CN107129103B - Comprehensive treatment and utilization process and method for furfural production wastewater - Google Patents
Comprehensive treatment and utilization process and method for furfural production wastewater Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F9/00—Multistage treatment of water, waste water or sewage
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- C02F1/00—Treatment of water, waste water, or sewage
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/46—Doubly bound oxygen atoms, or two oxygen atoms singly bound to the same carbon atom
- C07D307/48—Furfural
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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Abstract
The invention discloses a comprehensive treatment and utilization process and a method for furfural production wastewater, which comprise a process and a method for evaporating and concentrating wastewater at the bottom of a coarse distillation tower, coarse furfural separation water, wastewater at the bottom of a rectification tower, wastewater for cleaning the rectification tower and wastewater in an evaporator. After the wastewater at the bottom of the crude distillation tower is precipitated and filtered, part of the wastewater is pumped back to the acid mixing tank by a pump to be used as water for acid mixing for recycling; one part of the water is pumped back to the hydrolysis reaction kettle by a pump and is used as supplementary water of the hydrolysis reaction kettle for recycling; pumping the rest part into a film evaporator by a pump for evaporation and concentration, and recycling the rest part in the furfural production process; the crude furfural separation water completely reflows to the crude distillation tower by a pump; and pumping all the wastewater at the bottom of the rectifying tower and the washing water of the rectifying tower into a film evaporator by using a pump for evaporation and concentration, and then returning the wastewater to the furfural production process for recycling. The invention can realize the comprehensive utilization of all the furfural production wastewater, does not produce secondary pollution and realizes the zero discharge of the furfural process wastewater; the energy conservation and consumption reduction of furfural production are realized; the operation cost of the furfural production device and the wastewater treatment device is low; the investment of the wastewater treatment equipment is low.
Description
Technical Field
The invention belongs to the technical field of industrial production wastewater treatment, and particularly relates to a comprehensive wastewater treatment and utilization process for furfural production, which can realize the cyclic utilization of wastewater generated in furfural production and realize zero discharge of wastewater generated in furfural production.
Background
Furfural (also known as furfural) is a faint yellow oily liquid, and is an important organic chemical solvent and production raw material; it is widely used in the industries of plastics, medicine, pesticide and the like, and is used for directly and indirectly synthesizing furfuryl alcohol, maleic anhydride, tetrachlorofuran, furan resin, furfuryl ketone resin and the like.
Furfural production is to take plants rich in polypentaose as raw materials, such as corncobs, sunflower seed hulls, wheat straws, bagasse, cotton seed hulls, rape hulls and the like, to carry out high-temperature heating in the presence of a catalyst (5% dilute sulfuric acid) to hydrolyze the polypentaose, and then to dehydrate the pentose under the same conditions to produce the furfural. The production of furfural mainly comprises the working procedures of crushing, conveying, acid preparation, acid mixing, hydrolysis, distillation, refining and the like.
The furfural production process wastewater comprises crude distillation tower bottom wastewater, crude furfural separation water, and refining process dehydration and rectification tower cleaning wastewater:
(1) crude distillation tower bottom wastewater: the main source of the furfural production wastewater is wastewater from a crude distillation tower, the p H value in the wastewater is 2.0-4.0, the wastewater contains a large amount of organic acids, mainly acetic acid, accounting for about 2-2.5% of the total amount of the wastewater, and a considerable amount of high-boiling-point organic matters, wherein the content of methylfurfural and terpenes is 0.2-0.3%, and the content of furfural is 0.05%. The production amount of wastewater at the bottom of the crude distillation tower is about 15-30 times of the production amount of furfural, the production amount of wastewater at the bottom of the crude distillation tower is related to process parameters and management levels, for example, the pressure of a hydrolysis kettle is inversely proportional to the steam consumption, and the smaller the pressure of the hydrolysis kettle is, the more the production amount of wastewater at the bottom of the crude distillation tower is;
(2) separating water from crude furfural: the crude furfural from the crude distillation tower also contains a small amount of water, the crude furfural has aldehyde water stratification phenomenon in an aldehyde separating tank due to different specific gravities, the stratified water needs to be discharged to form crude furfural separation wastewater before rectification, and the crude furfural separation water separated from the aldehyde separating tank can directly flow back to the crude distillation tower due to higher furfural content in the wastewater;
(3) and (3) dewatering by a refining process: the wastewater generated in the rectification dehydration procedure is obtained by condensing water vapor and low-boiling-point substances, is completely discharged into a water evaporator system, and is evaporated and returned to the furfural production for recycling;
(4) washing wastewater of the rectifying tower: in order to ensure the quality of furfural products and prevent high-boiling-point resinous substances from being brought into finished products by aldehyde gas due to excessive accumulation, the rectifying tower needs to be cleaned, thereby generating cleaning wastewater.
