CN112679362A - Extraction system and process for preparing 2, 4-dinitrochlorobenzene to generate acid phase - Google Patents
Extraction system and process for preparing 2, 4-dinitrochlorobenzene to generate acid phase Download PDFInfo
- Publication number
- CN112679362A CN112679362A CN202011622568.9A CN202011622568A CN112679362A CN 112679362 A CN112679362 A CN 112679362A CN 202011622568 A CN202011622568 A CN 202011622568A CN 112679362 A CN112679362 A CN 112679362A
- Authority
- CN
- China
- Prior art keywords
- extraction
- acid
- chlorobenzene
- stage countercurrent
- phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000605 extraction Methods 0.000 title claims abstract description 158
- 239000002253 acid Substances 0.000 title claims abstract description 149
- VYZAHLCBVHPDDF-UHFFFAOYSA-N Dinitrochlorobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C([N+]([O-])=O)=C1 VYZAHLCBVHPDDF-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title description 5
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims abstract description 133
- 239000012071 phase Substances 0.000 claims abstract description 86
- 239000002699 waste material Substances 0.000 claims abstract description 52
- 239000012074 organic phase Substances 0.000 claims abstract description 41
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000006396 nitration reaction Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims description 8
- 230000035800 maturation Effects 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 25
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 25
- 238000000034 method Methods 0.000 abstract description 7
- 238000003860 storage Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000005191 phase separation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 description 2
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 1
- LXQOQPGNCGEELI-UHFFFAOYSA-N 2,4-dinitroaniline Chemical compound NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O LXQOQPGNCGEELI-UHFFFAOYSA-N 0.000 description 1
- UFBJCMHMOXMLKC-UHFFFAOYSA-N 2,4-dinitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O UFBJCMHMOXMLKC-UHFFFAOYSA-N 0.000 description 1
- BPPMIQPXQVIZNJ-UHFFFAOYSA-N 2-chloro-1,3-dinitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC([N+]([O-])=O)=C1Cl BPPMIQPXQVIZNJ-UHFFFAOYSA-N 0.000 description 1
- LHRIICYSGQGXSX-UHFFFAOYSA-N 2-chloro-4,6-dinitroaniline Chemical compound NC1=C(Cl)C=C([N+]([O-])=O)C=C1[N+]([O-])=O LHRIICYSGQGXSX-UHFFFAOYSA-N 0.000 description 1
- ZWUBBMDHSZDNTA-UHFFFAOYSA-N 4-Chloro-meta-phenylenediamine Chemical compound NC1=CC=C(Cl)C(N)=C1 ZWUBBMDHSZDNTA-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- XIWMTQIUUWJNRP-UHFFFAOYSA-N amidol Chemical compound NC1=CC=C(O)C(N)=C1 XIWMTQIUUWJNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940117389 dichlorobenzene Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an extraction system and an extraction process for producing an acid phase from 2, 4-dinitrochlorobenzene, wherein an organic phase inlet of a three-stage countercurrent supergravity extraction device and an organic phase inlet of a curing supergravity extraction reactor are both connected with a chlorobenzene source, a waste acid outlet of the three-stage countercurrent supergravity extraction device is connected with a waste acid inlet of the curing supergravity extraction reactor, and an acid phase inlet of the three-stage countercurrent supergravity extraction device is connected with the acid phase source. The process comprises the following steps: introducing an acid phase into the three-stage countercurrent hypergravity extraction device until liquid flows out from a waste acid outlet of the three-stage countercurrent hypergravity extraction device, and introducing chlorobenzene into the three-stage countercurrent hypergravity extraction device to perform three-stage countercurrent extraction and simultaneously perform nitration reaction; and conveying the waste acid subjected to the three-stage countercurrent extraction to an extraction reactor until liquid flows out from a waste acid outlet of the curing hypergravity extraction reactor, and introducing chlorobenzene into the extraction reactor for curing reaction. The invention not only has lower treatment temperature, but also has higher treatment efficiency on nitric acid and organic matters in the acid phase.
