CN1450006A - Treatment of phenol containing decanedioic acid waste water by extractive distillation - Google Patents
Treatment of phenol containing decanedioic acid waste water by extractive distillation Download PDFInfo
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- CN1450006A CN1450006A CN 02110255 CN02110255A CN1450006A CN 1450006 A CN1450006 A CN 1450006A CN 02110255 CN02110255 CN 02110255 CN 02110255 A CN02110255 A CN 02110255A CN 1450006 A CN1450006 A CN 1450006A
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Abstract
The method for treating waste water containing phenol which is produced in the course of producing sebacic acid includes five steps: regulation, filtration, extraction, removing phenol and isolating oil. After the phenol-containing waste water is filtered and its insoluble material is removed, in first extraction zone the high carbon alcohol is used as extraction agent to remove the organic material from waste water and effectively reduce content of phenol, the load extraction agent is fed into distillation procedure, the distilled high carbon alcohol can be reextracted and can be circularly used, and the organic material being in the waste water can be recovered in the form of high-boiling material, and the second extraction zone the mixture of phosphate and kerosene is used as extraction agent to make counter-current extraction with the phenol-containing waster water.
Description
Technical field
The present invention relates to a kind of wastewater treatment method, the method for the phenolic wastewater that to be a kind of processing specifically produce in the process of producing sebacic acid.
Technical background
In the production process of sebacic acid,, a certain amount of phenolic wastewater discharging there is every day because the needs of production technique need add phenol as thinner and catalyzer.The sebacic acid manufacturer in the whole nation does not all have good way.Commonly used have ricinolic acid extraction process and complexing abstraction, but because the partition ratio of ricinolic acid extraction phenol is lower, weak effect, solution loss is big in the water, and the content of the waste water phenol after the processing is up to 200PPM, and is not up to standard; Complexing abstraction is owing to be dissolved with large amount of organic in the sebacic acid phenolic wastewater, and back extraction generation saponification, extraction can't recycles, and the running cost height can't be applied.
Summary of the invention
The method that the purpose of this invention is to provide the processing sebacic acid phenolic wastewater that a kind of working cost is low, treatment effect is good, i.e. treatment of phenol containing decanedioic acid waste water by extractive distillation.
For achieving the above object, the present invention adopts following technical scheme:
Treatment of phenol containing decanedioic acid waste water by extractive distillation of the present invention is that the phenolic wastewater after sedimentation is filtered is handled with following steps:
(1) extraction, the waste water after the filtration are with being pumped into first extraction section, and in first extraction section, with B extraction agent and phenolic wastewater counter-current extraction, the volume ratio of B extraction agent and phenolic wastewater is 1: 30-50, and temperature is 10-50 ℃; The raffinate of first extraction section is delivered to second extraction section, and at the raffinate counter-current extraction of second extraction section with the A extraction agent and first extraction section, the volume ratio of A extraction agent and phenolic wastewater is 1: 30-50, and temperature is 10-50 ℃; The raffinate of second extraction section is put to oil trap, qualified discharge after the de-oiling, and the extraction liquid of first extraction section and second extraction section enters phenol removal process;
(2) dephenolize, the extraction liquid that first extraction section is emitted enters Distallation systm, at pressure is-0.09Mpa-0Mpa, temperature is under 80-170 ℃ the condition, distillation removes organism, and with being pumped into soda-wash tower, the sodium hydroxide solution with 5-30% in soda-wash tower carries out the dephenolize processing again; The extraction liquid that second extraction section is emitted directly enters soda-wash tower, carries out dephenolize with the sodium hydroxide solution of 5-30% and handles;
(3) oil removal utilizes the difference in specific gravity that exists naturally between the solvent oil and water in the raffinate, under 0.5-1.5 hour sluggish flow condition, allow it float to the water surface naturally, after oil slick reaches certain thickness, operation oil skimming pipe, by oil header, this part oil distillation back reuse of collecting.
Described A extraction agent is the mixture of phosphoric acid ester and kerosene, and wherein the content of phosphoric acid ester is 5-50% (weight ratio); The B extraction agent is higher alcohols (C5-C10).
Above-mentioned phenolic wastewater before entering first extraction section through overregulating and filtration treatment, the so-called adjusting is meant that the phenolic wastewater from the sebacic acid workshop at first enters the adjusting storage tank, in groove, stay for some time, be beneficial to the equilibrium of water quality, the water yield, for subsequent disposal is got ready; The so-called filtration is under the pressure of normal temperature and 0.2-0.35Mpa, adopts plate-and-frame filter press to filter the solid impurity that contains in the waste water after the sedimentation, compresses automatically, and filter residue is recycled with the form of filter cake.
