CN107029443A - A kind of method for being dehydrated ternary azeotrope by extracting rectifying - Google Patents
A kind of method for being dehydrated ternary azeotrope by extracting rectifying Download PDFInfo
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- CN107029443A CN107029443A CN201710318381.1A CN201710318381A CN107029443A CN 107029443 A CN107029443 A CN 107029443A CN 201710318381 A CN201710318381 A CN 201710318381A CN 107029443 A CN107029443 A CN 107029443A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/40—Extractive distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4205—Reflux ratio control splitter
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of method for being dehydrated ternary azeotrope by extracting rectifying, including configuration composite extractant, extracting rectifying are made anhydrous binary system, reclaim extractant.The present invention realizes the high-efficiency dehydration of triplex mixture system using the excellent properties of saline extraction agent.The recyclable recycling of extractant, it is to avoid environmental pollution, reduces cost, economic and environment-friendly.Simple to operate, heat is fully recycled, and energy consumption is low, and dewatering efficiency is high, is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of method for being dehydrated ternary azeotrope, it is more particularly to a kind of by extracting rectifying by ternary
The method of azeotropic mixture dehydration, belongs to technical field of chemical separation.
Background technology
In numerous areas such as chemical industry, coal chemical industry, petrochemical industry, medication chemistry, biochemical industry and environmental protection, not
It is evitable to need to separate various mixtures.Extractive distillation with salt is to contain salt solvent as the extraction of extracting rectifying
Agent is taken, its theoretical foundation is that theoretical and extracting rectifying the solvent selectivity of salt effect of dissolved salt rectifying is theoretical.Salt effect be exactly
Add non-volatile salt in the two-phase system mutually balanced, change mutual solubility and balance between the boiling point of mixture, component
Composition etc. so that the activity coefficient of each component changes, and then change the relative volatility of each component, improve separating effect.
Extractive distillation with salt is due to containing salt in extractant, and change of the salt ion the relative volatility solution component is more than
Change of the extractant the relative volatility solution component, i.e. salt effect are more than solvent effect, and this allows for saline extraction
Rectifying is compared with traditional extraction rectifying, and the consumption of extractant is greatly lowered, so as to reduce equipment investment and operating cost.
This method both improved relative volatility between separation component using salt effect, overcame traditional extraction rectifying
The shortcoming that solvent load is big, efficiency is low, solvent recovery energy consumption is big, and because salt is dissolved in extractant, can be with extractant
Reclaim and recycle, overcome salt in dissolved salt distillation process be difficult to reclaim, the deficiency such as inconvenience conveying, thus be easy to implement work
Industry metaplasia is produced.
Anhydrous binary system is prevalent in organic solvent and pharmaceutical industry, such as toluene-ethano system, benzene-ethanol body
System, hexamethylene-ethanol system etc., but aqueous ternary azeotrope is frequently resulted in actual production, it is therefore desirable to dehydration is made
Binary system.Wherein, the azeotropic point of toluene-ethano-water is 78.3 DEG C, and the azeotropic point of benzene-ethanol-water mixture is 64.9 DEG C,
The azeotropic point of hexamethylene-ethanol-water mixture is 62.39 DEG C.
The content of the invention
The need for the present invention is directed in actual production, extraction is passed through there is provided one kind using the advantage of extractive distillation with salt
The method that ternary azeotrope is dehydrated by rectifying, is mainly used in toluene-ethano-aqueous systems, benzene-ethanol-water system, and hexamethylene-
Ethanol-water system and other similar systems.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：One kind is taken off ternary azeotrope by extracting rectifying
The method of water, comprises the following steps：
(1) composite extractant is configured
Ethylene glycol and salt are added into configuration kettle, are uniformly mixed to form composite extractant；
(2) anhydrous binary system is made in extracting rectifying
Composite extractant in ternary azeotropic raw material and configuration kettle is inputted into extraction tower, the thing of extraction tower tower reactor is fallen into
Gasification rises to extraction column overhead after material is heated, and becomes liquid by the condensation of the first overhead condenser, a part is flowed back into
Enter extraction tower, another part enters binary system storage tank after then being cooled down through reactor product cooler；
(3) extractant is reclaimed
The aqueous composite extractant of extraction tower tower reactor extraction enters recovery tower, falls into the aqueous compound extraction of recovery tower tower reactor
After taking agent heated, moisture vaporization rises to recovery column overhead, and liquid, one are become by the condensation of the second overhead condenser
Divide and flow back into recovery tower, form stable concentration gradient and thermograde, another part then produces the wastewater treatment to outside battery limit (BL)
System；The extractant of recovery tower tower reactor returns to configuration kettle and recycled.
