CN109012220A - A kind of preparation of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane - Google Patents

A kind of preparation of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane Download PDF

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Publication number
CN109012220A
CN109012220A CN201811196767.0A CN201811196767A CN109012220A CN 109012220 A CN109012220 A CN 109012220A CN 201811196767 A CN201811196767 A CN 201811196767A CN 109012220 A CN109012220 A CN 109012220A
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China
Prior art keywords
mxene
film
preparation
infiltrating
sodium alginate
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CN201811196767.0A
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Chinese (zh)
Inventor
李赛赛
耿欣
王璐莹
代娟
严庆
雷建都
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Beijing Forestry University
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Beijing Forestry University
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Priority to CN201811196767.0A priority Critical patent/CN109012220A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002Organic membrane manufacture
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/74Natural macromolecular material or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/78Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation

Abstract

The invention discloses a kind of novel permeations for separating alcohol water to vaporize film, comprising the following steps: 1) pre-synthesis a kind of New Two Dimensional material (MXene);2) synthesized MXene is added in sodium alginate preparation liquid, is uniformly dispersed, stood, deaeration;3) knifing is carried out on ultrafiltration counterdie, obtains wet film, is dried at room temperature for;4) dry film base is put into calcium chloride solution and is crosslinked, thoroughly dried at room temperature after crosslinking to get infiltrating and vaporizing membrane is arrived.It is an advantage of the invention that using MXene more preferably than graphene interlayer structure, good electric conductivity and hydrophily are added it in preparation liquid, to improve the separating property of film.

