CN108905651A - A kind of preparation method for the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time - Google Patents
A kind of preparation method for the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time Download PDFInfo
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- CN108905651A CN108905651A CN201810603729.6A CN201810603729A CN108905651A CN 108905651 A CN108905651 A CN 108905651A CN 201810603729 A CN201810603729 A CN 201810603729A CN 108905651 A CN108905651 A CN 108905651A
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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
- B01D71/08—Polysaccharides
- B01D71/10—Cellulose; Modified cellulose
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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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
- B01D71/08—Polysaccharides
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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
- B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
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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
- B01D2325/36—Hydrophilic membranes
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Abstract
The invention discloses a kind of preparation methods of functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time, including（1）Prepared polymer Matrix Solution,（2）By the substrate of hydroxyl in conjunction with polymer matrix liquid solution, a step, which is realized, to be accelerated gelation and introduces charged functional groups, obtains the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time.One aspect of the present invention obtains super hydrophilic underwater superoleophobic property by the substrate high-ratio surface energy that polymer matrix liquid solution assigns hydroxyl, and then can realize efficiently separating for grease；On the other hand, charged functional groups are introduced, organic dyestuff is adsorbed by electrostatic interaction, so that organic dyestuff is removed, it is final to realize only by removing dyestuff contaminant while Gravity Separation oil hydrosol.
Description
Technical field
The invention belongs to chemical industry and polymer-function material technical fields, and in particular to oil hydrosol can be achieved at the same time in one kind
The preparation method of the functional membrane of separation and dyestuff removal.
Background technique
In recent years, due to the rapid growth of industrialization development and population, shortage of water resources and water pollution become there is an urgent need to
It solves the problems, such as.Therefore, people are that the toxic organic pollutant aspect handled in water has paid huge effort.It is many feasible
Technology has been applied to purifying water process, however pollutant kind is various, and most of reported method cannot handle more simultaneously
Kind pollutant.In complicated water pollutant, insoluble oil and water-soluble dyestuff are most important pollutants, they are difficult to
Degradation, not only results in environmental pollution and can threaten the health of the mankind.Therefore, the insoluble oil and water-soluble dye in water removal are removed
Material should more be paid close attention to.
Compared to traditional oily water separation technique, novel super infiltrating material has high separating efficiency, highly selective and low
The advantages such as energy consumption.Super infiltrating material is divided into super-hydrophobic super-oleophylic material and super hydrophilic underwater superoleophobic material, super hydrophilic underwater super
The excellent oil-stain-preventing performance of oleophobic material, so that the shortcomings which obviate super hydrophobic materials by oily secondary pollution, is widely used in
Oily waste water treatment.Adhere to hydrophilic polymer, inorganic nanoparticles, Anodic, the methods of chemical etching is for assigning
The super hydrophilic underwater superoleophobic property of material, can efficiently separate oil-water mixture.However these methods need using expensive device or
Toxic reagent.In addition, most of water-oil separating material is not biodegradable, material postpositive disposal becomes a difficult problem.
Under normal circumstances, contaminated separation material is simply discarded or burns, and inevitably results in secondary environmental pollution.Cause
This, constructs complete " green " biodegradable water-oil separating material and is of great significance.
Summary of the invention
It is an object of the invention to be directed to rarely have the UF membrane material that can handle oily waste water and waste water from dyestuff simultaneously in the market
Material, causes multiple pollutant to need step-by-step processing, operates tediously long problem, provide a kind of simple, green, low cost can be simultaneously
Realize the preparation method of the functional membrane of oil hydrosol separation and dyestuff removal.
