CN203295403U - Device system used for extracting and refining azophenylene in RT base waste - Google Patents

Device system used for extracting and refining azophenylene in RT base waste Download PDF

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Publication number
CN203295403U
CN203295403U CN2013203159218U CN201320315921U CN203295403U CN 203295403 U CN203295403 U CN 203295403U CN 2013203159218 U CN2013203159218 U CN 2013203159218U CN 201320315921 U CN201320315921 U CN 201320315921U CN 203295403 U CN203295403 U CN 203295403U
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communicated
reactor
mother liquor
whizzer
liquid outlet
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吴永廷
刘云龙
张兴会
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SHANXI XIANGYU CHEMICAL INDUSTRIES Co Ltd
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SHANXI XIANGYU CHEMICAL INDUSTRIES Co Ltd
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Abstract

The utility model belongs to the technical field of azophenylene refining, and provides a device system capable of being used for preparing a high-purity azophenylene crystal and capable of recovering used solvents without waste liquid pollution. The device system used for extracting and refining azophenylene in RT base waste adopts the technical scheme that the system comprises twice extraction and twice crystallization; the RT base waste and circulatory rough azophenylene are subjected to extraction twice and crystallization twice sequentially; solvents of the twice extraction and the primary crystallization are form an adjacent next technology; solid materials of the secondary extraction and the twice crystallization are form an adjacent previous technology; the solvent recovered after mother liquid of the primary extraction is rectified is used for the secondary crystallization; rough azophenylene after melt crystallization of rectified kettle liquid returns to the primary extraction; and residual liquid after the fusion crystallization of the kettle liquid returns to an RT production system. The solvents and the raw materials are recycled by such circulation, so that azophenylene can be extracted to the greatest extent, and the solvents can be used fully.

Description

For the 4-aminodiphenylamine waste material, extract the apparatus system of refining azophenlyene
Technical field
The utility model extracts the apparatus system of refining azophenlyene for the 4-aminodiphenylamine waste material, belong to azophenlyene purification techniques field.
Background technology
At nitrobenzene method, produce in the process of 4-aminodiphenylamine, aniline under the catalysis of the Tetramethylammonium hydroxide of alkalescence with oil of mirbane generation nucleophilic addition, the contraposition of nucleophilic reagent attack oil of mirbane, through reducing final generation main reaction product 4-aminodiphenylamine, the ortho position of attack oil of mirbane generates the by product azophenlyene of this reaction.We can find out from reaction mechanism, and azophenlyene is the by product that will inevitably produce in the 4-aminodiphenylamine production process, therefore it are fully utilized, and are the important topic of pendulum in face of RT manufacturing enterprise.
Yet, take oil of mirbane and aniline in the process of raw material production 4-aminodiphenylamine, the by product azophenlyene that produces is difficult to effectively separate by present production technique, with a small amount of aniline, 4-ADPA, nitrogen benzide, be mixed into waste material, directly discharge or burn not only contaminate environment, and causing the resource significant wastage.Existing from the method for extracting azophenlyene the RT waste material as described in patent (CN200810099916.1), take the technological operation of dissolution extraction, solid-liquid separation, recrystallization, drying, distillation, rectifying, but the azophenlyene product purity that obtains is lower, and adopt rectificating method to reclaim distillation residue aniline, 4-ADPA, nitrogen benzide etc., operational cycle is long, and cost recovery is high.
