CN204125401U - The production line of first, ethanol mixed solvent is reclaimed in sodium salt class drug manufacture - Google Patents
The production line of first, ethanol mixed solvent is reclaimed in sodium salt class drug manufacture Download PDFInfo
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- CN204125401U CN204125401U CN201420598897.8U CN201420598897U CN204125401U CN 204125401 U CN204125401 U CN 204125401U CN 201420598897 U CN201420598897 U CN 201420598897U CN 204125401 U CN204125401 U CN 204125401U
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Abstract
The utility model discloses the production line reclaiming first, ethanol mixed solvent in a kind of sodium salt class drug manufacture, comprise the thick rectifier unit of first, ethanol, ethylene glycol extracting rectifying device and glycol recovery device, wherein, the thick rectifier unit of first, ethanol comprises No. 1 rectifying tower and No. 1 condensing works be communicated with it and first, the ethanol surge tank collecting condensed fluid; Ethylene glycol extracting rectifying device comprises No. 2 rectifying tower and No. 2 condensing workss be communicated with it and first, the ethanol tank to be checked collecting condensed fluid, and the outlet of this tank to be checked is communicated with No. 2 rectifying column inlet with finished product storage tank entrance respectively; Glycol recovery device comprises No. 3 rectifying tower and No. 3 condensing workss be communicated with it, the tail of collecting condensed fluid coagulates tank and collects the ethylene glycol storage tank of No. 3 rectifying tower bottom products; The outlet of first, ethanol surge tank is communicated with No. 2 rectifying column inlet, and the outlet of ethylene glycol storage tank is communicated with No. 2 rectifying column inlet, and the outlet of No. 2 rectifier bottoms is communicated with No. 3 rectifying column inlet.
Description
Technical field
The utility model relates to the retrieving arrangement of solvent, is specifically related to the production line reclaiming first, ethanol mixed solvent in a kind of sodium salt class drug manufacture.
Background technology
Methyl alcohol and ethanol are the conventional recrystallisation solvents during medicine is produced, and wherein the mixed system of methyl alcohol and ethanol is crystallization solvent conventional in sodium salt class drug crystallization.After first, ethanol mixed solvent is used, a part of Organic pollutants can be accompanied with by water dilution during crystallization simultaneously, could use after needing re-distillation or rectifying to reach corresponding requirement.
The isolation of methyl alcohol and ethanol is only related to, if notification number is the utility model patent of CN203540097U in prior art; More rare scheme of first, ethanol mixed waste liquor being carried out simultaneously to rectifying, obtains first, ethanol mixed solvent water content higher, or the ratio of gained first, ethanol mixed solvent with can not directly reuse for ratio during crystallization changes.
Utility model content
The technical problems to be solved in the utility model is to provide the production line reclaiming first, ethanol mixed solvent in a kind of sodium salt class drug manufacture.First, the ethanol mixed solvent water content obtained through this production line process is low, and wherein the ratio of methyl alcohol and ethanol is with initial basically identical for ratio during crystallization, can directly again utilize.
