CN110170185B - Device and method for separating waste sulfuric acid nitro compounds - Google Patents
Device and method for separating waste sulfuric acid nitro compounds Download PDFInfo
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- CN110170185B CN110170185B CN201910462254.8A CN201910462254A CN110170185B CN 110170185 B CN110170185 B CN 110170185B CN 201910462254 A CN201910462254 A CN 201910462254A CN 110170185 B CN110170185 B CN 110170185B
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- separator
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- mononitrotoluene
- nitrotoluene
- nitro compound
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0208—Separation of non-miscible liquids by sedimentation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
- B01D17/0208—Separation of non-miscible liquids by sedimentation
- B01D17/0214—Separation of non-miscible liquids by sedimentation with removal of one of the phases
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to a device and a method for separating waste sulfuric acid nitro compounds, wherein the device comprises a waste acid tank, the left upper part of the waste acid tank is communicated with a waste acid/nitro compound feed pipe, the right upper part of the waste acid tank is connected with a dispersing pipe on a separator through a nitro compound pipeline, the top of the separator is connected with a liquid ring vacuum pump through an exhaust pipe, inlet and outlet pipelines of the liquid ring vacuum pump are connected through a reflux valve, the left side of the separator is connected with a mononitrotoluene pump through a first nitrotoluene discharge pipe, a transfer tank and a second nitrotoluene discharge pipe which are sequentially connected, the output of the mononitrotoluene pump is communicated with a DNT tank, the right side of the separator is provided with a sight glass, and the bottom of the separator is connected with a polymer discharge pipe. The device and the method for separating the waste sulfuric acid nitro compound can realize the separation of the mononitrotoluene and the polymer, reduce the toxicity in acidic wastewater, recycle the recovered mononitrotoluene to generate economic benefit, and reduce the environmental protection risk.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a device and a method for separating waste sulfuric acid nitro compounds.
Background
The trinitrotoluene waste sulfuric acid needs to be separated before being treated, the main components of the free nitro compounds are mononitrotoluene (accounting for 70% -80%), a small amount of dinitrotoluene, trinitrotoluene and polymers (the polymers are complex derivatives of polynitrotoluene, accounting for 20% -30%), and the specific gravity of the waste sulfuric acid is generally 1.60-1.63; the specific gravity of the nitro compound is generally 1.18-1.20, and dinitrotoluene and trinitrotoluene are dissolved in Mononitrotoluene (MNT); the polymer is insoluble in waste acid and mononitrotoluene, the specific gravity (1.19-1.2) of the polymer is similar to that (1.16-1.18) of the mononitrotoluene, the specific gravity of the polymer is slightly higher than that of the mononitrotoluene, the polymer is easy to mix with the mononitrotoluene, and due to the disturbance, in a waste acid tank, the liquid is generally divided into a nitro compound layer (upper layer) and a waste acid layer (lower layer), and the mononitrotoluene is mixed with the polymer; because the nitro compound contains more polymer (20% -30%), the nitro compound loses use value and needs to be separated and removed from the waste acid tank periodically.
However, in the existing separation of nitro compounds, the waste sulfuric acid at the lower layer of the nitro compound waste acid tank is pumped to other waste sulfuric acid tanks, the nitro compound at the upper layer is lowered to the bottom of the waste acid tank, a nitro compound valve at the bottom of the waste acid tank is opened, the residual waste acid and the nitro compound are placed in a tank area cofferdam, a large amount of fluid nitro compound and waste acid enter an acidic water treatment system, and a small amount of viscous polymer is packaged and cleaned and transported to a destruction field for destruction. This method not only causes a great deal of nitro compound waste, but also severely pollutes the environment.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a device and a method for separating the nitro-compound of the waste sulfuric acid, and solves the problems that a large amount of nitro-compound is wasted, the toxicity in acidic wastewater is high and serious pollution is caused to the environment in the prior separation of the nitro-compound in the waste sulfuric acid.
The invention is realized by the following technical scheme:
the utility model provides a device of useless sulfuric acid nitro compound separation, includes the spent acid groove and is located separator of spent acid groove one side, the upper left portion intercommunication spent acid/nitro compound inlet pipe of spent acid groove, the upper left side intercommunication spent acid discharging pipe of spent acid groove, the upper right portion of spent acid groove passes through the dispersion tube connection of nitro compound pipeline and separator upper left portion, the top of separator is connected to the liquid ring vacuum pump through the blast pipe, connect through the reflux valve between the import and export pipeline of liquid ring vacuum pump, the left side of separator is connected one nitrotoluene exhaust pipe through one nitrotoluene valve, one nitrotoluene exhaust pipe's output communicates to the transfer groove, the output of transfer groove is connected to one nitrotoluene pump through one nitrotoluene exhaust pipe two, one nitrotoluene pump's output intercommunication DNT groove, the right side from top down of separator is equipped with one, sight glass three and sight glass four in proper order, the bottom of separator is connected to the tank wagon through the polymer exhaust pipe, be equipped with the polymer exhaust valve on the polymer exhaust pipe.
