CN212451255U - Methylamine/ethylamine recovery processing system - Google Patents
Methylamine/ethylamine recovery processing system Download PDFInfo
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- CN212451255U CN212451255U CN202021215137.6U CN202021215137U CN212451255U CN 212451255 U CN212451255 U CN 212451255U CN 202021215137 U CN202021215137 U CN 202021215137U CN 212451255 U CN212451255 U CN 212451255U
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Abstract
The utility model discloses a methylamine/ethylamine recovery processing system, which aims to solve the technical problem of environmental pollution caused by methylamine/ethylamine in amination production wastewater. The utility model comprises an amine gasification tower, a multistage condensing device, a multistage negative pressure absorption device and a tail gas absorption tower which are sequentially communicated, wherein the amine gasification tower is sequentially provided with a heating unit, a liquid distribution unit and a reflux unit from bottom to top; the outlet of the reflux unit is communicated with the inlet of the multistage condensing device; the multistage negative pressure absorption device comprises at least two negative pressure absorption mechanisms; the negative pressure absorption mechanism comprises an absorption tank, a circulating pump and an ejector. The utility model has simple operation and control flow, easy use and maintenance and energy saving; utilize the utility model discloses can realize rectifying separation, condensation dewatering, the cooling circulation absorption step by step to amination waste water, realize that methylamine/ethylamine's abundant recovery and concentration improve in the waste water, and can with other relevant production facility and flow seamless connection, realize circulation, cleaner production.
Description
Technical Field
The utility model relates to an organic matter recovery unit technical field, concretely relates to methylamine/ethylamine recovery processing system.
Background
Methylamine/ethylamine is an important chemical raw material, is widely applied to organic chemical industries such as chemical industry, pesticides, medicine, rubber, leather and the like, is easily dissolved in water, and can generate a large amount of amine-containing wastewater in the production and use processes. Such as: in the production process of anion resin such as ion exchange resin 201 x 7/D201/D301, resin white balls need amination after chlorination. Amination is also required when raw materials dimethylamine is produced by adopting a one-step method or a two-step method for PZ (zinc dimethyldithiocarbamate) in the rubber accelerator industry and raw materials diethylamine is produced by ZDC (zinc diethyldithiocarbamate) series.
Amination is usually carried out by adopting methylamine/ethylamine, and the content of residual methylamine/ethylamine in the aminated mother liquor is 0.7-2.0%. Wherein trimethylamine is decomposed into dimethylamine under aerobic high temperature; while low concentration dimethylamine has a more unpleasant fish smell, higher concentrations can cause strong irritation to the eyes and respiratory tract. Therefore, if the amination mother liquor is not subjected to methylamine/ethylamine recovery, the amination mother liquor directly enters a wastewater treatment system or is discharged into a water body, so that environmental pollution is caused, the treatment difficulty of the wastewater treatment system is increased, and resources are wasted, so that effective treatment and recovery measures need to be taken.
At present, the methylamine/ethylamine wastewater is treated by adopting an incineration method in China mostly, but a low-concentration methylamine/ethylamine aqueous solution cannot be combusted and a large amount of heat must be provided for the combustion of the low-concentration methylamine/ethylamine aqueous solution, so that the combustion treatment method has high energy consumption and high cost; in addition, the amination waste water can generate harmful gases such as nitrogen dioxide, nitric oxide, carbon dioxide, carbon monoxide and the like after combustion, thereby causing secondary pollution to air.
In addition, other processing methods are as follows: the steam stripping method, the chemical precipitation method, the complex extraction method, the ion exchange method and the dimethylamine hydrochloride have the defects of high recovery cost, large investment and running power consumption and the like, and are not suitable for large-scale industrial production treatment.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to provide a methylamine/ethylamine recovery processing system to methylamine/ethylamine is difficult to carry out low-cost recycle among the amine-containing wastewater in can fundamentally solving prior art.
In order to solve the technical problem, the utility model adopts the following technical scheme:
the utility model provides a methylamine/ethylamine recovery processing system, including amine gasification tower, multistage condensing equipment, multistage negative pressure absorbing device and the tail gas absorption tower that communicates in proper order:
the amine gasification tower is sequentially provided with a heating unit, a liquid distribution unit and a reflux unit from bottom to top; the outlet of the reflux unit is communicated with the inlet of the multistage condensing device;
the multistage negative pressure absorption device comprises at least three negative pressure absorption mechanisms, each negative pressure absorption mechanism comprises an absorption tank, a circulating pump and an ejector, wherein the air suction port of the ejector of the primary negative pressure absorption mechanism is connected with the front stage of the primary negative pressure absorption mechanism for processing incoming air, and the air suction ports of the rest stages of ejectors are communicated with the air exhaust port of the front stage of the absorption tank; the liquid inlet of each stage of ejector is communicated to the circulating liquid outlet of the absorption tank of the stage through a corresponding circulating pump, and the liquid outlet of each stage of ejector is communicated to the liquid inlet of the absorption tank of the stage.
