CN209276417U - Realize the device of ethylene glycol by-product recycled in metronidazole production - Google Patents
Realize the device of ethylene glycol by-product recycled in metronidazole production Download PDFInfo
- Publication number
- CN209276417U CN209276417U CN201821987099.9U CN201821987099U CN209276417U CN 209276417 U CN209276417 U CN 209276417U CN 201821987099 U CN201821987099 U CN 201821987099U CN 209276417 U CN209276417 U CN 209276417U
- Authority
- CN
- China
- Prior art keywords
- outlet
- liquid level
- valve
- injector
- pipe
- 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.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model provides a kind of device for realizing ethylene glycol by-product recycled in metronidazole production.Sulfuric acid is introduced in injector using injector and is mixed with solution by the device of the utility model, improves mixing efficiency.It is concentrated by evaporation using steaming water kettle, mixing vessel mixed solution, condenser and tear drop pipe are connected by pipeline, the steam steamed in condenser is sucked in injector, the utilization rate of mixing drug is improved, while the subnormal ambient built in condenser when injector work is also conducive to the evaporation of moisture, condensation；In the present invention, by the acid vapor and glycol steam sucking injector in sulfuric acid and ethylene glycol mixture, to make full use of.
Description
Technical field
The utility model belongs to ethylene glycol by-product circulating sleeve in organic synthesis field more particularly to a kind of production of metronidazole
The application of method, apparatus and the device.
Background technique
Existing metronidazole synthesis technology, the utilization rate of raw material ethylene oxide only have 20%.Utility model patent metronidazole hydroxyl
Change reaction kettle (201020227836.2), the ratio between autoclave body height and internal diameter are increased；Utility model patent metronidazole hydroxylation reaction
Kettle ethylene oxide access equipment (201020247143.X) improves the distribution situation for being passed through gas；A kind of raising first of patent of invention
The Processes and apparatus (201310215220.1) of nitre azoles raw materials for production utilization rate of ethylene oxide, using three kettles series winding and multi-stage condensing
Measure.Although above three patent all increases ethylene oxide and the catalytic chance of material, epoxy to some extent
The utilization rate of ethane is still no more than 25%.This is because ethylene oxide is reacted with strong acid generates ethoxy carbonium ion, it is hydroxylated liquid
In there are following chemical reaction equilibriums:
Balance must be promoted mobile to metronidazole direction is generated, otherwise can reduce 2- with the presence of excessive above-mentioned carbonium ion
The hydroxylation rate of -5 nitroimidazole of methyl.Hydroxyl of the excessive ethoxy carbonium ion in product separation process, with aqueous alkali
Effect generates ethylene glycol by-product.
Utility model content
In view of the above technical problems, the utility model provides ethylene glycol by-product circulation in a kind of production of realization metronidazole
The device applied.In metronidazole production process, by-product ethylene glycol is recycled, using sulfuric acid and glycol reaction, is generated
Ethoxy carbonium ion recycled required for reaction system improves utilization rate of ethylene oxide, saves production cost.
In order to solve the above-mentioned technical problem, the technical solution adopted in the utility model are as follows:
A kind of device for realizing ethylene glycol by-product recycled in metronidazole production characterized by comprising
Liquid seal trough 10, inside fills lye；
Mixing vessel 20, top offer feed opening and by 21 sealings of capping, and upper part is equipped with outlet port, under
Portion walks around to import and first equipped with first and walks around to outlet, is equipped with liquid level alarm 22 in mixing vessel；The outlet port with
The connection of 10 pipeline of liquid seal trough；
Condenser 30, outlet are provided with outlet valve 31；
Steam water kettle 40, bottom is equipped with second and walks around to import, second walks around to outlet and discharge port, and top is equipped with steam and arranges
Outlet pipe, the vapour-discharge tube connect the import of the condenser 30；Described second, which walks around to import, walks around to outlet with first and passes through
Walk around to pipe 41 connection, walk around to pipe 41 be equipped with walk around to valve 42；The discharge outlet is provided with outlet valve 43；
The inlet pipeline connection described second of kinetic pump 50 and injector 60, kinetic pump 50 walks around to outlet, outlet and spray
First inlet pipeline of emitter 60 connects；Vertical tear drop pipe 61 is provided in second import of injector 60, tear drop pipe 61
Upper end is equipped with charge funnel 62, and tear drop pipe 61, which is equipped with, is added dropwise valve 63, is provided with winding pipe 64, winding pipe on tear drop pipe 61
On set air inlet valve 65；The outlet conduit of injector 60 is connected to described first and walks around to import；
Controller, the controller is interior to be arranged and is stored with predetermined high liquid level value, predetermined low liquid level value, controller and liquid level
22 connection of alarm.
