CN103553260B - Synergic extraction and negative-pressure flash evaporation dephenolizing method of high-concentration semi-coke phenolic wastewater - Google Patents
Synergic extraction and negative-pressure flash evaporation dephenolizing method of high-concentration semi-coke phenolic wastewater Download PDFInfo
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- 238000000605 extraction Methods 0.000 title claims abstract description 127
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 239000002351 wastewater Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 36
- 230000002195 synergetic effect Effects 0.000 title claims abstract description 25
- 238000001704 evaporation Methods 0.000 title abstract 4
- 230000008020 evaporation Effects 0.000 title abstract 4
- 239000000571 coke Substances 0.000 title abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 52
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims abstract description 50
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims abstract description 50
- 238000006481 deamination reaction Methods 0.000 claims abstract description 46
- 230000009615 deamination Effects 0.000 claims abstract description 44
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 150000002989 phenols Chemical class 0.000 claims abstract description 8
- 238000004064 recycling Methods 0.000 claims abstract description 8
- 229940043265 methyl isobutyl ketone Drugs 0.000 claims description 48
- 239000003610 charcoal Substances 0.000 claims description 23
- 238000001311 chemical methods and process Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 230000005484 gravity Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000002203 pretreatment Methods 0.000 claims description 7
- 238000007670 refining Methods 0.000 claims description 7
- 230000026676 system process Effects 0.000 claims description 7
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 235000013824 polyphenols Nutrition 0.000 description 28
- 239000012071 phase Substances 0.000 description 23
- 150000008442 polyphenolic compounds Chemical class 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 230000003247 decreasing effect Effects 0.000 description 6
- 230000005587 bubbling Effects 0.000 description 5
- 238000005192 partition Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 2
- GGNQRNBDZQJCCN-UHFFFAOYSA-N benzene-1,2,4-triol Chemical compound OC1=CC=C(O)C(O)=C1 GGNQRNBDZQJCCN-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229940035429 isobutyl alcohol Drugs 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- -1 methyl-isobutyl Chemical group 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Water Treatments (AREA)
Abstract
The invention belongs to the technical field of wastewater treatment and discloses a synergic extraction and negative-pressure flash evaporation dephenolizing method of high-concentration semi-coke phenolic wastewater. The method is mainly technically characterized in that the method comprises the steps of carrying out deacidification and deamination, extraction, separation of phenol and extracting agents in an extracting phase, and separation of wastewater and the extracting agents in an extraction raffinate phase, wherein diisopropyl ether and methyl isobutyl ketone are used as extracting agents to carry out synergic extraction dephenolizing, the volume ratio of diisopropyl ether to methyl isobutyl ketone is 1:10-1:1, and the volume ratio of the extracting agents to water is 1:18-1:5.5; then, feeding the treated wastewater into a phenol tower by a phenol tower charging pump for negative-pressure flash evaporation, and collecting the extracting agents for recycling, wherein the removal rate of total phenols is 91%, the removal rate of polyhydric phenol is greater than 70%, and the removal rate of COD (Chemical Oxygen Demand) is greater than 91%. Moreover, the synergic extraction and negative-pressure flash evaporation dephenolizing method disclosed by the invention is high in dephenolizing efficiency, a little in device application, small in solvent dosage, low in energy consumption, and beneficial to saving energy and protecting environment. Besides, economic benefits and social benefits are higher.
Description
Technical field
The invention belongs to blue charcoal high-concentration phenolic wastewater treatment process technical field, relate to the synergistic extraction vacuum flash dephenolization method of blue charcoal high-concentration phenolic wastewater concretely.
Background technology
Blue charcoal wastewater from chemical industry is the waste water produced in the retort process of blue charcoal, and total phenol content can up to 10500 more than mg/L.Pollutant levels are high, complicated component, containing multiple pollutants such as tar, aromatic hydrocarbons, ammonia nitrogen, sulfide, prussiates, are the maximum phenolic wastewater of a kind of intractability.
