CN114873823A - Coking wastewater comprehensive treatment device and technological method - Google Patents
Coking wastewater comprehensive treatment device and technological method Download PDFInfo
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- CN114873823A CN114873823A CN202210649785.XA CN202210649785A CN114873823A CN 114873823 A CN114873823 A CN 114873823A CN 202210649785 A CN202210649785 A CN 202210649785A CN 114873823 A CN114873823 A CN 114873823A
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- 239000002351 wastewater Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000004939 coking Methods 0.000 title claims abstract description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 136
- 239000002904 solvent Substances 0.000 claims abstract description 114
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 54
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000011084 recovery Methods 0.000 claims abstract description 36
- 239000002994 raw material Substances 0.000 claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 238000010992 reflux Methods 0.000 claims abstract description 20
- 238000000605 extraction Methods 0.000 claims abstract description 18
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims abstract description 7
- 238000009833 condensation Methods 0.000 claims abstract description 5
- 230000005494 condensation Effects 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 23
- 239000002253 acid Substances 0.000 claims description 20
- 239000012071 phase Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 13
- 239000008213 purified water Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 6
- 238000004581 coalescence Methods 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000010865 sewage Substances 0.000 claims description 4
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 101150115560 mpaG gene Proteins 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 claims 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 7
- 238000004821 distillation Methods 0.000 abstract description 5
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 3
- 238000012824 chemical production Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 14
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000000571 coke Substances 0.000 description 3
- 238000005204 segregation Methods 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 235000013824 polyphenols Nutrition 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- XABJJJZIQNZSIM-UHFFFAOYSA-N azane;phenol Chemical compound [NH4+].[O-]C1=CC=CC=C1 XABJJJZIQNZSIM-UHFFFAOYSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000295 fuel oil Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/10—Treatment of water, waste water, or sewage by heating by distillation or evaporation by direct contact with a particulate solid or with a fluid, as a heat transfer medium
-
- 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
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
-
- 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
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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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
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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- 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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
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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
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
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Abstract
A coking wastewater comprehensive treatment device and a process method relate to the field of chemical production, and in order to solve the problems of substandard treatment, long flow and high energy consumption of substances such as ammonia nitrogen, H2S, CO2, phenol and the like in the prior device and process treatment wastewater, the invention realizes the effects of separating gases such as H2S, CO2 and the like in the wastewater according to the process flow of pretreatment, ammonia distillation, extraction and solvent recovery by the connection design of a pretreatment device, a raw material buffer tank, an ammonia distillation tower, a dephenolization tower, a solvent stripping tower, a solvent recovery tower, a three-stage cooling fractional condensation device, a feed preheater a, a feed preheater b, a feed preheater c and a solvent cooler solvent reflux tank, recovering NH3, further recovering phenol products in the wastewater and reusing or directly performing biochemical treatment on the qualified water after treatment.
Description
Technical Field
The invention belongs to the field of chemical production, and particularly relates to a coking wastewater comprehensive treatment device and a process method.
Background
The main product is coke which is a high-quality fuel obtained by dry distillation of coal at a high temperature of more than 1000 ℃, and the coke can be used as a fuel for blast furnace smelting, non-ferrous metal smelting, water gas production and the like. 80% of coke products in China are used in the steel industry.
The coking wastewater is mainly residual ammonia waste liquid generated by pyrolysis and raw gas cooling, has complex water quality, various components and higher pollutant concentration, and contains elementary phenol, polyphenol, oil substances and the like besides inorganic substances such as NH3, H2S, CO2 and the like. The coking plant widely uses common biochemical treatment, and ammonia and phenol in the coking wastewater are difficult to be treated by the common biochemical technology, so that COD, BOD and other pollutants at a treated water outlet of the coking wastewater are difficult to reach the standard.
