CN103232402A - Method for extracting refined phenazine from RT base wastes - Google Patents
Method for extracting refined phenazine from RT base wastes Download PDFInfo
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- CN103232402A CN103232402A CN2013102171734A CN201310217173A CN103232402A CN 103232402 A CN103232402 A CN 103232402A CN 2013102171734 A CN2013102171734 A CN 2013102171734A CN 201310217173 A CN201310217173 A CN 201310217173A CN 103232402 A CN103232402 A CN 103232402A
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- mother liquor
- filter cake
- azophenlyene
- reextraction
- waste material
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- 239000002699 waste material Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 27
- VEPOHXYIFQMVHW-XOZOLZJESA-N 2,3-dihydroxybutanedioic acid (2S,3S)-3,4-dimethyl-2-phenylmorpholine Chemical compound OC(C(O)C(O)=O)C(O)=O.C[C@H]1[C@@H](OCCN1C)c1ccccc1 VEPOHXYIFQMVHW-XOZOLZJESA-N 0.000 title abstract 7
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 title abstract 7
- 238000002425 crystallisation Methods 0.000 claims abstract description 61
- 230000008025 crystallization Effects 0.000 claims abstract description 41
- 239000013078 crystal Substances 0.000 claims abstract description 30
- 238000000605 extraction Methods 0.000 claims abstract description 29
- 238000007670 refining Methods 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 17
- 239000012452 mother liquor Substances 0.000 claims description 75
- 239000012065 filter cake Substances 0.000 claims description 53
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000010992 reflux Methods 0.000 claims description 24
- 230000000630 rising effect Effects 0.000 claims description 24
- 238000001914 filtration Methods 0.000 claims description 16
- 238000005119 centrifugation Methods 0.000 claims description 15
- 238000004821 distillation Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 13
- 239000000706 filtrate Substances 0.000 claims description 10
- 239000002893 slag Substances 0.000 claims description 10
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 abstract description 18
- 239000007788 liquid Substances 0.000 abstract description 10
- 238000001953 recrystallisation Methods 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 16
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 5
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- ATGUVEKSASEFFO-UHFFFAOYSA-N p-aminodiphenylamine Chemical compound C1=CC(N)=CC=C1NC1=CC=CC=C1 ATGUVEKSASEFFO-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005935 nucleophilic addition reaction Methods 0.000 description 1
- 239000012434 nucleophilic reagent Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for extracting refined phenazine from RT base wastes, belonging to the technical field of phenazine refining. The method provided by the invention has the advantages that high-purity phenazine crystals can be obtained, used solvents are all recovered and repeatedly-used solvents, and no waste liquid pollution exists. The adopted technical scheme is as follows: the refined phenazine is obtained in a manner that the RT base wastes are subjected to extraction twice, recrystallization twice, drying, solvent recovery and melting crystallization. According to the phenazine produced by the method, the purity can be stabilized over 99.8%, is much higher than the requirements of a pharmaceutical grade and can fully meet the market demand. The method is widely applied to the field of extracting the refined phenazine from the RT base wastes.
Description
Technical field
A kind of method of extracting refining azophenlyene from RT training department waste material of the present invention belongs to azophenlyene purification techniques field.
Background technology
Produce in the process of RT training department in the oil of mirbane method, 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 RT training department, the ortho position of attack oil of mirbane then generates the by product azophenlyene of this reaction.From reaction mechanism we as can be seen, azophenlyene be in the RT training department production process the by product that will inevitably produce, therefore it is fully utilized, be the important topic of pendulum in face of RT manufacturing enterprise.
Yet, be in the process of raw material production RT training department with oil of mirbane and aniline, the by product azophenlyene that produces is difficult to effectively separate by present production technique, be mixed into waste material with minor amounts of aniline, 4-aminodiphenylamine, nitrogen benzide, directly discharge or burn not only contaminate environment, and cause the resource significant wastage.The existing method of extracting azophenlyene from the RT waste material is as described in the 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-aminodiphenylamine, nitrogen benzide etc., operational cycle is long, the cost recovery height.
