CN102675126A - Production method of o-nitro parachloroaniline - Google Patents
Production method of o-nitro parachloroaniline Download PDFInfo
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- CN102675126A CN102675126A CN2012101636547A CN201210163654A CN102675126A CN 102675126 A CN102675126 A CN 102675126A CN 2012101636547 A CN2012101636547 A CN 2012101636547A CN 201210163654 A CN201210163654 A CN 201210163654A CN 102675126 A CN102675126 A CN 102675126A
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- nitro
- parachloroaniline
- ortho
- dichloronitrobenzene
- ammoniacal liquor
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Abstract
The invention discloses a production method of o-nitro parachloroaniline, comprising the following steps of: mixing 2, 5-dichloronitrobenzene and ammonia water; generating o-nitro parachloroaniline and by-product ammonium chloride solution at a certain temperature and pressure; and using slaked lime to treat ammonium chloride to obtain ammonia gas which can be utilized repeatedly. The o-nitro parachloroaniline obtained by the method disclosed by the invention is environment-friendly and does not emit stench.
Description
Technical field
The present invention relates to a kind of working method of ortho-nitro-parachloroaniline.
Background technology
Ortho-nitro-parachloroaniline, product category: midbody/dyestuff intermediate.Molecular weight: 172.5691; EC NO:201-925-4; Molecular formula: C6H5ClN2O2; InChI:InChI=1/C6H5ClN2O2/c7-4-1-2-5 (8) 6 (3-4) 9 (10) 11/h1-3H, 8H2, outward appearance: safran to orange crystalline powder fusing point: >=115 ℃ of amino values (dry product): >=99% purposes: important dyestuff intermediate.Another name: 4-chloro-2-N-methyl-p-nitroaniline; Red bass 3GL; Red basic 3GL; Ortho-nitro-parachloroaniline; To the chlorine o-Nitraniline; P-chloro-0-N-methyl-p-nitroaniline; 1-amino-4-chloro-2-oil of mirbane; 2-amino-5-chloronitrobenzene.
In recent years chemical industry has obtained swift and violent development in China; Become one of riverine, main column support type industry in region following the line of the sea; But the technological reaction that chemical industry is complicated; Produced a large amount of offensive, responsive to people repugnant substances, the problem that disturbs residents of odor pollution recently is more and more outstanding, has become chemical industry to be badly in need of one of environmental protection difficult problem that solves.
Summary of the invention
Main task of the present invention is to provide a kind of working method of ortho-nitro-parachloroaniline.Specifically be a kind of employing aminating reaction, reduce a kind of working method that stench forms.
In order to solve above technical problem, the working method of a kind of ortho-nitro-parachloroaniline of the present invention is characterized in that: with 2, the 5-dichloronitrobenzene mixes with ammoniacal liquor, under certain temperature and pressure condition, generates ortho-nitro-parachloroaniline; And through utilizing white lime to handle ammonium chloride, make ammonia, recycling; Reaction equation
Further, said 2,5-dichloronitrobenzene and ammoniacal liquor hybrid reaction step are: with 2; The 5-dichloronitrobenzene is warmed up to 120 ℃ with after ammoniacal liquor mixes in half a hour, the control temperature rise rate is 1.5 ℃/minute; When temperature reaches 130 ℃; The steam off valve is opened cooling water valve simultaneously, and the control temperature rise rate is 0.5 ℃/minute.When the still temperature reached 170 ℃ in about one and a half hours, step of reaction was accomplished in insulation in three and a half hours under 170 ℃ of conditions.
Further: said 2,5-dichloronitrobenzene: ammoniacal liquor: the mass ratio of white lime is: 5:1:1.
Further: said 2,5-dichloronitrobenzene mass concentration is 99.5%.
Further: said ammoniacal liquor mass concentration is 30%.
The invention has the advantages that: adopt this technology to make ortho-nitro-parachloroaniline, have environment amenable advantage, ordorless flavor distributes.
Embodiment
Embodiment
The norm quota of consumption (to produce ortho-nitro-parachloroaniline per ton) 2,5-dichloronitrobenzene 1000kg, ammoniacal liquor 2000kg, white lime 200kg.
This reaction divides three phases:
A, step of reaction
2,5-dichloronitrobenzene of liquid state is squeezed in the reaction kettle through charging pump, then ammoniacal liquor is put into reaction kettle from header tank.
After starting stirring, startup reaction control system (TPRC001) is set in half a hour and is warmed up to 120 ℃, and the control temperature rise rate is 1.5 ℃/minute, and when temperature reached 130 ℃, the steam off valve was opened cooling water valve simultaneously, and the control temperature rise rate is 0.5 ℃/minute.When the still temperature reached 170 ℃ in about one and a half hours, step of reaction was accomplished in insulation in three and a half hours under 170 ℃ of conditions.
B, venting stage:
Reaction ends and gets into the step-down Bleed-Air Control System, and the rate of pressure rise basically of control venting variable valve is 0.01MPa/ minute, and finally keeping the vapor-liquid separation pressure tower is 0.3MPa, keeps variable valve 0.3MPa all to open up to the venting valve, puts clean ammonia vapor; Presetting ammonia stripping column overhead pressure is 0.02MPa, and ammonia regenerating column tower top pressure is preset to be changed to-0.08MPa, when reaction kettle pressure is lower than 0.00MPa, represents the venting stage to accomplish, and all by-pass valve controls are closed in termination routine control.
