CN106518598A - Device and method for purifying n-hexane with N,N-dimethylacetamide solvent - Google Patents
Device and method for purifying n-hexane with N,N-dimethylacetamide solvent Download PDFInfo
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- CN106518598A CN106518598A CN201610879154.1A CN201610879154A CN106518598A CN 106518598 A CN106518598 A CN 106518598A CN 201610879154 A CN201610879154 A CN 201610879154A CN 106518598 A CN106518598 A CN 106518598A
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- tower
- solvent
- normal hexane
- hexane
- reclamation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by 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
- B01D3/34—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
Abstract
The invention provides a device and a method for purifying n-hexane with a N,N-dimethylacetamide solvent. The device comprises an n-hexane tower, an n-hexane tower top condenser, an n-hexane tower reflux tank, an n-hexane tower reflux pump, an n-hexane tower reboiler, an n-hexane tower reactor liquid pump, a solvent regeneration tower, a solvent regeneration tower top condenser, a solvent regeneration tower reflux tank, a solvent regeneration tower reflux pump, a solvent regeneration tower reboiler, a solvent regeneration tower reactor liquid pump and a poor solvent cooler. The method comprises the following steps: firstly, introducing mixed materials into the n-hexane tower, wherein the n-hexane tower is an extraction and rectification tower; introducing N,N-dimethylacetamide, serving as an extraction solvent, from the upper part of the n-hexane tower. A tower top n-hexane product is up to 99.1 percent in purity. Compared with the conventional process, the method has the advantages of simple flow, high product purity, small solvent ratio, low level of a required thermal source in a solvent regeneration process, small loss amount of the solvent and the like.
Description
Technical field
The invention belongs to petrochemical industry hexane solvent field, is related to one kind and is just adopting N, N- dimethylacetamide solvent purification
The device and method of hexane.Particularly as be on the basis of existing common process, using extraction rectifying method separate normal hexane
Methyl cyclopentane system.Wherein, extractant selects N, N- dimethyl acetylamide, and normal hexane purity is more than 99% after purification.
Background technology
Normal hexane is important industrial chemicals and solvent, is widely used in the neck such as medicine, food industry and petrochemical industry
Domain.In the raw material of production normal hexane mostly reformer, Aromatics Extractive Project unit raffinates oil.Raffinate oil middle complicated components, predominantly
C4～C8 alkane, is mingled with a small amount of alkene and aromatic hydrocarbons.The industrial normal hexane main method that separates has：Conventional distillation, extracting rectifying,
Azeotropic distillation and molecular sieve adsorption etc..Wherein, conventional distillation method has that technological process is simple, bottom temperature is relatively low, required heat
The not high advantage of source grade；As normal hexane boiling point is 68.73 DEG C, methyl cyclopentane boiling point is 71.81 DEG C, the boiling of two key components
Point is close, it is impossible to obtain high-pure normal hexane product by conventional distillation method.There is the more difficult choosing of entrainer according to azeotropic distillation rule
The problem selected, and entrainer majority steam from tower top, cause energy expenditure larger.Molecular sieve adsorption is simple to operate, can obtain
To highly purified normal hexane, due to the easy saturation of adsorbent, frequent regeneration is needed, the reason such as operating cost is higher, molecular sieve adsorption
Method is not widely used.
At present, extraction fractional distillation is the effective ways for obtaining high-purity normal hexane, separable to obtain food stage normal hexane.Make
Extraction fractional distillation purified n-hexane is used, key is exactly to select suitable extractant, and extractant boiling point and solvent ratio are directly connected to
Whole process energy expenditure.
Patent CN103664446 proposes a kind of technique with separation of extractive distillation normal hexane methyl cyclopentane, this
As extractant, bright employing N-Methyl pyrrolidone has the advantages that technological process is simple, product purity is high, but N- methylpyrroles
Alkanone regeneration temperature is higher, and regeneration temperature is more than 205 DEG C, and needed for solvent reclamation, thermal source grade is higher.
Patent CN100447118C provides the extraction rectifying method of a kind of normal hexane and methyl cyclopentane, and the invention is adopted
Dibutyl phthalate is used as extractant.Normal hexane product purity is up to 98%, but dibutyl phthalate regeneration temperature
Higher, regeneration temperature is more than 220 DEG C, and needed for solvent reclamation, thermal source grade is higher, and whole system energy expenditure is larger.