Blue charing work Phenol for Waste Water and ammonia endanger large to biochemical system, but they can be recycled simultaneously.At present, the method commonly used containing phenol trade effluent is solvent method.Conventional solvent method has depickling-phenol extraction-deamination method, depickling deamination-mono-tower dephenolize method, depickling deamination-series connection double tower two-stage dephenolize method etc.Wherein, this total phenol of blue charcoal is greater than to the blue charcoal waste water of 10000 mg/L, depickling-phenol extraction-deamination method Process for Effluent does not reach biochemical water inlet index request; Depickling deamination-the decreasing ratio of mono-tower dephenolize method to unit phenol is higher, can reach more than 99%, but very poor to the effect of extracting of polyphenol, is generally no more than 68%.After extracting and dephenolizing, total phenol content is still greater than 5000mg/L up to 550mg/L, COD, because polyatomic phenol is difficult to biological degradation, and inhibit activities bacteria growing, must by just can biochemical treatment be carried out after the means regulating water quality indexs such as water distribution.Although depickling deamination-series connection double tower two-stage dephenolize method improves the clearance of polyphenol, add the investment of secondary extraction tower and phenol two tower and water tower.
Suitable extraction agent is selected to be the key improving waste water extracting and dephenolizing efficiency.Extraction agent must consider that it is to unit phenol and the solubleness of polyphenol, the water-soluble and problem such as energy consumption, price, operation difficulty or ease.Extraction agent Di Iso Propyl Ether conventional at present and methyl iso-butyl ketone (MIBK).The solubleness of Di Iso Propyl Ether in water is 0.8%, and boiling point is 68.5 DEG C, high to unit phenol extraction decreasing ratio, but due to the stronger polarity of polyphenol and water-soluble, extraction decreasing ratio is very low.Partition ratio as Di Iso Propyl Ether Pyrogentisinic Acid can reach 30-36.5, but Resorcinol and hydroxyquinol only have 0.8-1.2 and 0.1-0.25 respectively.So the extraction that Di Iso Propyl Ether is suitable only for unit phenol removes.Methyl iso-butyl ketone (MIBK) is a kind of dephenolize extraction agent efficiently, and higher to the partition ratio of polyphenol, Resorcinol and hydroxyquinol partition ratio are respectively 9-12 and 4-6.Therefore the extraction being suitable for polyphenol removes.(" colleges and universities' chemical engineering journal ", 2003,17(3): 261-265), relative to other solvent, higher to the solubleness of polyphenol.
The patent No. is 200610033936.X, 200610033932.1 patent discloses and adopt methyl iso-butyl ketone (MIBK) to carry out the method for extracting and dephenolizing, and total phenol removal rate can reach 92%.The operating practice of Harbin Gas Works proves, adopt methyl iso-butyl ketone (MIBK) extraction process, the total phenol content of waste water is about 300mg/L, and COD is about 2000mg/L.But the solubleness of methyl iso-butyl ketone (MIBK) in water is 1.9%, boiling point is 117-118 DEG C.Therefore, methyl iso-butyl ketone (MIBK) comparatively Di Iso Propyl Ether reclaims loss greatly, and steam consumption is large, and energy consumption is high.
In sum, the extracting and dephenolizing technology main difficulty of high-concentration phenolic wastewater is, because polyphenol has stronger polarity and water-soluble compared with unit phenol, extraction removal efficiency is low; And adopt efficient extraction agent, cause again that solvent recuperation energy consumption is high, loss is large, increase process cost.Two kinds of extraction agents are disclosed for this difficult problem patent ZL 2,010 1 0242537.0, depickling deamination-series connection double tower two-stage dephenolize method.Energy consumption slightly reduces, and the consumption of extraction agent decreases 10%, but adds secondary extraction and supporting phenol tower and water tower, adds investment.