Preferably: a tail gas circulating pump and a spraying unit are arranged in the tail gas absorption tower; and the inlet of the tail gas absorption tower is communicated with the exhaust port of the absorption tank in the final-stage negative pressure absorption mechanism.
Preferably: and a water supplementing inlet is formed in the spraying unit.
Preferably: and a water collector and a reflux liquid inlet are arranged in the reflux unit, and the distance between the reflux liquid inlet and the bottom of the water collector is more than or equal to 3 m.
Preferably: and a liquid outlet of the tail gas absorption tower is communicated with a liquid inlet of an absorption tank in the final-stage negative pressure absorption mechanism.
Preferably: and the liquid outlet of the absorption tank at the current stage between the negative pressure absorption mechanisms is communicated with the liquid inlet of the absorption tank at the previous stage.
Preferably: the multistage condensing device comprises at least two condensers.
Preferably: and the liquid outlet of the multistage condensing device is communicated with an amine recycling tank, and the liquid outlet of the absorption tank in the primary negative pressure absorption mechanism is communicated with the amine recycling tank.
Preferably: the liquid outlet of the multistage condensing device is communicated with a corresponding organic matter recovery tank; and a liquid outlet of the reflux unit is communicated with the organic matter recovery box.
Compared with the prior art, the utility model has the beneficial technical effects of:
1. the utility model discloses equipment constitutes retrencies, and the input cost is low, and each processing unit configuration is reasonable ingenious, and the operation control flow is simple, easily operates and maintains, and the energy consumption is saved.
2. Utilize the utility model discloses can effectively realize rectifying separation, condensation dewatering, the cooling circulation absorption step by step to amination waste water, realize in the waste water that the abundant recovery and the concentration of methylamine/ethylamine improve (containing methylamine or ethylamine 10% ~ 20%), make it can reach the standard of retrieval and utilization, just the utility model discloses can with other relevant production facility and flow seamless connection, realize circulation, cleaner production.
Drawings
FIG. 1 is a schematic diagram of an amination process wastewater treatment system.
FIG. 2 is a schematic view of the structure of a first absorption column.
In the above figures, 1 is an amine gasification tower; 11 is a heating unit, 12 is a liquid distribution unit, and 13 is a reflux unit; 2 is a multi-stage condensing device; 21 is a first condenser, 22 is a second condenser, and 23 is a third condenser; 3 is a multi-stage negative pressure absorption device; 31 is a first absorption tower, 311 is a first absorption tank, 312 is a first circulating pump, 313 is a first ejector, 32 is a second absorption tower, 33 is a third absorption tower, and 34 is a fourth absorption tower; 4 is a tail gas absorption tower; 41 is a tail gas circulating pump, 42 is a spraying unit, and 43 is a water replenishing inlet; 5 is an amine recovery box; 6 is an organic matter recycling box; a is a waste liquid inlet, B is an evacuation port, C is a waste liquid outlet, D is an outlet which is arranged on the organic matter recycling box and is discharged to the recycling point, and E is an outlet which is arranged on the amine recycling box and is discharged to the recycling point.
Detailed Description
The following embodiments are only intended to illustrate the present invention in detail, and do not limit the scope of the present invention in any way.
The instruments and devices referred to in the following examples are conventional instruments and devices unless otherwise specified; the raw materials are all conventional materials which are sold in the market if not specifically indicated; the treatment methods involved are conventional methods unless otherwise specified.
Example 1: amination waste water treatment system
As shown in fig. 1: the amination production wastewater treatment system comprises an amine gasification tower 1, a multistage condensing device 2, a multistage negative pressure absorption device 3 and a tail gas absorption tower 4 which are sequentially communicated.