The content of the invention
For above-mentioned practical situation, the present invention provides a kind of dress of employing N, N- dimethylacetamide solvent purified n-hexane
Put and method, including normal hexane tower, normal hexane overhead condenser, normal hexane tower return tank, normal hexane tower reflux pump, normal hexane tower
Bottom reboiler, normal hexane tower reactor liquid pump, solvent regeneration tower, solvent reclamation tower top condenser, solvent regeneration tower return tank, solvent are again
Raw tower reflux pump, solvent reclamation bottom of towe reboiler, solvent reclamation tower bottoms pump, lean solvent cooler.Material to be separated for just oneself
The mixture of the alkane such as alkane, methyl cyclopentane, 2,3- dimethylbutanes and 2,2- dimethyl pentane.Mixed material is initially entered
Normal hexane tower, normal hexane tower are an extractive distillation column, using N, N- dimethyl acetylamide as extractant, N, N- dimethyl second
Amide is entered from normal hexane tower top, and tower top obtains food stage normal hexane product, and wherein methyl cyclopentane content is less than 1%.It is surplus
The hydro carbons such as remaining normal hexane, methyl cyclopentane and solvent form rich solution and produce from normal hexane bottom of towe, and rich solution passes through normal hexane tower bottoms
Pump carries out solvent reclamation into solvent regeneration tower.Solvent reclamation tower top hydrocarbon mixture delivers to oil product mediation, in hydrocarbon mixture
N, N- dimethylacetamide amine content is less than 200ppm；Solvent reclamation bottom of towe obtains lean solvent N, N- dimethyl acetylamide, Jing solvents
After regeneration tower bottoms pump, lean solvent cooler, temperature is down to 40 DEG C of Posterior circles and is used.Especially, N, N- dimethyl acetylamide boiling
Point is 165 DEG C, and solvent reclamation bottom temperature will not be too high, can effectively reduce thermal source grade.
Technical scheme：
A kind of device of employing N, N- dimethylacetamide solvent purified n-hexane, including normal hexane tower, normal hexane tower top
Condenser, normal hexane tower return tank, normal hexane tower reflux pump, normal hexane tower bottom reboiler, normal hexane tower reactor liquid pump, solvent reclamation
It is tower, solvent reclamation tower top condenser, solvent regeneration tower return tank, solvent regeneration tower reflux pump, solvent reclamation bottom of towe reboiler, molten
Agent regenerates tower bottoms pump and lean solvent cooler；Normal hexane tower top outlet is connected with normal hexane overhead condenser tube-side inlet, just
The outlet of hexane overhead condenser tube side is connected with normal hexane tower return tank entrance, and the outlet of normal hexane tower return tank is returned with normal hexane tower
Stream pump intake is connected；The discharging point two-way connection of normal hexane tower reflux pump liquid phase：(1) normal hexane tower reflux pump liquid phase discharging all the way with
Normal hexane tower top entrance is connected；(2) normal hexane tower reflux pump liquid phase discharges another road for normal hexane product；Normal hexane bottom of towe liquid phase
Discharging point two-way connection：(1) normal hexane bottom of towe liquid phase discharging is connected with normal hexane tower bottom reboiler tube-side inlet all the way, normal hexane
The outlet of tower bottom reboiler tube side is connected with normal hexane bottom of towe entrance；(2) another road of normal hexane bottom of towe liquid phase discharging and normal hexane tower
Kettle liquid pump intake is connected, and normal hexane tower bottoms pump discharge is connected with solvent regeneration tower charging aperture；Solvent reclamation tower top outlet with it is molten
Agent regeneration overhead condenser tube-side inlet is connected, and solvent reclamation tower top condenser tube journey is exported and solvent regeneration tower return tank entrance
It is connected, the outlet of solvent regeneration tower return tank is connected with solvent regeneration tower backflow pump intake；Solvent regeneration tower reflux pump discharges all the way
Mouth is headed into solvent regeneration tower to be connected, hydrocarbon mixture is delivered to oil product mediation by another road；Solvent regeneration tower bottom outlet all the way with
Solvent reclamation bottom of towe reboiler tube-side inlet is connected, and solvent reclamation bottom of towe reboiler tube side is exported and solvent reclamation bottom of towe entrance phase
Even；Another road of solvent regeneration tower bottom outlet is connected with solvent reclamation tower bottoms pump intake, solvent reclamation tower bottoms pump discharge with it is lean
Solvent cooler tube-side inlet is connected, and the outlet of lean solvent cooler tube side is connected with normal hexane tower solvent feed mouth.