The traditional ammonia distillation device generally adopts a single-tower total-removal or double-tower process, wherein the single-tower total-removal process is to completely remove ammonia gas and acid gas by using an ammonia distillation tower and directly prepare ammonia water by condensation at the tower top, and has the advantages of less equipment, less investment and low defect of low concentration and poor quality of the prepared ammonia water; the double-tower process is to remove acid gas through the deacidification tower and then remove ammonia gas in the ammonia still, and has the advantages of high concentration of the prepared ammonia water, good quality, long process and high energy consumption.
Disclosure of Invention
In order to thoroughly and cleanly remove substances such as ammonia nitrogen, H2S, CO2 and phenol in the wastewater through multi-stage separation treatment, purified water is obtained after purification, and the purified water enters the next working procedure for recycling; the invention provides a device and a process method for comprehensively treating coking wastewater, which have the advantages that the effect of directly recovering products such as phenol, ammonia and the like is realized:
a coking wastewater comprehensive treatment device comprises a pretreatment device, a raw material buffer tank, a booster pump, an ammonia still, a dephenolizing tower, a solvent stripping tower, a solvent recovery tower, a three-stage cooling and dephlegmating device, a feeding preheater a, a feeding preheater b, a feeding preheater c, a solvent cooler and a solvent reflux tank;
the pretreatment device is connected with a raw material cache tank, the raw material cache tank is connected to the middle part of an ammonia still through a booster pump and a feeding preheater a in sequence, the bottom end of the ammonia still is connected to the upper part of a dephenolizing tower through the feeding preheater a, the middle part of the ammonia still is connected with a three-stage cooling and segregating device, and the bottom end of the three-stage cooling and segregating device is connected to the raw material cache tank;
the bottom end of the dephenolizing tower is connected with the middle part of the solvent stripping tower through a feeding preheater b, and the top of the dephenolizing tower is connected with the middle part of the solvent recovery tower through a feeding preheater c;
the bottom end of the solvent stripping tower is connected out through a feeding preheater b, and the top of the solvent stripping tower is connected with a solvent reflux tank through a solvent cooler on one hand and is connected with the top of a solvent recovery tower on the other hand;
the bottom end of the solvent recovery tower is connected out through a feed preheater c;
the bottom of the solvent reflux tank is connected to the bottom of the dephenolizing tower;
the pretreatment device comprises a cyclone separation and solid removal device, an electrochemical suspension removal device and a coalescence oil removal device.
The tertiary cooling and segregating device comprises: the system comprises a first-stage condenser, a second-stage condenser, a third-stage condenser, a first-stage dephlegmator, a second-stage dephlegmator and a third-stage dephlegmator, wherein one end of the first-stage condenser is connected with an ammonia still, and the other end of the first-stage condenser is connected with the middle part of the first-stage dephlegmator; the top end of the first-stage dephlegmator is connected with the middle part of the second-stage dephlegmator through a second-stage condenser, the top end of the second-stage dephlegmator is connected with the middle part of the third-stage dephlegmator through a third-stage condenser, and the bottom ends of the first-stage dephlegmator, the second-stage dephlegmator and the third-stage dephlegmator are connected to the raw material cache tank.
