CN108043247A - A kind of Kynoar matrix seperation film and preparation method thereof - Google Patents
A kind of Kynoar matrix seperation film and preparation method thereof Download PDFInfo
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- CN108043247A CN108043247A CN201810013970.3A CN201810013970A CN108043247A CN 108043247 A CN108043247 A CN 108043247A CN 201810013970 A CN201810013970 A CN 201810013970A CN 108043247 A CN108043247 A CN 108043247A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/38—Hydrophobic membranes
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Abstract
The present invention relates to a kind of Kynoar matrix seperation films and preparation method thereof, are related to technology field of membrane materials.Existing polymer compound film is solved since plasticizer easily volatilizees with membrane solvent, reduces the technical issues of composite membrane is to the separating effect of metal or organic matter.Kynoar matrix seperation film provided by the invention includes polyvinylidene fluoride film and the extractant being dispersed in polyvinylidene fluoride film.The preparation method of Kynoar matrix seperation film provided by the invention, this method by extractant by dissolving, blending, knifing, inversion of phases and etc. extractant is made to be dispersed in polyvinylidene fluoride film, and non-infiltration is in duct, it is ensured that the stability of the Kynoar matrix seperation film in later stage application process.The Kynoar matrix seperation film of the present invention is for when separating Heavy rare earth, with good separating effect, and contamination resistance to be strong, there is preferable circulating repetition usability；And its preparation method is simple.
Description
Technical field
The present invention relates to technology field of membrane materials, and in particular to a kind of Kynoar matrix seperation film and its preparation side
Method.
Background technology
At present, heavy rare earth separating technology mainly uses solvent extraction, although the separation method has easy to operate, process
The advantages that stablizing, but because it needs a large amount of extractants and rare earth to carry out indent in separation process, cause more waste, and divide
From substantial amounts of soda acid and organic solvent can be consumed in the process.In practical systems, the concentration of heavy rare earth feed liquid is usually relatively low, uses
The extraction series that Solvent Extraction Separation needs is more, and equipment is taken up an area greatly, and energy consumption is badly in need of developing a kind of new separation than relatively low
Method solves the problems, such as present in current heavy rare earth separation and concentration.
Membrane separating process will extract and stripping process is highly integrated, has extractant utilization rate high, and consumption of organic solvent is few,
There is no the problem of two-phase laminated flow, process is simple, low energy consumption, it is pollution-free the advantages that.These advantages cause membrane separation technique conduct
The effective supplement and replacement of conventional solvent extraction, continue to develop always in recent years.
The prior art has been disclosed for separation of a variety of polymer compound films for metal or organic matter, such as that three acetic acid are fine
Dimension element or polyvinyl chloride are dissolved in solvent, are then mixed with extractant and plasticizer, are obtained after solvent is volatilized containing extraction
Take the composite membrane of agent and plasticizer.Although these composite membranes have preferable separating property, because in membrane matrix and extractant
On the basis of be with the addition of plasticizer, make complicatedization of seperation film, and the plasticizer volatility of molecule type is higher, is preparing
Into easily volatilizing with membrane solvent during composite membrane, separating effect of the composite membrane to metal or organic matter is reduced.
The content of the invention
The invention solves in the prior art the technical issues of, a kind of Kynoar matrix seperation film and its preparation are provided
Method, Kynoar matrix seperation film of the invention resist for when separating Heavy rare earth, having good separating effect
Pollution capacity is strong, there is preferable circulating repetition usability；And its preparation method is simple.
In order to solve the above-mentioned technical problem, technical scheme is specific as follows：
A kind of Kynoar matrix seperation film, including：
Polyvinylidene fluoride film；
And it is dispersed in the extractant in the polyvinylidene fluoride film；
The extractant is phosphatic type extractant.
In the above-mentioned technical solutions, the mass ratio of the polyvinylidene fluoride film and extractant is 0.5：0.125-0.75.
In the above-mentioned technical solutions, the mass ratio of the polyvinylidene fluoride film and extractant is 0.5：0.34.
In the above-mentioned technical solutions, the extractant is two (2- ethylhexyls) phosphinic acids, 2- ethylhexyl phosphoric acid 2- second
Base hexyl ester or di-(2-ethylhexyl)phosphoric acid ester.
In the above-mentioned technical solutions, the pore structure of the Kynoar matrix seperation film is asymmetry duct structure.
