CN114230099A - Treatment method of DMF (dimethyl formamide) -containing wastewater - Google Patents
Treatment method of DMF (dimethyl formamide) -containing wastewater Download PDFInfo
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- 239000002351 wastewater Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 24
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 title description 93
- 230000009615 deamination Effects 0.000 claims abstract description 52
- 238000006481 deamination reaction Methods 0.000 claims abstract description 52
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000005904 alkaline hydrolysis reaction Methods 0.000 claims abstract description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 15
- 238000005086 pumping Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 238000011084 recovery Methods 0.000 claims abstract description 9
- 239000002699 waste material Substances 0.000 claims abstract description 5
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 2
- 239000000920 calcium hydroxide Substances 0.000 claims description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000292 calcium oxide Substances 0.000 claims description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 10
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000243 solution Substances 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 5
- LFETXMWECUPHJA-UHFFFAOYSA-N methanamine;hydrate Chemical compound O.NC LFETXMWECUPHJA-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 238000004062 sedimentation Methods 0.000 description 13
- 125000002147 dimethylamino group Chemical class [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 7
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 239000004376 Sucralose Substances 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- BAQAVOSOZGMPRM-QBMZZYIRSA-N sucralose Chemical compound O[C@@H]1[C@@H](O)[C@@H](Cl)[C@@H](CO)O[C@@H]1O[C@@]1(CCl)[C@@H](O)[C@H](O)[C@@H](CCl)O1 BAQAVOSOZGMPRM-QBMZZYIRSA-N 0.000 description 2
- 235000019408 sucralose Nutrition 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000007664 blowing Methods 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4211—Regulation; Control of columns
- B01D3/4227—Head- and bottom stream
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0078—Condensation of vapours; Recovering volatile solvents by condensation characterised by auxiliary systems or arrangements
- B01D5/009—Collecting, removing and/or treatment of the condensate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1418—Recovery of products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/90—Odorous compounds not provided for in groups B01D2257/00 - B01D2257/708
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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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
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- 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
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- C02F2209/02—Temperature
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- C02F2209/03—Pressure
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- C02F2209/16—Total nitrogen (tkN-N)
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2301/04—Flow arrangements
- C02F2301/043—Treatment of partial or bypass streams
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- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/30—Aerobic and anaerobic processes
- C02F3/302—Nitrification and denitrification treatment
- C02F3/307—Nitrification and denitrification treatment characterised by direct conversion of nitrite to molecular nitrogen, e.g. by using the Anammox process
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Abstract
The invention relates to a method for treating waste water containing DMF, which is characterized by comprising the following steps: (1) adjusting the pH of the waste water containing DMF to be 11-12.5, feeding the waste water to an alkaline hydrolysis tower after the water temperature is 110-135 ℃, carrying out alkaline hydrolysis for 80-100 min, and controlling the pH of the effluent to be 8.5-10; (2) then sending the mixture into a first deamination tower, controlling the temperature at the bottom of the tower to be 120-140 ℃, the pressure to be-5-10 KPa and the top temperature to be 65-75 ℃; absorbing the gas from the top to prepare a methylamine water solution, and sending the liquid at the bottom of the tower to biochemical treatment; (3) pumping the aqueous solution of the methylamine into a second deamination tower, and controlling the temperature of the tower bottom to be 130-145 ℃ and the pressure to be 1.15-1.35 MPa; the temperature at the top of the tower is 65-75 ℃, and the pressure is 1.10-1.20 MPa; ammonia gas coming out of the top is made into ammonia water for sale; (4) pumping the deamination secondary tower bottom liquid into a rectifying tower, and controlling the tower bottom temperature to be 135-150 ℃, the pressure to be 0.4-0.6 MPa, the tower top temperature to be 55-65 ℃ and the pressure to be 0.35-0.55 MPa; condensing the gas from the top to obtain dimethylamine product, and biochemical treating the waste liquid from the bottom of the tower. The invention has the advantages that: the DMF content in the biochemical treatment wastewater is controlled below 0.08g/L, the total nitrogen is controlled within 200mg/L, and the DMF removal efficiency is over 99.6 percent; and the methylamine recovery efficiency is more than 96 percent, and the content is more than 99.8.