The amine gasification tower 1 is sequentially provided with a heating unit 11, a liquid distribution unit 12 and a reflux unit 13 from bottom to top; the heating unit 11 is heated by steam, and the heating temperature is 85-105 ℃; the liquid distribution unit 12 is provided with a liquid distribution pipe, and an atomizing nozzle is arranged on the liquid distribution pipe, so that the atomizing particle size is 100-1000 mm; the bottom of the liquid distribution unit 12 is provided with a packing layer which is conventional irregular packing and mainly made of amine gas corrosion resistant materials such as stainless steel Raschig rings, pall rings, ladder rings and the like; the lower part of the packing layer is provided with a flushing mechanism, the flushing water adopts water to be treated, and is mainly used for flushing the packing through large flow, so that the blockage of the packing after long-time operation is prevented; the outlet of the reflux unit 13 is communicated with the multistage condensing device 2; an S-shaped water collector is arranged in the reflux unit 13, so that small liquid drops can be better captured, and the amine steam can be conveniently discharged from an exhaust port; the reflux unit 13 is also internally provided with a reflux liquid inlet, and the distance between the reflux liquid inlet and the bottom of the water collector is more than or equal to 3 m.
The multistage condensing device 2 comprises a first condenser 21, a second condenser 21 and a third condenser 23 which are communicated in sequence; an ice and water machine outlet and an ice and water machine inlet are arranged on the condenser, so that the temperature in the condenser is controlled to be 0-10 ℃; the condenser is also provided with a reflux liquid outlet which is communicated with a reflux liquid inlet in the reflux unit 13.
The multistage negative pressure absorption device 3 comprises a first absorption tower 31, a second absorption tower 32, a third absorption tower 33 and a fourth absorption tower 34; the absorption towers are provided with an ice water outlet and an ice water inlet, the temperature in the first absorption tower 31, the second absorption tower 32 and the third absorption tower 33 is controlled to be 4-10 ℃, and the temperature in the fourth absorption tower 34 is controlled to be 0-25 ℃.
The first absorption tower 31 includes a first absorption tank 311, a first circulation pump 312, and a first ejector 313; the first absorption tank 311 is provided with an inlet, a liquid inlet, an upper exhaust port and a lower outlet; the air suction port of the first ejector 313 communicates the air outlet of the third condenser 23 and the outlet of the first circulation pump 312; the outlet of the first ejector 313 is communicated with the inlet of the first absorption tank 311; the lower outlet of the first absorption tank 311 is communicated with the inlet of the first circulation pump 312.
The second absorption tower 32 includes a second absorption tank, a second circulation pump, and a second ejector; the second absorption tank is provided with an inlet, a liquid inlet, an upper exhaust port and a lower outlet; the suction port of the second ejector communicates the upper discharge port of the first absorption tank 311 and the outlet of the second circulation pump; the outlet of the second ejector is communicated with the inlet of the second absorption tank; and the lower outlet of the second absorption tank is communicated with the inlet of the second circulating pump.
The third absorption tower 33 includes a third absorption tank, a third circulation pump, and a third ejector; the third absorption tank is provided with an inlet, a liquid inlet, an upper exhaust port and a lower outlet; the air suction port of the third ejector is communicated with the upper exhaust port of the second absorption tank and the outlet of the third circulating pump; the outlet of the third ejector is communicated with the inlet of the third absorption tank; and the lower outlet of the third absorption tank is communicated with the inlet of the third circulating pump.
The fourth absorption tower 34 includes a fourth absorption tank, a fourth circulation pump, and a fourth ejector; the fourth absorption tank is provided with an inlet, a liquid inlet, an upper exhaust port and a lower outlet; the air suction port of the fourth ejector is communicated with the upper exhaust port of the third absorption tank and the outlet of the fourth circulating pump; the outlet of the fourth ejector is communicated with the inlet of the fourth absorption tank; and the lower outlet of the fourth absorption tank is communicated with the inlet of the fourth circulating pump.
A tail gas circulating pump 41 and a spraying unit 42 are arranged in the tail gas absorption tower 4; an inlet of the tail gas absorption tower 4 is communicated with an exhaust port of the fourth absorption tank; the shower unit 42 is provided with a water replenishment inlet 43.
A liquid outlet of the tail gas absorption tower 4 is communicated with a liquid inlet of a fourth absorption tank; a liquid outlet of the fourth absorption tank is communicated with a liquid inlet of the third absorption tank; a liquid outlet of the third absorption tank is communicated with a liquid inlet of the second absorption tank; the liquid outlet of the second absorption tank is communicated with the liquid inlet of the first absorption tank 311.
A liquid outlet of the third condenser 23 is communicated with an amine recovery tank 5; the liquid outlet of the first absorption tank 311 is communicated with the inlet of the amine recovery tank 5.