Summary of the invention
The technical problem that the present invention solves just is to provide the advantage that a kind of dephenolize efficiency is high, equipment is applied less, solvent load is little, energy consumption is low, is conducive to the synergistic extraction vacuum flash dephenolization method of the blue charcoal high-concentration phenolic wastewater of energy-conserving and environment-protective.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is: the method comprises the following steps:
The first step, depickling deamination
The high-concentration phenolic wastewater warp that blue charcoal chemical process produces
gravity settling and heating oil removal by air bubblingafter pre-treatment, enter depickling deammoniation tower, after depickling deamination, make waste water pH value control at 5.5-8.5;
Second step, extraction
Waste water after depickling deamination enters extraction tower, with Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) for extraction agent, carry out synergistic extraction dephenolize, the volume ratio of Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:10-1:1, and the volume ratio of extraction agent and water is 1:18-1:5.5;
3rd step, separating and extracting mutually in phenol and extraction agent
The extraction phase being rich in phenol enters water-and-oil separator, enters extract storage tank from the overflow of water-and-oil separator upper strata, is delivered in phenol tower carry out by phenol tower fresh feed pump
vacuum flash,the vacuum tightness of phenol tower remains within the scope of 200-400 mmhg, service temperature in phenol tower is 80-105 DEG C, working pressure in phenol tower is-0.03 ~-0.05MPa, and the solvent of volatilization enters solvent cycle tank for recycling after compressor and condenser are cooled to 40 DEG C; The crude phenols of tower reactor deliver to refining of crude phenol workshop section after water cooler cooling;
4th step, is separated the waste water in extracting phase and extraction agent
Extracting phase in extraction tower enters water tower to carry out
vacuum flashreclaim the extraction agent be dissolved in wherein to recycle, the vacuum tightness of water tower remains within the scope of 200-400 mmhg, service temperature in water tower is 40-60 DEG C, working pressure in phenol tower is-0.03 ~-0.05MPa, thereafter waste water total phenol content is 200-300mg/L, COD is 2000-4000mg/ L, enters biochemical system process.
Its additional technical feature is:
In described the first step depickling deamination step, depickling deamination bottom temperature is 100-160 DEG C, and depickling deamination tower reactor pressure is 0.3-0.6MPa, and extraction tower temperature is 30-50 DEG C, and extraction tower pressure is 0.3-0.5Mpa;
The volume ratio of described Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:5-1:1, and the volume ratio of extraction agent and water is 1:10-1:8.
The synergistic extraction vacuum flash dephenolization method of blue charcoal high-concentration phenolic wastewater provided by the invention, compared with the existing technology comparatively have the following advantages: one, blue charcoal high-concentration phenolic wastewater first stripping depickling deamination removes mechanical impurity, make the pH value of waste water control at 5-8, be conducive to improving extracting and dephenolizing effect; After synergistic extraction dephenolize, the backflow of an extraction phase part and extraction tower water inlet mixing, after another part enters water-and-oil separator separation, the aqueous phase of bottom enters extraction tower, oil phase enters phenol tower vacuum flash dephenolize, extraction phase backflow and oily water separation can improve concentration and the phenol removal rate of phenol, improve the extraction efficiency of extraction tower; , adopt Di Iso Propyl Ether and methyl-isobutyl alcohol/ketone mixtures synergistic extraction phenol time, its partition ratio is greater than the partition ratio sum of each extraction agent extraction separately under same concentrations condition significantly, synergistic extraction ensures polyphenol height decreasing ratio, improve dephenolization effect, meanwhile, energy consumption and the loss of solvent recuperation can be reduced; Through synergistic extraction, secondary extraction tower and corresponding supporting phenol two tower and water tower can be cancelled, thus save the energy consumption of phenol tower and water tower, reduce facility investment; The vacuum flash technique that phenol tower and water tower adopt, phenol tower and the water tower service temperature of vacuum flash technique are low, and extraction phase and extracting phase are without the need to heat transfer process before a series of loaded down with trivial details tower simultaneously, save energy consumption; The front waste water unit phenol content of process is 3000-9000mg/L, polyphenol content is 2000-7000 mg/L, total ammonia 3000-10000mg/L, COD is about 30000-70000 mg/L, pH value is 10-12, waste water total phenol content after extracting and dephenolizing is 200-300mg/L, COD is 2000-4000mg/L, and pH value is 5-8, and total phenol removal rate is greater than 91%, polyphenol decreasing ratio is greater than 70%, COD decreasing ratio and is greater than 91%;
Its two, in described the first step depickling deamination step, depickling deamination bottom temperature is 100-160 DEG C, and depickling deamination tower reactor pressure is 0.3-0.6MPa, and extraction tower temperature is 30-50 DEG C, and extraction tower pressure is 0.3-0.5MPa; Desulfurization, deamination and dephenolization effect are better;
Its three, the volume ratio of described Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:5-1:1, and the volume ratio of extraction agent and water is 1:10-1:8, and not only dephenolization effect is better, and when vacuum flash is separated, separating effect is better.
