CN202270377U - Continuous separating refining device for waste liquid containing high polymer - Google Patents

Continuous separating refining device for waste liquid containing high polymer Download PDF

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Publication number
CN202270377U
CN202270377U CN2011203513576U CN201120351357U CN202270377U CN 202270377 U CN202270377 U CN 202270377U CN 2011203513576 U CN2011203513576 U CN 2011203513576U CN 201120351357 U CN201120351357 U CN 201120351357U CN 202270377 U CN202270377 U CN 202270377U
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CN
China
Prior art keywords
waste liquid
high polymer
treating column
oxolane
ethyl acetate
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Expired - Lifetime
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CN2011203513576U
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Chinese (zh)
Inventor
张帆
刘素英
姜媛媛
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SHIJIAZHUANG DANTAI SOLVENT SEPARATION CO LTD
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SHIJIAZHUANG DANTAI SOLVENT SEPARATION CO LTD
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Priority to CN2011203513576U priority Critical patent/CN202270377U/en
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Abstract

The utility model discloses a continuous separating refining device for waste liquid containing high polymer, which comprises a waste liquid storage tank and a rectifying tower system for main components of the waste liquid, wherein the main components are connected in turn; the key point of improvement is that the continuous separating refining device further comprises a knifing evaporator and a centrifugal separator; a gas phase outlet in the upper part of the knifing evaporator is communicated with a feeding pipeline of the rectifying tower system; and a slurry outlet in the lower part of the knifing evaporator is communicated with the feeding pipeline on the upper part of the centrifugal separator. The continuous separating refining device provided by the utility model can be used for efficiently purifying and separating the waste liquid containing high polymer; the continuous rectification is realized; the high polymer coking is avoided; the degree of automation is high; the energy consumption of the process is lower; the quality of products is high; and the stability is excellent.