A kind of method of employing N, N- dimethylacetamide solvent purified n-hexane, step are as follows：
The mixed material of the alkane such as normal hexane, methyl cyclopentane, 2,3- dimethylbutanes and 2,2- dimethyl pentane is first
It is introduced in normal hexane tower, top gaseous phase enters back into normal hexane through normal hexane overhead condenser by circulating water to 40 DEG C
Tower return tank；Liquid phase Jing normal hexane tower reflux pump in normal hexane tower return tank, used as backflow, another part is used as just for a part
Hexane product is produced；Normal hexane tower bottom reboiler is heated using steam, normal hexane tower reactor Produced Liquid Jing normal hexane tower reactor liquid pumps, is made
Feed for solvent regeneration tower；Solvent reclamation tower overhead gas through solvent reclamation tower top condenser, by circulating water to 40 DEG C, then
Into solvent regeneration tower return tank；Liquid phase Jing solvent regeneration tower reflux pump in solvent regeneration tower return tank, a part of hydro carbons mixing
Used as backflow, another part hydrocarbon mixture delivers to oil product mediation to thing, and in hydrocarbon mixture, N, N- dimethylacetamide amine content is little
In 200ppm；Solvent reclamation bottom of towe obtains N, N- dimethyl acetylamide, Jing after solvent reclamation tower bottoms pump and lean solvent cooler,
Temperature is down to 40 DEG C of Posterior circles and is used.
Normal hexane tower process parameter：Mixed material charging Board position is 46～54, and feeding temperature is 100～110 DEG C；Solvent
Charging Board position is 8～12, and solvent feed temperature is 40 DEG C, and solvent ratio is more than 7.5；100～200kPa of operating pressure, tower top temperature
76～88 DEG C of degree, 138～150 DEG C of column bottom temperature, theoretical cam curve are more than 80, reflux ratio 4～10；Normal hexane product purity is more than
99%.
Solvent regeneration tower technological parameter：Normal hexane tower reactor Produced Liquid feeds Board position 8～12, and operating pressure 100～
200kPa, 84～98 DEG C of tower top temperature, 169～180 DEG C of column bottom temperature, theoretical cam curve 20～30, reflux ratio 4～10；Hydro carbons
In mixture, N, N- dimethyl acetylamide entrainment content is less than 200ppm, and bottom of towe N, N- dimethylacetamide solvent purity is more than
99.9%.
In the mixed materials of alkane such as normal hexane, methyl cyclopentane, 2,3- dimethylbutanes, 2,2- dimethyl pentanes just oneself
The content of alkane is 25%～30%；The content of methyl cyclopentane is 11%～15%；The content of 2,3- dimethylbutanes be 1%～
2%；The content of 2,2- dimethyl pentanes is 6%～8%；The content of remaining hydro carbons is 45%～57%.
In described mixed material, the mass percentage content of normal hexane is 25%～30%；The quality hundred of methyl cyclopentane
It is 11%～15% to divide than content；The mass percentage content of 2,3- dimethylbutanes is 1%～2%；2,2- dimethyl pentanes
Mass percentage content be 6%～8%；The mass percentage content of remaining hydro carbons is 45%～57%.
Using N, N- dimethyl acetylamide, Benzoylamide, caprolactam or dimethylformamide as normal hexane tower extraction
Agent.
Beneficial effects of the present invention：The extractant that N, N- dimethyl acetylamide is adopted as purified n-hexane of the invention, compared with
Existing common process, flow process is simple, product purity is high, solvent is more relatively low than required thermal source grade during little, solvent reclamation, solvent
Run damage amount little.
Description of the drawings
Fig. 1 is normal hexane purge process process schematic representation.
In figure：1 normal hexane tower；2 normal hexane tower bottom reboilers；3 normal hexane overhead condensers；4 normal hexane tower return tanks；5
Normal hexane tower reactor liquid pump；6 normal hexane tower reflux pumps；7 solvent regeneration towers；8 solvent reclamation bottom of towe reboilers；9 solvent reclamation tower tops
Condenser；10 solvent regeneration tower return tanks；11 solvent reclamation tower bottoms pumps；12 solvent regeneration tower reflux pumps；13 lean solvents are cooled down
Device.
Specific embodiment
Below in conjunction with technical scheme and accompanying drawing, the in detail specific embodiment of the narration present invention.
