CN102126926A - Method for recycling ethylene glycol and acetaldehyde from polyester waste water - Google Patents
Method for recycling ethylene glycol and acetaldehyde from polyester waste water Download PDFInfo
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- CN102126926A CN102126926A CN2010106021677A CN201010602167A CN102126926A CN 102126926 A CN102126926 A CN 102126926A CN 2010106021677 A CN2010106021677 A CN 2010106021677A CN 201010602167 A CN201010602167 A CN 201010602167A CN 102126926 A CN102126926 A CN 102126926A
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Abstract
The invention discloses a method for recycling ethylene glycol and acetaldehyde from polyester waste water. The method is implemented by the following steps of: (1) introducing esterification waste water into a stripping tower for treating and directly introducing organic matter gas and water vapor collected from a tower top into an acetaldehyde rectifying tower; (2) treating in the acetaldehyde rectifying tower, collecting high-purity acetaldehyde from the tower top and introducing waste water collected from a tower bottom into an ethylene glycol distillation tower; and (3) treating in the ethylene glycol distillation tower, collecting a high-purity ethylene glycol solution from the tower bottom and introducing waste gas and water vapor produced on the tower top into the stripping tower for cyclic treatment. In the method, acetaldehyde and ethylene glycol are continuously collected, so that hydrolysis of byproduct of 2-methyl-1,3-dioxolane in the esterification waste water is continuously performed positively and negatively, acetaldehyde with the concentration of over 95 percent and ethylene glycol with the concentration of over 70 percent are obtained at the end of treatment, and the 2-methyl-1,3-dioxolane is fully hydrolyzed.
Description
Technical field
The present invention relates in a kind of chemical process the recovery of polyester waste water and the method for utilizing again, the method for recovery ethylene glycol and acetaldehyde in particularly a kind of polyester waste water.
Background technology
Polyester (PET), the particularly production of differential polyester, domestic enterprise generally adopts terephthalic acid and ethylene glycol direct esterification method, and the concentration of the esterification waste water of its discharging is subjected to the esterification condition influence bigger, the about 20000-30000mg/L of the concentration of esterification waste water chemical oxygen demand cod.Main organic pollutant is ethylene glycol and acetaldehyde in the polyester waste water, wherein volatile components acetaldehyde accounts for about 50% of total organic pollutant, in addition because the technology that the device of China's polyester industrial adopts is irregular does not rise, the side components that various technologies produce also is not quite similar, 2-methyl isophthalic acid wherein, the 3-dioxolane is wherein bigger component.It can hydrolysis generate acetaldehyde and ethylene glycol, and its reaction is as follows:
At present, the following several method of main both at home and abroad employing is handled.
The anaerobic-aerobic method is handled this waste water.But because aldehyde material toxicity is very big, be unfavorable for bacterial growth, cause the biochemical method processing efficiency lower, and for the waste water of high COD value like this, adopt separately biological process handle not only the investment cost height and also processing cost also very expensive, the business burden weight.
The method of burning again behind the stripping is handled this waste water.Behind the stripping, the COD value drops to below the 5000mg/L, then the cat head material being fed pipestill for heat carrier burns, and fully utilize its heat energy, but burn the carbonic acid gas that generates and cause Greenhouse effect, incomplete combustion also can produce secondary pollution, and burns and to require quite height otherwise easily blast of safety coefficient, and the heat energy utilization of burning is uneconomical.
John Brown Deutsche Engineering GmbH adopts continuous underpressure distillation (CN16854A), thereby obtains the very high ethylene glycol of purity, and this method expense is higher, and energy consumption is bigger.
The method of reverse osmosis membrane (CN1301238C) reclaims ethylene glycol in the esterification waste water, but this method obtains the higher reverse osmosis membrane that acetaldehyde can not be separated especially employing of the purity of ethylene glycol all from external import, and technology dependence is big, the cost height.And aforesaid method is not considered the recovery of acetaldehyde, the by product 2-methyl isophthalic acid that especially content is bigger, the problems such as influence to water pollution or COD value of 3-dioxolane.
