CN111115789B - Method for treating refined waste water in acrylonitrile production process - Google Patents
Method for treating refined waste water in acrylonitrile production process Download PDFInfo
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- CN111115789B CN111115789B CN201811275739.8A CN201811275739A CN111115789B CN 111115789 B CN111115789 B CN 111115789B CN 201811275739 A CN201811275739 A CN 201811275739A CN 111115789 B CN111115789 B CN 111115789B
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention relates to a method for treating refined wastewater in an acrylonitrile production process, which mainly solves the problems of complex process, high operation cost and serious environmental pollution when the refined wastewater is treated by the prior art. The invention adopts the following steps: the acrylonitrile refined waste water and oxygen-containing gas enter a catalytic wet oxidation reaction zone after heat exchange and/or preheating, a treated material is obtained under the action of a catalyst, one part of the oxygen-containing gas enters from a refined waste water raw material inlet, and the rest part of the oxygen-containing gas enters into the reaction zone from the bottom of each section of catalyst bed layer in a mode of gradually increasing the air input.
Description
Technical Field
The invention relates to a method for treating refined wastewater in an acrylonitrile production process.
Background
Acrylonitrile is an important organic chemical basic raw material, and is mainly used for producing chemical products such as acrylic fiber, acrylonitrile-butadiene-styrene (ABS), polyacrylonitrile, acrylamide, nitrile rubber and the like, and the byproduct acetonitrile is an excellent solvent and an organic synthesis intermediate. The acrylonitrile production process is subjected to a cyanoethanol process and an acetylene process. At present, the production method at home and abroad is mainly an acrylic ammoniation oxidation method. In the above-mentioned acrylonitrile production process, the wastewater of the apparatus mainly comprising the quench tower wastewater and the refined wastewater is generated, and these wastewaters are highly toxic, highly colored and complicated in composition.
The COD value of the refined wastewater in the wastewater of the device is 10000-50000 mg/L. At present, the method of multi-effect evaporation concentration is mostly adopted for the treatment of acrylonitrile refining wastewater. The evaporated condensate is treated in a biochemical system, and the residual liquid and the waste water at the lower section of the quench tower are incinerated together. The disadvantages of this process route are: on one hand, the waste water contains high polymers, so that the multi-effect evaporator is blocked frequently, and the long-period operation of the device is influenced; on the other hand, the incineration belongs to a high energy consumption process, and SO is generated in the incineration process 2 、NO X And the gas causes secondary pollution to the environment. Therefore, a method for effectively treating the refining waste in the acrylonitrile production process is developedThe water method ensures that the treated wastewater meets the environmental protection requirement, and the realization of the green production of the acrylonitrile device is very important.
CN103663630A discloses an acrylonitrile wastewater electrolysis treatment method, comprising the following steps: (1) Adding a flocculating agent and a coagulant aid into the acrylonitrile wastewater, wherein the concentration of the flocculating agent is 20-80 mg/L; (2) Then entering a low-speed stirring flocculation reaction tank for reaction for 1-4 h; (3) entering a gravity settling tank after coagulation reaction; (4) Mixing the supernatant after precipitation with saturated saline of sodium chloride, and controlling the concentration of the added wastewater sodium chloride to be 1000-6000 mg/L according to the concentration of pollutants in the wastewater; (5) The mixed wastewater enters a stirring and mixing tank, so that the wastewater is uniformly mixed; (6) And lifting the effluent of the stirring and mixing tank by a pump to enter a closed reinforced electrolysis reactor, controlling the pressure of the electrolysis reactor to be less than 0.5MPa, setting overpressure protection, reacting for 3-10 hours, and discharging the effluent after the electrolysis reaches the standard. CN103420531A discloses a method for comprehensively treating waste water from acrylonitrile production, which comprises mixing waste water from refining and quenching acrylonitrile produced by propylene or propane ammoxidation at 200-300 deg.C under 4-10 MPa for 1-200 min, and passing the mixture through a wet oxidation reactor to remove organic substances