The beneficial effects of the invention are as follows：The present invention realizes triplex mixture system using the excellent properties of saline extraction agent
High-efficiency dehydration, the ternary azeotropic objects system of the amount again of the water that is particularly suitable for use in containing amount≤30%, obtained binary system reclaimed water
Han Liang≤100PPM.In addition, extractant is recycled, it is to avoid environmental pollution, cost is reduced, it is economic and environment-friendly.Energy consumption is low, dehydration
Efficiency high, is adapted to industrialized production.
On the basis of above-mentioned technical proposal, the present invention can also do following improvement.
Extractant returns to configuration kettle and carries out distilation after recycling repeatedly：Extraction in heater configuration kettle
Agent, rises to the steam at the top of configuration kettle after configuration kettle condenser condensation, is further cooled down by configuration kettle cooler again
Become liquid, into receiving tank, return again to configuration kettle and reconfigure composite extractant；Configure the remnants discharges of bottom portion.
Beneficial effect using further technical scheme is：The purpose of purifying extractant is reached, and can significantly be returned
Extractant is received, it is economic and environment-friendly.
Further, extractant heat exchanger is provided between configuration kettle and extraction tower, extraction tower is also connected with raw material heat exchange
Device, ternary azeotropic raw material enters back into extraction tower after heat exchange.
Beneficial effect using further technical scheme is：Control adds the raw material of extraction tower and the temperature of extractant, makes
Obtain raw material and extractant carries out extraction at appropriate temperatures.
Further, the extraction tower is normal pressure or negative-pressure operation, and reflux ratio is 0.4-1；The recovery tower is normal pressure or negative
Press operation, reflux ratio is 0.5-1.
Beneficial effect using further technical scheme is：Reflux ratio preferably, can balance extraction tower Ta Neire and matter
Balance, while obtaining more binary system.
Further, the ternary azeotropic raw material is fed from the bottom of extraction tower, and the aqueous composite extractant is from extraction
The top charging of tower；The aqueous composite extractant of the extraction tower tower reactor extraction is fed from the middle part of recovery tower.
Beneficial effect using further technical scheme is：So that composite extractant and ternary azeotropic raw material fully connect
Touch and react.
Further, the material of the extraction tower tower reactor is heated by the extraction tower reboiler of tower reactor；The recovery tower tower reactor
Material heated by the recovery tower reboiler of tower reactor.
Beneficial effect using further technical scheme is：Reboiler heat tower reactor material, make its produced in tower heat and
The distribution of matter, material is separated.
Further, the steam condensation water flowed out from the extraction tower reboiler and recovery tower reboiler enters steam generator,
Solidifying water heating and gasifying is gone to the corresponding units equipment and hot water thermal insulating unit of thermal medium by steam generator.
Beneficial effect using further technical scheme is：The technical scheme can form stable heating agent, refrigerant circulation system
System, can save heating institute calorific requirement.
Further, to it is described configuration kettle in extractant carry out heating be by the configuration kettle reboiler of tower reactor, coil pipe or
Chuck is realized.
Further, first overhead condenser is connected to extraction tower vacuum trap, and second overhead condenser connects
Recovery tower vacuum trap is connect, the uncooled tail gas got off of condenser can be trapped rapidly.
Beneficial effect using further technical scheme is：Avoid fixed gas aggregation build-up of pressure excessive, take away in time not
Solidifying tail gas, prevents from polluting environment.
