CN112694164A - Method for treating acrylonitrile device wastewater - Google Patents
Method for treating acrylonitrile device wastewater Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/727—Treatment of water, waste water, or sewage by oxidation using pure oxygen or oxygen rich gas
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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- C—CHEMISTRY; METALLURGY
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- C02F2209/03—Pressure
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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Abstract
The invention relates to a method for treating acrylonitrile device wastewater, which mainly solves the problems of high energy consumption and serious environmental pollution in the prior art for treating the acrylonitrile device wastewater. The invention adopts the following steps: the acrylonitrile device wastewater raw material and oxygen-containing gas enter a catalytic wet oxidation reactor after heat exchange, and a treated material is obtained under the action of a catalyst; the reactor is internally provided with a heat removal beam tube, and heat removal water enters the beam tube at a specific flow rate to carry out controlled heat removal.
Description
Technical Field
The invention relates to a method for treating acrylonitrile plant wastewater.
Background
Acrylonitrile (AN) is AN important basic organic feedstock. At present, the main process for producing acrylonitrile in China is a propylene ammoxidation method, namely, propylene, ammonia gas and air are used as main raw materials, acrylonitrile is obtained under certain reaction conditions and the action of a catalyst, and products such as acetonitrile, hydrocyanic acid and the like are produced as byproducts. In the above-mentioned acrylonitrile production process, the equipment waste mainly containing quench waste water and refined waste water is producedWater, which has high toxicity, high chroma and complex components. Wherein the quenching waste water is divided into one-section type and two-section type process quenching waste water according to different types of the quenching tower. The process wastewater of the one-section type quenching tower only has one stream of wastewater, and the wastewater is treated by concentration, incineration and sulfuric acid recovery. The two-section type quench tower process wastewater generates two wastewater streams, namely upper-section ammonium sulfate wastewater and lower-section tower kettle wastewater, the upper-section wastewater is concentrated to recover ammonium sulfate, condensate generated in the process returns to the upper section of the quench tower, and mother liquor and the lower-section wastewater of the quench tower are concentrated together and then are subjected to incineration treatment. The refined waste water is treated by multi-effect evaporation method, the evaporated condensate is treated by biochemical system, and the residual liquid is incinerated together with waste water at the lower section of the quench tower. The defects of the incineration method for treating the quenching wastewater are as follows: on one hand, the incineration belongs to a high energy consumption process; on the other hand, the incineration process will produce SO2、NOXAnd the like, and causes pollution to the environment. Therefore, it is important to develop a method for effectively treating wastewater of an acrylonitrile plant to realize green production of the acrylonitrile plant.
Wet oxidation is a technology developed in the 50 s of the 20 th century for treating toxic, harmful and high-concentration organic wastewater. The method is to oxidize organic pollutants into CO in a liquid phase by taking air or pure oxygen as an oxidant under the conditions of high temperature (125-320 ℃) and high pressure (0.5-20 MPa)2And inorganic substances such as water and the like or small molecular organic substances. The method has the advantages of wide application range, high treatment efficiency, high oxidation rate, less secondary pollution, low energy consumption, small occupied area and the like. On the basis of wet oxidation technology, the developed catalytic wet oxidation technology is to add a high-efficiency and stable catalyst designed according to the composition of wastewater in the traditional wet oxidation process. The technology can greatly improve the oxidation efficiency, shorten the reaction residence time, reduce the temperature and pressure required by the reaction and reduce the production cost. CN1167089A discloses a process for the treatment of acrylonitrile plant wastewater by first evaporating the wastewater to produce a gas stream containing steam, ammonia and volatile organic compounds, and then passing the gas stream to a catalytic reactor where it is converted at elevated temperature to a gas stream containing hydrogen, nitrogen and dioxygenA mixture of carbonized carbons. The method can only treat volatile substances in the wastewater and cannot treat high polymers and high-boiling-point organic matters. CN105084627A discloses a method for treating acrylonitrile ammonium sulfate wastewater, which comprises mixing ammonium sulfate wastewater with gas containing elemental oxygen, and feeding into a wet oxidation