CN109776256A - The recyclable device of methylene chloride in a kind of production of cefuroxime acid - Google Patents
The recyclable device of methylene chloride in a kind of production of cefuroxime acid Download PDFInfo
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- CN109776256A CN109776256A CN201910141666.1A CN201910141666A CN109776256A CN 109776256 A CN109776256 A CN 109776256A CN 201910141666 A CN201910141666 A CN 201910141666A CN 109776256 A CN109776256 A CN 109776256A
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Abstract
The present invention relates to the recyclable devices of methylene chloride in a kind of production of cefuroxime acid, including dehydration device, division box and acquisition device；The dehydration device, which is equipped with, is passed through methylene chloride mother liquor in the production of cefuroxime acid and the liquid inlet of methylene chloride liquid that mother liquor is distillated into impurity and entrapped moisture, and outlet connects the entrance of the division box so that the methylene chloride liquid for the entrapped moisture isolated to be sent into the division box and is separated into water and methylene chloride finished product after distilling；The outlet of the division box is separately connected the dehydration device and the acquisition device, and then isolated water is flowed back into the dehydration device circulation distillation and isolated methylene chloride finished product is sent into the acquisition device and is collected.The water content for the methylene chloride that the device is recovered to is lower than 0.05%, and purity > 99% can be reused directly.
Description
Technical field
The present invention relates to chemical products separation technology fields, and in particular to methylene chloride in a kind of production of cefuroxime acid
Recyclable device.
Background technique
Methylene chloride (CH2Cl2) is a kind of colorless and transparent, highly volatile, the liquid with irritation aromatic odor, boiling point
It is 40.2 DEG C.It dissolves in about 50 times of water, azeotropic mixture can be formed with water, ethyl alcohol, acetone, methanol etc..It is nonflammable, often
Substitution solvent as flammable solvent petroleum ether and ether.Methylene chloride is the common solvent in medication chemistry, especially in head
As common crystallization solvent in spore class pharmaceutical synthesis.Methylene chloride not only causes seriously to pollute to environment, economically caused by
Loss is also very big.In order to reduce production cost, the methylene chloride generated in production is recycled, to reach environmentally friendly row
Put the purpose of standard and waste liquid circulation recycling.
Cefuroxime acid is the key intermediate of the raw material of national essential drugs cefuroxime sodium for injection；Methylene chloride tool
Have that nonflammable, solvability is strong, the lesser feature of toxicity, is one of the solvent of cefuroxime acid synthesis technology first choice.Cephalo furan
The methylene chloride mother liquor that sad production process generates, it is complex in composition, comprising: moisture 2.5%, methylene chloride 85%, DMAC10%,
Solid salt 2.5% etc., and methylene chloride standard used in producing are as follows: moisture < 0.05%, coloration < (Pt-Co) 10 unit norm
Color solution, turbidity<5#, methylene chloride purity>99%.The process of methylene chloride solvent circular treatment is the molecular sieve pair with drying
Rectifying again after methylene chloride is dehydrated or is dried with calcium chloride.Use molecular sieve to the methylene chloride of recycling during former recovery process
Solvent is dehydrated, and since molecular sieve use process is lossy, and after molecular sieve water suction, regeneration treatment is not thorough, and is easily caused
The methylene chloride solvent moisture content of recovery processing is high, and menstruum is lower and operating process is time-consuming and laborious, labour effect
Rate is low, leads to this recovery method higher cost, it is therefore desirable to improve to former recovery process.
Summary of the invention
In conclusion in order to overcome the deficiencies of the prior art, technical problem to be solved by the invention is to provide a kind of cephalos
The recyclable device of methylene chloride, the methylene chloride being recovered to can be reused directly in the production of cefuroxime acid.
The technical scheme to solve the above technical problems is that methylene chloride returns in a kind of production of cefuroxime acid
Receiving apparatus, including dehydration device, division box and acquisition device；The dehydration device, which is equipped with, is passed through dichloro in the production of cefuroxime acid
The liquid inlet of methane mother liquor, and mother liquor is distillated into the dichloromethane solution of impurity and entrapped moisture by the dehydration device
Body, outlet connect the entrance of the division box will divide water described in the methylene chloride liquid for the entrapped moisture isolated feeding
Water and methylene chloride finished product are separated into device and after distilling；The outlet of the division box be separately connected the dehydration device and
The acquisition device, and then isolated water flowed back into the distillation of dehydration device circulation and by isolated methylene chloride finished product
It is sent into the acquisition device and collects.