Recently, (CN1974508A) come batch process 2-methyl isophthalic acid by catalysis ion-exchange after having reported stripping, 3-dioxolane by product and then handle the method that technologies such as reclaiming acetaldehyde and ethylene glycol reclaim ethylene glycol and acetaldehyde in the esterification waste waters respectively.This method can access the very high ethylene glycol of purity, but the time adopted water directly to absorb acetaldehyde steam, the acetaldehyde solution concentration that causes process water to strengthen and obtain is too low, need subsequent disposal, increased processing cost, and this method is a method intermittently, especially introduced gloxylic acid catalytic treatment by product 2-methyl isophthalic acid, the 3-dioxolane is because the corrodibility of acid, require very high to industrial equipment like this, and because the 2-methyl isophthalic acid, the 3-dioxolane generates acetaldehyde and ethylene glycol is a reversible reaction, after batch process is intact, the next process of entering cannot say for sure that acetaldehyde and ethylene glycol can regeneration 2-methyl isophthalic acids, the 3-dioxolane.
Summary of the invention
For solving the problems of the technologies described above, the invention provides the method that reclaims ethylene glycol and acetaldehyde in a kind of polyester waste water, in handling the waste water process, constantly reclaim high density acetaldehyde and ethylene glycol, make the 2-methyl isophthalic acid, the hydrolysis of 3-dioxolane under hot conditions constantly carried out to the positive reaction direction, final hydrolysis is complete, and the COD value of waste water is below 5000mg/L.
The present invention realizes by following technical scheme:
Reclaiming the method for ethylene glycol and acetaldehyde in a kind of polyester waste water, is a method of collecting continuously, is to realize by following step:
(1) esterification waste water enters gas stripping column and handles, at the bottom of tower, obtain gas and carry waste water and carry out sewage disposal, overhead collection to organic gas directly enter the acetaldehyde rectifying tower;
(2) after the acetaldehyde rectifying tower is handled, to high purity acetaldehyde, the waste water of collecting at the bottom of the tower enters the ethylene glycol distillation tower in overhead collection;
(3) after the ethylene glycol distillation tower is handled, collect the high purity ethylene glycol solution at the bottom of tower, waste gas and the incident gas water lift of whole flow process steam that cat head produces enter the gas stripping column circular treatment once more.
Gas stripping column in the described step (1) need add mass transfer, and heat source preferred is a water vapour, and tower top pressure is 0-1.0MPa, and tower top temperature is 60-140 ℃; Column bottom temperature is 80-160 ℃.
It is the waste water of COD value less than 5000mg/L that the gas of collecting at the bottom of tower in the described step (1) is carried waste water.Waste water after handling through this gas stripping column, the COD value can directly be carried out sewage disposal less than 5000mg/L.
In the described step (1) overhead collection to organic gas entering the acetaldehyde rectifying tower before, can also enter a waste water knockout tower, at the bottom of the tower of described waste water knockout tower, collect the COD value and carry out sewage disposal less than the waste water of 5000mg/L, overhead collection to organic gas enter the acetaldehyde rectifying tower.
Described gas stripping column and waste water knockout tower play the effect of a rectifying, the waste water knockout tower can make carries that the organic gas component more than 95% (comprises acetaldehyde, ethylene glycol and 2-methyl isophthalic acid in the esterification waste water that the gas cat head already collects, the 3-dioxolane) purity is higher after process waste water knockout tower, in entering follow-up technical process, can collect more highly purified acetaldehyde and ethylene glycol, and hydrolysis 2-methyl isophthalic acid more efficiently, the 3-dioxolane.
Described waste water knockout tower need add mass transfer, and heat source preferred is a water vapour, and tower top pressure is 0-1.0MPa, and tower top temperature is 60-140 ℃; Column bottom temperature is 80-160 ℃.
