CN108440245A - It is a kind of to produce the device and recovery process that butanol is recycled in waste water from esterification - Google Patents
It is a kind of to produce the device and recovery process that butanol is recycled in waste water from esterification Download PDFInfo
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- CN108440245A CN108440245A CN201810395565.2A CN201810395565A CN108440245A CN 108440245 A CN108440245 A CN 108440245A CN 201810395565 A CN201810395565 A CN 201810395565A CN 108440245 A CN108440245 A CN 108440245A
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- butanol
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- waste water
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
Abstract
The present invention discloses a kind of device for being produced from esterification and recycling butanol in waste water, including waste water storage tank, Butanol Recycling tower, tower reactor cooler, tower top cooler, first-stage condenser, secondary condenser, tower buffer tank, extraction pump, feed pump and highly concentrated butanol storage container；Butanol Recycling column overhead gaseous phase outlet is connect after being connect with first-stage condenser by pipeline with secondary condenser, and first-stage condenser liquid-phase outlet is connect with tower buffer tank entrance；Secondary condenser outlet is connect with tower buffer tank；Tower buffer tank is produced butanol product by producing pump.Invention additionally discloses a kind of techniques for being produced from esterification and recycling butanol in waste water.The present invention condenses the mixed vapour of high temperature gas phase butanol and water in recovery tower out by multi-stage condensing device, enriching and recovering butanol, improve condensation efficiency, reduce reflux ratio, increase produced quantity, reduce energy expenditure, reduces production cost, the output of butanol product is improved, while solving influence of the organic wastewater containing butanol to environment.
Description
Technical field
The present invention relates to esterification production wastewater treatment recovery technology fields, and in particular to a kind of produced in waste water from esterification is returned
Receive the device and technique of butanol.
Background technology
Butanol is a kind of important chemical products, serves many purposes, chemical raw material is used as in plastics industry, in food
Be used as extractant in perfume industry.
Currently, in butyl ester production process, to make acid, the reaction was complete, and reaction generally takes the excessive method of butanol, then exists
Contain more butanol in the light component generated in distillation process, direct emission is serious for environmental pollution, also produces serious
Material waste, therefore the organic raffinat containing butanol is handled using excellent processing recovery process and obtains high-concentration butanol, such as
This one both solves harm of the butanol waste water to human body and environment, moreover it is possible to save material, generate economic benefit.
Patent CN203923057U describes a kind of improved Butanol Recycling device, has used multiple destilling tower cooperations
Method, although the method can preferably recycle butanol, it is more that the uses of multiple destilling towers causes equipment, high energy consumption,
The characteristics of complex process.
Patent CN106008158A describes a kind of device and technique recycling butanol from low-concentration organic waste water, is transporting
During row, the gas phase that tower top leaves becomes liquid phase by tower top cooler, is back in rectifying column, while butanol is constantly enriched with
In the cooling separator of tower top, butanol product is then regard the butanol being enriched in cooling separator as by tower top return pump and is sent
Go out.But the high-temp butanol gas phase in rectifying column is only carried out condensation enrichment by this method by a tower top cooler, condensation is rich
Collecting inefficient, most butanol is back to together with vapor in rectifying column again, and the material to flow back into is more, that is,
Mean that cold conditions liquid absorbs that heat evaporating capacity is bigger, and energy consumption is higher in tower, carries out high temperature rectifying again, it will go out
Existing high energy consumption, production hour is long, defect of high cost.
Invention content
It is an object of the present invention to overcome defect existing in the prior art, a kind of low cost, low energy consumption, production are provided
Working hour is shorter, the high Butanol Recycling device of yield and recovery process.
