CN102107924A - Method for comprehensively recovering and treating furfural industrial wastewater - Google Patents
Method for comprehensively recovering and treating furfural industrial wastewater Download PDFInfo
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- CN102107924A CN102107924A CN200910263917XA CN200910263917A CN102107924A CN 102107924 A CN102107924 A CN 102107924A CN 200910263917X A CN200910263917X A CN 200910263917XA CN 200910263917 A CN200910263917 A CN 200910263917A CN 102107924 A CN102107924 A CN 102107924A
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Abstract
The invention discloses a method for comprehensively recovering and treating furfural industrial wastewater. The method comprises the following steps of: performing pre-extraction by using a polypropylene hollow fibrous membrane contactor serving as extraction equipment; allowing a pre-extraction residual phase obtained in the last step to enter a filler extraction tower to perform complexometric extraction; separating the obtained extraction phase by a reduced pressure rectification method to obtain aqueous solution of concentrated acetic acid and recover the extracting agent; and allowing the obtained extraction residual phase serving as material liquid to pass through a microporous hydrophobic hollow fibrous membrane contactor to perform posttreatment, wherein the posttreatment extracting agent is a low-boiling-point, low-viscosity and low-water-solubility nonpolar organic solvent; and in the microporous hydrophobic hollow fibrous membrane contactor, the membrane yarn internal diameter is 0.1 to 0.5 mm, the wall thickness is 50 to 200 mu m, and the membrane microporous aperture is 0.01 to 0.2 mu m. By the method, complexometric extraction efficiency can be improved; and economic and environmentally-friendly values are achieved in the furfural wastewater treatment.
Description
Technical field
The present invention relates to a kind of trade effluent recovery and treatment method, the comprehensive recovery and treatment method of specifically a kind of industrial wastewater from furfural production.
Background technology
Furfural claims furtural again, is important heterocyclic organic compound, also is important chemical material.China's furfurol industry is raw material mostly with the corn cob, ton surplus the annual production about 50,000.Furfural production is to obtain project than the large economy benefit with less economy input, for revitalize regional economy, promoting social development all has very important meaning.But the industrial wastewater pollution of furfural production has become the bottleneck of restriction the sector development.
Furfural waste-water contains 1.0%～2.5% acetic acid mainly from waste water under the tower in the waste water, 0.2%～0.5% furfural and multiple organic compound are turbid shape under the normal temperature, the organic pollution load height, and COD is about 20000mg/L, and BOD is about 5000mg/L, and SS is about 250mg/L.This waste water do not processed directly efflux, must make water body suffer severe contamination, destroyed environmental structure, the ecological flat Heng and the HUMAN HEALTH of water system caused detrimentally affect, fowl, poultry of drinking polluted-water and the farm crop of using polluted-water to irrigate have been caused great harm.Therefore, the waste water of furfural production eliminating must could discharge after treatment.
Acetic acid in the furfural waste-water is a kind of important basic chemical industry raw material, because acetic acid dilute solution recovery value is little, part enterprise is not to its processing and reclaim just directly discharging, not only causes environmental pollution but also waste resource.At present, a lot of researchs are arranged about the recycling of dilute acetic acid solution, traditional alkali neutralization, absorption chemical method such as grade and biological process all just lay particular emphasis on the improvement to waste water, and have ignored the recycling of waste water; The easily contaminated or obstruction of film in the electroosmose process operating process, the deposition fouling of suspended substance easily makes the current skewness, and resistance increases, and causes polarization, and the changeable easy oxypolymerization of furfural chemical property, and electroosmose process is difficult to adapt to; The method of simple distillation and physical extraction will be removed the very low acetic acid of concentration in the waste water, and its energy consumption is too big and the rate of recovery is all too low.
