B (en) | Method for preparing dehydromethyltestosterone product | |
| CN109456379B (en) | Preparation method of dehydromethyltestosterone product | |
| CN109369761B (en) | Preparation method of dehydromethyltestosterone |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111019 |