CN111995498B - Fusel oil waste liquid treatment system and method - Google Patents
Fusel oil waste liquid treatment system and method Download PDFInfo
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- CN111995498B CN111995498B CN202010504318.9A CN202010504318A CN111995498B CN 111995498 B CN111995498 B CN 111995498B CN 202010504318 A CN202010504318 A CN 202010504318A CN 111995498 B CN111995498 B CN 111995498B
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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 extraction rectifying tower, a methanol recovery tower and an ethanol recovery tower which are sequentially communicated; wherein, the bottom liquid outlet of the extraction rectifying tower is sequentially communicated with an azeotropic rectifying tower, a liquid-liquid decanter and a second dehydrating tower; the treatment system can dehydrate and separate fusel oil (waste liquid from a device for preparing methanol and glycol from coal) to separate alcohol products such as methanol, ethanol, propanol and high-carbon fusel oil (including butanol, amyl alcohol, hexanol and heptanol) of product grade, so as to realize the recycling utilization of the fusel oil, and the treatment method is simple, can realize the total recovery rate of the alcohol products to be more than 99%, has less three wastes and reduces secondary pollution.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a fusel oil waste liquid treatment system and method.
Background
In the process of preparing methanol or glycol from coal, the residual fusel oil after the distillation of the methanol or glycol contains substances such as methanol, ethanol, propanol, butanol, amyl alcohol, heptanol, water and the like, and the fusel oil waste liquid is often treated as dangerous waste, which not only causes environmental pollution, but also makes the resource not better utilized.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a fusel oil waste liquid treatment system and a fusel oil waste liquid treatment method, the treatment system can dehydrate and separate fusel oil (waste liquid from a coal-based methanol and ethylene glycol device) to separate alcohol products such as methanol, ethanol, propanol, high-carbon fusel oil (including butanol, amyl alcohol, hexanol and heptanol) and the like, thereby realizing the recycling utilization of the fusel oil.
In order to achieve the above purpose, the present invention is realized by the following technical scheme.
The fusel oil waste liquid treatment system comprises a first dehydration tower, an extraction rectifying tower, a methanol recovery tower and an ethanol recovery tower which are sequentially communicated; wherein, the bottom liquid outlet of the extraction rectifying tower is sequentially communicated with an azeotropic rectifying tower, a liquid-liquid decanter and a second dehydrating tower.
Preferably, the device further comprises 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.
Preferably, 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 rectifying tower is provided with a liquid inlet, the top of the extraction rectifying tower is provided with a solvent inlet and a material outlet, and the bottom of the extraction rectifying 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 top of the ethanol recovery tower is provided with an ethanol outlet, and the bottom of the ethanol recovery tower is provided with a propanol outlet;
the top of the azeotropic distillation tower is provided with a liquid inlet and a discharge outlet; the bottom of the azeotropic distillation tower is provided with a liquid outlet;
the solvent recovery tower is provided with a liquid inlet, the top of the solvent recovery tower is provided with a wastewater outlet, and the 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;
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 extraction rectifying tower, the material outlet of the extraction rectifying 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 rectifying tower is communicated with the liquid inlet of the azeotropic rectifying tower, the discharge outlet of the azeotropic rectifying 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 dehydrating 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 dehydrating 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, carrying out dehydration distillation, discharging most of dehydrated and distilled water from a waste water outlet at the bottom of the first dehydration tower, and delivering the dehydrated and distilled water to sewage treatment; the dehydrated and distilled fusel oil containing a small amount of water is discharged from a top liquid outlet of the first dehydration tower and enters the extractive distillation tower from a liquid inlet of the extractive distillation tower;
step 2, extracting agent glycol enters from a solvent inlet of an extraction rectifying tower, extracting and rectifying fusel oil containing a small amount of water by adopting glycol in the extraction rectifying tower, extracting water and high-carbon fusel, discharging the mixture of methanol, ethanol and propanol after extraction from a material outlet of the extraction rectifying tower, and entering from a liquid inlet of a methanol recovery tower; water, high-carbon impurity alcohol and extractant glycol are discharged from a liquid outlet of the extractive distillation tower and enter the azeotropic distillation tower;
step 3, the methanol recovery tower distills the mixture of methanol, ethanol and propanol in the tower, and distilled methanol is discharged from a methanol outlet of the methanol recovery tower for recovery;
the distilled mixture of ethanol and propanol enters an ethanol recovery tower from a liquid outlet of the methanol recovery tower, the ethanol recovery tower distills the mixture of ethanol and 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, high carbon impurity alcohol and extractant glycol in the tower by the azeotropic distillation tower, and discharging distilled water and extractant glycol from a liquid outlet of the extractive distillation tower; the distilled water and the azeotrope of the high-carbon fusel enter a liquid-liquid decanter from a discharge port of an azeotropic distillation tower to carry out phase separation to obtain a water phase and an oil phase with oil content; wherein, the water phase containing a small amount of oil enters a second dehydrating tower to dehydrate and recycle oil, the wastewater discharged from the bottom of the second recycling tower is treated with sewage, and the high-carbon impurity alcohol contained in the top of the tower is returned to a liquid-liquid decanter to carry out phase separation; the oil phase is extracted as high carbon impurity alcohol and sent to 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 rectifying tower for recycling; the removed wastewater is discharged from a liquid outlet of the solvent recovery tower for wastewater treatment.
