CN1313282A - Process for treating waste water containing furaldehyde and recovering furaldehyde and acetic acid - Google Patents
Process for treating waste water containing furaldehyde and recovering furaldehyde and acetic acid Download PDFInfo
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- CN1313282A CN1313282A CN 01106283 CN01106283A CN1313282A CN 1313282 A CN1313282 A CN 1313282A CN 01106283 CN01106283 CN 01106283 CN 01106283 A CN01106283 A CN 01106283A CN 1313282 A CN1313282 A CN 1313282A
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- furfural
- acetic acid
- mother liquor
- furaldehyde
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Abstract
A process for treating waste water of furaldehyde and recovering furaldehyde and acetic acid includes such steps as cooling said waste water to ordinary temp, filtering, loading it in phase-transfer separator full of multifunctional high-molecular polymer adsorbent, adsorbing to discharge purified nutral water (pH=7-8), using ammonia separating liquid in separator to obtain furaldehyde mother liquid and ammonium acetate mother liquid, evaporation concentrating and refining to obtain furaldehyde and acetic acid. Its purified water can be used for boiler, lowering its cost.
Description
The present invention relates to a kind of sewage treatment technique, the novel process of furfural and acetic acid is administered and reclaimed to particularly a kind of furfural waste-water.
As everyone knows, furfural is an important chemical material.China's furfurol industry is raw material mostly with the corn cob, ton surplus the annual production about 50,000.Because of its technology imperfection, resource is not only wasted in the discharging of furfural waste-water, and causes the severe contamination of environment, and waste water institute is withered through the part farm crop, and fishes and shrimps disappear, even jeopardizes the water source of domestic water.Confirm through environmental monitoring results, contain acetic acid 1.0%-2.5% in the furfural waste-water, furfural 0.2%-0.5% and multiple organic compound are yellow acid, PH＜2, and the about 15000mg/l of COD value is above 150 times of the wastewater discharge standards of stipulating.At present, factory does not all have ideal waste water treatment technology mostly, and for this reason, scientific and technical personnel once proposed many resolutions, but did not still have the practical application precedent so far.
Furfural waste-water commonly used is administered technology and is summarized as follows:
One, sodium-acetate method: adopt in the sodium hydroxide and the acetic acid in the furfural waste-water to sodium-acetate, then it is supplied water as low pressure boiler, make its concentration be evaporated to 15%-25%, at last its concentrated salt is changed into acetic acid.
The drawback of this method is that furfural do not separate, and the sodium-acetate of recovery is with low quality, and sodium hydroxide costs an arm and a leg, and is uneconomical.Therefore, this method is eliminated.
Two, extraction process: adopt the trialkylamine kind of extractants with the acetic acid in the extraction process recovery waste water, when carrying out production test, find,, cause extraction agent to be poisoned, so waste water is difficult to administer because of furfural disturbs.
Three, electroosmose process: adopt emerging membrane separation technique from furfural waste-water, to reclaim acetic acid.Reclaim the water quality of acetic acid through pretreated furfural waste-water with electrodialysis (ED), concentrate acetic acid with ED again, make by product acetic acid through extraction, rectifying with the control discharge water.In process of the test, find, the easily contaminated or obstruction of film, the deposition fouling of suspended substance easily makes the current skewness, and resistance increases, and causes polarization, is forced to stop trial production.Its reason is in advance furfural waste-water character to be understood not enough, the changeable easy oxypolymerization of furfural chemical property, and electroosmose process is difficult to adapt to.
Four, anaerobic process: the anaerobic treatment technology is a kind of biological process, and it can effectively be removed organic pollutant and make it pass through microbial process, changes organic compound into methane and carbonic acid gas.This method investment is big, working cost is high, and process control condition is strict.
Five, intermittent activated sludge process (SBR): the SBR method is more noticeable a kind of waste water treatment process in the active sludge processing system in recent ten years.But the automatic control technology of this treatment process is had relatively high expectations, the engineering operation operational administrative is comparatively complicated, invests greatlyyer, influences it and applies.