Reclaim the production line of first, ethanol mixed solvent in sodium salt class drug manufacture described in the utility model, comprise the thick rectifier unit of first, ethanol, ethylene glycol extracting rectifying device and glycol recovery device, wherein:
The thick rectifier unit of described first, ethanol comprises No. 1 rectifying tower, adopts No. 1 condensing works of outlet with the gas phase at No. 1 rectifying tower top and collect first, the ethanol surge tank of No. 1 condensing works condensation gained liquid, described No. 1 condensing works is made up of interchanger, No. 1 tower first-stage condenser and No. 1 tower secondary condenser, wherein, the gas phase at the thermal fluid inlet of interchanger and No. 1 rectifying tower top adopts outlet, and its hot fluid outlet ports is communicated with No. 1 tower first-stage condenser entrance; Cold fluid inlet and the pipeline communication carrying the first and second alcohol aqueous waste produced in sodium salt medicine production process of interchanger, its cold fluid outlet is communicated with No. 1 rectifying column inlet;
Described ethylene glycol extracting rectifying device comprises No. 2 rectifying tower, adopts No. 2 condensing workss of outlet with the gas phase at No. 2 rectifying tower tops and collect first, the ethanol tank to be checked of No. 2 condensing works condensation gained liquid, and described No. 2 condensing workss are made up of No. 2 tower first-stage condenser, No. 2 tower secondary condensers and No. 2 tower cooler devices; The outlet of described first, ethanol tank to be checked is communicated with No. 2 rectifying column inlet with finished product storage tank entrance respectively;
Described glycol recovery device comprises No. 3 rectifying tower, adopt No. 3 condensing workss of outlet with the gas phase at No. 3 rectifying tower tops, collect the tail of No. 3 condensing works condensation gained liquid coagulates tank and collects the ethylene glycol storage tank of No. 3 rectifying tower bottom products, and described No. 3 condensing workss are made up of No. 3 tower first-stage condenser, No. 3 tower secondary condensers and No. 3 tower cooler devices;
The outlet of described first, ethanol surge tank is communicated with No. 2 rectifying column inlet, and the outlet of ethylene glycol storage tank is communicated with No. 2 rectifying column inlet, and the outlet of No. 2 rectifier bottoms is communicated with No. 3 rectifying column inlet.
In No. 1 condensing works of technique scheme, the residual air outlet of No. 1 tower first-stage condenser is communicated with the entrance of No. 1 tower secondary condenser, and No. 1 tower first-stage condenser is all communicated with the entrance of first, ethanol surge tank with the liquid exit of No. 1 tower secondary condenser, No. 1 tower first-stage condenser is also communicated with (for controlling reflux ratio) with No. 1 rectifying tower with the liquid exit of No. 1 tower secondary condenser simultaneously.
In No. 2 condensing workss of technique scheme, the residual air outlet of No. 2 tower first-stage condenser is communicated with the entrance of No. 2 tower secondary condensers, and No. 2 tower first-stage condenser are all communicated with the entrance of No. 2 tower cooler devices with the liquid exit of No. 2 tower secondary condensers, No. 2 tower first-stage condenser are also communicated with (for controlling reflux ratio) with No. 2 rectifying tower with the liquid exit of No. 2 tower secondary condensers simultaneously.
In No. 3 condensing workss of technique scheme, the residual air outlet of No. 3 tower first-stage condenser is communicated with the entrance of No. 3 tower secondary condensers, and No. 3 tower first-stage condenser are all communicated with the entrance of No. 3 tower cooler devices with the liquid exit of No. 3 tower secondary condensers; No. 3 tower first-stage condenser are also communicated with (for controlling reflux ratio) with No. 3 rectifying tower with the liquid exit of No. 3 tower secondary condensers simultaneously.
Compared with prior art, the feature of production line described in the utility model is:
1, add interchanger at No. 1 condensing works, first, the ethanol mixed gas of condensation No. 1 rectifying tower top gas phase extraction mouth extraction can be reached, the object of preheating first, ethanol mixed waste liquor can be played again, effectively reduce energy consumption, reduce cost;
2, production line described in the utility model is applicable to the recovery of first, the ethanol mixed waste liquor produced in sodium salt class drug manufacture, is applicable to the recovery of first, the ethanol mixed waste liquor produced during cefobutazine sodium is produced;
3, production line structure described in the utility model is simple, first, the ethanol mixed solvent water content adopting this production line to reclaim is lower than 1%, wherein the ratio of methyl alcohol and ethanol is with initial basically identical for ratio during crystallization, the Crystallization Procedure in sodium salt class drug manufacture can be directly used in, effectively reduce the production cost of sodium drug class.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of embodiment of the utility model.