Embodiment
Below the synergistic extraction vacuum flash dephenolization method of blue charcoal high-concentration phenolic wastewater proposed by the invention is described further.
The synergistic extraction vacuum flash dephenolization method of the blue charcoal high-concentration phenolic wastewater that the present invention proposes comprises the following steps:
The first step, depickling deamination
The high-concentration phenolic wastewater that blue charcoal chemical process produces, after gravity settling and the pre-treatment of heating oil removal by air bubbling, enters depickling deammoniation tower, after depickling deamination, makes waste water pH value control at 5.5-8.5;
Second step, extraction
Waste water after depickling deamination enters extraction tower, with Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) for extraction agent, carry out synergistic extraction dephenolize, the volume ratio of Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:10-1:1, and the volume ratio of extraction agent and water is 1:18-1:5.5;
3rd step, separating and extracting mutually in phenol and extraction agent
The extraction phase being rich in phenol enters water-and-oil separator, enters extract storage tank from the overflow of water-and-oil separator upper strata, is delivered in phenol tower carry out vacuum flash by phenol tower fresh feed pump
,the vacuum tightness of phenol tower remains within the scope of 200-400 mmhg, service temperature in phenol tower is 80-105 DEG C, working pressure in phenol tower is-0.03 ~-0.05MPa, and the solvent of volatilization enters solvent cycle tank for recycling after compressor and condenser are cooled to 40 DEG C; The crude phenols of tower reactor deliver to refining of crude phenol workshop section after water cooler cooling;
4th step, is separated the waste water in extracting phase and extraction agent
Extracting phase in extraction tower enters water tower and carries out vacuum flash, and reclaim the extraction agent be dissolved in wherein and recycle, waste water total phenol content is thereafter 200-300mg/L, COD is 2000-4000mg/ L, enters biochemical system process.
In described the first step depickling deamination step, depickling deamination bottom temperature is 100-160 DEG C, and depickling deamination tower reactor pressure is 0.3-0.6MPa, and extraction tower temperature is 30-50 DEG C, and extraction tower pressure is 0.3-0.5MPa;
The volume ratio of described Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:5-1:1, and the volume ratio of extraction agent and water is 1:10-1:8.
Embodiment 1
The first step, depickling deamination
The high-concentration phenolic wastewater that blue charcoal chemical process produces is after gravity settling and the pre-treatment of heating oil removal by air bubbling, enter depickling deammoniation tower, depickling deamination bottom temperature is 100 DEG C, and depickling deamination tower reactor pressure is 0.6MPa, after depickling deamination, waste water pH value is made to control 5.5;
Second step, extraction
Waste water after depickling deamination enters extraction tower, and with Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) for extraction agent, carry out synergistic extraction dephenolize, the volume ratio of Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:10, and the volume ratio of extraction agent and water is 1:18;
3rd step, separating and extracting mutually in phenol and extraction agent
The extraction phase being rich in phenol enters water-and-oil separator, enters extract storage tank from the overflow of water-and-oil separator upper strata, is delivered in phenol tower carry out vacuum flash by phenol tower fresh feed pump
,the vacuum tightness of phenol tower remains within the scope of 200 mmhg, and the service temperature in phenol tower is 105 DEG C, and the working pressure in phenol tower is-0.05MPa, and the solvent of volatilization enters solvent cycle tank for recycling after compressor and condenser are cooled to 40 DEG C; The crude phenols of tower reactor deliver to refining of crude phenol workshop section after water cooler cooling;
4th step, is separated the waste water in extracting phase and extraction agent
Extracting phase in extraction tower enters water tower and carries out vacuum flash, reclaim the extraction agent be dissolved in wherein to recycle, the vacuum tightness of water tower remains within the scope of 200 mmhg, service temperature in water tower is 85 DEG C, working pressure in water tower is-0.03MPa, thereafter waste water total phenol content is 200mg/L, COD is 2000mg/ L, enters biochemical system process.