At present the complexing abstraction that uses in the actual production is handled the technology that reclaims acetic acid containing waste water and is had following defective: the one, owing to contain stripping stage is carried secretly in the furfural production process a small amount of macromolecule organic such as higher alcohols, high carbon acid in the waste water, or organism such as high-carbon ester produces diluting effect to complexing extractant, influences the extraction ability of complexing extractant; The 2nd, this complexing abstraction is that direct liquid-liquid disperses and polymerization process, meticulous drop easily causes and carries secretly, thereby make a certain amount of extraction agent dissolving, emulsification form small emulsion droplet and become entrained in the extracting phase, this can cause the waste of expensive extraction agent on the one hand, on the other hand, can make increase pollution factor in the waste water and influence wastewater treatment efficiency.Above-mentioned reason causes in the industrial wastewater from furfural production processing and exists the complexing extractant extraction efficiency on the low side, and the economic benefit that entrainment loss caused of complexing extractant reduces and the problem of secondary environmental pollution is a urgent problem in the furfurol industry production link.
Summary of the invention
Purpose of the present invention just provides the comprehensive recovery and treatment method of a kind of industrial wastewater from furfural production, to improve complexometric extraction efficient, makes industrial wastewater from furfural production handle and really has the economy and the value of environmental protection.
The present invention is achieved in that
The comprehensive recovery and treatment method of this industrial wastewater from furfural production may further comprise the steps:
A, employing polypropylene hollow fiber membrane contactor extract in advance as extraction equipment, and furfural waste-water flows in the tube side of described membrane contactor, and pre-extraction agent flows both countercurrent flows in the shell side of described membrane contactor; The pre-extraction phase of gained contains the macromolecule organic in pre-extraction agent and the industrial wastewater from furfural production;
The pre-extracting phase of b, a step gained enters packed extraction tower and carries out complexometric extraction; The gained extraction phase obtains dense aqueous acetic acid with the separation of rectification under vacuum method, reclaims extraction agent;
C, b step gained extracting phase carries out aftertreatment as feed liquid through the microporous hydrophobic hollow fiber membrane contactors, described feed liquid flows in the tube side of this microporous hydrophobic hollow fiber membrane contactors, and the aftertreatment extraction agent flows in the shell side of this microporous hydrophobic hollow fiber membrane contactors; It is characterized in that the aftertreatment extraction agent is the non-polar organic solvent of lower boiling, low viscosity, low water solubility; The film silk internal diameter of described microporous hydrophobic hollow fiber membrane contactors is 0.1～0.5mm, and wall thickness is 50～200 μ m, and membrane micropore directly is 0.01～0.2 μ m.
In the method for the present invention, before a step employing polypropylene hollow fiber membrane contactor extracts in advance as extraction equipment, can earlier the furfural waste-water temperature be heated to 40 ℃, then impurity such as the solid particulate in the combination of one or more in methods such as sand filtration, micro-filtration, ultrafiltration, charcoal absorption and the resins exchange removal water, suspended substance.The furfural waste-water of removing impurity through pre-treatment extracts in described membrane contactor in advance.Pre-extraction agent can be any one or a few the mixture in the organic solvents such as low-density oil ether, normal hexane, N-BUTYL ACETATE.The pre-extraction phase of this step gained goes out macromolecule organic and reclaims pre-extraction agent through normal pressure rectifying is separable, and the pre-extraction agent of recovery can recirculation use.
The inventive method b is in the step, and the pre-extracting phase of a step gained adopts complexing extractant to extract through packed extraction tower, separates the acetic acid in the waste water.In order to improve the extraction efficiency of extraction tower, can in extraction tower, add air pulse or pulse of nitrogen.Extraction agent is the tertiary amines complexing extractant, and complexing extractant comprises extraction agent, conditioning agent and thinner three parts; Extraction agent is the tertiary amine of carbon 8～carbon 10, and conditioning agent is mainly the higher alcohols that contain n-Octanol, and thinner is a kerosene.During extraction, because the density of furfural waste-water is greater than the density of extraction agent, waste water enters from cat head in extraction tower and flows downward, extraction agent charging at the bottom of the tower is upwards flowed, in filling surface extraction agent and the abundant contact mass transfer of waste water process, obtain extraction phase and extracting phase at the bottom of cat head and the tower respectively, the extraction efficiency in the extraction process is greater than 98.5%.