Description

A kind of preparation of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane
Technical field:
The present invention relates to a kind of preparations of sodium alginate infiltrating and vaporizing membrane for separating alcohol water, mainly for New Two Dimensional material The preparation method of the infiltrating and vaporizing membrane obtained that ethyl alcohol is concentrated is blended with sodium alginate by MXene.
Background technique:
New Two Dimensional material MXene is using the weak binding power in MAX phase between A lamella and MX lamella, and it is suitable to select Etching agent (such as HF, LiF+HCl, NH4HF2Deng) the A atomic layer in MAX phase is degraded and a kind of New Type of Carbon/nitride two for preparing Material is tieed up, good electric conductivity and compatibility are had both.Its general formula is represented by Mn+1XnTx, wherein TxIndicate that MXene is carved by chemistry The functional group (- OH ,-F ,=O etc.) for being attached to its surface for losing presoma MAX phase and generating.Using sonic oscillation or ball milling etc. Means peel off the MXene of multilayer, and the single layer MXene pattern of acquisition is similar with graphene.But it is monatomic compared to graphene Structure contains the better M of stability and X diatomic or polyatom in MX structure.In addition, being bonded between C and C atom in graphene It is single, and between M-X it is covalent bond-ionic bond-metallic bond mixing valence link, this also implies that such M-X two dimension substance will Possess and more enriches adjustable performance than graphene.
Prepare the hot spot that transparent conductive film is MXene recent research.MXene transparent conductive film can be used for making transparent Electrode, ultrathin display, flexible screen, solar battery and electrode tube, and preparation supercapacitor and metal ion battery The ideal material of electrode.
Utilize HF or NH4HF2Etch the long growth Ti of extension3AlC2Then film passes through NH3Or NH4 +Intercalation can get The Ti of 15nm thickness3C2TxFilm, with 85% light transmittance.And utilize the Ti of spray coating method preparation3C2TxFilm has soft, saturating Bright, conductive feature, highest light transmittance is up to 90%, and square resistance rate is between 0.5~8k Ω Sq-1, it is better than same thickness oxygen The performance of graphite film.Dillon etc. has found Ti3C2TxFilm wavelength be greater than 1130nm start to show free electron etc. from The phenomenon that daughter is vibrated, therefore can be used as plasma material for fields such as optical communication, bio-imaging, chemical sensitisations.
In addition to this layering MXene can be prepared into the adjustable film of thickness, and have soft, hydrophilic, conductive and excellent Mechanical property.Ren etc. has found Ti3C2TxThe performance that there is the film of preparation selectivity to penetrate water intermediate ion has and shows half-and-half Diameter is less thanThe ion that valence state is+2~+4 has preferable centrifugation, and filter effect is better than graphene film.This is The application of MXene opens a new direction --- water body treatment and purification.
Advantage based on MXene or more is applied to the film for preparing alcohol-water separation, can use its hydrophily and superior Molecular structure have reached improve membrane separating property purpose.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of New Two Dimensional material/sodium alginate infiltrating and vaporizing membranes, by it Applied to alcohol-water separation, have the characteristics that separating property is high using infiltrating and vaporizing membrane prepared by this kind of method.The following steps are included:
1) preparation of MXene: weighing suitable LiF and be added in hydrochloric acid (9mol/L), and stirring obtains mixed liquor,
Again by TiAlC2It is slowly added in mixed liquor, is stirred at room temperature for 24 hours, the precipitating after reaction is cleaned repeatedly,
Until neutral, vacuum drying at room temperature, as MXene;
2) configuration of preparation liquid: sodium alginate constant temperature soluble in water is stirred to the seaweed for being completely dissolved configuration 0.03g/ml Then the MXene of certain mass is added in sour sodium preparation liquid, by mixed liquor is agitated and ultrasonic disperse uniformly after standing and defoaming obtain Preparation liquid;
3) preparation liquid stood is equably poured on dry, clean, smooth polyacrylonitrile ultrafiltration counterdie,
Certain thickness wet film is spread to hymenotome is scraped, is dried at room temperature for, then dried film is placed into 0.5mol/L It is crosslinked 10 minutes in calcium chloride solution, washes film water after crosslinking, thoroughly dried at room temperature to get infiltrating and vaporizing membrane is arrived.
Preparation method as a kind of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane of the invention further changes Into: the additive amount of MXene is 0.0125mg/mL, 0.025mg/mL, 0.0375mg/mL, 0.05mg/mL.
The method of the present invention simple possible, easily operated, prepared infiltrating and vaporizing membrane is a kind of composite membrane, has perfection Infiltrating and vaporizing membrane structure, have preferable selectivity to alcohol type organic;And utilize infiltrating and vaporizing membrane of the invention from hair Ethyl alcohol is concentrated in zymotic fluid, has the advantages that efficient, low energy consumption, the call of national energy conservation and emission reduction can be sufficiently responded to.
Specific implementation method:
Comparative example:
Sodium alginate infiltrating and vaporizing membrane:
1) configuration of preparation liquid is stirred 1.2g sodium alginate is molten with constant temperature in 40ml water to being completely dissolved, gained film Liquid is stood overnight to remove bubble;
2) then the preparation liquid stood is equably poured on dry, clean, smooth polyacrylonitrile ultrafiltration counterdie, It carries out scraping film process with hymenotome is scraped, obtains certain thickness wet film, be completely dried at room temperature;
3) then dried film is placed into the calcium chloride solution of 0.5mol/L and carries out crosslinking 10 minutes, it will after crosslinking Film water is washed, and is completely dried at room temperature to get infiltrating and vaporizing membrane is arrived.
Above-mentioned infiltrating and vaporizing membrane is used for separating alcohol-water system, concrete operations are as follows:
Manufactured infiltrating and vaporizing membrane is fitted into the osmotic cell of infiltration evaporation device, 90% ethyl alcohol is added in feed liquid bottle Aqueous solution, heating make feed liquid temperature maintain 40 DEG C, and film downstream vacuum degree is controlled in 180Pa.Receiving flask is put into cold in liquid nitrogen Freeze, open vacuum pump, alcohol vapour is condensed collections, by quality in weighing receiving flask and with gas chromatographic analysis permeate The concentration of middle ethyl alcohol, so that the permeation flux and separation factor of the infiltrating and vaporizing membrane separating alcohol-water system are obtained, as a result such as table 1。
Embodiment 1-4:
A kind of preparation method of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane, successively follows the steps below:
1) preparation of MXene: TiAlC is weighed respectively2With each 2g of LiF, weighed LiF is first added to the hydrochloric acid of 40ml In (9mol/L), stirring obtains mixed liquor, then by TiAlC2It is slowly added in mixed liquor, is stirred at room temperature for 24 hours, it will be heavy after reaction Shallow lake is cleaned repeatedly, until neutral, vacuum drying at room temperature, as MXene;
2) configuration of preparation liquid: sodium alginate constant temperature soluble in water is stirred to the seaweed for being completely dissolved configuration 0.03g/ml Then the MXene of certain mass is added in sour sodium preparation liquid, by mixed liquor is agitated and ultrasonic disperse uniformly after standing and defoaming obtain Preparation liquid;
Subsequent process steps are consistent with comparative example.Above-mentioned infiltrating and vaporizing membrane is used for separating alcohol-water system, to obtain The permeation flux and separation factor of the infiltrating and vaporizing membrane separating alcohol-water system, as a result such as table 1.
The permeation flux and separation factor of 1 SA film of table and MXene/SA composite membrane separating alcohol-water system