Summary of the invention
The present invention provides a kind of and can access highly purified azophenlyene crystal in order to overcome the deficiencies in the prior art, and solvent for use is all the recovery set solvent, the method for purification of no waste liquor contamination.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of extracting refining azophenlyene from RT training department waste material is carried out according to following steps:
The first step, single extraction
RT training department waste material is added in the reextraction mother liquor, and the ratio of described RT training department's waste material and reextraction mother liquor is 1:5-9(g:mL), temperature rising reflux 30-60min is cooled to 25 ℃ of centrifugations again, obtains filter cake and single extraction mother liquor;
Second step, fusion-crystallization
Described single extraction mother liquor is collected 77-80 ℃ of cut and is obtained reclaiming ethanol 80 ℃ of down distillations, and the raffinate after the distillation is at 80 ℃ down behind the insulation 30min, and pouring in the suction funnel that is preheating to 80 ℃ and the filter flask fast, filtration obtains thick azophenlyene and fusion-crystallization mother liquor;
The 3rd step, reextraction
Described filter cake is added in the primary crystallization mother liquor, and the ratio of described filter cake and primary crystallization mother liquor is 1:8-12(g:mL), temperature rising reflux 45-90min, suction filtration when being cooled to 25 ℃ obtains reextraction filter cake and described reextraction mother liquor;
The 4th step, primary crystallization
Described reextraction filter cake is added in the secondary crystal mother liquor, the ratio of described reextraction filter cake and secondary crystal mother liquor is 1:5-9(g:mL), temperature rising reflux 30-60min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 120-180min, obtains primary crystallization filter cake and described primary crystallization mother liquor through centrifugation;
The 5th step, secondary crystal
Described primary crystallization filter cake is added in the described recovery ethanol, the ratio of described primary crystallization filter cake and described recovery ethanol is 1:7-10(g:mL), temperature rising reflux 30-60min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 120-180min, obtains refining azophenlyene and described secondary crystal mother liquor through centrifugation.
The second described thick azophenlyene that obtain of step is sneaked in the described RT training department waste material and is entered the single extraction step together, further makes with extra care; Described fusion-crystallization mother liquor returns in the production of RT training department.
Near ctystallizing point, leave standstill the refining azophenlyene product that can obtain big crystalline form in described the 5th step secondary crystal step.
The present invention compared with prior art has following beneficial effect.
1, according to the technology of having reported of separation and purification azophenlyene from the RT waste material to recently, twice solvent extraction of this process using, twice recrystallization process, all solvents are all the recovery set solvent, have the route science, and are simple to operate, but advantage such as continuity is strong.
2, this technology is only carried out the solvent distillation recycling step one time to the single extraction mother liquor behind single extraction, gained reclaims solvent as the solvent of secondary crystal, the solvent of all the other single extractions, reextraction, primary crystallization is all the filtrated stock of next step, reduce the solvent recuperation cost greatly, reduce energy consumption, also reduced the consumption to solvent simultaneously.
3, product purity height, 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%, is higher than the pharmaceutical grade requirement far away, can meet the need of market fully.
4, product good crystalline and controlled, product is the solvent recrystallization gained, it is even to have crystalline form, grain size is controlled, the dispersity advantages of higher, and can be according to customer demand, the control crystal growing process, produce the product of different grain sizes, can avoid the pollution that feeds intake that causes because of dust fully, make things convenient for suitability for industrialized production.When recrystallization, if near ctystallizing point, do not stir, can obtain the big product of crystalline form; If near ctystallizing point, stir, can obtain crystalline form than miscellaneous goods.The big product purity of crystalline form can generally reach more than 99.8%; And the less product purity of crystalline form is mostly between 99.7 ~ 99.8%.Consider the downstream client in addition in use, the wetting property of the big product of crystalline form, the accessibility that feeds intake may be better.
