CN111995498A - Fusel oil waste liquid treatment system and method - Google Patents
Fusel oil waste liquid treatment system and method Download PDFInfo
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- CN111995498A CN111995498A CN202010504318.9A CN202010504318A CN111995498A CN 111995498 A CN111995498 A CN 111995498A CN 202010504318 A CN202010504318 A CN 202010504318A CN 111995498 A CN111995498 A CN 111995498A
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- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
Abstract
The invention belongs to the field of chemical industry, and discloses a fusel oil waste liquid treatment system and a fusel oil waste liquid treatment method, wherein the fusel oil waste liquid treatment system comprises a first dehydration tower, an extractive distillation tower, a methanol recovery tower and an ethanol recovery tower which are sequentially communicated; wherein a liquid outlet at the bottom of the extractive distillation tower is sequentially communicated with an azeotropic distillation tower, a liquid-liquid decanter and a second dehydration tower; the treatment system can dehydrate and separate fusel oil (waste liquid from a coal-to-methanol and glycol device) to separate out product-grade methanol, ethanol, propanol, high-carbon fusel oil (including butanol, pentanol, hexanol and heptanol) and other alcohol products, so that the resource utilization of the fusel oil is realized, the treatment method is simple, the total recovery rate of the alcohol products can reach more than 99 percent, the three wastes are less in generation amount, and the secondary pollution is reduced.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a fusel oil waste liquid treatment system and a fusel oil waste liquid treatment method.
Background
In the process of preparing methanol or glycol from coal, the residual fusel oil after distilling the methanol or the glycol contains methanol, ethanol, propanol, butanol, pentanol, heptanol, water and other substances, and fusel oil waste liquid is often treated as hazardous waste, so that not only is environmental pollution caused, but also resources are not better utilized.
Disclosure of Invention
The invention aims to provide a fusel oil waste liquid treatment system and a fusel oil waste liquid treatment method, wherein the treatment system can be used for dehydrating and separating fusel oil (waste liquid from a coal-based methanol and ethylene glycol device) to separate product-grade methanol, ethanol, propanol and high-carbon fusel oil (including butanol, pentanol, hexanol and heptanol) and other alcohol products, so that the resource utilization of the fusel oil is realized, the treatment method is simple, the total recovery rate of the alcohol products can reach more than 99%, the three-waste generation amount is small, and the secondary pollution is reduced.
In order to achieve the purpose, the invention is realized by adopting the following technical scheme.
The fusel oil waste liquid treatment system comprises a first dehydration tower, an extractive distillation tower, a methanol recovery tower and an ethanol recovery tower which are sequentially communicated; wherein, a liquid outlet at the bottom of the extractive distillation tower is sequentially communicated with an azeotropic distillation tower, a liquid-liquid decanter and a second dehydration tower.
Preferably, the device further comprises a solvent recovery tower, a bottom liquid outlet of the azeotropic distillation tower is communicated with the solvent recovery tower, and a bottom liquid outlet of the solvent recovery tower is communicated with a solvent inlet of the extractive distillation tower.
Preferably, the upper part of the side wall of the first dehydrating tower is provided with a liquid inlet, the bottom of the first dehydrating tower is provided with a waste water outlet, and the top of the first dehydrating tower is provided with a liquid outlet;
the upper part of the side wall of the extraction and rectification tower is provided with a liquid inlet, the top of the extraction and rectification tower is provided with a solvent inlet and a material outlet, and the bottom of the extraction and rectification tower is provided with a liquid outlet;
the methanol recovery tower is provided with a liquid inlet, the top of the methanol recovery tower is provided with a methanol outlet, and the bottom of the methanol recovery tower is provided with a liquid outlet;
the ethanol recovery tower is provided with a liquid inlet, the tower top of the ethanol recovery tower is provided with an ethanol outlet, and the tower bottom of the ethanol recovery tower is provided with a propanol outlet;
the tower top of the azeotropic distillation tower is provided with a liquid inlet and a discharge hole; the tower bottom of the azeotropic distillation tower is provided with a liquid outlet;
the solvent recovery tower is provided with a liquid inlet, the tower top of the solvent recovery tower is provided with a wastewater outlet, and the tower bottom of the solvent recovery tower is provided with a liquid outlet;
the liquid-liquid decanter is provided with a liquid inlet, a liquid outlet and a water-containing fusel oil outlet;
and the upper part of the side wall of the second dehydration tower is provided with a liquid inlet, the bottom of the second dehydration tower is provided with a wastewater outlet, and the top of the second dehydration tower is provided with a liquid outlet.