in the waste water and to increase COD value of the waste water<500mg/l, then enters a distillation tower, is neutralized by alkali in the tower, and evaporates ammonia in the wastewater under the conditions of 60-150 ℃ and 0.05-0.15 MPa to ensure ammonia nitrogen<20mg/l. CN101422700A discloses a chemical cleaning method of an ultrafiltration membrane, which aims at the ultrafiltration membrane for treating PTA refined wastewater, and comprises the following steps in sequence: a. preparing an acid washing solution, and positively washing the ultrafiltration membrane component; the acid washing solution contains citric acid and sodium bisulfite; b. preparing alkaline washing liquor, and positively washing the ultrafiltration membrane component; the alkaline washing liquid contains sodium hypochlorite, and the pH of the washing liquid is adjusted to be alkaline by alkali. CN103420473A discloses a method for treating waste water from acrylonitrile refining process, which comprises mixing waste water from acrylonitrile refining process of propylene or propane ammoxidation production with a gas containing simple substance oxygen at 260-350 deg.C, 7-18 MPa and 1-200 min of retention timeA wet oxidation reactor for removing organic substances in the wastewater to ensure the COD value of the wastewater<500mg/l, wherein the used catalyst comprises the following components in parts by weight: a) 90 to 99.9 portions of TiO 2 、Al 2 O 3 MgO or ZrO 2 At least one oxide support; and b) 0.1 to 5 parts of at least one metal or oxide selected from Pt, pd, ru and Ir supported thereon.
Disclosure of Invention
The invention relates to a method for treating refined wastewater in an acrylonitrile production process. The invention aims to solve the technical problems of complex process, high operation cost and serious environmental pollution when treating refined wastewater in the prior art. Provides a new method for treating refined wastewater in the production process of acrylonitrile. When the method is used for treating refined wastewater, the method has the characteristics of simple process flow, high COD removal rate, byproduct heat, environmental protection and high economic benefit.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: the method for treating the refined wastewater in the acrylonitrile production process comprises the following steps:
after heat exchange and/or preheating of acrylonitrile refined wastewater and oxygen-containing gas, the acrylonitrile refined wastewater and the oxygen-containing gas pass through a catalyst bed layer of a catalytic wet oxidation reaction zone to obtain a treated material;
the catalytic wet oxidation reaction zone comprises at least one adiabatic fixed bed reactor, and each adiabatic fixed bed reactor comprises at least one section of catalyst bed layer; the serial numbers of catalyst bed layers passing through the catalytic wet oxidation reaction zone along the material flow direction are sequentially 1 st, 2 nd, 8230, i nd, 8230, n-1 th and n th sections; one part of oxygen-containing gas enters from the raw material inlet of the refined wastewater, and the rest part of the oxygen-containing gas enters from the bottom of each section of catalyst bed layer respectively in n strands; the air input of the oxygen-containing gas corresponding to the serial number of the catalyst bed layers is V respectively 1 、V 2 、…、V i 、…V n-1 、V n In which V is 1 <V 2 <…<V i <…V n-1 <V n 。
In the technical scheme, oxygen-containing gas enters from the bottoms of two adjacent sections of catalyst bed layersAir inflow V of body i 、V i+1 There are the following relationships between: v i+1 ＝(1.01～4.0)V i More preferably, V i+1 ＝(1.01～3.0)V i 。
In the technical scheme, the COD value of the fed refined wastewater is 10000 mg/L-50000 mg/L, and the removal rate of the treated COD is more than 95%.
In the above technical solution, the catalytic wet oxidation reaction zone includes at least one adiabatic fixed bed reactor, and the specific number is not particularly limited. For example, but not limited to, adiabatic fixed bed reactors having from 1 to 3, such as 1, 2, or 3. A steam generator or a heat recoverer can be arranged between two adjacent heat-insulating fixed bed reactors, and the waste water discharged from the previous heat-insulating fixed bed reactor can enter the next heat-insulating fixed bed reactor after being subjected to heat recovery and temperature reduction through the steam generator or the heat recoverer.
In the above technical scheme, each adiabatic fixed bed reactor comprises at least one section of catalyst bed layer, and the number of the specific sections is not particularly limited. For example, but not limited to, 1 to 4 stages, such as 1, 2, 3, or 4 stages, of catalyst beds contained in each adiabatic fixed bed reactor.