The beneficial effects of the present invention are: the water content for the methylene chloride that the device is recovered to be lower than 0.05%, purity >
99%, it can directly reuse.
Based on the above technical solution, the present invention can also be improved as follows:
Further, the dehydration device include dichloro weight-removing column kettle, dichloro weight-removing column, dichloro weight-removing column first-stage condenser and
Dichloro weight-removing column secondary condenser；The dichloro weight-removing column kettle is equipped with the liquid inlet, on the dichloro weight-removing column kettle also
Mother liquor is heated equipped with steam is passed through to isolate the steam inlet of the methylene chloride gas of entrapped moisture from mother liquor；The dichloro
The gaseous phase outlet of weight-removing column kettle connects the gas phase entrance of the dichloro weight-removing column；The gaseous phase outlet of the dichloro weight-removing column connects institute
State the gas phase entrance of dichloro weight-removing column first-stage condenser, the residual air outlet connection described two of the dichloro weight-removing column first-stage condenser
The gas phase entrance of chlorine weight-removing column secondary condenser；The dichloro weight-removing column first-stage condenser and the dichloro weight-removing column B-grade condensation
The methylene chloride gas of entrapped moisture is condensed into liquid and is separated into two-way after flowing out and converge from respective cold liquid outlet by device
Branch, wherein branch described in the first via is flowed back into the dichloro weight-removing column by circulation line so that a part of entrapped moisture
Methylene chloride liquid redistillation, branch described in the second tunnel connect the entrance of the division box so that another portion by water-division pipeline
The methylene chloride liquid of entrapped moisture is divided to be sent into the division box.
Beneficial effect using above-mentioned further scheme is: mother liquor being carried out primary thick steaming, removes DMAC, solid in mother liquor
Salt and portion of water.
Further, dehydration pneumatic control valve and dehydration flow are equipped on the circulation line and the water-division pipeline
Meter.
Further, the dehydration device further includes dichloro weight-removing column B-grade condensation gas-liquid separator；The dichloro weight-removing column
The cold liquid outlet of secondary condenser after the dichloro weight-removing column B-grade condensation gas-liquid separator again with the dichloro weight-removing column one
The cold liquid outlet confluence of grade condenser.
Beneficial effect using above-mentioned further scheme is: a small amount of gas can be mingled with by slightly steaming condensed liquid, be removed
It is mingled with this portion gas in a liquid, is allowed to not be blended in pipeline.
Further, the division box includes dichloro dehydration column reboiler, dichloro dehydrating tower, the condensation of dichloro dehydrating tower level-one
Device, dichloro dehydrating tower secondary condenser, phase separation tank and dichloro dehydrating tower cooler；Branch described in second tunnel passes through the distributive pipe
The methylene chloride liquid of entrapped moisture is sent into the dichloro dehydrating tower by the entrance that road connects the dichloro dehydrating tower；The dichloro
Dehydration column reboiler is equipped with the steam port for being passed through steam；The leakage fluid dram of the dichloro dehydration tower bottom connects the dichloro dehydrating tower
The liquid phase entrance of reboiler the methylene chloride liquid of entrapped moisture to be heated into the gas of the methylene chloride of entrapped moisture, and
The gaseous phase outlet of the dichloro dehydration column reboiler connects the gas phase entrance of the dichloro dehydrating tower；The gas of the dichloro dehydrating tower
Mutually outlet connects the gas phase entrance of the dichloro dehydrating tower first-stage condenser, and the residual air of the dichloro dehydrating tower first-stage condenser goes out
Mouth connects the gas phase entrance of the dichloro dehydrating tower secondary condenser；The dichloro dehydrating tower first-stage condenser and the dichloro are de-
The methylene chloride gas of entrapped moisture is condensed into liquid and converged again from the outflow of respective cold liquid outlet by water tower secondary condenser
The entrance of the dichloro dehydrating tower cooler is connected afterwards, and the outlet of the dichloro dehydrating tower cooler connects in the middle part of the phase separation tank
Import aqueous is separated into so that the methylene chloride liquid of entrapped moisture is sent into the phase separation tank and up and down in the phase separation tank
Layer and dichloromethane layer；The light phase export of the phase separation tank by return line connect the dichloro weight-removing column kettle return liquid mouth with
Isolated upper layer aqueous is flowed back into after the dichloro weight-removing column kettle to recycle and is distilled to recover, heavy out passes through acquisition pipeline
Lower layer's methylene chloride reflux that the refluxing opening at the top of the dichloro dehydrating tower is connected will separate is into the dichloro dehydrating tower；?