Description
Technical Field
The invention belongs to the field of chemical wastewater treatment, relates to the field of sucralose production, and particularly relates to a method for treating DMF (dimethyl formamide) -containing wastewater.
Technical Field
In the production process of sucralose, DMF recovery can generate DMF-containing wastewater, and DMF-containing wastewater can also be generated during high-salt wastewater treatment (evaporation and condensation). At present, the treatment of DMF-containing wastewater mainly comprises two types: one is to prepare dilute ammonia water from waste water containing DMF, but because the waste water contains more impurities, the dilute ammonia water has other special odor, and meanwhile, the ammonia water can turn black, the selling pressure is higher, and the influence on the DMF recovery of the previous working section is larger; the other is that the sewage is directly led to a sewage station to be treated by anaerobic treatment and aerobic treatment and then is discharged after reaching the discharge standard, but the load of biochemical treatment is larger because more ammonia nitrogen is generated after DMF decomposition, the wastewater treatment capacity is restricted, and the production influence is larger.
Patent publication No. CN107673571A provides a method and a system for comprehensively treating DMF wastewater in membrane production, wherein DMF wastewater is subjected to alkaline washing and then is blown off, waste gas dimethylamine after blowing off is absorbed by a packed tower, and then dimethylamine salt is obtained by distillation and drying; treating the blown-off wastewater by adopting a multi-stage anaerobic and aerobic biochemical treatment combined process, performing coagulation sedimentation on biochemical effluent, and performing membrane treatment on supernatant; however, the method uses normal-temperature alkaline hydrolysis and normal-temperature stripping; the alkaline hydrolysis efficiency is poor, and the content of residual DMF in the wastewater is high; the normal-temperature stripping is adopted, the stripping efficiency of dimethylamine in the wastewater is more than 81%, and more remained dimethylamine can not be removed. The pressure for subsequent biochemical treatment is higher, and the cost is increased because the utilization efficiency is poorer and the dimethylamine is recovered less.
Disclosure of Invention
The invention aims to solve the problems in the patent publication No. CN107673571A and provide a method for treating DMF-containing wastewater.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a treatment method of DMF-containing wastewater is characterized by adopting the following devices:
the alkaline hydrolysis tower is sequentially connected with a first deamination tower, a first methylamine storage tank, a second deamination tower (a floating valve tower), a rectifying tower and a biochemical treatment system;
the method comprises the following steps:
(1) adjusting the pH (adopting alkalis and oxides thereof) of DMF-containing wastewater (from the processes of DMF recovery and high-salt wastewater evaporation and condensation) to 11-12.5, adjusting the water temperature to 110-135 ℃, and then conveying the wastewater to an alkaline hydrolysis tower for alkaline hydrolysis reaction for 80-100 min, wherein the pH of effluent is controlled to be 8.5-10;
(2) feeding the wastewater from the alkaline hydrolysis tower into a first deamination tower to remove dimethylamine gas, controlling the temperature at the bottom of the first deamination tower to be 120-140 ℃, the pressure to be-5-10 KPa and the temperature at the top of the first deamination tower to be 65-75 ℃; collecting gas (dimethylamino) from the top of the deamination tower by an absorption tank to prepare a 18-35% concentration methylamine water solution, and sending the liquid at the bottom of the deamination tower to a biochemical treatment system;
(3) pumping the ammonia solution obtained in the step (2) into a second deamination tower to remove ammonia again, and controlling the temperature at the bottom of the second deamination tower to be 130-145 ℃ and the pressure to be 1.15-1.35 MPa; the temperature of the top of the second deamination tower is 65-75 ℃, and the pressure is 1.10-1.20 MPa; preparing ammonia water (with the concentration of 20-28%) from gas (ammonia gas) from the top of the deamination tower, and selling the ammonia water;
(4) pumping the bottom liquid of the second deamination tower into a rectifying tower for rectification, and controlling the temperature of the bottom of the rectifying tower to be 135-150 ℃, the pressure to be 0.4-0.6 MPa, the temperature of the top of the rectifying tower to be 55-65 ℃ and the pressure to be 0.35-0.55 MPa; and (3) condensing (15-30 ℃) the gas (dimethylamine) from the top of the rectifying tower to obtain a finished dimethylamine product, and sending the waste liquid at the bottom of the rectifying tower into a biochemical treatment system.