Further, the salt is one kind in potassium acetate, calcium chloride or potassium carbonate.It is preferred that, the salt is potassium acetate.
Beneficial effect using further technical scheme is：With the use of salt, the consumption of extractant is substantially reduced, is extracted
Effect is good, and the recyclable recycling of extractant, reduces operating cost and equipment cost, is easy to implement industrialized production.
Brief description of the drawings
Fig. 1 is the structural representation of the embodiment of the present invention 1；
Fig. 2 is the structural representation of configuration composite extractant in the embodiment of the present invention 2；
Fig. 3 is the structural representation of the embodiment of the present invention 3；
Fig. 4 is the attachment structure schematic diagram of configuration kettle and extraction tower in the embodiment of the present invention 4.
Wherein, 1, configuration kettle；2nd, extraction tower；3rd, recovery tower；4th, extraction tower reboiler；5th, the first overhead condenser；6th, recovery tower
Reboiler；7th, the second overhead condenser；8th, kettle condenser is configured；9th, kettle cooler is configured；10th, receiving tank；11st, product cooling
Device；12nd, binary system storage tank；13rd, extraction tower return tank；14th, recovery tower return tank；15th, steam generator；16th, extraction tower is true
Empty trap；17th, recovery tower vacuum trap；18th, extractant heat exchanger；19th, raw material heat exchanger.
Embodiment
The principle and feature of the present invention are described below in conjunction with accompanying drawing, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
Embodiment 1
As shown in figure 1, a kind of method for being dehydrated ternary azeotrope by extracting rectifying, comprises the following steps：
(1) composite extractant is configured
Ethylene glycol and salt are added into configuration kettle 1, are uniformly mixed to form composite extractant；
(2) anhydrous binary system is made in extracting rectifying
Ternary azeotropic raw material is fed from the bottom of extraction tower 2, and aqueous composite extractant is fed from the top of extraction tower 2,
So that composite extractant and ternary azeotropic raw material are fully contacted and had an effect, the material for falling into the tower reactor of extraction tower 2 is extracted tower
It is atmospheric operation that gasification, which is risen in the tower top of extraction tower 2, extraction tower 2, after reboiler 4 is heated；By the first overhead condenser 5
Condensation becomes liquid into extraction tower return tank 13, and a part of liquid flows back into extraction tower 2, and it is 0.4-1 to control reflux ratio,
Another part liquid enters binary system storage tank 12 after then being cooled down through reactor product cooler 11；
(3) extractant is reclaimed
The aqueous composite extractant of the tower reactor of extraction tower 2 extraction is fed from the middle part of recovery tower 3, is normal in control recovery tower 3
Press operation；The aqueous composite extractant for falling into the tower reactor of recovery tower 3 is recovered after the heating of tower reboiler 6, and moisture vaporization rises to back
The tower top of tower 3 is received, liquid is become into recovery tower return tank 14, a part of liquid backflow by the condensation of the second overhead condenser 7
Into recovery tower 3, stable concentration gradient and thermograde is formed, reflux ratio is 0.5-1, and another part liquid is then produced
Waste Water Treatment outside battery limit (BL)；The extractant of the tower reactor of recovery tower 3 returns to configuration kettle 1 and recycled；
(4) after extracting rectifying is completed, when the configuration kettle 1, extraction tower 2 and the parking of recovery tower 3, protected by nitrogen
Vacuum breaker.
Embodiment 2
On the basis of embodiment 1, change in the operating condition in extraction tower 2 and recovery tower 3, extraction tower as negative pressure behaviour
Make, reflux ratio is 0.4-1；Recovery tower is negative-pressure operation, and reflux ratio is 0.5-1.
Extractant is after recycling repeatedly, and the extractant of the tower reactor of recovery tower 3 returns to configuration kettle 1 and carries out heating distillation,
As shown in Fig. 2 the steam for rising to the top of configuration kettle 1 passes through configuration kettle cooler 9 after configuration kettle condenser 8 is condensed, again
Further cooling becomes liquid, into receiving tank 10, returns again to configuration kettle 1 and reconfigures composite extractant；Configure the bottom of kettle 1
Remnants discharges；The purpose of purifying extractant is finally reached, and can significantly reclaim extractant, it is economic and environment-friendly.