The bottom side of the dichloro dehydrating tower is equipped with the extraction mouth of discharge methylene chloride, and the extraction mouth connects the acquisition device.
Beneficial effect using above-mentioned further scheme is: the mother liquor once slightly steam being carried out rectifying again, and is evaporated
Divide and continuously divide water with phase separation tank, is recovered to satisfactory methylene chloride to remove remaining moisture.
Further, point water pneumatic control valve and point water flow are equipped on the return line and the collection tube road
Meter.
Further, the acquisition device includes dichloro finished product cooler and dichloro tank to be checked；Described in the extraction mouth connection
The entrance of dichloro finished product cooler, the outlet of the dichloro finished product cooler, which will connect dichloro tank to be checked by discharge nozzle, to be divided
From dichloro finished product it is cooling after obtain finished product and be sent into dichloro tank to be checked；Control valve is equipped on the discharge nozzle.
Beneficial effect using above-mentioned further scheme is: the satisfactory methylene chloride finished product being recovered to is gathered up
Come.
Further, the dehydration device further includes dichloro dehydrating tower B-grade condensation gas-liquid separator；The dichloro dehydrating tower
The cold liquid outlet of secondary condenser after the dichloro dehydrating tower B-grade condensation gas-liquid separator again with the dichloro dehydrating tower one
The cold liquid outlet confluence of grade condenser.
Beneficial effect using above-mentioned further scheme is: the condensed liquid of rectifying can be mingled with a small amount of gas, remove
It is mingled with this portion gas in a liquid, is allowed to not be blended in pipeline.
It further, further include handling the dichloro weight-removing column B-grade condensation gas-liquid separator, the dichloro dehydrating tower second level
The tail for condensing the tail gas of gas-liquid separator, the phase separation tank and dichloro tank discharge to be checked coagulates system；The dichloro weight-removing column
B-grade condensation gas-liquid separator, the dichloro dehydrating tower B-grade condensation gas-liquid separator, the phase separation tank and the dichloro are to be checked
The evacuation port of tank connects the tail and coagulates system.
Further, it includes tail condenser, tail condenser gas-liquid separator and tail lime set tank that the tail, which coagulates system,；The de- weight of the dichloro
Tower B-grade condensation gas-liquid separator, the dichloro dehydrating tower B-grade condensation gas-liquid separator, the phase separation tank and the dichloro wait for
The evacuation port of inspection tank is incorporated to the gas phase entrance of the tail condenser, and the condensate outlet of the tail condenser is through the tail condenser gas-liquid point
It is solidifying that evacuation port from the entrance for reconnecting the tail lime set tank after device, and the tail condenser gas-liquid separator also connects the tail
The gas phase entrance of device, the outlet connection dichloro weight-removing column kettle of the tail lime set tank return liquid mouth.
Beneficial effect using above-mentioned further scheme is: handling the tail gas condensing being discharged in each link and carries out again
Methylene chloride is recycled, the pollution of environment is reduced and improves the rate of recovery.
Detailed description of the invention
Fig. 1 is that overall structure of the invention is illustrated.
In attached drawing, parts list represented by the reference numerals are as follows:
1. dichloro weight-removing column kettle；2. dichloro weight-removing column；3. dichloro weight-removing column first-stage condenser；4. dichloro weight-removing column second level is cold
Condenser；5. dichloro weight-removing column B-grade condensation gas-liquid separator；6. dichloro dehydration column reboiler；7. dichloro dehydrating tower；8. dichloro is de-
Water tower first-stage condenser；9. dichloro dehydrating tower secondary condenser；10. dichloro dehydrating tower B-grade condensation gas-liquid separator；11. split-phase
Tank；12. dichloro dehydrating tower cooler；13. dichloro finished product cooler；14. dichloro tank to be checked；15. tail condenser；16. tail condenser gas
Liquid/gas separator；17. tail lime set tank.
Specific embodiment
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the invention.
