CN112209467A - Phenol-containing wastewater treatment method of phenol-acetone device - Google Patents
Phenol-containing wastewater treatment method of phenol-acetone device Download PDFInfo
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- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title claims abstract description 69
- XDTRNDKYILNOAP-UHFFFAOYSA-N phenol;propan-2-one Chemical compound CC(C)=O.OC1=CC=CC=C1 XDTRNDKYILNOAP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 150
- 239000002351 wastewater Substances 0.000 claims abstract description 116
- 238000000605 extraction Methods 0.000 claims abstract description 63
- 238000005406 washing Methods 0.000 claims abstract description 46
- 230000003647 oxidation Effects 0.000 claims abstract description 22
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 22
- 239000003518 caustics Substances 0.000 claims abstract description 16
- RWGFKTVRMDUZSP-UHFFFAOYSA-N cumene Chemical compound CC(C)C1=CC=CC=C1 RWGFKTVRMDUZSP-UHFFFAOYSA-N 0.000 claims description 100
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 239000003513 alkali Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- 238000007599 discharging Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 claims description 14
- 238000011084 recovery Methods 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 6
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims description 5
- 238000005984 hydrogenation reaction Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 239000003921 oil Substances 0.000 abstract description 48
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000000926 separation method Methods 0.000 abstract description 6
- 239000010729 system oil Substances 0.000 abstract description 4
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000012071 phase Substances 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 241000510672 Cuminum Species 0.000 description 3
- 235000007129 Cuminum cyminum Nutrition 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 2
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- JESIHYIJKKUWIS-UHFFFAOYSA-N 1-(4-Methylphenyl)ethanol Chemical compound CC(O)C1=CC=C(C)C=C1 JESIHYIJKKUWIS-UHFFFAOYSA-N 0.000 description 1
- JLIDVCMBCGBIEY-UHFFFAOYSA-N 1-penten-3-one Chemical compound CCC(=O)C=C JLIDVCMBCGBIEY-UHFFFAOYSA-N 0.000 description 1
- VGVHNLRUAMRIEW-UHFFFAOYSA-N 4-methylcyclohexan-1-one Chemical compound CC1CCC(=O)CC1 VGVHNLRUAMRIEW-UHFFFAOYSA-N 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- OLBCVFGFOZPWHH-UHFFFAOYSA-N propofol Chemical compound CC(C)C1=CC=CC(C(C)C)=C1O OLBCVFGFOZPWHH-UHFFFAOYSA-N 0.000 description 1
- 229960004134 propofol Drugs 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000004457 water analysis Methods 0.000 description 1
- 239000003403 water pollutant 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/72—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/80—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/18—Removal of treatment agents after treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a phenol-containing wastewater treatment method of a phenol acetone device, which comprises the following steps: step S1: and (3) recovering and treating the oxidation feed caustic tower wastewater, and performing step S2: and (4) performing vacuum separation on the fine acetone tower, and performing step S3: replacing an oil extraction tower and an extracted oil alkaline washing tower of the OEC system; the invention has the advantages that: recovering and treating the wastewater of the alkaline washing tower, and oxidizing and feeding the wastewater of the alkaline washing tower to recover phenol in the high-concentration wastewater, wherein 2.4 tons of phenol are recovered all the year round; by adding the vacuum discrete treatment of the fine acetone tower, after the vacuum discrete measures of the fine acetone tower are implemented, the content of acetone in the wastewater in the tower bottom tank is reduced from 0.28 percent to 0.01 percent; 40.32 tons of acetone are recovered; the OEC system oil extraction tower and the extraction oil alkaline tower are replaced, and the replaced OEC system oil extraction tower and the replaced extraction oil alkaline tower reduce the COD concentration of the waste water of the oil extraction tower from about 5000mg/L to below 2500mg/L, reduce the phenol content of the waste water from 120mg/L to 40mg/L and recover 2.36 tons of phenol due to the improvement of the extraction efficiency.
Description
Technical Field
The invention relates to the technical field of phenol-acetone processes, in particular to a phenol-containing wastewater treatment method of a phenol-acetone device.
Background
The existing 13.5 million tons/year phenol-acetone device is the first bigger phenol-acetone production device in China. By adopting the U.S. Propofol method molecular sieve catalyst patent technology, the device is always in a safe and stable operation state after being built into a production, and all economic and technical indexes are in the leading position in China and abroad.