Furthermore, the content of DMF in the DMF-containing wastewater is 15-20 g/L.
Further, in the step (1), the alkali and the oxide thereof are one of sodium hydroxide, calcium hydroxide and calcium oxide.
According to the invention, the waste water containing DMF is subjected to alkaline hydrolysis (the alkaline hydrolysis temperature is controlled to be 110-135 ℃) by using a float valve tower, then ammonia nitrogen content (no specific requirements on alkaline hydrolysis and ammonia removal time) at the bottom of the ammonia removal tower is controlled by ammonia removal (the temperature at the bottom of the tower is controlled to be 120-140 ℃ and the pressure is controlled to be-5-10 KPa), and gas (dimethylamino) discharged from the top of the ammonia removal tower is collected by an absorption tank to prepare a methylamine water solution with the concentration of 18-35%.
The invention has the advantages that: the content of DMF in the effluent can be controlled below 0.08g/L, the total nitrogen can be controlled within 200mg/L, and the removal efficiency of DMF is over 99.6 percent through alkaline hydrolysis; the methylamine recovery efficiency is more than 96 percent, and pure dimethylamine with the content of more than 99.8 can be obtained and sold as a finished product; greatly reduces the pressure of subsequent biochemical treatment and reduces the treatment cost (the dimethylamine recovery efficiency is higher).
Drawings
FIG. 1 is a schematic diagram of a process for treating DMF-containing wastewater and evaporative condensate.
Detailed Description
The invention is further illustrated with reference to fig. 1:
a treatment device for DMF-containing wastewater comprises the following devices: the alkaline hydrolysis tower (float valve tower) is sequentially connected with a deamination tower I, a deamination storage tank, a deamination tower II, a rectifying tower (float valve tower) and a biochemical treatment system;
a method for treating DMF-containing wastewater and evaporative condensate comprises the following specific implementation steps:
example 1
(1) Carrying out 20m dry distillation on DMF-containing wastewater (containing 16.21g/L of DMF and 4930mg/L of ammonia nitrogen, and from DMF recovery and high-salt wastewater evaporation and condensation processes) by adjusting the pH to =12 with 20% sodium hydroxide solution, adjusting the water temperature to 125 ℃, and then sending the wastewater to an alkaline hydrolysis tower for alkaline hydrolysis reaction for 85min, wherein the pH of the effluent is controlled to = 9.5;
(2) feeding the wastewater from the alkaline hydrolysis tower into a first deamination tower to remove dimethylamine gas, controlling the temperature at the bottom of the first deamination tower to be 135 ℃ and the pressure to be 5KPa, and controlling the temperature at the top of the first deamination tower to be 70 ℃ and the pressure to be 2 KPa; gas (dimethylamino) from the top of the deamination tower is collected by an absorption tank and prepared into 655.35Kg of aqueous solution of the dimethylamino (30.2 percent of dimethylamine), and bottom liquid (wastewater, the DMF content is 0.07g/l, and the total nitrogen content is 150 mg/l) of the deamination tower is transported to a biochemical treatment system at 19.9 m;
(3) pumping the ammonia water solution obtained in the step (2) into a second deamination tower to remove ammonia again, and controlling the temperature at the bottom of the second deamination tower to be 142 ℃ and the pressure to be 1.25 MPa; the temperature at the top of the second deamination tower is 66 ℃ and the pressure is 1.05 MPa; preparing ammonia water 206.5L (concentration 20%) from gas (ammonia gas) from the top of the deamination tower, and selling the ammonia water 206.5L;
(4) 616kg of deamination secondary tower bottom liquid is pumped into a rectifying tower for rectification, the tower bottom temperature of the rectifying tower is controlled at 140 ℃, the pressure is controlled at 0.52MPa, the tower top temperature is controlled at 57 ℃, and the pressure is controlled at 0.4 MPa; 190Kg of finished dimethylamine (96% yield) was obtained by condensing (25 ℃) the gas (dimethylamine) coming out of the top of the rectification column, and 420L of the waste liquid from the bottom of the rectification column was sent to a biochemical treatment system.