Further, the separator is a trough separator with a conical bottom.
Further, the mononitrotoluene valve comprises a mononitrotoluene valve I and a mononitrotoluene valve II, the left side of the separator is connected to one side of the mononitrotoluene valve I and the mononitrotoluene valve II respectively through pipelines, and the other sides of the mononitrotoluene valve I and the mononitrotoluene valve II are connected to a mononitrotoluene discharge pipe I.
The method for separating the waste sulfate nitro compound specifically comprises the following steps:
step S1: the mononitrotoluene valve one, mononitrotoluene valve two and polymer discharge valve were closed.
Step S2: closing the reflux valve, starting the liquid ring vacuum pump, and maintaining the pressure in the separator in a negative pressure state;
step S3: continuously injecting waste acid into a waste acid tank through a waste acid/nitro compound feed pipe, pressing the nitro compound at the upper part of the waste acid tank into a dispersing pipe through a nitro compound pipeline, dispersing the nitro compound into a film shape under the action of the dispersing pipe, locally separating nitrogen oxide gas under a negative pressure state, and pumping the separated nitrogen oxide gas by a liquid ring vacuum pump;
step S4: the nitro compound after separating the nitrogen oxide gas enters a separator, and is observed through a sight glass, and the liquid level in the separator reaches the height of a sight glass I, so that the nitro compound is stopped being conveyed to the separator;
step S5: opening a reflux valve, and increasing the pressure in the separator to 1 atmosphere, wherein the nitro compound in the separator is static for more than 18 hours;
step S6: observing a first sight glass, a second sight glass and a third sight glass, judging the interface between the mononitrotoluene and the polymer, opening a mononitrotoluene valve or a second mononitrotoluene valve, putting the mononitrotoluene into a transfer tank, and sending the mononitrotoluene into a DNT tank through a mononitrotoluene pump after the transfer tank is full;
step S7: viewing mirror four, open the polymer valve and place the polymer into the tank car.
Further, the negative pressure in the step S2 is 70-80kPa absolute.
Further, the mononitrotoluene in step S6 occupies 70-80% of the separator volume.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a device and a method for separating waste sulfuric acid nitro compounds, which separate nitro compounds from waste acid from the upper part of a waste acid tank, separate nitrogen oxide in the nitro compounds by adopting an atomization dispersing nitro compounds and a decompression technology, eliminate gas stirring factors, realize static separation of mononitrotoluene (1.16-1.18) with similar specific gravity and polymers (1.19-1.20), and recover 70% -80% of mononitrotoluene contained in the nitro compounds; the method can greatly reduce the acidic wastewater generated by the traditional nitro compound cleaning mode, reduce the content of nitrites in the acidic wastewater, reduce the biotoxicity of the acidic wastewater, and is favorable for improving the production capacity and the production quality of the subsequent wastewater treatment process; the economic benefit is improved, and the environmental protection risk is reduced; and recycling the recovered mononitrotoluene not only generates economic benefit, but also greatly reduces the destruction quantity of nitro compounds and reduces environmental pollution.
Drawings
FIG. 1 is a schematic diagram of the apparatus for separating waste sulfate nitro compounds according to the present invention.
In the figure:
1. a waste acid tank; 2. a separator; 3. a transfer tank; 4. a mononitrotoluene pump; 5. a nitro compound conduit; 6. a mononitrotoluene discharge pipe I; 7. a mononitrotoluene discharge pipe II; 8. a polymer discharge pipe; 9. mononitrotoluene valve one; 10. a mononitrotoluene valve II; 11. a polymer discharge valve; 12. a first sight glass; 13. a second sight glass; 14. a third sight glass; 15. a sight glass IV; 16. an exhaust pipe; 17. a liquid ring vacuum pump; 18. a return valve; 19. a dispersion tube; 20. waste acid/nitro compound feed pipe; 21. waste acid discharging pipe.
Detailed Description
The following examples are presented to specifically illustrate certain embodiments of the invention and should not be construed as limiting the scope of the invention. Modifications to the disclosure of the invention may be made in the materials, methods, and reaction conditions, all of which are intended to fall within the spirit and scope of the invention.