To achieve the goals above, the present invention uses following technical scheme：
A kind of preparation method for the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time, includes the following steps：
（1）Prepared polymer Matrix Solution（That is hydrogel）
Polymeric matrix is activated first, the present invention is activated using the method for exchange of solvent, and high-temperature activation will cause fiber
Element degradation, and the method for exchange of solvent hardly causes the degradation of cellulose, the activation is successively to soak polymeric matrix
Bubble in water, methanol, dimethyl acetamide 1-12 h, polymeric matrix needed after impregnating in a kind of solvent to polymeric matrix into
Row, which filters, removes the solvent, then polymeric matrix is dipped into another solvent again, the effect of exchange of solvent is weak
Fluidized polymer matrix（Such as cellulose chain）Between strong interaction of hydrogen bond obtain loose conformation, finally by polymeric matrix
It is dissolved in dicyandiamide solution, obtains 0.1 ~ 2 wt% polymer matrix liquid solution（That is hydrogel）；
When the polymeric matrix is cellulose, lignin, hemicellulose, chitosan, chitin, the dicyandiamide solution is
The ratio of DMAc/LiCl solution, the DMAc and LiCl are 91-93g: 7-9g；
When the polymeric matrix is polyvinyl alcohol, the dicyandiamide solution is the isopropanol/water solution that volume ratio is 7/3；
（2）The preparation of functional membrane
The substrate of hydroxyl is immersed in 0.1-4 h in above-mentioned polymer matrix liquid solution, it is soaked sufficiently, is subsequently dipped to dense
Degree is 0.1-4 h in the carboxylic acids crosslinking agent of 2-5wt%, then heats 1-5h at 80-110 DEG C, obtains that grease can be achieved at the same time
The functional membrane of lotion separation and dyestuff removal.
The substrate of the hydroxyl is one of filter paper, PVA film or polylactic acid membrane.
The carboxylic acids crosslinking agent is citric acid solution, seaweed acid solution, acrylic acid solution, amino acid solution or maleic acid
One of polyacids such as anhydride solution.Carboxylic acid reagents play a part of crosslinking agent and introduce charged functional groups.
The solvent of the carboxylic acids crosslinking agent is one of water, ethyl alcohol or octane, and ethyl alcohol etc., which plays, accelerates gelation
Effect.
The substrate of the hydroxyl and the combination of polymer matrix liquid solution can be dipping, spraying, spin coating or brushing.
Step of the present invention（2）A step is realized by simple method coats hydrogel and in water on the substrate of hydroxyl
Charged functional groups are introduced in gel.On the one hand it is obtained by the substrate high-ratio surface energy that the coating of hydrogel assigns hydroxyl super
Hydrophilic underwater superoleophobic property, and then can realize efficiently separating for grease.On the other hand, charged functional groups are introduced, electrostatic phase is passed through
Organic dyestuff is adsorbed in interaction, to remove organic dyestuff.It is final to realize that removal contaminates while only leaning on Gravity Separation oil hydrosol
Expect pollutant.
In addition, the underwater superoleophobic property material such as Metal Substrate, ceramic base, synthetic polymer base is not biodegradable, directly throw
It is put into environment and be easy to cause environmental pollution.The substrate of hydroxyl used in the present invention and polymer for substrate modifications
Matrix Solution（That is hydrogel）It is Biodegradable material, integral material is biodegradable, is easy to post-process, will not be to environment
Generate secondary pollution.
The building of super infiltrating material needs to meet layering surface roughness and high-ratio surface can two conditions.Hydrogel has
Excellent water absorbs and water holding capacity, itself has high-ratio surface energy.Hydrogel can assign material high-ratio surface and give it
Hydrophily.Present invention introduces rich carboxylic acids as crosslinking agent, on the one hand facilitates ester bond cross-linked network and increases hydrogel
Between stability between the substrate and hydrogel of hydroxyl, on the other hand introduce electronegative functional group, assign water-setting
Glue adsorbs the ability of dyestuff, and prepared functional membrane can remove dyestuff while oil-water separation lotion, reach oil hydrosol and
Duplex treatment effect of dyestuff.The invention has the advantages that：
1, the range of choice of Inventive polymers matrix is very wide, and cellulose, lignin, hemicellulose, chitosan, crust can be selected
The biological materials such as element are basis material, and the synthetic materials such as cellulose acetate, polyvinyl alcohol also can be selected as matrix material
Material, can prepare multi-functional water-oil separationg film.Use different polymer for basis material, obtained multifunctional membrane has difference
Physics, chemical property, can be applicable to different field.As the cellulose of one of polymeric matrix, there is from a wealth of sources, cost
It is low, renewable, it is biodegradable, it is environmental-friendly the features such as.