This step gained extraction phase separates through the rectification under vacuum method, obtains acetate concentration and is 40～50% the aqueous solution, and be recovered to extraction agent.
Since contain formic acid in the furfural waste-water, low-carbon (LC) carboxylic acids such as acetate, and under long-time high-temperature operation, the n-Octanol in aforementioned low-carbon (LC) carboxylic acid and the extraction agent might react the generation ester, and the extraction activity of ester is much smaller than the extraction activity of n-Octanol.For this reason, use the extraction agent mixing solutions of for some time to strip, thereby purpose is to make the hydrolysis such as methyl ethyl of n-Octanol formation recover the characteristic of the auxiliary complexometric extraction of n-Octanol with the sodium hydroxide hydrothermal solution.
In order to obtain pure acetate products, the concentration that obtains is that 40～50% aqueous acetic acid needs through rectifying to obtain product purity greater than 98% acetic acid again.
C of the present invention carries out aftertreatment to b step gained extracting phase in the step.The microporous hydrophobic hollow-fibre membrane can be polypropylene, polyvinylidene difluoride (PVDF) or tetrafluoroethylene microporous hydrophobic hollow-fibre membrane in this step.The aftertreatment extraction agent that uses is any one or a few the mixture in the organic solvents such as low-density oil ether, normal hexane, N-BUTYL ACETATE.In the Membrane Extraction in this step, feed liquid and extraction agent two-phase and stream or adverse current all can, need to guarantee that feed liquid side static pressure be slightly larger than extraction agent side static pressure, but pressure reduction is no more than and penetrates pressure.So, be beneficial to the carrying out of Separation and Recovery.Extractant concentration in the waste water after this step handles can be reduced to 100ppm even lower.The aftertreatment extraction phase that this step separates can separate and recovery complexing extractant and aftertreatment extraction agent through rectifying, and the complexing extractant of recovery can join b to be continued in the step to use.
Method of the present invention compared with prior art has following advantage:
1. before entering packed extraction tower and carrying out complexometric extraction, industrial wastewater from furfural production is extracted in advance removing higher alcohols, the high carbon acid that stripping stage is carried secretly in the furfural production process, or a small amount of macromolecule organic such as high-carbon ester.High-molecular-weight organic material content in the industrial wastewater from furfural production after this pre-extraction treatment reduces greatly, therefore can not cause obvious influence to the performance of the extraction agent in next step the complexation extraction, thereby obviously improve the utilization ratio of extraction agent in the complexometric extraction.
2. after carrying out complexometric extraction, adopt film silk internal diameter little to the furfural waste-water extracting phase to 0.1～0.5mm, wall thickness is 50～200 μ m, membrane micropore directly is that the hollow fiber membrane contactors of 0.01～0.2 μ m carries out membrane extraction, thereby not only reclaimed the extraction agent that is dissolved in the waste water, and make the organic concentration in the waste water can reduce to 100ppm even lower, make the easier reuse up to standard of waste water.The present invention adopts the principle of membrane extraction high efficiente callback complexing extractant to be: when feed liquid flows in the tube side of the hollow-fibre membrane of above-mentioned size, the small emulsion droplet of the minimal amounts of dissolved in the feed liquid, emulsive complexing extractant has more, and multimachine can contact with the membranous wall of hydrophobic microporous, in case this contact takes place, under the effect of interfacial tension, thereby reach the purpose of Separation and Recovery complexing extractant from extracting phase in the extraction agent of the low viscosity of these small emulsion droplets in can very fast remittance membrane micropore, low surface tension.
Embodiment
The present invention will be further described below by embodiment
Embodiment 1:
With acetate concentration is that 1.65% furfural waste-water is a raw material, and waste water is heated to 40 ℃ (if the furfural waste-water self-temperature at 40 ℃～60 ℃, can directly advance pretreatment system without interchanger) through interchanger.Impurity such as the solid particulate in pre-treatment (sand filtration, micro-filtration) removal waste water, suspended substance; Flow in the tube side of membrane contactor through pretreated furfural waste-water, flow is 200ml/min, and pre-extraction agent low-density oil ether flows in the shell side of described membrane contactor, and flow is 150ml/min.The film silk internal diameter of described membrane contactor is 0.38mm, and wall thickness is 150 μ m, and membrane micropore directly is 0.01 μ m, through having removed a spot of macromolecule organic in the waste water after the pre-extraction, as higher alcohols, high carbon acid or high-carbon ester etc.