Further, the top of the condenser 30 is equipped with non-condensable gas export, and the non-condensable gas export pipeline is connected to
The tear drop pipe 61.Condenser and tear drop pipe are connected by pipeline, makes the negative pressure for spraying mixed process generation for being evaporated in vacuo
Moisture content.
Further, blender is provided in the steaming water kettle 40.Blender can accelerate to mix.
Further, baffle plate 23 is provided in the mixing vessel 20.Baffle plate 23 can accelerate to mix.
A kind of application of described device in metronidazole production in the method for ethylene glycol by-product recycled, feature exist
In comprising the following steps:
Step 1): 2- 5-nitro imidazole is added in reaction kettle, and the formic acid that mass percent concentration 85% is added dropwise is molten
Agent dissolves 2- 5-nitro imidazole, ethylene oxide is gradually added at 30-40 DEG C, while adding mass percent concentration
98% sulfuric acid is warming up to 85-95 DEG C, and reaction 1h must be hydroxylated liquid；
Step 2): liquid to be hydroxylated is cooled to 10 DEG C, is adjusted to pH=10 with alkali hydroxide soln, places cooling, knot
A metronidazole and first-time filtrate is obtained by filtration in crystalline substance；Obtained first-time filtrate is concentrated by evaporation, is cooling, crystallization, filtering, obtains alkali
Metal sulfate solid product and secondary filtrate；
Step 3): the secondary filtrate that vacuum distillation step 2) obtains obtains ethylene glycol by-product；
Step 4): closing outlet valve 31 and outlet valve 43, and standard-sized sheet walks around to valve 42 and air inlet valve 65, opens capping 21, will walk
Mixing vessel 20 is added by feed opening in the rapid ethylene glycol 3) obtained, covers capping 21, and quality percentage is added into charge funnel 62
Specific concentration be 60-98% with the equimolar sulfuric acid of sulfuric acid added by step 1)；That is 60-98% sulfuric acid solution institute added by this step
The sulfuric acid molal quantity contained is equal with sulfuric acid molal quantity contained by 98% sulfuric acid solution added by step 1)；
Step 5): starting kinetic pump 50 is slowly opened and the dropwise addition sulfuric acid of valve 63 is added dropwise, and ethylene glycol is mixed with sulfuric acid, controlled
It is arranged and stores predetermined high liquid level value, predetermined low liquid level value on device processed, adjusts the opening size for walking around to valve 42, make mixing vessel 20
Interior liquid level maintains between predetermined high liquid level value and predetermined low liquid level value；If it is high to be higher than the liquid level for liquid level in mixing vessel 20
Value, liquid level alarm 22 alarm, tune up and walk around to valve 42；If liquid level is lower than the liquid level low value, liquid level warning in mixing vessel 20
Device 22 is alarmed, and is turned down and is walked around to valve 42；
Step 6): holding meanss work, it is 100 DEG C to 120 DEG C that water kettle temperature degree is steamed in control, in 0.01-0.9 normal atmosphere
Pressure is evaporated under reduced pressure, and starts condenser 30, half-open to walk around to valve 42, slowly closing air inlet valve 65；To the sulfuric acid in charge funnel 62
It is added dropwise, closes and valve 63 is added dropwise, be evaporated to when there is no moisture to be distilled out of in water kettle 40, slowly unlatching air inlet valve 65 simultaneously tunes up
Walk around to valve 42；Turn off kinetic pump 50；Then outlet valve 31 is opened, the moisture content steamed is bled off；Outlet valve 43 is finally opened, is taken out
Steam raffinate；
Step 7): the 2- 5-nitro imidazole of mass percent concentration 100% is added in reaction kettle, and quality is added dropwise
The formic acid solvent of percent concentration 85-95% dissolves 2- 5-nitro imidazole, and quality percentage is gradually added at 30-40 DEG C
The ethylene oxide of specific concentration 100%, while a dropping step 6) obtained steaming raffinate, it is warming up to 85-95 DEG C, reaction 1h must be hydroxylated
Liquid；
Step 8): liquid to be hydroxylated is cooled to 10 DEG C, is adjusted to pH=10 with alkali hydroxide soln, places cooling, knot
Secondary metronidazole is obtained by filtration in crystalline substance.