The phenol-acetone device has the disadvantages of complex production process, long process flow and more side reactions. The apparatus has four main production zones, respectively: zone a (alkylation unit), zone B (oxidation, concentration, decomposition unit), zone C (neutralization, phenol recovery unit), and zone D (rectification, AMS hydrogenation, AMS purification unit). The waste water produced in each area is collected in a waste water tank, oil-water separation is carried out, the oil phase returns to the process, and the water phase is discharged into a factory production waste water pipe network. The wastewater discharged by the device is high-concentration phenol-containing wastewater, has high organic matter content and complex composition, and belongs to refractory organic wastewater. The treatment of the phenol-acetone production wastewater becomes the key point of the environmental protection treatment of the company.
The existing solutions to the above problems are as follows:
(1) waste water produced by oxidation feed caustic wash tower
The cumin in the oxidation day storage tank is pumped out by a fresh cumin feeding pump, mixed with the circulating cumin from the hydrogenation section and the concentration section, and sent to a feeding alkaline washing tower to remove a small amount of acid and trace phenol. The alkali liquor comes from a 15% alkali liquor storage tank, the waste alkali is continuously discharged to a waste water collection tank, the cumene after alkali washing is sent to a mixed feeding buffer tank to be statically separated from part of water, and then the cumene is pumped to a coalescer by a mixed feeding pump to further separate the entrained water. The water separated in the buffer tank and the coalescer goes to a phenol-containing waste water collecting tank and then to a waste water separating tank.
(2) Waste water from oil extraction tower
The water-containing phenol discharged from each station is collected into a phenol-containing waste water tank, the water phase of the phenol-containing waste water tank is pumped out by a waste water pump, and is mixed with sulfuric acid injected into the tank from OEC acid and then enters an OEC mixing tank. After reaction, the material is extracted from the top oil-removing extraction tower, in the tower, phenol in the waste water is extracted by cumene, then the waste water is directly discharged to a waste water collecting underground tank, the phenol-containing extractant cumene enters an extraction oil alkaline washing tower, after the phenol is washed away by 15% aqueous alkali, the cumene is collected in a solvent tank for recycling, and the sodium phenolate liquid in the extraction oil alkaline washing tower is removed to a sodium phenolate storage tank.
(3) Wastewater of refined acetone tower bottom tank
Adding alkali and water into a fine acetone tower to remove aldehyde in the material, and collecting the product acetone from the side line of the tower top. Pumping a part of materials (isopropyl benzene and water) at the bottom of the refined acetone tower to a phenol rectifying tower condenser through a tower bottom pump for heat exchange, and returning the materials to the refined acetone tower; and part of the water enters a bottom tank of the refined acetone tower after being cooled by a bottom cooler, the cumene at the top is sent to an organic phase pump discharge pipeline at the top of the AMS tower and is sent to the cumene alkali washing tower, and the water at the bottom of the bottom tank of the refined acetone tower is sent to a condensate pump outlet pipeline of a rectification ejector. And the other part of the acetone is pumped into a tar tower condenser for heat exchange through an acetone refining tower residue circulating pump and then returns to the acetone rectifying tower.
② wastewater generated by a vacuum system of the fine acetone tower.
Reduce operating pressure (62KPa) of tower, improve the relative volatility of light and heavy components, the separation efficiency of tower improves, tower cauldron acetone content descends, and the acetone content will rise in the tail gas that the top of the tower discharged by the groove after the operating pressure of tower reduces, uses solitary vacuum, extracts this part tail gas, then with spray steam together, the condensation under the malleation state, in the smart acetone tower of backward flow income, avoids material loss and pollution.
The problems with the above solution are as follows:
the source of the wastewater is as follows:
the waste water produced by phenol-acetone is mainly formed by gathering the waste water produced in the areas A, B and D, and is discharged after being subjected to oil-water separation by a waste water tank at the total sewage discharge point of the device, the main components of the waste water comprise phenol, acetone and isopropyl benzene, and also butanone, acetophenone, pentenone, methylcyclohexanone, benzene, ethylbenzene, diacetone alcohol, dimethyl benzyl alcohol, aldehyde, organic acid and the like, and the average COD concentration is up to 5000 mg/L.
1. Oxidized feed caustic wash tower wastewater
Before cumene enters an oxidizer, the process requires that alkali is added into an oxidation feeding alkali washing tower to remove phenol, organic acid and other impurities in the cumene, waste water after alkali washing is directly discharged into a factory production waste water line, COD in the waste water accounts for 32% of the total amount, and the pollution is serious.