The utility model content
The utility model, in order to overcome the deficiencies in the prior art, provides a kind of and can be used in the highly purified azophenlyene crystal of preparation, and can reclaim solvent for use, without the apparatus system of waste liquor contamination.
for solving the problems of the technologies described above, the technical scheme that the utility model adopts is: the apparatus system that extracts refining azophenlyene for the 4-aminodiphenylamine waste material, comprise the single extraction reactor, the reextraction reactor, the primary crystallization reactor, the secondary crystal reactor, rectifying tower, the bottom discharge mouth of described single extraction reactor is communicated with the opening for feed of the first whizzer, the liquid outlet of described the first whizzer is communicated with the fluid inlet of single extraction mother liquor groove, the liquid outlet of described single extraction mother liquor groove is connected with single extraction mother liquor transferpump, described single extraction mother liquor carries delivery side of pump to be communicated with the fluid inlet of preheater, the liquid outlet of described preheater is communicated with the inlet opening of rectifying tower,
At the bottom of the tower of described rectifying tower, the tubing of still liquid outlet is divided into two branch roads, and wherein branch road is communicated with the fluid inlet of reboiler, and the vapor outlet port of described reboiler is communicated with the vapour inlet of rectifying tower; Another branch road is communicated with the fluid inlet of still liquid groove, and the liquid outlet of described still liquid groove is communicated with the opening for feed of the 5th whizzer, and the liquid outlet of described the 5th whizzer is connected with the raffinate transferpump, and described raffinate carries delivery side of pump to lead to the RT production system;
The overhead vapours outlet of described rectifying tower is communicated with the vapour inlet of preheater, the vapor outlet port of described preheater is communicated with the opening for feed of gas-liquid separator, the overhead vapor outlet of described gas-liquid separator is communicated with the inlet mouth of cool condenser, the liquid outlet of described condenser is communicated with the fluid inlet that reclaims the solvent groove, the bottom liquid outlet of described gas-liquid separator is communicated with the fluid inlet that reclaims the solvent groove equally, the liquid outlet of described recovery solvent groove is communicated with recovery solvent storage tank, and described recovery solvent storage tank is connected with and reclaims the solvent delivery pump;
Described recovery solvent delivery delivery side of pump is divided into two branch roads, and wherein branch road is communicated with the phegma mouth of rectifying tower, and another branch road is communicated with the top fluid inlet of secondary crystal reactor;
The bottom discharge mouth of described secondary crystal reactor is communicated with the opening for feed of the 4th whizzer, the liquid outlet of described the 4th whizzer is communicated with the fluid inlet of secondary crystal mother liquor groove, the liquid outlet of described secondary crystal mother liquor groove is connected with secondary crystal mother liquor transferpump, and described secondary crystal mother liquor carries delivery side of pump to be communicated with the top fluid inlet of primary crystallization reactor;
The bottom discharge mouth of described primary crystallization reactor is communicated with the opening for feed of the 3rd whizzer, the liquid outlet of described the 3rd whizzer is communicated with the fluid inlet of primary crystallization mother liquor groove, the liquid outlet of described primary crystallization mother liquor groove is connected with primary crystallization mother liquor transferpump, and described primary crystallization mother liquor carries delivery side of pump to be communicated with the top fluid inlet of reextraction reactor;
The bottom discharge mouth of described reextraction reactor is communicated with the opening for feed of the second whizzer, the liquid outlet of described the second whizzer is communicated with the fluid inlet of reextraction mother liquor groove, the liquid outlet of described reextraction mother liquor groove is connected with reextraction mother liquor transferpump, and described reextraction mother liquor carries delivery side of pump to be communicated with the top fluid inlet of single extraction reactor;
The discharge port of described the first whizzer is communicated with the first filter cake warehouse, and described the first filter cake warehouse is communicated with the top solid materials import of reextraction reactor;
The discharge port of described the second whizzer is communicated with the second filter cake warehouse, and described the second filter cake warehouse is communicated with the top solid materials import of primary crystallization reactor;
The discharge port of described the 3rd whizzer is communicated with the 3rd filter cake warehouse, and described the 3rd filter cake warehouse is communicated with the top solid materials import of secondary crystal reactor;
The discharge port of described the 4th whizzer is communicated with vacuum drier;
The discharge port of described the 5th whizzer is communicated with thick azophenlyene warehouse, and described thick azophenlyene warehouse is communicated with the top solid materials import of single extraction reactor;
The top of described single extraction reactor also is provided with the import of RT waste material;
The top of described secondary crystal reactor also is provided with the external solvent import.