As shown in Figure 1, in a kind of production of cefuroxime acid methylene chloride recyclable device, including dehydration device, water is divided to fill
It sets and acquisition device.The dehydration device is equipped with the liquid inlet for being passed through methylene chloride mother liquor in the production of cefuroxime acid, and described
Mother liquor is distillated into the methylene chloride liquid of impurity and entrapped moisture by dehydration device, and outlet connects the division box
The methylene chloride liquid for the entrapped moisture isolated to be sent into the division box and be separated into water and two after distilling by entrance
Chloromethanes finished product.The outlet of the division box is separately connected the dehydration device and the acquisition device, and then by separation
Water flows back into the dehydration device circulation distillation and isolated methylene chloride finished product is sent into the acquisition device and gathers up
Come.
The dehydration device includes dichloro weight-removing column kettle 1, dichloro weight-removing column 2, dichloro weight-removing column first-stage condenser 3 and dichloro
Weight-removing column secondary condenser 4.The dichloro weight-removing column kettle 1 is equipped with the liquid inlet, also sets on the dichloro weight-removing column kettle 1
There is the steam inlet for being passed through steam heating mother liquor to isolate the methylene chloride gas of entrapped moisture from mother liquor.The dichloro is de-
The gaseous phase outlet of weight tower reactor 1 connects the gas phase entrance of the dichloro weight-removing column 2.The gaseous phase outlet of the dichloro weight-removing column 2 connects
The gas phase entrance of the dichloro weight-removing column first-stage condenser 3, the residual air outlet connection institute of the dichloro weight-removing column first-stage condenser 3
State the gas phase entrance of dichloro weight-removing column secondary condenser 4.The dichloro weight-removing column first-stage condenser 3 and the dichloro weight-removing column two
The methylene chloride gas of entrapped moisture is condensed into liquid and divided again after flowing out and converge from respective cold liquid outlet by grade condenser 4
At two-way branch, wherein branch described in the first via is flowed back into the dichloro weight-removing column 2 by circulation line so that a part is pressed from both sides
Methylene chloride liquid redistillation with moisture, branch described in the second tunnel by water-division pipeline connect the entrance of the division box with
It is sent into the methylene chloride liquid of another part entrapped moisture in the division box.In the circulation line and the distributive pipe
Road is equipped with dehydration pneumatic control valve and dehydration flowmeter.The dehydration device further includes dichloro weight-removing column B-grade condensation gas
Liquid/gas separator 5.The cold liquid outlet of the dichloro weight-removing column secondary condenser 4 is through the dichloro weight-removing column B-grade condensation gas-liquid separation
Converge again with the cold liquid outlet of the dichloro weight-removing column first-stage condenser 3 after device 5.
The division box include dichloro dehydration column reboiler 6, dichloro dehydrating tower 7, dichloro dehydrating tower first-stage condenser 8,
Dichloro dehydrating tower secondary condenser 9, phase separation tank 11 and dichloro dehydrating tower cooler 12.Branch described in second tunnel divides water by described
The methylene chloride liquid of entrapped moisture is sent into the dichloro dehydrating tower 7 by the entrance that pipeline connects the dichloro dehydrating tower 7.It is described
Dichloro dehydration column reboiler 6 is equipped with the steam port for being passed through steam.The leakage fluid dram of 7 bottom of dichloro dehydrating tower connects the dichloro
The methylene chloride liquid of entrapped moisture to be heated into the gas of the methylene chloride of entrapped moisture by the liquid phase entrance of dehydration column reboiler 6
Body, and the gaseous phase outlet of the dichloro dehydration column reboiler 6 connects the gas phase entrance of the dichloro dehydrating tower 7.The dichloro
The gaseous phase outlet of dehydrating tower 7 connects the gas phase entrance of the dichloro dehydrating tower first-stage condenser 8, and the dichloro dehydrating tower level-one is cold
The residual air outlet of condenser 8 connects the gas phase entrance of the dichloro dehydrating tower secondary condenser 9.The dichloro dehydrating tower level-one condensation
The methylene chloride gas of entrapped moisture is condensed into liquid and from respective cold by device 8 and the dichloro dehydrating tower secondary condenser 9
Liquid outlet outflow connects the entrance of the dichloro dehydrating tower cooler 12 after converging again, the dichloro dehydrating tower cooler 12 goes out
Mouth connects the import at 11 middle part of phase separation tank the methylene chloride liquid of entrapped moisture is sent into the phase separation tank 11 and in institute
It states and is separated into aqueous layer and dichloromethane layer in phase separation tank 11 up and down.The light phase export of the phase separation tank 11 is connected by return line
Connect the dichloro weight-removing column kettle 1 returns liquid mouth to recycle after isolated upper layer aqueous is flowed back into the dichloro weight-removing column kettle 1
It is distilled to recover, lower layer of the heavy out by the refluxing opening at 7 top of dichloro dehydrating tower described in acquisition piping connection will separate
Methylene chloride reflux is into the dichloro dehydrating tower 7.It is dynamic that point aqueous vapor is equipped on the return line and the collection tube road
Regulating valve and divide water ga(u)ge.The extraction mouth of discharge methylene chloride, the extraction are equipped in the bottom side of the dichloro dehydrating tower 7
Mouth connects the acquisition device.The dehydration device further includes dichloro dehydrating tower B-grade condensation gas-liquid separator 10.The dichloro
The cold liquid outlet of dehydrating tower secondary condenser 9 after the dichloro dehydrating tower B-grade condensation gas-liquid separator 10 again with the dichloro
The cold liquid outlet of dehydrating tower first-stage condenser 8 is converged.