The water quality analysis data in the present embodiment 1 different treatment stage are as shown in table 1.
The water quality analysis data in table 1 different treatment stage.
Embodiment 2
The first step, depickling deamination
The high-concentration phenolic wastewater that blue charcoal chemical process produces is after gravity settling and the pre-treatment of heating oil removal by air bubbling, enter depickling deammoniation tower, depickling deamination bottom temperature is 160 DEG C, and depickling deamination tower reactor pressure is 0.3MPa, after depickling deamination, waste water pH value is made to control 8.5;
Second step, extraction
Waste water after depickling deamination enters extraction tower, and with Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) for extraction agent, carry out synergistic extraction dephenolize, the volume ratio of Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:1, and the volume ratio of extraction agent and water is 1:5.5;
3rd step, separating and extracting mutually in phenol and extraction agent
The extraction phase being rich in phenol enters water-and-oil separator, enters extract storage tank from the overflow of water-and-oil separator upper strata, is delivered in phenol tower carry out vacuum flash by phenol tower fresh feed pump
,the solvent of volatilization enters solvent cycle tank for recycling after compressor and condenser are cooled to 40 DEG C; The crude phenols of tower reactor deliver to refining of crude phenol workshop section after water cooler cooling;
4th step, is separated the waste water in extracting phase and extraction agent
Extracting phase in extraction tower enters water tower and carries out vacuum flash, reclaim the extraction agent be dissolved in wherein to recycle, the vacuum tightness of water tower remains within the scope of 400 mmhg, service temperature in water tower is 60 DEG C, working pressure in water tower is-0.05MPa, thereafter waste water total phenol content is 400mg/L, COD is 4000mg/ L, enters biochemical system process.
The water quality analysis data in the present embodiment 2 different treatment stage are as shown in table 2.
The water quality analysis data in table 2 different treatment stage.
Embodiment 3
The first step, depickling deamination
The high-concentration phenolic wastewater that blue charcoal chemical process produces is after gravity settling and the pre-treatment of heating oil removal by air bubbling, enter depickling deammoniation tower, depickling deamination bottom temperature is 130 DEG C, and depickling deamination tower reactor pressure is 0.5MPa, after depickling deamination, waste water pH value is made to control 6.8;
Second step, extraction
Waste water after depickling deamination enters extraction tower, and with Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) for extraction agent, carry out synergistic extraction dephenolize, the volume ratio of Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:5, and the volume ratio of extraction agent and water is 1:10;
3rd step, separating and extracting mutually in phenol and extraction agent
The extraction phase being rich in phenol enters water-and-oil separator, enters extract storage tank from the overflow of water-and-oil separator upper strata, is delivered in phenol tower carry out vacuum flash by phenol tower fresh feed pump
,the vacuum tightness of phenol tower remains within the scope of 300 mmhg, and the service temperature in phenol tower is 90 DEG C, and the working pressure in phenol tower is-0.04MPa, and the solvent of volatilization enters solvent cycle tank for recycling after compressor and condenser are cooled to 40 DEG C; The crude phenols of tower reactor deliver to refining of crude phenol workshop section after water cooler cooling;
4th step, is separated the waste water in extracting phase and extraction agent
Extracting phase in extraction tower enters water tower and carries out vacuum flash, reclaim the extraction agent be dissolved in wherein to recycle, the vacuum tightness of water tower remains within the scope of 300 mmhg, service temperature in water tower is 70 DEG C, working pressure in water tower is-0.04MPa waste water total phenol content is thereafter 300mg/L, COD is 3000mg/ L, enters biochemical system process.