Preferably, the liquid outlet of the first dehydration tower is communicated with the liquid inlet of the extractive distillation tower, the material outlet of the extractive distillation tower is communicated with the liquid inlet of the methanol recovery tower, and the liquid outlet of the methanol recovery tower is communicated with the liquid inlet of the ethanol recovery tower;
the liquid outlet of the extraction and rectification tower is communicated with the liquid inlet of the azeotropic rectification tower, the discharge port of the azeotropic rectification tower is communicated with the liquid inlet of the liquid-liquid decanter, and the liquid outlet of the liquid-liquid decanter is communicated with the liquid inlet of the second dehydration tower;
the liquid outlet of the azeotropic distillation tower is communicated with the liquid inlet of the solvent recovery tower, and the liquid outlet of the solvent recovery tower is communicated with the solvent inlet of the extractive distillation tower.
Preferably, the liquid outlet of the second dehydration tower is communicated with the liquid inlet of the liquid-liquid decanter.
(II) a fusel oil waste liquid treatment method, which comprises the following steps:
step 1, pumping fusel oil waste liquid into a first dehydration tower from a liquid inlet of the first dehydration tower through a feed pump, performing dehydration distillation, discharging most of water after dehydration distillation from a tower bottom waste water outlet of the first dehydration tower, and sending the water to a sewage treatment; the fusel oil containing a small amount of water after dehydration and distillation is discharged from a liquid outlet at the top of the first dehydration tower and enters the extractive distillation tower from a liquid inlet of the extractive distillation tower;
step 2, an extractant glycol enters from a solvent inlet of an extractive distillation tower, fusel oil containing a small amount of water is subjected to extractive distillation by using the glycol in the extractive distillation tower, water and high-carbon fusel are extracted out, and a mixture of extracted methanol, ethanol and propanol is discharged from a material outlet of the extractive distillation tower and enters from a liquid inlet of a methanol recovery tower; discharging water, high-carbon fusel and an extractant glycol from a liquid outlet of the extractive distillation tower and feeding the water, the high-carbon fusel and the extractant glycol into an azeotropic distillation tower;
step 3, distilling a mixture of methanol, ethanol and propanol in the rectifying tower by using a methanol recovery tower, and discharging the distilled methanol from a methanol outlet of the methanol recovery tower for recovery;
the mixture of the ethanol and the propanol after distillation enters an ethanol recovery tower from a liquid outlet of the methanol recovery tower, the ethanol recovery tower is used for distilling the mixture of the ethanol and the propanol, and the distilled ethanol is discharged from an ethanol outlet of the ethanol recovery tower and is recovered; the distilled propanol is discharged from a propanol outlet of the ethanol recovery tower and is recovered;
step 4, distilling the water, the high-carbon fusel and the extractant glycol in the azeotropic distillation tower, and discharging the distilled water and the extractant glycol from a liquid outlet of the extractive distillation tower; feeding the azeotrope of distilled water and high-carbon fusel into a liquid-liquid decanter from a discharge hole of an azeotropic distillation tower for phase separation to obtain a water phase and an oil phase containing oil; wherein, the water phase containing a small amount of oil enters a second dehydration tower for dehydration and oil component recovery, the wastewater discharged from the bottom of the second recovery tower is subjected to sewage treatment, and the high-carbon fusel containing water at the tower top is returned to a liquid decanter for phase separation; the oil phase is extracted as high-carbon fusel and sent to a tank area.
Preferably, in the step 4, the discharged water and the extractant glycol enter from a liquid inlet of a solvent recovery tower, the solvent recovery tower is dehydrated, and the dehydrated extractant glycol enters from a solvent inlet of an extraction rectification tower for recycling; and discharging the removed wastewater from a liquid outlet of the solvent recovery tower for wastewater treatment.
Preferably, the higher fusel alcohols comprise butanol, pentanol, hexanol and heptanol.
Compared with the prior art, the invention has the beneficial effects that:
1) the fusel oil waste liquid treatment system is a continuous rectification system, can dehydrate and separate fusel oil (waste liquid from a coal-based methanol and ethylene glycol device) to separate out methanol, ethanol, propanol and high-carbon fusel oil (including butanol, pentanol, hexanol and heptanol) with product grade, and realizes resource utilization of the fusel oil.
2) The treatment method of the fusel oil waste liquid is simple and continuous, can fully recover and utilize alcohols (including alcohol, ethanol, propanol and high-carbon fusel oil) in the fusel oil waste liquid, has the total recovery rate of the alcohol products of over 99 percent, generates less three wastes and reduces secondary pollution.