Number in the figure is:
1, No. 1 rectifying tower; 2, interchanger; 3, No. 1 tower first-stage condenser; 4, No. 1 tower secondary condenser; 5, first, ethanol surge tank; 6, No. 2 rectifying tower; 7, No. 2 tower first-stage condenser; 8, No. 2 tower secondary condensers; 9, No. 2 tower cooler devices; 10, first, ethanol tank to be checked; 11, No. 3 rectifying tower; 12, No. 3 tower first-stage condenser; 13, No. 3 tower secondary condensers; 14, No. 3 tower cooler devices; 15, tail coagulates tank; 16, ethylene glycol storage tank.
Embodiment
As shown in Figure 1, reclaim the production line of first, ethanol mixed solvent in sodium salt class drug manufacture described in the utility model, comprise the thick rectifier unit of first, ethanol, ethylene glycol extracting rectifying device and glycol recovery device, wherein:
The thick rectifier unit of described first, ethanol comprises No. 1 rectifying tower 1, adopts No. 1 condensing works of outlet with the gas phase at No. 1 rectifying tower 1 top and collect first, the ethanol surge tank 5 of No. 1 condensing works condensation gained liquid, described No. 1 condensing works is made up of interchanger 2, No. 1 tower first-stage condenser 3 and No. 1 tower secondary condenser 4, wherein, the gas phase at the thermal fluid inlet of interchanger 2 and No. 1 rectifying tower 1 top adopts outlet, and its hot fluid outlet ports is communicated with No. 1 tower first-stage condenser 3 entrance; Cold fluid inlet and the pipeline communication carrying the first and second alcohol aqueous waste produced in sodium salt medicine production process of interchanger 2, its cold fluid outlet is communicated with No. 1 rectifying tower 1 entrance; The residual air outlet of No. 1 tower first-stage condenser 3 is communicated with the entrance of No. 1 tower secondary condenser 4, and No. 1 tower first-stage condenser 3 is all communicated with the entrance of first, ethanol surge tank 5 with the liquid exit of No. 1 tower secondary condenser 4, No. 1 tower first-stage condenser 3 is also communicated with (for controlling reflux ratio) with No. 1 rectifying tower 1 with the liquid exit of No. 1 tower secondary condenser 4 simultaneously;
Described ethylene glycol extracting rectifying device comprises No. 2 rectifying tower 6, adopts No. 2 condensing workss of outlet with the gas phase at No. 2 rectifying tower 6 tops and collect first, the ethanol tank 10 to be checked of No. 2 condensing works condensation gained liquid, and described No. 2 condensing workss are made up of No. 2 tower first-stage condenser 7, No. 2 tower secondary condensers 8 and No. 2 tower cooler devices 9; The outlet of described first, ethanol tank 10 to be checked is communicated with No. 2 rectifying tower 6 entrances with finished product storage tank entrance respectively; The residual air outlet of No. 2 tower first-stage condenser 7 is communicated with the entrance of No. 2 tower secondary condensers 8, and No. 2 tower first-stage condenser 7 are all communicated with the entrance of No. 2 tower cooler devices 9 with the liquid exit of No. 2 tower secondary condensers 8, No. 2 tower first-stage condenser 7 are also communicated with (for controlling reflux ratio) with No. 2 rectifying tower 6 with the liquid exit of No. 2 tower secondary condensers 8 simultaneously;
Described glycol recovery device comprises No. 3 rectifying tower 11, adopt No. 3 condensing workss of outlet with the gas phase at No. 3 rectifying tower 11 tops, collect the tail of No. 3 condensing works condensation gained liquid coagulates tank 15 and collects the ethylene glycol storage tank 16 of No. 3 rectifying tower 11 bottom products, and described No. 3 condensing workss are made up of No. 3 tower first-stage condenser 12, No. 3 tower secondary condensers 13 and No. 3 tower cooler devices 14; The residual air outlet of No. 3 tower first-stage condenser 12 is communicated with the entrance of No. 3 tower secondary condensers 13, and No. 3 tower first-stage condenser 12 are all communicated with the entrance of No. 3 tower cooler devices 14 with the liquid exit of No. 3 tower secondary condensers 13; No. 3 tower first-stage condenser 12 are also communicated with (for controlling reflux ratio) with No. 3 rectifying tower 11 with the liquid exit of No. 3 tower secondary condensers 13 simultaneously;
The outlet of described first, ethanol surge tank 5 is communicated with No. 2 rectifying tower 6 entrances, and the outlet of ethylene glycol storage tank 16 is communicated with No. 2 rectifying tower 6 entrances, and the outlet bottom No. 2 rectifying tower 6 is communicated with No. 3 rectifying tower 11 entrances.
