CN105294451A - Treatment method for extracting aniline by means of nitrobenzene - Google Patents

Treatment method for extracting aniline by means of nitrobenzene Download PDF

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Publication number
CN105294451A
CN105294451A CN201510721849.2A CN201510721849A CN105294451A CN 105294451 A CN105294451 A CN 105294451A CN 201510721849 A CN201510721849 A CN 201510721849A CN 105294451 A CN105294451 A CN 105294451A
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China
Prior art keywords
extraction
aniline
nitrobenzene
treatment
solution
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Pending
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CN201510721849.2A
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Chinese (zh)
Inventor
李定山
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CHONGQING CHANGFENG CHEMICAL INDUSTRY Co Ltd
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CHONGQING CHANGFENG CHEMICAL INDUSTRY Co Ltd
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Priority to CN201510721849.2A priority Critical patent/CN105294451A/en
Publication of CN105294451A publication Critical patent/CN105294451A/en
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Abstract

The invention discloses a treatment method for extracting aniline by means of nitrobenzene. The treatment method comprises the steps that 1, extraction is performed; 2, standing is performed; 3, separation is performed; 4, leaching is performed; 5, after leaching is performed, the temperature of a leached nitrobenzene solution is increased to 50 DEG C-60 DEG C, impurities on the solution level of the nitrobenzene solution are adsorbed by adopting a vacuum adsorbing method, and treatment is completed. According to the treatment method for extracting the aniline by means of the nitrobenzene, the frequency of treating a catalyst and a distribution plate is reduced, and the production efficiency is improved.