In the technical scheme, the total number n of the catalyst beds in the catalytic wet oxidation reaction zone is not more than 8.
In the above technical scheme, the contact mode of the feed quenching wastewater and the oxygen-containing gas in the catalytic wet oxidation reaction zone is preferably countercurrent.
In the technical scheme, the air input of the oxygen-containing gas entering from the raw material inlet of the refined wastewater is not more than 25% of the total air input, and the rest gas enters from the bottom of each section of catalyst bed layer.
In the technical scheme, the oxygen amount in the oxygen-containing gas is 1.0-1.4 times of the theoretical oxygen consumption required by the COD value of the fed refined wastewater.
In the technical scheme, the adiabatic fixed bed reactors have the same and/or different specifications and sizes, and the catalyst beds in all the sections are filled with the same and/or different types and quantities of catalysts.
In the above technical solution, the catalytic wet oxidation catalyst is at least one of a composite metal oxide catalyst and a noble metal supported catalyst.
In the above technical solution, the oxygen-containing gas is air, oxygen or a mixture of air and oxygen.
In the technical scheme, the reaction temperature of the catalytic wet oxidation reaction is preferably 180-320 ℃, and more preferably 200-300 ℃; the reaction pressure is preferably 6 to 15MPaG, more preferably 8 to 12MPaG; the volume space velocity is preferably 0.2-2.0 h -1 . More preferably 0.5 to 1.5 hours -1 。
The invention adopts the catalytic wet oxidation technology to treat the refined wastewater in the acrylonitrile production process, thereby avoiding the problems of complex process, high operation cost and serious environmental pollution when the refined wastewater is treated by adopting a multi-effect evaporation concentration method at present; the reaction progress degree of each adiabatic reaction zone is optimized and improved by adjusting the air input of the oxygen-containing gas before entering the catalytic wet oxidation reaction zone and in each catalyst bed layer; meanwhile, a steam generator or a heat recoverer is arranged between two adjacent heat-insulating fixed bed reactors, so that heat generated by reaction is recovered, the feeding requirement of the last reactor for discharging wastewater to enter the next reactor to continue reaction is met, high-efficiency treatment of refined wastewater is realized, the whole catalytic wet oxidation reaction zone is ensured to be in a stable, mild and controllable state, the treatment effect of the refined wastewater is improved, the process is simple, the heat is generated as a byproduct, the environmental protection and economic benefits are high, industrialization is easy to realize, and a better technical effect is achieved.
Drawings
FIG. 1 and FIG. 2 are schematic views of the process flow of the method for treating wastewater from the production of acrylonitrile according to the present invention.
In the figures 1 and 2, 1 is a refined wastewater raw material, 2 is an oxygen-containing gas feed, 3 is a catalytic wet oxidation reaction discharge, 4 is non-condensable gas, 5 is treated wastewater, 6 is reaction waste gas, R1 and R2 are catalytic wet oxidation adiabatic reactors, E1 is a feed and discharge heat exchanger, E2 is a gas preheater, E3 is a steam generator or a heat recoverer, E4 is a discharge cooler, D1 is a product gas-liquid separation tank, and D2 is an intermediate product gas-liquid separation tank.
According to the process shown in fig. 1, a refined wastewater raw material 1 enters a catalytic wet oxidation adiabatic reactor R1 after being subjected to heat exchange and temperature rise through a feeding and discharging heat exchanger E1, and a reaction discharge material of the R1 enters a catalytic wet oxidation adiabatic reactor R2 after being subjected to heat exchange and temperature drop through a steam generator or a heat recoverer E3. Reaction off-gas 6 is discharged at the upper part of each reactor. And the reaction discharge 3 of the R2 enters a gas-liquid separation tank D1 after being subjected to heat exchange and temperature reduction by a feeding and discharging heat exchanger E1 and cooled by a discharge cooler E5. The top of the gas-liquid separation tank D1 is discharged with non-condensable gas 4, and the bottom is discharged with treated wastewater 5. The oxygen-containing gas feed 2 is divided into a plurality of strands and respectively enters from the raw material inlet of the refined wastewater and the bottom of each section of catalyst bed layer of the catalytic wet oxidation adiabatic reactors R1 and R2 by respectively and independently setting the air input. The flow shown in fig. 2 is substantially similar to that of fig. 1, with the main differences that: in the flow scheme shown in FIG. 2, the raw purification wastewater is operated in cocurrent with the oxygen-containing gas.
