CN105237408A - Method for extracting aniline with nitrobenzene - Google Patents
Method for extracting aniline with nitrobenzene Download PDFInfo
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- CN105237408A CN105237408A CN201510721669.4A CN201510721669A CN105237408A CN 105237408 A CN105237408 A CN 105237408A CN 201510721669 A CN201510721669 A CN 201510721669A CN 105237408 A CN105237408 A CN 105237408A
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Abstract
The invention discloses a method for extracting aniline with nitrobenzene. The operation of the method comprises the following steps: A, extracting is carried out by adding nitrobenzene into an aniline solution in an extraction device, wherein a solvent ratio is 1.20-1.27, and a temperature is controlled at 20-25 DEG C; and stirring is carried out; B, the solution obtained in the step A is allowed to stand for 36-42min; and C, separation is carried out, wherein an extracted phase is separated from a raffinate phase. The invention aims at solving a technical problem of providing a method for extracting aniline with nitrobenzene. With the method, the content of extracted aniline is high.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of extracting process of 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; The aniline content of existing nitrobenzene extraction is generally between 80 ~ 90, and the content of extraction is lower.
Summary of the invention
The technical problem to be solved in the present invention is to provide the extracting process of the high nitrobenzene extraction aniline of a kind of aniline content of extraction.
In order to solve the problems of the technologies described above, the invention provides following technical scheme: the extracting process of nitrobenzene extraction aniline: its working method is, A, extraction: added by oil of mirbane in the aniline solution in extraction plant, solvent ratio is 1.20 ~ 1.27, control temperature is 20 ~ 25 DEG C, stirs;
B, leave standstill: by the solution left standstill 36 ~ 42min of steps A;
C, separation: extraction phase is separated with extracting phase.
Adopt the extracting process of the nitrobenzene extraction aniline of technical solution of the present invention, issue after examination and approval existing factually, when solvent ratio is 1.20 ~ 1.27, the content of aniline is high; When temperature is 20 ~ 25 DEG C, leave standstill 36 ~ 42min, the aniline content obtained after extraction is the highest.
The invention has the beneficial effects as follows: compared with the mode of existing extraction parameters, the aniline content of extraction is high.
Further, the temperature during extraction process of described steps A is between 22 DEG C.
Further, the time of repose of described step B is 38min.
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 mixes the extraction phase after being separated for three times after repeating A, B, C.
Further, in the extraction process of described steps A, solvent ratio is 1.27.
Further, also include step e after described extraction step: 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.Oil of mirbane after extraction, due to containing suspended substance, in the process of producing, blocks grid distributor usually, 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, therefore, contriver adds after extraction and is warming up to 50 ~ 60 DEG C, and after suspended substance is vaporized, suspended substance removes by recycling vacuum suck, verify reality factually, the suspended impurity of in oil of mirbane 90% can be removed.
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 (6)
1. the extracting process of nitrobenzene extraction aniline, is characterized in that: its working method is,
A, extraction: oil of mirbane is added in the aniline solution in extraction plant, solvent ratio is 1.20 ~ 1.27, and control temperature is 20 ~ 25 DEG C, stirs;
B, leave standstill: by the solution left standstill 36 ~ 42min of steps A;
C, separation: extraction phase is separated with extracting phase.
2. the extracting process of nitrobenzene extraction aniline according to claim 1, is characterized in that: the temperature during extraction process of described steps A is between 22 DEG C.
3. the extracting process of nitrobenzene extraction aniline according to claim 2, is characterized in that: the time of repose of described step B is 38min.
4. the extracting process of nitrobenzene extraction aniline according to claim 3, 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 mixes the extraction phase after being separated for three times after repeating A, B, C.
5. the extracting process of nitrobenzene extraction aniline according to claim 4, is characterized in that: in the extraction process of described steps A, solvent ratio is 1.27.
6. the extracting process of nitrobenzene extraction aniline according to claim 5, it is characterized in that: after described 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510721669.4A CN105237408A (en) | 2015-10-30 | 2015-10-30 | Method for extracting aniline with nitrobenzene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510721669.4A CN105237408A (en) | 2015-10-30 | 2015-10-30 | Method for extracting aniline with nitrobenzene |
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| CN105237408A true CN105237408A (en) | 2016-01-13 |
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Citations (7)
| 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 |
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2015
- 2015-10-30 CN CN201510721669.4A patent/CN105237408A/en active Pending
Patent Citations (7)
| 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)
| Title |
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| 霍艳敏等: "废水中邻氯苯胺的提取", 《化工中间体》 * |
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Application publication date: 20160113 |
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