Beneficial effect obtained by the utility model has:
1. utilizing sulfuric acid and glycol reaction, ethoxy carbonium ion recycled required for reaction system is generated, is mentioned
High utilization rate of ethylene oxide, saves production cost；And the water that ethylene glycol and sulfuric acid reaction generate is unfavorable for the synthesis of metronidazole,
Therefore evaporate the water that reaction generates simultaneously in step d).
2. sulfuric acid is introduced in injector using injector and mixed with solution by the device of the utility model, mixing effect is improved
Rate.
3. connecting condenser and tear drop pipe using water kettle evaporation and concentration, mixing vessel mixed solution is steamed by pipeline, steaming
Enter in the on-condensible gas and a small amount of uncondensated steam sucking injector in condenser, not only reduces material loss, but also reduce environment
Pollution, while the subnormal ambient built in condenser when injector work is also conducive to the evaporation of moisture, condensation；It is practical new at this
In type, by the acid vapor and glycol steam sucking injector in sulfuric acid and ethylene glycol mixture, to make full use of；With saturation
The ethylene glycol and sulfuric acid mixture liquid that steam forces down replace water to make stock solution, and the negative pressure for generating injection is lower, are more advantageous to vacuum
Evaporate moisture content.
4. sulfuric acid is added dropwise the vacuum that injection generates and is used to be evaporated in vacuo moisture content by the device, sulfuric acid and ethylene glycol were mixed
The heat that journey generates is also used for evaporation moisture content, so that kinetic energy and thermal energy is fully used, further saves production cost.
Detailed description of the invention
Fig. 1 is a kind of schematic diagram for realizing the device of ethylene glycol by-product recycled in metronidazole production.
Appended drawing reference: 10- liquid seal trough；20- mixing vessel；21- capping；22- liquid level alarm；23- baffle plate；30- is cold
Condenser；31- outlet valve；40- steams water kettle；41- walks around to pipe；42- walks around to valve；43- outlet valve；44- collet；50- kinetic pump；60-
Injector；61- tear drop pipe；62- charge funnel；Valve is added dropwise in 63-；64- winding pipe；65- air inlet valve.
Specific embodiment
The embodiments of the present invention is illustrated now in conjunction with attached drawing.
As shown in Figure 1, a kind of device for realizing ethylene glycol by-product recycled in metronidazole production, which is characterized in that
Include:
Liquid seal trough 10, inside fills lye；
Mixing vessel 20, top offer feed opening and by 21 sealings of capping, and upper part is equipped with outlet port, under
Portion walks around to import and first equipped with first and walks around to outlet, is equipped with liquid level alarm 22 in mixing vessel；The outlet port with
The connection of 10 pipeline of liquid seal trough；
Condenser 30, outlet are provided with outlet valve 31；
Steam water kettle 40, bottom is equipped with second and walks around to import, second walks around to outlet and discharge port, and top is equipped with steam and arranges
Outlet pipe, the vapour-discharge tube connect the import of the condenser 30；Described second, which walks around to import, walks around to outlet with first and passes through
Walk around to pipe 41 connection, walk around to pipe 41 be equipped with walk around to valve 42；The discharge outlet is provided with outlet valve 43；
The inlet pipeline connection described second of kinetic pump 50 and injector 60, kinetic pump 50 walks around to outlet, outlet and spray
First inlet pipeline of emitter 60 connects；Vertical tear drop pipe 61 is provided in second import of injector 60, tear drop pipe 61
Upper end is equipped with charge funnel 62, and tear drop pipe 61, which is equipped with, is added dropwise valve 63, is provided with winding pipe 64, winding pipe on tear drop pipe 61
On set air inlet valve 65；The outlet conduit of injector 60 is connected to described first and walks around to import；
Controller, the controller is interior to be arranged and is stored with predetermined high liquid level value, predetermined low liquid level value, controller and liquid level
22 connection of alarm.