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 fed refined wastewater is 11028mg/L, the catalytic wet oxidation reaction zone comprises 1 adiabatic fixed bed reactor, the reactor comprises 2 sections of catalyst bed layers, the 1 st section of catalyst bed layer is filled with a composite metal oxide catalyst, and the 2 nd section of catalyst bed layer is filled with a noble metal loaded catalyst; the total volume space velocity is 2.0h -1 The inlet temperature of the reactor was 240 ℃ and the inlet pressure was 7.6MPaG; the oxygen-containing gas adopts air, and the amount of the air is 1.1 times of the theoretical oxygen consumption required by the COD value of the fed refined wastewater; the gas quantity entering from the raw material inlet of the refined wastewater is 24 percent of the total air input quantity, the gas quantity entering from the bottoms of the catalyst bed layers of the 1 st section and the 2 nd section are respectively 18 percent and 58 percent of the total air input quantity, and the COD removal rate of the obtained refined wastewater is 97.3 percent.
[ example 2 ]
As shown in fig. 1, the COD value of the fed refined wastewater is 35372mg/L, the catalytic wet oxidation reaction zone comprises 3 adiabatic fixed bed reactors, the 1 st reactor comprises 3 catalyst beds, the 1 st and 2 nd catalyst beds are filled with composite metal oxide catalysts, the 3 rd catalyst bed is filled with noble metal supported catalysts, and the latter two reactors both comprise 1 catalyst bed and are filled with noble metal supported catalysts; the total volume space velocity is 0.5h -1 The inlet temperature of each reactor was 210 ℃ and the inlet pressure of the 1 st reactor was 9.8MPaG; 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 fed refined wastewater; the gas quantity entering from the refined wastewater raw material inlet is 10% of the total air input, and the gas quantity entering from the bottom of the catalyst bed layers from the 1 st section to the 5 th section is 11%, 14%, 17%, 21% and 27% of the total air input respectively; the removal rate of COD of the obtained refined wastewater was 97.5%.
[ example 3 ]
As shown in figure 1, the COD value of the fed refined wastewater is 48457mg/L, the catalytic wet oxidation reaction zone comprises 3 adiabatic fixed bed reactors, each reactor comprises 2 sections of catalyst beds, the catalyst beds from the 1 st section to the 3 rd section are filled with composite metal oxide catalysts, and the catalyst beds from the 4 th section to the 6 th section are filled with noble metal supported catalysts; the total volume space velocity is 0.8h -1 The inlet temperature of each reactor was 220 ℃ and the inlet pressure of the 1 st reactor was 11.6MPaG; oxygen is adopted as oxygen-containing gas, and the amount of oxygen is 1.4 times of the theoretical oxygen consumption required by the COD value of the fed refined wastewater; the gas quantity entering from the raw material inlet of the refined wastewater is 16% of the total air input quantity, the gas quantity entering from the bottom of the catalyst bed layers from the 1 st section to the 6 th section is respectively 8%, 11%, 12%, 15%, 17% and 21% of the total air input quantity, and the COD removal rate of the obtained refined wastewater is 98.4%.
[ example 4 ]
As shown in FIG. 1, the COD value of the feed refining wastewater was 28509mg/L, and the catalytic wet oxidation reaction zone included 2 adiabatic solidsA fixed bed reactor, wherein the 1 st reactor comprises 1 section of catalyst bed layer and is filled with composite metal oxide catalyst, and the 2 nd reactor comprises 2 sections of catalyst bed layers and is filled with noble metal supported catalyst; the total volume space velocity is 1.5h -1 The inlet temperature of the 1 st reactor was 210 ℃ and the inlet pressure of the 1 st reactor was 8.7MPaG; the oxygen-containing gas adopts air, and the amount of the air is 1.2 times of the theoretical oxygen consumption required by the COD value of the fed refined wastewater; the gas quantity entering from the raw material inlet of the refined wastewater is 30 percent of the total gas input quantity, the gas quantity entering from the bottom of the catalyst bed layers from the 1 st section to the 3 rd section is respectively 13 percent, 18 percent and 39 percent of the total gas input quantity, and the COD removal rate of the obtained refined wastewater is 97.9 percent.