The refrigerant of described condenser is cold water.
The heating agent of described reboiler is water vapour.
Compared with prior art the utlity model has following beneficial effect.
1, according to the technique from separation and purification azophenlyene the RT waste material reported to recently, the utility model can be realized twice solvent extraction, twice recrystallization process, solvent for use is recoverable all, and is few to the consumption of solvent; And have the route science, simple to operate, but the advantage such as continuity is strong
2, this technique only after single extraction the mother liquor to single extraction carry out the solvent distillation recycling step one time, gained reclaims the solvent of solvent as secondary crystal, the solvent of all the other single extractions, reextraction, primary crystallization is all the filtrated stock of next step, greatly reduce the solvent recuperation cost, reduce energy consumption, also reduced the consumption to solvent simultaneously.
3, the product purity that adopts system of the present utility model to produce is high, the commercialization pharmaceutical grade azophenlyene product purity the highest to purity requirement requires >=99.5%, adopts the azophenlyene of this explained hereafter, and purity can be stabilized in more than 99.8%, higher than the pharmaceutical grade requirement, can meet the need of market fully far away.
4, the azophenlyene product good crystalline produced of system of the present utility model and controlled, product is the solvent recrystallization gained, has crystalline form even, grain size is controlled, the dispersity advantages of higher, and can be according to customer demand, control crystal growing process, produce the product of different grain sizes, can avoid the pollution that feeds intake that causes because of dust fully, facilitate suitability for industrialized production.When recrystallization, if do not stir, can obtain the larger product of crystalline form near ctystallizing point; If stir, can obtain crystalline form than miscellaneous goods near ctystallizing point.The larger product purity of crystalline form can generally reach more than 99.8%; And crystalline form than miscellaneous goods purity mostly between 99.7 ~ 99.8%.Consider in addition the downstream client in use, the wetting property of the larger product of crystalline form, the accessibility that feeds intake may be better.
5, the single extraction mother liquor is reclaimed to rear gained raffinate through fusion-crystallization, in solid-liquid separation gained filter cake, azophenlyene content can reach 89.61%, can be used as thick azophenlyene fully and makes with extra care.And directly carry out rectifying, and be difficult to obtain the very high azophenlyene of purity, because azophenlyene boiling point (360 ℃) and fusing point (171 ℃) are all very high, the rectifying difficulty is very large.The main following points of the reason of fusion-crystallization: 1) the fusing point difference between material is very big, and the azophenlyene fusing point is 171 ℃; Nitrogen benzide is 71 ℃; 4-aminodiphenylamine is 75 ℃; Aniline is-6.2 ℃, therefore utilizes storeroom fusing point difference can adopt the mode of fusion-crystallization to separate, and controlling raffinate is 80 ℃, and all the other organism are all liquid except azophenlyene, therefore can separate; 2) fusion-crystallization employing when carrying out solvent recuperation, contained organic content except ethanol itself be with regard to less (its main component is still ethanol), not too suitablely carries out rectifying production; 3) resulting raffinate after carrying out solvent recuperation, wherein material component is very complicated, and organism kinds is a lot, and content is relatively all few, and the rectifying difficulty is very big, thus raffinate is carried out to fusion-crystallization, and do not carry out distillation operation.
Mother liquid obtained middle material consists of nitrogen benzide 38.83%, azophenlyene 21.42%, 4-aminodiphenylamine 2.62% simultaneously, can be used as raw material and returns to the RT production system, and can not increase the system burden.
6, adopt this technique purification azophenlyene, solvent is recovery all, and without residue contamination, liquid residue can be used as raw material and returns to the RT production system and do not produce waste liquor contamination, and whole process is the separating-purifying process, does not produce exhaust emission.