The purpose of this invention is to provide a kind of furfural waste-water and administer and reclaim furfural and acetic acid technology, this technical process is controlled easily, operate steadily, compare with other existing treatment process, can not only effectively furfural and acetic acid be separated from waste water and be reclaimed, and purifying waste water after handling can be directly used in oiler feed, obviously reduces the working cost of wastewater treatment.
The object of the present invention is achieved like this: earlier waste water is cooled to room temperature, after the filtration, filtrate putting into is equipped with the phase transition tripping device of multifunctional macromolecule polymer absorbant, handle under the sorbent material effect in device, making it to discharge continuously pH value purifies waste water for 7-8 neutrality, in tripping device, isolate furfural mother liquor and ammonium acetate mother liquor then with the ammonia parting liquid, carry out evaporation concentration more respectively, further make with extra care and promptly obtain furfural and acetic acid, the consumption of ammonia parting liquid is 1/10th of a furfural waste-water amount.
Above-mentioned isolated furfural mother liquor returns as the ammonia parting liquid with aldehyde gas evaporation concentration, distillation phlegma, and residue is a mao aldehyde at the bottom of the still, delivers to the furfural primary tower and reclaims furfural.
Above-mentioned isolated ammonium acetate mother liquor is 40% o'clock through further evaporation concentration to concentration, is the vitriol oil acidifying of 93-98% with concentration, and pH value reaches 1-2, is 105-116 ℃ of distillation in temperature, obtains thick acetic acid, and process for refining can obtain pure acetic acid routinely.
After the acidifying of above-mentioned ammonium acetate mother liquor, can add the vitriol oil of solution cumulative volume 1-2% and the industrial alcohol of one times of amount of overall solution volume again, under 70-78 ℃ of condition, backflow 5-10 hour, 70-71 ℃ fraction was got in distillation then, carries out rectifying, promptly gets ethyl acetate.
Used ammonia parting liquid is the ammoniacal liquor of concentration 5-7%, and it is directly prepared by strong aqua or is prepared by the distillation phlegma of strong aqua and furfural mother liquor.
Used multifunctional macromolecule polymer absorbant adopts commercially available 506 type polystyrene pyridine resins, II type porous resin, LDX-602 type sorbent material, GDX-103 type sorbent material.
Because the present invention adopts phase transfer of technology that furfural waste-water is carried out the comprehensive regulation, this technical process is controlled easily, easy to operate, operate steadily, it has fundamentally changed existing improvement technology, not only furfural and acetic acid can be separated from furfural waste-water effectively, and be reclaimed, and the waste water after handling becomes and purifies waste water, can be directly used in oiler feed, thereby realize the zero release that furfural is produced.Owing to do not use expensive equipment and raw material, so obviously reduce the working cost of wastewater treatment.Therefore, the present invention very easily applies.
Below in conjunction with embodiment the present invention is further described, but in this technical process the recovery of furfural and acetic acid is not subjected to the restriction of embodiment.
Embodiment one:
Get furfural mill waste water 10L, use filter paper filtering, filtrate entering is equipped with in the phase transition tripping device of high molecular polymer GDX-103 type sorbent material, and the control flow velocity is the 50ml/ branch, and discharge neutrality continuously and purify waste water, pH value 7-8, the COD clearance reaches more than 95%.In tripping device, use the ammonia parting liquid 1L that directly prepares by strong aqua then, furfural and acetic acid are separated.The further evaporation concentration of furfural mother liquor obtains the about 2.5.ml of hair aldehyde.The further evaporation concentration of ammonium acetate mother liquor, concentration is about 40%.After vitriol oil acidifying, distillation can obtain thick acetic acid about 105-116 ℃.Also can after vitriol oil acidifying, add 93% sulfuric acid 3-6ml again, add industrial alcohol 500ml,, backflow 5-10 hour, distill then at 70-78 ℃.Get 70-71 ℃ of fraction, carry out rectifying, promptly get ethyl acetate product, purity＞96%.