A process method for the comprehensive treatment of coking wastewater,
the method comprises the following steps:
the first step is as follows: organic wastewater from a front working section of an enterprise firstly enters a pretreatment device, and colloid, fine suspended matters and oil in the organic wastewater are effectively removed through cyclone separation and solid removal, electrochemical suspension removal and coalescence oil removal, so that oil and impurities in the wastewater are removed;
the second step is that: the pretreated wastewater enters a raw material cache tank, the outlet pressure of a booster pump is 1.5 +/-0.2 mpaG, the wastewater enters an ammonia still after being pressurized by the booster pump and exchanging heat with the tower bottom liquid of the ammonia still through a feeding preheater a, acid gases such as CO2 and H2S enter an ammonia still from an acid gas pipeline at the top of the ammonia still, ammonia-containing steam collected from a lateral line is cooled step by step through a first-stage condenser, a second-stage condenser and a third-stage condenser respectively, then gas-liquid separation is carried out on the first-stage partial condenser, the second-stage partial condenser and the third-stage partial condenser, the separated liquid phase returns to the raw material cache tank again, and ammonia gas separated from the third-stage cooling partial condenser is discharged from a device;
the third step: the material that comes out from ammonia still tower cauldron enters dephenolization tower top of the tower after feeding preheater a cools off, contacts with the extractant countercurrent flow that gets into from dephenolization tower cauldron, extracts the phenol in the waste water, and the extraction condition is: the temperature is selected to be 50-70 ℃ so as to reduce the consumption of cooling water; and (3) extraction: the volume ratio of the oil phase to the water phase of the extractant is as follows: 1: 4; the extraction stage number is as follows: in order to reduce the total phenol content in the sewage to below 350mg/L, 4-5 grades are adopted for extraction. (ii) a
The fourth step: the raffinate phase from the bottom of the dephenolizing tower and the tower bottom liquid of the solvent stripping tower enter the solvent stripping tower after heat exchange through a feeding preheater b, the solvent stripped from the top of the solvent stripping tower is cooled to 40-45 ℃ through a solvent cooler and then enters a solvent reflux tank, and the purified water from the tower bottom of the solvent stripping tower is discharged out of the device after being heated and fed through the feeding preheater b;
the fifth step: the extraction phase coming out of the tower top of the dephenolizing tower and the tower bottom liquid of the solvent recovery tower enter a solvent recovery tower after heat exchange through a feeding preheater c, the solvent is recovered through the rectification principle, the solvent coming out of the tower top of the solvent recovery tower is cooled to 40-45 ℃ through a solvent cooler and then enters a solvent reflux tank, then returns to the dephenolizing tower for utilization, and the crude phenol product coming out of the tower bottom of the solvent recovery tower passes through the feeding preheater c and then is discharged out of the device.
The solvent reflux tank can also be directly supplemented with MIBK methyl isobutyl ketone from the outside.
The tower bottom liquid of the ammonia still is high-temperature wastewater from which acid gas and ammonia gas are removed at 163 +/-5 ℃.
The tower bottom liquid of the solvent stripping tower is high-temperature purified water from which acid gas, ammonia gas and phenol are removed at the temperature of 107 +/-5 ℃, wherein NH3 is less than 100mg/L, and H2S is less than 30 mg/L; phenol is less than 350mg/L.
The tower bottom liquid of the solvent recovery tower is high-temperature crude phenol product phenol at the temperature of 204 +/-5 ℃, and the phenol is more than 85 percent.
The invention has the advantages that:
the original process wastewater is collected and then directly enters an ammonia still for evaporation and concentration, and an ammonia water product is directly obtained after condensation from the top of the tower, so that the concentration of the ammonia water product is low; acid gases such as H2S, CO2 and the like can also enter the ammonia water product together, so that the quality of the ammonia water is influenced; the phenol content of the tower bottom liquid of the ammonia still exceeds the standard, and the biochemical treatment is directly carried out, so that the operation of a biochemical system is difficult. The device and the process method can thoroughly and cleanly remove ammonia nitrogen, H2S, CO2, phenol and other substances in the wastewater through multi-stage separation treatment, the purified qualified water enters the next process, and phenol ammonia and other products are directly recovered.
Drawings
FIG. 1 is a schematic of the present invention:
description of reference numerals: 1. a pretreatment device; 2. a raw material buffer tank; 3. a booster pump; 4. an ammonia still; 5. a dephenolizing tower; 6. a solvent stripper; 7. a solvent recovery column; 8. a first-stage condenser; 9. a first-stage dephlegmator; 10. a secondary condenser; 11. a secondary dephlegmator; 12. a third-stage condenser; 13. a third-stage dephlegmator; 14. a feed preheater a; 15. a feed preheater b; 16. a feed preheater c; 17. a solvent cooler; 18. and (5) a solvent reflux tank.