Description

A kind of continuous separation and purification device that contains the waste liquid of high polymer
Technical field
The utility model belongs to the device of chemical separation process, is specifically related to a kind of continuous separation and purification device that contains the waste liquid of high polymer.
Background technology
In fine chemistry industry is produced, can produce the high polymer that contains higher boiling, thermal sensitivity in a large number, is prone to the knot charcoal, as: be derived from the mother liquor in the sweat, wherein contain a large amount of albumen; Have plenty of the mother liquor that is derived from the medicine intermediate building-up process, wherein contain a large amount of unreacteds or unsegregated reaction raw materials and reactor product.All these material systems with higher boiling, thermal sensitivity, easy knot charcoal character are referred to as high polymer; The waste liquid that contains high polymer is extremely hard to manage; Be prone to knot charcoal occluding device, treating capacity is big and can't realize continued operation, and traditional handicraft can only adopt the batch fractionating technology of gradation in batches.
As everyone knows; Because the process characteristic of batch fractionating; Thereby make phenomenons such as in the batch fractionating separating technology, certainly existing compound decomposition, polymerization, knot charcoal influence the quality and the yield of product, so that the less stable of the product quality of whole technology, the knot charcoal might be attached between heating tube bundle; Even blocking device, be difficult to cleaning.The compound heated time is long in the batch fractionating processing procedure simultaneously, and interim fraction is on the high side between its each component, need repeat rectifying, also causes the energy consumption of whole separation process bigger.Obviously from reliability of technology and economy, batch fractionating is made with extra care separator and suitable high polymer and the big system of treating capacity of containing of technology thereof.
The utility model content
The technical problem that the utility model will solve provides a kind ofly can realize continuous rectification, avoid high polymer knot charcoal and the big continuous separation and purification device that contains the high polymer waste liquid of treating capacity.
For solving the problems of the technologies described above, the technical scheme that the utility model adopts is:
A kind of continuous separation and purification device that contains the waste liquid of high polymer, it comprises waste tank and the rectifying column system of the waste liquid major constituent that connects successively, crucial improvement is also to comprise luwa evaporator and whizzer;
The gas phase discharging opening on said luwa evaporator top is communicated with the feeding line of said rectifying column system, and the slurry row of bottom mouthful is communicated with the feeding line on said whizzer top.
Said rectifying column system is oxolane treating column and the ethyl acetate treating column that connects successively;
The gas phase discharging opening of said luwa evaporator is communicated with the feeding line at oxolane treating column middle part;
The cat head of said oxolane treating column connects the discharging pipeline of oxolane product, and the discharging pipeline of tower bottom connects the feeding line at ethyl acetate treating column middle part;
The cat head of said ethyl acetate treating column connects the discharging pipeline of ethyl acetate product, and the discharging pipeline of tower bottom is connected to said waste tank.
Preferably, the rectifying section of said oxolane treating column is efficient structured packing structure, and the stripping section section is a tower plate structure; Said ethyl acetate treating column is identical with the structure of oxolane treating column.
The liquid phase outlet at said whizzer middle part connects said waste tank.
The beneficial effect that adopts technique scheme to produce is:
(1) operating flexibility of luwa evaporator is big; It is suitable for handling the waste liquid that contains high polymer; Because the luwa evaporator heating surface has higher surface heat flux, therefore have higher volatility, other component can flash evaporation and then entering rectifying column system except that high polymer; The high polymer that can not be evaporated is then arranged a mouthful discharge through the slurry of bottom, because most of high polymer does not get into distillation column system, has avoided the phenomenon of high polymer knot charcoal even obstruction rectifying column;
(2) time of staying of the waste liquid that contains high polymer in luwa evaporator is short, evaporating temperature is lower, and the waste liquid that therefore in evaporation process, contains high polymer also is difficult for the knot charcoal;
(3) waste liquid does not have delay in luwa evaporator, and product change amount or loss amount are less, efficiently solves the problems such as impurity of taking off of waste liquid, makes that follow-up refining product quality is higher;
(4) possibly contain by the slurry of the solid residue of charing from what discharged the luwa evaporator bottom; Make solid-liquid obtain separating through whizzer; Solid phase is directly delivered to incinerator and is burned; Liquid phase is returned the waste liquid storage tank and is continued to handle, and has improved the yield of active ingredient greatly, has also avoided pollution simultaneously;
(5) the utility model can be realized continuous rectification, and its automaticity is high, and the process energy consumption is lower, product quality is high and good stability, is a kind of continuous rectification separator of efficient energy-saving.
Description of drawings
Fig. 1 is the structural representation of the continuous separation and purification device of the utility model embodiment;
Wherein, 1, luwa evaporator, 2, whizzer; 3, oxolane treating column, 4, the ethyl acetate treating column, A represents waste liquid; B represents the liquid of Separation of Solid and Liquid gained, and C represents the knot charcoal solid of Separation of Solid and Liquid gained, and D represents the oxolane product; E represents ethyl acetate product, and F represents the raffinate after the rectification process.
The specific embodiment
Present embodiment is an example to produce waste liquid in the synthetic production process of certain medicine intermediate, and the device that the utility model is described contains in the high polymer waste liquid in processing to be used.Wherein, contain the polymer reaction raw material 5 ~ 8wt% of said medicine in the waste liquid, all the other compositions are mainly oxolane and ethyl acetate.
Referring to Fig. 1, the device of present embodiment comprises waste tank, luwa evaporator 1, whizzer 2, oxolane treating column 3 and ethyl acetate treating column 4; Said luwa evaporator 1 is provided with gas phase discharging opening, liquid phase feeding mouth and slurry row mouth; The top of said whizzer 2 is provided with charging aperture, and the middle part is provided with the liquid phase outlet, and the bottom is provided with the solid phase outlet.
Said waste tank is connected with the liquid phase feeding mouth of luwa evaporator 1 through pipeline, and the gas phase discharging opening of said luwa evaporator 1 is communicated with the feeding line at oxolane treating column 3 middle parts; The cat head of oxolane treating column 3 connects the discharging pipeline of oxolane product D, and the discharging pipeline of the tower bottom of oxolane treating column 3 connects the feeding line at ethyl acetate treating column 4 middle parts; The cat head of said ethyl acetate treating column 4 connects ethyl acetate product E discharging pipeline, and the raffinate F after the rectification process that the discharge nozzle linear flow of tower bottom goes out is back to waste tank.
The slurry row mouth of said luwa evaporator 1 bottom is communicated with the feeding line on said whizzer 2 tops, promptly gets in the whizzer 2 through luwa evaporator 1 pretreated heavy ends; The liquid B of gained is back in the waste tank after whizzer 2 separates, and the knot charcoal solid C of gained delivers to incinerator.Adopt whizzer not only to improve the yield of active ingredient in the waste liquid, avoided environmental pollution simultaneously.
Oxolane treating column 3 operating conditions are in the present embodiment: cat head operating pressure normal pressure, and reflux ratio 3/1~6/1, tower top temperature are 66 ℃, column bottom temperature is 76~78 ℃; Ethyl acetate treating column 4 operating conditions are: cat head operating pressure normal pressure, and reflux ratio 0.5/1~1/1, tower top temperature are 77 ℃, column bottom temperature is 78~80 ℃.
To sum up, the operating procedure of present embodiment device is following:
The waste liquid that 1) will contain high polymer gets into luwa evaporator 1 from waste tank, luwa evaporator 1 adopts the jacket type Steam Heating, and heavy ends to whizzer 2 is discharged in its bottom, and the gaseous component on top gets into oxolane treating column 3;
2) liquid phase component of whizzer 2 discharges returns the material liquid storage tank, and isolated knot charcoal solid is delivered to incinerator and burned;
3) feed liquid that gets into oxolane treating column 3 after treatment, cat head distillates oxolane product D, cut to the ethyl acetate treating column 4 of discharging at the bottom of the tower;
4) ethyl acetate product F is from the 4 cat head extraction of ethyl acetate treating column, cut to the material liquid storage tank that discharge the bottom.
Adopt technique scheme, can carry out the removal of impurity, separation to the waste liquid that contains high polymer effectively, finally obtain high pure tetrahydrofuran (> 99.5%) and high purity acetic acid ethyl ester (> 99.5%) product.Whole process flow is reasonable, automaticity is high, and has that the process energy consumption is lower, product quality is high and characteristics such as good stability, is a kind of continuous rectification separator of efficient energy-saving.