In the present apparatus, the effect of each section is as follows: filling lye in liquid seal trough 10, is steamed with the acid overflowed in absorption process
Vapour；Mixing vessel 20 is mixed for ethylene glycol with the further of sulfuric acid, in liquid level alarm 22 can monitor in mixing vessel
Liquid level depth value and capable of emitting alarm, liquid level alarm 22 can be made of liquid level sensor and alarm device, and liquid level sensor
It is connect with controller line with alarm device, the liquid level depth value in liquid level sensor real-time monitoring mixing vessel is simultaneously transmitted to control
Device, alarm device are issued alarm signal by the control of controller, are higher than liquid level high level for liquid level in mixing vessel and are lower than liquid level
Different alarm signals can be used in the case where low value, as set two different colors of lamp on liquid level alarm 22 as alarm device
(such as red light and blue lamp), when liquid level is higher than liquid level high level in mixing vessel, a kind of lamp of color is bright (such as red light), when mixed
When liquid level is lower than liquid level low value in conjunction container, the lamp of another color is bright (such as blue lamp), naturally it is also possible to use different sound
Sound signal；Condenser 30 will steam the water vapour that water kettle 40 steams and congeal into water；Water kettle 40 is steamed, evaporates the vapor in it, and be
Ethylene glycol provides place with reacting for sulfuric acid；Kinetic pump 50 provides power for the mixing of ethylene glycol and sulfuric acid, circulation；Injector
60, the sulfuric acid negative pressure in charge funnel 62 is sucked, is mixed rapidly with ethylene glycol, to prevent local concentration excessive, temperature is excessively high,
Generate side reaction；Controller is inside set with predetermined high liquid level value, predetermined low liquid level value, and receives and sent out by liquid level alarm 22
The 20 liquid level depth value of mixing vessel sent, when the liquid level depth value received is not in predetermined high liquid level value and predetermined low liquid level value
Between when, controller control liquid level alarm 22 sound an alarm, controller can be single-chip microcontroller in practical application.
Further, the top of the condenser 30 is equipped with non-condensable gas export, and the non-condensable gas export pipeline is connected to
The tear drop pipe 61.Condenser and tear drop pipe are connected by pipeline, by the on-condensible gas steamed in condenser and a small amount of solidifying steaming
Vapour sucks in injector, not only reduces material loss, but also reduce environmental pollution, while seeking in condenser when injector work
The subnormal ambient made also is conducive to the evaporation of moisture, condensation；In the present invention, by sulfuric acid and ethylene glycol mixture acid vapor and
Glycol steam sucks injector, to make full use of.
Further, blender is provided in the steaming water kettle 40.Blender can accelerate to mix.
Further, baffle plate 23 is provided in the mixing vessel 20.Baffle plate 23 can accelerate to mix.
When it is implemented, 44 top of collet, the lower part of steaming water kettle 40 set collet import and jacket outlet respectively, hot fluid from
Collet import enters collet and heats to water kettle 40 is steamed, and flows out from jacket outlet.
Now in conjunction with the production process of metronidazole, illustrate present apparatus application method.