To achieve the above object, the technical solution of the present invention is to provide a kind of dresses producing recycling butanol in waste water from esterification
It sets, including waste water storage tank, Butanol Recycling tower, tower reactor cooler, tower top cooler, first-stage condenser, secondary condenser, tower top are slow
Rush tank, extraction pump, feed pump and highly concentrated butanol storage container；The waste water storage tank passes through feed pump and Butanol Recycling tower feed inlet
Connection；The Butanol Recycling column overhead gaseous phase outlet is connected to first-stage condenser by pipeline, first-stage condenser gaseous phase outlet with
Secondary condenser connects, and first-stage condenser liquid-phase outlet is connect with tower buffer tank；The liquid-phase outlet of the secondary condenser with
Tower buffer tank connects, and tower buffer tank gaseous phase outlet is connect with secondary condenser；The tower buffer tank liquid-phase outlet passes through
Extraction pump is connect with tower top cooler entrance；Tower top cooler liquid-phase outlet is connect with highly concentrated butanol storage container；The tower reactor
Cooler is connect with Butanol Recycling tower.
Preferred technical solution is that heat exchanger is additionally provided between the waste water storage tank and Butanol Recycling tower, and the butanol returns
It receives after column overhead gaseous phase outlet is connect by pipeline with heat exchanger and is connect again with first-stage condenser；The waste water storage tank and heat exchanger
It is connect again with Butanol Recycling tower feed inlet after connection.Material and the high-temp butanol gas phase of Butanol Recycling column overhead extraction pass through heat exchange
Device carries out heat exchange, reduces the thermic load of Butanol Recycling tower, reduces the energy expenditure of Butanol Recycling tower material heating, is conducive to
Device it is energy saving.
Preferred technical solution is that being additionally provided with one between the tower top cooler and highly concentrated butanol storage container detaches
Device, the separator include water phase outlet and oil phase outlet；The water phase outlet is connect with water phase recycling can, and water phase recycling can goes out
Mouth is connect with waste water storage tank；The oil phase outlet is connect with oil phase recycling can, and oil phase recycling can connects with highly concentrated butanol storage container
It connects.Liquid phase butanol by the condensation enrichment of tower top cooler also contains a large amount of water, is directly connected to Butanol Recycling tank, recycles butanol
Concentration is relatively low；Add separator, the water phase in the liquid phase butanol of separation tower top cooler enrichment and oil phase, the butanol in oil phase
The liquid phase butanol concentration of concentration ratio condenser enrichment further increases；Water phase is connect with liquid waste tank, is again gone into butanol and is returned
Receipts system improves material utilization, reduces loss.
In order to make condenser be enriched with liquid phase butanol oil phase and separation of oil, ensure extraction water phase in butanol loss
It is less, be conducive to improve the rate of recovery of butanol and obtain high-purity butanol, further preferred embodiment is that the separator is poly-
Tie separator or decanter.
Preferred technical solution is that the device that recycling butanol in waste water is produced from esterification further includes reboiler and tower reactor
Extraction pump, the Butanol Recycling tower materials at bottom of tower outlet are connect with reboiler tube-side inlet, and the tube side outlet of reboiler divides two-way,
It connect in the middle part of Butanol Recycling tower, is in addition connect all the way with the tower reactor cooler of Butanol Recycling tower by tower reactor extraction pump all the way；
It is additionally provided with valve between the reboiler and tower reactor extraction pump.The material of Butanol Recycling tower bottom of tower passes through reboiler vapour again
Change, boil-off vapor enters Butanol Recycling tower by a way outlet, and unboiled complete material is by reboiler and tower reactor cooler
Between connecting line enrichment, when being enriched to a certain concentration, by tower reactor produce pump extraction after be back to Butanol Recycling tower, carry
The amount of gas phase butanol in high recovery tower.
For the reliability for improving the corrosion resistance of recovery tower and using, reduce energy expenditure, improves separation accuracy, it is excellent
The technical solution of choosing is that the Butanol Recycling tower is column plate rectifying column.
