CN109722272A - A kind of solvent purification methods and device - Google Patents
A kind of solvent purification methods and device Download PDFInfo
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- CN109722272A CN109722272A CN201811540673.0A CN201811540673A CN109722272A CN 109722272 A CN109722272 A CN 109722272A CN 201811540673 A CN201811540673 A CN 201811540673A CN 109722272 A CN109722272 A CN 109722272A
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- coal tar
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Abstract
The present invention relates to a kind of solvent purification methods and devices, belong to solvent refining technical field.Using ceramic filtration membrane technology, easy to operate, superior product quality, low energy consumption, realizes clean manufacturing, reduces occupied area.Ceramic filtration membrane technology has been obviously improved product quality, and coal tar moisture content is down to 100mg/L hereinafter, suspension content is down to 0.5mg/L hereinafter, being suitable for industrial production.
Description
Technical field
The present invention relates to a kind of solvent purification methods and devices, belong to solvent refining technical field.
Background technique
Coal tar is a kind of complex mixture of the hydrocarbon of high aromaticity, and the overwhelming majority is for band side chain or without side
The heterocyclic compound of the polycyclic of chain, fused ring compound and oxygen-containing, sulphur, nitrogen, and contain a small amount of aliphatic hydrocarbon, cycloalkane and unsaturation
Hydrocarbon is also entrained with coal dust, burnt dirt and pyrolytic carbon.The coal tar just recycled is also containing 5% or so dissolved with plurality of inorganic salt and other
The moisture of impurity.Due to the presence for the pyrolytic carbon for having particle superfine, moisture often forms stable emulsion with oil.
In the prior art, not there is the method that purification process preferably is carried out to coal tar.
Summary of the invention
The object of the present invention is to provide a kind of methods that coal tar carries out purification process.
Technical solution is:
The first aspect of the invention provides:
A kind of solvent purification methods, the solvent are coal tar, are included the following steps:
Coal tar crude product is filtered using ceramic membrane, obtains trapped fluid and penetrating fluid, wherein penetrating fluid is by after purification
Coal tar.
In one embodiment, the coal tar water content ranges are in 0.001~10wt%, preferred range
0.01~5wt% is further preferably 0.05~2wt%.The coal tar suspension content range is in 0.001~5wt%, more preferably
Range be 0.01~2wt%, be further preferably 0.05~1wt%.
In one embodiment, coal tar first passes through the mode of stratification before being filtered into ceramic membrane
Water removal.
In one embodiment, the ceramic membrane can be ceramic micro filter film either ceramic super-filtering film, microfiltration membranes
The film that can be 0.05 μm~1 μm for average pore size can be 0.005 μm~0.05 for Average Pore Size of UF Membrane of the invention
μm, or be the film of 10000~500000Da for molecular cut off.
In one embodiment, during ceramic membrane filter, transmembrane pressure range is 0.01~1Mpa, preferably 0.05~
0.2MPa。
In one embodiment, during ceramic membrane filter, crossflow velocity is 0.1~10m/s, preferably 3~5m/s.
In one embodiment, during ceramic membrane filter, filtration temperature is preferably 10~100 DEG C, preferably 20~40
℃。
In one embodiment, it is added molecular sieve in coal tar, the additional amount of molecular sieve the 1 of coal tar weight~
5%。
The second aspect of the invention provides:
A kind of solvent purification device, the solvent are coal tar, comprising:
Washing oil tower, for carrying out carrying out washing treatment to coal gas using absorbing liquid；
Primary distillation tower is connected to washing oil tower, and the rich solution for obtaining to washing carries out pre-distillation processing, removes heavy constituent, obtains coal
Tar steam；
Condenser is connected to primary distillation tower, coal tar coal tar；
First layer tank, is connected to condenser, for carrying out stratification to coal tar；
Purpose ceramic-film filter is connected to first layer tank, for being filtered processing to coal tar obtained in first layer tank；
Product collecting tank is connected to the per-meate side of purpose ceramic-film filter, for collecting the coal tar after purification obtained.
In one embodiment, further include the second layering tank, be connected to the retention side of purpose ceramic-film filter, for cut
Liquid is stayed to carry out layered shaping, the second layering tank is also attached to the import of purpose ceramic-film filter.
In one embodiment, the ceramic membrane in purpose ceramic-film filter can be ceramic micro filter film either Ceramic excessive filtration
Film, microfiltration membranes are the film that average pore size can be 0.05 μm~1 μm, be can be for Average Pore Size of UF Membrane of the invention
0.005 μm~0.05 μm, or be the film of 10000~500000Da for molecular cut off.