Embodiment 1
Step 1): 2- 5-nitro imidazole 48.07g is added in reaction kettle, and mass percent concentration 85% is added dropwise
Formic acid solvent 115.03g dissolves 2- 5-nitro imidazole, ethylene oxide 112.53g is gradually added at 30-40 DEG C, simultaneously
The sulfuric acid 115.02g for adding mass percent concentration 98% is warming up to 95 DEG C, and reaction 1h must be hydroxylated liquid；
Step 2): liquid to be hydroxylated is cooled to 10 DEG C, is adjusted to pH=10 with alkali hydroxide soln, places cooling, knot
A metronidazole 30.01g and first-time filtrate is obtained by filtration in crystalline substance；Obtained first-time filtrate is concentrated by evaporation, is cooling, crystallization, mistake
Filter, obtains alkali metal sulfates solid product and secondary filtrate；
Step 3): the secondary filtrate that vacuum distillation step 2) obtains obtains ethylene glycol by-product；
Step 4): closing outlet valve 31 and outlet valve 43, and standard-sized sheet walks around to valve 42 and air inlet valve 65, opens capping 21, will walk
Mixing vessel 20 is added by feed opening in the rapid ethylene glycol 3) obtained, covers capping 21, and quality percentage is added into charge funnel 62
The sulfuric acid 187.87g that specific concentration is 60%；
Step 5): starting kinetic pump 50 is slowly opened and the dropwise addition sulfuric acid of valve 63 is added dropwise, and ethylene glycol is mixed with sulfuric acid, controlled
It is arranged and stores predetermined high liquid level value, predetermined low liquid level value on device processed, adjusts the opening size for walking around to valve 42, make mixing vessel 20
Interior liquid level maintains between predetermined high liquid level value and predetermined low liquid level value；If it is high to be higher than the liquid level for liquid level in mixing vessel 20
Value, liquid level alarm 22 alarm, tune up and walk around to valve 42；If liquid level is lower than the liquid level low value, liquid level warning in mixing vessel 20
Device 22 is alarmed, and is turned down and is walked around to valve 42；
Step 6): holding meanss work, it is 100 DEG C to 120 DEG C that water kettle temperature degree is steamed in control, in 0.01-0.9 normal atmosphere
Pressure is evaporated under reduced pressure, and starts condenser 30, half-open to walk around to valve 42, slowly closing air inlet valve 65；To the sulfuric acid in charge funnel 62
It is added dropwise, closes and valve 63 is added dropwise, be evaporated to when there is no moisture to be distilled out of in water kettle 40, slowly unlatching air inlet valve 65 simultaneously tunes up
Walk around to valve 42；Turn off kinetic pump 50；Then outlet valve 31 is opened, the moisture content steamed is bled off；Outlet valve 43 is finally opened, is taken out
Steam raffinate；
Step 7): the 2- 5-nitro imidazole 47.97g of mass percent concentration 100% is added in reaction kettle, drop
Add the formic acid solvent 114.97g of mass percent concentration 85% to dissolve 2- 5-nitro imidazole, gradually adds at 30-40 DEG C
Enter the ethylene oxide 100.01g of mass percent concentration 100%, while the steaming raffinate that a dropping step 6 obtains, is warming up to 85-95
DEG C, reaction 1h must be hydroxylated liquid；
Step 8): liquid to be hydroxylated is cooled to 10 DEG C, is adjusted to pH=10 with alkali hydroxide soln, places cooling, knot
Secondary metronidazole 29.98g is obtained by filtration in crystalline substance.
In embodiment 1,112.53g ethylene oxide is put into for the first time, obtains a metronidazole 30.01g in step 2)；By second two
Containing sulfuric acid ethylene glycol rouge in the steaming raffinate that alcohol and sulfuric acid reaction obtain, 100.01g ethylene oxide is put into step 7), simultaneously
It is added dropwise and steams raffinate, secondary metronidazole 29.98g is obtained in step 8).Comparison is it is found that applying for ethylene glycol reduces ethylene oxide
Dosage, saved production cost.