The present invention is a kind of technique producing recycling butanol in waste water from esterification for solving prior art problem and providing, including
Following steps：
S1：The organic wastewater for coming from esterification production system is discharged into waste water storage tank；
S2：Under the conveying of feed pump, organic wastewater enters recovery tower from Butanol Recycling column overhead；
S3：To persistently be kept the temperature after the heating of Butanol Recycling tower, the high temperature gas phase that Butanol Recycling Ta Tanei rises from tower top into
Enter first-stage condenser, the liquid phase being condensed into first-stage condenser enter tower buffer tank storage, uncooled gas phase continue into
Enter after secondary condenser is condensed into liquid phase again and enter tower buffer tank storage, also has the gas of non-total condensation in tower buffer tank
Secondary condenser is mutually again introduced into be condensed；
S4：The liquid phase stored in tower buffer tank is pumped by extraction after tower top cooler carries out cooling and is used as product
It send to highly concentrated butanol storage container, Butanol Recycling tower waste water is sent behind constantly enrichment to bottom of tower to subsequent wastewater treatment device.
In order to reduce the consumption of energy, the produced quantity of butanol product is improved, preferred technical solution is the Butanol Recycling
Tower is atmospheric operation, reflux ratio 0.3-1:1.
In order to avoid the output of high-temp butanol product, operating personnel are scalded, preferred technical solution cools down for the tower top
The temperature control of device is 10-70 DEG C.
Preferred technical solution is that the mass concentration of butanol is≤20% in the esterification production waste water.
The advantages of the present invention are：The present invention is by multi-stage condensing device to the High Temperature Gas in recovery tower out
The mixed vapour of phase fourth alcohol and water is condensed, enriching and recovering butanol, improves condensation efficiency, and reduction flows back into Butanol Recycling tower
Material, reduce reflux ratio, increase produced quantity, reduce energy expenditure, reduce production cost, improve butanol product output, together
When solve influence of the organic wastewater containing butanol to environment, be particularly suitable for the recovery processing of low concentration butanol.
Description of the drawings
Fig. 1 is the structural schematic diagram of the embodiment of the present invention 1；
Fig. 2 is the structural schematic diagram of the embodiment of the present invention 2；
Fig. 3 is the structural schematic diagram of the embodiment of the present invention 3；
In figure：1, waste water storage tank；2, feed pump；3, Butanol Recycling tower；4, first-stage condenser；4.1, first-stage condenser gas phase
Outlet；4.2, first-stage condenser liquid-phase outlet；5, secondary condenser；5.1, secondary condenser liquid-phase outlet；6, tower buffer tank；
6.1, tower buffer tank gaseous phase outlet；6.2, tower buffer tank liquid-phase outlet；7, tower top cooler；8, extraction pump；9, heat exchanger；
10, coalescing separator；11, water phase recycling can；12, oil phase recycling can；13, tower reactor cooler；14, highly concentrated butanol storage container.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is further described.Following embodiment is only
For clearly illustrating technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1
As shown in Figure 1, the present invention is a kind of device for being produced from esterification and recycling butanol in waste water, including waste water storage tank 1, fourth
Alcohol recovery tower 3, tower reactor cooler 13, tower top cooler 7, first-stage condenser 4, secondary condenser 5, tower buffer tank 6, extraction pump
8, feed pump 2 and highly concentrated butanol storage container 14；The waste water storage tank 1 is connected by feed pump 2 and 3 feed inlet of Butanol Recycling tower
It connects；The Butanol Recycling tower tower 3 pushes up gaseous phase outlet and is connected to first-stage condenser 4,4 gaseous phase outlet of first-stage condenser by pipeline
4.1 connect with secondary condenser 5, and 4 liquid-phase outlet 4.2 of first-stage condenser is connect with tower buffer tank 6；The secondary condenser 5
Liquid-phase outlet 5.1 connect with tower buffer tank 6,6 gaseous phase outlet 6.1 of tower buffer tank is connect with secondary condenser 5；The tower
Top 6 liquid-phase outlet 6.2 of surge tank is connect by producing pump 8 with 7 entrance of tower top cooler；7 liquid-phase outlet of tower top cooler and height
Dense butanol storage container 14 connects；The tower reactor cooler 13 is connect with Butanol Recycling tower 3.