Drawings
The invention is described in further detail below with reference to the figures and specific embodiments.
FIG. 1 is a schematic diagram of a fusel oil waste liquid treatment system of the present invention.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
Referring to fig. 1, a fusel oil waste liquid treatment system comprises a first dehydration tower, an extractive distillation tower, a methanol recovery tower, an ethanol recovery tower and a solvent recovery tower which are sequentially communicated; wherein, a liquid outlet at the bottom of the extractive distillation tower is sequentially communicated with an azeotropic distillation tower, a liquid-liquid decanter and a second dehydration tower. And a liquid outlet at the bottom of the azeotropic distillation tower is communicated with a solvent recovery tower, and a liquid outlet at the bottom of the solvent recovery tower is communicated with a solvent inlet of the extractive distillation tower.
Specifically, the liquid outlet of the first dehydration tower is communicated with the liquid inlet of the extractive distillation tower, the material outlet of the extractive distillation tower is communicated with the liquid inlet of the methanol recovery tower, and the liquid outlet of the methanol recovery tower is communicated with the liquid inlet of the ethanol recovery tower;
the liquid outlet of the extraction and rectification tower is communicated with the liquid inlet of the azeotropic rectification tower, the discharge port of the azeotropic rectification tower is communicated with the liquid inlet of the liquid-liquid decanter, and the liquid outlet of the liquid-liquid decanter is communicated with the liquid inlet of the second dehydration tower;
the liquid outlet of the azeotropic distillation tower is communicated with the liquid inlet of the solvent recovery tower, and the liquid outlet of the solvent recovery tower is communicated with the solvent inlet of the extractive distillation tower, so that the cyclic utilization of the extractant glycol can be realized.
And after the second dehydration tower dehydrates the azeotrope of the water and the high-carbon fusel in the tower, the high-carbon fusel containing a small amount of water can return to the liquid-liquid decanter for cyclic phase separation, so that the recovery rate of the high-carbon fusel is improved.
(II) a fusel oil waste liquid treatment method, which comprises the following steps:
step 1, pumping fusel oil waste liquid into a first dehydration tower from a liquid inlet of the first dehydration tower through a feed pump, performing dehydration distillation, discharging most of water after dehydration distillation from a tower bottom waste water outlet of the first dehydration tower, and sending the water to a sewage treatment; and the fusel oil containing a small amount of water after dehydration and distillation is discharged from a liquid outlet at the top of the first dehydration tower and enters the extractive distillation tower from a liquid inlet of the extractive distillation tower.
Step 2, an extractant glycol enters from a solvent inlet of an extractive distillation tower, fusel oil containing a small amount of water is subjected to extractive distillation by using the glycol in the extractive distillation tower, water and high-carbon fusel are extracted out, and a mixture of extracted methanol, ethanol and propanol is discharged from a material outlet of the extractive distillation tower and enters from a liquid inlet of a methanol recovery tower; discharging water, high-carbon fusel and an extractant glycol from a liquid outlet of the extractive distillation tower and feeding the water, the high-carbon fusel and the extractant glycol into an azeotropic distillation tower; wherein the higher fusel alcohols comprise butanol, pentanol, hexanol and heptanol.
And 3, distilling the mixture of the methanol, the ethanol and the propanol in the rectifying tower by the methanol recovery tower, and discharging the distilled methanol from a methanol outlet of the methanol recovery tower for recovery.
The mixture of the ethanol and the propanol after distillation enters an ethanol recovery tower from a liquid outlet of the methanol recovery tower, the ethanol recovery tower is used for distilling the mixture of the ethanol and the propanol, and the distilled ethanol is discharged from an ethanol outlet of the ethanol recovery tower and is recovered; and the distilled propanol is discharged from a propanol outlet of the ethanol recovery tower and is recovered.
Step 4, distilling the water, the high-carbon fusel and the extractant glycol in the azeotropic distillation tower, and discharging the distilled water and the extractant glycol from a liquid outlet of the extractive distillation tower; feeding the azeotrope of distilled water and high-carbon fusel into a liquid-liquid decanter from a discharge hole of an azeotropic distillation tower for phase separation to obtain a water phase and an oil phase; wherein, the water phase contains a small amount of oil in the lower layer and enters a second dehydration tower for dehydration and oil component recovery, the wastewater discharged from the bottom of the second recovery tower is subjected to sewage treatment, and the high-carbon fusel containing water in the tower top is returned to a liquid decanter for phase separation; the oil phase is extracted and sent to a tank area as high-carbon fusel on the upper layer, and the high-carbon fusel is not separated one by one because the content of the high-carbon fusel is low (the total content is less than 4 percent); the drained water and the extractant glycol enter from a liquid inlet of a solvent recovery tower, the solvent recovery tower is dehydrated, and the dehydrated extractant glycol enters from a solvent inlet of an extraction rectification tower for recycling; and discharging the removed wastewater from a liquid outlet of the solvent recovery tower for wastewater treatment.