The water quality analysis data in the present embodiment 3 different treatment stage are as shown in table 3.
The water quality analysis data in table 3 different treatment stage.
Embodiment 4
The first step, depickling deamination
The high-concentration phenolic wastewater that blue charcoal chemical process produces is after gravity settling and the pre-treatment of heating oil removal by air bubbling, enter depickling deammoniation tower, depickling deamination bottom temperature is 120 DEG C, and depickling deamination tower reactor pressure is 0.4MPa, after depickling deamination, waste water pH value is made to control 6.5;
Second step, extraction
Waste water after depickling deamination enters extraction tower, and with Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) for extraction agent, carry out synergistic extraction dephenolize, the volume ratio of Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:5, and the volume ratio of extraction agent and water is 1:8;
3rd step, separating and extracting mutually in phenol and extraction agent
The extraction phase being rich in phenol enters water-and-oil separator, enters extract storage tank from the overflow of water-and-oil separator upper strata, is delivered in phenol tower carry out vacuum flash by phenol tower fresh feed pump
,the vacuum tightness of phenol tower remains within the scope of 250 mmhg, and the service temperature in phenol tower is 100 DEG C, and the working pressure in phenol tower is-0.04MPa, and the solvent of volatilization enters solvent cycle tank for recycling after compressor and condenser are cooled to 40 DEG C; The crude phenols of tower reactor deliver to refining of crude phenol workshop section after water cooler cooling;
4th step, is separated the waste water in extracting phase and extraction agent
Extracting phase in extraction tower enters water tower and carries out vacuum flash, reclaim the extraction agent be dissolved in wherein to recycle, the vacuum tightness of water tower remains within the scope of 250 mmhg, service temperature in water tower is 80 DEG C, working pressure in water tower is-0.04MPa, thereafter waste water total phenol content is 300mg/L, COD is 3000mg/ L, enters biochemical system process.
The water quality analysis data in the present embodiment 4 different treatment stage are as shown in table 4.
The water quality analysis data in table 4 different treatment stage.
Protection scope of the present invention is not only confined to above-described embodiment, as long as structure is identical with the synergistic extraction vacuum flash dephenolization method structure of the blue charcoal high-concentration phenolic wastewater of the present invention, just drops on the scope of protection of the invention.
Claims (3)
1. the synergistic extraction vacuum flash dephenolization method of blue charcoal high-concentration phenolic wastewater, is characterized in that: the method comprises the following steps:
The first step, depickling deamination
The high-concentration phenolic wastewater warp that blue charcoal chemical process produces
gravity settling and heating oil removal by air bubblingafter pre-treatment, enter depickling deammoniation tower, after depickling deamination, make waste water ph control at 5.5-8.5;
Second step, extraction
Waste water after depickling deamination enters extraction tower, with Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) for extraction agent, carry out synergistic extraction dephenolize, the volume ratio of Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:10-1:1, and the volume ratio of extraction agent and water is 1:18-1:5.5;
3rd step, separating and extracting mutually in phenol and extraction agent
The extraction phase being rich in phenol enters water-and-oil separator, enters extract storage tank from the overflow of water-and-oil separator upper strata, is delivered in phenol tower carry out by phenol tower fresh feed pump
vacuum flash,service temperature in phenol tower is 80-105 DEG C, and the working pressure in phenol tower is-0.03 ~-0.05MPa, and the solvent of volatilization enters solvent cycle tank for recycling after compressor and condenser are cooled to 40 DEG C; The crude phenols of tower reactor deliver to refining of crude phenol workshop section after water cooler cooling;
4th step, is separated the waste water in extracting phase and extraction agent
Extracting phase in extraction tower enters water tower to carry out
vacuum flash, reclaim the extraction agent be dissolved in wherein and recycle, the service temperature in water tower is 60-85 DEG C, working pressure in phenol tower is-0.03 ~-0.05MPa, thereafter waste water total phenol content is 200-300mg/L, COD is 2000-4000mg/ L, enters biochemical system process.