China is a large country for producing furfural, more than 500 furfural production enterprises are shared in China at present, and the yield and the quality of furfural are in the forefront of the world. The furfural wastewater belongs to high-concentration and difficultly-degraded organic wastewater, the treatment process and technology of the furfural wastewater at home and abroad mainly comprise a neutralization method, an extraction-rectification method, an electrodialysis method, a phase transfer technology, a catalytic oxidation method, a biochemical method, an artificial wetland method and the like, and the wastewater can not be comprehensively utilized, secondary pollution can be generated, the zero discharge of the furfural process wastewater can not be realized, and the operation cost of a furfural production device and a wastewater treatment device is high; high investment of wastewater treatment equipment and the like. At present, a considerable part of furfural production enterprises still have the three-waste treatment which can not meet the requirements of national environmental protection treatment, and although the waste water is treated, the zero discharge can not be realized due to the treatment process, and the environment and the underground water are seriously polluted. Along with the increasingly strengthened environmental protection treatment strength of China, the environmental protection pressure of furfural production enterprises is increasing, and the problem of three-waste pollution treatment is still a problem to be deeply and thoroughly solved by many furfural production enterprises.
Disclosure of Invention
The invention provides a furfural wastewater comprehensive treatment and utilization process and a method aiming at the crude distillation tower bottom wastewater, the crude furfural separation water, the dehydration of a refining process, the cleaning wastewater of a rectifying tower and the evaporation concentrated solution of a wastewater evaporator generated in the existing furfural production, so that the furfural production wastewater can be comprehensively utilized, no secondary pollution is generated, and the zero discharge of the furfural process wastewater is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
a furfural production process comprises the working procedures of crushing, conveying, acid preparation and mixing, hydrolysis, distillation, aldehyde-water separation and furfural refining, wherein the furfural production process flow is schematic, and furfural production wastewater generation nodes are shown as a box 1 in a figure 1. The process flow of the treatment process of the furfural production wastewater is schematically shown as the content of a frame 2 in fig. 1, and comprises a treatment process of crude distillation tower bottom wastewater, crude furfural separation water, dehydration of a refining process and cleaning wastewater of a rectifying tower in furfural production, and a waste liquid treatment process of evaporator concentrated solution treatment; respectively treating the 5 kinds of wastewater according to different components and working conditions of the wastewater, and simultaneously recycling a part of wastewater in time according to the requirements of a furfural production process; and returning the other part of the wastewater which cannot be recycled in time to the film evaporator for evaporation and concentration and then recycling the wastewater to the furfural production process.
The comprehensive treatment and utilization process of the furfural production wastewater comprises a crude distillation tower bottom wastewater treatment process, a crude furfural separation water treatment process, a refining process dehydration treatment process, a rectification tower cleaning wastewater treatment process and an evaporator evaporation concentrated solution treatment process.
The process for treating wastewater at the bottom of the crude distillation tower is wastewater discharged from the bottom of the crude distillation tower for producing furfural, wherein the wastewater contains a large amount of acetic acid, methylfurfural, furfural and the like; after the partial waste water is precipitated and filtered, one part of the waste water is returned to the acid mixing process to be used as acid mixing water for recycling, one part of the waste water is returned to the hydrolysis process to be used as supplementary water for recycling of the hydrolysis reaction kettle, and the rest of the waste water is returned to the film evaporator to be evaporated and concentrated to be reused in the furfural production process.