Enter and carry out complexometric extraction in the packed extraction tower through pre-stripped waste water, furfural waste-water enters from the filler extraction column overhead and flows downward, and complexing extractant charging at the bottom of the tower is upwards flowed.Be in a ratio of 0.7 (extraction agent mass rate: wastewater quality flow=7: 10), in filling surface extraction agent and the abundant contact mass transfer of waste water process, obtain extraction phase and extracting phase at the bottom of cat head and the tower respectively, extraction efficiency in the extraction process is 99.6%, after extraction, the acetate concentration in the furfural waste-water becomes 0.012%.
The extracting phase of at the bottom of the filler extraction Tata, collecting (extractant concentration is through being measured as 4324.5ppm), measurement is carried out aftertreatment as feed liquid through the microporous hydrophobic hollow fiber membrane contactors, described feed liquid flows in the tube side of this microporous hydrophobic hollow fiber membrane contactors, and flow is 120ml/min; The aftertreatment extraction agent flows in the shell side of this microporous hydrophobic hollow fiber membrane contactors; Flow is 60ml/min, and the aftertreatment extraction agent is a normal hexane; The film silk internal diameter of described microporous hydrophobic hollow fiber membrane contactors is 0.28mm, and wall thickness is 50 μ m, and membrane micropore directly is 0.01 μ m.Extractant concentration in the waste water after treatment is through being measured as 116ppm, and only needing again can reuse up to standard through simple biochemical treatment.
The comparative example 1
With acetate concentration is that 1.65% furfural waste-water is a raw material, carries out complexometric extraction in the packed extraction tower through directly entering after the pre-treatment, and preprocessing process is with embodiment 1.
Furfural waste-water enters from the filler extraction column overhead and flows downward, and complexing extractant charging at the bottom of the tower is upwards flowed.Be in a ratio of 0.7 (extraction agent mass rate: wastewater quality flow=7: 10), in filling surface extraction agent and the abundant contact mass transfer of waste water process, obtain extraction phase and extracting phase at the bottom of cat head and the tower respectively, extraction efficiency in the extraction process is 98.5%, after extraction, the acetate concentration in the furfural waste-water becomes 0.023%.
The extracting phase of collecting at the bottom of the filler extraction Tata (extractant concentration is through being measured as 4638.4ppm) carries out aftertreatment as feed liquid through the microporous hydrophobic hollow fiber membrane contactors, described feed liquid flows in the tube side of this microporous hydrophobic hollow fiber membrane contactors, and flow is 120ml/min; The aftertreatment extraction agent flows in the shell side of this microporous hydrophobic hollow fiber membrane contactors; Flow is 60ml/min, and the aftertreatment extraction agent is a normal hexane; The film silk internal diameter of described microporous hydrophobic hollow fiber membrane contactors is 0.8mm, and wall thickness is 150 μ m, and membrane micropore directly is 0.02 μ m.Extractant concentration in the waste water after treatment is through being measured as 132ppm.
Embodiment 2:
With acetate concentration is that 2.06% furfural waste-water is a raw material, and waste water is heated to 40 ℃ (if the furfural waste-water self-temperature at 40 ℃～60 ℃, can directly advance pretreatment system without interchanger) through interchanger.Impurity such as the solid particulate in pre-treatment (sand filtration, micro-filtration) removal waste water, suspended substance; Flow in the tube side of membrane contactor through pretreated furfural waste-water, flow is 200ml/min, and pre-extraction agent low-density oil ether flows in the shell side of described membrane contactor, and flow is 150ml/min.The film silk internal diameter of described membrane contactor is 0.38mm, and wall thickness is 150 μ m, and membrane micropore directly is 0.01 μ m, through having removed a spot of macromolecule organic in the waste water after the pre-extraction, as higher alcohols, high carbon acid or high-carbon ester etc.
