CN102617354B - Refining process of o-nitrophenol - Google Patents
Refining process of o-nitrophenol Download PDFInfo
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- CN102617354B CN102617354B CN201210065388.4A CN201210065388A CN102617354B CN 102617354 B CN102617354 B CN 102617354B CN 201210065388 A CN201210065388 A CN 201210065388A CN 102617354 B CN102617354 B CN 102617354B
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- pot
- water
- squeezed
- nitrophenol
- distillation
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000007670 refining Methods 0.000 title claims abstract description 11
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 title abstract 5
- CFBYEGUGFPZCNF-UHFFFAOYSA-N 2-nitroanisole Chemical compound COC1=CC=CC=C1[N+]([O-])=O CFBYEGUGFPZCNF-UHFFFAOYSA-N 0.000 claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004821 distillation Methods 0.000 claims abstract description 12
- 238000010521 absorption reaction Methods 0.000 claims abstract description 8
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 15
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 238000003808 methanol extraction Methods 0.000 claims description 3
- 230000020477 pH reduction Effects 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- 230000008929 regeneration Effects 0.000 abstract description 2
- 238000011069 regeneration method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 238000003889 chemical engineering Methods 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 abstract 1
- 239000003610 charcoal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical group [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
Abstract
The invention belongs to the technical field of chemical engineering and particularly relates to a refining process of o-nitrophenol. According to the refining process of the o-nitrophenol, 100kg of o-nitroanisole is excessively recovered from per 10 tons of waste water, and the production cost of the o-nitroanisole is reduced. Active carbon is added for absorption, the purity of the o-nitrophenol is improved, and the original content lower than 95 percent is improved to the content higher than 99 percent. The activated carbon regeneration is carried out, the o-nitroanisole is further extracted, activated carbon can be cyclically utilized, and meanwhile, the recovery rate of the o-nitroanisole is improved. In the original process, the purification can be carried out only through the rectification. According to the refining process provided by the invention, the purity of the o-nitrophenol can be improved through distillation, and energy sources and equipment are saved. The waste water chemical oxygen demand (COD) is reduced by a half through being compared with the results of the original process, impurities are absorbed by the active carbon, the content of the impurities is greatly reduced, and the waste water treatment by resin absorption is favorably realized.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of process for refining of o-NP.
Background technology
The production technique of o-NP, comparatively ripe at present, still,, all there are some defects in various production technique, and for example, while by o-Nitrophenyl methyl ether, producing o-NP, defective workmanship mainly is present in:
1, o-NP content is difficult to surpass 95%.
2, the o-Nitrophenyl methyl ether in removal process is mixture, is difficult to process and recycle.
3, the waste water COD produced is higher, reaches 4000mg/l, and the environment-protective water intractability is larger.
4, this technique needs acid out-distillation operation, and to improve purity, but energy consumption is higher.
Summary of the invention
For problems of the prior art, the present invention aims to provide the process for refining of the o-NP that a kind of cost is lower, product purity is higher.
The technical solution used in the present invention is as follows:
The process for refining of o-NP, is characterized in that, comprises the steps:
1., methyl ether oxidation mother liquor water is squeezed into to storage tank, utilize condenser to carry out circulation temperature lowering, temperature drops to below 30 ℃;
2., standing 1 hour, water is at the middle and upper levels squeezed into to Decolouring pot; Lower floor's material can be returned oxidation system, reclaims o-Nitrophenyl methyl ether;
3., in Decolouring pot, add 1% powdered carbon, be warming up to 60 ℃, decolour 1 hour;
4., decolour qualified after, destainer carries out press filtration by pressure filter, the filter residue gac goes out o-Nitrophenyl methyl ether with methanol extraction, then recovered carbon;
5., filtrate is squeezed into to the acidifying pot, drip the vitriol oil, control the pH value and reach 3, stopping acidification; Cool to 25 ℃ after acidifying, o-NP is fully separated out;
6., under whipped state, acidizing fluid is squeezed into and is taken out hopper, take out the hopper material and proceed to the material pot, lower layer of water enters the pot that draws water, draw water the pot water enter the resin absorption system;
7., distillation material pot material, distillation temperature is no more than 140 ℃, distillation pressure-0.25～0MPa.