Example 2
(1) Carrying out dry distillation on DMF (DMF content is 18g/L, ammonia nitrogen is 4900mg/L, and the process comes from DMF recovery and high-salt wastewater evaporation and condensation) at 30m by adjusting pH =11.5 with 32% sodium hydroxide, adjusting water temperature to 130 ℃, and then sending to an alkaline hydrolysis tower for alkaline hydrolysis reaction for 95min, wherein the pH =9.5 of the effluent is controlled;
(2) feeding the wastewater from the alkaline hydrolysis tower into a first deamination tower to remove dimethylamine gas, controlling the temperature at the bottom of the first deamination tower to be 125 ℃ and the pressure to be-5 KPa, and controlling the temperature at the top of the first deamination tower to be 66 ℃ and the pressure to be 10 KPa; after being collected by an absorption tank, gas (dimethylamino) from the top of the deamination tower is prepared into 1663L Kg of aqueous solution of the dimethylamino (25 percent of dimethylamine), and a bottom solution (wastewater, the DMF content is 0.05g/L, and the total nitrogen content is 123 mg/L) of the deamination tower is shipped at 29.6m to a biochemical treatment system;
(3) pumping the water solution of the methylamine obtained in the step (2) into a second deamination tower to remove ammonia again, and controlling the temperature at the bottom of the second deamination tower to be 135 ℃ and the pressure to be 1.2 MPa; the temperature at the top of the second deamination tower is 70 ℃, and the pressure is 1.15 MPa; preparing 400kg (with the concentration of 20%) of ammonia water from gas (ammonia gas) discharged from the top of the deamination tower, and selling the ammonia water;
(4) pumping 1563L of the deamination secondary tower bottom liquid into a rectifying tower for rectification, and controlling the tower bottom temperature of the rectifying tower to be 145 ℃, the pressure to be 0.55MPa, the tower top temperature to be 52 ℃ and the pressure to be 0.45 MPa; the gas (dimethylamine) from the top of the rectifying tower is condensed (20 ℃) to obtain 321.1 Kg of finished dimethylamine (the rectification yield is 96.5%), and the waste liquid 918.4L at the bottom of the rectifying tower is sent into a biochemical treatment system.