A kind of preparation method of Kynoar matrix seperation film, comprises the following steps：
(1) Kynoar and membrane solvent are mixed be placed on 65 DEG C of stirrings 4 it is small when, then be cooled to 50 DEG C of stirrings 1 it is small when,
Obtain the first mixed liquor；
(2) extractant is added in first mixed liquor, obtains the second mixed liquor；By second mixed liquor at 50 DEG C
Stir 12 it is small when after, room temperature supersound process remove bubble removing, obtain casting solution；
(3) casting solution is toppled over into striking on a glass for primary membrane, is placed 1 minute in air；
(4) glass plate with primary membrane is put into the solvent removed in deionized water in primary membrane, is gathered after dry
Vinylidene matrix seperation film.
In the above-mentioned technical solutions, the mass ratio of the Kynoar and extractant is 0.5：0.125-0.75.
In the above-mentioned technical solutions, the mass ratio of the Kynoar and extractant is 0.5：0.34.
In the above-mentioned technical solutions, the extractant is two (2- ethylhexyls) phosphinic acids, 2- ethylhexyl phosphoric acid 2- second
Base hexyl ester or di-(2-ethylhexyl)phosphoric acid ester.
In the above-mentioned technical solutions, the pore structure of the Kynoar matrix seperation film is asymmetry duct structure.
The beneficial effects of the invention are as follows：
Kynoar matrix seperation film provided by the invention includes polyvinylidene fluoride film and is dispersed in polyvinylidene fluoride film
In extractant；It is formed simply, without additionally adding plasticizer or pore-foaming agent, is reduced film cost, is simplified film stream
Journey.Wherein, polyvinylidene fluoride film is host material, has high hydrophobicity, high chemical stability, high thermal stability and good machine
Tool performance；The extractant uses phosphatic type extractant, is supported in polyvinylidene fluoride film, by extraction by metal ion from original
Feed liquid side separates, while extractant also plays similar plasticizer while the carrier as extract and separate metallic element
Effect, thus it is possible to vary the pore passage structure of polyvinylidene fluoride film improves its transmission performance to metal ion, and kind of extractants business
Product chemical conversion is ripe, can directly buy.
Kynoar matrix seperation film provided by the invention can separate metal ion, and with good
Separating effect and higher separative efficiency, and can be used in stronger soda acid or the special isolating environment of strong oxidizing property,
Environmental suitability is strong.The present invention is by the way that extractant is dispersed in polyvinylidene fluoride film simultaneously, and non-infiltration is in duct, therefore
Extractant not easily runs off, and does not interfere with the stability and service life of film.
The preparation method of Kynoar matrix seperation film provided by the invention, this method, which passes through extractant, to be dissolved, altogether
Mixed, knifing, inversion of phases and etc. extractant is made to be dispersed in polyvinylidene fluoride film, and non-infiltration is in duct, it is ensured that this is poly-
Stability of the vinylidene matrix seperation film in later stage application process.
Description of the drawings
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Fig. 1 is the stereoscan photograph of Kynoar matrix seperation film prepared by the embodiment of the present invention 1.
Fig. 2 is the Kynoar matrix seperation film of the preparation of the embodiment of the present invention 1 to Lu3+Separated extraction yield variation is bent
Line.
Fig. 3 is the Kynoar matrix seperation film of the preparation of the embodiment of the present invention 1 to Lu3+Separated back extraction ratio variation is bent
Line.
Fig. 4 is the Kynoar matrix seperation film of the preparation of the embodiment of the present invention 1,4 and 5 to Lu3+Separated extraction yield becomes
Change curve.
Fig. 5 is the Kynoar matrix seperation film of the preparation of the embodiment of the present invention 1,4 and 5 to Lu3+Separated back extraction ratio becomes
Change curve.
Fig. 6 is the Kynoar matrix seperation film of the preparation of the embodiment of the present invention 1 to Lu3+Separated material liquid and strip liquor
Middle Lu3+Concentration and time changing curve.
Fig. 7 is the Kynoar matrix seperation film of the prior art containing ionic liquid to rare earth element Lu3+(open circles
Point) and Yb3+(black circle) carries out Lu in separated material liquid and strip liquor3+And Yb3+Concentration and time changing curve.
Fig. 8 is the Kynoar matrix seperation film that provides of the embodiment of the present invention 1 to Lu3+The amount of flux of separative efficiency variation
J and cycle-index relational graph.
