CN203878081U - Device system for solvent recovery in process of purifying phenazine by using RT base byproduct - Google Patents

Device system for solvent recovery in process of purifying phenazine by using RT base byproduct Download PDF

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Publication number
CN203878081U
CN203878081U CN201420281691.2U CN201420281691U CN203878081U CN 203878081 U CN203878081 U CN 203878081U CN 201420281691 U CN201420281691 U CN 201420281691U CN 203878081 U CN203878081 U CN 203878081U
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communicated
outlet
feed
opening
solvent
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CN201420281691.2U
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张彩凤
吴永廷
刘云龙
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Zhang Guozhu
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SHANXI XIANGYU CHEMICAL INDUSTRIES Co Ltd
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Abstract

The utility model discloses a device system for solvent recovery in the process of purifying phenazine by using an RT base byproduct, belonging to the technical field of solvent recovery devices. The technical problem to be solved is to provide the device system which can be used for recycling 100% of a solvent in the process of purifying phenazine by using the RT base byproduct. Particularly, the device system comprises a circulating distillation recovery system consisting of three main devices namely a primary distillation kettle, a crystallization filter and a secondary rectifying tower, and can be used for performing 100% solvent recovery on extraction mother liquid in a phenazine purification process. The device system can be used for recycling 100% of an ethanol solvent in the extraction mother liquid, reducing the consumption of raw materials, and avoiding the ethanol solvent from being brought back to an RT production system, thus the production system disorders caused by the accumulation of a phenazine purification solvent in the RT production system can be avoided.