reactor to remove organic substances therein. The method has low removal rate of organic matters, high residual COD value of the waste water after reaction and no consideration of the full utilization of heat. CN104761041A discloses a catalytic wet oxidation treatment reaction tower and a method and a device for treating high-concentration organic wastewater by using the same, in the method, the high-concentration organic wastewater enters the reaction tower from the bottom of the reaction tower after passing through a storage tank, a high-pressure pump, a filter, a high-pressure buffer tank and a heat exchanger in sequence, the high-concentration organic wastewater in the reaction tower contacts with air and fully reacts, then the high-concentration organic wastewater enters a gas-liquid separation tank, and the treated wastewater is obtained at the bottom of the gas-liquid separation tank. The COD concentration of the wastewater treated by the method is low, and the method is suitable for treatment occasions where the COD concentration of the wastewater does not exceed 40000 mg/L. CN106348421A discloses a continuous wet oxidation process for degrading high-concentration organic wastewater and equipment thereof, the method comprises the steps of firstly exchanging heat between raw wastewater and treated wastewater, then mixing the heated wastewater with an oxidant, then feeding the mixture into a reactor for oxidation reaction, and feeding the treated wastewater into a separation process after exchanging heat and cooling. The method adopts a homogeneous catalyst, so that the separation of the treated wastewater is complex; in addition, when the COD concentration of the wastewater is high, the excessive heat generated by the reaction can cause a large amount of reaction wastewater to be vaporized, the heat loss is large, and the reaction effect is influenced. CN106380021A discloses a wet oxidation treatment system and method for high-concentration organic wastewater, which comprises the steps of firstly pretreating raw material wastewater, mixing the pretreated raw material wastewater with oxygen heated by heat exchange after heat exchange and heating, feeding the mixture into a reaction system, and feeding the reaction discharge into a gas-liquid separation system after heat exchange and cooling. The COD removal rate of the method is low, and similarly, when the COD concentration of the treated wastewater is high, a large amount of reaction wastewater in the reactor is vaporized, the heat loss is large, and the reaction effect is influenced. CN108455719A discloses a wet oxidation treatment system and a treatment method for high-concentration organic wastewater, wherein wastewater and oxygen are introduced into the wet oxidation treatment systemAnd carrying out oxidation reaction in a reactor with heating and stirring functions, and cooling the reaction discharge material and then feeding the cooled reaction discharge material into a gas-liquid separation system. The reaction device of the method is complex and discontinuous in wastewater treatment.
Disclosure of Invention
The invention relates to a method for treating acrylonitrile plant wastewater. The invention aims to solve the technical problems of environmental pollution and high energy consumption in the process of treating acrylonitrile device wastewater in the prior art. Provides a new method for treating acrylonitrile plant wastewater. When the method is used for treating wastewater, the method has the characteristics of simple process flow, high COD removal rate, full heat utilization, environmental protection and high economic benefit.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the acrylonitrile device wastewater treatment method comprises the following steps:
mixing acrylonitrile device wastewater raw materials and oxygen-containing gas, then feeding the mixture into a feeding and discharging heat exchanger, carrying out heat exchange and temperature rise, then feeding the mixture into a catalytic wet oxidation reactor, and carrying out heat exchange and temperature reduction on the obtained reaction discharge wastewater through the feeding and discharging heat exchanger (preferably, through a secondary temperature reduction unit) to obtain treated wastewater;
the COD value of the raw material wastewater is 20000 mg/L-300000 mg/L, and the COD removal rate of the wastewater after catalytic wet oxidation treatment is more than 90%.
A heat removal bundle pipe is arranged in the catalytic wet oxidation reactor, heat removal water with set flow is introduced into the bundle pipe, and a catalyst bed layer is arranged outside the bundle pipe;
the total flow of the heat removing water is L, the flow of the raw material wastewater is F, and the two satisfy the following relational expression:
L/F is (0.05-0.09) multiplied by the COD value of the raw material wastewater/10000-0.175.
The inlet temperature of the catalytic wet oxidation reactor is 200-250 ℃, the reaction pressure is 8-15 MPaG, and the reaction temperature is raised to 35-60 ℃.
In the technical scheme, the secondary cooling unit comprises a heat recoverer for recovering heat and/or a discharge cooler for cooling; optionally, the treated wastewater enters a gas-liquid separation tank for gas-liquid separation.