Acetaldehyde rectifying tower in the described step (2) need add mass transfer, and heat source preferred is a water vapour, and tower top pressure is 0-1.0MPa, and tower top temperature is 20-80 ℃, and column bottom temperature is 80-160 ℃, and reflux ratio is 0.1-50, and working pressure is 0-1.0MPa.
Acetaldehyde rectifying tower in the described step (2) in the acetaldehyde purity of overhead collection greater than 95%.
The tower top pressure of the ethylene glycol distillation tower in the described step (3) is 0-1.0MPa, and tower top temperature is 30-140 ℃, and column bottom temperature is 80-160 ℃, and reflux ratio is 0.1-30.
The ethylene glycol solution purity that ethylene glycol distillation tower in the described step (3) is collected at the bottom of tower is greater than 70%.The 2-methyl isophthalic acid of the minute quantity that arrives in overhead collection, 3-dioxolane and acetaldehyde steam reenter gas stripping column and carry out circular treatment.
The present invention also provides 2-methyl isophthalic acid in a kind of esterification waste water, the treatment process of 3-dioxolane, according to the 2-methyl isophthalic acid, the 3-dioxolane is hydrolyzed to the reversible reaction principle of acetaldehyde and ethylene glycol under the condition of heating, esterification waste water is at the gas stripping column by described temperature, the waste water knockout tower, in acetaldehyde rectifying tower and the ethylene glycol distillation tower process, constantly hydrolysis, and collect acetaldehyde steam and ethylene glycol solution continuously at acetaldehyde rectifying tower and ethylene glycol distillation tower respectively, hydrolysis reaction is carried out to the positive reaction direction continuously, finally collect undecomposed 2-methyl isophthalic acid at described ethylene glycol distillation cat head, the 3-dioxolane comes back to described gas stripping column, carry out circular treatment, final complete hydrolysis.
Beneficial effect of the present invention is: the present invention not only can obtain purity and surpass 70% ethylene glycol solution and greater than 95% acetaldehyde liquid, reduced the COD value of handling the back esterification waste water simultaneously greatly, and the COD value is dropped to below the 5000mg/L from 30000mg/L.The acetaldehyde solution that the present invention reclaims has good economic interests.Simultaneously, the effective organic by-products 2-methyl isophthalic acid that content is bigger, 3-dioxolane hydrolysis in sepn process becoming acetaldehyde and ethylene glycol, in summary, the present invention has not only overcome the safety issue that stripping cat head material burning disposal is brought, and has obtained highly purified ethylene glycol and acetaldehyde product simultaneously, reduced follow-up treatment process, turn waste into wealth, the gained refuse can directly be sold as quality products on the market, has good economy and environmental benefit.
Description of drawings
Fig. 1 is the processing technological flow figure that does not add the waste water knockout tower
The 1-gas stripping column, 101-steam, 102-waste water collection device, 103-vapor-recovery unit;
2-acetaldehyde rectifying tower, 201-steam, 202-waste water collection device, 203-vapor-recovery unit;
3-ethylene glycol distillation tower, 301-ethylene glycol heating unit, 302-vapor-recovery unit.
Fig. 2 is the processing technological flow figure that adds the waste water knockout tower
The 1-gas stripping column, 101-steam, 102-waste water collection device, 103-vapor-recovery unit;
2-acetaldehyde rectifying tower, 201-steam, 202-waste water collection device, 203-vapor-recovery unit;
3-ethylene glycol distillation tower, 301-ethylene glycol heating unit, 302-vapor-recovery unit;
4-waste water knockout tower, 401-steam, 402-waste water collection device, 403-vapor-recovery unit.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
Describe with the processing technological flow of not adding the waste water knockout tower.
Technology of the present invention and device have obtained practical application at the esbablished corporation of PET industry.Concrete process results is as described below:
According to practical condition, with the esterification waste water of gained, handle to obtain each product component and content thereof through technological process device provided by the invention, as shown in table 1.
