CN1626494A - Method for recovering acetic acid from wastewater generated in production of furfural - Google Patents
Method for recovering acetic acid from wastewater generated in production of furfural Download PDFInfo
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- CN1626494A CN1626494A CN 200410020266 CN200410020266A CN1626494A CN 1626494 A CN1626494 A CN 1626494A CN 200410020266 CN200410020266 CN 200410020266 CN 200410020266 A CN200410020266 A CN 200410020266A CN 1626494 A CN1626494 A CN 1626494A
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Abstract
A process for recovering acetic acid from the sewage generated by preparing furfural includes such steps as counter-flow extracting by extractant in pulse extraction tower, vacuum rectifying for separating acetic acid from extractant, refining acetic acid by intermittent azeotropic distilling, and regenerating extractant. Its advatnages are high output rate, and no pollution.
Description
Technical field
The present invention relates to a kind of method that from the waste water of producing furfural, reclaims acetic acid.Belong to the technology of from furfural waste-water, extracting by product.
Background technology
Furfural is a kind of important chemical material, and it is to be made through hydrolysis by plant straws such as corn cob, bagasse.The hydrolytic process primary product is a furfural, accounts for 5～8% in hydrolyzed solution, generates by products such as acetic acid, methyl alcohol, acetone in addition, and wherein acetic acid accounts for about 2.5% in hydrolyzed solution.At present each manufacturer all will not reclaim above-mentioned by product, all discharges simultaneously with waste water, causes that the COD value is up to more than 35000 in the waste water, and this not only can produce pollution to environment, and the while is again a kind of waste to resource.
If the acetic acid in the waste water is reclaimed, by producing 1 ton of furfural, recyclable about 0.35 ton acetic acid, and the COD value in the waste water can being reduced to below 5000, this carries out next step to waste water handles and has created favourable condition, is two at one stroke beneficial.
Summary of the invention
The object of the present invention is to provide a kind of method that from the waste water of producing furfural, reclaims acetic acid, this procedure advantages of simple, energy consumption is low, the product recovery rate height.
The present invention is realized by following technical proposals.A kind of method that reclaims acetic acid from the waste water of producing furfural is characterized in that comprising following process:
1, makes extraction agent with octanol, employing is up to the pulsed extraction column more than the 10m, to containing mass ratio is that the furfural waste-water of 5～8% acetic acid carries out extracting and separating, this tower operational condition is: the ratio of raw material and extraction agent is 0.5-2.5, service temperature 20-40 ℃, air pulse frequency 1: 4, air-pulse pressure 150kPa, discharging frequency 1: 20-1: 80.
2, send into the extractant regeneration tower by the extraction phase of pulse extraction column overhead extraction, the operational condition of this tower is: tower top pressure 20-35kPa, reflux ratio 1.5-2.5.
3, be that acetic acid mixed solution more than 60% is sent into treating tower and made with extra care by the cat head extraction mass ratio of extractant regeneration tower, the operational condition of this tower is: use the cyclohexane give entrainer, tower top pressure is a normal pressure, reflux ratio 1-3.
The invention has the advantages that, adopted first extraction back purified method, the extraction agent wide material sources, pollution-free, the technological process advantages of simple, energy consumption is low, the product recovery rate height, waste discharge COD value is low.
Embodiment
Embodiment 1
With the acetic acid in the pulsed extraction column extraction wastewater.Extraction conditions is: the extraction tower internal diameter is φ 400mm, and tower height is 10m,
Extraction agent is an octanol, and the ratio of raw material and extraction agent is 1.2,24 ℃ of service temperatures, air pulse frequency 1: 4, air-pulse pressure 150kPa, discharging frequency 1: 60.The percentage extraction of acetic acid is 99.5%.
From extraction agent, isolate acetic acid with the rectification under vacuum method, and make extractant regeneration.Operational condition is: the rectifying tower internal diameter is φ 250mm, and tower height is 8m, tower top pressure 28kPa, reflux ratio 2.2.Acetic acid content in the cat head mixed solution reaches 63%.
The cat head mixed solution adopts intermittent azeotropic rectifying method Dichlorodiphenyl Acetate to dewater refining again.Operational condition is: the rectifying tower internal diameter is φ 200mm, and tower height is 15m, uses the cyclohexane give entrainer, and tower top pressure is a normal pressure, reflux ratio 1.2.Can obtain purity and be 99.1% finished product acetic acid
Embodiment 2
Adopt the process unit identical, identical extraction agent and entrainer with embodiment 1.Other operational conditions are: the ratio 1.3 of raw material and extraction agent, 21 ℃ of service temperatures, air pulse frequency 1: 4, air-pulse pressure 150kPa, discharging frequency 1: 50.The percentage extraction that can obtain acetic acid is 97.8%.The operational condition of rectification under vacuum tower is: tower top pressure 30kPa, reflux ratio 2.0.Acetic acid content in the cat head mixed solution reaches 61%.The operational condition of intermittent azeotropic rectifying is with embodiment 1, can obtain purity and be 99.13% finished product acetic acid
Embodiment 3
Adopt the process unit identical, identical extraction agent and entrainer with embodiment 1.Other operational conditions are: the ratio 1.7 of raw material and extraction agent, 23 ℃ of service temperatures, air pulse frequency 1: 4, air-pulse pressure 150kPa, discharging frequency 1: 30.The percentage extraction of acetic acid is 93.7%.The operational condition of rectification under vacuum tower is: tower top pressure 30kPa, reflux ratio 1.6.Acetic acid content in the cat head mixed solution reaches 58%.The operational condition of intermittent azeotropic rectifying is with embodiment 1, can obtain purity and be 99.0% finished product acetic acid.