5, the single extraction mother liquor is reclaimed back gained raffinate through fusion-crystallization, azophenlyene content can reach 89.61% in the solid-liquid separation gained filter cake, can be used as thick azophenlyene fully and makes with extra care.And directly carry out rectifying, and then 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 big.The main following points of the reason of fusion-crystallization: 1) the fusing point difference between the material is very big, and the azophenlyene fusing point is 171 ℃; Nitrogen benzide is 71 ℃; RT training department is 75 ℃; Aniline is-6.2 ℃, therefore utilizes storeroom fusing point difference can adopt the mode of fusion-crystallization to separate, and the control raffinate is 80 ℃, and all the other organism are all liquid except azophenlyene, therefore can separate; 2) fusion-crystallization adopts when carrying out solvent recuperation, and the organic content except ethanol that itself contains is with regard to less (its main component still is ethanol), and rectifying production not too suits to carry out; 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 fusion-crystallization, and do not carry out distillation operation.
Material consists of nitrogen benzide 38.83%, azophenlyene 21.42%, RT training department 2.62% in simultaneously mother liquid obtained, can be used as raw material and returns the RT production system, and can not increase the system burden.
6, adopt this technology purification azophenlyene, solvent is recovery set usefulness all, and no residue contamination, liquid residue can be used as raw material and return the RT production system and do not produce waste liquor contamination, and whole process does not produce exhaust emission for separating purification process.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
A kind of method of extracting refining azophenlyene from RT training department waste material is carried out according to following steps:
The first step, single extraction
RT training department waste material is added in the reextraction mother liquor, and the ratio of described RT training department's waste material and reextraction mother liquor is 1:5(g:mL), temperature rising reflux 60min is cooled to 25 ℃ of centrifugations again, obtains filter cake and single extraction mother liquor;
Second step, fusion-crystallization
Described single extraction mother liquor is collected 77-80 ℃ of cut and is obtained reclaiming ethanol 80 ℃ of down distillations, and the raffinate after the distillation is at 80 ℃ down behind the insulation 30min, and pouring in the suction funnel that is preheating to 80 ℃ and the filter flask fast, filtration obtains thick azophenlyene and fusion-crystallization mother liquor;
The 3rd step, reextraction
Described filter cake is added in the primary crystallization mother liquor, and the ratio of described filter cake and primary crystallization mother liquor is 1:12(g:mL), temperature rising reflux 45min, suction filtration when being cooled to 25 ℃ obtains reextraction filter cake and described reextraction mother liquor;
The 4th step, primary crystallization
Described reextraction filter cake is added in the secondary crystal mother liquor, the ratio of described reextraction filter cake and secondary crystal mother liquor is 1:9(g:mL), temperature rising reflux 30min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 120min, obtains primary crystallization filter cake and described primary crystallization mother liquor through centrifugation;
The 5th step, secondary crystal
Described primary crystallization filter cake is added in the described recovery ethanol, the ratio of described primary crystallization filter cake and described recovery ethanol is 1:7(g:mL), temperature rising reflux 30min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 180min, obtains refining azophenlyene and described secondary crystal mother liquor through centrifugation.
The second described thick azophenlyene that obtain of step is sneaked in the described RT training department waste material and is entered the single extraction step together, further makes with extra care; Described fusion-crystallization mother liquor returns in the production of RT training department.
Embodiment 2
Solvent extraction process: 100gRT training department waste material is joined in the 700mL reextraction mother liquor, and temperature rising reflux 1h places the about 1h of cold water chilling cooling then, suction filtration when being chilled to 25 ℃, fully filter is done, and obtains the about 70g single extraction of weight in wet base filter cake, the about 700mL of single extraction mother liquor.To once slightly go filter cake to join in the 700mL primary crystallization mother liquor, temperature rising reflux 1h places the about 1h of cold water chilling cooling again, suction filtration when being chilled to 25 ℃, and fully filter is done, and obtains the about 62g reextraction of weight in wet base filter cake, the about 700mL of reextraction mother liquor.
Recrystallization process: the reextraction filter cake is joined in the 800mL secondary crystal mother liquor, temperature rising reflux 30min, after leaving standstill 3min again, supernatant liquid is inclined to about 2/3 and go in the filter flask, lower floor's liquid poured in the suction funnel that is preheating to 80 ℃ and the filter flask filter fast, mother liquid obtainedly in filter flask, slowly be cooled to 25 ℃, filter, obtain the primary crystallization filter cake of the about 60g of weight in wet base, the about 740mL of primary crystallization mother liquor.Gained primary crystallization filter cake is joined in 800mL dehydrated alcohol or the recovery ethanol, temperature rising reflux 15min, gained solution is left standstill the visual crystallite size of wanting of about 2.4h(in room temperature, after separating out solid, sway and namely get crystalline form than miscellaneous goods), be chilled to 25 ℃ of after-filtration, get the refining azophenlyene of the about 50g of weight in wet base, the about 800mL of secondary crystal mother liquor.