Beneficial effect
The present invention provides a kind of methods of membrane separation technique purifying coal tar impurity, using ceramic filtration membrane technology, easy to operate,
Superior product quality, low energy consumption, realizes clean manufacturing, reduces occupied area.
Detailed description of the invention
Fig. 1 is solvent purification device figure provided by the invention；
Wherein, 1, washing oil tower；2, primary distillation tower；3, condenser；4, first layer tank；5, purpose ceramic-film filter；6, product collecting tank；
7, the second layering tank.
Specific embodiment
The object of the present invention is to provide a kind of purification process of solvent and devices, pass through UF membrane skill more particularly to one kind
The method that art purifies coal tar impurity needs to reduce coal tar suspension content, reduces water content in coal tar, and operates letter
List, pollution is small, be able to achieve clean manufacturing, is suitable for large-scale production.Purifying dehydration is mainly carried out by ceramic filtration membrane technology
Except miscellaneous operation.
Coal tar is a kind of complex mixture of the hydrocarbon of high aromaticity, and the overwhelming majority is for band side chain or without side
The heterocyclic compound of the polycyclic of chain, fused ring compound and oxygen-containing, sulphur, nitrogen, and contain a small amount of aliphatic hydrocarbon, cycloalkane and unsaturation
Hydrocarbon is also entrained with coal dust, burnt dirt and pyrolytic carbon.The coal tar just recycled is also containing 5% or so dissolved with plurality of inorganic salt and other
The moisture of impurity.Due to the presence for the pyrolytic carbon for having particle superfine, moisture often forms stable emulsion with oil.
The ceramic membrane polishing purification method that the present invention is applicable in, the material coal tar water content ranges being applicable in are 0.001
~10wt%, preferred range are 0.01~5wt%, are further preferably 0.05~2wt%, be also possible to such as 0.1%, 0.3%,
0.8%, the water contents range such as 1.2%, 2.2%, 3.4%, 4.2%.The coal tar suspension content range in 0.001~5wt%,
Preferred range is 0.01~2wt%, is further preferably 0.05~1wt%, be also possible to such as 0.2%, 0.4%, 0.8%, 1.2%,
1.6%, the suspension contents range such as 2%.
In order to keep the removal rate of moisture and impurity in ceramic membrane separation coal tar more preferable, in a preferred embodiment,
Standing, layered shaping can be first passed through to above-mentioned reaction material liquid in advance, water layer is removed, then water content, object amount containing suspension are dropped
Low organic phase is sent into ceramic membrane and is filtered, since the moisture content in organic phase is lower, so that oil is mutually in fenestra
Continuous phase can make to soak in fenestra, keep the rejection of moisture higher.
In the methods described above, ceramic membrane used can be ceramic micro filter film or ceramic super-filtering film, and microfiltration membranes are
Average pore size can be 0.05 μm~1 μm of film, can be 0.005 μm~0.05 μ for Average Pore Size of UF Membrane of the invention
M, or be the film of 10000~500000Da for molecular cut off, here, being difficult to use electronics since the aperture of ultrafiltration membrane is too small
Microscope etc. measures the aperture of film surface, so replace average pore size as pore size with the value of referred to as molecular cut off
Index.About molecular cut off, as documented in the textbook of this field: " will be using molecular weight solute as horizontal axis, resistance
Only rate is the longitudinal axis, and curve made of drawing to data is known as molecular cut off curve.And by prevention rate be 90% molecule
Amount is known as the molecular cut off of film ", index of the molecular cut off as the film properties for indicating ultrafiltration membrane is those skilled in the art
It is known.Its filter core shape includes plate membrane, tubular film, multi-channel type film, spiral membrane, hollow-fibre membrane etc., all module shapes
Formula.