The accompanying drawing explanation
Fig. 1 is apparatus system schematic diagram of the present utility model.
in figure, 1 is the single extraction reactor, 2 is the reextraction reactor, 3 is the primary crystallization reactor, 4 is the secondary crystal reactor, 5 is single extraction mother liquor groove, 6 is reextraction mother liquor groove, 7 is primary crystallization mother liquor groove, 8 is secondary crystal mother liquor groove, 9 is still liquid groove, 10 for reclaiming the solvent groove, 11 for reclaiming the solvent storage tank, 12 is gas-liquid separator, 13 is rectifying tower, 14 is preheater, 15 is condenser, 16 is reboiler, 17 is the first whizzer, 18 is the second whizzer, 19 is the 3rd whizzer, 20 is the 4th whizzer, 21 is the 5th whizzer, 22 is single extraction mother liquor transferpump, 23 is reextraction mother liquor transferpump, 24 is primary crystallization mother liquor transferpump, 25 is secondary crystal mother liquor transferpump, 26 for reclaiming the solvent delivery pump, 27 is the raffinate transferpump, 28 is vacuum drier.
Embodiment
The utility model is described in further detail below in conjunction with specific embodiment.
for the 4-aminodiphenylamine waste material, extract the apparatus system of refining azophenlyene, as shown in Figure 1, comprise single extraction reactor 1, reextraction reactor 2, primary crystallization reactor 3, secondary crystal reactor 4, rectifying tower 13, the bottom discharge mouth of described single extraction reactor 1 is communicated with the opening for feed of the first whizzer 17, the liquid outlet of described the first whizzer 17 is communicated with the fluid inlet of single extraction mother liquor groove 5, the liquid outlet of described single extraction mother liquor groove 5 is connected with single extraction mother liquor transferpump 22, the output terminal of described single extraction mother liquor transferpump 22 is communicated with the fluid inlet of preheater 14, the liquid outlet of described preheater 14 is communicated with the inlet opening of rectifying tower 13,
At the bottom of the tower of described rectifying tower 13, the tubing of still liquid outlet is divided into two branch roads, and wherein branch road is communicated with the fluid inlet of reboiler 16, and the vapor outlet port of described reboiler 16 is communicated with the vapour inlet of rectifying tower 13; Another branch road is communicated with the fluid inlet of still liquid groove 9, the liquid outlet of described still liquid groove 9 is communicated with the opening for feed of the 5th whizzer 21, the liquid outlet of described the 5th whizzer 21 is connected with raffinate transferpump 27, and the output terminal of described raffinate transferpump 27 leads to the RT production system;
The overhead vapours outlet of described rectifying tower 13 is communicated with the vapour inlet of preheater 14, the vapor outlet port of described preheater 14 is communicated with the opening for feed of gas-liquid separator 12, the overhead vapor outlet of described gas-liquid separator 12 is communicated with the inlet mouth of cool condenser 15, the liquid outlet of described condenser 15 is communicated with the fluid inlet that reclaims solvent groove 10, the bottom liquid outlet of described gas-liquid separator 12 is communicated with the fluid inlet that reclaims solvent groove 10 equally, the liquid outlet of described recovery solvent groove 10 is communicated with recovery solvent storage tank 11, and described recovery solvent storage tank 11 is connected with and reclaims solvent delivery pump 26;
The output terminal of described recovery solvent delivery pump 26 is divided into two branch roads, and wherein branch road is communicated with the phegma mouth of rectifying tower 13, and another branch road is communicated with the top fluid inlet of secondary crystal reactor 4;
The bottom discharge mouth of described secondary crystal reactor 4 is communicated with the opening for feed of the 4th whizzer 20, the liquid outlet of described the 4th whizzer 20 is communicated with the fluid inlet of secondary crystal mother liquor groove 8, the liquid outlet of described secondary crystal mother liquor groove 8 is connected with secondary crystal mother liquor transferpump 25, and the output terminal of described secondary crystal mother liquor transferpump 25 is communicated with the top fluid inlet of primary crystallization reactor 3;