Adopt above-mentioned production line to carry out reclaiming the technique of first, ethanol solvent, comprise the following steps:
1) material inlet valve of first, ethanol surge tank 5 is closed, moisture for first, ethanol mixed waste liquor is squeezed into interchanger 2 from the cold fluid inlet of interchanger 2, entered in No. 1 rectifying tower 1 by liquid exit cold on interchanger 2 after interchanger 2 preheating (carry out rectifying first and can not realize preheating object) and carry out rectifying, enter the total reflux stage; The gas phase of overhead extraction carries out interchanger 2 by interchanger 2 thermal fluid inlet, after interchanger 2 heat exchange again by interchanger 2 hot fluid outlet ports successively through 3, No. 1 tower secondary condenser 4 condensation of No. 1 tower first-stage condenser, the phlegma obtained all enters No. 1 rectifying tower 1; When the column bottom temperature of No. 1 rectifying tower 1 reach 95 ~ 110 DEG C, pressure reaches 0.005 ~ 0.015Mpa, tower top temperature reaches 70 ~ 80 DEG C, pressure is when reaching 0.001 ~ 0.003MPa, (control reflux ratio is more than 3:1 to the material inlet valve of adjustment first, ethanol surge tank 5, be preferably 5:1), make the phlegma partial reflux through No. 1 tower first-stage condenser 3 and the condensation of No. 1 tower secondary condenser 4 enter No. 1 rectifying tower 1, part enters first, ethanol surge tank 5; When the water content of first, the ethanol mixed solvent crude product collected in first, ethanol surge tank 5 reaches 5% ~ 6%, stop the rectifying (during continuous seepage can without the need to stop) of No. 1 rectifying tower 1, the waste liquid of No. 1 rectifying tower 1 tower reactor by the outlet drain bottom No. 1 rectifying tower 1 to wastewater disposal basin;
2) feed valve of No. 2 tower cooler devices 9 is closed, ethylene glycol is squeezed into (if not reclaiming first, ethanol solvent first in No. 2 rectifying tower 6, the ethylene glycol collected in last recovery process directly can be pumped in No. 2 rectifying tower 6), unlatching steam valve heats, when the column bottom temperature of No. 2 rectifying tower 6 reaches 98 ~ 105 DEG C, first, the ethanol mixed solvent crude product in first, ethanol surge tank 5 is pumped into No. 2 rectifying tower 6; The bottom temperature controlling No. 2 rectifying tower 6 is 110 ~ 130 DEG C, pressure is 0.005 ~ 0.015MPa, and tower top temperature is 70 ~ 80 DEG C, pressure is 0.001 ~ 0.003Mpa, enters the total reflux stage.Regulate extraction agent (i.e. ethylene glycol) and feed liquid inlet amount, make the volume ratio of extraction agent flow and feed liquid flow be 2:1); The gas phase of overhead extraction is successively through 7, No. 2 tower secondary condenser 8 condensations of No. 2 tower first-stage condenser, and the phlegma obtained all enters No. 2 rectifying tower 6; After tower each section of temperature, pressure-stabilisation, regulate the material inlet valve of No. 2 tower cooler devices 9 (controlling reflux ratio 1:1), make the phlegma partial reflux through No. 2 tower first-stage condenser 7 and the condensation of No. 2 tower secondary condensers 8 enter No. 2 rectifying tower 6, part enters No. 2 tower cooler devices 9 and then enters first, ethanol tank 10 to be checked; When water content≤1% (being generally 0.5 ~ 0.7%) of first, the ethanol mixed solvent collected in first, ethanol tank 10 to be checked, first, the ethanol mixed solvent collected is sent into finished product storage tank; If in first, ethanol tank 10 to be checked collect first, ethanol mixed solvent water content higher than 1% time, first, the ethanol of collection mixed solvent is returned No. 2 rectifying tower 6 and continues rectifying, until water content reaches requirement;