Enter and carry out complexometric extraction in the packed extraction tower through pre-stripped waste water, furfural waste-water enters from the filler extraction column overhead and flows downward, and complexing extractant charging at the bottom of the tower is upwards flowed.Be in a ratio of 0.6 (extraction agent mass rate: wastewater quality flow=6: 10), in filling surface extraction agent and the abundant contact mass transfer of waste water process, obtain extraction phase and extracting phase at the bottom of cat head and the tower respectively, extraction efficiency in the extraction process is 98.7%, after extraction, the acetate concentration in the furfural waste-water becomes 0.015%.
The extracting phase of at the bottom of the filler extraction Tata, collecting (extractant concentration is through being measured as 4356.5ppm), measurement is carried out aftertreatment as feed liquid through the microporous hydrophobic hollow fiber membrane contactors, described feed liquid flows in the tube side of this microporous hydrophobic hollow fiber membrane contactors, and flow is 120ml/min; The aftertreatment extraction agent flows in the shell side of this microporous hydrophobic hollow fiber membrane contactors; Flow is 60ml/min, and the aftertreatment extraction agent is a normal hexane; The film silk internal diameter of described microporous hydrophobic hollow fiber membrane contactors is 0.28mm, and wall thickness is 100 μ m, and membrane micropore directly is 0.01 μ m.Extractant concentration in the waste water after treatment is through being measured as 87ppm, and only needing again can reuse up to standard through simple biochemical treatment.
The comparative example 2
With acetate concentration is that 2.06% furfural waste-water is a raw material, and waste water is heated to 40 ℃ (if the furfural waste-water self-temperature at 40 ℃～60 ℃, can directly advance pretreatment system without interchanger) through interchanger.Impurity such as the solid particulate in pre-treatment (sand filtration, micro-filtration) removal waste water, suspended substance; Flow in the tube side of membrane contactor through pretreated furfural waste-water, flow is 200ml/min, and pre-extraction agent low-density oil ether flows in the shell side of described membrane contactor, and flow is 150ml/min.The film silk internal diameter of described membrane contactor is 0.38mm, and wall thickness is 150 μ m, and membrane micropore directly is 0.02 μ m, through having removed a spot of macromolecule organic in the waste water after the pre-extraction, as higher alcohols, high carbon acid or high-carbon ester etc.
Enter and carry out complexometric extraction in the packed extraction tower through pre-stripped waste water, furfural waste-water enters from the filler extraction column overhead and flows downward, and complexing extractant charging at the bottom of the tower is upwards flowed.Be in a ratio of 0.6 (extraction agent mass rate: wastewater quality flow=6: 10), in filling surface extraction agent and the abundant contact mass transfer of waste water process, obtain extraction phase and extracting phase at the bottom of cat head and the tower respectively, extraction efficiency in the extraction process is 98.7%, after extraction, the acetate concentration in the furfural waste-water becomes 0.015%.
The extracting phase of at the bottom of the filler extraction Tata, collecting (extractant concentration is through being measured as 4356.5ppm), measurement is carried out aftertreatment as feed liquid through the microporous hydrophobic hollow fiber membrane contactors, described feed liquid flows in the tube side of this microporous hydrophobic hollow fiber membrane contactors, and flow is 120ml/min; The aftertreatment extraction agent flows in the shell side of this microporous hydrophobic hollow fiber membrane contactors; Flow is 60ml/min, and the aftertreatment extraction agent is a normal hexane; The film silk internal diameter of described microporous hydrophobic hollow fiber membrane contactors is 1.2mm, and wall thickness is 150 μ m, and membrane micropore directly is 0.02 μ m.Extractant concentration in the waste water after treatment is through being measured as 136ppm, and only needing again can reuse up to standard through simple biochemical treatment.