[ example 5 ]
According to the figure 1, the COD value of the fed refined wastewater is 15844mg/L, the catalytic wet oxidation reaction zone comprises 1 adiabatic fixed bed reactor, 4 sections of catalyst beds are arranged in the reactor, the catalyst beds from the 1 st section to the 3 rd section are filled with composite metal oxide catalysts, and the catalyst bed layer from the 4 th section is filled with noble metal supported catalysts; the total volume space velocity is 1.2h -1 The inlet temperature of the reactor was 220 ℃ and the inlet pressure was 10.5MPaG; 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 fed refined wastewater; the gas quantity entering from the raw material inlet of the refined wastewater is 0% of the total air input quantity, the gas quantity entering from the bottom of the catalyst bed layers from the 1 st section to the 4 th section is respectively 11%, 24%, 25% and 40% of the total air input quantity, and the COD removal rate of the obtained refined wastewater is 99.1%.
[ example 6 ]
As shown in fig. 2, the COD value of the fed refined wastewater is 20311mg/L, the catalytic wet oxidation reaction zone comprises 2 adiabatic fixed bed reactors, the 1 st reactor comprises 1 section of catalyst bed layer and is filled with composite metal oxide catalyst, and the 2 nd reactor comprises 1 section of catalyst bed layer and is filled with noble metal supported catalyst; the total volume space velocity is 1.0h -1 The inlet temperature of the 1 st reactor was 230 ℃ and the inlet pressure of the 1 st reactor was 9.2MPaG; 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 fed refined wastewater; the gas quantity entering from the raw material inlet of the refined wastewater is 7% of the total air input quantity, the gas quantity entering from the bottoms of the catalyst bed layers of the 1 st section and the 2 nd section is respectively 38% and 55% of the total air input quantity, and the COD removal rate of the obtained refined wastewater is 98.7%.
[ COMPARATIVE EXAMPLE 1 ]
According to the conditions and steps of the example 1, other conditions are kept unchanged, the gas amount entering from the bottom of the catalyst bed layers of the 1 st section and the 2 nd section is respectively 58 percent and 18 percent of the total air input amount, and the COD removal rate of the obtained refined wastewater is 94.2 percent.
[ COMPARATIVE EXAMPLE 2 ]
According to the conditions and steps of example 2, the other conditions are kept unchanged, and the gas quantities entering from the bottom of the catalyst bed layers from the 1 st section to the 5 th section are respectively 27%, 21%, 17%, 14% and 11% of the total gas inflow; the COD removal rate of the obtained refined wastewater is 92.3 percent.
[ COMPARATIVE EXAMPLE 3 ]
According to the conditions and steps of the example 3, the other conditions are kept unchanged, the gas quantity entering from the bottom of the catalyst bed layers from the 1 st section to the 6 th section is 14 percent of the total gas input quantity respectively, and the COD removal rate of the obtained refined wastewater is 96.0 percent.