Description
Technical Field
The invention relates to a preparation process of 2, 4-dinitrochlorobenzene, in particular to an extraction system and a process for preparing an acid phase generated by the 2, 4-dinitrochlorobenzene.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
2, 4-dinitrochlorobenzene is an important fine chemical intermediate, and is widely applied to the fields of medicines, pesticides, dyes, explosives, chemical auxiliaries and the like, and a plurality of important fine chemical intermediates can be derived at the downstream, wherein the main varieties comprise 2, 4-dinitroaniline, 2, 4-dinitrophenol, 2, 4-diaminochlorobenzene, 2, 4-diaminophenol, 6-chloro-2, 4-dinitroaniline and the like. At present, two traditional processes are mainly used for generating 2, 4-dinitrochlorobenzene, one process is to carry out one-step nitration by taking p-nitrochlorobenzene as a raw material; the other method uses chlorobenzene as raw material to carry out two-step nitration. In any process, the mixed acid is required to be used for nitration reaction in the reaction process, in order to complete the organic reaction of the raw materials, the nitric acid in the mixed acid is required to be excessive, and an acid phase containing the nitric acid is generated after the reaction is finished and through phase separation. The acid phase also contains organic substances such as 2, 4-dinitrochlorobenzene (24DNC), 2, 6-dinitrochlorobenzene (26DNC), and 4-nitrochlorobenzene (4 MNC).
The acid phase generated by the 2, 4-dinitrochlorobenzene is heated and concentrated, and the concentrated waste acid is recycled. Nitric acid is easily decomposed to generate nitrogen oxides by heating, and if waste acid is directly heated and concentrated, pollution is generated due to the existence of nitric acid. Meanwhile, the acid phase also contains partial organic matters, which influence the concentration and the reutilization of the acid phase. Therefore, before the waste acid is concentrated, the nitric acid and organic matters in the waste acid need to be removed. The inventor researches and discovers that the prior reports on the treatment of nitric acid and organic matters in the acid phase generated by 2, 4-dinitrochlorobenzene are less, and the prior treatment process has the problems of high energy consumption, poor treatment effect and the like when treating the nitric acid and the organic matters in the nitrified waste acid.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to provide an extraction system and an extraction process for preparing 2, 4-dinitrochlorobenzene to generate an acid phase, which not only do not need to provide an external heat source and have lower treatment temperature, but also have higher treatment efficiency on nitric acid and organic matters in the acid phase.
In order to achieve the purpose, the technical scheme of the invention is as follows:
on the one hand, the extraction system for producing the acid phase from the 2, 4-dinitrochlorobenzene comprises a three-stage countercurrent hypergravity extraction device, a curing hypergravity extraction reactor, a chlorobenzene source and an acid phase source, wherein an organic phase inlet of the three-stage countercurrent hypergravity extraction device and an organic phase inlet of the curing hypergravity extraction reactor are connected with the chlorobenzene source, a waste acid outlet of the three-stage countercurrent hypergravity extraction device is connected with a waste acid inlet of the curing hypergravity extraction reactor, and an acid phase inlet of the three-stage countercurrent hypergravity extraction device is connected with the acid phase source.
On the other hand, the extraction process for preparing the acid phase generated by the 2, 4-dinitrochlorobenzene comprises the steps of providing the extraction system, introducing the acid phase into the three-stage countercurrent super-gravity extraction device until liquid flows out from a waste acid outlet of the three-stage countercurrent super-gravity extraction device, and introducing chlorobenzene into the three-stage countercurrent super-gravity extraction device to perform three-stage countercurrent extraction and nitration reaction;
conveying the waste acid subjected to the three-stage countercurrent extraction to a curing hypergravity extraction reactor until liquid flows out from a waste acid outlet of the curing hypergravity extraction reactor, and introducing chlorobenzene to the curing hypergravity extraction reactor for curing reaction;
wherein the temperature of the nitration reaction and the curing reaction is 60-80 ℃.
Firstly, chlorobenzene is used as an extracting agent, nitration reaction can be carried out at 60-80 ℃, nitric acid in an acid phase is consumed, secondly, the chlorobenzene and the acid phase can be mixed more uniformly by adopting a three-stage countercurrent extraction mode, and the chlorobenzene can be completely reacted with the nitric acid at 60-80 ℃, so that energy consumption is reduced. However, it was found through experiments that only chlorobenzene was fed in from the primary extraction, the amount of chlorobenzene increased by 50% and the removal efficiency of nitric acid decreased by 40%. Therefore, the invention adopts fresh chlorobenzene for further curing reaction treatment of waste acid after three-stage countercurrent extraction, and realizes the effects of greatly improving the extraction efficiency of organic matters and greatly reducing the residual quantity of nitric acid on the premise of reducing the dosage of chlorobenzene.