Fig. 9 is ln (the c/c when extractant of different quality is added in embodiment 1,2 and 3i) change over time relational graph.
Specific embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
Kynoar matrix seperation film provided by the invention, and applied in heavy rare earth separation process.This is poly-
Vinylidene matrix seperation film is using phosphatic type extractant as addition phase carrier, using Kynoar as matrix, utilizes non-solvent
The Kynoar matrix seperation film containing extractant that phase separation method is caused to prepare.The present invention is by by Kynoar, film
Solvent and extraction agent carrier make the extractant support dispersion in polyvinylidene fluoride film by dissolving, blending, knifing, inversion of phases etc.
Inside, extractant not easily runs off, and does not interfere with the stability and service life of the Kynoar matrix seperation film.With it is existing
Technology is compared, and Kynoar matrix seperation film preparation process provided by the invention is simple, and in terms of heavy rare earth separation and concentration
There is good result.Compared with conventional solvent extraction, membrane separating process is highly integrated, it is possible to reduce the occupation of land of equipment reduces acid
The consumption of alkali and organic solvent is a kind of new method for separating and concentrating for having large development potentiality.
A kind of Kynoar matrix seperation film provided by the invention, including：Polyvinylidene fluoride film；And it is dispersed in described poly-
Extractant in vinylidene fluoride film；The extractant is phosphatic type extractant.The quality of the polyvinylidene fluoride film and extractant
Than being preferably 0.5：0.125-0.75, the most preferably mass ratio of the polyvinylidene fluoride film and extractant are 0.5：0.34.Institute
It is preferably two (2- ethylhexyls) phosphinic acids (P227), 2- ethylhexyl phosphoric acid 2- ethylhexyls (P507) or two to state extractant
(2- ethylhexyls) phosphate (P204) is most preferably two (2- ethylhexyls) phosphinic acids (P227).The polyvinylidene fluoride
The pore structure of matter seperation film is asymmetry duct structure, and separated transmission direction is the lateral film macropore side transmission of film aperture.
The present invention also provides a kind of preparation methods of Kynoar matrix seperation film, comprise the following steps：
(1) Kynoar and membrane solvent are mixed be placed on 65 DEG C of stirrings 4 it is small when, then be cooled to 50 DEG C of stirrings 1 it is small when,
Obtain the first mixed liquor；
(2) extractant is added in first mixed liquor, obtains the second mixed liquor；By second mixed liquor at 50 DEG C
Stir 12 it is small when after, room temperature supersound process remove bubble removing, obtain casting solution；
(3) casting solution is toppled over into striking on a glass for primary membrane, is placed 1 minute in air；
(4) glass plate with primary membrane is put into the solvent removed in deionized water in primary membrane, is gathered after dry
Vinylidene matrix seperation film；Wherein, the mass ratio of preferably described Kynoar and extractant is 0.5：0.125-0.75, most
It is preferred that the mass ratio of the Kynoar and extractant is 0.5：0.34.It is preferred that the extractant is secondary for two (2- ethylhexyls)
Phosphonic acids (P227), 2- ethylhexyl phosphoric acid 2- ethylhexyls (P507) or di-(2-ethylhexyl)phosphoric acid ester (P204), it is optimal
Elect two (2- ethylhexyls) phosphinic acids (P227) as.
Embodiment 1
The Kynoar powder of the Solef6010 of 0.50g, 5.0mL n,N-dimethylacetamide are mixed, 65 DEG C are stirred
Mix 4 it is small when, be then cooled to 50 DEG C stirring 1 it is small when, then by 0.34g bis- (2- ethylhexyls) phosphinic acids add in mixed liquor in, 50
DEG C stirring 12 it is small when, then by casting solution room temperature be ultrasonically treated 10 minutes, obtain casting solution.Under room temperature by casting solution striking
On smooth glass plate, after being placed 1 minute in air, the glass plate with casting solution is put into 25 DEG C of deionized water and is solidified
In liquid, film forming nature floats after making casting solution generation inversion of phases, obtains primary membrane.The primary membrane is put into deionized water and is soaked
3h removal n,N-dimethylacetamide is steeped, dries to obtain two (the 2- ethylhexyls) containing extractant quality is 0.34g after picking up
The Kynoar matrix seperation film of phosphinic acids.