Description

For the apparatus system of 4-aminodiphenylamine by-product purification azophenlyene solvent recuperation
Technical field
A kind of apparatus system for 4-aminodiphenylamine by-product purification azophenlyene solvent recuperation of the utility model, belongs to solvent recovery unit technical field.
Background technology
At present, the synthetic 4-aminodiphenylamine technique of nitrobenzene method is widely adopted, and in its production process, can supervene the high by product azophenlyene residue of added value, therefore, investigator proposes purification and reclaims azophenlyene, main technique is extraction, crystallization, the extracting mother liquid producing in process, after rectifying/Distillation recovery partial solvent, can produce rectifying/distillation kettle liquid, and its direct discharge can cause environmental pollution, send into RT production system and can, because containing Partial purification solvent (ethanol) upset system, increase system loading.Therefore, reclaim and become a urgent problem solving 100% of the azophenlyene solvent of purifying in 4-aminodiphenylamine by-product.
To the recovery of purification azophenlyene solvent, the existing method of extracting azophenlyene from 4-aminodiphenylamine waste material is as described in patent CN201310217173.4, by extracting mother liquid is carried out to rectifying, fusion-crystallization, purification solvent recovering rate is the highest only can reach 95%, remaining 5% purification solvent will be brought in RT production system, and long-time running will certainly be upset RT production system.
Utility model content
The utility model overcomes the deficiencies in the prior art, and technical problem to be solved is to provide a kind of can realization in the process of the azophenlyene of purifying from 4-aminodiphenylamine by-product, the apparatus system that solvent is wherein carried out to 100% recovery.
For solving the problems of the technologies described above, the technical scheme that the utility model adopts is: for the apparatus system of 4-aminodiphenylamine by-product purification azophenlyene solvent recuperation, comprise single flash still, crystal filter and after-fractionating tower;
Described single flash still opening for feed is communicated with the outlet of distillation fresh feed pump, and the import of described distillation fresh feed pump is communicated with azophenlyene extracting mother liquid storage tank; The vapour outlet of described single flash still is communicated with the steam inlet of distiller condenser, and the outlet of described distiller condenser is communicated with the import of reclaiming solvent tank; The bottom discharge mouth of described single flash still is communicated with the opening for feed of single flash raffinate transferpump, and described single flash raffinate carries pump outlet to be communicated with the opening for feed of crystal filter;
The liquid outlet opening of described crystal filter is communicated with single flash filtrate tanks, the opening for feed of the discharge port connecting secondary rectifying fresh feed pump of described single flash filtrate tanks, the outlet of described secondary rectifying fresh feed pump is communicated with the opening for feed of preheater, and the liquid outlet of described preheater is communicated with after-fractionating tower top opening for feed;
At the bottom of described after-fractionating tower tower, the tubing of still liquid outlet is divided into Liang Tiaozhi road, the wherein opening for feed of a branch road connection reboiler, and the discharge port of described reboiler is communicated with the bottom steam inlet of rectifying tower; Another branch road is communicated with the import of secondary rectifying still liquid groove, and the discharge port of described secondary rectifying still liquid groove is communicated with the opening for feed of still liquid transferpump, and described still liquid transferpump is delivered to feed liquid in RT production system;
The overhead vapor outlet of described after-fractionating tower is communicated with the heating agent steam inlet of preheater, described preheater heating agent vapour outlet is communicated with the import of vapour liquid separator, the vapour outlet of described vapour liquid separator is communicated with secondary condenser import, the liquid outlet of described vapour liquid separator is communicated with the import of one-level phlegma storage tank, the outlet of described one-level phlegma storage tank is communicated with the import of distillation fresh feed pump, and described distillation fresh feed pump is communicated with the opening for feed of single flash still; The outlet of described secondary condenser is communicated with the import of reclaiming solvent tank;
The outlet of described recovery solvent tank is communicated with the opening for feed that reclaims solvent delivery pump, and the discharge port of described recovery solvent delivery pump is divided into two branch roads, wherein the backflow import of a branch road connection after-fractionating tower; Another branch road is for delivery of reclaiming solvent to azophenlyene purification system.
The refrigerant of described distiller condenser and secondary condenser is cold water; The thermal medium that adds of described single flash still, crystal filter and reboiler is low-pressure steam.
The beneficial effect compared with prior art the utlity model has is: the extracting mother liquid of the azophenlyene of purifying in 4-aminodiphenylamine by-product all reclaims the purification solvent in mother liquor by processes such as single flash, crystallization filtration and secondary rectifying, can reduce on the one hand the consumption of azophenlyene purification solvent, can directly be delivered in existing RT production system through the rectifying still liquid of secondary rectifying on the other hand, neither can be because containing the disorderly existing RT production system of purification solvent, can not cause environmental pollution, realize the theory of energy-saving and emission-reduction yet.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model.
In figure, 1 is azophenlyene extracting mother liquid storage tank, 2 is distillation fresh feed pump, and 3 is single flash still, and 4 is distiller condenser, 5 is single flash raffinate transferpump, 6 is crystal filter, and 7 is single flash filtrate tanks, and 8 is secondary rectifying fresh feed pump, 9 is preheater, 10 is after-fractionating tower, and 11 is reboiler, and 12 is secondary rectifying still liquid groove, 13 is vapour liquid separator, 14 is one-level phlegma storage tank, and 15 is secondary condenser, and 16 for reclaiming solvent tank, 17 for reclaiming solvent delivery pump, and 18 is rectifying still liquid transferpump.