The acquisition device includes dichloro finished product cooler 13 and dichloro tank 14 to be checked.The extraction mouth connects the dichloro
The entrance of finished product cooler 13, the outlet of the dichloro finished product cooler 13 connects dichloro tank 14 to be checked by discharge nozzle will
Finished product is obtained after isolated dichloro finished product is cooling and is sent into dichloro tank 14 to be checked.Control valve is equipped on the discharge nozzle
Door.
The device further includes handling the dichloro weight-removing column B-grade condensation gas-liquid separator 5, the dichloro dehydrating tower second level
The tail for condensing the tail gas that gas-liquid separator 10, the phase separation tank 11 and dichloro tank 14 to be checked are discharged coagulates system.The dichloro
Weight-removing column B-grade condensation gas-liquid separator 5, the dichloro dehydrating tower B-grade condensation gas-liquid separator 10, the phase separation tank 11 and institute
The evacuation port for stating dichloro tank 14 to be checked connects the tail and coagulates system.It includes tail condenser 15, tail condenser gas-liquid point that the tail, which coagulates system,
From device 16 and tail lime set tank 17.The dichloro weight-removing column B-grade condensation gas-liquid separator 5, the dichloro dehydrating tower B-grade condensation gas
The evacuation port of liquid/gas separator 10, the phase separation tank 11 and dichloro tank 14 to be checked is incorporated to the gas phase entrance of the tail condenser 15,
The condensate outlet of the tail condenser 15 reconnects the entrance of the tail lime set tank 17 after the tail condenser gas-liquid separator 16,
And the evacuation port of the tail condenser gas-liquid separator 16 also connects the gas phase entrance of the tail condenser 15, the tail lime set tank 17
Outlet connect the dichloro weight-removing column kettle 1 return liquid mouth.
One complete course of work of the device is described below:
First step dehydration: cefuroxime acid dichloride methane mother liquor (composition: moisture 2.5%, methylene chloride 85%, DMAC10%, salt
2.5%) entered in dichloro weight-removing column kettle 1 by liquid inlet, there is U-shaped heating tube bundle and collet in dichloro weight-removing column kettle 1,0.45-
To heat mother liquor in the U-shaped heating tube bundle and collet that 0.60Mpa steam is passed through in dichloro weight-removing column kettle 1, pneumatic control valve is adjusted
The quantity of steam being passed through is 400-800kg/h.Since the boiling point of water is 100 DEG C, the boiling point of methylene chloride is 39.5 DEG C, and
DMAC and salt are solid, therefore a part of water, DMAC and salt are discharged into treatment tank after dichloro weight-removing column kettle 1 in mother liquor
It performs corresponding processing, and the methylene chloride in mother liquor becomes gas and entrapped moisture (two after heating in dichloro weight-removing column kettle 1
Chloromethanes and water can generate azeotropic meeting entrapped moisture: moisture content 0.3%, methylene chloride 99.7%) pass sequentially through dichloro weight-removing column one
Grade condenser 3 and dichloro weight-removing column secondary condenser 4 so far remove a part of water, DMAC and salt in mother liquor.To dichloro weight-removing column
The collet of first-stage condenser 3 leads to recirculated water, and the collet of dichloro weight-removing column secondary condenser 4 leads to formation of 7 DEG C of cold water to heating
The methylene chloride gas phase of entrapped moisture carries out heat exchange condensation, and recirculated water, 7 DEG C of cold water walk dichloro weight-removing column first-stage condenser 3 or two
The tube layer of chlorine weight-removing column secondary condenser 4, methylene chloride gas phase walk the shell side of condenser.3 He of dichloro weight-removing column first-stage condenser
Fraction, that is, entrapped moisture methylene chloride liquid phase a part of the heat exchange condensation of dichloro weight-removing column secondary condenser 4 passes through each autocondensation
Liquid outlet carries out chemical industry distillation operation through first via branch return to dichloro weight-removing column 2；The dichloro of another part entrapped moisture
Methane liquid phase branches into dichloro dehydrating tower 7, first via branch and the second tunnel branch through the second tunnel and is gated by pneumatic control valve
System, control reflux ratio are 3-4.The temperature for controlling 7 middle part of dichloro dehydrating tower is 37.5-39.5 DEG C, the temperature 37.5-of tower top
39.0 DEG C, tower top pressure is 0-5Kpa.The methylene chloride of thick rectifying and dewatering is produced into dichloro dehydrating tower 7, produced quantity control exists
400—700L/h.7 column bottom temperature of dichloro dehydrating tower is controlled at 75 DEG C or more, 0-15Kpa of pressure, kettle liquid is emitted into highly concentrated dirt
Water treating pond.