The liquid outlet of the third condenser 23 is also communicated with an organic matter recovery tank 6; the liquid outlet of the reflux unit 13 in the amine gasification tower 1 is communicated with the inlet of the organic matter recovery tank 6.
The method for treating the amination production wastewater by using the wastewater treatment system comprises the following steps:
taking amination wastewater treatment of D301 anion resin of certain ion exchange resin enterprises as an example, the pH value of the amination wastewater is 8-9, and the amination wastewater is detected to mainly contain dimethylamine, methylal, methanol and the like as organic components; methylal is relatively stable to alkali, is easily decomposed into formaldehyde and methanol when heated together with dilute hydrochloric acid, reacts with concentrated hydrochloric acid to generate methyl chloride, and normally exists in the form of formaldehyde in water.
The wastewater of a certain batch of production is detected, the content of dimethylamine (detection standard: methylamine solution inspection HGT 2971-1999; determination GB/T23961-.
The specific treatment steps are as follows:
(1) after large-particle substances in the wastewater are filtered out, the wastewater flows into an amine gasification tower 1 from a wastewater inlet A, a bag filter is adopted for filtering, the filtering aperture is 0.1-0.5 mm, and the filtering material is an amine corrosion resistant material such as plastic or stainless steel. Liquid sodium hydroxide is added before the waste liquid inlet A to adjust the pH value of the waste water to 11.5. Heating a heating unit 11 of the amine gasification tower 1 by adopting steam at the heating temperature of 85-105 ℃; pumping the heated wastewater to the liquid distribution unit 12 through a circulating pump; the atomizing nozzle on the liquid distribution unit 12 atomizes the heated waste liquid into atomized liquid with the particle size of 100-1000 microns; because the outlet of the reflux unit 13 is communicated with the multistage condensing device 2, a temperature difference is formed between a low-temperature region arranged on the multistage condensing device 2 and a high-temperature region of the heating unit 11, so that negative pressure is formed at the reflux unit 13, part of water vapor and organic matters are condensed, the water vapor and the organic matters flow back to the reflux unit 13 from the outlet of the reflux unit 13, and the liquid outlet of the reflux unit 13 is further communicated with the inlet of the organic matter recycling box 6;
so far, dimethylamine gas with the mass percentage of 1-5% is detected by using portable dimethylamine gas detection equipment (Shenzhen Dong Ying energy science and technology Co., Ltd.).
(2) Because the methylamine/ethylamine gas has a high boiling point and a low melting point, according to the theory that the solubility of gas in liquid is reduced along with the temperature rise and the solubility of gas is reduced along with the pressure reduction, dimethylamine gas and water vapor in the amine gasification tower 1 enter the multistage condensing device 2 together; most of the water vapor is condensed into liquid, meanwhile, the condensate contains a small amount of dimethylamine oil, the condensate flows back to the top of the amine gasification tower 1 to continuously distill out dimethylamine gas, and the temperature parameters of all stages of condensers are well controlled:
the temperature in the first condenser 21, the second condenser 22 and the third condenser 23 is controlled to be 4 ℃; determining that the content of dimethylamine in the third condenser 23 is less than 300mg/L, wherein one part of condensate is recycled by a liquid outlet of the third condenser 23 communicated with an inlet of the organic matter recycling tank 6, and one part of condensate and the condensate of the first condenser 21 and the second condenser 22 flow back to the amine gasification tower 1;
at this moment, water vapor and other organic matters are firstly recovered through the multistage condensing device 2, and dimethylamine gas which is not condensed and has the mass percentage of 1-5% is obtained at the outlet of the third condenser 23 by adopting portable detection of the dimethylamine gas.
(3) The methylamine/ethylamine gas obtained by the treatment in the step (2) enters a multistage negative pressure absorption device 3; the temperature in the first absorption column 31 was controlled to 10 ℃, the temperature in the second absorption column 32 was controlled to 6 ℃, the temperature in the third absorption column 33 was controlled to 2 ℃ and the temperature in the fourth absorption column 34 was controlled to 20 ℃.
Pure water is supplemented to the spraying unit 42 in the tail gas absorption tower 4, and the conductivity is less than 1 mu s/cm; a liquid outlet of the tail gas absorption tower 4 is communicated with a liquid inlet of a fourth absorption tank; a liquid outlet of the fourth absorption tank is communicated with a liquid inlet of the third absorption tank; a liquid outlet of the third absorption tank is communicated with a liquid inlet of the second absorption tank; the liquid outlet of the second absorption tank is communicated with the liquid inlet of the first absorption tank 311; and (4) gradually conveying the supplemented water to the previous stage until the solubility of the dimethylamine solution in the first absorption tank 311 is 10-20%, and then flowing into the amine recovery tank 5 for recovery.