Embodiment
Below in conjunction with specific embodiment, the utility model is described in further detail.
As shown in Figure 1, for the apparatus system of 4-aminodiphenylamine by-product purification azophenlyene solvent recuperation, comprise single flash still 3, crystal filter 6 and after-fractionating tower 10;
Described single flash still 3 opening for feeds are communicated with distillation fresh feed pump 2 and export, and the import of described distillation fresh feed pump 2 is communicated with azophenlyene extracting mother liquid storage tank 1; The vapour outlet of described single flash still 3 is communicated with the steam inlet of distiller condenser 4, and the outlet of described distiller condenser 4 is communicated with the import of reclaiming solvent tank 16; The bottom discharge mouth of described single flash still 3 is communicated with the opening for feed of single flash raffinate transferpump 5, and the outlet of described single flash raffinate transferpump 5 is communicated with the opening for feed of crystal filter 6;
The liquid outlet opening of described crystal filter 6 is communicated with single flash filtrate tanks 7, the opening for feed of the discharge port connecting secondary rectifying fresh feed pump 8 of described single flash filtrate tanks 7, the outlet of described secondary rectifying fresh feed pump 8 is communicated with the opening for feed of preheater 9, and the liquid outlet of described preheater 9 is communicated with after-fractionating tower 10 top opening for feeds;
At the bottom of described after-fractionating tower 10 towers, the tubing of still liquid outlet is divided into Liang Tiaozhi road, the wherein opening for feed of a branch road connection reboiler 11, and the discharge port of described reboiler 11 is communicated with the bottom steam inlet of rectifying tower 10; Another branch road is communicated with the import of secondary rectifying still liquid groove 12, and the discharge port of described secondary rectifying still liquid groove 12 is communicated with the opening for feed of still liquid transferpump 18, and described still liquid transferpump 18 is delivered to feed liquid in RT production system;
The overhead vapor outlet of described after-fractionating tower 10 is communicated with the heating agent steam inlet of preheater 9, described preheater 9 heating agent vapour outlets are communicated with the import of vapour liquid separator 13, the vapour outlet of described vapour liquid separator 13 is communicated with secondary condenser 15 imports, the liquid outlet of described vapour liquid separator 13 is communicated with the import of one-level phlegma storage tank 14, the outlet of described one-level phlegma storage tank 14 is communicated with the import of distillation fresh feed pump 2, and described distillation fresh feed pump 2 is communicated with the opening for feed of single flash still 3; The outlet of described secondary condenser 15 is communicated with the import of reclaiming solvent tank 16;
The outlet of described recovery solvent tank 16 is communicated with the opening for feed that reclaims solvent delivery pump 17, and the discharge port of described recovery solvent delivery pump 17 is divided into two branch roads, wherein the backflow import of a branch road connection after-fractionating tower 10; Another branch road is for delivery of reclaiming solvent to azophenlyene purification system.
The refrigerant of described distiller condenser 4 and secondary condenser 15 is cold water; The thermal medium that adds of described single flash still 3, crystal filter 6 and reboiler 11 is low-pressure steam.
Working process of the present utility model is as follows:
Send in azophenlyene extracting mother liquid storage tank 1 and store from the extracting mother liquid of the azophenlyene technique extraction step of purifying in 4-aminodiphenylamine by-product.Extracting mother liquid in azophenlyene extracting mother liquid storage tank 1 is delivered to single flash still 3 by distillation fresh feed pump 2 and distills, and distillation steam is delivered in recovery solvent tank 16 after entering distiller condenser 4 condensations.
The single flash raffinate of single flash still 3 is delivered to crystal filter 6 by single flash raffinate transferpump 5, and after filtering, solid slag is sent into azophenlyene purification workshop, as purification raw material; After filtering, filtrate is from flowing to single flash filtrate tanks 7.
Distillation filtrate in single flash filtrate tanks 7 is delivered to preheater 9 by secondary rectifying fresh feed pump 8, described distillation filtrate through with the secondary rectifying steam heat-exchanging exporting from after-fractionating tower 10 overhead vapours after be delivered to after-fractionating tower 10; Described secondary rectifying steam is delivered to vapour liquid separator 13 after heat exchange, after vapour liquid separator 13 separates, gas phase enters secondary condenser 15 and is delivered to after cooling and reclaims solvent tank 16, liquid phase is from flowing to one-level phlegma storage tank 14, material in described one-level phlegma storage tank 14 is delivered to single flash still 3 by distillation fresh feed pump 2, carries out fractionation by distillation again.
At the bottom of after-fractionating tower 10 towers, a still liquid part enters after reboiler 11 boils again and returns to rectifying tower 10, and a part enters secondary rectifying still liquid groove 12, and the feed liquid in described secondary rectifying still liquid groove 12 is delivered in RT production system by rectifying still liquid transferpump 18.
Recovery solvent in described recovery solvent tank 16, a part is sent into after-fractionating tower 10 through recovery solvent delivery pump 17 and is refluxed, and another part is delivered in azophenlyene purification system and uses as solvent.
By reference to the accompanying drawings embodiment of the present utility model is explained in detail above, but the utility model is not limited to above-described embodiment, in the ken possessing those of ordinary skill in the art, can also under the prerequisite that does not depart from the utility model aim, make various variations.