Each component concentration of table 1 esterification waste water and product
By the result after handling as can be seen: after handling through the gas stripping column treatment system of technical process, from acetaldehyde rectifying tower system recoveries purity surpass 99.0% acetaldehyde solution, from the extraction of ethylene glycol distillation tower purity be 83.5% ethylene glycol solution, and the 2-methyl isophthalic acid, the 3-dioxolane also almost decomposes fully in this process.Therefore, this technical process can highly purified ethanol of extraction and acetaldehyde solution, reaches the purpose that reduces COD value in the esterification waste water simultaneously.
Describe with the processing technological flow of adding the waste water knockout tower.
Technology of the present invention and device have obtained practical application at the esbablished corporation of PET industry.Concrete process results is as described below:
According to practical condition, with the esterification waste water of gained, handle to obtain each product component and content thereof through technological process device provided by the invention, as shown in table 2.
Each component concentration of table 2 esterification waste water and product
By the result after handling as can be seen: after handling through the waste water knockout tower treatment system of technical process, from acetaldehyde rectifying tower system recoveries purity surpass 95.0% acetaldehyde solution, from the extraction of ethylene glycol distillation tower purity be 86.5% ethylene glycol solution, and the 2-methyl isophthalic acid, the 3-dioxolane also almost decomposes fully in this process.Therefore, this technical process can highly purified ethanol of extraction and acetaldehyde solution, reaches the purpose that reduces COD value in the esterification waste water simultaneously.
Contrast The above results as can be seen, the industrial acetaldehyde purity that the acetaldehyde purity accords that process unit of the present invention obtains is sold on the market.Therefore, process unit of the present invention can access highly purified acetaldehyde solution, turns waste into wealth, and has created bigger economic interests.
Should be appreciated that above narration only is an example and illustrative for the present invention who sets forth as claim, is limited it.The of the present invention content disclosed according to this paper, other embodiment of the present invention is conspicuous for a person skilled in the art.Should be noted that this specification sheets and embodiment only should be regarded as is example, and actual range of the present invention and spirit should be determined by claim.
Claims (10)
1. reclaiming the method for ethylene glycol and acetaldehyde in the polyester waste water, is a method of collecting continuously, it is characterized in that being realizing by following step:
(1) esterification waste water enters gas stripping column and handles, at the bottom of tower, obtain gas and carry waste water and carry out sewage disposal, overhead collection to organic gas directly enter the acetaldehyde rectifying tower;
(2) after the acetaldehyde rectifying tower is handled, to high purity acetaldehyde, the waste water of collecting at the bottom of the tower enters the ethylene glycol distillation tower in overhead collection;
(3) after the ethylene glycol distillation tower is handled, collect the high purity ethylene glycol solution at the bottom of tower, waste gas and the incident gas water lift of whole flow process steam that cat head produces enter the gas stripping column circular treatment once more.
2. reclaim the method for ethylene glycol and acetaldehyde in a kind of polyester waste water as claimed in claim 1, it is characterized in that the gas stripping column in the described step (1) need add mass transfer, heat source preferred is a water vapour, and tower top pressure is 0-1.0MPa, and tower top temperature is 60-140 ℃; Column bottom temperature is 80-160 ℃.
3. reclaim the method for ethylene glycol and acetaldehyde in a kind of polyester waste water as claimed in claim 1, it is characterized in that in the described step (1) overhead collection to organic gas entering the acetaldehyde rectifying tower before, can also enter a waste water knockout tower, overhead collection to organic gas enter the acetaldehyde rectifying tower.
4. reclaim the method for ethylene glycol and acetaldehyde in a kind of polyester waste water as claimed in claim 1, it is characterized in that the waste water that described gas stripping column and waste water knockout tower are collected is the waste water of COD less than 5000mg/L at the bottom of tower; Organic gas in overhead collection is to contain the organic gas more than 95% in the esterification waste water.