The device for separating the waste sulfuric acid nitro compounds shown in fig. 1 comprises a waste acid tank 1 and a separator 2 positioned at one side of the waste acid tank 1, wherein the upper left part of the waste acid tank 1 is communicated with a waste acid/nitro compound feed pipe 20, the lower left part of the waste acid tank 1 is communicated with a waste acid discharge pipe 21, the upper right part of the waste acid tank 1 is connected with a dispersion pipe 19 at the upper left part of the separator 2 through a nitro compound pipeline 5, the nitro compounds in the waste acid tank 1 are discharged from the upper part of the tank, waste acid entrained in the nitro compounds is eliminated, the dispersion pipe 19 is used for forming a film shape under the action of impact force of the nitro compounds, and the nitrogen oxide gas is beneficial to separating out of the nitro compounds; the top of the separator 2 is connected to a liquid ring vacuum pump 17 through an exhaust pipe 16, inlet and outlet pipelines of the liquid ring vacuum pump 17 are connected through a reflux valve 18, and the pressure of the separator 2 is maintained at 70kPa-80kPa (absolute pressure) through the adjustment of the reflux valve 18 so as to be beneficial to the discharge of nitrogen oxide gas; the left side of the separator 2 is connected with a mononitrotoluene discharge pipe I6 through a mononitrotoluene valve, the output end of the mononitrotoluene discharge pipe I6 is communicated with a transfer tank 3, the output end of the transfer tank 3 is connected with a mononitrotoluene pump 4 through a mononitrotoluene discharge pipe II 7, the output end of the mononitrotoluene pump 4 is communicated with a DNT tank, and the mononitrotoluene is recycled to the DNT tank to be used as a solvent; the right side of the separator 2 is sequentially provided with a first sight glass 12, a second sight glass 13, a third sight glass 14 and a fourth sight glass 15 from top to bottom, the bottom of the separator 2 is connected to a tank car through a polymer discharge pipe 8, and polymers are destroyed; the polymer discharge pipe 8 is provided with a polymer discharge valve 11.
In this embodiment, the separator 2 is a trough separator with a conical bottom.
In this embodiment, the mononitrotoluene valve comprises a mononitrotoluene valve one 9 and a mononitrotoluene valve two 10, the left side of the separator 2 is connected to one side of the mononitrotoluene valve one 9 and the mononitrotoluene valve two 10 respectively through pipelines, and the other sides of the mononitrotoluene valve one 9 and the mononitrotoluene valve two 10 are connected to a mononitrotoluene discharge pipe one 6.
The method for separating the waste sulfate nitro compound specifically comprises the following steps:
step S1: the mononitrotoluene valve one 9, the mononitrotoluene valve two 10 and the polymer discharge valve 11 were closed.
Step S2: closing the reflux valve 18, starting the liquid ring vacuum pump 17, and maintaining the pressure in the separator 2 in a negative pressure state;
step S3: continuously injecting waste acid into the waste acid tank 1 through a waste acid/nitro compound feed pipe 20, pressing the nitro compound at the upper part of the waste acid tank 1 into a dispersing pipe 19 through a nitro compound pipeline 5, dispersing the nitro compound into a film shape under the action of the dispersing pipe 19, locally separating nitrogen oxide gas under a negative pressure state, and pumping the separated nitrogen oxide gas out by a liquid ring vacuum pump 17;
step S4: the nitro compound after separating the nitrogen oxide gas enters the separator 2, and is observed through the sight glass, and the nitro compound is stopped to be conveyed to the separator 2 when the liquid level in the separator 2 reaches the height of the sight glass I12;
step S5: opening reflux valve 18 to raise the pressure in separator 2 to 1 atm to facilitate separation of mononitrotoluene from polymer, and standing the nitro compound in separator 2 for 18 hr or more;
step S6: observing a first sight glass 12, a second sight glass 13 and a third sight glass 14, judging the interface between the mononitrotoluene and the polymer, opening a mononitrotoluene valve 9 or a mononitrotoluene valve 10, putting the mononitrotoluene into a transfer tank 3, and after the transfer tank 3 is full, sending the mononitrotoluene into a DNT tank through a mononitrotoluene pump 4;
step S7: viewing mirror four 15, the polymer valve was opened and the polymer was placed in the tank truck.
In this embodiment, the negative pressure in step S2 is 70-80kPa absolute.
In this example, the mononitrotoluene in step S6 is 70-80% by volume of the separator 2.