Claims (11)
1. The method for treating the refined wastewater in the acrylonitrile production process comprises the following steps:
acrylonitrile refined wastewater and oxygen-containing gas enter a catalytic wet oxidation reaction zone after heat exchange and/or preheating, and treated materials are obtained under the action of a catalyst;
the catalytic wet oxidation reaction zone comprises at least one adiabatic fixed bed reactor, and each adiabatic fixed bed reactor comprises at least one section of catalyst bed layer; the serial numbers of catalyst beds passing through the catalytic wet oxidation reaction zone along the material flow direction are sequentially 1 st, 2 nd, 8230st, i nd, 8230st and n th sections; one part of oxygen-containing gas enters from a raw material inlet of the refined wastewater, and the rest part of the oxygen-containing gas is divided into n strands and respectively enters from the bottom of each section of catalyst bed layer; and withThe air input of the oxygen-containing gas corresponding to the serial number of the catalyst bed layers is sequentially F 1 、F 2 、…、F i 、…、F n In which F i+1 ＝(1.01～4.0)F i ；
A steam generator or a heat recoverer is arranged between two adjacent heat-insulating fixed bed reactors in the catalytic wet oxidation reaction zone;
the contact mode of the fed refined wastewater and the oxygen-containing gas in the catalytic wet oxidation reaction zone is countercurrent;
the air input of the oxygen-containing gas entering from the raw material inlet of the refined wastewater is not more than 25 percent of the total air input, and the rest gas enters from the bottom of each section of catalyst bed layer.
2. The method according to claim 1, wherein the amount F of the oxygen-containing gas introduced from the bottoms of the two adjacent catalyst beds is set to the amount F of the oxygen-containing gas introduced from the bottoms of the two adjacent catalyst beds i 、F i+1 There are the following relationships between: f i+1 ＝(1.01～3.0)F i 。
3. The method according to claim 1, wherein the COD value of the fed refining wastewater is 10000mg/L to 50000mg/L.
4. The method for treating wastewater from the purification of acrylonitrile production as claimed in claim 1, wherein the number of adiabatic fixed bed reactors in the catalytic wet oxidation reaction zone is 1 to 3.
5. The method of treating waste water from the purification of acrylonitrile production according to claim 1, wherein the number of stages of the catalyst bed in each adiabatic fixed bed reactor is 1 to 4.
6. The method of treating waste water from the purification of acrylonitrile production as claimed in claim 1, wherein the total number of stages n of the catalyst bed in the catalytic wet oxidation reaction zone is not more than 8.
7. The method according to claim 1, wherein the amount of oxygen contained in the oxygen-containing gas is 1.0 to 1.4 times the theoretical oxygen consumption as calculated on the COD value of the fed purified wastewater.
8. The method according to claim 1, wherein the adiabatic fixed-bed reactors have the same and/or different specifications, and the catalyst beds in the respective stages are packed with the same and/or different kinds and amounts of catalysts.
9. The method 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.
10. The method according to claim 1, wherein the oxygen-containing gas is air, oxygen or a mixture of air and oxygen.
11. The method according to claim 1, wherein the reaction temperature of the catalytic wet oxidation reaction is 180 to 320 ℃, the reaction pressure is 6 to 15MPaG, and the volume space velocity is 0.2 to 2.0h -1 。
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| US5192453A (en) * | 1992-01-06 | 1993-03-09 | The Standard Oil Company | Wet oxidation process for ACN waste streams |
| CN103663665A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Wastewater treatment method for acrylonitrile production and refining process |
| CN104108780A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Method for treating wastewater in acrylonitrile production refining process |
| CN105084506A (en) * | 2014-05-14 | 2015-11-25 | 中国石油化工股份有限公司 | Method for reducing COD of waste water by wet type oxidation |
| CN108480375A (en) * | 2018-04-03 | 2018-09-04 | 中国环境科学研究院 | Thermal desorption in situ-oxidation the repair system and restorative procedure in organic contamination place |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5192453A (en) * | 1992-01-06 | 1993-03-09 | The Standard Oil Company | Wet oxidation process for ACN waste streams |
| CN103663665A (en) * | 2012-09-05 | 2014-03-26 | 中国石油化工股份有限公司 | Wastewater treatment method for acrylonitrile production and refining process |
| CN104108780A (en) * | 2013-04-16 | 2014-10-22 | 中国石油化工股份有限公司 | Method for treating wastewater in acrylonitrile production refining process |
| CN105084506A (en) * | 2014-05-14 | 2015-11-25 | 中国石油化工股份有限公司 | Method for reducing COD of waste water by wet type oxidation |
| CN108480375A (en) * | 2018-04-03 | 2018-09-04 | 中国环境科学研究院 | Thermal desorption in situ-oxidation the repair system and restorative procedure in organic contamination place |
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