Detailed Description
The description is made with reference to fig. 1:
a coking wastewater comprehensive treatment device comprises a pretreatment device 1, a raw material buffer tank 2, a booster pump 3, an ammonia still 4, a dephenolizing tower 5, a solvent stripping tower 6, a solvent recovery tower 7, a three-stage cooling and dephlegmating device, a feeding preheater a14, a feeding preheater b15, a feeding preheater c16, a solvent cooler 17 and a solvent reflux tank 18;
the pretreatment device 1 is connected with a raw material cache tank 2, the raw material cache tank 2 is connected to the middle of an ammonia still 4 through a booster pump 3 and a feed preheater a14 in sequence, the bottom end of the ammonia still 4 is connected to the upper part of a dephenolizing tower 5 through a feed preheater a14, the middle of the ammonia still 4 is connected with a three-stage cooling and segregation device, and the bottom end of the three-stage cooling and segregation device is connected to the raw material cache tank 2;
the bottom end of the dephenolizing tower 5 is connected with the middle part of the solvent stripping tower 6 through a feed preheater b15, and the top of the dephenolizing tower 5 is connected with the middle part of the solvent recovery tower 7 through a feed preheater c 16;
the bottom end of the solvent stripping tower 6 is connected out through a feed preheater b15, and the top of the solvent stripping tower 6 is connected with the solvent reflux tank 18 through a solvent cooler 17 on one hand and is connected with the top of the solvent recovery tower 7 on the other hand;
the bottom end of the solvent recovery column 7 is tapped off through a feed preheater c 16;
the bottom of the solvent reflux tank 18 is connected to the bottom of the dephenolizing tower 5;
the pretreatment device 1 comprises a cyclone separation and solid removal device, an electrochemical suspension removal device and a coalescence oil removal device, and colloid, fine suspended matters and oil in the organic wastewater are effectively removed by adopting treatment modes of cyclone separation and solid removal, electrochemical suspension removal, coalescence oil removal and the like, so that the treated wastewater meets the requirements of a subsequent treatment system.
The tertiary cooling and segregating device comprises: the system comprises a first-stage condenser 8, a second-stage condenser 10, a third-stage condenser 12, a first-stage dephlegmator 9, a second-stage dephlegmator 11 and a third-stage dephlegmator 13, wherein one end of the first-stage condenser 8 is connected with an ammonia still 4, and the other end of the first-stage condenser is connected with the middle part of the first-stage dephlegmator 9; the top end of the first-stage dephlegmator 9 is connected with the middle part of a second-stage dephlegmator 11 through a second-stage condenser 10, the top end of the second-stage dephlegmator 11 is connected with the middle part of a third-stage dephlegmator 13 through a third-stage condenser 12, and the bottom ends of the first-stage dephlegmator 9, the second-stage dephlegmator 11 and the third-stage dephlegmator 13 are connected to the raw material cache tank 2.
A novel coking wastewater comprehensive treatment process method comprises the following steps:
the first step is as follows: organic wastewater from a front working section of an enterprise firstly enters a pretreatment device 1, and colloid, fine suspended matters and oil in the organic wastewater are effectively removed through cyclone separation solid removal, electrochemical suspension removal and coalescence oil removal, so that oil and impurities in the wastewater are removed;
the second step is that: the pretreated wastewater enters a raw material cache tank 2, the outlet pressure of a booster pump 3 is 1.5 +/-0.2 mpaG, the wastewater is pressurized by the booster pump 3 and exchanges heat with tower bottom liquid of an ammonia still 4 through a feeding preheater a14, the wastewater enters the ammonia still 4, acid gases such as CO2, H2S and the like are discharged from an acid gas pipeline at the top of the ammonia still 4, ammonia-containing steam collected from a lateral line is cooled step by step through a first-stage condenser 8, a second-stage condenser 10 and a third-stage condenser 12 respectively, gas-liquid separation is carried out in a first-stage partial condenser 9, a second-stage partial condenser 11 and a third-stage partial condenser 13, the separated liquid phase returns to the raw material cache tank 2 again, and ammonia gas separated from the third-stage cooling partial condenser is discharged from a device;