The process for treating the crude furfural separation water is characterized in that a small amount of water contained in crude furfural distilled from a crude distillation tower is subjected to aldehyde water stratification in an aldehyde separation tank due to different specific gravities, the stratified water is discharged to form crude furfural separation wastewater before entering a rectification tower, the furfural content in the wastewater is high, and the wastewater is directly and completely refluxed into the crude distillation tower to be supplemented for recycling of a crude distillation tower liquid.
The refining process dehydration treatment process is waste water generated by condensation of water vapor and low-boiling-point substances in the rectification process dehydration working procedure, and the waste water is completely discharged into a film evaporator for evaporation and concentration and then is recycled in the furfural production process.
The process for treating the washing wastewater of the rectifying tower aims to ensure the quality of furfural products and prevent excessive accumulation of high-boiling-point resinous substances from being brought into the furfural finished products by furfural gas, the rectifying tower needs to be periodically cleaned to generate washing wastewater, and the wastewater is completely discharged into a film evaporator for evaporation and concentration and then is recycled in the furfural production process.
The evaporator evaporation concentration treatment process is characterized in that residual part of wastewater discharged from the bottom of the coarse distillation tower is recycled, and dehydration of a refining process and wastewater cleaned by the rectification tower are discharged into the double-effect thin film evaporator for evaporation and concentration and then are recycled in the furfural production process. According to the double-effect film evaporator, the first-effect evaporator heats the wastewater by adopting high-temperature furfural gas generated in the production process, the furfural gas is cooled, a heat source for heating the wastewater is also solved, and the second-effect evaporator heats the wastewater by adopting steam generated by the first-effect evaporator. The double-effect evaporator is matched with the use of the steam of the production boiler according to the self operation requirement, and insufficient heat is provided by the steam of the boiler. And steam generated by the double-effect evaporator is mixed and regulated in a steam mixer by using boiler steam according to the requirements of the operating temperature and pressure of the rough distillation tower, and is supplied to the rough distillation tower. Adding sodium hydroxide or sodium carbonate into the concentrated solution generated by the double-effect evaporator, and decoloring, evaporating and crystallizing to obtain a finished product of sodium acetate. The evaporated liquor of the concentrated solution returns to the wastewater treatment system for circular treatment, and the residual liquor after the concentrated solution is evaporated is recycled.
The invention has the beneficial effects that:
(1) the invention can realize the comprehensive utilization of all the furfural production wastewater, does not produce secondary pollution and realizes the zero discharge of the furfural process wastewater;
(2) the invention can realize energy saving and consumption reduction in furfural production. The acetic acid in the wastewater is recycled, and the usage amount of sulfuric acid of 50-80 kg per ton of furfural can be saved; the waste water is recycled, about 12-16 tons of fresh water is saved for each ton of furfural, the comprehensive utilization of waste heat is realized, and the energy conservation is realized; recycling the waste water, wherein the waste water produced by each ton of furfural can recover about 16-18kg of furfural;
(3) the invention can realize that the running cost of the device for producing the furfural and the wastewater treatment device is lower than that of other sewage treatment modes;
(4) compared with other sewage treatment modes, the wastewater treatment device for furfural production has low equipment investment.
Drawings
The content of a frame 1 in fig. 1 is a schematic view of a furfural production wastewater generation node of the present invention, and the content of a frame 2 in fig. 1 is a schematic view of a process flow of furfural production wastewater treatment of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following examples and drawings:
as shown in a box 1 of figure 1, the comprehensive treatment and utilization process and method for furfural production wastewater comprise the steps of generating crude distillation tower bottom wastewater at the bottom of a crude distillation tower, generating crude furfural separation water by a crude furfural separator, generating rectification tower bottom wastewater at the bottom of a rectification tower, generating rectification tower cleaning wastewater and performing evaporation concentration treatment and utilization process and method by an evaporator in the furfural production process.