In the technical scheme, the COD value of the raw material wastewater is preferably 35000 mg/L-300000 mg/L; more preferably 50000mg/L to 200000 mg/L.
In the technical scheme, when the COD value of the raw material wastewater is more than 35000mg/L, the heat removing bundle pipe in the reactor is filled with heat removing water.
In the technical scheme, the pressure of the heat removing water is 1.2-3.0 MPaG, and the heat is absorbed by the reaction and then vaporized into water vapor.
In the technical scheme, the inlet temperature of the catalytic wet oxidation reactor is more preferably 210-240 ℃.
In the technical scheme, the catalytic wet oxidation reaction pressure is more preferably 9-13 MPaG.
In the technical scheme, the reaction temperature rise of the catalytic wet oxidation reactor is more preferably 40-55 ℃.
In the technical scheme, the volume airspeed of the catalytic wet oxidation reaction is 0.2-2.0 h-1Preferably 0.5 to 1.5 hours-1。
In the technical scheme, the amount of oxygen in the oxygen-containing gas is 1.1-1.3 times of the theoretical oxygen consumption required by the COD value of the raw material wastewater.
In the above technical scheme, the oxygen-containing gas is air, oxygen or a mixture of air and oxygen.
In the above technical scheme, the catalytic wet oxidation catalyst is at least one of a composite metal oxide catalyst and a noble metal supported catalyst.
The method adopts the catalytic wet oxidation technology to treat the acrylonitrile device wastewater, thereby avoiding the problems of high energy consumption, high operation cost and serious environmental pollution when the wastewater is treated by adopting a traditional multiple-effect evaporation and incineration method; the reactor is internally provided with the heat removal beam tube, the flow of the heat removal water entering the beam tube is regulated and controlled according to the COD value of the raw material wastewater, the reaction temperature rise is controlled, the vaporization rate of reaction materials is reduced as far as possible on the basis of ensuring the mutual matching of the heat exchange of feeding and discharging, the treatment of the wastewater with a high COD value is realized, the catalytic wet oxidation reaction is ensured to be in a stable, controllable and efficient state, the process is simple, the COD removal rate is high, the environmental protection and economic benefits are high, the industrialization is easy to realize, and a better technical effect is obtained.
Drawings
FIG. 1 is a schematic process flow diagram of the method for catalytic wet oxidation of acrylonitrile plant wastewater according to the present invention.
In fig. 1, 1 is an acrylonitrile device wastewater raw material, 2 is an oxygen-containing gas feed, 3 is heat removal water, 4 is water vapor, 5 is a reaction discharge, 6 is non-condensable gas, 7 is treated wastewater, R1 is a catalytic wet oxidation reactor, E1 is a feed and discharge heat exchanger, E2 is a steam generator or a heat recoverer, E3 is a discharge cooler, D1 is a steam buffer tank, and D2 is a product gas-liquid separation tank.
According to the flow shown in figure 1, an acrylonitrile device wastewater raw material 1 and an oxygen-containing gas feed 2 are mixed and then enter a feed and discharge heat exchanger E1, and enter the shell side of a catalytic wet oxidation reactor R1 from the bottom after heat exchange and temperature rise. And heat removing water is introduced into an inner pipeline of the R1, the entering amount of the heat removing water is regulated to remove certain reaction heat, and the generated water vapor 4 enters a vapor buffer tank D1. The reaction discharge material enters a product gas-liquid separation tank D2 after being subjected to heat exchange and temperature reduction by a feeding and discharging heat exchanger E1, heat recovery by a steam generator or a heat recoverer E2 and cooling by a discharge cooler E3 in sequence. The noncondensable gas 6 was discharged from the top of the gas-liquid separation tank D2, and the treated wastewater 7 was obtained from the bottom.
The present invention will be further described with reference to specific examples, but the scope of the present invention is not limited to the scope covered by the examples.