Claims (2)
1. comprehensive recovery and treatment method of industrial wastewater from furfural production is characterized in that may further comprise the steps:
A, employing polypropylene hollow fiber membrane contactor extract in advance as extraction equipment, and furfural waste-water flows in the tube side of described membrane contactor, and pre-extraction agent flows both countercurrent flows in the shell side of described membrane contactor; The pre-extraction phase of gained contains the macromolecule organic in pre-extraction agent and the industrial wastewater from furfural production;
The pre-extracting phase of b, a step gained enters packed extraction tower and carries out complexometric extraction; The gained extraction phase obtains dense aqueous acetic acid with the separation of rectification under vacuum method, reclaims extraction agent;
C, b step gained extracting phase carries out aftertreatment as feed liquid through the microporous hydrophobic hollow fiber membrane contactors, described feed liquid flows in the tube side of this microporous hydrophobic hollow fiber membrane contactors, and the aftertreatment extraction agent flows in the shell side of this microporous hydrophobic hollow fiber membrane contactors; It is characterized in that the aftertreatment extraction agent is the non-polar organic solvent of lower boiling, low viscosity, low water solubility; The film silk internal diameter of described microporous hydrophobic hollow fiber membrane contactors is 0.1～0.5mm, and wall thickness is 50～200 μ m, and membrane micropore directly is 0.01～0.2 μ m.
2. the comprehensive recovery and treatment method of industrial wastewater from furfural production according to claim 1 is characterized in that a goes on foot the aftertreatment extraction agent that uses in the pre-extraction agent that uses in the pre-extraction process and the c step last handling process and is any one or a few mixture in the organic solvents such as low-density oil ether, normal hexane, N-BUTYL ACETATE.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102921299A (en) * | 2012-11-13 | 2013-02-13 | 常州大学 | Method for processing furfural industrial sewage |
| CN103772329A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Method for simultaneous extraction and recovery of furfural and acetic acid from furfural stripping steam condensate |
| CN112007515A (en) * | 2019-05-29 | 2020-12-01 | 农业部沼气科学研究所 | Method for reducing reverse osmosis separation rejection rate of furan formaldehyde |
| CN114874161A (en) * | 2022-04-22 | 2022-08-09 | 浙江恒逸石化研究院有限公司 | Method for continuously synthesizing and purifying 5-hydroxymethylfurfural by means of hollow fiber membrane tube |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1141302C (en) * | 2001-03-08 | 2004-03-10 | 水志良 | Process for treating waste water containing furaldehyde and recovering furaldehyde and acetic acid |
| CN1282615C (en) * | 2004-12-24 | 2006-11-01 | 长春市佳辰环保设备有限公司 | Process for treating industrial waste water from production of furfural |
| CN100374378C (en) * | 2006-05-19 | 2008-03-12 | 高武 | Treatment process for recovering industrial wastewater from producing furfural |
| KR101620117B1 (en) * | 2008-03-25 | 2016-05-11 | 씨피씨 코포레이션, 타이완 | Improved extractive distillation processes using water-soluble extractive solvents |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103772329A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Method for simultaneous extraction and recovery of furfural and acetic acid from furfural stripping steam condensate |
| CN103772329B (en) * | 2012-10-24 | 2015-04-15 | 中国石油化工股份有限公司 | Method for simultaneous extraction and recovery of furfural and acetic acid from furfural stripping steam condensate |
| CN102921299A (en) * | 2012-11-13 | 2013-02-13 | 常州大学 | Method for processing furfural industrial sewage |
| CN112007515A (en) * | 2019-05-29 | 2020-12-01 | 农业部沼气科学研究所 | Method for reducing reverse osmosis separation rejection rate of furan formaldehyde |
| CN114874161A (en) * | 2022-04-22 | 2022-08-09 | 浙江恒逸石化研究院有限公司 | Method for continuously synthesizing and purifying 5-hydroxymethylfurfural by means of hollow fiber membrane tube |
| CN114874161B (en) * | 2022-04-22 | 2024-02-02 | 浙江恒逸石化研究院有限公司 | Method for continuously synthesizing and purifying 5-hydroxymethylfurfural by means of hollow fiber membrane tube |
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