2. Waste water of fine acetone tower
And refluxing a part of the tower bottom material of the fine acetone tower, cooling a part of the tower bottom material, allowing the cooled part of the tower bottom material to enter a tower bottom tank of the fine acetone tower for layering, and discharging a water phase into a waste water system, wherein the main pollutant is acetone. The concentration of the discharged water pollutant of the bottom tank of the fine acetone tower is higher due to incomplete separation of the fine acetone tower kettle, and COD in the wastewater accounts for 28 percent of the total discharge amount.
3. Cumene extraction column waste water
The phenol-containing wastewater discharged from each process of the phenol recovery system is collected into a phenol-containing wastewater tank, after cumene is used for extraction in an extraction tower, the water phase is discharged into a plant wastewater system, and COD in the wastewater accounts for 25% of the total amount.
4. Wastewater treatment technology comparing and selecting
In the process of researching the phenol-acetone wastewater treatment technology, the phenol-acetone wastewater treatment technology was cooperated with various scientific research institutions and domestic and foreign companies, and the specific selection situation of the phenol-acetone production wastewater treatment technology is shown in table 1.
TABLE 1 phenol wastewater treatment method selection List
Although the treatment technology can reduce the concentration of the wastewater pollutants to the required control index, some technologies have high energy consumption, some technologies generate secondary pollution, some technologies have higher operating cost, and the once investment of foreign advanced technologies is very large, thereby undoubtedly increasing the enterprise cost.
Disclosure of Invention
In view of the above problems, the present invention provides a method for treating phenol-containing wastewater from a phenol acetone plant, which is used to treat phenol-containing wastewater from the phenol acetone plant, so as to overcome the above disadvantages of the prior art.
The invention provides a phenol-containing wastewater treatment method of a phenol acetone device, which comprises the following steps:
step S1: recycling and treating the wastewater of the oxidation feeding alkaline washing tower, pumping the wastewater into an OEC system (a mixing tank before an oil extraction tower and an extraction oil alkaline washing tower are combined into the tower) by using a pump after the wastewater is connected with a phenolic wastewater tank in a C area by using a pipeline, wherein an alkaline washing circulating pump of the oxidation feeding alkaline washing tower is replaced by an alkaline washing circulating pump with the flow of 8m 3/h;
step S2: separating the fine acetone tower in vacuum, wherein the fine acetone tower adopts an independent separated vacuum system, the vacuum jet steam condensate flows back into the fine acetone tower, the material discharged from the top of the crude acetone tower flows into the fine acetone tower, and the operating pressure of the fine acetone tower is reduced to 55 Kpa;
step S3: the oil extraction tower and the extraction oil alkaline washing tower of the OEC system are replaced, the recovery of phenol in the phenol-containing wastewater is carried out in the OEC system, the circulation amount of the extraction oil is increased from 20m3/h to 60m3/h, and the phenol content is reduced from 72g/l to 12 g/l; the method comprises the following steps of mixing wastewater containing sodium phenolate and sulfuric acid in a mixing tank, adding the mixture into an oil extraction tower, discharging the wastewater to a wastewater removal tank in the oil extraction tower, adding cumene and phenol into an extraction oil alkaline washing tower in the oil extraction tower, discharging the wastewater to a sodium phenolate removal wastewater tank after alkaline reaction is carried out in the extraction oil alkaline washing tower, discharging the cumene and water to a solvent tank in the extraction oil alkaline washing tower, discharging the wastewater in the solvent tank to the wastewater tank, and circulating the cumene to the oil extraction tower through a loop pipeline to be continuously used as an extracting agent.
Preferably, in step S1, the oxidation feed caustic tower in the oxidation feed caustic tower wastewater recovery process mixes fresh cumene, cumene in the hydrogenation unit and cumene in the concentration unit, and then adds water and alkali for washing, a wastewater outlet of the oxidation feed caustic tower is connected with a feed tank of the OEC system, the washed cumene mixture in the oxidation feed caustic tower is discharged into a receiving tank for further water diversion, the separated cumene mixture in the receiving tank is discharged into a coalescer, the cumene mixture is further diverted into a coalescer by the coalescer, and then the cumene is discharged out of the oxidizer for reaction.