Embodiment 2
As shown in Fig. 2, the present invention is a kind of device for being produced from esterification and recycling butanol in waste water, including waste water storage tank 1, fourth
Alcohol recovery tower 3, tower reactor cooler 13, tower top cooler 7, first-stage condenser 4, secondary condenser 5, tower buffer tank 6, extraction pump
8, feed pump 2 and highly concentrated butanol storage container 14；The waste water storage tank 1 is connected by feed pump 2 and 3 feed inlet of Butanol Recycling tower
It connects；The Butanol Recycling tower tower 3 pushes up gaseous phase outlet and is connected to first-stage condenser 4,4 gaseous phase outlet of first-stage condenser by pipeline
4.1 connect with secondary condenser 5, and 4 liquid-phase outlet 4.2 of first-stage condenser is connect with tower buffer tank 6；The secondary condenser 5
Liquid-phase outlet 5.1 connect with tower buffer tank 6,6 gaseous phase outlet 6.1 of tower buffer tank is connect with secondary condenser 5；The tower
Top 6 liquid-phase outlet 6.2 of surge tank is connect by producing pump 8 with 7 entrance of tower top cooler；7 liquid-phase outlet of tower top cooler and height
Dense butanol storage container 14 connects；The tower reactor cooler 13 is connect with Butanol Recycling tower 3.The waste water storage tank 1 is returned with butanol
Receive and be additionally provided with heat exchanger 9 between tower 3,3 top gaseous phase of the Butanol Recycling tower outlet connect with heat exchanger 9 by pipeline after again with
First-stage condenser 4 connects；The waste water storage tank 1 is connect with 3 feed inlet of Butanol Recycling tower again after being connect with heat exchanger 9.
Embodiment 3
As shown in figure 3, the present invention is a kind of device for being produced from esterification and recycling butanol in waste water, including waste water storage tank 1, fourth
Alcohol recovery tower 3, tower reactor cooler 13, tower top cooler 7, first-stage condenser 4, secondary condenser 5, tower buffer tank 6, extraction pump
8, feed pump 2 and highly concentrated butanol storage container 14；The waste water storage tank 1 is connected by feed pump 2 and 3 feed inlet of Butanol Recycling tower
It connects；The Butanol Recycling tower tower 3 pushes up gaseous phase outlet and is connected to first-stage condenser 4,4 gaseous phase outlet of first-stage condenser by pipeline
4.1 connect with secondary condenser 5, and 4 liquid-phase outlet 4.2 of first-stage condenser is connect with tower buffer tank 6；The secondary condenser 5
Liquid-phase outlet 5.1 connect with tower buffer tank 6,6 gaseous phase outlet 6.1 of tower buffer tank is connect with secondary condenser 5；The tower
Top 6 liquid-phase outlet 6.2 of surge tank is connect by producing pump 8 with 7 entrance of tower top cooler；7 liquid-phase outlet of tower top cooler and height
Dense butanol storage container 14 connects；The tower reactor cooler 13 is connect with Butanol Recycling tower 3.The waste water storage tank 1 is returned with butanol
Receive and be additionally provided with heat exchanger 9 between tower 3,3 top gaseous phase of the Butanol Recycling tower outlet connect with heat exchanger 9 by pipeline after again with
First-stage condenser 4 connects；The waste water storage tank 1 is connect with 3 feed inlet of Butanol Recycling tower again after being connect with heat exchanger 9.The tower
A separator 10 is additionally provided between top cooler 7 and highly concentrated butanol storage container 14, the separator 10 is exported including water phase
It is exported with oil phase；The water phase outlet is connect with water phase recycling can 11, and the outlet of water phase recycling can 11 is connect with waste water storage tank 1；Institute
It states oil phase outlet to connect with oil phase recycling can 12, oil phase recycling can 12 is connect with highly concentrated butanol storage container 14.The separator
10 be coalescing separator.