The invention has the beneficial effects that:
1. the invention adopts chlorobenzene as the extractant of the waste acid, which not only reduces the energy consumption of introducing and recovering the exogenous extractant, but also produces nitrochlorobenzene after reacting a small amount of residual nitric acid in the waste acid.
2. According to the invention, a mode of combining three-stage countercurrent extraction with chlorobenzene as an extractant of an acid phase is adopted, and at the temperature of 60-80 ℃, the extraction efficiency is improved, the reaction efficiency of residual nitric acid and chlorobenzene is ensured, the residual amount of nitric acid in waste acid is reduced, the exhaust emission of nitrogen oxides and the concentration difficulty of waste acid are reduced, and thus the energy consumption of acid phase treatment is reduced.
3. The invention adopts the mode that the primary hypergravity curing hypergravity extraction reactor is combined with the chlorobenzene to be used as the three-stage countercurrent extraction outlet waste acid to carry out curing reaction treatment, thereby not only enhancing the mass transfer and heat transfer efficiency, but also improving the nitric acid treatment efficiency and reducing the consumption of the chlorobenzene.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic diagram of an extraction system for producing an acid phase from 2, 4-dinitrochlorobenzene according to an embodiment of the present invention;
the device comprises a three-level countercurrent hypergravity extraction device 1, a curing hypergravity extraction reactor 2, a chlorobenzene storage tank 3, an acid phase storage tank 4, a waste acid receiving tank 5, an organic phase receiving tank 6, a first chlorobenzene metering pump 7, a second chlorobenzene metering pump 8 and an acid phase metering pump 9.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In view of the problems of high energy consumption and poor treatment effect in the prior art of treating nitric acid and organic matters in an acid phase generated by 2, 4-dinitrochlorobenzene, the invention provides an extraction system and a process for preparing the acid phase generated by the 2, 4-dinitrochlorobenzene.
The invention provides an extraction system for producing 2, 4-dinitrochlorobenzene to generate an acid phase, which comprises a three-stage countercurrent hypergravity extraction device, a curing hypergravity extraction reactor, a chlorobenzene source and an acid phase source, wherein an organic phase inlet of the three-stage countercurrent hypergravity extraction device and an organic phase inlet of the curing hypergravity extraction reactor are connected with the chlorobenzene source, a waste acid outlet of the three-stage countercurrent hypergravity extraction device is connected with a waste acid inlet of the curing hypergravity extraction reactor, and the acid phase inlet of the three-stage countercurrent hypergravity extraction device is connected with the acid phase source.
And the pump bodies are respectively arranged on the organic phase inlet of the three-stage countercurrent hypergravity extraction device and the pipeline connecting the organic phase inlet of the curing hypergravity extraction reactor with the chlorobenzene source and are used for conveying chlorobenzene. In some examples of this embodiment, chlorobenzene metering pumps are installed in the pipelines connecting the organic phase inlet of the three-stage countercurrent hypergravity extraction device, the organic phase inlet of the aging hypergravity extraction reactor and the chlorobenzene source. Adopt the measuring pump to carry chlorobenzene, be favorable to controlling the volume of chlorobenzene to produce better effect to acid phase extraction.
The aging reaction of the invention means that a small amount of chlorobenzene is additionally supplemented when the reaction is near the end point, so that the nitric acid in the acid phase can react more thoroughly, and the quality of the extracted acid phase is better.
In some examples of this embodiment, the organic phase outlet of the maturation hypergravity extraction reactor and the organic phase outlet of the three-stage countercurrent hypergravity extraction apparatus are both connected to an organic phase receiving tank. The extracted organic phase not only contains chlorobenzene, but also contains mononitrochlorobenzene and dinitrochlorobenzene, and the organic phase can be further used as a raw material of 2, 4-dinitrochlorobenzene, so that the safety of nitration reaction is ensured, and the total energy consumption of the production of the 2, 4-dinitrochlorobenzene is reduced.
In some embodiments of this embodiment, the maturing hypergravity extraction reactor is a counter-current extractor. And (4) carrying out countercurrent extraction reaction to further ensure the complete removal of nitric acid and organic matters.