Embodiment 2
Step 1): 2- 5-nitro imidazole 48.06g is added in reaction kettle, and mass percent concentration 85% is added dropwise
Formic acid solvent 115.01g dissolves 2- 5-nitro imidazole, ethylene oxide 112.55g is gradually added at 30-40 DEG C, simultaneously
The sulfuric acid 115.03g for adding mass percent concentration 98% is warming up to 95 DEG C, and reaction 1h must be hydroxylated liquid；
Step 2): liquid to be hydroxylated is cooled to 10 DEG C, is adjusted to pH=10 with alkali hydroxide soln, places cooling, knot
A metronidazole 30.02g and first-time filtrate is obtained by filtration in crystalline substance；Obtained first-time filtrate is concentrated by evaporation, is cooling, crystallization, mistake
Filter, obtains alkali metal sulfates solid product and secondary filtrate；
Step 3): the secondary filtrate that vacuum distillation step 2) obtains obtains ethylene glycol by-product；
Step 4): closing outlet valve 31 and outlet valve 43, and standard-sized sheet walks around to valve 42 and air inlet valve 65, opens capping 21, will walk
Mixing vessel 20 is added by feed opening in the rapid ethylene glycol 3) obtained, covers capping 21, and quality percentage is added into charge funnel 62
Specific concentration is 70% sulfuric acid 161.04g；
Step 5): starting kinetic pump 50 is slowly opened and the dropwise addition sulfuric acid of valve 63 is added dropwise, and ethylene glycol is mixed with sulfuric acid, controlled
It is arranged and stores predetermined high liquid level value, predetermined low liquid level value on device processed, adjusts the opening size for walking around to valve 42, make mixing vessel 20
Interior liquid level maintains between predetermined high liquid level value and predetermined low liquid level value；If it is high to be higher than the liquid level for liquid level in mixing vessel 20
Value, liquid level alarm 22 alarm, tune up and walk around to valve 42；If liquid level is lower than the liquid level low value, liquid level warning in mixing vessel 20
Device 22 is alarmed, and is turned down and is walked around to valve 42；
Step 6): holding meanss work, it is 100 DEG C to 120 DEG C that water kettle temperature degree is steamed in control, in 0.01-0.9 normal atmosphere
Pressure is evaporated under reduced pressure, and starts condenser 30, half-open to walk around to valve 42, slowly closing air inlet valve 65；To the sulfuric acid in charge funnel 62
It is added dropwise, closes and valve 63 is added dropwise, be evaporated to when there is no moisture to be distilled out of in water kettle 40, slowly unlatching air inlet valve 65 simultaneously tunes up
Walk around to valve 42；Turn off kinetic pump 50；Then outlet valve 31 is opened, the moisture content steamed is bled off；Outlet valve 43 is finally opened, is taken out
Steam raffinate；
Step 7): the 2- 5-nitro imidazole 48.03g of mass percent concentration 100% is added in reaction kettle, drop
Add the formic acid solvent 108.3g of mass percent concentration 90% to dissolve 2- 5-nitro imidazole, is gradually added at 30-40 DEG C
The ethylene oxide 90.05g of mass percent concentration 100%, while a dropping step 6) obtained steaming raffinate, it is warming up to 85-95 DEG C,
Reaction 1h must be hydroxylated liquid；
Step 8): liquid to be hydroxylated is cooled to 10 DEG C, is adjusted to pH=10 with alkali hydroxide soln, places cooling, knot
Secondary metronidazole 30.02g is obtained by filtration in crystalline substance.
In embodiment 2,112.55g ethylene oxide is put into for the first time, obtains a metronidazole 30.02g in step 2)；By second two
Containing sulfuric acid ethylene glycol rouge in the steaming raffinate that alcohol and sulfuric acid reaction obtain, 90.05g ethylene oxide is put into step 7), simultaneously
It is added dropwise and steams raffinate, secondary metronidazole 30.02g is obtained in step 8).Comparison is it is found that applying for ethylene glycol reduces ethylene oxide
Dosage, saved production cost.