The pressure in the absorption tank is controlled to be-0.05 to-0.01 MPa.
(4) Other tail gases (mainly non-condensable gas nitrogen and trace water-insoluble organic hydrocarbon gas) are discharged by the tail gas absorption tower 4 according to the discharge standard DB 41/1135-2016 Henan chemical industry water pollutant indirect discharge standard reaching the standard; and finishing the wastewater treatment.
Wherein, the 13 steam of backward flow unit and organic matter condensation backward flow have guaranteed to contain a small amount of water in the methylamine/ethylamine gas in the waste liquid steam as far as possible, guarantee that multistage negative pressure absorbing device 3 normal water can only the moisturizing, can mix with salinity and a large amount of moisture in the dimethylamine of avoiding retrieving, lead to the unable in-production retrieval and utilization of methylamine/ethylamine of retrieving.
The invention is explained in detail above with reference to the drawings and the embodiments; however, it will be understood by those skilled in the art that various changes in the specific parameters of the embodiments described above may be made or equivalents may be substituted for elements thereof without departing from the technical spirit of the invention, so as to form a plurality of specific embodiments, which are all common variations of the invention and will not be described in detail herein.
Claims (9)
1. The utility model provides a methylamine/ethylamine recovery processing system, includes amine gasification tower, multistage condensing equipment, multistage negative pressure absorbing device and the tail gas absorption tower that communicates in proper order, its characterized in that:
the amine gasification tower is sequentially provided with a heating unit, a liquid distribution unit and a reflux unit from bottom to top; the outlet of the reflux unit is communicated with the inlet of the multistage condensing device;
the multistage negative pressure absorption device comprises at least three negative pressure absorption mechanisms, each negative pressure absorption mechanism comprises an absorption tank, a circulating pump and an ejector, wherein an ejector suction port of a primary negative pressure absorption mechanism is connected with a preceding stage of the absorption tank for processing incoming gas, and suction ports of the rest stages of the ejectors are communicated with an exhaust port of the preceding stage of the absorption tank; the liquid inlet of each ejector is communicated to the circulating liquid outlet of the absorption tank of the stage through a corresponding circulating pump, and the liquid outlet of each ejector is communicated to the liquid inlet of the absorption tank of the stage.
2. The methylamine/ethylamine recovery processing system as claimed in claim 1, wherein: a tail gas circulating pump and a spraying unit are arranged in the tail gas absorption tower; and the inlet of the tail gas absorption tower is communicated with the exhaust port of the absorption tank in the final-stage negative pressure absorption mechanism.
3. A methylamine/ethylamine recovery processing system as claimed in claim 2, wherein: and a water supplementing inlet is formed in the spraying unit.
4. The methylamine/ethylamine recovery processing system as claimed in claim 1, wherein: and a water collector and a reflux liquid inlet are arranged in the reflux unit, and the distance between the reflux liquid inlet and the bottom of the water collector is more than or equal to 3 m.
5. The methylamine/ethylamine recovery processing system as claimed in claim 1, wherein: and a liquid outlet of the tail gas absorption tower is communicated with a liquid inlet of an absorption tank in the final-stage negative pressure absorption mechanism.
6. The methylamine/ethylamine recovery processing system as claimed in claim 1, wherein: and the liquid outlet of the absorption tank at the current stage between the negative pressure absorption mechanisms is communicated with the liquid inlet of the absorption tank at the previous stage.
7. The methylamine/ethylamine recovery processing system as claimed in claim 1, wherein: the multistage condensing device comprises at least two condensers.
8. The methylamine/ethylamine recovery processing system as claimed in claim 1, wherein: and the liquid outlet of the multistage condensing device is communicated with an amine recycling tank, and the liquid outlet of the absorption tank in the primary negative pressure absorption mechanism is communicated with the amine recycling tank.
9. The methylamine/ethylamine recovery processing system as claimed in claim 1, wherein: the liquid outlet of the multistage condensing device is communicated with a corresponding organic matter recovery tank; and a liquid outlet of the reflux unit is communicated with the organic matter recovery box.
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| CN111960950A (en) * | 2020-06-28 | 2020-11-20 | 魏毅宏 | Treatment system and method for recovering methylamine/ethylamine from amine-containing wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111960950A (en) * | 2020-06-28 | 2020-11-20 | 魏毅宏 | Treatment system and method for recovering methylamine/ethylamine from amine-containing wastewater |
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