In some embodiments of this embodiment, the pipeline connecting the acid phase inlet of the three-stage counter-current hypergravity extraction device to the acid phase source is provided with an acid phase metering pump. The acid phase feeding in the extraction process is controlled to achieve better extraction effect.
Some embodiments of this embodiment include a spent acid receiving tank, the spent acid outlet of the extraction reactor being connected to the spent acid receiving tank.
The invention also provides an extraction process for preparing 2, 4-dinitrochlorobenzene to generate an acid phase, wherein the extraction system is provided, the acid phase is introduced into the three-stage countercurrent super-gravity extraction device until liquid flows out from a waste acid outlet of the three-stage countercurrent super-gravity extraction device, and then chlorobenzene is introduced into the three-stage countercurrent super-gravity extraction device to perform three-stage countercurrent extraction and nitration reaction;
conveying the waste acid subjected to three-stage countercurrent extraction to an extraction reactor until liquid flows out from a waste acid outlet of a curing hypergravity extraction reactor, and introducing chlorobenzene into the extraction reactor for curing reaction;
wherein the temperature of the nitration reaction and the curing reaction is 60-80 ℃.
The method takes chlorobenzene as an extractant of an acid phase, and adopts a three-stage countercurrent extraction mode to perform extraction and nitration reactions at 60-80 ℃ to remove organic matters and nitric acid in the acid phase. The invention greatly improves the removal effect of organic matters and nitric acid in the acid phase through the curing reaction.
In some examples of this embodiment, the temperature of the nitration reaction and the aging reaction is 60 to 65 ℃. Under the condition, the extraction efficiency is better.
In some examples of this embodiment, the ratio of the volumetric flow rate of the acid phase to the volumetric flow rate of chlorobenzene in the three-stage countercurrent extraction is 8:0.70 to 0.80.
In some examples of this embodiment, the sum of the volume flow rate of chlorobenzene in the three-stage countercurrent extraction and the volume flow rate of chlorobenzene in the aging reaction is used as the total volume flow rate of chlorobenzene, and the volume flow rate of chlorobenzene in the aging reaction is 20 to 30% of the total volume flow rate of chlorobenzene.
In some examples of this embodiment, countercurrent extraction is performed simultaneously during the maturation reaction.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Examples
The main equipment is shown in table 1.
TABLE 1 Main Equipment
| Serial number | Device name | Equipment position number | Number/table | |
| 1 | Extraction reactor | M101A/B/C/ |
4 | |
| 2 | Chlorobenzene metering pump | P101A/B | 2 | |
| 3 | Acid phase | P102 | 1 | |
| 4 | Chlorobenzene | V101 | 1 | |
| 5 | Acid phase | V102 | 1 | |
| 6 | Spent acid receiving | V103 | 1 | |
| 7 | Organic phase receiving | V104 | 1 |
Wherein, 4 extraction reactors are all countercurrent extractors, wherein, extraction reactor M101A, extraction reactor M101B, extraction reactor M101C are connected in series in proper order and form tertiary countercurrent hypergravity extraction device, and extraction reactor M101D is as curing hypergravity extraction reactor. The metering pump P101A served as the first chlorobenzene metering pump, the metering pump P101B as the second chlorobenzene metering pump, and the metering pump P102 as the acid phase metering pump.
The extraction system for preparing 2, 4-dinitrochlorobenzene acid-producing phase, which is composed of the main equipment, is shown in fig. 1, wherein an organic phase inlet of a three-stage countercurrent hypergravity extraction device 1 and an organic phase inlet of a curing hypergravity extraction reactor 2 are both connected with a chlorobenzene storage tank 3, a waste acid outlet of the three-stage countercurrent hypergravity extraction device 1 is connected with a waste acid inlet of the curing hypergravity extraction reactor 2, an acid phase inlet of the three-stage countercurrent hypergravity extraction device 1 is connected with an acid phase storage tank 4, a waste acid outlet of the curing hypergravity extraction reactor 2 is connected with a waste acid receiving tank 5, and an organic phase outlet of the curing hypergravity extraction reactor 2 and an organic phase outlet of the three-stage countercurrent hypergravity extraction device 1 are both connected with an organic phase receiving.
A first chlorobenzene metering pump 7 is arranged on a pipeline connecting an organic phase inlet of the curing hypergravity extraction reactor 2 with the chlorobenzene storage tank 3.