After phenolic wastewater removes by filter insolubles, remove the organism in the waste water with higher alcohols as extraction agent and effectively reduce the content of phenol in first extraction section, the load extraction agent removes distillation process, recycle after the higher alcohols back extraction that steams, organism in the waste water reclaims with the form of high boiling material, recycle after the extraction agent back extraction after second extraction section is made extraction agent and phenolic wastewater counter-current extraction with the mixture of phosphoric acid ester and kerosene, be saturated, the discharged wastewater met the national standard after the extraction.
Adopt above-mentioned technology, the sebacic acid phenolic wastewater is the recovery part sebacic acid after sedimentation, filtration, extracts the organism of removing in the waste water with higher alcohols, dissolved organic matter is separated, the saponification reaction when having avoided the extraction agent back extraction from waste water.Can reduce to below the 2.0mg/l by 2000-2500mg/l through counter-current extraction sebacic acid phenolic wastewater phenol content, reach three grades of emission standards of national regulation.Because a large amount of phenol have been reclaimed in extraction, the processing working cost is reduced greatly.Economic benefit, environmental benefit are obvious.
Description of drawings
Accompanying drawing is the process flow sheet of one embodiment of the present of invention.
Specific embodiment
Embodiment 1:
Treatment of phenol containing decanedioic acid waste water by extractive distillation of the present invention comprises the steps:
1, regulates.Discharging rule, water quality difference because of workshop waste water, for guarantee that subsequent treatment process can move under a more stable operating mode, to obtain higher removal, phenolic wastewater from the sebacic acid workshop at first enters the adjusting storage tank, in groove, stay for some time, be beneficial to the equilibrium of water quality, the water yield, for subsequent disposal is got ready.Certainly,, or obtained other forms of adjusting, also can omit this step if the water quality of waste water, the water yield are relatively more balanced.
2, filter.Contain solid impurity in the waste water after the sedimentation, under the pressure of normal temperature and 0.2-0.35Mpa, adopt plate-and-frame filter press to filter, compress automatically, filter residue is recycled with the form of filter cake.Certainly, also can adopt other filter method, as long as the solid impurity in the waste water can be removed.
3, extraction.Waste water after the filtration in first extraction section, is made extraction agent and phenolic wastewater counter-current extraction with higher alcohols (C5) with being pumped into first extraction section, and the volume ratio of extraction agent and phenolic wastewater is 1: 30, and temperature is 20 ℃; Raffinate is delivered to second extraction section, make the raffinate counter-current extraction of the extraction agent and first extraction section with the mixture of organophosphate and kerosene in second extraction section, the volume ratio of extraction agent and phenolic wastewater is 1: 30, and temperature is 20 ℃, and the weight content of phosphoric acid ester is 5% in the extraction agent.Raffinate is put to oil trap, qualified discharge after the de-oiling.The extraction liquid of two extraction section enters phenol removal process.
4, dephenolize.The extraction liquid that first extraction section is emitted enters Distallation systm, and at pressure-0.09Mpa, under 80 ℃ of the temperature, distillation removes organism, and with being pumped into soda-wash tower, the sodium hydroxide solution with 5% in soda-wash tower carries out the dephenolize processing again; The extraction liquid that second extraction section is emitted directly enters the soda-wash tower dephenolize and handles, and the sodium hydroxide solution with 5% in soda-wash tower carries out dephenolize processing, the equal recycle of the extraction liquid after the dephenolize.The saturated sodium phenolate of emitting from soda-wash tower is flowed to the phenates groove, and the sulfuric acid acidation distillation with 50% obtains crude phenols and returns the utilization of sebacic acid workshop.
5, oil removal.Utilize the difference in specific gravity that exists naturally between the solvent oil and water in the raffinate, under the sluggish flow condition of certain hour (about 1.5 hours), allow it float to the water surface naturally, after oil slick reaches certain thickness, operation oil skimming pipe, by oil header, this part oil distillation back reuse of collecting.
Embodiment 2:
The process of adjusting, filtration and oil removal is with embodiment 1.
3, extraction.Waste water after the filtration in first extraction section, is made extraction agent and phenolic wastewater counter-current extraction with higher alcohols (C8) with being pumped into first extraction section, and the volume ratio of extraction agent and phenolic wastewater is 1: 40, and temperature is 30 ℃; Raffinate is delivered to second extraction section, make the raffinate counter-current extraction of the extraction agent and first extraction section with the mixture of organophosphate and kerosene in second extraction section, the volume ratio of extraction agent and phenolic wastewater is 1: 40, and temperature is 30 ℃, and the weight content of phosphoric acid ester is 20% in the extraction agent.Raffinate is put to oil trap, qualified discharge after the de-oiling.The extraction liquid of two extraction section enters phenol removal process.