Second step is a point water: 6 steam-heating pipe entrance of dichloro dehydration column reboiler leads to 0.45-0.60Mpa steam heating two
Chlorine dehydrating tower 7 controls 400-800kg/h of quantity of steam by pneumatic control valves.The dichloro of entrapped moisture in dichloro dehydrating tower 7
Become the dichloromethane solution gas of entrapped moisture after the heating of methane liquid phase and passes sequentially through dichloro dehydrating tower first-stage condenser 8 and two
Chlorine dehydrating tower secondary condenser 9.Lead to recirculated water, dichloro dehydrating tower B-grade condensation to the collet of dichloro dehydrating tower first-stage condenser 8
The collet of device 9 leads to 7 DEG C of cold water and condenses to the dichloromethane solution gas converting heat of entrapped moisture, and recirculated water, 7 DEG C of cold water walk dichloro dehydration
The tube layer of tower first-stage condenser 8 or dichloro dehydrating tower secondary condenser 9, methylene chloride gas phase walk dichloro dehydrating tower first-stage condenser
8 and dichloro dehydrating tower secondary condenser 9 shell side.By dichloro dehydrating tower first-stage condenser 8 and dichloro dehydrating tower secondary condenser 9
Dichloromethane fraction, that is, entrapped moisture methylene chloride liquid of heat exchange condensation enters dichloro dehydrating tower through respective cold liquid outlet
Cooler 12 leads to 7 DEG C of cold water to 12 tube layer of methylene chloride cooler and carries out heat exchange cooling to the methylene chloride liquid of entrapped moisture,
The methylene chloride liquid of entrapped moisture after cooling enters phase separation tank 11 by pipeline from the outlet of dichloro dehydrating tower cooler 12 and divides
Water is separated into aqueous layer and methylene chloride according to the methylene chloride liquid of density difference entrapped moisture above and below in phase separation tank 11
Layer, i.e. methylene chloride is in lower layer, and for aqueous on upper layer, the methylene chloride of lower layer, which all flows back into, participates in heat transfer in dichloro dehydrating tower 7
Process, upper layer aqueous are flowed back into recycle in dichloro weight-removing column kettle 1 and be distilled to recover.
By 7 continuous band water of dichloro dehydrating tower to phase separation tank 11, phase separation tank 11 continuously divides water, in 7 bottom side of dichloro dehydrating tower
Mouth sample detection is produced, moisture when purity is greater than 99%, passes through 7 side take-off mouth of dichloro dehydrating tower and dichloro less than 0.05%
The pipeline of 14 entrance of tank to be checked produces qualified methylene chloride into dichloro tank 14 to be checked.