And a third dichlorobenzene metering pump 8 is arranged on a pipeline connecting an organic phase inlet of the three-stage countercurrent hypergravity extraction device 1 with the chlorobenzene storage tank 3.
An acid phase metering pump 9 is arranged on a pipeline of an acid phase inlet of the three-stage countercurrent hypergravity extraction device 1 connected with the acid phase storage tank 4.
The main raw materials are shown in table 2.
TABLE 2 Main raw materials
An extraction process for producing an acid phase from 2, 4-dinitrochlorobenzene comprises the following steps:
(1) starting the heat-preservation heating device of the extraction reactor, and controlling the temperature of the equipment to be 60-65 ℃.
(2) And starting an acid phase metering pump, and conveying 8 parts of acid phase with volume flow into the extraction reactor M101A until liquid flows out from a waste acid outlet in the extraction reactor M101C.
(3) When liquid flows out from a waste acid outlet, a third chlorobenzene metering pump is started to convey 0.75 part of chlorobenzene with volume flow rate into an extraction reactor M101C for extraction nitration; chlorobenzene reacts with an acid phase to separate phases, and waste acid 3 and an organic phase 1 are obtained.
(4) And the organic phase 1 enters an extraction reactor M101B to perform extraction nitration reaction with the waste acid 1 to obtain waste acid 2 and an organic phase 2.
(5) And the organic phase 2 enters an extraction reactor M101A to be subjected to extraction nitration reaction with the acid phase therein to be subjected to phase separation to obtain waste acid 1 and an organic phase 3, and the organic phase 3 enters an organic phase receiving tank.
(6) And (4) feeding waste acid 3 obtained after phase splitting of the extraction reaction in the step (3) into an extraction reactor M101D, and starting a first chlorobenzene metering pump to convey 0.25 part of chlorobenzene with volume flow into the waste acid outlet of the extraction reactor M101D for curing reaction when liquid flows out.
(7) After the curing reaction is finished, the extraction phase separator obtains waste acid 4 and an organic phase 4, the waste acid 4 enters a waste acid receiving tank, and the organic phase 4 enters an organic phase receiving tank.
The types and contents of impurities in the acid phase and the waste acid 4 are shown in Table 3.
TABLE 3 types and contents of impurities in acid phase, spent acid 3 and spent acid 4
| Name of material | Nitric acid/% | 24DNC％ | 26DNC％ | 4MNC％ | Organic matter/%) |
| Acid phase | 2 | 6.83 | 0.23 | 0.38 | 7.44 |
| |
0.88 | 1.26 | 0.04 | 0.12 | 1.42 |
| |
0.10 | 0.18 | 0 | 0 | 0.18 |
Wherein the organic substances are 24DNC, 26DNC and 4 MNC.
Table 3 shows that after the extraction reaction phase separation of the embodiment, the organic content of the obtained waste acid is less than or equal to 0.3 percent, and the nitric acid content is less than or equal to 0.2 percent. The removal rate of nitric acid in the acid phase is 95% and the removal rate of organic matters is 97.58%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An extraction system for producing an acid phase from 2, 4-dinitrochlorobenzene is characterized by comprising a three-stage countercurrent hypergravity extraction device, a curing hypergravity extraction reactor, a chlorobenzene source and an acid phase source, wherein an organic phase inlet of the three-stage countercurrent hypergravity extraction device and an organic phase inlet of the curing hypergravity extraction reactor are connected with the chlorobenzene source, a waste acid outlet of the three-stage countercurrent hypergravity extraction device is connected with a waste acid inlet of the curing hypergravity extraction reactor, and the acid phase inlet of the three-stage countercurrent hypergravity extraction device is connected with the acid phase source.
2. The extraction system for producing an acid phase of 2, 4-dinitrochlorobenzene according to claim 1, wherein chlorobenzene metering pumps are installed in the pipelines connecting the organic phase inlet of the three-stage countercurrent super-gravity extraction apparatus, the organic phase inlet of the aging super-gravity extraction reactor and the chlorobenzene source.
3. The extraction system for producing an acid phase of 2, 4-dinitrochlorobenzene according to claim 1, wherein the organic phase outlet of the aging hypergravity extraction reactor and the organic phase outlet of the three-stage countercurrent hypergravity extraction apparatus are connected to an organic phase receiving tank.
4. The extraction system for producing 2, 4-dinitrochlorobenzene acid-producing acid phase according to claim 1, wherein said mature hypergravity extraction reactor is a counter-current extractor.