Embodiment 3
On the basis of embodiment 1, the operation for changing extraction tower 2 is negative-pressure operation, and reflux ratio is 0.4-1.In addition, such as
(structural representation for showing configuration kettle again not in figure) shown in Fig. 3, boils again from the extraction tower reboiler 4 and recovery tower
The steam condensation water that device 6 flows out enters steam generator 15, and solidifying water heating and gasifying is gone to thermal medium by steam generator 15
Corresponding units equipment and hot water thermal insulating unit.The technical scheme can form stable heating agent, coolant circulating system, can save
Save heating institute calorific requirement.First overhead condenser 5 is connected to extraction tower vacuum trap 16, and the second overhead condenser 7 is connected back to
Tower vacuum trap 17 is received, the uncooled tail gas got off of condenser, extraction tower vacuum trap 16 and recovery can be trapped rapidly
Tower vacuum trap 17 is connected to vacuum buffer tank, and the tail gas of vacuum trap trapping enters vacuum buffer tank (vacuum buffer tank
Do not drawn in figure).
Embodiment 4
Only as the control to adding the raw material of extraction tower 2 and the temperature of extractant, between configuration kettle 1 and extraction tower 2
Extractant heat exchanger 18 is set, raw material heat exchanger 19 is set at the ternary azeotrope import of extraction tower 2, and raw material is by heat exchange
After enter back into extraction tower 2, referring to Fig. 4.The setting of extractant heat exchanger 18 and raw material heat exchanger 19 does not influence remaining various device
Combination.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (10)
1. a kind of method for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that comprise the following steps：
(1) composite extractant is configured
Ethylene glycol and salt are added into configuration kettle, are uniformly mixed to form composite extractant；
(2) anhydrous binary system is made in extracting rectifying
Composite extractant in ternary azeotropic raw material and configuration kettle is inputted into extraction tower, the material for falling into extraction tower tower reactor is added
Gasification rises to extraction column overhead after heat, becomes liquid by the condensation of the first overhead condenser, a part flows back into extraction
Tower, another part enters binary system storage tank after then being cooled down through reactor product cooler；
(3) extractant is reclaimed
The aqueous composite extractant of extraction tower tower reactor extraction enters recovery tower, falls into the aqueous composite extractant quilt of recovery tower tower reactor
After heating, moisture vaporization rises to recovery column overhead, and liquid is become by the condensation of the second overhead condenser, and a part is flowed back into
Enter recovery tower, form stable concentration gradient and thermograde, another part then produces the Waste Water Treatment to outside battery limit (BL)；Reclaim
The extractant of tower tower reactor returns to configuration kettle and recycled.
2. the method according to claim 1 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that extractant
After recycling repeatedly, return to configuration kettle and carry out distilation：Extractant in heater configuration kettle, rises to configuration kettle top
The steam in portion is after configuration kettle condenser condensation, and by configuration kettle cooler, further cooling becomes liquid again, into reception
Tank, returns again to configuration kettle and reconfigures composite extractant；Configure the remnants discharges of bottom portion.
3. the method according to claim 1 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that in configuration
Extractant heat exchanger is provided between kettle and extraction tower；Extraction tower is also connected with raw material heat exchanger, and ternary azeotropic raw material is by former
Extraction tower is entered back into after material heat exchanger heat exchange.
4. the method according to claim 1 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that the extraction
It is normal pressure or negative-pressure operation to take tower, and reflux ratio is 0.4-1；The recovery tower is normal pressure or negative-pressure operation, and reflux ratio is 0.5-1.
5. the method according to claim 1 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that described three
First azeotropic raw material is fed from the bottom of extraction tower, and the aqueous composite extractant is fed from the top of extraction tower；The extraction
The aqueous composite extractant of tower tower reactor extraction is fed from the middle part of recovery tower.