Third step tail gas condensing: the dichloro weight-removing column B-grade condensation gas-liquid separator 5, the dichloro dehydrating tower second level are cold
The gas phase that the evacuation port of solidifying gas-liquid separator 10, the phase separation tank 11 and dichloro tank 14 to be checked is incorporated to the tail condenser 15 enters
Mouthful, lead to low-temperature glycol condensation, the dichloro weight-removing column B-grade condensation gas-liquid separator 5, dichloro dehydration to tail condenser 15
The tail gas of tower B-grade condensation gas-liquid separator 10, the phase separation tank 11 and dichloro tank 14 to be checked enters the condensation of tail condenser 15
It collects.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. the recyclable device of methylene chloride in a kind of cefuroxime acid production, which is characterized in that including dehydration device, division box
And acquisition device；The dehydration device is equipped with the liquid inlet for being passed through methylene chloride mother liquor in the production of cefuroxime acid, and described de-
Mother liquor is distillated into the methylene chloride liquid of impurity and entrapped moisture by water installations, and outlet connects entering for the division box
Mouthful the methylene chloride liquid for the entrapped moisture isolated to be sent into the division box and is separated into water and dichloro after distilling
Methane finished product；The outlet of the division box is separately connected the dehydration device and the acquisition device, and then by isolated water
It flows back into the dehydration device circulation distillation and isolated methylene chloride finished product is sent into the acquisition device and collect.
2. the recyclable device of methylene chloride in cefuroxime acid production according to claim 1, which is characterized in that described de-
Water installations include dichloro weight-removing column kettle (1), dichloro weight-removing column (2), dichloro weight-removing column first-stage condenser (3) and dichloro weight-removing column two
Grade condenser (4)；The dichloro weight-removing column kettle (1) is equipped with the liquid inlet, is additionally provided on the dichloro weight-removing column kettle (1)
Steam heating mother liquor is passed through to isolate the steam inlet of the methylene chloride gas of entrapped moisture from mother liquor；The de- weight of the dichloro
The gaseous phase outlet of tower reactor (1) connects the gas phase entrance of the dichloro weight-removing column (2)；The gaseous phase outlet of the dichloro weight-removing column (2)
The gas phase entrance of the dichloro weight-removing column first-stage condenser (3) is connected, the residual air of the dichloro weight-removing column first-stage condenser (3) goes out
Mouth connects the gas phase entrance of the dichloro weight-removing column secondary condenser (4)；The dichloro weight-removing column first-stage condenser (3) and described
The methylene chloride gas of entrapped moisture is condensed into liquid and from respective cold liquid outlet stream by dichloro weight-removing column secondary condenser (4)
It is separated into two-way branch out and after converging, wherein branch described in the first via flows back into the dichloro weight-removing column by circulation line
(2) so that the methylene chloride liquid redistillation of a part of entrapped moisture in, branch described in the second tunnel connects institute by water-division pipeline
The entrance of division box is stated so that the methylene chloride liquid of another part entrapped moisture is sent into the division box.
3. the recyclable device of methylene chloride in cefuroxime acid production according to claim 2, which is characterized in that described
Dehydration pneumatic control valve and dehydration flowmeter are equipped on circulation line and the water-division pipeline.
4. the recyclable device of methylene chloride in cefuroxime acid production according to claim 2, which is characterized in that described de-
Water installations further include dichloro weight-removing column B-grade condensation gas-liquid separator (5)；The cold liquid of the dichloro weight-removing column secondary condenser (4)
Outlet after the dichloro weight-removing column B-grade condensation gas-liquid separator (5) again with the dichloro weight-removing column first-stage condenser (3)
Cold liquid outlet confluence.