By the Kynoar matrix seperation film as under scanning electron microscope, obtaining electromicroscopic photograph as shown in Figure 1, Fig. 1
For the stereoscan photograph for the Kynoar matrix seperation film that the embodiment of the present invention 1 provides, it is known that the Kynoar of preparation
The pore structure of matrix seperation film is asymmetry duct structure.
Embodiment 2
Difference with embodiment 1 be the quality of addition two (2- ethylhexyls) phosphinic acids for 0.125g, other same embodiments
1, obtain the Kynoar matrix seperation film containing two (2- ethylhexyls) phosphinic acids that extractant quality is 0.125g.
Embodiment 3
Difference with embodiment 1 be the quality of addition two (2- ethylhexyls) phosphinic acids for 0.75g, the other the same as in Example 1,
Obtain the Kynoar matrix seperation film containing two (2- ethylhexyls) phosphinic acids that extractant quality is 0.75g.
Fig. 9 is ln (the c/c when extractant of different quality is added in embodiment 1,2 and 3i) (by Lu during certain time3+Concentration with
The ratio of its initial concentration is taken the logarithm) relational graph is changed over time, figure cathetus slope is bigger to illustrate that laser propagation effect is better, because of extraction
Agent addition quality is taken to add quality 0.34g laser propagation effects compared with extractant for 0.75g and promotes very little, so the addition matter by extractant
It is 0.34g as optimal selection to measure, as the adding proportion in subsequent experimental.
Embodiment 4
Difference with embodiment 1 is that extractant replaces with 2- ethylhexyl phosphoric acid 2- ethylhexyls, and quality is
0.34g, the other the same as in Example 1 are obtained containing the poly- of the 2- ethylhexyl phosphoric acid 2- ethylhexyls that extractant quality is 0.34g
Vinylidene matrix seperation film.
Embodiment 5
Difference with embodiment 1 is that extractant replaces with di-(2-ethylhexyl)phosphoric acid ester, quality 0.34g, other
With embodiment 1, the Kynoar matrix separation containing the di-(2-ethylhexyl)phosphoric acid ester that extractant quality is 0.34g is obtained
Film.
Embodiment 6
Kynoar matrix seperation film prepared by embodiment 1 is fixed in membrane separation device, effective contact surface of film
Product is 7.07cm2；The HCl strip liquors of various concentration are added in into back extraction pond, the concentration of HCl is respectively 1.0mol/L, 2.5mol/
L and 4.0mol/L；The Lu of the 1mmol/L of 100mL is added in into feed liquid pond3+Material liquid.Agitating device is opened, with 500 revs/min
Speed stirring, make Lu3+It is migrated, respectively obtains film to Lu3+Separated extraction yield and back extraction ratio change curve, the result is shown in
Fig. 2 and Fig. 3.
As it can be seen that Kynoar matrix seperation film prepared by the embodiment of the present invention 1 can be used for separating Lu3+, and can compared with
It is used under strong acid condition, there is preferable environmental suitability, application range is wider.
Embodiment 7
Kynoar matrix seperation film prepared by embodiment 1, Kynoar matrix seperation film prepared by embodiment 4
With Kynoar matrix seperation film prepared by embodiment 5 Lu is carried out according to the method and steps of embodiment 63+Separating experiment,
It is preferably 2.5mol/L to be stripped side HCl concentration, respectively obtains film to Lu3+Separated extraction yield and back extraction ratio change curve, as a result
See Fig. 4 and Fig. 5.
As it can be seen that Kynoar matrix seperation film prepared by the embodiment of the present invention 1,4 may be incorporated for separation Lu3+.Anti-
Under conditions of extraction side HCl concentration is 2.5mol/L, because the back extraction acidity is relatively low for di-(2-ethylhexyl)phosphoric acid ester, because
Kynoar matrix seperation film prepared by this embodiment 5 is with this condition only to Lu3+There are extraction, no back extraction effect.
Embodiment 8
Kynoar matrix seperation film prepared by embodiment 1 carries out Lu according to the method and steps of embodiment 63+'s
Separating experiment, back extraction side HCl concentration is preferably 2.5mol/L, in triplicate, the result is shown in Fig. 6, and by result and existing document report
Road (Asymmetric Membrane Containing Ionic Liquid [A336] [P507] for the
Preconcentration and Separation ofHeavy Rare Earth Lutetium.《ACS Sustainable
Chemistry&Engineering》2644-2650 pages of 5 phases of volume 4 in 2016) experimental data (Fig. 7) be compared.