Embodiment 3
Step 1): 2- 5-nitro imidazole 48.05g is added in reaction kettle, and mass percent concentration 85% is added dropwise
Formic acid solvent 115.05g dissolves 2- 5-nitro imidazole, ethylene oxide 112.53g is gradually added at 30-40 DEG C, simultaneously
The sulfuric acid 115.05g for adding mass percent concentration 98% is warming up to 95 DEG C, and reaction 1h must be hydroxylated liquid；
Step 2): liquid to be hydroxylated is cooled to 10 DEG C, is adjusted to pH=10 with alkali hydroxide soln, places cooling, knot
A metronidazole 29.98g and first-time filtrate is obtained by filtration in crystalline substance；Obtained first-time filtrate is concentrated by evaporation, is cooling, crystallization, mistake
Filter, obtains alkali metal sulfates solid product and secondary filtrate；
Step 3): the secondary filtrate that vacuum distillation step 2) obtains obtains ethylene glycol by-product；
Step 4): closing outlet valve 31 and outlet valve 43, and standard-sized sheet walks around to valve 42 and air inlet valve 65, opens capping 21, will walk
Mixing vessel 20 is added by feed opening in the rapid ethylene glycol 3) obtained, covers capping 21, and quality percentage is added into charge funnel 62
The sulfuric acid 140.94g that specific concentration is 80%；
Step 5): starting kinetic pump 50 is slowly opened and the dropwise addition sulfuric acid of valve 63 is added dropwise, and ethylene glycol is mixed with sulfuric acid, controlled
It is arranged and stores predetermined high liquid level value, predetermined low liquid level value on device processed, adjusts the opening size for walking around to valve 42, make mixing vessel 20
Interior liquid level maintains between predetermined high liquid level value and predetermined low liquid level value；If it is high to be higher than the liquid level for liquid level in mixing vessel 20
Value, liquid level alarm 22 alarm, tune up and walk around to valve 42；If liquid level is lower than the liquid level low value, liquid level warning in mixing vessel 20
Device 22 is alarmed, and is turned down and is walked around to valve 42；
Step 6): holding meanss work, it is 100 DEG C to 120 DEG C that water kettle temperature degree is steamed in control, in 0.01-0.9 normal atmosphere
Pressure is evaporated under reduced pressure, and starts condenser 30, half-open to walk around to valve 42, slowly closing air inlet valve 65；To the sulfuric acid in charge funnel 62
It is added dropwise, closes and valve 63 is added dropwise, be evaporated to when there is no moisture to be distilled out of in water kettle 40, slowly unlatching air inlet valve 65 simultaneously tunes up
Walk around to valve 42；Turn off kinetic pump 50；Then outlet valve 31 is opened, the moisture content steamed is bled off；Outlet valve 43 is finally opened, is taken out
Steam raffinate；
Step 7): the 2- 5-nitro imidazole 48.03g of mass percent concentration 100% is added in reaction kettle, drop
Add the formic acid solvent 102.5g of mass percent concentration 95% to dissolve 2- 5-nitro imidazole, is gradually added at 30-40 DEG C
The ethylene oxide 70.02g of mass percent concentration 100%, while a dropping step 6) obtained steaming raffinate, it is warming up to 85-95 DEG C,
Reaction 1h must be hydroxylated liquid；
Step 8): liquid to be hydroxylated is cooled to 10 DEG C, is adjusted to pH=10 with alkali hydroxide soln, places cooling, knot
Secondary metronidazole 30.05g is obtained by filtration in crystalline substance.
In embodiment 3,112.53g ethylene oxide is put into for the first time, obtains a metronidazole 29.98g in step 2)；By second two
Containing sulfuric acid ethylene glycol rouge in the steaming raffinate that alcohol and sulfuric acid reaction obtain, 70.02g ethylene oxide is put into step 7), simultaneously
It is added dropwise and steams raffinate, secondary metronidazole 30.05g is obtained in step 8).Comparison is it is found that applying for ethylene glycol reduces ethylene oxide
Dosage, saved production cost.
Claims (4)
1. a kind of device for realizing ethylene glycol by-product recycled in metronidazole production characterized by comprising
Liquid seal trough (10), inside fills lye；
Mixing vessel (20), top offer feed opening and by covering (21) sealing, and upper part is equipped with outlet port, under
Portion walks around to import and first equipped with first and walks around to outlet, is equipped with liquid level alarm (22) in mixing vessel；The outlet port
It is connect with liquid seal trough (10) pipeline；
Condenser (30), outlet are provided with outlet valve (31)；
It steams water kettle (40), bottom is equipped with second and walks around to import, second walks around to outlet and discharge port, and top is equipped with steam and is discharged
Pipe, the vapour-discharge tube connect the import of the condenser (30)；Described second, which walks around to import, walks around to outlet with first and passes through
Walk around to pipe (41) connection, walk around to pipe (41) be equipped with walk around to valve (42)；The discharge outlet is provided with outlet valve (43)；
The inlet pipeline connection described second of kinetic pump (50) and injector (60), kinetic pump (50) walks around to outlet, outlet and
First inlet pipeline of injector (60) connects；It is provided with vertical tear drop pipe (61) in second import of injector (60), drips
The upper end of expects pipe (61) is equipped with charge funnel (62), and tear drop pipe (61), which is equipped with, is added dropwise valve (63), and tear drop pipe is provided on (61)
Winding pipe (64) sets air inlet valve (65) in winding pipe；The outlet conduit of injector (60) be connected to described first walk around into
Mouthful；
Controller, the controller is interior to be arranged and is stored with predetermined high liquid level value, predetermined low liquid level value, controller and liquid level warning
Device (22) connection.