The bottom discharge mouth of described primary crystallization reactor 3 is communicated with the opening for feed of the 3rd whizzer 19, the liquid outlet of described the 3rd whizzer 19 is communicated with the fluid inlet of primary crystallization mother liquor groove 7, the liquid outlet of described primary crystallization mother liquor groove 7 is connected with primary crystallization mother liquor transferpump 24, and the output terminal of described primary crystallization mother liquor transferpump 24 is communicated with the top fluid inlet of reextraction reactor 2;
The bottom discharge mouth of described reextraction reactor 2 is communicated with the opening for feed of the second whizzer 18, the liquid outlet of described the second whizzer 18 is communicated with the fluid inlet of reextraction mother liquor groove 6, the liquid outlet of described reextraction mother liquor groove 6 is connected with reextraction mother liquor transferpump 23, and the output terminal of described reextraction mother liquor transferpump 23 is communicated with the top fluid inlet of single extraction reactor 1;
The discharge port of described the first whizzer 17 is communicated with the first filter cake warehouse, and described the first filter cake warehouse is communicated with the top solid materials import of reextraction reactor 2;
The discharge port of described the second whizzer 18 is communicated with the second filter cake warehouse, and described the second filter cake warehouse is communicated with the top solid materials import of primary crystallization reactor 3;
The discharge port of described the 3rd whizzer 19 is communicated with the 3rd filter cake warehouse, and described the 3rd filter cake warehouse is communicated with the top solid materials import of secondary crystal reactor 4;
The discharge port of described the 4th whizzer 20 is communicated with vacuum drier 28;
The discharge port of described the 5th whizzer 21 is communicated with thick azophenlyene warehouse, and described thick azophenlyene warehouse is communicated with the top solid materials import of single extraction reactor 1;
The top of described single extraction reactor 1 also is provided with the import of RT waste material;
The top of described secondary crystal reactor 4 also is provided with the external solvent import.
Its workflow is as follows:
The solid materials of the 5th whizzer 21 and send into single extraction reactor 1 by solid materials import and the import of RT waste material at single extraction reactor 1 top respectively from the RT waste material of RT production system, the reextraction mother liquor is sent into single extraction reactor 1 by reextraction mother liquor transferpump 23 by the fluid inlet at single extraction reactor 1 top, material after 1 extraction of single extraction reactor is sent into the first whizzer 17 and is carried out solid-liquid separation, and the gained solid materials is sent into reextraction reactor 2 by the solid materials import at reextraction reactor 2 tops;
The isolated single extraction mother liquor of the first whizzer 17 is sent into single extraction mother liquor groove 5, and single extraction mother liquor transferpump 22 is sent the single extraction mother liquor in single extraction mother liquor groove 5 into preheater 14 and carried out after preheating being transported to rectifying tower 13 from the fluid inlet of rectifying tower 13 and carry out rectifying; Described preheater 14 heats by the solvent vapour of rectifying tower 13 overhead vapor outlet outputs;
After described solvent vapour carries out heat exchange with the single extraction mother liquor of sending into preheater 14, enter gas-liquid separator 12 and carry out gas-liquid separation, liquid solvent is delivered directly to and reclaims solvent groove 10, gaseous solvent is transported to equally and reclaims solvent groove 10 after condenser 15 is condensed into liquid state, the solvent that reclaims in solvent groove 10 is sent into recovery solvent storage tank 11, reclaim solvent delivery pump 26 and will reclaim a recovery solvent part in solvent storage tank 11 and be transported to rectifying tower 13 and reflux, another part is transported to secondary crystal reactor 4;
Described primary crystallization mother liquor is sent into reextraction reactor 2 by primary crystallization mother liquor transferpump 24 by the fluid inlet at reextraction reactor 2 tops, solid materials from the first whizzer 17 is extracted, material after 2 extractions of reextraction reactor is sent into the second whizzer 18 and is carried out solid-liquid separation, and the gained solid materials enters primary crystallization reactor 3 by the solid materials import at primary crystallization reactor 3 tops; The isolated reextraction mother liquor of the second whizzer 18 is sent into reextraction mother liquor groove 6;