Preferably, in step S2, in the vacuum discrete processing of the fine acetone tower, the fine acetone tower adds water and alkali to the crude acetone to process aldehyde impurities, cumene in a tower bottom tank of the fine acetone tower is removed from an alkali washing tower and water is removed from a wastewater tank, a condenser is installed on a pipeline between the fine acetone tower and a receiving tank, one end of the receiving tank returns to the fine acetone tower through the pipeline, the other end of the receiving tank is respectively connected with a total vacuum system for rectification and a discrete vacuum system, condensed water in the total vacuum system for rectification is removed from the wastewater tank, and condensed water in the discrete vacuum system is removed from the fine acetone tower.
The invention has the advantages and positive effects that:
1. the method recycles phenol in high-concentration wastewater through wastewater recycling treatment of the alkaline washing tower and wastewater recycling treatment measures of the oxidation feeding alkaline washing tower, and recycles 2.4 tons of phenol all the year round.
2. The invention reduces the acetone content in the wastewater in the tower bottom tank from 0.28% to 0.01% by adding the vacuum discrete treatment of the fine acetone tower and implementing the vacuum discrete measure of the fine acetone tower; 40.32 tons of acetone are recovered.
3. According to the invention, the OEC system oil extraction tower and the extraction oil alkaline tower are replaced, and the replaced OEC system oil extraction tower and the replaced extraction oil alkaline tower have the advantages that the extraction efficiency is improved, the COD concentration of the waste water of the oil extraction tower is reduced to below 2500mg/L from about 5000mg/L, the phenol content in the waste water is reduced to 40mg/L from 120mg/L, and 2.36 tons of phenol are recovered.
Drawings
Other objects and results of the present invention will become more apparent and more readily appreciated as the same becomes better understood by reference to the following description taken in conjunction with the accompanying drawings. In the drawings:
FIG. 1 is a schematic diagram of the structure of the wastewater recovery treatment of an oxidation feed caustic tower according to an embodiment of the invention.
Fig. 2 is a schematic view of a vacuum discrete processing structure of a fine acetone tower according to an embodiment of the invention.
FIG. 3 is a schematic diagram of an OEC system processing architecture according to an embodiment of the present invention.
Detailed Description
In the following description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of one or more embodiments. It may be evident, however, that such embodiment(s) may be practiced without these specific details. In other instances, well-known structures and devices are shown in block diagram form in order to facilitate describing one or more embodiments.
Example 1
Fig. 1-3 show an overall structural schematic according to an embodiment of the present invention.
As shown in fig. 1 to 3, the method for treating phenol-containing wastewater of a phenol acetone plant provided by the embodiment of the present invention includes the following steps:
step S1: recycling and treating the wastewater of the oxidation feeding alkaline washing tower, pumping the wastewater into an OEC system (a mixing tank before an oil extraction tower and an extraction oil alkaline washing tower are combined into the tower) by using a pump after the wastewater is connected with a phenolic wastewater tank in a C area by using a pipeline, wherein an alkaline washing circulating pump of the oxidation feeding alkaline washing tower is replaced by an alkaline washing circulating pump with the flow of 8m 3/h;
step S2: separating the fine acetone tower in vacuum, wherein the fine acetone tower adopts an independent separated vacuum system, the vacuum jet steam condensate flows back into the fine acetone tower, the material discharged from the top of the crude acetone tower flows into the fine acetone tower, and the operating pressure of the fine acetone tower is reduced to 55 Kpa;
step S3: the oil extraction tower and the extraction oil alkaline washing tower of the OEC system are replaced, the recovery of phenol in the phenol-containing wastewater is carried out in the OEC system, the circulation amount of the extraction oil is increased from 20m3/h to 60m3/h, and the phenol content is reduced from 72g/l to 12 g/l; the method comprises the following steps of mixing wastewater containing sodium phenolate and sulfuric acid in a mixing tank, adding the mixture into an oil extraction tower, discharging the wastewater to a wastewater removal tank in the oil extraction tower, adding cumene and phenol into an extraction oil alkaline washing tower in the oil extraction tower, discharging the wastewater to a sodium phenolate removal wastewater tank after alkaline reaction is carried out in the extraction oil alkaline washing tower, discharging the cumene and water to a solvent tank in the extraction oil alkaline washing tower, discharging the wastewater in the solvent tank to the wastewater tank, and circulating the cumene to the oil extraction tower through a loop pipeline to be continuously used as an extracting agent.
In step S1, in the oxidized feed caustic scrubber wastewater recovery process, fresh cumene, cumene in the hydrogenation unit and cumene in the concentration unit are mixed and then washed by adding water and alkali, a wastewater outlet discharged from the oxidized feed caustic scrubber is connected to a feed tank of the OEC system, the washed cumene mixture in the oxidized feed caustic scrubber is discharged into a receiving tank for further water diversion, the separated cumene mixture in the receiving tank is discharged into a coalescer for further water diversion, and the cumene mixture is discharged into the coalescer for further reaction.