The method separates the nitro compound from the upper part of a waste acid tank and the waste acid, adopts an atomization dispersion nitro compound, separates nitrogen oxide in the nitro compound by a decompression technology, eliminates gas stirring factors, realizes static separation of mononitrotoluene (1.16-1.18) with similar specific gravity and polymers (1.19-1.20), and recovers 70% -80% of mononitrotoluene contained in the nitro compound; the method can greatly reduce the acidic wastewater generated by the traditional nitro compound cleaning mode, reduce the content of nitrites in the acidic wastewater, reduce the biotoxicity of the acidic wastewater, and is favorable for improving the production capacity and the production quality of the subsequent wastewater treatment process; the economic benefit is improved, and the environmental protection risk is reduced; and recycling the recovered mononitrotoluene not only generates economic benefit, but also greatly reduces the destruction quantity of nitro compounds and reduces environmental pollution.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (4)
1. The utility model provides a device of useless sulfuric acid nitro compound separation, its characterized in that includes spent acid groove (1) and is located separator (2) of spent acid groove (1) one side, the upper left portion intercommunication spent acid of spent acid groove (1) waste acid/nitro compound inlet pipe (20), the lower left side intercommunication spent acid discharging pipe (21) of spent acid groove (1), the upper right portion of spent acid groove (1) is connected with dispersion tube (19) of separator (2) upper left portion through nitro compound pipeline (5), the top of separator (2) is connected to liquid ring vacuum pump (17) through blast pipe (16), be connected through reflux valve (18) between the import and export pipeline of liquid ring vacuum pump (17), the left side of separator (2) is through one nitrotoluene valve connection one nitrotoluene exhaust pipe (6), the output of one nitrotoluene exhaust pipe one (6) is linked to transfer groove (3), the output of transfer groove (3) is connected to one nitrotoluene exhaust pipe two (7) through one nitrotoluene exhaust pipe two (4), one nitrotoluene pump (4) is equipped with one nitrotoluene pump (14), one side of three sight glass (12) are equipped with in proper order from top to bottom, one sight glass (12), the bottom of separator (2) is connected to the tank wagon through polymer drain pipe (8), be equipped with polymer discharge valve (11) on polymer drain pipe (8), separator (2) are the trough type separator of taking the cone end, one nitrotoluene valve includes one nitrotoluene valve (9) and one nitrotoluene valve two (10), the left side of separator (2) is connected to one side of one nitrotoluene valve (9), one nitrotoluene valve two (10) through the pipeline respectively, one nitrotoluene valve (9), one nitrotoluene valve two (10)'s opposite side is connected to one nitrotoluene drain pipe (6) respectively.
2. A method for separating waste sulfuric acid nitro compounds by using the device as claimed in claim 1, characterized by comprising the following steps:
step S1: closing a mononitrotoluene valve one (9), a mononitrotoluene valve two (10) and a polymer discharge valve (11);
step S2: closing the reflux valve (18), starting the liquid ring vacuum pump (17), and maintaining the pressure in the separator (2) in a negative pressure state;
step S3: continuously injecting waste acid into a waste acid tank (1) through a waste acid/nitro compound feed pipe (20), pressing nitro compound at the upper part of the waste acid tank (1) into a dispersing pipe (19) through a nitro compound pipeline (5), dispersing the nitro compound into a film shape under the action of the dispersing pipe (19), and locally separating nitrogen oxide gas under a negative pressure state, wherein the separated nitrogen oxide gas is pumped out by a liquid ring vacuum pump (17);
step S4: the nitro compound after separating the nitrogen oxide gas enters the separator (2), and the liquid level in the separator (2) reaches the height of the first sight glass (12) through sight glass observation, so that the nitro compound is stopped from being conveyed to the separator (2);
step S5: opening a reflux valve (18) to raise the pressure in the separator (2) to 1 atmosphere, and standing the nitro compound in the separator (2) for more than 18 hours;
step S6: observing a first sight glass (12), a second sight glass (13) and a third sight glass (14), judging the interface between the mononitrotoluene and the polymer, opening a first mononitrotoluene valve (9) or a second mononitrotoluene valve (10), putting the mononitrotoluene into a transfer tank (3), and sending the mononitrotoluene into a DNT tank through a mononitrotoluene pump (4) after the transfer tank (3) is full;
step S7: viewing mirror IV (15), open the polymer valve and place the polymer into the tank car.
3. A method for separating off waste sulphate nitro compounds according to claim 2, wherein the negative pressure in step S2 is 70-80kPa absolute.
4. A method for separating waste sulfuric acid nitro compounds according to claim 2, characterized in that the mononitrotoluene volume in step S6 is 70-80% of the separator (2) volume.
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| CN113371768B (en) * | 2021-05-31 | 2023-04-18 | 湖北东方化工有限公司 | TNT waste acid-residual liquid recovery process and device |
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