Description

For the treatment process of nitrobenzene extraction aniline
Technical field
The present invention relates to chemical field, be specifically related to a kind for the treatment of process for nitrobenzene extraction aniline.
Background technology
Aniline aniline also known as phenylamine, aniline oils, amino-benzene, molecular formula: C 6h 7n.Colourless oil liquid.Slightly water-soluble, be soluble in the organic solvent such as ethanol, ether, aniline is one of most important amine substance, mainly for the manufacture of dyestuff, medicine, resin, thiofide etc. can also be used as, itself also can be used as black dyes and uses, and its derivative tropeolin-D can be used as the indicator of acid base titration.
Aniline Production mainly adopts oil of mirbane to make, waste water can be produced in process, in waste water, main component is aniline, containing aniline about 1000ppm in aniline waste water, enters environment friendly system and carries out wastewater treatment, this process energy consumption is high, waste water needs environmental protection to carry out end-o f-pipe-control, therefore, needs aniline recovery to use, common recovery method has: distillation method, extraction process, biological process, the most frequently used distillation method and extraction process.Distillation method uses steam distillation aniline recovery, and because the latent heat of water is comparatively large, adopt rectification process aniline recovery from water, energy consumption is higher, and fluctuation of service, often occurs aniline too high levels phenomenon in the waste water of discharge; Therefore, adopt extraction process more, be utilize nitrobenzene extraction aniline, reclaimed the aniline in waste water, the aniline waste water after extraction is used for oil of mirbane and produces, and has accomplished the zero release of aniline waste water and the saving of steam; After existing nitrobenzene extraction aniline, produce in the process of aniline due to oil of mirbane and can produce other impurity, therefore after extraction, oil of mirbane contains suspended substance, amine substance, use this oil of mirbane to produce aniline, distribuor of fluidized bed can be caused within one month, just to occur blocking, and must stop processes catalyzer and grid distributor, maintenance is frequent, thus affects production efficiency.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of frequency reducing process catalyzer and grid distributor, the treatment process for nitrobenzene extraction aniline of enhancing productivity.
In order to solve the problems of the technologies described above, the invention provides following technical scheme: for the treatment process of nitrobenzene extraction aniline, comprise steps A: extraction, B: standing, C: separation, D: extraction step, also step e is included: the operation of step e is as follows: the nitrobenzene solution after extracting is warming up to 50 ~ 60 DEG C after extraction step, adopt vacuum suck method to be drawn by the ullage impurity of nitrobenzene solution, process completes.
Adopt the treatment process for nitrobenzene extraction aniline of technical solution of the present invention, oil of mirbane after extraction is due to containing suspended substance, in the process of producing, usual blocking grid distributor, existing way is cleared up by the suspended substance that grid distributor is piled up, in the process of practice, contriver finds, suspended substance can be vaporized at a certain temperature, and therefore, contriver adds after extraction and is warming up to 50 ~ 60 DEG C, after suspended substance is vaporized, suspended substance removes by recycling vacuum suck, verifies reality factually, can remove the suspended impurity of in oil of mirbane 90%.
The invention has the beneficial effects as follows: compare with the mode of catalyzer with existing cleaning grid distributor, fundamentally remove suspended substance, thus reduce the risk of blocking grid distributor and catalyzer, reduce the frequency of process catalyzer and grid distributor, enhance productivity.
Further, in described step e, the temperature of p-nitrophenyl solution warms is 58 DEG C.According to experimental studies have found that, 58 DEG C of effects removing suspended substance are best.
Further, in described step e, while p-nitrophenyl heats up, it is stirred.Suspended impurity in oil of mirbane fully can be vaporized, thus remove fully.
Further, described step e vacuum suck method adopts swirl vacuum absorption method.Namely swirl vacuum absorption adopt swirl shape absorption, in the process of absorption, suspended substance can be collected in vacuum absorption device, thus be convenient to cleaning.
Further, after the swirl vacuum absorption of described step e, with gac by impurity absorption.Gac is positioned in swirl vacuum adsorption unit, utilizes the adsorption of gac to be removed by the suspended impurity removed.
Further, in the extraction process of described steps A, solvent ratio is 1.27.Extraction is using oil of mirbane as extraction agent, is added in aniline, and aniline is dissolved in oil of mirbane, finds according to the study, and when solvent ratio is 1.27, the aniline content of its extraction is the highest.
Further, the temperature during extraction process of described steps A is between 20 ~ 25 DEG C.When temperature is between 20 ~ 25 DEG C, the aniline content of extraction is the highest.
Further, the time of repose of described step B is 36 ~ 42min.When time of repose is 36 ~ 42min, the aniline content of separation is the highest.
Further, in triplicate, the extracting phase after first time is separated adds oil of mirbane again for described steps A, B, C, second time repeating step A, B, C; Extracting phase after second time is separated adds oil of mirbane again, and third time repeats A, B, C, mixes the extraction phase after being separated for three times, then operation steps D.Through three extractions, leave standstill and be separated, the aniline content obtained is the highest, and the rate of recovery is maximum.
Embodiment
Embodiment one:
The present invention is used for the treatment process of nitrobenzene extraction aniline, and its operation steps is as follows:
A, extraction: oil of mirbane is added in the aniline solution in extraction plant, solvent ratio is 1.27, and control temperature is 20 DEG C, and stirs 2min clockwise;
B, leave standstill: by steps A extract solution left standstill 36min;
C, separation: by the mode separating and extracting phase of leakage, i.e. the mixture of aniline and oil of mirbane;
Repeat A, B, C: add new oil of mirbane again in the extracting phase after separation, solvent ratio is 1.27, and control temperature is 20 DEG C, and stirs 2min clockwise; By the solution left standstill 36min that steps A extracts; By the mode of leakage by the solution separating of layering;
Again repeat A, B, C: add new oil of mirbane again in the extracting phase after separation, solvent ratio is 1.27, and control temperature is 20 DEG C, and stirs 2min clockwise; By the solution left standstill 36min that steps A extracts; By the mode of leakage by the solution separating of layering;
D, extraction: merge the extraction phase obtained for three times, hydrogenation generates aniline; The extracting phase that third time obtains is saturated nitrobenzene solution;
E, heating nitrobenzene solution to 58 DEG C, stir 2min simultaneously, utilize scroll vacuum pump to be extracted by suspended substance, the scroll vacuum pump afterbody after extraction adds storing device, adds gac in storing device, by the suspended substance absorption extracted.
Embodiment two:
Be with the difference of embodiment one, be heated to 50 DEG C in step e, the temperature of extraction is 25 DEG C, and the time that step B leaves standstill is 42min.
Embodiment three:
Be with the difference of embodiment one, be heated to 60 DEG C in step e, the temperature of extraction is 23 DEG C, and the time that step B leaves standstill is 38min.
Embodiment four:
Be with the difference of embodiment one, be heated to 55 DEG C in step e, the temperature of extraction is 22 DEG C, and the time that step B leaves standstill is 40min.
Comparative example one:
Be with the difference of embodiment one: omit step e.
Comparative example two:
Be with the difference of embodiment one:
Experiment: omit twice and repeat A, B, step C.
Comparative example three:
Be with the difference of embodiment one:
The solvent ratio of steps A is 1.25, and the temperature of extraction is 18 DEG C, and the time left standstill is 35min.
Experiment one:
The content of the aniline that mensuration embodiment one ~ embodiment four, comparative example one ~ comparative example three obtain.
Embodiment one: aniline 99.6%;
Embodiment two: aniline 91.3%;
Embodiment three: aniline 90.5%;
Embodiment four: aniline 85.1%;
Comparative example one: aniline 98.8%;
Comparative example two: aniline 87.9%;
Comparative example three: aniline 89.5%;
Experiment two:
Measure the suspended substance in nitrobenzene solution in embodiment one ~ embodiment four, comparative example one ~ comparative example three, result is:
Embodiment one ~ embodiment four is without obvious suspended substance, and the suspended substance of comparative example one is more, and comparative example two, comparative example three are many compared with the suspended substance of embodiment one ~ embodiment four, but few compared with the suspended substance of comparative example one.
As can be seen here: the aniline content of the gain of parameter of extraction process of the present invention is high, adds the embodiment of step e of the present invention, greatly reduces the suspended substance in its oil of mirbane.
For a person skilled in the art, under the prerequisite not departing from structure of the present invention, can also make some distortion and improvement, these also should be considered as protection scope of the present invention, and these all can not affect effect of the invention process and practical applicability.