Compared with prior art, the process for refining of o-NP of the present invention, beneficial effect shows:
1, every 10 tons of waste water reclaim the 100kg o-Nitrophenyl methyl ether more, reduce adjacent amino phenylate production cost.
2, add charcoal absorption, improve the purity of o-NP, improve more than 99% by the content that originally was less than 95%.
3, regeneration of activated carbon, further extract adjacent nitre methyl-phenoxide, and the gac reusable edible simultaneously, improves the o-Nitrophenyl methyl ether rate of recovery.
4, original technique must could be purified by rectifying, now by distillation, just can improve the purity of o-NP, save energy and equipment.
5, the result of the more original technique of waste water COD reduces half, and impurity is by charcoal absorption, and foreign matter content greatly reduces, and is conducive to resin absorption and processes waste water.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
The process for refining of o-NP, comprise the steps:
1., methyl ether oxidizing reaction mother liquid coming is squeezed into to storage tank, utilize condenser to carry out circulation temperature lowering, temperature drops to below 30 ℃;
2., standing 1 hour (layering is comparatively obvious), in, upper water squeezes into Decolouring pot; Lower floor's material can be returned oxidation system, reclaims o-Nitrophenyl methyl ether;
3., in Decolouring pot, add 1% powdered carbon, be warming up to 60 ℃, decolour 1 hour;
4., decolour qualified after indexs such as (detect) colourities, destainer carries out press filtration by pressure filter, the filter residue gac goes out o-Nitrophenyl methyl ether with methanol extraction, gac reclaims, recycling;
5., filtrate is squeezed into to the acidifying pot, drip the vitriol oil, control the pH value and reach 3, stopping acidification; Cool to 25 ℃ after acidifying, o-NP is fully separated out;
6., under whipped state, acidizing fluid is squeezed into and is taken out hopper, take out the hopper material and proceed to the material pot, lower layer of water enters the pot that draws water, draw water the pot water enter the resin absorption system;
7., distillation material pot material, distillation temperature is no more than 140 ℃, distillation pressure-0.25～0MPa.
Above content is only to operating procedure example of the present invention and explanation; affiliated those skilled in the art make various modifications to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the design of invention; perhaps surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Claims (1)
1. the process for refining of o-NP, is characterized in that, comprises the steps:
1., methyl ether oxidation mother liquor water is squeezed into to storage tank, utilize condenser to carry out circulation temperature lowering, temperature drops to below 30 ℃;
2., standing 1 hour, water is at the middle and upper levels squeezed into to Decolouring pot; Lower floor's material is returned oxidation system, reclaims o-Nitrophenyl methyl ether;
3., in Decolouring pot, add 1% powdered carbon, be warming up to 60 ℃, decolour 1 hour;
4., decolour qualified after, destainer carries out press filtration by pressure filter, the filter residue gac goes out o-Nitrophenyl methyl ether with methanol extraction, then recovered carbon;
5., filtrate is squeezed into to the acidifying pot, drip the vitriol oil, control the pH value and reach 3, stopping acidification; Cool to 25 ℃ after acidifying, o-NP is fully separated out;
6., under whipped state, acidizing fluid is squeezed into and is taken out hopper, take out the hopper material and proceed to the material pot, lower layer of water enters the pot that draws water, draw water the pot water enter the resin absorption system;
7., distillation material pot material, distillation temperature is no more than 140 ℃, distillation pressure-0.25～0MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210065388.4A CN102617354B (en) | 2012-03-07 | 2012-03-07 | Refining process of o-nitrophenol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210065388.4A CN102617354B (en) | 2012-03-07 | 2012-03-07 | Refining process of o-nitrophenol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102617354A CN102617354A (en) | 2012-08-01 |