3) liquid sampling in No. 2 rectifying tower 6 tower reactors is detected, when first, alcohol residue≤0.5% in sample (content of methyl alcohol and ethanol amounts to lower than 0.5%), stop the rectifying (during continuous seepage can without the need to stop) of rectifying tower 2, the liquid of No. 2 rectifying tower 6 tower reactors sends into No. 3 rectifying tower 11 by the outlet bottom No. 2 rectifying tower 6; Vacuum pumping is carried out to No. 3 rectifying tower 11 inside, open steam valve heating simultaneously, control bottom temperature is 130 ~ 150 DEG C, pressure is-0.08 ~-0.09MPa, tower top temperature is 35 ~ 45 DEG C, pressure is-0.08 ~-0.09MPa, open the feed valves of No. 3 rectifying tower 11, the reflux ratio controlled containing water glycol is that 2:1 carries out ethylene glycol continuously dehydrating; Liquid sampling in No. 3 rectifying tower 11 tower reactors is detected, when water content≤0.5% of sample, stop rectifying (during continuous seepage can without the need to stop), the liquid in No. 3 rectifying tower 11 tower reactors delivers to ethylene glycol storage tank 16 from the outlet bottom No. 3 rectifying tower 11.
Applicant by above-mentioned production line in conjunction with above-mentioned technique cefobutazine sodium produce in Crystallization Procedure in use, the yield 90 ~ 95% of first, ethanol mixed solvent, the ratio reclaiming methyl alcohol and ethanol in first, the ethanol mixed solvent obtained, with initial basically identical for ratio during crystallization, can be directly used in the Crystallization Procedure in sodium salt class drug manufacture.
Claims (4)
1. reclaim the production line of first, ethanol mixed solvent in sodium salt class drug manufacture, comprise the thick rectifier unit of first, ethanol, ethylene glycol extracting rectifying device and glycol recovery device, it is characterized in that:
Described first, the thick rectifier unit of ethanol comprises No. 1 rectifying tower (1), adopt No. 1 condensing works of outlet with the gas phase at No. 1 rectifying tower (1) top and collect the first of No. 1 condensing works condensation gained liquid, ethanol surge tank (5), described No. 1 condensing works is by interchanger (2), No. 1 tower first-stage condenser (3) and No. 1 tower secondary condenser (4) composition, wherein, the thermal fluid inlet of interchanger (2) and the gas phase at No. 1 rectifying tower (1) top adopt outlet, its hot fluid outlet ports is communicated with No. 1 tower first-stage condenser (3) entrance, cold fluid inlet and the pipeline communication carrying the first and second alcohol aqueous waste produced in sodium salt medicine production process of interchanger (2), its cold fluid outlet is communicated with No. 1 rectifying tower (1) entrance,
Described ethylene glycol extracting rectifying device comprises No. 2 rectifying tower (6), adopts No. 2 condensing workss of outlet with the gas phase at No. 2 rectifying tower (6) tops and collect first, the ethanol tank to be checked (10) of No. 2 condensing works condensation gained liquid, and described No. 2 condensing workss are made up of No. 2 tower first-stage condenser (7), No. 2 tower secondary condensers (8) and No. 2 tower cooler devices (9); The outlet of described first, ethanol tank to be checked (10) is communicated with No. 2 rectifying tower (6) entrances with finished product storage tank entrance respectively;
Described glycol recovery device comprises No. 3 rectifying tower (11), adopt No. 3 condensing workss of outlet with the gas phase at No. 3 rectifying tower (11) tops, collect the tail of No. 3 condensing works condensation gained liquid coagulates tank (15) and collects the ethylene glycol storage tank (16) of No. 3 rectifying tower (11) bottom products, and described No. 3 condensing workss are made up of No. 3 tower first-stage condenser (12), No. 3 tower secondary condensers (13) and No. 3 tower cooler devices (14);
The outlet of described first, ethanol surge tank (5) is communicated with No. 2 rectifying tower (6) entrances, the outlet of ethylene glycol storage tank (16) is communicated with No. 2 rectifying tower (6) entrances, and the outlet of No. 2 rectifying tower (6) bottoms is communicated with No. 3 rectifying tower (11) entrances.