5. the recyclable device of methylene chloride in cefuroxime acid production according to claim 4, which is characterized in that described point
Water installations include dichloro dehydration column reboiler (6), dichloro dehydrating tower (7), dichloro dehydrating tower first-stage condenser (8), dichloro dehydration
Tower secondary condenser (9), phase separation tank (11) and dichloro dehydrating tower cooler (12)；Branch described in second tunnel passes through the distributive pipe
The methylene chloride liquid of entrapped moisture is sent into the dichloro dehydrating tower (7) by the entrance that road connects the dichloro dehydrating tower (7)；Institute
It states dichloro dehydration column reboiler (6) and is equipped with the steam port for being passed through steam；The leakage fluid dram of dichloro dehydrating tower (7) bottom connects institute
The liquid phase entrance for stating dichloro dehydration column reboiler (6) is heated into the dichloro of entrapped moisture with the methylene chloride liquid by entrapped moisture
The gas of methane, and the gas phase of the gaseous phase outlet connection dichloro dehydrating tower (7) of the dichloro dehydration column reboiler (6) enters
Mouthful；The gaseous phase outlet of the dichloro dehydrating tower (7) connects the gas phase entrance of the dichloro dehydrating tower first-stage condenser (8), described
The residual air outlet of dichloro dehydrating tower first-stage condenser (8) connects the gas phase entrance of the dichloro dehydrating tower secondary condenser (9)；Institute
Dichloro dehydrating tower first-stage condenser (8) and the dichloro dehydrating tower secondary condenser (9) are stated by the methylene chloride gas of entrapped moisture
Body is condensed into liquid and connects the entrance of the dichloro dehydrating tower cooler (12) after converging again from the outflow of respective cold liquid outlet,
The outlet of the dichloro dehydrating tower cooler (12) connects the import in the middle part of the phase separation tank (11) with by the dichloro of entrapped moisture
Methane liquid is sent into the phase separation tank (11) and is separated into aqueous layer and dichloromethane layer up and down in the phase separation tank (11)；Institute
State the light phase export of phase separation tank (11) by return line connect the dichloro weight-removing column kettle (1) to return liquid mouth upper will separate
Layer aqueous flows back into the dichloro weight-removing column kettle (1) and recycles distillation recovery afterwards, and heavy out passes through acquisition piping connection institute
Lower layer's methylene chloride reflux that the refluxing opening at the top of dichloro dehydrating tower (7) is stated will separate is into the dichloro dehydrating tower (7)；?
The bottom side of the dichloro dehydrating tower (7) is equipped with the extraction mouth of discharge methylene chloride, and the extraction mouth connects the acquisition device.
6. the recyclable device of methylene chloride in cefuroxime acid production according to claim 5, which is characterized in that described
Return line and collection tube road are equipped with point water pneumatic control valve and divide water ga(u)ge.
7. the recyclable device of methylene chloride in cefuroxime acid production according to claim 5, which is characterized in that described to adopt
Acquisition means include dichloro finished product cooler (13) and dichloro tank to be checked (14)；The extraction mouth connects the dichloro finished product cooler
(13) entrance, the outlet of the dichloro finished product cooler (13), which will connect dichloro tank to be checked (14) by discharge nozzle, to be separated
Dichloro finished product it is cooling after obtain finished product and be sent into dichloro tank to be checked (14)；Control valve is equipped on the discharge nozzle.
8. the recyclable device of methylene chloride in cefuroxime acid production according to claim 5, which is characterized in that described de-
Water installations further include dichloro dehydrating tower B-grade condensation gas-liquid separator (10)；The dichloro dehydrating tower secondary condenser (9) it is cold
Liquid outlet after the dichloro dehydrating tower B-grade condensation gas-liquid separator (10) again with the dichloro dehydrating tower first-stage condenser (8)
Cold liquid outlet confluence.
9. the recyclable device of methylene chloride in cefuroxime acid production according to claim 8, which is characterized in that further include
Handle the dichloro weight-removing column B-grade condensation gas-liquid separator (5), the dichloro dehydrating tower B-grade condensation gas-liquid separator (10),
The tail of the tail gas of the phase separation tank (11) and dichloro tank to be checked (14) discharge coagulates system；The dichloro weight-removing column B-grade condensation
Gas-liquid separator (5), the dichloro dehydrating tower B-grade condensation gas-liquid separator (10), the phase separation tank (11) and the dichloro wait for
The evacuation port for examining tank (14) connects the tail and coagulates system.
10. the recyclable device of methylene chloride in cefuroxime acid production according to claim 9, which is characterized in that described
It includes tail condenser (15), tail condenser gas-liquid separator (16) and tail lime set tank (17) that tail, which coagulates system,；The dichloro weight-removing column second level
Condense gas-liquid separator (5), the dichloro dehydrating tower B-grade condensation gas-liquid separator (10), the phase separation tank (11) and described two
The evacuation port of chlorine tank to be checked (14) is incorporated to the gas phase entrance of the tail condenser (15), the condensate outlet warp of the tail condenser (15)
The tail condenser gas-liquid separator (16) reconnects the entrance of the tail lime set tank (17), and the tail condenser gas-liquid separation afterwards
The evacuation port of device (16) also connects the gas phase entrance of the tail condenser (15), the outlet connection described two of the tail lime set tank (17)
Chlorine weight-removing column kettle (1) returns liquid mouth.
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| CN201910141666.1A CN109776256A (en) | 2019-02-26 | 2019-02-26 | The recyclable device of methylene chloride in a kind of production of cefuroxime acid |
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