2, the substrate and polymer matrix liquid solution for the hydroxyl that the present invention selects（That is hydrogel）Raw material is mostly natural
Polymer, have it is renewable, it is biodegradable, it is environmental-friendly the features such as.
3, the present invention introduces charged functional groups during accelerating gelation, assigns dyestuff removal ability, simplifies system
Standby step, improves preparation efficiency.
4, it is used in preparation process of the present invention without costly, complicated instrument, no toxic reagent uses, simple, green, easy scale
Metaplasia produces.
5, functional membrane of the invention only lean on gravity can simultaneously oil-water separation mixed liquor（Oil hydrosol）With removal organic dyestuff.
Functional membrane（2.5 cm2）94% or more still can reach to the removal efficiency of dyestuff under the rate of 10 mL/min.System of the present invention
Functional membrane has ultralow oily adhesion strength.The resistance to hypersaline environment of functional membrane of the invention can be used for the improvement of Crude oil from CNOOC leakage.This
The functional membrane of invention removal of heavy metal ions, in terms of have potential application.
It 6, can absorption with adjusting function film to variety classes dyestuff by changing the type of charged functional groups；By changing
Become the concentration of crosslinking agent and immerse the time in crosslinking agent, electrification functional group content can be regulated and controled；By changing polymer matrix
The concentration of liquid solution can regulate and control the thickness of hydrogel layer；It, can be with controlled material by changing the amount and heating duration of crosslinking agent
Crosslinking degree.
Detailed description of the invention
Fig. 1 is the SEM figure of filter paper and functional membrane of the invention, and wherein a, b are that the SEM of filter paper different amplification schemes, c, d
SEM figure under the functional membrane different amplification prepared for embodiment 1；
Fig. 2（a）For the process on 4 μ L water droplets to film, Fig. 2（b）For the contact of 2 μ L 1,2 dichloroethanes and film under water
Journey；
Fig. 3 is the infrared spectrogram of the cellulose aquagel film of pure cellulose hydrogel and introducing citric acid；
Fig. 4 is separation process of the functional membrane of the preparation of embodiment 1 to n-hexane and methylene blue mixed liquor（N-hexane oil red O
It incarnadines, aqueous solution of methylene blue is blue）；
Fig. 5 is the petrographic microscope figure that functional membrane prepared by embodiment 1 separates front and back to the oil hydrosol of addition methylene blue.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
A kind of preparation for the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time（Using filter paper as substrate）：
（1）Prepared polymer Matrix Solution
The cellulose fibres such as cotton, wood pulp, bamboo pulp are activated first, i.e., are successively soaked the cellulose fibres such as cotton, wood pulp, bamboo pulp
Bubble in water, methanol, dimethyl acetamide 1 h, every time impregnate along with filter with remove in cellulose there are immersion solvent,
It is finally 92 in DMAc/LiCl ratio by the cellulose dissolution after activation:In 8 dicyandiamide solution, the polymer of 0.25wt% is obtained
Matrix Solution（That is hydrogel）；
（2）Prepare functional membrane
Filter paper is immersed in 2 h in above-mentioned polymer matrix liquid solution, soaks it sufficiently, being subsequently dipped to concentration is 3wt %'s
2h in the ethanol solution of citric acid, ethyl alcohol plays a part of accelerating gelation in the step, and citric acid plays crosslinking agent and introduces band
The effect of electric functional group heats 4h at 100 DEG C later to get the functional membrane of oil hydrosol separation and dyestuff removal is realized simultaneously
（Cellulose aquagel film）.