Although the present invention has been described in detail in this specification with reference to specific embodiments and illustrative embodiments, it will be apparent to those skilled in the art that modifications and improvements can be made thereto based on the present invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (8)
1. A fusel oil waste liquid treatment system is characterized by comprising a first dehydration tower, an extractive distillation tower, a methanol recovery tower and an ethanol recovery tower which are sequentially communicated; wherein, a liquid outlet at the bottom of the extractive distillation tower is sequentially communicated with an azeotropic distillation tower, a liquid-liquid decanter and a second dehydration tower.
2. The fusel oil waste liquid treatment system according to claim 1, further comprising a solvent recovery tower, wherein a bottom liquid outlet of the azeotropic distillation tower is communicated with the solvent recovery tower, and a bottom liquid outlet of the solvent recovery tower is communicated with a solvent inlet of the extractive distillation tower.
3. The fusel oil waste liquid treatment system as claimed in claim 2, wherein the upper part of the side wall of the first dehydration tower is provided with a liquid inlet, the bottom of the first dehydration tower is provided with a waste water outlet, and the top of the first dehydration tower is provided with a liquid outlet;
the upper part of the side wall of the extraction and rectification tower is provided with a liquid inlet, the top of the extraction and rectification tower is provided with a solvent inlet and a material outlet, and the bottom of the extraction and rectification tower is provided with a liquid outlet;
the methanol recovery tower is provided with a liquid inlet, the top of the methanol recovery tower is provided with a methanol outlet, and the bottom of the methanol recovery tower is provided with a liquid outlet;
the ethanol recovery tower is provided with a liquid inlet, the tower top of the ethanol recovery tower is provided with an ethanol outlet, and the tower bottom of the ethanol recovery tower is provided with a propanol outlet;
the tower top of the azeotropic distillation tower is provided with a liquid inlet and a discharge hole; the tower bottom of the azeotropic distillation tower is provided with a liquid outlet;
the solvent recovery tower is provided with a liquid inlet, the tower top of the solvent recovery tower is provided with a wastewater outlet, and the tower bottom of the solvent recovery tower is provided with a liquid outlet;
the liquid-liquid decanter is provided with a liquid inlet, a liquid outlet and a water-containing fusel oil outlet;
and the upper part of the side wall of the second dehydration tower is provided with a liquid inlet, the bottom of the second dehydration tower is provided with a wastewater outlet, and the top of the second dehydration tower is provided with a liquid outlet.
4. The fusel oil waste liquid treatment system as claimed in claim 3, wherein the liquid outlet of the first dehydration tower is communicated with the liquid inlet of the extractive distillation tower, the material outlet of the extractive distillation tower is communicated with the liquid inlet of the methanol recovery tower, and the liquid outlet of the methanol recovery tower is communicated with the liquid inlet of the ethanol recovery tower;
the liquid outlet of the extraction and rectification tower is communicated with the liquid inlet of the azeotropic rectification tower, the discharge port of the azeotropic rectification tower is communicated with the liquid inlet of the liquid-liquid decanter, and the liquid outlet of the liquid-liquid decanter is communicated with the liquid inlet of the second dehydration tower;
the liquid outlet of the azeotropic distillation tower is communicated with the liquid inlet of the solvent recovery tower, and the liquid outlet of the solvent recovery tower is communicated with the solvent inlet of the extractive distillation tower.
5. The fusel oil waste liquid treatment system according to claim 4, wherein the liquid outlet of the second dehydration tower is communicated with the liquid inlet of the liquid-liquid decanter.