The mixed material of the alkane such as normal hexane, methyl cyclopentane, 2,3- dimethylbutanes and 2,2- dimethyl pentane, it is first
Be introduced in normal hexane tower 1, top gaseous phase through normal hexane overhead condenser 3, by circulating water to 40 DEG C, enter back into just oneself
Alkane tower return tank 4；Liquid phase Jing normal hexane tower reflux pump 6 in normal hexane tower return tank 4, a part is used as backflow, another part
Produce as normal hexane product；Normal hexane tower bottom reboiler 2 is heated using steam, tower reactor Produced Liquid Jing normal hexane tower reactors liquid pump 5,
Feed as solvent regeneration tower 7；Solvent reclamation tower overhead gas through solvent reclamation tower top condenser 9, by circulating water to 40
DEG C, enter back into solvent regeneration tower return tank 10；Liquid phase Jing solvent regeneration tower reflux pump 12 in solvent regeneration tower return tank 10, one
Used as backflow, another part hydrocarbon mixture delivers to oil product mediation to some hydrocarbon mixture；7 bottom of solvent regeneration tower obtains N, N- bis-
Methylacetamide, Jing after solvent reclamation tower bottoms pump 11, lean solvent cooler 13, temperature is down to 40 DEG C of Posterior circles and is used.
Embodiment：
For 8,000 tons/year of normal hexane devices of certain petro-chemical corporation, normal hexane, methyl cyclopentane, 2,3- dimethylbutanes, 2,
In the mixed material of the alkane such as 2- dimethyl pentanes, normal hexane content is 25.6%；The content of methyl cyclopentane is 12.7%；2,
The content of 3- dimethylbutanes is 1.3%；The content of 2,2- dimethyl pentanes is 6.9%；The content of remaining hydro carbons is 53.5%.
Jing after the carried device and method of the present invention is separated, normal hexane purity reaches 99.1%；Wherein, methyl cyclopentane content≤0.8%；
In solvent reclamation tower top hydrocarbon mixture, N, N- dimethyl acetylamide entrainment is less than 200ppm；Solvent reclamation bottom of towe N, N- diformazan
Yl acetamide solvent purity is more than 99.9%.
Normal hexane tower process parameter：Mixed material charging Board position is 50, and feeding temperature is 109 DEG C；Solvent feed plate position
10 are set to, solvent feed temperature is 40 DEG C, and solvent compares 8；Operating pressure 150kPa, 82 DEG C of tower top temperature, 144 DEG C of column bottom temperature,
Theoretical cam curve 84, reflux ratio 8；Normal hexane product purity 99.1%.
Solvent regeneration tower technological parameter：Normal hexane tower reactor Produced Liquid charging Board position is 10, operating pressure 100kPa, tower top
84 DEG C of temperature, 169 DEG C of column bottom temperature, theoretical cam curve 22, reflux ratio 8；N, N- dimethyl acetylamide entrainment in hydrocarbon mixture
Content is less than 200ppm, and bottom of towe N, N- dimethylacetamide solvent purity is more than 99.9%.
The invention provides a kind of device and method of employing N, N- dimethylacetamide solvent purified n-hexane, more existing
Common process, with flow process it is simple, product purity is high, solvent is more relatively low than thermal source grade needed for during little, solvent reclamation, solvent
The advantages of race damage amount is little.
Claims (4)
1. a kind of device of employing N, N- dimethylacetamide solvent purified n-hexane, it is characterised in that the device include just oneself
Alkane tower, normal hexane overhead condenser, normal hexane tower return tank, normal hexane tower reflux pump, normal hexane tower bottom reboiler, normal hexane tower
Kettle liquid pump, solvent regeneration tower, solvent reclamation tower top condenser, solvent regeneration tower return tank, solvent regeneration tower reflux pump, solvent are again
Raw tower bottom reboiler, solvent reclamation tower bottoms pump and lean solvent cooler；Normal hexane tower top outlet and normal hexane overhead condenser
Tube-side inlet is connected, and the outlet of normal hexane overhead condenser tube side is connected with normal hexane tower return tank entrance, normal hexane tower return tank
Outlet is connected with normal hexane tower backflow pump intake；The discharging point two-way connection of normal hexane tower reflux pump liquid phase：(1) normal hexane tower backflow
Pump liquid is mutually discharged；(2) normal hexane tower reflux pump liquid phase discharges another road for normal hexane product
Product；The discharging point two-way connection of normal hexane bottom of towe liquid phase：(1) normal hexane bottom of towe liquid phase discharging all the way with normal hexane tower bottom reboiler pipe
Journey entrance is connected, and the outlet of normal hexane tower bottom reboiler tube side is connected with normal hexane bottom of towe entrance；(2) normal hexane bottom of towe liquid phase discharging
Another road is connected with normal hexane tower bottoms pump intake, and normal hexane tower bottoms pump discharge is connected with solvent regeneration tower charging aperture；Solvent
Regeneration overhead outlet is connected with solvent reclamation tower top condenser tube journey entrance, and solvent reclamation tower top condenser tube journey is exported and solvent
Regenerator return tank entrance is connected, and the outlet of solvent regeneration tower return tank is connected with solvent regeneration tower backflow pump intake；Solvent reclamation
The discharging of tower reflux pump heads into mouth with solvent regeneration tower all the way and is connected, and hydrocarbon mixture is delivered to oil product mediation by another road；Solvent is again
Raw bottom of towe outlet is connected with solvent reclamation bottom of towe reboiler tube-side inlet all the way, solvent reclamation bottom of towe reboiler tube side export with it is molten
Agent regenerator bottom entrance is connected；Another road of solvent regeneration tower bottom outlet is connected with solvent reclamation tower bottoms pump intake, solvent reclamation
Tower bottoms pump discharge is connected with lean solvent cooler tube-side inlet, and lean solvent cooler tube side is exported and normal hexane tower solvent feed
Mouth is connected.