Described secondary crystal mother liquor is sent into primary crystallization reactor 3 by secondary crystal mother liquor transferpump 25 by the fluid inlet at primary crystallization reactor 3 tops, solid materials from the second whizzer 18 is dissolved and crystallization, material after 3 dissolvings of primary crystallization reactor, crystallization is sent into the 3rd whizzer 19 and is carried out solid-liquid separation, and the gained solid materials enters secondary crystal reactor 4 by the solid materials import at secondary crystal reactor 4 tops; The isolated primary crystallization mother liquor of the 3rd whizzer 19 is sent into primary crystallization mother liquor groove 7;
Described secondary crystal reactor 4 utilizes the recovery solvent to dissolve and crystallization the solid materials from the 3rd whizzer 19, through secondary crystal reactor 4 dissolve, material after crystallization sends into the 4th whizzer 20 and carries out solid-liquid separation, the gained solid materials is sent into vacuum drier 28 and is carried out drying and obtain refining azophenlyene; The isolated secondary crystal mother liquor of the 4th whizzer 20 is sent into secondary crystal mother liquor groove 8;
At the bottom of the tower of described rectifying tower 13, a still liquid part enters reboiler 16 gasification and by the bottom vapour inlet of rectifying tower 13, enters rectifying tower 13 rectifying that circulates for solvent vapour, another part is transported to still liquid groove 9 carries out crystallization in still liquid groove 9 after to be sent into the 5th whizzer 21 and carries out solid-liquid separation, the gained solid materials is sent into single extraction reactor 1, and the raffinate after centrifugal is sent to the RT production system;
Described secondary crystal reactor 4, when operation first or recovery solvent deficiency, can add solvent by the external solvent import at its top.
The above is explained in detail embodiment of the present utility model by reference to the accompanying drawings, but the utility model is not limited to above-described embodiment, in the ken that those of ordinary skills possess, can also under the prerequisite that does not break away from the utility model aim, make various variations.

Claims (3)

1. for the 4-aminodiphenylamine waste material, extract the apparatus system of refining azophenlyene, comprise single extraction reactor (1), reextraction reactor (2), primary crystallization reactor (3), secondary crystal reactor (4), rectifying tower (13), it is characterized in that:
The bottom discharge mouth of described single extraction reactor (1) is communicated with the opening for feed of the first whizzer (17), the liquid outlet of described the first whizzer (17) is communicated with the fluid inlet of single extraction mother liquor groove (5), the liquid outlet of described single extraction mother liquor groove (5) is connected with single extraction mother liquor transferpump (22), the output terminal of described single extraction mother liquor transferpump (22) is communicated with the fluid inlet of preheater (14), and the liquid outlet of described preheater (14) is communicated with the inlet opening of rectifying tower (13);
At the bottom of the tower of described rectifying tower (13), the tubing of still liquid outlet is divided into two branch roads, and wherein branch road is communicated with the fluid inlet of reboiler (16), and the vapor outlet port of described reboiler (16) is communicated with the vapour inlet of rectifying tower (13); Another branch road is communicated with the fluid inlet of still liquid groove (9), the liquid outlet of described still liquid groove (9) is communicated with the opening for feed of the 5th whizzer (21), the liquid outlet of described the 5th whizzer (21) is connected with raffinate transferpump (27), and the output terminal of described raffinate transferpump (27) leads to the RT production system;
the overhead vapours outlet of described rectifying tower (13) is communicated with the vapour inlet of preheater (14), the vapor outlet port of described preheater (14) is communicated with the opening for feed of gas-liquid separator (12), the overhead vapor outlet of described gas-liquid separator (12) is communicated with the inlet mouth of cool condenser (15), the liquid outlet of described condenser (15) is communicated with the fluid inlet that reclaims solvent groove (10), the bottom liquid outlet of described gas-liquid separator (12) is communicated with the fluid inlet that reclaims solvent groove (10) equally, the liquid outlet of described recovery solvent groove (10) is communicated with recovery solvent storage tank (11), described recovery solvent storage tank (11) is connected with and reclaims solvent delivery pump (26),