In this embodiment, in step S2, in the vacuum discrete processing of the fine acetone tower, the fine acetone tower adds water and alkali to the crude acetone to process aldehyde impurities, cumene in a bottom tank of the fine acetone tower goes to an alkali washing tower and water goes to a wastewater tank, a condenser is installed on a pipeline between the fine acetone tower and a receiving tank, one end of the receiving tank returns to the fine acetone tower through the pipeline, the other end of the receiving tank is connected to a total vacuum system for rectification and a discrete vacuum system, condensed water in the total vacuum system for rectification goes to the wastewater tank, and condensed water in the vacuum system for rectification goes to the fine acetone tower.
Example 2
(1) Oxidized feed caustic wash tower wastewater
Phenol device COD monitoring data (steady state)
(2) Vacuum discrete pre-and post-data of fine acetone tower
Fine acetone tower waste water analysis data
The COD monitoring data method is based on the dichromate method GB11914-89 for determining the chemical oxygen demand of national standard water quality of the people's republic of China;
to obtain: after the project is implemented, the average value of COD (mg/L) of the wastewater of the refined acetone tower detected 12 times is 1769 which is far lower than the average value of COD (mg/L) of the wastewater of the refined acetone tower detected 12 times before the project is implemented, namely 6527.
To obtain: after the performance of the item, the average value of acetone (%) in the oil extraction column tested 12 times was 0.01 which was much lower than the average value of phenol (mg/L) in the oil extraction column tested 12 times (before the performance of the item), which was 0.28.
(3) oEC front and back data of oil extraction tower and extracted oil alkaline washing tower of system
Analytical data of oil extraction column
(Table 1)
The COD monitoring data method is based on the dichromate method GB11914-89 for determining the chemical oxygen demand of national standard water quality of the people's republic of China;
to obtain: after the experiment, the average value of COD (mg/L) of the oil extraction tower tested 12 times was 1942, which is much lower than the average value of COD (mg/L) of the oil extraction tower tested 12 times before the experiment, 3785.
To obtain: after the performance of the project, the average value of phenol (mg/L) measured in the oil extraction column 12 times was 50.25, which was much lower than the average value of phenol (mg/L) measured in the oil extraction column 12 times before the performance of the project 101.
Phenol plant waste water total outlet analysis data
(Table 2)
The COD monitoring data method is obtained according to a dichromate method GB11914-89 for determining the chemical oxygen demand of national standard water quality of the people's republic of China: after the project was performed, the average value of COD (mg/L) at the total outlet of the phenol plant wastewater detected 12 times was 1946.1, which was much lower than 9293 which was the average value of COD (mg/L) at the total outlet of the phenol plant wastewater detected 12 times before the project was performed.
After the company implements the treatment measures, the annual average benefit is 89.21 ten thousand yuan. And considerable economic benefit, environmental benefit and social benefit can be obtained with a small amount of investment.
Example 3
Phenol recovery station
Collecting the water-containing phenol discharged from each post into a sodium phenolate tank, standing for separation, taking oil phase impurities as a byproduct of the water-containing phenol, pumping the water-containing phenol from the sodium phenolate tank to a three-waste loading platform for loading and transporting, sending a water phase to a neutral phenol recovery post, extracting with cumene, discharging to the outside of a boundary area, and feeding into acid sewage of a factory, and decontaminating the water factory.
The water phase of the phenol-containing wastewater tank is pumped out by a wastewater pump, mixed with sulfuric acid injected into the tank from OEC acid and then enters an OEC mixing tank. After reaction, the material is extracted from the top oil-removing extraction tower with isopropyl benzene, the waste water is discharged directly to waste water collecting underground tank, isopropyl benzene as phenol-containing extractant is fed into extracted oil alkali washing tower, after phenol is washed away with 15% alkali solution, isopropyl benzene is collected in solvent tank for reuse, sodium phenolate liquid in extracted oil alkali washing tower is fed into sodium phenolate storage tank, the solvent tank is provided with separator, the unqualified solvent in the separator is discharged to sodium phenolate storage tank through underground tank at the post of recovering neutralized phenol periodically, when the content of isopropyl benzene in the solvent tank is less than or equal to 90%, the material is discharged to rectifying material feeding tank.