Schemed by SEM（Fig. 1）As can be seen that hydrogel layer is adhering closely to surface, and coarse structure is formd, increased
Roughness is added.According to wetability theoretical model, this is beneficial to realize super wetability.By Fig. 2（a）As it can be seen that working as water drop contact
When to film, water droplet infiltrates quickly, and water contact angle shows Superhydrophilic close to 0 ° to film in air；By Fig. 2（b）As it can be seen that oil/
Gu in water/three-phase system, cellulose aquagel film will not be soaked by 1,2 dichloroethanes under water, when oil and film contact even quilt
After extruding, film will not still be soaked.This shows cellulose aquagel film under water not only with superoleophobic property but also with super
Low oily adhesion strength.This may be that cellulose aquagel film has high surface energy and the coefficient result of rough surface.Due to
With Superhydrophilic, when water is contacted with film, film can capture hydrone quickly, form one layer of water layer in its surface roughness,
To form one layer of separation layer between oil droplet and membrane material.Since water and oil pole repel each other on the contrary, therefore cellulose aquagel
Film has ultralow oily adhesion strength, the potential application separated predictive of it in high efficiency oil-water.
Fig. 3 is the infrared spectrogram of the cellulose aquagel film of pure cellulose hydrogel and introducing citric acid.For pure fibre
Hydrogel is tieed up, main signal peak is in 3388 cm-1Place corresponds to O-H stretching vibration（Intermolecular hydrogen bonding）.1645 cm-1Place
It is then the characteristic peak for adsorbing water.For cellulose aquagel film, in 1730 cm-1Nearby there is new feature peak, corresponds on ester group
The stretching vibration peak of C=O illustrates that citric acid has successfully been grafted on cellulose aquagel film.
Fig. 4 is as it can be seen that functional membrane prepared by embodiment 1 can be by the water shape of the n-hexane of oil red O stain and methylene blue staining
At the isolated almost colourless transparent filtrate of mixed liquor, illustrate its high water-oil separating efficiency and dyestuff removal efficiency, lead to
It crosses ultraviolet-visible photometer and measures water-oil separating efficiency and dyestuff removal efficiency 97% or more.In addition, the membrane material is to adding
Having added the oil hydrosol of methylene blue can also efficiently separate.
Fig. 5 is the petrographic microscope that functional membrane prepared by embodiment 1 separates front and back to the oil hydrosol of addition methylene blue.
Left side is the petrographic microscope photo of lotion before separating, and contains a large amount of dispersant liquid drops in lotion, and the figure of filtrate after isolation
As in, drop is not observed in the visual field, very completely, absolutely proving can while functional membrane of the invention efficiently separates lotion
Effectively to remove dyestuff, by ultraviolet-visible spectrophotometer measure water-oil separating efficiency and dyestuff removal efficiency 94% with
On.
Functional membrane prepared by the present invention can simultaneously oil-water separation lotion and removal organic dyestuff the reason of：Since hydrogel has
There is a high surface energy, the attachment of hydrogel layer enables material with high-ratio surface and forms coarse structure that material is had is super
Hydrophilic underwater superoleophobic property, there is opposite wetability to make material that can carry out effective water-oil separating oil and water.In addition, negative
The introducing of electric functional group is so that material can adsorb positively charged organic dyestuff by electrostatic interaction, so that organic dye can be realized
Material effectively removes.
Embodiment 2
A kind of preparation for the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time（Using PVA film as substrate）：
（1）Prepared polymer Matrix Solution
First by cellulose activation, cellulose is successively immersed in water, methanol, 2 h in dimethyl acetamide, is impregnated every time adjoint
Filter to remove the immersion solvent in cellulose, finally by activated cellulose dissolution DMAc/LiCl ratio be 93:7
Dicyandiamide solution in, obtain the polymer matrix liquid solution of 0.1 wt%.
（2）Prepare functional membrane
PVA film is immersed in 0.1-0.5 h in above-mentioned polymer matrix liquid solution, soaks it sufficiently, being subsequently dipped to concentration is 2
0.1-0.5 h in the ethanol solution of the maleic anhydride of wt% heats 5h at 80 DEG C later to get oil hydrosol can be achieved at the same time
The functional membrane of separation and dyestuff removal.
Embodiment 3
A kind of preparation for the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time（Using polylactic acid membrane as substrate）：
（1）Prepared polymer Matrix Solution
Polyvinyl alcohol is successively immersed in water, methanol, 4 h in dimethyl acetamide, then dissolve polyvinyl alcohol in isopropanol/
Water（7/3,v/v）In dicyandiamide solution, the polymer matrix liquid solution of 2wt % is obtained.