C, blowing stage
When reaction kettle pressure is lower than 0MPa, when being lower than 85 ℃, temperature gets into the blowing stage, and open the pressurized air valve and slowly make the still internal pressure reach 0.3MPa, in the segregation still, add 1m in advance
30 ℃ low temperature clear water; Then open baiting valve and put feed liquid only, utilize interchanger to carry out conventional material decrease temperature crystalline, material put to strainer filter when the liquid temperature is lower than 40 ℃; Remove large granular materials; Centrifugal crystal washs with clear water, and mother liquor gets into collecting tank, wet finished product packing or carry out drying.
Claims (5)
1. the working method of an ortho-nitro-parachloroaniline, it is characterized in that: with 2, the 5-dichloronitrobenzene mixes with ammoniacal liquor; Under certain temperature and pressure condition, generate ortho-nitro-parachloroaniline and side product sodium chloride solution, and through utilizing white lime to handle ammonium chloride; Make ammonia, recycling; Reaction equation
。
2. the working method of a kind of ortho-nitro-parachloroaniline according to claim 1 is characterized in that: said 2,5-dichloronitrobenzene and ammoniacal liquor hybrid reaction step are: with 2; The 5-dichloronitrobenzene is warmed up to 120 ℃ with after ammoniacal liquor mixes in half a hour, the control temperature rise rate is 1.5 ℃/minute; When temperature reaches 130 ℃; The steam off valve is opened cooling water valve simultaneously, and the control temperature rise rate is 0.5 ℃/minute.When the still temperature reached 170 ℃ in about one and a half hours, step of reaction was accomplished in insulation in three and a half hours under 170 ℃ of conditions.
3. the working method of a kind of ortho-nitro-parachloroaniline according to claim 1 is characterized in that: said 2,5-dichloronitrobenzene: ammoniacal liquor: the mass ratio of white lime is: 5:1:1.
4. according to the working method of claim 1 or 3 described a kind of ortho-nitro-parachloroanilines, it is characterized in that: said 2,5-dichloronitrobenzene mass concentration is 99.5%.
5. according to the working method of claim 1 or 3 described a kind of ortho-nitro-parachloroanilines, it is characterized in that: said ammoniacal liquor mass concentration is 30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101636547A CN102675126A (en) | 2012-05-24 | 2012-05-24 | Production method of o-nitro parachloroaniline |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101636547A CN102675126A (en) | 2012-05-24 | 2012-05-24 | Production method of o-nitro parachloroaniline |
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| Publication Number | Publication Date |
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| CN102675126A true CN102675126A (en) | 2012-09-19 |
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| CN2012101636547A Pending CN102675126A (en) | 2012-05-24 | 2012-05-24 | Production method of o-nitro parachloroaniline |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435498A (en) * | 2013-08-15 | 2013-12-11 | 江苏隆昌化工有限公司 | Process for synthesizing arene amine through catalyzing and aminolysis of polychlorinated aromatic hydrocarbons by modified Cu-13X molecular sieve |
| CN106008258A (en) * | 2016-06-22 | 2016-10-12 | 江苏隆昌化工有限公司 | Testing method for optimal treatment conditions for 3GL (4-chloro-2-nitroaniline) diazotization solid residues |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693301A (en) * | 2004-05-07 | 2005-11-09 | 杨宝德 | Process for preparing ortho nitrophenylamine |
| WO2011084773A2 (en) * | 2009-12-21 | 2011-07-14 | E. I. Du Pont De Nemours And Company | Process for the synthesis of 1-amino-3-halo-4,6-dinitrobenzene |
| CN102351715A (en) * | 2011-09-05 | 2012-02-15 | 江苏隆昌化工有限公司 | Production process of high-purity o-nitro-p-chloroaniline |
| CN102432033A (en) * | 2011-09-05 | 2012-05-02 | 江苏隆昌化工有限公司 | Mother liquid post treatment process for high-purity nitro parachloroaniline |
-
2012
- 2012-05-24 CN CN2012101636547A patent/CN102675126A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1693301A (en) * | 2004-05-07 | 2005-11-09 | 杨宝德 | Process for preparing ortho nitrophenylamine |
| WO2011084773A2 (en) * | 2009-12-21 | 2011-07-14 | E. I. Du Pont De Nemours And Company | Process for the synthesis of 1-amino-3-halo-4,6-dinitrobenzene |
| CN102351715A (en) * | 2011-09-05 | 2012-02-15 | 江苏隆昌化工有限公司 | Production process of high-purity o-nitro-p-chloroaniline |
| CN102432033A (en) * | 2011-09-05 | 2012-05-02 | 江苏隆昌化工有限公司 | Mother liquid post treatment process for high-purity nitro parachloroaniline |
Non-Patent Citations (2)
| Title |
|---|
| 曹广宏: "3,5-二氯苯胺的合成及其在农药上的应用", 《江苏化工》, vol. 21, no. 2, 31 December 1993 (1993-12-31), pages 6 - 9 * |
| 袁俊秀: "《对硝基氯苯氨解制备对硝基苯胺工艺研究》", 《化学工业与工程技术》, vol. 32, no. 3, 30 June 2011 (2011-06-30), pages 11 - 13 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435498A (en) * | 2013-08-15 | 2013-12-11 | 江苏隆昌化工有限公司 | Process for synthesizing arene amine through catalyzing and aminolysis of polychlorinated aromatic hydrocarbons by modified Cu-13X molecular sieve |
| CN103435498B (en) * | 2013-08-15 | 2015-04-15 | 江苏隆昌化工有限公司 | Process for synthesizing arene amine through catalyzing and aminolysis of polychlorinated aromatic hydrocarbons by modified Cu-13X molecular sieve |
| CN106008258A (en) * | 2016-06-22 | 2016-10-12 | 江苏隆昌化工有限公司 | Testing method for optimal treatment conditions for 3GL (4-chloro-2-nitroaniline) diazotization solid residues |
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Application publication date: 20120919 |