5. The extraction system for producing an acid phase of 2, 4-dinitrochlorobenzene according to claim 1, wherein the acid phase inlet of the three-stage countercurrent supergravity extraction unit is connected to the pipeline of the acid phase source by an acid phase metering pump.
6. The extraction system for producing 2, 4-dinitrochlorobenzene acid-producing acid phase according to claim 1, comprising a waste acid receiving tank, wherein the waste acid outlet of the extraction reactor is connected to the waste acid receiving tank.
7. An extraction process for preparing 2, 4-dinitrochlorobenzene to generate an acid phase, which is characterized in that an extraction system as claimed in any one of claims 1 to 6 is provided, the acid phase is introduced into a three-stage countercurrent supergravity extraction device until liquid flows out from a waste acid outlet of the three-stage countercurrent supergravity extraction device, and chlorobenzene is introduced into the three-stage countercurrent supergravity extraction device to perform three-stage countercurrent extraction and nitration reaction;
conveying the waste acid subjected to three-stage countercurrent extraction to an extraction reactor until liquid flows out from a waste acid outlet of a curing hypergravity extraction reactor, and introducing chlorobenzene into the extraction reactor for curing reaction;
wherein the temperature of the nitration reaction and the curing reaction is 60-80 ℃.
8. The extraction process for producing an acid phase of 2, 4-dinitrochlorobenzene according to claim 7, wherein the temperature of the nitration reaction and the aging reaction is 60 to 65 ℃.
9. The extraction process for producing an acid phase from 2, 4-dinitrochlorobenzene according to claim 7, wherein in the three-stage countercurrent extraction, the ratio of the volume flow rate of the acid phase to the volume flow rate of chlorobenzene is 8:0.70 to 0.80;
or taking the sum of the volume flow of the chlorobenzene in the three-stage countercurrent extraction and the volume flow of the chlorobenzene in the curing reaction as the total volume flow of the chlorobenzene, wherein the volume flow of the chlorobenzene in the curing reaction is 20-30% of the total volume flow of the chlorobenzene.
10. The extraction process for producing 2, 4-dinitrochlorobenzene acid-producing acid phase according to claim 7, wherein countercurrent extraction is carried out simultaneously during the maturation reaction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011622568.9A CN112679362B (en) | 2020-12-30 | 2020-12-30 | Extraction system and process for preparing 2, 4-dinitrochlorobenzene to generate acid phase |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011622568.9A CN112679362B (en) | 2020-12-30 | 2020-12-30 | Extraction system and process for preparing 2, 4-dinitrochlorobenzene to generate acid phase |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112679362A true CN112679362A (en) | 2021-04-20 |
| CN112679362B CN112679362B (en) | 2022-03-22 |
Family
ID=75453888
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011622568.9A Active CN112679362B (en) | 2020-12-30 | 2020-12-30 | Extraction system and process for preparing 2, 4-dinitrochlorobenzene to generate acid phase |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112679362B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1951802A (en) * | 2005-10-18 | 2007-04-25 | 约瑟夫·迈斯纳两合公司 | Recovery of the nitration acid mixtures from nitration processes |
| CN102070457A (en) * | 2011-02-15 | 2011-05-25 | 河南洛染股份有限公司 | Method for continuously preparing dinitrochlorobenzene |
| 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 |
| WO2015125095A1 (en) * | 2014-02-20 | 2015-08-27 | Reliance Industries Limited | Process for oxidation of alkyl aromatic compound to aromatic carboxylic acid |
| CN107226775A (en) * | 2016-03-24 | 2017-10-03 | 中国石油化工股份有限公司 | The method that the chloro- 3,5- xylenols of 4- are synthesized in continuous stream micro-pipe reactor |
| CN108721942A (en) * | 2018-06-04 | 2018-11-02 | 甘肃泓旭化工科技有限责任公司 | A kind of continuous flow upstream extraction of liquid phase mixture washes reaction process and application |
| 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 |
-
2020