the third step: the material from the tower bottom of the ammonia still 4 enters the top of the dephenolizing tower 5 after being cooled by a feeding preheater a14, and is in countercurrent contact with an extractant entering from the tower bottom of the dephenolizing tower 5 to extract phenol in the wastewater, and the extraction conditions are as follows: the temperature is selected to be 50-70 ℃ so as to reduce the consumption of cooling water; and (3) extraction: the volume ratio of the oil phase to the water phase of the extractant is as follows: 1: 4; the extraction stage number is as follows: in order to reduce the total phenol content in the sewage to below 350mg/L, 4-5 grades are adopted for extraction. (ii) a
The fourth step: the raffinate phase from the bottom of the dephenolizing tower 5 and the tower bottom liquid of the solvent stripping tower 6 are subjected to heat exchange through a feeding preheater b15 and then enter the solvent stripping tower 6, the solvent stripped from the top of the solvent stripping tower 6 is cooled to 40-45 ℃ through a solvent cooler 17 and then enters a solvent reflux tank 18, and the purified water from the tower bottom of the solvent stripping tower 6 is heated through a feeding preheater b15 and then is discharged out of the device after being fed;
the fifth step: the extraction phase coming out from the tower top of the dephenolizing tower 5 and the tower bottom liquid of the solvent recovery tower 7 enter the solvent recovery tower 7 after heat exchange through a feeding preheater c16, the solvent is recovered through the rectification principle, the solvent coming out from the tower top of the solvent recovery tower 7 enters a solvent reflux tank 18 after being cooled to 40-45 ℃ through a solvent cooler 17, then returns to the dephenolizing tower 5 for utilization again, and the crude phenol product coming out from the tower bottom of the solvent recovery tower 7 passes through a feeding preheater c16 and then is discharged out of the device.
The solvent reflux tank 18 can also be directly supplemented with MIBK methyl isobutyl ketone, superior products from the outside.
And the tower bottom liquid of the ammonia still 4 is high-temperature wastewater from which acid gas and ammonia gas are removed at 163 +/-5 ℃.
The tower bottom liquid of the solvent stripping tower 6 is high-temperature purified water from which acid gas, ammonia gas and phenol are removed at the temperature of 107 +/-5 ℃, wherein NH3 is less than 100mg/L, and H2S is less than 30 mg/L; phenol is less than 350mg/L.
The tower bottom liquid of the solvent recovery tower 7 is high-temperature crude phenol product phenol with the temperature of 204 +/-5 ℃, and the phenol is more than 85 percent. Can also be directly supplemented from the outside.
The recovery device has the characteristics that:
1. the separation and recovery of three substances (1, acid gas 2, purified water 3 and pure ammonia) are completed in an ammonia still 4, the content of NH3 in the acid gas is less than 500ppm, and the content of the acid gas is more than 98 percent; the ammonia content of the purified water at the tower bottom of the ammonia still 4 is less than 100ppm, and the hydrogen sulfide content is less than 30 ppm; the pure ammonia gas content obtained by three-stage segregation is more than 98 percent.
2. The phenol content of the purified water from the tower bottom of the solvent stripping tower 6 is less than 350ppm, and the phenol content of the phenol product from the solvent recovery tower 7 is more than 85%.
3. A pretreatment device is added to remove light oil heavy oil and impurities in the wastewater, the load of a subsequent device is reduced, and necessary conditions are provided for stable operation of the subsequent device.
4. And an ammonia still 4 is added, and the ammonia gas and the acid gas in the wastewater are completely evaporated by adopting the process of single-tower steam stripping and side line extraction.
5. And a three-stage cooling and dephlegmating device is added, ammonia-containing steam extracted from the side line of the ammonia still 4 is gradually dephlegmated and cooled, and acid gas is further removed in the dephlegmating and cooling process, so that pure ammonia gas with the purity of more than or equal to 98% is obtained.
6. The dephenolizing tower 5 is added, so that phenolic substances in the sewage are transferred to the extracting agent through the characteristic that the solubility of phenol in the extracting agent is higher than that of phenol in water, and the removal of phenol is realized.