6. The fusel oil waste liquid treatment method is characterized by comprising the following steps:
step 1, pumping fusel oil waste liquid into a first dehydration tower from a liquid inlet of the first dehydration tower through a feed pump, performing dehydration distillation, discharging most of water after dehydration distillation from a tower bottom waste water outlet of the first dehydration tower, and sending the water to a sewage treatment; the fusel oil containing a small amount of water after dehydration and distillation is discharged from a liquid outlet at the top of the first dehydration tower and enters the extractive distillation tower from a liquid inlet of the extractive distillation tower;
step 2, an extractant glycol enters from a solvent inlet of an extractive distillation tower, fusel oil containing a small amount of water is subjected to extractive distillation by using the glycol in the extractive distillation tower, water and high-carbon fusel are extracted out, and a mixture of extracted methanol, ethanol and propanol is discharged from a material outlet of the extractive distillation tower and enters from a liquid inlet of a methanol recovery tower; discharging water, high-carbon fusel and an extractant glycol from a liquid outlet of the extractive distillation tower and feeding the water, the high-carbon fusel and the extractant glycol into an azeotropic distillation tower;
step 3, distilling a mixture of methanol, ethanol and propanol in the rectifying tower by using a methanol recovery tower, and discharging the distilled methanol from a methanol outlet of the methanol recovery tower for recovery;
the mixture of the ethanol and the propanol after distillation enters an ethanol recovery tower from a liquid outlet of the methanol recovery tower, the ethanol recovery tower is used for distilling the mixture of the ethanol and the propanol, and the distilled ethanol is discharged from an ethanol outlet of the ethanol recovery tower and is recovered; the distilled propanol is discharged from a propanol outlet of the ethanol recovery tower and is recovered;
step 4, distilling the water, the high-carbon fusel and the extractant glycol in the azeotropic distillation tower, and discharging the distilled water and the extractant glycol from a liquid outlet of the extractive distillation tower; feeding the azeotrope of distilled water and high-carbon fusel into a liquid-liquid decanter from a discharge hole of an azeotropic distillation tower for phase separation to obtain a water phase and an oil phase containing oil; wherein, the water phase containing a small amount of oil enters a second dehydration tower for dehydration and oil component recovery, the wastewater discharged from the bottom of the second recovery tower is subjected to sewage treatment, and the high-carbon fusel containing water at the tower top is returned to a liquid decanter for phase separation; the oil phase is extracted as high-carbon fusel and sent to a tank area.
7. The method for treating the fusel oil waste liquid according to claim 6, wherein in the step 4, the discharged water and the extractant glycol enter from a liquid inlet of a solvent recovery tower, the solvent recovery tower is dehydrated, and the dehydrated extractant glycol enters from a solvent inlet of an extraction rectification tower and is recycled; and discharging the removed wastewater from a liquid outlet of the solvent recovery tower for wastewater treatment.
8. The method of claim 6, wherein in step 2, the higher fusel alcohol comprises butanol, pentanol, hexanol, and heptanol.
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| CN202010504318.9A CN111995498B (en) | 2020-06-05 | 2020-06-05 | Fusel oil waste liquid treatment system and method |
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| CN102442882A (en) * | 2010-10-12 | 2012-05-09 | 中科合成油技术有限公司 | Separating and recovering method for organic oxygen-containing compounds in Fischer-Tropsch synthesis water phase |
| CN104529703A (en) * | 2015-01-22 | 2015-04-22 | 神华集团有限责任公司 | Separation system and separation method of low-carbon mixed alcohol |
| CN105669377A (en) * | 2016-01-22 | 2016-06-15 | 北京凯文特科技有限公司 | Technique for separating mixed alcohol |
| CN107488104A (en) * | 2017-08-25 | 2017-12-19 | 山东扬子化工有限公司 | It is a kind of to be used to purify the energy-saving distillation system of fusel oil and energy-saving rectificating method |
| CN109251133A (en) * | 2018-09-17 | 2019-01-22 | 青岛科技大学 | A kind of liquid-liquid extraction-azeotropic distillation hybrid technique of separating propylene glycol methyl ether and water |
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2020
- 2020-06-05 CN CN202010504318.9A patent/CN111995498B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102442882A (en) * | 2010-10-12 | 2012-05-09 | 中科合成油技术有限公司 | Separating and recovering method for organic oxygen-containing compounds in Fischer-Tropsch synthesis water phase |
| CN104529703A (en) * | 2015-01-22 | 2015-04-22 | 神华集团有限责任公司 | Separation system and separation method of low-carbon mixed alcohol |
| CN105669377A (en) * | 2016-01-22 | 2016-06-15 | 北京凯文特科技有限公司 | Technique for separating mixed alcohol |
| CN107488104A (en) * | 2017-08-25 | 2017-12-19 | 山东扬子化工有限公司 | It is a kind of to be used to purify the energy-saving distillation system of fusel oil and energy-saving rectificating method |
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