Claims (1)
1, a kind of method that from the waste water of producing furfural, reclaims acetic acid, this method feature comprises following process:
(1), makes extraction agent with octanol, employing is up to the pulsed extraction column more than the 10m, to containing mass ratio is that the furfural waste-water of 5～8% acetic acid carries out extracting and separating, this tower operational condition is: the ratio of raw material and extraction agent is 0.5-2.5, service temperature 20-40 ℃, air pulse frequency 1: 4, air-pulse pressure 150kPa, discharging frequency 1: 20-1: 80;
(2), send into the extractant regeneration tower, the operational condition of this tower is: tower top pressure 20-35kPa, reflux ratio 1.5-2.5 by the extraction phase of pulse extraction column overhead extraction;
(3), be that acetic acid mixed solution more than 60% is sent into treating tower and made with extra care by the cat head extraction mass ratio of extractant regeneration tower, the operational condition of this tower is: use the cyclohexane give entrainer, tower top pressure is a normal pressure, reflux ratio 1-3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410020266 CN1626494A (en) | 2004-08-09 | 2004-08-09 | Method for recovering acetic acid from wastewater generated in production of furfural |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410020266 CN1626494A (en) | 2004-08-09 | 2004-08-09 | Method for recovering acetic acid from wastewater generated in production of furfural |
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| Publication Number | Publication Date |
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| CN1626494A true CN1626494A (en) | 2005-06-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200410020266 Pending CN1626494A (en) | 2004-08-09 | 2004-08-09 | Method for recovering acetic acid from wastewater generated in production of furfural |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101881941A (en) * | 2010-06-04 | 2010-11-10 | 华东理工大学 | Expert control method for aqueous-phase reflux of acetic acid dehydration and azeotropic distillation system |
| CN101696196B (en) * | 2009-10-27 | 2011-08-31 | 山东万盛环保科技发展有限公司 | Method for increasing furfural yield and recovering methanol |
| CN102175795A (en) * | 2011-01-16 | 2011-09-07 | 青海电力科学试验研究院 | Method for calculating furfural component in shake extraction test oil |
| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
| CN102372619A (en) * | 2010-08-23 | 2012-03-14 | 刘同清 | Process for producing acetate by using dilute acetic acid |
| CN101508640B (en) * | 2009-04-02 | 2012-08-08 | 湖北民生生物医药有限公司 | Method for recycling dilute acetic acid with azeotropic abstraction distillation |
| CN109575088A (en) * | 2019-01-30 | 2019-04-05 | 四川金象赛瑞化工股份有限公司 | The refining methd of xylose in a kind of hemicellulose hydrolysate |
| CN110040894A (en) * | 2019-04-16 | 2019-07-23 | 南京工业大学 | Method for treating low-concentration acetic acid wastewater containing mineral acid and organic impurities |
-
2004
- 2004-08-09 CN CN 200410020266 patent/CN1626494A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508640B (en) * | 2009-04-02 | 2012-08-08 | 湖北民生生物医药有限公司 | Method for recycling dilute acetic acid with azeotropic abstraction distillation |
| CN101696196B (en) * | 2009-10-27 | 2011-08-31 | 山东万盛环保科技发展有限公司 | Method for increasing furfural yield and recovering methanol |
| CN101881941A (en) * | 2010-06-04 | 2010-11-10 | 华东理工大学 | Expert control method for aqueous-phase reflux of acetic acid dehydration and azeotropic distillation system |
| CN101881941B (en) * | 2010-06-04 | 2012-01-04 | 华东理工大学 | Expert control method for aqueous-phase reflux of acetic acid dehydration and azeotropic distillation system |
| CN102372619A (en) * | 2010-08-23 | 2012-03-14 | 刘同清 | Process for producing acetate by using dilute acetic acid |
| CN102175795A (en) * | 2011-01-16 | 2011-09-07 | 青海电力科学试验研究院 | Method for calculating furfural component in shake extraction test oil |
| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
| CN109575088A (en) * | 2019-01-30 | 2019-04-05 | 四川金象赛瑞化工股份有限公司 | The refining methd of xylose in a kind of hemicellulose hydrolysate |
| CN110040894A (en) * | 2019-04-16 | 2019-07-23 | 南京工业大学 | Method for treating low-concentration acetic acid wastewater containing mineral acid and organic impurities |
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