7. And a solvent stripping tower 6 is added, stripping is carried out on raffinate phase obtained by the dephenolizing tower 5 in the solvent stripping tower 6, and the stripped solvent is recycled after cooling.
8. And a solvent recovery tower 7 is added, an extract phase obtained by the solvent stripping tower 6 enters the solvent recovery tower 7, the solvent is separated from phenol by utilizing the rectification principle, the solvent at the top of the tower is recycled after being cooled, and a phenol product is obtained at the bottom of the tower.
9. A raw material buffer tank 2, a solvent reflux tank 18 and a booster pump 3 are added to supply raw materials to each tower, so that the subsequent system can operate more stably.
The invention provides a comprehensive treatment device and a process method for coking wastewater, which are used for separating gases such as H2S, CO2 and the like from the wastewater and recovering NH3 by the working procedures of pretreatment, ammonia distillation, extraction, solvent recovery and the like of residual ammonia water from the previous working section of a coking plant, and simultaneously further recovering phenol products in the wastewater, and reusing the treated qualified water or directly performing biochemical treatment on the treated qualified water.
Claims (8)
1. The utility model provides a coking wastewater comprehensive treatment device, includes preprocessing device (1), raw materials buffer tank (2), booster pump (3), ammonia still (4), dephenolizing tower (5), solvent stripping tower (6), solvent recovery tower (7), tertiary cooling dephlegmation device, feeding preheater a (14), feeding preheater b (15), feeding preheater c (16), solvent cooler (17), solvent backflow jar (18), its characterized in that:
the pretreatment device (1) is connected with a raw material cache tank (2), the raw material cache tank (2) is connected to the middle part of an ammonia still (4) sequentially through a booster pump (3) and a feed preheater a (14), the bottom end of the ammonia still (4) is connected to the upper part of a dephenolizing tower (5) through the feed preheater a (14), the middle part of the ammonia still (4) is connected with a three-stage cooling and fractional condensation device, and the bottom end of the three-stage cooling and fractional condensation device is connected to the raw material cache tank (2);
the bottom end of the dephenolizing tower (5) is connected with the middle part of the solvent stripping tower (6) through a feeding preheater b (15), and the top of the dephenolizing tower (5) is connected with the middle part of the solvent recovery tower (7) through a feeding preheater c (16);
the bottom end of the solvent stripping tower (6) is connected out through a feed preheater b (15), and the top of the solvent stripping tower (6) is connected with a solvent reflux tank (18) through a solvent cooler (17) on one hand and is connected with the top of a solvent recovery tower (7) on the other hand;
the bottom end of the solvent recovery tower (7) is connected out through a feed preheater c (16);
the bottom of the solvent reflux tank (18) is connected to the bottom of the dephenolizing tower (5).
2. The coking wastewater comprehensive treatment device of claim 1, which is characterized in that: the pretreatment device (1) comprises a cyclone separation and solid removal device, an electrochemical suspension removal device and a coalescence oil removal device.
3. The coking wastewater comprehensive treatment device of claim 1, which is characterized in that: the tertiary cooling and segregating device comprises: the system comprises a primary condenser (8), a secondary condenser (10), a tertiary condenser (12), a primary dephlegmator (9), a secondary dephlegmator (11) and a tertiary dephlegmator (13), wherein one end of the primary condenser (8) is connected with an ammonia still (4), and the other end of the primary condenser is connected with the middle part of the primary dephlegmator (9); the top end of the first-stage dephlegmator (9) is connected with the middle part of the second-stage dephlegmator (11) through the second-stage condenser (10), the top end of the second-stage dephlegmator (11) is connected with the middle part of the third-stage dephlegmator (13) through the third-stage condenser (12), and the bottom ends of the first-stage dephlegmator (9), the second-stage dephlegmator (11) and the third-stage dephlegmator (13) are connected to the raw material cache tank (2).