6. the method according to claim 1 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that the extraction
The material of tower tower reactor is taken to be heated by the extraction tower reboiler of tower reactor；The recovery tower that the material of the recovery tower tower reactor passes through tower reactor
Reboiler is heated.
7. the method according to claim 6 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that from described
Extraction tower reboiler and the steam condensation water of recovery tower reboiler outflow enter steam generator, and solidifying water is heated gas by steam generator
Change, go to the corresponding units equipment and hot water thermal insulating unit of thermal medium.
8. the method according to claim 2 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that described to match somebody with somebody
Putting the extractant in kettle can be heated by the configuration kettle reboiler, coil pipe or chuck of tower reactor.
9. the method according to claim 1 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that described
One overhead condenser is connected to extraction tower vacuum trap, and second overhead condenser connects recovery tower vacuum trap.
10. the method according to claim 1 for being dehydrated ternary azeotrope by extracting rectifying, it is characterised in that described
Salt is one kind in potassium acetate, calcium chloride or potassium carbonate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710318381.1A CN107029443A (en) | 2017-05-08 | 2017-05-08 | A kind of method for being dehydrated ternary azeotrope by extracting rectifying |
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| CN201710318381.1A CN107029443A (en) | 2017-05-08 | 2017-05-08 | A kind of method for being dehydrated ternary azeotrope by extracting rectifying |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827779A (en) * | 2017-10-30 | 2018-03-23 | 烟台国邦化工机械科技有限公司 | Batch reactive distillation production cyanoacetate compound, malonate compound device and its production technology |
| CN107998677A (en) * | 2017-10-30 | 2018-05-08 | 烟台国邦化工机械科技有限公司 | The environment-protecting clean device and process of a kind of solvent recovery |
| CN117224988A (en) * | 2023-11-16 | 2023-12-15 | 内蒙古华欣药业有限公司 | Solvent recovery method and system |
| CN107827779B (en) * | 2017-10-30 | 2024-06-04 | 烟台国邦化工机械科技有限公司 | Device for producing cyanoacetic acid ester and malonic acid ester by batch reaction rectification and production process thereof |
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| CN102816178A (en) * | 2012-09-14 | 2012-12-12 | 南通鸿志化工有限公司 | Method and special device for separating trimethyl borate from carbinol mixture |
| CN203043589U (en) * | 2012-11-23 | 2013-07-10 | 江苏和时利新材料股份有限公司 | Heat exchange energy saving device between rectifying towers |
| CN103467246A (en) * | 2013-08-20 | 2013-12-25 | 天津科林泰克科技有限公司 | Method for separating isopropanol-water compound |
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| CN101502721A (en) * | 2009-02-12 | 2009-08-12 | 南京工业大学 | Adsorption type heat pump rectification system |
| CN102816178A (en) * | 2012-09-14 | 2012-12-12 | 南通鸿志化工有限公司 | Method and special device for separating trimethyl borate from carbinol mixture |
| CN203043589U (en) * | 2012-11-23 | 2013-07-10 | 江苏和时利新材料股份有限公司 | Heat exchange energy saving device between rectifying towers |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827779A (en) * | 2017-10-30 | 2018-03-23 | 烟台国邦化工机械科技有限公司 | Batch reactive distillation production cyanoacetate compound, malonate compound device and its production technology |
| CN107998677A (en) * | 2017-10-30 | 2018-05-08 | 烟台国邦化工机械科技有限公司 | The environment-protecting clean device and process of a kind of solvent recovery |
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| CN107827779B (en) * | 2017-10-30 | 2024-06-04 | 烟台国邦化工机械科技有限公司 | Device for producing cyanoacetic acid ester and malonic acid ester by batch reaction rectification and production process thereof |
| CN117224988A (en) * | 2023-11-16 | 2023-12-15 | 内蒙古华欣药业有限公司 | Solvent recovery method and system |
| CN117224988B (en) * | 2023-11-16 | 2024-01-30 | 内蒙古华欣药业有限公司 | Solvent recovery method and system |
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