Claims (2)

1. a kind of preparation method of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane, it is characterized in that the following steps are included:
1) preparation of MXene: weighing suitable LiF and be added in hydrochloric acid (9mol/L), and stirring obtains mixed liquor, then TiAlC2 is delayed It is slow to be added in mixed liquor, it is stirred at room temperature for 24 hours, the precipitating after reaction is cleaned repeatedly, until neutral, vacuum drying at room temperature, as MXene;
2) configuration of preparation liquid: sodium alginate constant temperature soluble in water is stirred to the sodium alginate for being completely dissolved configuration 0.03g/ml Then the MXene of certain mass is added in preparation liquid, by mixed liquor is agitated and ultrasonic disperse uniformly after standing and defoaming be film-made Liquid;
3) preparation liquid stood is equably poured on dry, clean, smooth polyacrylonitrile ultrafiltration counterdie, with scraping hymenotome Certain thickness wet film is spread to, is dried at room temperature for, then dried film is placed into 0.5mol/L calcium chloride solution and is crosslinked 10 minutes, film water is washed after crosslinking, is thoroughly dried at room temperature to get infiltrating and vaporizing membrane is arrived.
2. a kind of preparation method of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane according to claim 1, feature Be: the additive amount of the MXene is 0.0125mg/mL, 0.025mg/mL, 0.0375mg/mL, 0.05mg/mL.
CN201811196767.0A 2018-10-15 2018-10-15 A kind of preparation of New Two Dimensional material/sodium alginate infiltrating and vaporizing membrane Pending CN109012220A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109802163A (en) * 2019-03-19 2019-05-24 中国科学院理化技术研究所 A kind of application of MXene film in electrodialysis reversal power generation
CN110252159A (en) * 2019-06-25 2019-09-20 杭州电子科技大学 A kind of composite hybridization film and its preparation method and application
CN110449032A (en) * 2019-07-08 2019-11-15 西安建筑科技大学 A kind of swelling resistance two dimension SA-MXene stratiform nanofiltration membrane, preparation and application
CN110808266A (en) * 2019-10-15 2020-02-18 深圳市华星光电技术有限公司 Display substrate with transparent electrode and preparation method thereof
CN110868842A (en) * 2019-11-29 2020-03-06 北京林业大学 Mechanically-enhanced ultrathin semitransparent electromagnetic shielding film and preparation method thereof
CN111266019A (en) * 2020-01-23 2020-06-12 天津大学 Preparation method and application of vertically-oriented magnetic nanosheet/sodium alginate composite membrane
CN111422873A (en) * 2020-03-23 2020-07-17 北京化工大学 MXene/sodium alginate derived carbon three-dimensional aerogel and preparation method and application thereof
CN111718518A (en) * 2020-07-30 2020-09-29 北京航空航天大学 Preparation method of high-strength high-conductivity titanium carbide composite film
CN112501546A (en) * 2020-11-30 2021-03-16 江苏瑞悦轨道装备有限公司 Non-ferrous metal surface strengthening treatment method
CN112644016A (en) * 2020-12-11 2021-04-13 东北电力大学 Construction method of natural amphiprotic biomass gel artificial muscle device
CN112724427A (en) * 2021-01-29 2021-04-30 西北师范大学 Preparation of corn starch/sodium alginate/MXene composite hydrogel and application of composite hydrogel in seawater desalination