Embodiment 4
With reference to attached drawing 1, the technique of butanol is recycled in a kind of production waste water from esterification described in the present embodiment, including walk as follows
Suddenly：
S1：The organic wastewater for being 10% containing butanol concentration for coming from esterification production system is discharged into waste water storage tank 1；
S2：Under the conveying of feed pump 2, organic wastewater enters recovery tower from 3 tower top of Butanol Recycling tower；
S3：Butanol Recycling tower 3 is warming up to after 120 DEG C and is persistently kept the temperature, the high temperature gas phase risen in 3 tower of Butanol Recycling tower
Enter first-stage condenser 4 from tower top, the liquid phase being condensed into first-stage condenser 4 enters the storage of tower buffer tank 6, uncooled
Gas phase goes successively to enter the storage of tower buffer tank 6 after secondary condenser 5 is condensed into liquid phase again, also has in tower buffer tank 6
The gas phase of non-total condensation is again introduced into secondary condenser 5 and is condensed；
S4：When the liquid concentration stored in tower buffer tank 6 is reached 80%, tower top cooler 7 is sent by producing pump 8
Carry out it is cooling after sent to highly concentrated butanol storage container 14 as product, 3 waste water of Butanol Recycling tower sent after being constantly enriched with to bottom of tower to
The temperature control of subsequent wastewater treatment device, the tower top cooler is 40 DEG C.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improvements and modifications
Also it should be regarded as protection scope of the present invention.
Claims (10)
1. it is a kind of from esterification produce waste water in recycle butanol device, which is characterized in that including waste water storage tank, Butanol Recycling tower,
Tower reactor cooler, tower top cooler, first-stage condenser, secondary condenser, tower buffer tank, extraction pump, feed pump and highly concentrated fourth
Alcohol storage container；The waste water storage tank is connect by feed pump with Butanol Recycling tower feed inlet；The Butanol Recycling column overhead gas
Mutually outlet is connected to first-stage condenser by pipeline, and first-stage condenser gaseous phase outlet is connect with secondary condenser, first-stage condenser
Liquid-phase outlet is connect with tower buffer tank；The liquid-phase outlet of the secondary condenser is connect with tower buffer tank, tower buffer tank
Gaseous phase outlet is connect with secondary condenser；The tower buffer tank liquid-phase outlet is connected by producing pump with tower top cooler entrance
It connects；Tower top cooler liquid-phase outlet is connect with highly concentrated butanol storage container；The tower reactor cooler is connect with Butanol Recycling tower.
2. according to claim 1 produce the device for recycling butanol in waste water from esterification, which is characterized in that the waste water storage
Heat exchanger is additionally provided between slot and Butanol Recycling tower, the Butanol Recycling column overhead gaseous phase outlet is connect by pipeline with heat exchanger
It is connect again with first-stage condenser afterwards；The waste water storage tank is connect with Butanol Recycling tower feed inlet again after being connect with heat exchanger.
3. according to claim 1 or 2 produce the device for recycling butanol in waste water from esterification, which is characterized in that the tower
A separator is additionally provided between top cooler and highly concentrated butanol storage container, the separator includes that water phase outlet and oil phase go out
Mouthful；The water phase outlet is connect with water phase recycling can, and the outlet of water phase recycling can is connect with waste water storage tank；The oil phase outlet and oil
Phase recycling can connects, and oil phase recycling can is connect with highly concentrated butanol storage container.
4. according to claim 3 produce the device for recycling butanol in waste water from esterification, which is characterized in that the separator
It is coalescing separator or decanter.
5. according to claim 1 produce the device for recycling butanol in waste water from esterification, which is characterized in that described from esterification
The device of recycling butanol further includes reboiler and tower reactor extraction pump in production waste water, Butanol Recycling tower materials at bottom of tower outlet with
Reboiler tube-side inlet connects, and the tube side outlet of reboiler divides two-way, is connect all the way in the middle part of Butanol Recycling tower, in addition a-road-through
Tower reactor extraction pump is crossed to connect with the tower reactor cooler of Butanol Recycling tower；It is additionally provided with valve between the reboiler and tower reactor extraction pump
Door.