Embodiment two:
After the cooling of furfural mill waste water, filter through sand-bed filter, filtrate entering is equipped with in the tripping device of multifunctional macromolecule polymkeric substance 506 type polystyrene pyridine resin sorbents, and the control flow velocity is 5m
3/ hour, discharge neutrality continuously and purify waste water, pH value 7-8, the COD clearance is done boiler water supply below 95%.The ammonia parting liquid of preparing with the phlegma by strong aqua and furfural mother liquor of wastewater flow rate 1/10th consumptions in tripping device is isolated furfural mother liquor and ammonium acetate mother liquor then.The furfural mother liquor returns as the ammonia parting liquid with the further evaporation concentration of aldehyde gas, distillation phlegma, and residue is a mao aldehyde at the bottom of the still, and purity is 85%, send the furfural primary tower to reclaim furfural.The further evaporation concentration of ammonium acetate mother liquor, concentration is about 40%, is 1-2 with PH after the vitriol oil acidifying of 93-98%, distills about 105-116 ℃, can obtain the acetic acid of concentration 30-40%, and ethyl acetate can be sold or further be processed into to the about 3-4 ton of day output.
Claims (6)
1, a kind of furfural waste-water is administered technology, it is characterized in that earlier waste water being cooled to room temperature: after the filtration, filtrate putting into is equipped with the phase transition tripping device of multifunctional macromolecule polymer absorbant, under device internal adsorption agent effect, handle, making it to discharge continuously pH value purifies waste water for 7-8 neutrality, in tripping device, isolate furfural mother liquor and ammonium acetate mother liquor then with the ammonia parting liquid, carry out evaporation concentration more respectively, further make with extra care and promptly obtain furfural and acetic acid, the consumption of ammonia parting liquid is 1/10th of a furfural waste-water amount.
2, technology according to claim 1 is characterized in that isolated furfural mother liquor with aldehyde gas evaporation concentration, distills phlegma and returns as the ammonia parting liquid, and residue is a mao aldehyde at the bottom of the still, delivers to the furfural primary tower and reclaims furfural.
3, technology according to claim 1, it is characterized in that isolated ammonium acetate mother liquor is through further evaporation concentration to concentration at 40% o'clock, with concentration is the vitriol oil acidifying of 93-98%, pH value reaches 1-2, in temperature is 105-116 ℃ of distillation, obtain thick acetic acid, process for refining can obtain pure acetic acid routinely.
4, technology according to claim 3, after it is characterized in that the acidifying of ammonium acetate mother liquor, the vitriol oil and the long-pending industrial alcohol of overall solution volume monoploid that can add the 1-2% of solution cumulative volume again, under 70-78 ℃ of condition, backflow 5-10 hour, 70-71 ℃ fraction was got in distillation then, carry out rectifying, promptly get ethyl acetate.
5, technology according to claim 3 is characterized in that used ammonia parting liquid is the ammoniacal liquor of concentration 5-7%, and it is directly prepared by strong aqua or is prepared by strong aqua and furfural mother liquor distillation phlegma.