As the porous film material for constituting ceramic membrane, can suitably be selected from conventionally known ceramic material.For example, can
To use aluminium oxide, zirconium oxide, magnesia, silica, titanium oxide, cerium oxide, yttrium oxide, the oxide materials such as barium titanate；
The combined oxidations species material such as cordierite, mullite, forsterite, steatite, sialon, zircon, ferrite；
Silicon nitride, aluminum nitride and other nitride class material；The carbon compounds material such as silicon carbide；The hydroxides composition material such as hydroxyapatite；
The elements class material such as carbon, silicon；Or the two or more inorganic composite materials etc. containing them.Natural minerals can also be used
(clay, clay mineral, grog, silica sand, pottery stone, feldspar, white sand) or blast-furnace slag, flying dust etc..Wherein, it is preferably selected from oxidation
It is aluminium, zirconium dioxide, titanium oxide, magnesia, one kind or two or more in silica, more preferably with aluminium oxide, zirconium dioxide or
The ceramic powders that titanium oxide is constituted as main body.Wherein, the 50wt% of " as main body " mentioned here expression ceramic powders totality
(preferably 75wt% or more, more preferable 80wt%~100wt%) is aluminium oxide or silica above.For example, in the porous material,
Aluminium oxide is relatively inexpensive and operational excellent.Further, it is possible to be readily formed with the porous of the aperture for being suitable for liquid separation
Structure, therefore the ceramic separation film with excellent liquid permeability can be easily manufactured.Also, in above-mentioned aluminium oxide,
Particularly preferably use Alpha-alumina.Alpha-alumina has stable in chemical aspect and fusing point and high mechanical strength characteristic.Cause
This can manufacture the ceramic separation film that can be utilized in broad use (such as industrial circle) by using Alpha-alumina.Separately
Outside, can also be had preferable lipophilic using the ceramic membrane for carrying out organic matter graft modification to ceramic membrane surface.
Grope by a large number of experiments, the range of the average pore size of filter membrane is 50~200nm, because aperture is too big, be will lead to
The purity of product declines；Aperture is too small, and flux is lower.During filtering filter, the selection of transmembrane pressure and being averaged for ultrafiltration membrane
There is interactional relationship in aperture, filtration flux, if transmembrane pressure is excessive, fouling membrane is accelerated, and system stability weakens, such as
Fruit transmembrane pressure is too small, then filtration flux is too small, and cost of investment increases.By groping for a large number of experiments, preferred transmembrane pressure
Range is 0.05~0.2MPa.Crossflow velocity influences whether filtration flux, if crossflow velocity is excessive, energy consumption increase causes to run
Increased costs, if crossflow velocity is too small, film surface pollution can aggravate, and flux stability can reduce, and preferred range is 3~5m/
s.Filtration temperature is preferably 20~40 DEG C, and cocnentration factor is preferably material and is concentrated 20~30 times.In an improved embodiment,
The 3A molecular sieve of 1~5wt%, molecular sieve can be added in coal tar when carrying out coal tar purifying using purpose ceramic-film filter
With preferable soaking effect, after entering purpose ceramic-film filter jointly with coal tar, one layer of filter cake can be formed on the surface of film
Layer；Since ceramic membrane is when the material to main oil-containing is filtered, oil is continuous phase, and water can be trapped in outside fenestra, therefore,
Molecular sieve is formed after cake layer, due to the water imbibition that it has, prevents water from forming concentration polarization layer, oil can be kept as company
Continuous phase, improves the rejection to water, simultaneously because molecular sieve has the character of particulate matter, it can be effectively with cross-flow object on surface
Material is moved, and is prevented the fine suspension in coal tar from forming fine and close cake layer, is further prevented fouling membrane, is improved
Film operating flux.Above-mentioned purpose ceramic-film filter can be ceramic micro filter film either ceramic super-filtering film, and microfiltration membranes are average
Aperture can be 0.05 μm~1 μm of film, can be 0.005 μm~0.05 μm for Average Pore Size of UF Membrane of the invention, or
Person is the film that molecular cut off is 10000~500000Da, in a preferred embodiment, the average pore size 50 of ceramic membrane~
200nm。
Based on above method, the present invention also provides solvent purification devices, as shown in Figure 1:
Include:
Washing oil tower 1, for carrying out carrying out washing treatment to coal tar using absorbing liquid；
Primary distillation tower 2 is connected to washing oil tower 1, and the rich solution for obtaining to washing carries out pre-distillation processing, removes heavy constituent, obtains
Coal tar oil vapour；
Condenser 3 is connected to primary distillation tower 2, coal tar coal tar；
First layer tank 4 is connected to condenser 3, for carrying out stratification to coal tar；
Purpose ceramic-film filter 4 is connected to first layer tank 4, for being filtered place to coal tar obtained in first layer tank 2
Reason；
Product collecting tank 6 is connected to the per-meate side of purpose ceramic-film filter 4, for collecting the coal tar after purification obtained.