Claims (2)

1. for the apparatus system of 4-aminodiphenylamine by-product purification azophenlyene solvent recuperation, it is characterized in that: comprise single flash still (3), crystal filter (6) and after-fractionating tower (10);
Described single flash still (3) opening for feed is communicated with distillation fresh feed pump (2) outlet, and the import of described distillation fresh feed pump (2) is communicated with azophenlyene extracting mother liquid storage tank (1); The vapour outlet of described single flash still (3) is communicated with the steam inlet of distiller condenser (4), and the outlet of described distiller condenser (4) is communicated with the import of reclaiming solvent tank (16); The bottom discharge mouth of described single flash still (3) is communicated with the opening for feed of single flash raffinate transferpump (5), and the outlet of described single flash raffinate transferpump (5) is communicated with the opening for feed of crystal filter (6);
The liquid outlet opening of described crystal filter (6) is communicated with single flash filtrate tanks (7), the opening for feed of the discharge port connecting secondary rectifying fresh feed pump (8) of described single flash filtrate tanks (7), the outlet of described secondary rectifying fresh feed pump (8) is communicated with the opening for feed of preheater (9), and the liquid outlet of described preheater (9) is communicated with after-fractionating tower (10) top opening for feed;
At the bottom of described after-fractionating tower (10) tower, the tubing of still liquid outlet is divided into Liang Tiaozhi road, the wherein opening for feed of a branch road connection reboiler (11), and the discharge port of described reboiler (11) is communicated with the bottom steam inlet of rectifying tower (10); Another branch road is communicated with the import of secondary rectifying still liquid groove (12), and the discharge port of described secondary rectifying still liquid groove (12) is communicated with the opening for feed of still liquid transferpump (18), and described still liquid transferpump (18) is delivered to feed liquid in RT production system;
The overhead vapor outlet of described after-fractionating tower (10) is communicated with the heating agent steam inlet of preheater (9), described preheater (9) heating agent vapour outlet is communicated with the import of vapour liquid separator (13), the vapour outlet of described vapour liquid separator (13) is communicated with secondary condenser (15) import, the liquid outlet of described vapour liquid separator (13) is communicated with the import of one-level phlegma storage tank (14), the outlet of described one-level phlegma storage tank (14) is communicated with the import of distillation fresh feed pump (2), and described distillation fresh feed pump (2) is communicated with the opening for feed of single flash still (3); The outlet of described secondary condenser (15) is communicated with the import of reclaiming solvent tank (16);
The outlet of described recovery solvent tank (16) is communicated with the opening for feed that reclaims solvent delivery pump (17), and the discharge port of described recovery solvent delivery pump (17) is divided into two branch roads, wherein the backflow import of a branch road connection after-fractionating tower (10); Another branch road is for delivery of reclaiming solvent to azophenlyene purification system.
2. the apparatus system for 4-aminodiphenylamine by-product purification azophenlyene solvent recuperation according to claim 1, is characterized in that: the refrigerant of described distiller condenser (4) and secondary condenser (15) is cold water; The thermal medium that adds of described single flash still (3), crystal filter (6) and reboiler (11) is low-pressure steam.
CN201420281691.2U 2014-05-29 2014-05-29 Device system for solvent recovery in process of purifying phenazine by using RT base byproduct Expired - Lifetime CN203878081U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106316969A (en) * 2015-06-19 2017-01-11 中国石油化工股份有限公司 Separation method of RT base production wastes
CN106543011A (en) * 2015-09-16 2017-03-29 中国石油化工股份有限公司 A kind of 4-aminodiphenylamine produces the processing method of waste material
CN109665996A (en) * 2017-10-17 2019-04-23 中国石油化工股份有限公司 The refining methd and device of caprolactam

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106316969A (en) * 2015-06-19 2017-01-11 中国石油化工股份有限公司 Separation method of RT base production wastes
CN106543011A (en) * 2015-09-16 2017-03-29 中国石油化工股份有限公司 A kind of 4-aminodiphenylamine produces the processing method of waste material
CN106543011B (en) * 2015-09-16 2018-08-07 中国石油化工股份有限公司 A kind of processing method of 4-aminodiphenylamine production waste material
CN109665996A (en) * 2017-10-17 2019-04-23 中国石油化工股份有限公司 The refining methd and device of caprolactam

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C14 Grant of patent or utility model
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TR01 Transfer of patent right

Effective date of registration: 20180117

Address after: Bei Jing 044100 Shanxi Province Linyi County Shijiazhuang Township Village residents group ninth

Patentee after: Zhang Guozhu

Address before: Hi tech Industrial Park, 044100 Shanxi city of Yuncheng Province Linyi County

Patentee before: SHANXI XIANGYU CHEMICAL INDUSTRIAL CO.,LTD.

TR01 Transfer of patent right
CX01 Expiry of patent term

Granted publication date: 20141015

CX01 Expiry of patent term