（2）Prepare functional membrane
Polylactic acid membrane is immersed in 4 h in above-mentioned polymer matrix liquid solution, soaks it sufficiently.Being subsequently dipped to concentration is 5wt%
4h in the ethanol solution of alginic acid heats 1 h at 110 DEG C later to get multi-functional polyethylene alcohol hydrogel water-oil separationg film.
Embodiment 4
A kind of preparation for the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time（Using filter paper as substrate）：
（1）Prepared polymer Matrix Solution
Chitosan is successively immersed in water, methanol, 3 h in dimethyl acetamide, then dissolves chitosan in DMAc/LiCl ratio
Example is 93:In 7 dicyandiamide solution, the polymer matrix liquid solution of 1 wt% is obtained.
（2）Prepare functional membrane film
Filter paper is immersed in 2 h in above-mentioned polymer matrix liquid solution, soaks it sufficiently.It is subsequently dipped to third that concentration is 4wt%
2h in the octane solution of olefin(e) acid heats 2 h at 100 DEG C later to get multi-functional polyethylene alcohol hydrogel water-oil separationg film.
Claims (5)
1. a kind of preparation method for the functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time, it is characterised in that：It is wrapped
Include following steps：
（1）Prepared polymer Matrix Solution
Polymeric matrix is activated first, i.e., polymeric matrix is successively immersed in water, methanol, 1-2 h in dimethyl acetamide,
Finally polymeric matrix is dissolved in dicyandiamide solution, obtains the polymer matrix liquid solution of 0.1 ~ 2 wt%；
When the polymeric matrix is cellulose, lignin, hemicellulose, chitosan, chitin, the dicyandiamide solution is
The ratio of DMAc/LiCl solution, the DMAc and LiCl are 91-93g: 7-9g；
When the polymeric matrix is polyvinyl alcohol, the dicyandiamide solution is the isopropanol/water solution that volume ratio is 7/3；
（2）The preparation of functional membrane
The substrate of hydroxyl is immersed in 0.1-4h in above-mentioned polymer matrix liquid solution, it is soaked sufficiently, is subsequently dipped to dense
Degree is 0.1-4h in the carboxylic acids crosslinking agent of 2-5wt%, then heats 1-5h at 80-110 DEG C, obtains that grease can be achieved at the same time
The functional membrane of lotion separation and dyestuff removal.
2. a kind of preparation side of functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time according to claim 1
Method, it is characterised in that：The substrate of the hydroxyl is one of filter paper, PVA film or polylactic acid membrane.
3. a kind of preparation side of functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time according to claim 1
Method, it is characterised in that：The carboxylic acids crosslinking agent be citric acid solution, seaweed acid solution, acrylic acid solution, amino acid solution or
One of maleic anhydride solution.
4. a kind of preparation side of functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time according to claim 3
Method, it is characterised in that：The solvent of the carboxylic acids crosslinking agent is one of water, ethyl alcohol or octane.
5. a kind of preparation side of functional membrane that oil hydrosol separation and dyestuff removal can be achieved at the same time according to claim 1
Method, it is characterised in that：The combination that the substrate of hydroxyl is immersed in polymer matrix liquid solution be could alternatively be into spraying, rotation
The combination for applying or brushing.
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| CN110201551A (en) * | 2019-05-08 | 2019-09-06 | 西南石油大学 | For the self-cleaning nona cellulose membrane of water-oil separating, preparation method and applications |
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| CN110201551B (en) * | 2019-05-08 | 2021-09-28 | 西南石油大学 | Self-cleaning nano cellulose membrane for oil-water separation, preparation method and application thereof |
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| CN114405287A (en) * | 2022-01-24 | 2022-04-29 | 中国科学院苏州纳米技术与纳米仿生研究所 | Superstrong oil stain resistance oil-water separation membrane and preparation method and application thereof |
| CN114957779A (en) * | 2022-06-10 | 2022-08-30 | 湖北工业大学 | Preparation method of oil-water separation hydrogel capable of adsorbing dye and resisting salt |
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