Detailed Description
[ example 1 ]
As shown in figure 1, the COD value of the wastewater raw material is 291630mg/L, the inlet temperature of the catalytic wet oxidation reactor is 205 ℃, the reaction pressure is 8.5MPaG, and the volume space velocity is 1.5h-1The catalyst is composite metal oxide catalyst Al2O3(ii) a Oxygen is adopted as oxygen-containing gas, and the amount of oxygen is 1.2 times of the theoretical oxygen consumption required by the COD value of the wastewater raw material; the ratio of the flow rate of the heat removing water to the flow rate of the raw material wastewater is 1.9; the pressure of the heat removal water is 1.4 MPaG; the temperature rise at the outlet of the reactor is 60 ℃; the COD removal rate of the obtained wastewater was 93.2%.
[ example 2 ]
As shown in figure 1, the COD value of the wastewater raw material is 250972mg/L, the inlet temperature of the catalytic wet oxidation reactor is 210 ℃, the reaction pressure is 9.0MPaG, and the volume space velocity is 1.2h-1The catalyst is composite metal oxide catalyst Al2O3(ii) a Oxygen is adopted as oxygen-containing gas, and the amount of oxygen is 1.2 times of the theoretical oxygen consumption required by the COD value of the wastewater raw material; the ratio of the flow rate of the heat removing water to the flow rate of the raw material wastewater is 1.7; the pressure of the heat removal water is 1.65 MPaG; the temperature rise at the outlet of the reactor is 55 ℃; the COD removal rate of the obtained wastewater was 93.9%.
[ example 3 ]
As shown in figure 1, the COD value of the wastewater raw material is 193785mg/L, the inlet temperature of the catalytic wet oxidation reactor is 220 ℃, the reaction pressure is 9.5MPaG, and the volume space velocity is 0.8h-1The loaded catalyst is a noble metal supported catalyst Pd/Al2O3(ii) a Oxygen is adopted as oxygen-containing gas, and the amount of oxygen is 1.1 times of the theoretical oxygen consumption required by the COD value of the wastewater raw material; the ratio of the flow rate of the heat removing water to the flow rate of the raw material wastewater is 1.2; the pressure of the heat removal water is 1.9 MPaG; the temperature of the outlet of the reactor is raised to 50 ℃; the COD removal rate of the obtained wastewater is 94.3%.
[ example 4 ]
As shown in figure 1, the COD value of the wastewater raw material is 145869mg/L, the inlet temperature of the catalytic wet oxidation reactor is 220 ℃, the reaction pressure is 10.5MPaG, and the volume space velocity is 0.4h-1The loaded catalyst is a composite metal oxide catalyst ZrO2(ii) a Oxygen is adopted as oxygen-containing gas, and the amount of oxygen is 1.1 times of the theoretical oxygen consumption required by the COD value of the wastewater raw material; the ratio of the flow rate of the heat removing water to the flow rate of the raw material wastewater is 0.9; the pressure of the heat removal water is 1.9 MPaG; the temperature rise at the outlet of the reactor is 45 ℃; the COD removal rate of the obtained wastewater was 95.0%.
[ example 5 ]
As shown in figure 1, the COD value of the wastewater raw material is 97426mg/L, the inlet temperature of the catalytic wet oxidation reactor is 230 ℃, the reaction pressure is 11.0MPaG, and the volume space velocity is 1.8h-1The loaded catalyst is a composite metal oxide catalystAgent ZrO2(ii) a Oxygen is adopted as oxygen-containing gas, and the amount of oxygen is 1.3 times of the theoretical oxygen consumption required by the COD value of the wastewater raw material; the ratio of the flow rate of the heat removing water to the flow rate of the raw material wastewater is 0.6; the pressure of the heat removal water is 2.4 MPaG; the temperature rise at the outlet of the reactor is 45 ℃; the COD removal rate of the obtained wastewater is 96.6%.
[ example 6 ]
As shown in figure 1, the COD value of the wastewater raw material is 36295mg/L, the inlet temperature of the catalytic wet oxidation reactor is 240 ℃, the reaction pressure is 12.5MPaG, and the volume space velocity is 1.0h-1The loaded catalyst is a noble metal supported catalyst Ru/ZrO2(ii) a The oxygen-containing gas adopts air, and the amount of the air is 1.3 times of the theoretical oxygen consumption required by the COD value of the feed wastewater; the ratio of the flow rate of the heat removing water to the flow rate of the raw material wastewater is 0.09; the pressure of the heat removal water is 2.9 MPaG; the temperature rise at the outlet of the reactor is 35 ℃; the COD removal rate of the obtained wastewater is 97.5%.