Product oven dry: place 80 ℃ of baking ovens to dry 6h secondary crystal gained solid, namely get the refining about 43g of dry azophenlyene.
Solvent recuperation: 2000mL single extraction mother liquor under 80 ℃, is collected 77 ~ 80 ℃ of cuts, namely get and reclaim ethanol 1820mL, the rate of recovery is about 91.0%, can be used for substituting in the secondary crystal dehydrated alcohol.The gained raffinate is at 80 ℃ down behind the insulation 30min, pours in the suction funnel that is preheating to 80 ℃ and the filter flask and filters fast.Azophenlyene content is 89.61% in the gained filter cake, can make with extra care with thick azophenlyene, mother liquid obtained in nitrogen benzide content be 38.31%, azophenlyene content is 21.42%, can return condensation workshop section.
Embodiment 3
A kind of method of extracting refining azophenlyene from RT training department waste material is carried out according to following steps:
The first step, single extraction
RT training department waste material is added in the reextraction mother liquor, and the ratio of described RT training department's waste material and reextraction mother liquor is 1:9(g:mL), temperature rising reflux 60min is cooled to 25 ℃ of centrifugations again, obtains filter cake and single extraction mother liquor;
Second step, fusion-crystallization
Described single extraction mother liquor is collected 77-80 ℃ of cut and is obtained reclaiming ethanol 80 ℃ of down distillations, and the raffinate after the distillation is at 80 ℃ down behind the insulation 30min, and pouring in the suction funnel that is preheating to 80 ℃ and the filter flask fast, filtration obtains thick azophenlyene and fusion-crystallization mother liquor;
The 3rd step, reextraction
Described filter cake is added in the primary crystallization mother liquor, and the ratio of described filter cake and primary crystallization mother liquor is 1:8(g:mL), temperature rising reflux 45min, suction filtration when being cooled to 25 ℃ obtains reextraction filter cake and described reextraction mother liquor;
The 4th step, primary crystallization
Described reextraction filter cake is added in the secondary crystal mother liquor, the ratio of described reextraction filter cake and secondary crystal mother liquor is 1:9(g:mL), temperature rising reflux 30min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 180min, obtains primary crystallization filter cake and described primary crystallization mother liquor through centrifugation;
The 5th step, secondary crystal
Described primary crystallization filter cake is added in the described recovery ethanol, the ratio of described primary crystallization filter cake and described recovery ethanol is 1:10(g:mL), temperature rising reflux 60min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 120min, obtains refining azophenlyene and described secondary crystal mother liquor through centrifugation.
The second described thick azophenlyene that obtain of step is sneaked in the described RT training department waste material and is entered the single extraction step together, further makes with extra care; Described fusion-crystallization mother liquor returns in the production of RT training department.
Embodiment 4
A kind of method of extracting refining azophenlyene from RT training department waste material is carried out according to following steps:
The first step, single extraction
RT training department waste material is added in the reextraction mother liquor, and the ratio of described RT training department's waste material and reextraction mother liquor is 1:7(g:mL), temperature rising reflux 50min is cooled to 25 ℃ of centrifugations again, obtains filter cake and single extraction mother liquor;
Second step, fusion-crystallization
Described single extraction mother liquor is collected 77-80 ℃ of cut and is obtained reclaiming ethanol 80 ℃ of down distillations, and the raffinate after the distillation is at 80 ℃ down behind the insulation 30min, and pouring in the suction funnel that is preheating to 80 ℃ and the filter flask fast, filtration obtains thick azophenlyene and fusion-crystallization mother liquor;
The 3rd step, reextraction
Described filter cake is added in the primary crystallization mother liquor, and the ratio of described filter cake and primary crystallization mother liquor is 1:10(g:mL), temperature rising reflux 60min, suction filtration when being cooled to 25 ℃ obtains reextraction filter cake and described reextraction mother liquor;
The 4th step, primary crystallization
Described reextraction filter cake is added in the secondary crystal mother liquor, the ratio of described reextraction filter cake and secondary crystal mother liquor is 1:6(g:mL), temperature rising reflux 45min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 120-180min, obtains primary crystallization filter cake and described primary crystallization mother liquor through centrifugation;
The 5th step, secondary crystal
Described primary crystallization filter cake is added in the described recovery ethanol, the ratio of described primary crystallization filter cake and described recovery ethanol is 1:8(g:mL), temperature rising reflux 50min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 150min, obtains refining azophenlyene and described secondary crystal mother liquor through centrifugation.