4. A novel process method for comprehensive treatment of coking wastewater is characterized by comprising the following steps:
the method comprises the following steps:
the first step is as follows: organic wastewater from a front working section of an enterprise firstly enters a pretreatment device (1), solid removal, electrochemical suspension removal and coalescent oil removal are carried out through cyclone separation, colloid, fine suspended matters and oil in the organic wastewater are effectively removed, and oil and impurities in the wastewater are removed;
the second step is that: the pretreated wastewater enters a raw material cache tank (2), the outlet pressure of a booster pump (3) is 1.5 +/-0.2 mpaG, the wastewater is pressurized by the booster pump (3) and exchanges heat with tower bottom liquid of an ammonia still (4) through a feeding preheater a (14) and then enters the ammonia still (4), acid gases such as CO2 and H2S and the like enter an acid gas pipeline discharge device at the top of the ammonia still (4), ammonia-containing steam extracted from the side line respectively passes through a primary condenser (8), a secondary condenser (10) and a tertiary condenser (12) to be cooled step by step, gas-liquid separation is carried out in a primary dephlegmator (9), a secondary dephlegmator (11) and a tertiary dephlegmator (13), the separated liquid phase returns to the raw material cache tank (2) again, and the ammonia gas separated from the tertiary cooling dephlegmator is discharged from the ammonia discharge device;
the third step: the material from the tower bottom of the ammonia still (4) enters the top of the dephenolizing tower (5) after being cooled by a feeding preheater a (14) and is in countercurrent contact with an extractant entering from the tower bottom of the dephenolizing tower (5) to extract phenol in the wastewater, and the extraction conditions are as follows: the temperature is selected to be 50-70 ℃ so as to reduce the consumption of cooling water; and (3) extraction: the volume ratio of the oil phase to the water phase of the extractant is as follows: 1: 4; the extraction stage number is as follows: 4-5 grades are adopted for extraction in order to reduce the total phenol content in the sewage to be below 350 mg/L;
the fourth step: the raffinate phase coming out of the bottom of the dephenolizing tower (5) and the tower bottom liquid of the solvent stripping tower (6) are subjected to heat exchange through a feeding preheater b (15) and then enter the solvent stripping tower (6), the solvent stripped from the top of the solvent stripping tower (6) is cooled to 40-45 ℃ through a solvent cooler (17) and then enters a solvent reflux tank (18), and the purified water coming out of the tower bottom of the solvent stripping tower (6) is heated through the feeding preheater b (15) and fed and then is discharged out of the device;
the fifth step: the extraction phase coming out of the tower top of the dephenolizing tower (5) and the tower bottom liquid of the solvent recovery tower (7) enter the solvent recovery tower (7) after heat exchange through a feeding preheater c (16), the solvent is recovered through the rectification principle, the solvent coming out of the tower top of the solvent recovery tower (7) is cooled to 40-45 ℃ through a solvent cooler (17) and then enters a solvent reflux tank (18), and then returns to the dephenolizing tower (5) for utilization, and the crude phenol product coming out of the tower bottom of the solvent recovery tower (7) passes through the feeding preheater c (16) and then is discharged out of the device.
5. The novel coking wastewater comprehensive treatment process method of claim 4, which is characterized in that: the solvent reflux tank (18) can also be directly supplemented with MIBK methyl isobutyl ketone from the outside.
6. The novel coking wastewater comprehensive treatment process method of claim 4, which is characterized in that: the tower bottom liquid of the ammonia still (4) is high-temperature wastewater from which acid gas and ammonia gas are removed at 163 +/-5 ℃.
7. The novel coking wastewater comprehensive treatment process method of claim 4, which is characterized in that: the tower bottom liquid of the solvent stripping tower (6) is high-temperature purified water from which acid gas, ammonia gas and phenol are removed at the temperature of 107 +/-5 ℃, wherein NH3 is less than 100mg/L, and H2S is less than 30 mg/L; phenol is less than 350mg/L.
8. The novel coking wastewater comprehensive treatment process method of claim 4, which is characterized in that: the tower bottom liquid of the solvent recovery tower (7) is a high-temperature crude phenol product phenol with the temperature of 204 +/-5 ℃, and the phenol is more than 85 percent.
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