Preferably, the higher 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 device for preparing methanol and ethylene glycol from coal), separate out product-grade methanol, ethanol, propanol and high-carbon fusel oil (including butanol, amyl alcohol, hexanol and heptanol), and realize the recycling utilization of the fusel oil.
2) The fusel oil waste liquid treatment method is simple, continuous operation can fully recycle and utilize alcohols (including alcohol, ethanol, propanol and high-carbon fusel oil) in the fusel oil waste liquid, the total recovery rate of the alcohol products can reach more than 99%, the three-waste generation amount is small, and secondary pollution is reduced.
Drawings
The invention will now be described in further detail with reference to the drawings and to specific examples.
FIG. 1 is a diagram of a fusel oil waste liquid treatment system according to 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 for illustrating 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 extraction rectifying tower, a methanol recovery tower, an ethanol recovery tower and a solvent recovery tower which are sequentially communicated; wherein, the bottom liquid outlet of the extraction rectifying tower is sequentially communicated with an azeotropic rectifying tower, a liquid-liquid decanter and a second dehydrating tower. The bottom liquid outlet of the azeotropic distillation tower is communicated with a solvent recovery tower, and the bottom liquid outlet of the solvent recovery tower is communicated with the solvent inlet of the extractive distillation tower.
Specifically, the liquid outlet of the first dehydration tower is communicated with the liquid inlet of the extraction rectifying tower, the material outlet of the extraction rectifying 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 rectifying tower is communicated with the liquid inlet of the azeotropic rectifying tower, the discharge outlet of the azeotropic rectifying 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 dehydrating 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 extraction distillation tower, so that the recycling of the extractant glycol can be realized.
The liquid outlet of the second dehydration tower is communicated with the liquid inlet of the liquid-liquid decanter, the second dehydration tower dehydrates the azeotrope of water and high-carbon fusel in the tower, and the high-carbon fusel containing a small amount of water can return to the liquid-liquid decanter for circulating 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, carrying out dehydration distillation, discharging most of dehydrated and distilled water from a waste water outlet at the bottom of the first dehydration tower, and delivering the dehydrated and distilled water to sewage treatment; and discharging the dehydrated and distilled fusel oil containing a small amount of water from a top liquid outlet of the first dehydration tower, and entering the extractive distillation tower from a liquid inlet of the extractive distillation tower.
Step 2, extracting agent glycol enters from a solvent inlet of an extraction rectifying tower, extracting and rectifying fusel oil containing a small amount of water by adopting glycol in the extraction rectifying tower, extracting water and high-carbon fusel, discharging the mixture of methanol, ethanol and propanol after extraction from a material outlet of the extraction rectifying tower, and entering from a liquid inlet of a methanol recovery tower; water, high-carbon impurity alcohol and extractant glycol are discharged from a liquid outlet of the extractive distillation tower and enter the azeotropic distillation tower; wherein the higher hetero alcohols include butanol, pentanol, hexanol and heptanol.