The second described thick azophenlyene that obtain of step is sneaked in the described RT training department waste material and is entered the single extraction step together, further makes with extra care; Described fusion-crystallization mother liquor returns in the production of RT training department.
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character.Therefore, no matter from that, above-mentioned embodiment of the present invention all can only be thought can not limit invention to explanation of the present invention, claims have been pointed out scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, in the implication suitable with claims of the present invention and any variation in the scope, all should think to be included in the scope of claims.
Claims (3)
1. one kind is extracted the method made from extra care azophenlyene from RT training department waste material, it is characterized in that carrying out according to following steps:
The first step, single extraction
RT training department waste material is added in the reextraction mother liquor, and the ratio of described RT training department's waste material and reextraction mother liquor is 1:5-9(g:mL), temperature rising reflux 30-60min is cooled to 25 ℃ of centrifugations again, obtains filter cake and single extraction mother liquor;
Second step, fusion-crystallization
Described single extraction mother liquor is collected 77-80 ℃ of cut and is obtained reclaiming ethanol 80 ℃ of down distillations, and the raffinate after the distillation is at 80 ℃ down behind the insulation 30min, and pouring in the suction funnel that is preheating to 80 ℃ and the filter flask fast, filtration obtains thick azophenlyene and fusion-crystallization mother liquor;
The 3rd step, reextraction
Described filter cake is added in the primary crystallization mother liquor, and the ratio of described filter cake and primary crystallization mother liquor is 1:8-12(g:mL), temperature rising reflux 45-90min, suction filtration when being cooled to 25 ℃ obtains reextraction filter cake and described reextraction mother liquor;
The 4th step, primary crystallization
Described reextraction filter cake is added in the secondary crystal mother liquor, the ratio of described reextraction filter cake and secondary crystal mother liquor is 1:5-9(g:mL), temperature rising reflux 30-60min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 120-180min, obtains primary crystallization filter cake and described primary crystallization mother liquor through centrifugation;
The 5th step, secondary crystal
Described primary crystallization filter cake is added in the described recovery ethanol, the ratio of described primary crystallization filter cake and described recovery ethanol is 1:7-10(g:mL), temperature rising reflux 30-60min, heat filtering is removed insoluble slag, filtrate is at room temperature slowly lowered the temperature behind the 120-180min, obtains refining azophenlyene and described secondary crystal mother liquor through centrifugation.
2. a kind of method of extracting refining azophenlyene from RT training department waste material according to claim 1 is characterized in that described thick azophenlyene that second step obtained is sneaked in the described RT training department waste material to enter the single extraction step together, further makes with extra care; Described fusion-crystallization mother liquor returns in the production of RT training department.
3. a kind of method of extracting refining azophenlyene from RT training department waste material according to claim 1 is characterized in that leaving standstill the refining azophenlyene product that can obtain big crystalline form in described the 5th step secondary crystal step near ctystallizing point.
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| CN103992281B (en) * | 2014-05-29 | 2016-07-06 | 山西翔宇化工有限公司 | A kind of method extracting high-purity azophenlyene from 4-aminodiphenylamine by-product waste material |
| 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 |
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Effective date of registration: 20180110 Address after: Bei Jing 044100 Shanxi Province Linyi County Shijiazhuang Township Village residents group ninth Patentee after: Zhang Guozhu Address before: The 044100 Shanxi city of Yuncheng Province Linyi County TOYOKI Industrial Park (East) Patentee before: Shanxi Xiangyu Chemical Industries Co., Ltd. |