The biochemical treatment step of the wastewater:
(1) pumping the wastewater generated in the examples 1 and 2 into an intermediate tank, mixing, pumping into a first-stage hydrolysis acidification tank, adding sulfuric acid to control the pH to be 8.5, pumping into a first-stage anaerobic tank for circulation for 84 hours, and controlling the pH to be 8.5 and the temperature to be 38 ℃;
(2) enabling the effluent from the top of the primary anaerobic tank to enter a primary sedimentation tank, pumping the water from the top of the sedimentation tank into a secondary hydrolysis acidification tank, adjusting the pH to 8.0, then pumping into a secondary anaerobic tank for circulation for 84 hours, and controlling the pH to be 8.0 and the temperature to be 34 ℃;
(3) water at the top of the secondary anaerobic tank enters a secondary sedimentation tank, water at the top of the sedimentation tank is pumped into a primary A/O, and the retention time is 48 h; controlling the pH value of the A/O to be 7.8-8.6 and the temperature to be 33-34 ℃, and enabling the water at the top of the tank to enter a middle sedimentation tank for sludge sedimentation;
(4) allowing water at the top of the intermediate sedimentation tank to enter a second-level A/0, standing for 24 hours, and controlling the A/O PH to be 7.9-8.8 and the temperature to be 34-36 ℃; the top water of the second-stage A/O pool enters a secondary sedimentation pool for secondary sedimentation, and the top water of the secondary sedimentation pool enters a clean water pool 1;
(5) pumping the water in the clean water tank 1 into a high-density sedimentation tank, carrying out coagulating sedimentation on the water by adding PAC and PAM, and feeding the supernatant into the clean water tank 2, wherein the total nitrogen of the water in the clean water tank 2 is 10mg/l, and the COD is 40 mg/l.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (5)
1. A treatment method of DMF-containing wastewater is characterized by adopting the following devices:
the alkaline hydrolysis tower is sequentially connected with a first deamination tower, a first deamination storage tank, a second deamination tower, a rectifying tower and a biochemical treatment system;
the method comprises the following steps:
(1) adjusting the pH value of the DMF-containing wastewater to 11-12.5, adjusting the water temperature to 110-135 ℃, and then conveying the DMF-containing wastewater to an alkaline hydrolysis tower for alkaline hydrolysis reaction for 80-100 min, wherein the pH value of effluent is controlled to 8.5-10;
(2) feeding the wastewater from the alkaline hydrolysis tower into a first deamination tower to remove dimethylamine gas, controlling the temperature at the bottom of the first deamination tower to be 120-140 ℃, the pressure to be-5-10 KPa and the temperature at the top of the first deamination tower to be 65-75 ℃; collecting the dimethyl ammonia gas from the top of the deamination tower by an absorption tank to prepare a 18-35% concentration aqueous solution of the deamination tower, and sending the liquid at the bottom of the deamination tower to a biochemical treatment system;
(3) pumping the ammonia solution obtained in the step (2) into a second deamination tower to remove ammonia again, and controlling the temperature at the bottom of the second deamination tower to be 130-145 ℃ and the pressure to be 1.15-1.35 MPa; the temperature of the top of the second deamination tower is 65-75 ℃, and the pressure is 1.10-1.20 MPa; preparing ammonia gas from the top of the deamination tower into ammonia water with the concentration of 18-35% and selling the ammonia water;
(4) pumping the bottom liquid of the second deamination tower into a rectifying tower for rectification, and controlling the temperature of the bottom of the rectifying tower to be 135-150 ℃, the pressure to be 0.4-0.6 MPa, the temperature of the top of the rectifying tower to be 55-65 ℃ and the pressure to be 0.35-0.55 MPa; and (3) condensing dimethylamine gas from the top of the rectifying tower to obtain a finished dimethylamine product, and sending the waste liquid at the bottom of the rectifying tower into a biochemical treatment system.
2. The method for treating DMF-containing wastewater according to claim 1, which comprises the following steps: the alkaline hydrolysis tower is a float valve tower.
3. The method for treating DMF-containing wastewater according to claim 1, which comprises the following steps: the DMF-containing wastewater is obtained from the processes of DMF recovery and high-salt wastewater evaporation and condensation, and the DMF content is 15-20 g/L.
4. The method for treating DMF-containing wastewater according to claim 1, which comprises the following steps: the alkali and the oxide thereof in the step (1) are one of sodium hydroxide, calcium hydroxide and calcium oxide.
5. A method according to any one of claims 1 to 4, wherein: the condensation temperature in the step (4) is 15-30 ℃.
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