As it can be seen that Kynoar matrix seperation film prepared by the embodiment of the present invention 1 is in separation Lu3+Favorable reproducibility in the process,
Process is stablized.Simultaneously compared with the prior art, have a distinct increment, have in maximum separation efficiency very big in separated transmission speed
It is promoted.
Embodiment 9
Kynoar matrix seperation film prepared by embodiment 1 carries out Lu according to the method and steps of embodiment 63+'s
Separating experiment.After experiment carries out 6h, feed liquid and strip liquor are discarded, and seperation film 1h is impregnated with 2.5mol/L HCl, it then will be new
Fresh feed liquid and strip liquor add in, and repeat the above steps and carry out 6 circulation experiments, obtain film to Lu3+Separative efficiency variation is led to
Magnitude J, the result is shown in Fig. 8.
As it can be seen that Kynoar matrix seperation film prepared by the embodiment of the present invention 1 is in separation Lu3+Have in the process good
Stability and recycling can be applied in long-term separation process.
Obviously, the above embodiments are merely examples for clarifying the description, and is not intended to limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation thus extended out or
Among changing still in the protection domain of the invention.
Claims (10)
1. a kind of Kynoar matrix seperation film, which is characterized in that including：
Polyvinylidene fluoride film；
And it is dispersed in the extractant in the polyvinylidene fluoride film；
The extractant is phosphatic type extractant.
2. Kynoar matrix seperation film according to claim 1, which is characterized in that the polyvinylidene fluoride film and extraction
The mass ratio for taking agent is 0.5：0.125-0.75.
3. Kynoar matrix seperation film according to claim 1, which is characterized in that the polyvinylidene fluoride film and extraction
The mass ratio for taking agent is 0.5：0.34.
4. the Kynoar matrix seperation film according to claim 1-3 any one, which is characterized in that the extractant
For two (2- ethylhexyls) phosphinic acids, 2- ethylhexyl phosphoric acid 2- ethylhexyls or di-(2-ethylhexyl)phosphoric acid ester.
5. Kynoar matrix seperation film according to claim 4, which is characterized in that the Kynoar matrix point
Pore structure from film is asymmetry duct structure.
6. a kind of preparation method of Kynoar matrix seperation film described in claim 1, which is characterized in that including following step
Suddenly：
(1) Kynoar and membrane solvent are mixed be placed on 65 DEG C of stirrings 4 it is small when, then be cooled to 50 DEG C of stirrings 1 it is small when, obtain
First mixed liquor；
(2) extractant is added in first mixed liquor, obtains the second mixed liquor；By second mixed liquor in 50 DEG C of stirrings
12 it is small when after, room temperature supersound process remove bubble removing, obtain casting solution；
(3) casting solution is toppled over into striking on a glass for primary membrane, is placed 1 minute in air；
(4) glass plate with primary membrane is put into the solvent removed in deionized water in primary membrane, obtains gathering inclined fluorine after dry
Ethylene matrix seperation film.
7. the preparation method of Kynoar matrix seperation film according to claim 6, which is characterized in that described to gather inclined fluorine
The mass ratio of ethylene and extractant is 0.5：0.125-0.75.
8. the preparation method of Kynoar matrix seperation film according to claim 6, which is characterized in that described to gather inclined fluorine
The mass ratio of ethylene and extractant is 0.5：0.34.
9. the preparation method of the Kynoar matrix seperation film according to claim 6-8 any one, which is characterized in that
The extractant is two (2- ethylhexyls) phosphinic acids, 2- ethylhexyl phosphoric acid 2- ethylhexyls or two (2- ethylhexyls) phosphorus
Acid esters.
10. the preparation method of Kynoar matrix seperation film according to claim 9, which is characterized in that described poly- inclined
The pore structure of vinyl fluoride matrix seperation film is asymmetry duct structure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111653785A (en) * | 2020-06-28 | 2020-09-11 | 福建师范大学 | Preparation method of modified polyvinylidene fluoride conductive binder |
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| CN111653785B (en) * | 2020-06-28 | 2022-09-30 | 福建师范大学 | Preparation method of modified polyvinylidene fluoride conductive adhesive |
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Application publication date: 20180518 |