6, technology according to claim 1, its feature adopts 506 type polystyrene pyridine resins at the multifunctional macromolecule polymer absorbant, II type porous resin, LDX-602 type sorbent material, the absorption of GDX-103 type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011062835A CN1141302C (en) | 2001-03-08 | 2001-03-08 | Process for treating waste water containing furaldehyde and recovering furaldehyde and acetic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011062835A CN1141302C (en) | 2001-03-08 | 2001-03-08 | Process for treating waste water containing furaldehyde and recovering furaldehyde and acetic acid |
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| CN1313282A true CN1313282A (en) | 2001-09-19 |
| CN1141302C CN1141302C (en) | 2004-03-10 |
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| CNB011062835A Expired - Fee Related CN1141302C (en) | 2001-03-08 | 2001-03-08 | Process for treating waste water containing furaldehyde and recovering furaldehyde and acetic acid |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006066469A1 (en) * | 2004-12-24 | 2006-06-29 | Changchun Jiachen Environment Protecting Equipment Co., Ltd | Production method of snow-melting agent of calcium acetate |
| CN100374378C (en) * | 2006-05-19 | 2008-03-12 | 高武 | Treatment process for recovering industrial wastewater from producing furfural |
| CN100376495C (en) * | 2006-09-13 | 2008-03-26 | 吉林省环科环保技术有限公司 | Cleansing production method for producing furfural with zero dischrge of waste water |
| CN101343091B (en) * | 2008-08-22 | 2010-06-09 | 肥城金塔机械有限公司 | Wastewater treatment system for furfurol preparation |
| CN102107924B (en) * | 2009-12-29 | 2012-08-22 | 石家庄国华环保科技有限公司 | Method for comprehensively recovering and treating furfural industrial wastewater |
| CN102863405A (en) * | 2012-10-16 | 2013-01-09 | 天津科技大学 | Dissolving pulp prehydrolysis solution autocatalysis furfuraldehyde preparation method and recycling method for acetic acid in prehydrolysis solution waste water and furfuraldehyde waste water |
| CN109081821A (en) * | 2018-10-22 | 2018-12-25 | 江阴市大洋固废处置利用有限公司 | A kind of the furfural recyclable device and recovery method of Production of Ceramics condensate liquid |
| CN109195958A (en) * | 2016-06-02 | 2019-01-11 | 巴斯夫欧洲公司 | The processing method of aqueous effluent |
| CN111689635A (en) * | 2020-06-10 | 2020-09-22 | 南京工业大学 | Method for treating waste water containing ammonium acetate |
-
2001
- 2001-03-08 CN CNB011062835A patent/CN1141302C/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006066469A1 (en) * | 2004-12-24 | 2006-06-29 | Changchun Jiachen Environment Protecting Equipment Co., Ltd | Production method of snow-melting agent of calcium acetate |
| CN100374378C (en) * | 2006-05-19 | 2008-03-12 | 高武 | Treatment process for recovering industrial wastewater from producing furfural |
| CN100376495C (en) * | 2006-09-13 | 2008-03-26 | 吉林省环科环保技术有限公司 | Cleansing production method for producing furfural with zero dischrge of waste water |
| CN101343091B (en) * | 2008-08-22 | 2010-06-09 | 肥城金塔机械有限公司 | Wastewater treatment system for furfurol preparation |
| CN102107924B (en) * | 2009-12-29 | 2012-08-22 | 石家庄国华环保科技有限公司 | Method for comprehensively recovering and treating furfural industrial wastewater |
| CN102863405A (en) * | 2012-10-16 | 2013-01-09 | 天津科技大学 | Dissolving pulp prehydrolysis solution autocatalysis furfuraldehyde preparation method and recycling method for acetic acid in prehydrolysis solution waste water and furfuraldehyde waste water |
| CN109195958A (en) * | 2016-06-02 | 2019-01-11 | 巴斯夫欧洲公司 | The processing method of aqueous effluent |
| CN109195958B (en) * | 2016-06-02 | 2023-06-20 | 巴斯夫欧洲公司 | Method for treating aqueous effluents |
| CN109081821A (en) * | 2018-10-22 | 2018-12-25 | 江阴市大洋固废处置利用有限公司 | A kind of the furfural recyclable device and recovery method of Production of Ceramics condensate liquid |
| CN109081821B (en) * | 2018-10-22 | 2023-09-15 | 江阴市大洋固废处置利用有限公司 | Furfural recovery device and recovery method for condensate liquid in ceramic production |
| CN111689635A (en) * | 2020-06-10 | 2020-09-22 | 南京工业大学 | Method for treating waste water containing ammonium acetate |
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| Publication number | Publication date |
|---|---|
| CN1141302C (en) | 2004-03-10 |
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