4, dephenolize.The extraction liquid that first extraction section is emitted enters Distallation systm, and at pressure-0.01Mpa, under 100 ℃ of the temperature, distillation removes organism, and with being pumped into soda-wash tower, the sodium hydroxide solution with 10% in soda-wash tower carries out the dephenolize processing again; The extraction liquid that second extraction section is emitted directly enters the soda-wash tower dephenolize and handles, and the sodium hydroxide solution with 10% in soda-wash tower carries out dephenolize processing, the equal recycle of the extraction liquid after the dephenolize.The saturated sodium phenolate of emitting from soda-wash tower is flowed to the phenates groove, and the sulfuric acid acidation distillation with 70% obtains crude phenols and returns the utilization of sebacic acid workshop.
Embodiment 3:
The process of adjusting, filtration and oil removal is with embodiment 1.
3, extraction.Waste water after the filtration in first extraction section, is made extraction agent and phenolic wastewater counter-current extraction with higher alcohols (C10) with being pumped into first extraction section, and the volume ratio of extraction agent and phenolic wastewater is 1: 50, and temperature is 45 ℃; Raffinate is delivered to second extraction section, make the raffinate counter-current extraction of the extraction agent and first extraction section with the mixture of organophosphate and kerosene in second extraction section, the volume ratio of extraction agent and phenolic wastewater is 1: 50, and temperature is 45 ℃, and the weight content of phosphoric acid ester is 50% in the extraction agent.Raffinate is put to oil trap, qualified discharge after the de-oiling.The extraction liquid of two extraction section enters phenol removal process.
4, dephenolize.The extraction liquid that first extraction section is emitted enters Distallation systm, and at pressure 0Mpa, under 170 ℃ of the temperature, distillation removes organism, and with being pumped into soda-wash tower, the sodium hydroxide solution with 30% in soda-wash tower carries out the dephenolize processing again; The extraction liquid that second extraction section is emitted directly enters the soda-wash tower dephenolize and handles, and the sodium hydroxide solution with 30% in soda-wash tower carries out dephenolize processing, the equal recycle of the extraction liquid after the dephenolize.The saturated sodium phenolate of emitting from soda-wash tower is flowed to the phenates groove, and the sulfuric acid acidation distillation with 90% obtains crude phenols and returns the utilization of sebacic acid workshop.
Claims (3)
1, treatment of phenol containing decanedioic acid waste water by extractive distillation is characterized in that: the phenolic wastewater after sedimentation is filtered is handled with following steps,
(1) extraction, waste water are with being pumped into first extraction section, and in first extraction section, with B extraction agent and phenolic wastewater counter-current extraction, the volume ratio of B extraction agent and phenolic wastewater is 1: 30-50, and temperature is 10-50 ℃; The raffinate of first extraction section is delivered to second extraction section, and at the raffinate counter-current extraction of second extraction section with the A extraction agent and first extraction section, the volume ratio of the raffinate of the A extraction agent and first extraction section is 1: 30-50, and temperature is 10-50 ℃; The raffinate of second extraction section is put to oil trap, enters the oil removal operation, qualified discharge after the de-oiling, and the extraction liquid of first extraction section and second extraction section enters phenol removal process;
(2) dephenolize, the extraction liquid that first extraction section is emitted enters Distallation systm, at pressure is-0.09Mpa-0Mpa, temperature is under 80-170 ℃ the condition, distillation removes organism, and with being pumped into soda-wash tower, the sodium hydroxide solution with 5-30% in soda-wash tower carries out the dephenolize processing again; The extraction liquid that second extraction section is emitted directly enters soda-wash tower, carries out dephenolize with the sodium hydroxide solution of 5-30% and handles;
(3) oil removal utilizes the difference in specific gravity that exists naturally between the solvent oil and water in the raffinate, under 0.5-1.5 hour sluggish flow condition, allow it float to the water surface naturally, after oil slick reaches certain thickness, operation oil skimming pipe, by oil header, this part oil distillation back reuse of collecting.
2, treatment of phenol containing decanedioic acid waste water by extractive distillation according to claim 1 is characterized in that: described A extraction agent is the mixture of phosphoric acid ester and kerosene, and wherein the content of phosphoric acid ester is 5-50% (weight ratio); The B extraction agent is higher alcohols (C5-C10).