In one embodiment, further include the second layering tank 7, be connected to the retention side of purpose ceramic-film filter 4, for pair
Trapped fluid carries out layered shaping, and the second layering tank 7 is also attached to the import of purpose ceramic-film filter 4.
In one embodiment, it is super to can be ceramic micro filter film either ceramics for the ceramic membrane in purpose ceramic-film filter 4
Filter membrane, microfiltration membranes are the film that average pore size can be 0.05 μm~1 μm, be can be for Average Pore Size of UF Membrane of the invention
0.005 μm~0.05 μm, or be the film of 10000~500000Da for molecular cut off.
Following embodiment investigates following index
1. the suspended matter of ceramic membrane penetrating fluid: being measured using GB11901-89.
2. material moisture: being measured using karl Fischer moisture titration.
3. rejection=(1-C1/C2) × 100%, wherein C1 is ultrafiltrate concentration, and C2 is original liquid concentration.
Embodiment 1
The liquor carbonis detergens of aqueous about 5wt%, suspended matter 1.4wt% are passed through settling tank, reaction product are layered, water layer discarded,
Organic layer (aqueous about 2wt%) is sent into ceramic membrane and is filtered, and feed liquid temperature is 30 DEG C, and the average pore size of ceramic filtration membrane is difference
It is 5, nm, 20nm, 50 nm, 200nm, 500nm, material is aluminium oxide, and transmembrane pressure 0.1Mpa, 3.5 m/s of crossflow velocity will
Feed liquid stops after being concentrated 25 times, obtains coal tar after purification.
From the aforegoing it can be seen that method provided by the invention can effectively purify coal tar.
Embodiment 2
The liquor carbonis detergens of aqueous about 1.4wt%, suspended matter 0.8wt% are passed through settling tank, reaction product is layered, water layer is abandoned
It goes, organic layer (aqueous about 0.4wt%) is sent into ceramic membrane and is filtered, and feed liquid temperature is 25 DEG C, and the average pore size of ceramic filtration membrane is
50nm, material are aluminium oxide, and transmembrane pressure is 0.05,0.1,0.2,0.3,0.4Mpa, 4 m/s of crossflow velocity, by feed liquid respectively
Stop after 25 times of concentration, obtains coal tar after purification.
From the aforegoing it can be seen that method provided by the invention can effectively purify coal tar.
Embodiment 3
The liquor carbonis detergens of aqueous about 2wt%, suspended matter 1.1wt% are passed through settling tank, reaction product are layered, water layer discarded,
Organic layer (aqueous about 0.5wt%) is sent into ceramic membrane and is filtered, and feed liquid temperature is 35 DEG C, and the average pore size of ceramic filtration membrane is
50nm, material are aluminium oxide, and transmembrane pressure is 0.1Mpa respectively, and crossflow velocity is 0.5,1,2,3,4,5 m/s respectively, by feed liquid
Stop after 30 times of concentration, obtains coal tar after purification.
From the aforegoing it can be seen that method provided by the invention can effectively purify coal tar.
Embodiment 4
The liquor carbonis detergens of aqueous about 5wt%, suspended matter 1.4wt% are passed through settling tank, reaction product are layered, water layer discarded,
3wt%3A molecular sieve feeding ceramic membrane is added in organic layer (aqueous about 2wt%) to be filtered, feed liquid temperature is 30 DEG C, ceramic filtering
The average pore size of film be 5, nm, 20nm, 50 nm, 200nm, 500nm respectively, material is aluminium oxide, transmembrane pressure 0.1Mpa,
3.5 m/s of crossflow velocity stops after feed liquid is concentrated 25 times, obtains coal tar after purification.
From the aforegoing it can be seen that method provided by the invention can effectively purify coal tar.
Claims (11)
1. a kind of solvent purification methods, the solvent is coal tar, which comprises the steps of: is made to coal tar
It is filtered with ceramic membrane, obtains trapped fluid and penetrating fluid, wherein penetrating fluid is by coal tar after purification.
2. solvent purification methods according to claim 1, which is characterized in that the coal tar water content ranges exist
0.001~10wt%, preferred range are 0.01~5wt%, are further preferably 0.05~2wt%.
3. coal tar suspension content range described in is in 0.001~5wt%, and preferred range is 0.01~2wt%, further preferably
It is 0.05~1wt%.
4. solvent purification methods according to claim 1, which is characterized in that coal tar is being filtered it into ceramic membrane
Before, the mode for first passing through stratification removes water.