Claims (9)

1. for the treatment process of nitrobenzene extraction aniline, comprise steps A: extraction, B: standing, C: separation, D: extraction step, it is characterized in that: after extraction step, also include step e: the operation of step e is as follows: the nitrobenzene solution after extracting is warming up to 50 ~ 60 DEG C, adopt vacuum suck method to be drawn by the ullage impurity of nitrobenzene solution, process completes.
2. the treatment process for nitrobenzene extraction aniline according to claim 1, is characterized in that: in described step e, and the temperature of p-nitrophenyl solution warms is 58 DEG C.
3. the treatment process for nitrobenzene extraction aniline according to claim 2, is characterized in that: in described step e, stirs while p-nitrophenyl heats up to it.
4. the treatment process for nitrobenzene extraction aniline according to claim 3, is characterized in that: described step e vacuum suck method adopts swirl vacuum absorption method.
5. the treatment process for nitrobenzene extraction aniline according to claim 4, is characterized in that: after the swirl vacuum absorption of described step e, with gac by impurity absorption.
6. the treatment process for nitrobenzene extraction aniline according to claim 5, is characterized in that: in the extraction process of described steps A, solvent ratio is 1.27.
7. the treatment process for nitrobenzene extraction aniline according to claim 6, is characterized in that: the temperature during extraction process of described steps A is between 20 ~ 25 DEG C.
8. the treatment process for nitrobenzene extraction aniline according to claim 7, is characterized in that: the time of repose of described step B is 36 ~ 42min.
9. the treatment process for nitrobenzene extraction aniline according to claim 8, is characterized in that: in triplicate, the extracting phase after first time is separated adds oil of mirbane again for described steps A, B, C, second time repeating step A, B, C; Extracting phase after second time is separated adds oil of mirbane again, and third time repeats A, B, C, mixes the extraction phase after being separated for three times, then operation steps D.
CN201510721849.2A 2015-10-30 2015-10-30 Treatment method for extracting aniline by means of nitrobenzene Pending CN105294451A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110563069A (en) * 2018-06-06 2019-12-13 中国石油化工股份有限公司 Comprehensive utilization method of nitrobenzene tar and aniline wastewater

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6147446A (en) * 1984-08-13 1986-03-07 Mitsui Toatsu Chem Inc Preparation of aniline
CN1600696A (en) * 2004-10-12 2005-03-30 南化集团研究院 Nitrobenzene extraction method for treating aniline wastewater
US20050240058A1 (en) * 2003-07-04 2005-10-27 Nongyue Wang And Guangqiang Shi Process for preparing 4-aminodiphenylamine
DE102006008000A1 (en) * 2006-02-21 2006-11-30 Basf Ag Extraction of an aromatic amine from an aqueous phase trough extraction of the aromatic amine with a corresponding nitroaromatic
CN101759244A (en) * 2008-11-19 2010-06-30 陶伟平 Method for treating wastewater in manufacturing process of aniline through nitrobenzene hydrogenation
CN102421745A (en) * 2009-05-07 2012-04-18 巴斯夫欧洲公司 Method for producing an aromatic amine and device therefor
CN102936079A (en) * 2011-12-30 2013-02-20 滨州学院 Method for removing aniline from industrial high salt-containing aniline wastewater

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6147446A (en) * 1984-08-13 1986-03-07 Mitsui Toatsu Chem Inc Preparation of aniline
US20050240058A1 (en) * 2003-07-04 2005-10-27 Nongyue Wang And Guangqiang Shi Process for preparing 4-aminodiphenylamine
CN1600696A (en) * 2004-10-12 2005-03-30 南化集团研究院 Nitrobenzene extraction method for treating aniline wastewater
DE102006008000A1 (en) * 2006-02-21 2006-11-30 Basf Ag Extraction of an aromatic amine from an aqueous phase trough extraction of the aromatic amine with a corresponding nitroaromatic
CN101759244A (en) * 2008-11-19 2010-06-30 陶伟平 Method for treating wastewater in manufacturing process of aniline through nitrobenzene hydrogenation
CN102421745A (en) * 2009-05-07 2012-04-18 巴斯夫欧洲公司 Method for producing an aromatic amine and device therefor
CN102936079A (en) * 2011-12-30 2013-02-20 滨州学院 Method for removing aniline from industrial high salt-containing aniline wastewater

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
霍艳敏等: "废水中邻氯苯胺的提取", 《化工中间体》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110563069A (en) * 2018-06-06 2019-12-13 中国石油化工股份有限公司 Comprehensive utilization method of nitrobenzene tar and aniline wastewater
CN110563069B (en) * 2018-06-06 2020-12-22 中国石油化工股份有限公司 Comprehensive utilization method of nitrobenzene tar and aniline wastewater

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Application publication date: 20160203