2. the synergistic extraction vacuum flash dephenolization method of blue charcoal high-concentration phenolic wastewater according to claim 1, it is characterized in that: in described the first step depickling deamination step, depickling deamination bottom temperature is 100-160 DEG C, depickling deamination tower reactor pressure is 0.3-0.6MPa, extraction tower temperature is 30-50 DEG C, and extraction tower pressure is 0.3-0.5MPa.
3. the synergistic extraction vacuum flash dephenolization method of blue charcoal high-concentration phenolic wastewater according to claim 1, is characterized in that: the volume ratio of described Di Iso Propyl Ether and methyl iso-butyl ketone (MIBK) is 1:5-1:1, and the volume ratio of extraction agent and water is 1:10-1:8.
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| CN104671384A (en) * | 2014-12-31 | 2015-06-03 | 西北大学 | Method for recycling semi-coke wastewater or coking wastewater |
| CN105016554B (en) * | 2015-06-15 | 2017-09-05 | 天津市创举科技股份有限公司 | Semi-coke wastewater treatment process |
| CN106830156B (en) * | 2015-12-07 | 2020-03-24 | 中国石油化工股份有限公司 | Treatment method of phenol-containing wastewater |
| CN108147612B (en) * | 2016-12-05 | 2021-01-26 | 中国科学院大连化学物理研究所 | Method for treating coal carbonization wastewater |
| CN107434335B (en) * | 2017-09-01 | 2021-01-12 | 中国科学院过程工程研究所 | Comprehensive treatment method for recycling semi-coke wastewater phenol ammonia |
| CN109503333A (en) * | 2018-12-04 | 2019-03-22 | 青岛科技大学 | A kind of liquid-liquid extraction-flash separation phenol and water method |
| CN110204146A (en) * | 2019-06-05 | 2019-09-06 | 南京化工园博瑞德水务有限公司 | A kind of coal chemical wastewater treating technique |
| CN110526325B (en) * | 2019-07-29 | 2021-10-08 | 华南理工大学 | Diisopropyl ether-based high-concentration phenol-containing wastewater extracting agent and extracting method |
| CN110498564A (en) * | 2019-08-20 | 2019-11-26 | 石家庄惠洁科技有限公司 | A kind of coking, semi-coke wastewater low-cost high-efficiency treatment process |
| CN110540329B (en) * | 2019-09-09 | 2020-07-28 | 陕西煤业化工集团神木天元化工有限公司 | Phenol-ammonia wastewater treatment method and system |
| CN112062332A (en) * | 2020-09-02 | 2020-12-11 | 查都（上海）科技有限公司 | Semi-coke phenolic wastewater phenol extraction process |
| CN113354174A (en) * | 2021-06-21 | 2021-09-07 | 华电水务工程有限公司 | Method for extracting and dephenolizing phenolic wastewater |
| CN114349253A (en) * | 2022-01-25 | 2022-04-15 | 毛锦生 | Treatment process for semi-coke wastewater dephenolization recovered water |
| CN115196810B (en) * | 2022-08-16 | 2024-02-13 | 华电水务工程有限公司 | Method for extracting and dephenolizing phenol-containing wastewater |
| CN115583764A (en) * | 2022-11-04 | 2023-01-10 | 上海宝冶工程技术有限公司 | Method for treating coal gasification wastewater |
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| CN101186347A (en) * | 2007-11-22 | 2008-05-28 | 山东东昌精细化工科技有限公司 | Method for reclaiming low boiling point organic solvent from waste water |
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