2. in sodium salt class drug manufacture according to claim 1, reclaim the production line of first, ethanol mixed solvent, it is characterized in that: in No. 1 condensing works, the residual air outlet of No. 1 tower first-stage condenser (3) is communicated with the entrance of No. 1 tower secondary condenser (4), and No. 1 tower first-stage condenser (3) is all communicated with the entrance of first, ethanol surge tank (5) with the liquid exit of No. 1 tower secondary condenser (4), No. 1 tower first-stage condenser (3) is also communicated with No. 1 rectifying tower (1) with the liquid exit of No. 1 tower secondary condenser (4) simultaneously.
3. in sodium salt class drug manufacture according to claim 1, reclaim the production line of first, ethanol mixed solvent, it is characterized in that: in No. 2 condensing workss, the residual air outlet of No. 2 tower first-stage condenser (7) is communicated with the entrance of No. 2 tower secondary condensers (8), and No. 2 tower first-stage condenser (7) are all communicated with the entrance of No. 2 tower cooler devices (9) with the liquid exit of No. 2 tower secondary condensers (8), No. 2 tower first-stage condenser (7) are also communicated with No. 2 rectifying tower (6) with the liquid exit of No. 2 tower secondary condensers (8) simultaneously.
4. reclaim first in sodium salt class drug manufacture according to claim 1, the production line of ethanol mixed solvent, it is characterized in that: in No. 3 condensing workss, the residual air outlet of No. 3 tower first-stage condenser (12) is communicated with the entrance of No. 3 tower secondary condensers (13), and No. 3 tower first-stage condenser (12) are all communicated with the entrance of No. 3 tower cooler devices (14) with the liquid exit of No. 3 tower secondary condensers (13), No. 3 tower first-stage condenser (12) are also communicated with No. 3 rectifying tower (11) with the liquid exit of No. 3 tower secondary condensers (13) simultaneously.
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| CN201420598897.8U CN204125401U (en) | 2014-10-16 | 2014-10-16 | The production line of first, ethanol mixed solvent is reclaimed in sodium salt class drug manufacture |
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| CN201420598897.8U CN204125401U (en) | 2014-10-16 | 2014-10-16 | The production line of first, ethanol mixed solvent is reclaimed in sodium salt class drug manufacture |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114405041A (en) * | 2022-02-25 | 2022-04-29 | 明士新材料有限公司 | Rectification device and method for electronic-grade gamma-butyrolactone |
| CN114522435A (en) * | 2022-02-28 | 2022-05-24 | 明士新材料有限公司 | Continuous rectification device for producing electronic-grade triethylamine and application method thereof |
-
2014
- 2014-10-16 CN CN201420598897.8U patent/CN204125401U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114405041A (en) * | 2022-02-25 | 2022-04-29 | 明士新材料有限公司 | Rectification device and method for electronic-grade gamma-butyrolactone |
| CN114522435A (en) * | 2022-02-28 | 2022-05-24 | 明士新材料有限公司 | Continuous rectification device for producing electronic-grade triethylamine and application method thereof |
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