The process and the method for treating and utilizing the wastewater at the bottom of the crude distillation tower are characterized in that a large amount of residual liquid containing acetic acid, methylfurfural, furfural and the like is extracted from the crude distillation tower for producing furfural through distillation, the residual liquid is discharged from the bottom of the crude distillation tower, after precipitation and filtration, one part of the residual liquid is pumped back to an acid mixing and acid mixing tank by a pump to be used as acid mixing water for recycling, one part of the residual liquid is pumped back to a hydrolysis reaction kettle by a pump to be used as supplementary water for the hydrolysis reaction kettle to be recycled, and the residual liquid is pumped back to a film evaporator by a pump to be evaporated and concentrated to be recycled in the furfural production process.
The process and the method for treating the crude furfural separation water discharge layered water generated in the aldehyde-water separation tank of crude furfural from the aldehyde-water separation tank to form crude furfural separation wastewater, and directly refluxing the wastewater to a crude distillation tower by a pump due to the higher furfural content in the wastewater, and supplementing the wastewater for recycling the tower liquid of the crude distillation tower.
The process and the method for treating the wastewater at the bottom of the rectifying tower are characterized in that residual liquid extracted from furfural by rectification in a rectifying tower for producing the furfural is discharged from the bottom of the rectifying tower to form wastewater at the bottom of the rectifying tower, and the wastewater is pumped into a thin film evaporator by a pump to be evaporated and concentrated and then is recycled in the furfural production process.
The process and the method for treating the washing wastewater of the rectifying tower are characterized in that high-boiling-point resinous substances accumulated in the rectifying tower are periodically washed by high-temperature steam to generate washing wastewater which is discharged from the bottom of the rectifying tower, and the washing wastewater is pumped into a film evaporator by a pump to be evaporated and concentrated and then is recycled in the furfural production process.
The evaporation concentration treatment process and the method of the evaporator are characterized in that the residual part of the wastewater discharged from the bottom of the coarse distillation tower after the wastewater is recycled, the wastewater at the bottom of the rectification tower and the wastewater for cleaning the rectification tower are pumped into a double-effect film evaporator by a pump to be evaporated and concentrated, in the double-effect evaporator, the first-effect evaporator adopts high-temperature furfural gas generated in the production process to heat the wastewater, the furfural gas is cooled, the heat source for heating the wastewater is also solved, and the second-effect evaporator adopts steam generated by the first-effect evaporator to heat the wastewater. The double-effect evaporator is matched with the steam of a production boiler for use according to the self operation condition requirements, and insufficient heat is provided by the steam of the boiler. And steam generated by the double-effect evaporator is mixed and regulated in a steam mixer by using boiler steam according to the requirements of the operating temperature and pressure of the rough distillation tower, and is supplied to the rough distillation tower. Adding sodium hydroxide or sodium carbonate into the concentrated solution generated by the double-effect evaporator, and decoloring, evaporating and crystallizing to obtain a finished product of sodium acetate. The evaporated liquor of the concentrated solution returns to the wastewater treatment system for circular treatment, and the residual liquor after the concentrated solution is evaporated is recycled.
Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.