5. solvent purification methods according to claim 1, which is characterized in that the ceramic membrane can be ceramic micro filter film
Either ceramic super-filtering film, microfiltration membranes are the film that average pore size can be 0.05 μm~1 μm, average for ultrafiltration membrane of the invention
Aperture can be 0.005 μm~0.05 μm, or be the film of 10000~500000Da for molecular cut off.
6. solvent purification methods according to claim 1, which is characterized in that during ceramic membrane filter, transmembrane pressure model
Enclosing is 0.01~1Mpa, preferably 0.05~0.2MPa.
7. solvent purification methods according to claim 1, which is characterized in that during ceramic membrane filter, crossflow velocity is
0.1~10m/s, preferably 3~5m/s.
8. solvent purification methods according to claim 1, which is characterized in that during ceramic membrane filter, filtration temperature is excellent
Choosing is 10~100 DEG C, preferably 20~40 DEG C.
9. a kind of solvent purification device, the solvent are coal tar characterized by comprising
Washing oil tower (1), for carrying out carrying out washing treatment to coal gas using absorbing liquid；
Primary distillation tower (2) is connected to washing oil tower (1), and the rich solution for obtaining to washing carries out pre-distillation processing, removes heavy constituent,
Obtain coal tar oil vapour；
Condenser (3) is connected to primary distillation tower (2), coal tar coal tar；
First layer tank (4) is connected to condenser (3), for carrying out stratification to coal tar；
Purpose ceramic-film filter (4) is connected to first layer tank (4), for carrying out to coal tar obtained in first layer tank (2)
Filtration treatment；
Product collecting tank (6), is connected to the per-meate side of purpose ceramic-film filter (4), for collecting the coal tar after purification obtained.
10. solvent purification device according to claim 9, which is characterized in that further include the second layering tank (7), be connected to
The retention side of purpose ceramic-film filter (4), for carrying out layered shaping to trapped fluid, the second layering tank (7) is also attached to ceramic membrane
The import of filter (4).
11. solvent purification device according to claim 9, which is characterized in that the ceramic membrane in purpose ceramic-film filter (4) can
To be ceramic micro filter film either ceramic super-filtering film, microfiltration membranes are the film that average pore size can be 0.05 μm~1 μm, are used for this hair
Bright Average Pore Size of UF Membrane can be 0.005 μm~0.05 μm, or for molecular cut off be 10000~500000Da
Film.
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| CN201811540673.0A CN109722272A (en) | 2018-12-17 | 2018-12-17 | A kind of solvent purification methods and device |
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| CN201811540673.0A CN109722272A (en) | 2018-12-17 | 2018-12-17 | A kind of solvent purification methods and device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773868A (en) * | 2021-09-29 | 2021-12-10 | 南京工业大学苏州传感与纳米产业技术研究院 | Method for purifying high-viscosity oil and co-producing coke |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5843298A (en) * | 1996-09-27 | 1998-12-01 | Ucar Carbon Technology Corporation | Method of production of solids-free coal tar pitch |
| CN204293996U (en) * | 2014-11-17 | 2015-04-29 | 西北大学 | A kind of coal tar filtration unit |
| CN105778964A (en) * | 2016-04-19 | 2016-07-20 | 郑州四维特种材料有限责任公司 | Coal tar dehydration method and coal tar dehydration device |
| CN105968362A (en) * | 2016-07-25 | 2016-09-28 | 江苏久吾高科技股份有限公司 | Purifying method and device for hydroxyl silicone oil |
-
2018
- 2018-12-17 CN CN201811540673.0A patent/CN109722272A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5843298A (en) * | 1996-09-27 | 1998-12-01 | Ucar Carbon Technology Corporation | Method of production of solids-free coal tar pitch |
| CN204293996U (en) * | 2014-11-17 | 2015-04-29 | 西北大学 | A kind of coal tar filtration unit |
| CN105778964A (en) * | 2016-04-19 | 2016-07-20 | 郑州四维特种材料有限责任公司 | Coal tar dehydration method and coal tar dehydration device |
| CN105968362A (en) * | 2016-07-25 | 2016-09-28 | 江苏久吾高科技股份有限公司 | Purifying method and device for hydroxyl silicone oil |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113773868A (en) * | 2021-09-29 | 2021-12-10 | 南京工业大学苏州传感与纳米产业技术研究院 | Method for purifying high-viscosity oil and co-producing coke |
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Application publication date: 20190507 |