3, treatment of phenol containing decanedioic acid waste water by extractive distillation according to claim 1, it is characterized in that: phenolic wastewater before entering first extraction section through overregulating and filtration treatment, the so-called adjusting is meant that the phenolic wastewater from the sebacic acid workshop at first enters the adjusting storage tank, in groove, stay for some time, reach the equilibrium of water quality, the water yield; The so-called filtration is under the pressure of normal temperature and 0.2-0.35Mpa, adopts plate-and-frame filter press to filter the solid impurity that contains in the waste water after the sedimentation, compresses automatically, and filter residue is recycled with the form of filter cake.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 02110255 CN1450006A (en) | 2002-04-05 | 2002-04-05 | Treatment of phenol containing decanedioic acid waste water by extractive distillation |
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| CN 02110255 CN1450006A (en) | 2002-04-05 | 2002-04-05 | Treatment of phenol containing decanedioic acid waste water by extractive distillation |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654305B (en) * | 2009-09-18 | 2011-11-09 | 清华大学 | Process for changing phenolic nitrate effluent into useful material by extracting, evaporating, crystallizing and coupling |
| CN102311195A (en) * | 2011-06-24 | 2012-01-11 | 扬州大学 | Recycling utilization and processing method for wastewater generated in sebacic acid production process |
| CN102351357A (en) * | 2011-06-24 | 2012-02-15 | 扬州大学 | Resource utilization of waste water containing phenol and sodium sulfate and treating method |
| CN102372378A (en) * | 2011-10-10 | 2012-03-14 | 山东天兴生物科技有限公司 | Treatment method of waste water produced by adopting castor oil to prepare decanedioic acid |
| CN102503034A (en) * | 2011-11-08 | 2012-06-20 | 中蓝连海设计研究院 | Treatment method of phenol-containing liquid waste in sebacic acid production |
| CN102745760A (en) * | 2011-10-25 | 2012-10-24 | 河北凯徳生物材料有限公司 | Waste water treatment process in sebacic acid production |
| CN103073084A (en) * | 2011-10-25 | 2013-05-01 | 河北凯徳生物材料有限公司 | Treatment process for phenolic wastewater generated in production of sebacic acid |
| CN103787542A (en) * | 2014-01-28 | 2014-05-14 | 广州新普利节能环保科技有限公司 | Process and device for recovering and treating wastewater generated by preparing sebacic acid with castor oil |
| CN104609641A (en) * | 2013-11-05 | 2015-05-13 | 中蓝连海设计研究院 | Sebacic acid wastewater evaporative desalination pretreatment method |
| CN104609541A (en) * | 2013-11-05 | 2015-05-13 | 中蓝连海设计研究院 | Sebacic acid wastewater direct biochemical treatment method without desalination |
-
2002
- 2002-04-05 CN CN 02110255 patent/CN1450006A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654305B (en) * | 2009-09-18 | 2011-11-09 | 清华大学 | Process for changing phenolic nitrate effluent into useful material by extracting, evaporating, crystallizing and coupling |
| CN102351357B (en) * | 2011-06-24 | 2012-10-17 | 扬州大学 | Resource utilization of waste water containing phenol and sodium sulfate and treating method |
| CN102311195A (en) * | 2011-06-24 | 2012-01-11 | 扬州大学 | Recycling utilization and processing method for wastewater generated in sebacic acid production process |
| CN102351357A (en) * | 2011-06-24 | 2012-02-15 | 扬州大学 | Resource utilization of waste water containing phenol and sodium sulfate and treating method |
| CN102372378A (en) * | 2011-10-10 | 2012-03-14 | 山东天兴生物科技有限公司 | Treatment method of waste water produced by adopting castor oil to prepare decanedioic acid |
| CN102745760A (en) * | 2011-10-25 | 2012-10-24 | 河北凯徳生物材料有限公司 | Waste water treatment process in sebacic acid production |
| CN103073084A (en) * | 2011-10-25 | 2013-05-01 | 河北凯徳生物材料有限公司 | Treatment process for phenolic wastewater generated in production of sebacic acid |
| CN102503034A (en) * | 2011-11-08 | 2012-06-20 | 中蓝连海设计研究院 | Treatment method of phenol-containing liquid waste in sebacic acid production |
| CN102503034B (en) * | 2011-11-08 | 2013-06-19 | 中蓝连海设计研究院 | Treatment method of phenol-containing liquid waste in sebacic acid production |
| CN104609641A (en) * | 2013-11-05 | 2015-05-13 | 中蓝连海设计研究院 | Sebacic acid wastewater evaporative desalination pretreatment method |
| CN104609541A (en) * | 2013-11-05 | 2015-05-13 | 中蓝连海设计研究院 | Sebacic acid wastewater direct biochemical treatment method without desalination |
| CN104609541B (en) * | 2013-11-05 | 2016-05-25 | 中蓝连海设计研究院 | The direct biochemical processing method of a kind of decanedioic acid not desalination of waste water |
| CN104609641B (en) * | 2013-11-05 | 2017-02-15 | 中蓝连海设计研究院 | Sebacic acid wastewater evaporative desalination pretreatment method |
| CN103787542A (en) * | 2014-01-28 | 2014-05-14 | 广州新普利节能环保科技有限公司 | Process and device for recovering and treating wastewater generated by preparing sebacic acid with castor oil |
| CN103787542B (en) * | 2014-01-28 | 2015-09-30 | 广州新普利节能环保科技有限公司 | The wastewater recovery processing technique that a kind of Preparation of Sebacic Acid From Castor Oil produces and device |
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