2. the apparatus according to claim 1, which is characterized in that the top of the condenser (30) goes out equipped with on-condensible gas
Mouthful, the non-condensable gas export pipeline is connected to the tear drop pipe (61).
3. the apparatus according to claim 1, which is characterized in that be provided with blender in the steaming water kettle (40).
4. device as claimed in any of claims 1 to 3, which is characterized in that setting in the mixing vessel (20)
There are baffle plate (23).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821987099.9U CN209276417U (en) | 2018-11-29 | 2018-11-29 | Realize the device of ethylene glycol by-product recycled in metronidazole production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821987099.9U CN209276417U (en) | 2018-11-29 | 2018-11-29 | Realize the device of ethylene glycol by-product recycled in metronidazole production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN209276417U true CN209276417U (en) | 2019-08-20 |
Family
ID=67608853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201821987099.9U Expired - Fee Related CN209276417U (en) | 2018-11-29 | 2018-11-29 | Realize the device of ethylene glycol by-product recycled in metronidazole production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN209276417U (en) |
-
2018
- 2018-11-29 CN CN201821987099.9U patent/CN209276417U/en not_active Expired - Fee Related
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN209276417U (en) | Realize the device of ethylene glycol by-product recycled in metronidazole production | |
| CN103373747B (en) | The evaporating concentrating method of yeast wastewater | |
| CN207362101U (en) | A kind of crude naphthalene fine-processing production line | |
| CN109293573A (en) | The method, apparatus and application of ethylene glycol by-product recycled in metronidazole production | |
| CN107722053A (en) | A kind of rectificating method of dimethylphosphite | |
| CN109277050B (en) | Acetaldehyde negative pressure dropwise adding method and device in metronidazole production | |
| CN217367186U (en) | Dealcoholization device for producing special plasticizer for automotive interior | |
| CN215462095U (en) | Alkali adding device for wool aldehyde refining | |
| CN207276584U (en) | A kind of fragrant plant hydrosol extraction of essential oil system | |
| CN103387483B (en) | Production device and process of methanol alkali metal salts | |
| CN109096206A (en) | A kind of method of acidity photocatalytic method synthesis carbendazim | |
| CN216653417U (en) | Chlorobutane apparatus for producing | |
| CN215027688U (en) | Complex iron desulfurization sulfur thick liquid integration processing apparatus | |
| CN211215473U (en) | Fluorescent brightener waste liquid enrichment facility | |
| CN213528616U (en) | Hydrolysis reaction kettle with constant temperature heat preservation function | |
| CN109179331A (en) | A kind of production system of neutralisation production bromide | |
| CN209271399U (en) | Acetaldehyde negative pressure Dropping feeder in a kind of production of metronidazole | |
| CN107281772A (en) | Destilling tower, stoste purification system and process for purifying raw | |
| CN113274751A (en) | Preparation system of potassium persulfate | |
| CN202823359U (en) | Reactor capable of preparing anhydrous peroxycarboxylic acid continuously | |
| CN207738478U (en) | A kind of intermittent MVR structures | |
| CN207079008U (en) | A kind of fine phosphate production system | |
| CN220258037U (en) | Paint synthesis reaction device | |
| CN218130014U (en) | Distillation device for preparing furfural | |
| CN218530884U (en) | Methyl ethyl carbonate yield increasing device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190820 Termination date: 20201129 |