5. reclaim the method for ethylene glycol and acetaldehyde in a kind of polyester waste water as claimed in claim 1, it is characterized in that described waste water knockout tower need add mass transfer, heat source preferred is a water vapour, and tower top pressure is 0-1.0MPa, and tower top temperature is 60-140 ℃; Column bottom temperature is 80-160 ℃.
6. reclaim the method for ethylene glycol and acetaldehyde in a kind of polyester waste water as claimed in claim 1, it is characterized in that the acetaldehyde rectifying tower in the described step (2) need add mass transfer, heat source preferred is a water vapour, tower top pressure is 0-1.0MPa, tower top temperature is 20-80 ℃, column bottom temperature is 80-160 ℃, and reflux ratio is 0.1-50, and working pressure is 0-1.0MPa.
7. reclaim the method for ethylene glycol and acetaldehyde in a kind of polyester waste water as claimed in claim 1, it is characterized in that acetaldehyde rectifying tower in the described step (2) in the acetaldehyde purity of overhead collection greater than 95%.
8. reclaim the method for ethylene glycol and acetaldehyde in a kind of polyester waste water as claimed in claim 1, the tower top pressure that it is characterized in that the ethylene glycol distillation tower in the described step (3) is 0-1.0MPa, tower top temperature is 30-140 ℃, and column bottom temperature is 80-160 ℃, and reflux ratio is 0.1-30.
9. reclaim the method for ethylene glycol and acetaldehyde in a kind of polyester waste water as claimed in claim 1, it is characterized in that ethylene glycol solution purity that the ethylene glycol distillation tower in the described step (3) collects is greater than 70% at the bottom of tower.The 2-methyl isophthalic acid of the minute quantity that arrives in overhead collection, 3-dioxolane and acetaldehyde steam reenter gas stripping column and carry out circular treatment.
10. 2-methyl isophthalic acid in the esterification waste water, the treatment process of 3-dioxolane, it is characterized in that methyl isophthalic acid according to 2-, the 3-dioxolane is hydrolyzed to the reversible reaction principle of acetaldehyde and ethylene glycol under the condition of heating, esterification waste water is at the gas stripping column by described temperature, the waste water knockout tower, in acetaldehyde rectifying tower and the ethylene glycol distillation tower process, constantly hydrolysis, and collect acetaldehyde steam and ethylene glycol solution continuously at acetaldehyde rectifying tower and ethylene glycol distillation tower respectively, hydrolysis reaction is successively carried out to the positive reaction direction, finally collect undecomposed 2-methyl isophthalic acid at described ethylene glycol distillation cat head, 3-dioxolane steam comes back to described gas stripping column, carry out circular treatment, final complete hydrolysis.
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| CN201010602167.7A CN102126926B (en) | 2010-12-23 | 2010-12-23 | Method for recycling ethylene glycol and acetaldehyde from polyester waste water |
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Cited By (12)
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| CN103012090A (en) * | 2011-09-20 | 2013-04-03 | 上海聚友化工有限公司 | Method for recovering organic matters in polyester wastewater |
| CN103212424A (en) * | 2013-03-08 | 2013-07-24 | 上海聚友化工有限公司 | Method for recycling glycol and acetaldehyde in polyester waste water |