The output terminal of described recovery solvent delivery pump (26) is divided into two branch roads, and wherein branch road is communicated with the phegma mouth of rectifying tower (13), and another branch road is communicated with the top fluid inlet of secondary crystal reactor (4);
The bottom discharge mouth of described secondary crystal reactor (4) is communicated with the opening for feed of the 4th whizzer (20), the liquid outlet of described the 4th whizzer (20) is communicated with the fluid inlet of secondary crystal mother liquor groove (8), the liquid outlet of described secondary crystal mother liquor groove (8) is connected with secondary crystal mother liquor transferpump (25), and the output terminal of described secondary crystal mother liquor transferpump (25) is communicated with the top fluid inlet of primary crystallization reactor (3);
The bottom discharge mouth of described primary crystallization reactor (3) is communicated with the opening for feed of the 3rd whizzer (19), the liquid outlet of described the 3rd whizzer (19) is communicated with the fluid inlet of primary crystallization mother liquor groove (7), the liquid outlet of described primary crystallization mother liquor groove (7) is connected with primary crystallization mother liquor transferpump (24), and the output terminal of described primary crystallization mother liquor transferpump (24) is communicated with the top fluid inlet of reextraction reactor (2);
The bottom discharge mouth of described reextraction reactor (2) is communicated with the opening for feed of the second whizzer (18), the liquid outlet of described the second whizzer (18) is communicated with the fluid inlet of reextraction mother liquor groove (6), the liquid outlet of described reextraction mother liquor groove (6) is connected with reextraction mother liquor transferpump (23), and the output terminal of described reextraction mother liquor transferpump (23) is communicated with the top fluid inlet of single extraction reactor (1);
The discharge port of described the first whizzer (17) is communicated with the first filter cake warehouse, and described the first filter cake warehouse is communicated with the top solid materials import of reextraction reactor (2);
The discharge port of described the second whizzer (18) is communicated with the second filter cake warehouse, and described the second filter cake warehouse is communicated with the top solid materials import of primary crystallization reactor (3);
The discharge port of described the 3rd whizzer (19) is communicated with the 3rd filter cake warehouse, and described the 3rd filter cake warehouse is communicated with the top solid materials import of secondary crystal reactor (4);
The discharge port of described the 4th whizzer (20) is communicated with vacuum drier (28);
The discharge port of described the 5th whizzer (21) is communicated with thick azophenlyene warehouse, and described thick azophenlyene warehouse is communicated with the top solid materials import of single extraction reactor (1);
The top of described single extraction reactor (1) also is provided with the import of RT waste material;
The top of described secondary crystal reactor (4) also is provided with the external solvent import.
2. for the 4-aminodiphenylamine waste material, extract according to claim 1 the apparatus system of refining azophenlyene, it is characterized in that: the refrigerant of described condenser (15) is cold water.
3. for the 4-aminodiphenylamine waste material, extract according to claim 1 the apparatus system of refining azophenlyene, it is characterized in that: the heating agent of described reboiler (16) is water vapour.
CN2013203159218U 2013-06-04 2013-06-04 Device system used for extracting and refining azophenylene in RT base waste Expired - Fee Related CN203295403U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104529916A (en) * 2014-12-25 2015-04-22 天津大学 Method for separating high-purity phenazine from waste material generated in chemical product production
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104529916A (en) * 2014-12-25 2015-04-22 天津大学 Method for separating high-purity phenazine from waste material generated in chemical product production
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

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