CN106276817A - A kind of method of organics removal from nitrating wasting acid - Google Patents
A kind of method of organics removal from nitrating wasting acid Download PDFInfo
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- CN106276817A CN106276817A CN201510307691.4A CN201510307691A CN106276817A CN 106276817 A CN106276817 A CN 106276817A CN 201510307691 A CN201510307691 A CN 201510307691A CN 106276817 A CN106276817 A CN 106276817A
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- acid
- nitrating wasting
- nitrating
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- wasting acid
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Abstract
Nitration reaction is typically to react Organic substance under conditions of stirring with nitration mixture, again by isolated nitration product and nitrating wasting acid, containing the Organic substance of trace in nitrating wasting acid after separation, the present invention introduces a kind of organic method in removal nitrating wasting acid.The present invention uses extraction process, removes the Organic substance in spent acid and purifies utilization, then being used by spent acid.The present invention passes through extraction process, by the organic matter removal in nitrating wasting acid, is on the one hand conducive to spent acid to process；On the other hand can effectively reduce spent acid COD, reach the purpose of environmental protection low-carbon (LC).
Description
Technical field
The present invention relates to organic chemistry filed, introduce a kind of method of organics removal from nitrating wasting acid, the method extracts after adding organic solvent mix homogeneously in nitrating wasting acid, after standing, with spent acid, organic facies is separated reality, it is achieved remove organic purpose in nitrating wasting acid.By the process of the inventive method, the active princlple in nitrating wasting acid can be made full use of, the content of organics in the most basic spent acid.
Background technology
Polyparaphenylene's benzo dioxazole (hereinafter referred PBO) is a kind of high-performance fiber, have been used for the field such as military affairs, space flight at present, 4,6-diamino resorcin (hereinafter referred DAR) hydrochlorate is one of important monomer of synthetic fibers PBO, DAR is with 1,2,3-trichloro-benzenes are raw material, through nitrification, hydrolyze, be hydrogenated with and the operation such as recrystallization is prepared from.1，2，3-trichlorobenzene obtains 1 after nitration reaction, 2,3-tri-chloro-4,6-dinitro benzene, producing substantial amounts of nitrating wasting acid simultaneously, contain the Organic substance of 0.10-0.25% (weight) in produced nitrating wasting acid, this organic existence affects the process of nitrating wasting acid.This nitrating wasting acid is only taked suitable method carry out processing, utilizing, this technique just can be made to possess industrialized feasibility.
Summary of the invention
The technical problem to be solved in the present invention: at present, the processing method of nitrating wasting acid mainly has: the reduction concentration discharge that adds water, neutralizes, directly utilize and concentration and recovery.Owing to the di-nitrated reaction of 1，2，3-trichlorobenzene is high to original acid concentration, acid ratio requirement, after reaction, sulfuric acid concentration is still up to 86 ~ 88%, uses concentration method uneconomical, and feasibility is the highest；Because spent acid contains Organic substance, neutralize and directly utilize two kinds of processing methods the most infeasible.
The present invention uses extraction process, removes the Organic substance in spent acid and purifies utilization, then being used by spent acid.Its technology technical scheme: the method for organics removal from nitrating wasting acid, removes Organic substance in nitrating wasting acid by extraction process, it is characterised in that comprise the following steps:
a)
In nitrating wasting acid, add extractant, vibrate or stir to two-phase mixtures uniform；
b)
Moving in separatory funnel by the mixed liquor of nitrating wasting acid and extractant, stratification, upper strata is extraction organic facies, and lower floor is nitrating wasting acid；
c)
Lower floor's spent acid is repeated (a) and (b) operate twice.
Usually, in the inventive method, nitrating wasting acid derives from 1，2，3-trichlorobenzene nitration processes.
In described nitrating wasting acid, sulfuric acid concentration is 85%～88%(weight), concentration of nitric acid is 1%～2%(weight), organic concentration 0.002%～0.2%(weight).
Organic components in described nitrating wasting acid is 1,2,3-tri-chloro-4,6-dinitro benzene and 2,4-bis-chloro-5-Nitrobenzol, and its mass ratio is 4:1～4.5:1.
In described method, the extractant of employing is 1,2-dichloroethanes；
In described method, it is the 10% of spent acid volume that single extractant adds volume.
Beneficial effects of the present invention: compared with prior art, present invention have the advantage that the present invention passes through extraction process, by the organic matter removal in nitrating wasting acid, is on the one hand conducive to spent acid to process；On the other hand can effectively reduce spent acid COD, reach the purpose of environmental protection low-carbon (LC).
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment
1
On the four-hole bottle device of band stirring, 100 grams of 0.11%(mass percents Han Organic substance are added in four-hole bottle, nitrating wasting acid the most together) and 10 grams of dichloroethanes, stir 10 minutes, mixed liquor is transferred in separatory funnel, stand 30 minutes, separate organic facies and acid phase, analyzing biphase middle content of organics respectively, in organic facies, content of organics is 1.04%, and after extraction, in spent acid, the content of organic facies is 0.0122%.