[ COMPARATIVE EXAMPLE 1 ]
The conditions and the steps of the example 6 are kept unchanged, and the catalytic wet oxidation reactor is not provided with a heat removal beam pipe and is not introduced with heat removal water. The COD removal rate of the waste water obtained at this time was 91.7%.
[ COMPARATIVE EXAMPLE 2 ]
The conditions and procedures of example 6 were followed, with the other operating conditions being kept constant, and the ratio of the flow rate of the withdrawal water to the flow rate of the raw wastewater being 0.2. At the moment, a feeding heater is required to be added between the feeding and discharging heat exchanger and the reactor to make up for the problem that the raw material wastewater cannot be preheated to the inlet temperature required by the reaction due to the lower outlet temperature of the reactor. Not only increases the equipment investment, but also needs to provide 46kW extra heat per ton of waste water.
Claims (11)
1. The acrylonitrile device wastewater treatment method comprises the following steps:
mixing acrylonitrile device wastewater raw materials and oxygen-containing gas, then feeding the mixture into a feeding and discharging heat exchanger, carrying out heat exchange and temperature rise, then feeding the mixture into a catalytic wet oxidation reactor, and carrying out heat exchange and temperature reduction on the obtained reaction discharge wastewater through the feeding and discharging heat exchanger (preferably, through a secondary temperature reduction unit) to obtain treated wastewater;
the COD value of the raw material wastewater is 20000mg/L to 300000 mg/L;
a heat removal bundle pipe is arranged in the catalytic wet oxidation reactor, heat removal water with set flow is introduced into the bundle pipe, and a catalyst bed layer is arranged outside the bundle pipe;
the total flow of the heat removing water is L, the flow of the raw material wastewater is F, and the two satisfy the following relational expression:
L/F is (0.05-0.09) multiplied by the COD value of the raw material wastewater/10000-0.175.
2. The method for treating acrylonitrile plant wastewater according to claim 1, wherein the inlet temperature of the catalytic wet oxidation reactor is 200 to 250 ℃, and/or the reaction pressure is 8 to 15MPaG, and/or the reaction temperature is 35 to 60 ℃.
3. The method for treating the acrylonitrile plant wastewater as claimed in claim 1, wherein the secondary cooling unit comprises a heat recoverer for recovering heat and/or a discharge cooler for cooling; optionally, the treated wastewater enters a gas-liquid separation tank for gas-liquid separation.
4. The method according to claim 1, wherein the heat removal water is introduced into the heat removal bundle pipe in the reactor when the COD value of the raw material wastewater is greater than 35000 mg/L.
5. The method for treating acrylonitrile plant wastewater according to claim 1, wherein the COD value of the raw material wastewater is 35000mg/L to 300000 mg/L; preferably 50000mg/L to 200000 mg/L.
6. The method for treating acrylonitrile plant wastewater according to claim 1, wherein the pressure of the heat-removing water is 1.2 to 3.0MPaG, and the heat is absorbed by the reaction and vaporized into steam.
7. The method for treating acrylonitrile plant wastewater according to claim 1, wherein the inlet temperature of the catalytic wet oxidation reactor is 210 to 240 ℃, and/or the reaction pressure is 9 to 13MPaG, and/or the reaction temperature is 40 to 55 ℃.
8. The method for treating acrylonitrile plant wastewater according to claim 1, wherein the volume space velocity of the catalytic wet oxidation reaction is 0.2-2.0 h-1Preferably 0.5 to 1.5 hours-1。
9. The method according to claim 1, wherein the amount of oxygen in the raw material of acrylonitrile plant wastewater prior to the oxygen-containing gas is 1.1 to 1.3 times the theoretical oxygen consumption based on the COD value of the raw material wastewater.
10. The method for treating acrylonitrile plant wastewater according to claim 1, wherein the oxygen-containing gas is air, oxygen or a mixture of air and oxygen.
11. The method for treating acrylonitrile plant wastewater according to claim 1, wherein the catalytic wet oxidation catalyst is at least one of a composite metal oxide catalyst and a noble metal-supported catalyst.
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