| CN103360226A (en) * | 2013-04-27 | 2013-10-23 | 祁栋 | Method for recovering acetaldehyde and 2-MD (2-Methyl-1,3-Dioxolane) from polyester wastewater system and recovery system thereof |
| CN103936572A (en) * | 2014-03-22 | 2014-07-23 | 江阴市飞鸿机械有限公司 | System for recovering acetaldehyde and glycol in polyester waste water |
| CN104591474A (en) * | 2013-11-01 | 2015-05-06 | 中国石油化工股份有限公司大连石油化工研究院 | Unsaturated polyester wastewater treatment and reuse method |
| CN104844434A (en) * | 2015-05-21 | 2015-08-19 | 江苏华亚化纤有限公司 | Ethanal and ethylene glycol recovery system |
| CN104945235A (en) * | 2015-05-21 | 2015-09-30 | 江苏华亚化纤有限公司 | Method for extracting acetaldehyde and ethylene glycol from polyester wastewater |
| CN105152863A (en) * | 2015-08-13 | 2015-12-16 | 上海聚友化工有限公司 | Method for recovering ethylene glycol and acetaldehyde from polyester wastewater |
| CN110316996A (en) * | 2018-06-20 | 2019-10-11 | 杭州斯曼特建材科技有限公司 | A kind of grinding aid adding organic liquid waste |
| CN114671561A (en) * | 2022-03-08 | 2022-06-28 | 江苏德赛化纤有限公司 | Method for controlling COD of wastewater by water content of esterified substance |
| CN115353262A (en) * | 2022-10-20 | 2022-11-18 | 威海蓝创环保设备有限公司 | Esterification wastewater treatment process |
| CN115353261A (en) * | 2022-10-19 | 2022-11-18 | 威海蓝创环保设备有限公司 | Polyester waste water treatment system |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012090B (en) * | 2011-09-20 | 2015-02-11 | 上海聚友化工有限公司 | Method for recovering organic matters in polyester wastewater |
| CN103012090A (en) * | 2011-09-20 | 2013-04-03 | 上海聚友化工有限公司 | Method for recovering organic matters in polyester wastewater |
| CN103212424A (en) * | 2013-03-08 | 2013-07-24 | 上海聚友化工有限公司 | Method for recycling glycol and acetaldehyde in polyester waste water |
| CN103212424B (en) * | 2013-03-08 | 2015-02-11 | 上海聚友化工有限公司 | Method for recycling glycol and acetaldehyde in polyester waste water |
| CN103360226A (en) * | 2013-04-27 | 2013-10-23 | 祁栋 | Method for recovering acetaldehyde and 2-MD (2-Methyl-1,3-Dioxolane) from polyester wastewater system and recovery system thereof |
| CN103360226B (en) * | 2013-04-27 | 2016-05-04 | 祁栋 | A kind of method and recovery system thereof that reclaims acetaldehyde and 2-MD from polyester waste water system |
| CN104591474A (en) * | 2013-11-01 | 2015-05-06 | 中国石油化工股份有限公司大连石油化工研究院 | Unsaturated polyester wastewater treatment and reuse method |
| CN103936572B (en) * | 2014-03-22 | 2016-03-23 | 江阴市飞鸿机械有限公司 | The device of acetaldehyde and ethylene glycol is reclaimed in polyester waste water |
| CN103936572A (en) * | 2014-03-22 | 2014-07-23 | 江阴市飞鸿机械有限公司 | System for recovering acetaldehyde and glycol in polyester waste water |
| CN104945235A (en) * | 2015-05-21 | 2015-09-30 | 江苏华亚化纤有限公司 | Method for extracting acetaldehyde and ethylene glycol from polyester wastewater |
| CN104844434A (en) * | 2015-05-21 | 2015-08-19 | 江苏华亚化纤有限公司 | Ethanal and ethylene glycol recovery system |
| CN105152863A (en) * | 2015-08-13 | 2015-12-16 | 上海聚友化工有限公司 | Method for recovering ethylene glycol and acetaldehyde from polyester wastewater |
| CN110316996A (en) * | 2018-06-20 | 2019-10-11 | 杭州斯曼特建材科技有限公司 | A kind of grinding aid adding organic liquid waste |
| CN114671561A (en) * | 2022-03-08 | 2022-06-28 | 江苏德赛化纤有限公司 | Method for controlling COD of wastewater by water content of esterified substance |
| CN115353261A (en) * | 2022-10-19 | 2022-11-18 | 威海蓝创环保设备有限公司 | Polyester waste water treatment system |
| CN115353262A (en) * | 2022-10-20 | 2022-11-18 | 威海蓝创环保设备有限公司 | Esterification wastewater treatment process |
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