- 2020-12-30 CN CN202011622568.9A patent/CN112679362B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1951802A (en) * | 2005-10-18 | 2007-04-25 | 约瑟夫·迈斯纳两合公司 | Recovery of the nitration acid mixtures from nitration processes |
| CN102070457A (en) * | 2011-02-15 | 2011-05-25 | 河南洛染股份有限公司 | Method for continuously preparing dinitrochlorobenzene |
| WO2015125095A1 (en) * | 2014-02-20 | 2015-08-27 | Reliance Industries Limited | Process for oxidation of alkyl aromatic compound to aromatic carboxylic acid |
| 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 |
| CN107226775A (en) * | 2016-03-24 | 2017-10-03 | 中国石油化工股份有限公司 | The method that the chloro- 3,5- xylenols of 4- are synthesized in continuous stream micro-pipe reactor |
| CN108721942A (en) * | 2018-06-04 | 2018-11-02 | 甘肃泓旭化工科技有限责任公司 | A kind of continuous flow upstream extraction of liquid phase mixture washes reaction process and application |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 张恒: "萃取法处理模拟含硝酸废水的应用基础研究", 《中国优秀硕士学位论文全文数据库（电子期刊）工程科技I辑》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112679362B (en) | 2022-03-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102648152B (en) | Method and plant for reprocessing waste sulphuric acids from nitriding processes | |
| CN102070457B (en) | Method for continuously preparing dinitrochlorobenzene | |
| CN112225642B (en) | Method for preparing resorcinol by micro-channel reaction | |
| CN1119286C (en) | Process for pre-treating waste liquid of p-benzoic acid by complexing and extraction | |
| CN106241758B (en) | Retracting device and technique for acid waste liquid | |
| CN105693560A (en) | Method for preparing energy-efficient H-acid | |
| CN106830601B (en) | Energy-saving sludge wet oxidation device and method | |
| CN112679362B (en) | Extraction system and process for preparing 2, 4-dinitrochlorobenzene to generate acid phase | |
| CN104045563A (en) | Production method of highly pure 2,4-dinitrochlorobenzene | |
| CN108658051A (en) | Recovery method, device and its sulfuric acid of recycling of nitrating wasting acid | |
| CN109320014A (en) | One kind is based on supercritical water oxidation itrogenous organic substance classification processing system and method | |
| CN104003564A (en) | Wet-process rare earth smelting high ammonia-nitrogen wastewater resource utilization method and device | |
| CN109438283B (en) | Synthesis method and device of beta-aminopropionitrile | |
| CN107033005B (en) | Nitration method of aromatic compound | |
| CN112707823B (en) | Green, safe, efficient and continuous 2, 4-dinitrochlorobenzene production system and method | |
| CN104418752B (en) | Method for synthesizing single nitro-o-xylene employing catalytic nitration in micro-reactor | |
| CN105566171B (en) | A kind of device for preparing H acid | |
| CN213446234U (en) | Waste phosphoric acid extraction phosphoric acid treatment system | |
| CN213231531U (en) | Continuous nitric oxide production device | |
| CN115043382A (en) | Method for producing nitrogen dioxide and device for continuously producing nitrogen dioxide | |
| JP5602143B2 (en) | A method for reducing the formation of by-product dinitrobenzene in the production of mononitrobenzene | |
| CN105753744A (en) | Energy-saving H-acid preparation device | |
| CN219363265U (en) | Separation system of fluorine-containing sulfuric acid mixed solution | |
| CN104478733B (en) | The method reclaiming double DMAPA from DMAPA heavy constituent | |
| CN103664650A (en) | Method of preparing N-methyldiethanolamine at normal temperature |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20221019 Address after: 257200 Hekou Beiying Road, Hekou economic Park, Shandong Province Patentee after: DONGYING ANOKY TEXTILE MATERIALS Co.,Ltd. Patentee after: Shandong anoqi Chemical Technology Research Co.,Ltd. Address before: 779 Haining Road, Hekou District, Dongying City, Shandong Province 257299 Patentee before: DONGYING ANOKY TEXTILE MATERIALS Co.,Ltd. |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240415 Address after: 257200 Hekou Beiying Road, Hekou economic Park, Shandong Province Patentee after: DONGYING ANOKY TEXTILE MATERIALS Co.,Ltd. Country or region after: China Patentee after: Shandong annuoqi Fine Chemical Co.,Ltd. Address before: 257200 Hekou Beiying Road, Hekou economic Park, Shandong Province Patentee before: DONGYING ANOKY TEXTILE MATERIALS Co.,Ltd. Country or region before: China Patentee before: Shandong anoqi Chemical Technology Research Co.,Ltd. |