Embodiment
2
Device is with embodiment 1.Adding content of organics in four-hole bottle is 0.0122% nitrification extraction spent acid, and adds 10 grams of dichloroethanes, ibid operates, analyzes biphase middle content of organics respectively, and in organic facies, content of organics is 0.065%, and after extraction, the content of Organic Materials of Spent acid is 0.0022%.
Embodiment
3
Device is with embodiment 1.Adding the extraction spent acid in embodiment 1 in four-hole bottle, and add 10 grams of dichloroethanes, ibid operate, analyze biphase middle content of organics respectively, in organic facies, content of organics is 0.0155%, and after extraction, Organic Materials of Spent acid content does not detects.
Above example shows: can effectively remove organic matter component in nitrating wasting acid by extraction process.
Claims (6)
1. a method for organics removal from nitrating wasting acid, removes Organic substance in nitrating wasting acid by extraction process, it is characterised in that comprise the following steps:
A) in nitrating wasting acid, add extractant, vibrate or stir to two-phase mixtures uniform；
B) moving in separatory funnel by the mixed liquor of nitrating wasting acid and extractant, stratification, upper strata is extraction organic facies, and lower floor is nitrating wasting acid；
C) lower floor's spent acid is repeated (a) and (b) to operate twice.
Method the most according to claim 1, it is characterised in that nitrating wasting acid derives from 1，2，3-trichlorobenzene nitration processes.
Method the most according to claim 1 and 2, it is characterised in that in nitrating wasting acid, sulfuric acid concentration is 85%～88%(weight), concentration of nitric acid is 1%～2%(weight), organic concentration 0.002%～0.2%(weight).
Method the most according to claim 1 and 2, it is characterised in that the organic components in nitrating wasting acid is 1,2,3-tri-chloro-4,6-dinitro benzene and 2,4-bis-chloro-5-Nitrobenzol, its mass ratio is 4:1～4.5:1.
Method the most according to claim 1, it is characterised in that extractant used is 1,2-dichloroethanes.
Method the most according to claim 1 or 5, it is characterised in that it is the 10% of spent acid volume that single extractant adds volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510307691.4A CN106276817A (en) | 2015-06-08 | 2015-06-08 | A kind of method of organics removal from nitrating wasting acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510307691.4A CN106276817A (en) | 2015-06-08 | 2015-06-08 | A kind of method of organics removal from nitrating wasting acid |
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| CN106276817A true CN106276817A (en) | 2017-01-04 |
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| CN201510307691.4A Pending CN106276817A (en) | 2015-06-08 | 2015-06-08 | A kind of method of organics removal from nitrating wasting acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156605A (en) * | 2019-05-05 | 2019-08-23 | 南京师范大学 | A kind of method of resource for the spent acid by-product that ethylbenzene nitration reaction generates |
| CN111559737A (en) * | 2020-05-27 | 2020-08-21 | 河南洛染股份有限公司 | Method for continuously extracting nitration waste acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234233A (en) * | 2010-04-20 | 2011-11-09 | 安徽八一化工股份有限公司 | Method for extracting organic matters from waste acid during nitrochlorobenzene production |
| CN102836570A (en) * | 2012-09-19 | 2012-12-26 | 辽宁庆阳特种化工有限公司 | Extracting and separating method and device for waste acid generated in production procedure of m-dinitrobenzene |
| CN104045563A (en) * | 2014-06-03 | 2014-09-17 | 安徽华润涂料有限公司 | Production method of highly pure 2,4-dinitrochlorobenzene |
-
2015
- 2015-06-08 CN CN201510307691.4A patent/CN106276817A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234233A (en) * | 2010-04-20 | 2011-11-09 | 安徽八一化工股份有限公司 | Method for extracting organic matters from waste acid during nitrochlorobenzene production |
| CN102836570A (en) * | 2012-09-19 | 2012-12-26 | 辽宁庆阳特种化工有限公司 | Extracting and separating method and device for waste acid generated in production procedure of m-dinitrobenzene |
| CN104045563A (en) * | 2014-06-03 | 2014-09-17 | 安徽华润涂料有限公司 | Production method of highly pure 2,4-dinitrochlorobenzene |
Non-Patent Citations (1)
| Title |
|---|
| 张德义: "《石油化工危险化学品实用手册》", 31 January 2006, 中国石化出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110156605A (en) * | 2019-05-05 | 2019-08-23 | 南京师范大学 | A kind of method of resource for the spent acid by-product that ethylbenzene nitration reaction generates |
| CN111559737A (en) * | 2020-05-27 | 2020-08-21 | 河南洛染股份有限公司 | Method for continuously extracting nitration waste acid |
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Application publication date: 20170104 |