2. a kind of method of employing N, N- dimethylacetamide solvent purified n-hexane, it is characterised in that step is as follows：
Mixed material is initially entered in normal hexane tower, and solvent enters normal hexane tower top, and top gaseous phase is cold through normal hexane tower top
Condenser, by circulating water to 40 DEG C, enters back into normal hexane tower return tank；Liquid phase Jing normal hexane tower in normal hexane tower return tank
Reflux pump, a part are produced as normal hexane product as backflow, another part；Normal hexane tower bottom reboiler is added using steam
Heat, normal hexane tower reactor Produced Liquid Jing normal hexane tower reactor liquid pumps are fed as solvent regeneration tower；Solvent reclamation tower overhead gas is through molten
Agent regeneration overhead condenser, by circulating water to 40 DEG C, enters back into solvent regeneration tower return tank；In solvent regeneration tower return tank
Liquid phase Jing solvent regeneration tower reflux pump, used as backflow, another part hydrocarbon mixture delivers to oil product tune to a part of hydrocarbon mixture
With in hydrocarbon mixture, N, N- dimethylacetamide amine content is less than 200ppm；Solvent reclamation bottom of towe obtains N, N- dimethylacetamide
Amine, Jing after solvent reclamation tower bottoms pump and lean solvent cooler, temperature is down to 40 DEG C of Posterior circles and is used；
Normal hexane tower process parameter：Mixed material charging Board position is 46～54, and feeding temperature is 100～110 DEG C；Solvent feed
Board position is 8～12, and feeding temperature is 40 DEG C, and solvent ratio is more than 7.5；100～200kPa of operating pressure, tower top temperature 76～88
DEG C, 138～150 DEG C of column bottom temperature, theoretical cam curve are more than 80, reflux ratio 4～10；Normal hexane product purity is more than 99%；
Solvent regeneration tower technological parameter：Normal hexane tower reactor Produced Liquid feeds Board position 8～12, and 100～200kPa of operating pressure is molten
84～98 DEG C of agent regeneration overhead temperature, 169～180 DEG C of solvent reclamation bottom of towe temperature, theoretical cam curve 20～30, reflux ratio 4～
10；In hydrocarbon mixture, N, N- dimethyl acetylamide entrainment content is less than 200ppm, solvent reclamation bottom of towe N, N- dimethylacetamide
Amine solvent purity is more than 99.9%.
3. method according to claim 2, it is characterised in that the mass percent of normal hexane contains in described mixed material
Measure as 25%～30%；The mass percentage content of methyl cyclopentane is 11%～15%；The quality hundred of 2,3- dimethylbutanes
It is 1%～2% to divide than content；The mass percentage content of 2,2- dimethyl pentanes is 6%～8%；The quality hundred of remaining hydro carbons
It is 45%～57% to divide than content.
4. according to the method in claim 2 or 3, it is characterised in that using N, N- dimethyl acetylamide, Benzoylamide, oneself
The extractant of lactams or dimethylformamide as normal hexane tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610879154.1A CN106518598A (en) | 2016-10-09 | 2016-10-09 | Device and method for purifying n-hexane with N,N-dimethylacetamide solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610879154.1A CN106518598A (en) | 2016-10-09 | 2016-10-09 | Device and method for purifying n-hexane with N,N-dimethylacetamide solvent |
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| CN106518598A true CN106518598A (en) | 2017-03-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610879154.1A Withdrawn CN106518598A (en) | 2016-10-09 | 2016-10-09 | Device and method for purifying n-hexane with N,N-dimethylacetamide solvent |
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Cited By (1)
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| CN107216231A (en) * | 2017-06-23 | 2017-09-29 | 太仓沪试试剂有限公司 | A kind of purification process of electron level n-hexane |
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Application publication date: 20170322 |