| CN102617354B true CN102617354B (en) | 2014-01-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210065388.4A Active CN102617354B (en) | 2012-03-07 | 2012-03-07 | Refining process of o-nitrophenol |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107512810B (en) * | 2017-07-13 | 2021-04-16 | 安徽东至广信农化有限公司 | Method for treating wastewater generated after nitrochlorobenzene production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4925565A (en) * | 1988-09-12 | 1990-05-15 | First Chemical Corporation | Process for extracting and disposing of nitrophenolic by-products |
| US4986917A (en) * | 1989-07-10 | 1991-01-22 | First Chemical Corporation | Selective recovery of a nitrophenolic by-product from nitration waste water by extraction |
| CN1562790A (en) * | 2004-04-06 | 2005-01-12 | 南京大学 | Method for treating wastewater generated from fabricating nitrophenol as well as for reclaiming and using resources |
| CN101481311A (en) * | 2008-12-12 | 2009-07-15 | 天津市德凯化工有限公司 | Preparation of 4-chloro-2-nitrophenol |
-
2012
- 2012-03-07 CN CN201210065388.4A patent/CN102617354B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4925565A (en) * | 1988-09-12 | 1990-05-15 | First Chemical Corporation | Process for extracting and disposing of nitrophenolic by-products |
| US4986917A (en) * | 1989-07-10 | 1991-01-22 | First Chemical Corporation | Selective recovery of a nitrophenolic by-product from nitration waste water by extraction |
| CN1562790A (en) * | 2004-04-06 | 2005-01-12 | 南京大学 | Method for treating wastewater generated from fabricating nitrophenol as well as for reclaiming and using resources |
| CN101481311A (en) * | 2008-12-12 | 2009-07-15 | 天津市德凯化工有限公司 | Preparation of 4-chloro-2-nitrophenol |
Non-Patent Citations (6)
| Title |
|---|
| A facile demethylation of ortho substituted aryl methyl ethers promoted by AlCl3;Zhen-Ting Du等;《Journal of Chemical Research》;20100430;第34卷(第4期);第222-227页 * |
| Angela M. Bernard等.Dealkylation of Activated Alkyl Aryl Ethers Using Lithium Chloride in Dimethylformamide.《Synthesis》.1989,(第4期),第287-289页. |
| Dealkylation of Activated Alkyl Aryl Ethers Using Lithium Chloride in Dimethylformamide;Angela M. Bernard等;《Synthesis》;19890430(第4期);第287-289页 * |
| Zhen-Ting Du等.A facile demethylation of ortho substituted aryl methyl ethers promoted by AlCl3.《Journal of Chemical Research》.2010,第34卷(第4期),第222-227页. |
| 姜华等.树脂吸附法处理邻硝基苯酚废水的研究.《离子交换与吸附》.2000,第16卷(第6期),第540-546页. |
| 树脂吸附法处理邻硝基苯酚废水的研究;姜华等;《离子交换与吸附》;20001231;第16卷(第6期);第540-546页 * |
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| CN102617354A (en) | 2012-08-01 |
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Address after: Hekou Economic Development Zone Industrial Park in Anhui city of Bengbu province Wuhe County 233300 Mo Applicant after: Anhui Haihua Chemical Technology Co., Ltd. Address before: Hekou Economic Development Zone Industrial Park in Anhui city of Bengbu province Wuhe County 233300 Mo Applicant before: Anhui Haihua Chemical Co., Ltd. |
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Denomination of invention: Refining process of o-nitrophenol Effective date of registration: 20150508 Granted publication date: 20140101 Pledgee: Bengbu financing guarantee Group Co., Ltd. Pledgor: Anhui Haihua Chemical Technology Co., Ltd. Registration number: 2015990000328 |
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Date of cancellation: 20160816 Granted publication date: 20140101 Pledgee: Bengbu financing guarantee Group Co., Ltd. Pledgor: Anhui Haihua Chemical Technology Co., Ltd. Registration number: 2015990000328 |
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Address after: 233300 No.36 Kaiyuan Avenue, mohekou Industrial Park, Huaishang District, Bengbu City, Anhui Province Patentee after: Anhui Haihua Technology Co., Ltd. Address before: Hekou Economic Development Zone Industrial Park in Anhui city of Bengbu province Wuhe County 233300 Mo Patentee before: Anhui Haihua Chemical Technology Co., Ltd. |
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Address after: 233000 No.36, Kaiyuan Avenue, mohekou Industrial Park, Huaishang District, Bengbu City, Anhui Province Patentee after: Anhui Haihua Technology Group Co.,Ltd. Address before: 233300 No.36, Kaiyuan Avenue, mohekou Industrial Park, Huaishang District, Bengbu City, Anhui Province Patentee before: Anhui Haihua Technology Co.,Ltd. |