The waste water from oxidation concentration decomposition, neutralization phenol recovery and rectification is collected into a waste water collecting underground tank, pumped into an oil-water separator by a waste water underground tank pump, separated into a phenol-containing waste water tank or a sodium phenolate storage tank, and discharged to the outside of the boundary area to enter acid sewage of the factory for decontamination of the water factory.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. A phenol-containing wastewater treatment method of a phenol acetone device is characterized by comprising the following steps:
step S1: recycling waste water of the oxidation feeding alkaline washing tower, connecting the waste water tank containing phenol in the area C by using a pipeline, and pumping the waste water into an OEC system for treatment, wherein an alkaline washing circulating pump of the oxidation feeding alkaline washing tower is replaced by an alkaline washing circulating pump with the flow of 8m 3/h;
step S2: separating the fine acetone tower in vacuum, wherein the fine acetone tower adopts an independent separated vacuum system, the vacuum jet steam condensate flows back into the fine acetone tower, the material discharged from the top of the crude acetone tower flows into the fine acetone tower, and the operating pressure of the fine acetone tower is reduced to 55 Kpa;
step S3: the oil extraction tower and the extraction oil alkaline washing tower of the OEC system are replaced, the recovery of phenol in the phenol-containing wastewater is carried out in the OEC system, the circulation amount of the extraction oil is increased from 20m3/h to 60m3/h, and the phenol content is reduced from 72g/l to 12 g/l; the method comprises the following steps of mixing wastewater containing sodium phenolate and sulfuric acid in a mixing tank, adding the mixture into an oil extraction tower, discharging the wastewater to a wastewater removal tank in the oil extraction tower, adding cumene and phenol into an extraction oil alkaline washing tower in the oil extraction tower, discharging the wastewater to a sodium phenolate removal wastewater tank after alkaline reaction is carried out in the extraction oil alkaline washing tower, discharging the cumene and water to a solvent tank in the extraction oil alkaline washing tower, discharging the wastewater in the solvent tank to the wastewater tank, and circulating the cumene to the oil extraction tower through a loop pipeline to be continuously used as an extracting agent.
2. The phenol-containing wastewater treatment method of phenol-acetone plant according to claim 1, wherein in step S1, the oxidation feed caustic tower in the wastewater recovery treatment of oxidation feed caustic tower mixes the fresh cumene of the feed, the cumene of the hydrogenation unit and the cumene of the concentration unit, and then adds water and alkali for washing, a wastewater outlet of the oxidation feed caustic tower is connected to a feed tank of the OEC system, the washed cumene mixture in the oxidation feed caustic tower is discharged to a receiving tank for further water diversion, the fractionated cumene mixture in the receiving tank is discharged to a coalescer, the cumene mixture is further fractionated to the coalescer, and then the cumene mixture is discharged to the oxidizer for reaction.
3. The phenol-containing wastewater treatment method of a phenol-acetone plant according to claim 1, wherein in step S2, the fine acetone tower in the fine acetone tower vacuum discrete treatment adds water and alkali to the crude acetone to treat the aldehyde impurities, the cumene in the bottom tank of the fine acetone tower is used to remove the alkali washing tower and the water to remove the wastewater tank, a condenser is installed on the pipeline between the fine acetone tower and the receiving tank, one end of the receiving tank returns to the fine acetone tower through the pipeline, the other end of the receiving tank is connected with the total vacuum system for rectification and the discrete vacuum system respectively, the condensed water in the total vacuum system for rectification is removed from the wastewater tank, and the condensed water in the discrete vacuum system is removed to the fine acetone tower.
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| US20080281129A1 (en) * | 2007-05-09 | 2008-11-13 | Palmer David P | BPA Process Improvement |
| CN105819588A (en) * | 2016-04-01 | 2016-08-03 | 中国环境科学研究院 | Method for reducing pollutant discharge in phenol-acetone production |
| CN110228885A (en) * | 2019-04-30 | 2019-09-13 | 实友化工（扬州）有限公司 | A kind of sewage-treatment plant for phenol and acetone synthetic reaction |
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| US20080281129A1 (en) * | 2007-05-09 | 2008-11-13 | Palmer David P | BPA Process Improvement |
| CN105819588A (en) * | 2016-04-01 | 2016-08-03 | 中国环境科学研究院 | Method for reducing pollutant discharge in phenol-acetone production |
| CN110228885A (en) * | 2019-04-30 | 2019-09-13 | 实友化工（扬州）有限公司 | A kind of sewage-treatment plant for phenol and acetone synthetic reaction |
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