And 3, distilling the mixture of the methanol, the ethanol and the propanol in the methanol recovery tower by the methanol recovery tower, and discharging distilled methanol from a methanol outlet of the methanol recovery tower for recovery.
The distilled mixture of ethanol and propanol enters an ethanol recovery tower from a liquid outlet of the methanol recovery tower, the ethanol recovery tower distills the mixture of ethanol and 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 recovered.
Step 4, distilling the water, high carbon impurity alcohol and extractant glycol in the tower by the azeotropic distillation tower, and discharging distilled water and extractant glycol from a liquid outlet of the extractive distillation tower; the distilled water and the azeotrope of the high-carbon fusel enter a liquid-liquid decanter from a discharge port of an azeotropic distillation tower to carry out phase separation to obtain a water phase and an oil phase; the water phase contains a small amount of oil at the lower layer, enters a second dehydrating tower for dehydration and oil recovery, wastewater discharged from the bottom of the second recovering tower is treated by sewage, and high-carbon impurity alcohol contained in the top of the tower is returned to a liquid-liquid decanter for phase separation; the oil phase is extracted as high carbon impurity alcohol at the upper layer and sent to a tank area, and the high carbon impurity alcohol is low (less than 4 percent in total) and is not separated one by one; the discharged water and the extractant glycol enter from a liquid inlet of the solvent recovery tower, the solvent recovery tower is dehydrated, and the dehydrated extractant glycol enters from a solvent inlet of the extraction rectifying tower for recycling; the removed wastewater is discharged from a liquid outlet of the solvent recovery tower for wastewater treatment.
While the invention has been described in detail in this specification with reference to the general description and the specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (3)
1. 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, carrying out dehydration distillation, discharging most of dehydrated and distilled water from a waste water outlet at the bottom of the first dehydration tower, and delivering the dehydrated and distilled water to sewage treatment; the dehydrated and distilled fusel oil containing a small amount of water is discharged from a top liquid outlet of the first dehydration tower and enters the extractive distillation tower from a liquid inlet of the extractive distillation tower;
step 2, extracting agent glycol enters from a solvent inlet of an extraction rectifying tower, extracting and rectifying fusel oil containing a small amount of water by adopting glycol in the extraction rectifying tower, extracting water and high-carbon fusel, discharging the mixture of methanol, ethanol and propanol after extraction from a material outlet of the extraction rectifying tower, and entering from a liquid inlet of a methanol recovery tower; water, high-carbon impurity alcohol and extractant glycol are discharged from a liquid outlet of the extractive distillation tower and enter the azeotropic distillation tower;
step 3, the methanol recovery tower distills the mixture of methanol, ethanol and propanol in the tower, and distilled methanol is discharged from a methanol outlet of the methanol recovery tower for recovery;
the distilled mixture of ethanol and propanol enters an ethanol recovery tower from a liquid outlet of the methanol recovery tower, the ethanol recovery tower distills the mixture of ethanol and 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, high carbon impurity alcohol and extractant glycol in the tower by the azeotropic distillation tower, and discharging distilled water and extractant glycol from a liquid outlet of the extractive distillation tower; the distilled water and the azeotrope of the high-carbon fusel enter a liquid-liquid decanter from a discharge port of an azeotropic distillation tower to carry out phase separation to obtain a water phase and an oil phase with oil content; wherein, the water phase containing a small amount of oil enters a second dehydrating tower to dehydrate and recycle oil, the wastewater discharged from the bottom of the second recycling tower is treated with sewage, and the high-carbon impurity alcohol contained in the top of the tower is returned to a liquid-liquid decanter to carry out phase separation; the oil phase is extracted as high carbon impurity alcohol and sent to tank area.
2. The method for treating fusel oil waste liquid according to claim 1, 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 extractant glycol after dehydration enters from a solvent inlet of an extraction rectifying tower for recycling; the removed wastewater is discharged from a liquid outlet of the solvent recovery tower for wastewater treatment.
3. The method for treating fusel oil waste liquid according to claim 1, wherein in the step 2, the high carbon fusel alcohol comprises butanol, pentanol, hexanol and heptanol.
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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 |
| 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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