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CN104801208A (en) * 2015-04-07 2015-07-29 天津大学 Sodium alginate-flaky ZIF-8 hybrid composite membrane, and preparation and application thereof
CN105597567A (en) * 2016-03-18 2016-05-25 郑州大学 Organic and inorganic hybridized solvent-resistant nanofiltration composite membrane and preparation method thereof
CN107983161A (en) * 2017-11-23 2018-05-04 华南理工大学 A kind of application of two dimension MXene films in water and separation of ethanol

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CN102743981A (en) * 2012-07-18 2012-10-24 盐城工学院 Preparation and application of sodium alginate pervaporation hybrid membrane
CN103170250A (en) * 2013-04-02 2013-06-26 天津工业大学 Hybridization hydrogel flat membrane for water filtration and preparation method thereof
CN104772043A (en) * 2015-04-07 2015-07-15 天津大学 Sodium alginate-graphite phase carbon nitride nano-sheet hybridized composite membrane as well as preparation and application of composite membrane
CN104801208A (en) * 2015-04-07 2015-07-29 天津大学 Sodium alginate-flaky ZIF-8 hybrid composite membrane, and preparation and application thereof
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Publication number Priority date Publication date Assignee Title
CN109802163A (en) * 2019-03-19 2019-05-24 中国科学院理化技术研究所 A kind of application of MXene film in electrodialysis reversal power generation
CN110252159A (en) * 2019-06-25 2019-09-20 杭州电子科技大学 A kind of composite hybridization film and its preparation method and application
CN110449032A (en) * 2019-07-08 2019-11-15 西安建筑科技大学 A kind of swelling resistance two dimension SA-MXene stratiform nanofiltration membrane, preparation and application
CN110449032B (en) * 2019-07-08 2021-10-08 西安建筑科技大学 Swelling-resistant two-dimensional SA-MXene layered nanofiltration membrane, and preparation and application thereof
CN110808266A (en) * 2019-10-15 2020-02-18 深圳市华星光电技术有限公司 Display substrate with transparent electrode and preparation method thereof
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CN110868842B (en) * 2019-11-29 2021-03-05 北京林业大学 Mechanically-enhanced ultrathin semitransparent electromagnetic shielding film and preparation method thereof
CN110868842A (en) * 2019-11-29 2020-03-06 北京林业大学 Mechanically-enhanced ultrathin semitransparent electromagnetic shielding film and preparation method thereof
CN111266019A (en) * 2020-01-23 2020-06-12 天津大学 Preparation method and application of vertically-oriented magnetic nanosheet/sodium alginate composite membrane
CN111422873A (en) * 2020-03-23 2020-07-17 北京化工大学 MXene/sodium alginate derived carbon three-dimensional aerogel and preparation method and application thereof
CN111718518A (en) * 2020-07-30 2020-09-29 北京航空航天大学 Preparation method of high-strength high-conductivity titanium carbide composite film
CN111718518B (en) * 2020-07-30 2021-08-17 北京航空航天大学 Preparation method of high-strength high-conductivity titanium carbide composite film
CN112501546A (en) * 2020-11-30 2021-03-16 江苏瑞悦轨道装备有限公司 Non-ferrous metal surface strengthening treatment method
CN112644016A (en) * 2020-12-11 2021-04-13 东北电力大学 Construction method of natural amphiprotic biomass gel artificial muscle device
CN112724427A (en) * 2021-01-29 2021-04-30 西北师范大学 Preparation of corn starch/sodium alginate/MXene composite hydrogel and application of composite hydrogel in seawater desalination
CN112724427B (en) * 2021-01-29 2022-09-13 西北师范大学 Preparation of corn starch/sodium alginate/MXene composite hydrogel and application of composite hydrogel in seawater desalination

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Application publication date: 20181218