6. producing the device for recycling butanol in waste water, feature from esterification according to 1,2,4,5 any one of claim
It is, the Butanol Recycling tower is column plate rectifying column.
7. a kind of produced in waste water from esterification using the device described in claim 1 for producing recycling butanol in waste water from esterification is returned
The technique for receiving butanol, which is characterized in that include the following steps：
S1：The organic wastewater for coming from esterification production system is discharged into waste water storage tank；
S2：Under the conveying of feed pump, organic wastewater enters recovery tower from Butanol Recycling column overhead；
S3：It is persistently kept the temperature after Butanol Recycling tower is heated up, enters one from tower top in the high temperature gas phase that Butanol Recycling Ta Tanei rises
Grade condenser, the liquid phase being condensed into first-stage condenser enter tower buffer tank storage, and uncooled gas phase goes successively to two
Grade condenser enters tower buffer tank storage after being condensed into liquid phase again, also has the gas phase of non-total condensation again in tower buffer tank
It is secondary to be condensed into secondary condenser；
S4：By the liquid phase stored in tower buffer tank by extraction be pumped into tower top cooler carry out it is cooling after be used as product send to
Highly concentrated butanol storage container, Butanol Recycling tower waste water are sent behind constantly enrichment to bottom of tower to subsequent wastewater treatment device.
8. according to claim 7 produce the technique for recycling butanol in waste water from esterification, which is characterized in that the butanol returns
Receipts tower is atmospheric operation, reflux ratio 0.3-1:1.
9. according to claim 7 produce the technique for recycling butanol in waste water from esterification, which is characterized in that the tower top is cold
But the temperature control of device is 10-70 DEG C.
10. according to claim 7 produce the technique for recycling butanol in waste water from esterification, which is characterized in that the esterification
The mass concentration for producing butanol in waste water is≤20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810395565.2A CN108440245A (en) | 2018-04-27 | 2018-04-27 | It is a kind of to produce the device and recovery process that butanol is recycled in waste water from esterification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810395565.2A CN108440245A (en) | 2018-04-27 | 2018-04-27 | It is a kind of to produce the device and recovery process that butanol is recycled in waste water from esterification |
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| Publication Number | Publication Date |
|---|---|
| CN108440245A true CN108440245A (en) | 2018-08-24 |
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| CN201810395565.2A Pending CN108440245A (en) | 2018-04-27 | 2018-04-27 | It is a kind of to produce the device and recovery process that butanol is recycled in waste water from esterification |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508847A (en) * | 2013-09-30 | 2014-01-15 | 天津大学 | Method and device for recycling high-purity butyl alcohol by dehydrating butyl alcohol |
| CN203487061U (en) * | 2013-09-30 | 2014-03-19 | 潍坊金信达生物化工有限公司 | Methanol recycling device for biodiesel production process |
| CN106008158A (en) * | 2016-05-24 | 2016-10-12 | 新疆天业（集团）有限公司 | Device and process for recovering butanol from low-concentration organic wastewater |
| CN106810450A (en) * | 2017-02-23 | 2017-06-09 | 天津大学 | The apparatus and method that a kind of catalytic reaction rectification prepares dibutyl phthalate |
-
2018
- 2018-04-27 CN CN201810395565.2A patent/CN108440245A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103508847A (en) * | 2013-09-30 | 2014-01-15 | 天津大学 | Method and device for recycling high-purity butyl alcohol by dehydrating butyl alcohol |
| CN203487061U (en) * | 2013-09-30 | 2014-03-19 | 潍坊金信达生物化工有限公司 | Methanol recycling device for biodiesel production process |
| CN106008158A (en) * | 2016-05-24 | 2016-10-12 | 新疆天业（集团）有限公司 | Device and process for recovering butanol from low-concentration organic wastewater |
| CN106810450A (en) * | 2017-02-23 | 2017-06-09 | 天津大学 | The apparatus and method that a kind of catalytic reaction rectification prepares dibutyl phthalate |
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