Claims (4)

1. continuous separation and purification device that contains the waste liquid of high polymer, it comprises waste tank and the rectifying column system of the waste liquid major constituent that connects successively, it is characterized in that also comprising luwa evaporator (1) and whizzer (2);
The gas phase discharging opening on said luwa evaporator (1) top is communicated with the feeding line of said rectifying column system, and the slurry row of bottom mouthful is communicated with the feeding line on said whizzer (2) top.
2. a kind of continuous separation and purification device that contains the waste liquid of high polymer according to claim 1 is characterized in that oxolane treating column (3) and the ethyl acetate treating column (4) of said rectifying column system for connecting successively;
The gas phase discharging opening of said luwa evaporator (1) is communicated with the feeding line at oxolane treating column (3) middle part;
The cat head of said oxolane treating column (3) connects the discharging pipeline of oxolane product D, and the discharging pipeline of tower bottom connects the feeding line at ethyl acetate treating column (4) middle part;
The cat head of said ethyl acetate treating column (4) connects the discharging pipeline of ethyl acetate product E, and the discharging pipeline of tower bottom is connected to said waste tank.
3. a kind of continuous separation and purification device that contains the waste liquid of high polymer according to claim 2, the rectifying section that it is characterized in that said oxolane treating column (3) is efficient structured packing structure, stripping section is a tower plate structure; Said ethyl acetate treating column (4) is identical with the structure of oxolane treating column (3).
4. a kind of continuous separation and purification device that contains the waste liquid of high polymer according to claim 1 and 2 is characterized in that the liquid phase outlet at said whizzer (2) middle part connects said waste tank.
CN2011203513576U 2011-09-20 2011-09-20 Continuous separating refining device for waste liquid containing high polymer Expired - Lifetime CN202270377U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2011203513576U CN202270377U (en) 2011-09-20 2011-09-20 Continuous separating refining device for waste liquid containing high polymer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2011203513576U CN202270377U (en) 2011-09-20 2011-09-20 Continuous separating refining device for waste liquid containing high polymer

Publications (1)

Publication Number Publication Date
CN202270377U true CN202270377U (en) 2012-06-13

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN2011203513576U Expired - Lifetime CN202270377U (en) 2011-09-20 2011-09-20 Continuous separating refining device for waste liquid containing high polymer

Country Status (1)

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CN (1) CN202270377U (en)

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Granted publication date: 20120613