Claims (1)
1. A comprehensive treatment and utilization process for furfural production wastewater realizes the comprehensive utilization of all furfural production wastewater, does not produce secondary pollution, and realizes the zero discharge of furfural process wastewater; the comprehensive treatment and utilization process of the furfural production wastewater comprises the steps of crude distillation tower bottom wastewater treatment, crude furfural separation water treatment, refining process dehydration treatment, distillation tower cleaning wastewater treatment and thin film evaporator evaporation concentrated solution treatment;
the crude distillation tower bottom wastewater treatment comprises the steps of distilling a crude distillation tower for producing furfural to extract residual liquid containing a large amount of acetic acid, methylfurfural and furfural, discharging the residual liquid from the bottom of the crude distillation tower to form crude distillation tower bottom wastewater, precipitating and filtering the wastewater, pumping one part of the wastewater back to an acid mixing and acid stirring tank by using a pump, and recycling the wastewater used for acid mixing; one part of the water is pumped back to the hydrolysis reaction kettle by a pump and is used as supplementary water of the hydrolysis reaction kettle for recycling; pumping the rest part of the furfural residue to a film evaporator by a pump for evaporation and concentration, and recycling the residue to the furfural production process;
the crude furfural separation water treatment is to discharge layered water generated in the aldehyde-water separation tank from the crude furfural to form crude furfural separation wastewater, directly reflux the wastewater to the crude distillation tower by a pump, and supplement the wastewater for recycling of the crude distillation tower liquid;
the rectification tower bottom wastewater treatment is to discharge residual liquid extracted from furfural by rectification in a rectification tower for producing furfural from the bottom of the rectification tower to form rectification tower bottom wastewater, and the wastewater is pumped into a film evaporator by a pump to be evaporated and concentrated and then returns to the furfural production process for recycling;
the treatment of the washing wastewater of the rectifying tower is to use high-boiling point resinous substances accumulated in the rectifying tower to be regularly washed by high-temperature steam to generate washing wastewater to be discharged from the bottom of the rectifying tower, and the wastewater is pumped into a film evaporator by a pump to be evaporated and concentrated and then returns to the furfural production process for recycling;
the thin film evaporator evaporation concentration treatment is to pump the residual part of the wastewater discharged from the bottom of the crude distillation tower after cyclic utilization, the wastewater at the bottom of the rectification tower and the wastewater for washing the rectification tower into a double-effect thin film evaporator by a pump for evaporation and concentration, wherein in the double-effect evaporator, the first-effect evaporator heats the wastewater by using high-temperature furfural gas generated in the production process and generates first-effect evaporation steam, the furfural gas is cooled, the heat source for heating the wastewater is also solved, and the second-effect evaporator heats the wastewater by using the first-effect evaporation steam and generates second-effect evaporation steam; the double-effect evaporator is matched with the steam of a production boiler for use according to the self operating condition requirements, and insufficient heat is provided by the steam of the boiler; mixing, regulating temperature and pressure by using boiler steam in a steam mixer according to the requirements of the operating temperature and pressure of the coarse distillation tower on the primary effect evaporation steam and the secondary effect evaporation steam generated by the double-effect evaporator, and supplying the mixed steam to the coarse distillation tower; adding sodium hydroxide or sodium carbonate into the concentrated solution generated by the double-effect evaporator, and decoloring, evaporating and crystallizing to obtain a finished product of sodium acetate; the evaporated liquor of the concentrated solution returns to the wastewater treatment system for circular treatment, and the residual liquor after the concentrated solution is evaporated is continuously recycled.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4032412A (en) * | 1971-07-23 | 1977-06-28 | Deutsche Texaco Aktiengesellschaft | Process for optimal pressure control in a multi-stage evaporation unit |
| CN1915853A (en) * | 2006-09-13 | 2007-02-21 | 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 |
| CN1923729A (en) * | 2006-06-07 | 2007-03-07 | 济南圣泉集团股份有限公司 | Method and system for treating furfural production waste water and method and system for furfural production |
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| CN101012092A (en) * | 2007-01-24 | 2007-08-08 | 沈阳理工大学 | Process for treating furfural waste water |
| US20110049054A1 (en) * | 2007-09-20 | 2011-03-03 | Verenium Corporation | Wastewater treatment system |
| CN105198150A (en) * | 2015-10-23 | 2015-12-30 | 上海毅知实业有限公司 | Reuse treatment process device for furfural wastewater |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4032412A (en) * | 1971-07-23 | 1977-06-28 | Deutsche Texaco Aktiengesellschaft | Process for optimal pressure control in a multi-stage evaporation unit |
| CN1923729A (en) * | 2006-06-07 | 2007-03-07 | 济南圣泉集团股份有限公司 | Method and system for treating furfural production waste water and method and system for furfural production |
| CN100352776C (en) * | 2006-06-07 | 2007-12-05 | 济南圣泉集团股份有限公司 | Method and system for treating furfural production waste water and method and system for furfural production |
| CN1915853A (en) * | 2006-09-13 | 2007-02-21 | 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 |
| 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 |
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