CN109971002A - A kind of three-dimensional Ti3C2Hydrogel material and its preparation method and application - Google Patents
A kind of three-dimensional Ti3C2Hydrogel material and its preparation method and application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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Abstract
The invention belongs to the preparation technical fields of sorbent material, and in particular to a kind of three-dimensional Ti3C2Hydrogel material and its preparation method and application the described method comprises the following steps: polyvinyl alcohol is add to deionized water, PVA aqueous solution is prepared in 2 ~ 3h of mechanical stirring under the conditions of 85 ~ 95 DEG C；A certain amount of two dimension Ti is added3C2Nano material continues 1 ~ 3h of stirring until being uniformly mixed at 85 ~ 95 DEG C；Mixture is cast in mold, freeze forming in -15 ~ -25 DEG C of refrigerators is put into, the time is 8 ~ 16h；Sample is taken out, 4 ~ 8h is placed at room temperature and thaws, freeze-thaw cycle-index is 3 ~ 10 times；Sample is placed in -30 in vacuum freeze drier ~ -40 DEG C of low temperature are lyophilized to obtain sample.Preparation method of the present invention is easy to operate, and cost is relatively low, quickly environmental protection, and the hydrogel material porosity being prepared is high, large specific surface area, is expected to be applied to the fields such as dyestuff, heavy metal, waste oil absorption, have broad application prospects.
Description
Technical field
The invention belongs to the preparation technical field of gel rubber material, it is related to a kind of gel rubber material and preparation method thereof, specifically relates to
And a kind of three-dimensional Ti3C2Hydrogel material and its preparation method and application.
Background technique
Two-dimentional Ti3C2It is a kind of novel nano material, there is the layer structure similar with graphene, big specific surface area
Excellent absorption property and interlayer control are made it have with active site abundant, can be used as potential novel absorption material.
But practical application also faces many urgent problems to be solved: being Ti first3C2Scantling is small, and is easily dispersed in water, uses
After doing adsorbent absorption water pollutant, it is difficult to be removed from water, to bring secondary pollution problem.Followed by how further
Improve Ti3C2The specific surface area and hole configurations of material.Try to explore to improve Ti by multiple technologies means3C2The ratio of material
Surface area and hole configurations are to improve the inevitable approach of its absorption property.
Hydrogel is the gel using water as decentralized medium, is a kind of high molecular polymer with three-dimensional net structure,
In water can water absorption and swelling, solution pass through cross-bond between space diffusion, and be swollen after keep original structure it is constant.Hydrogel is containing parent
Aqueous group such as hydroxyl, amide groups, sulfonic group, carboxyl etc. can absorb even thousands of times of sole mass hundred times of water.Except this
Except, the minor change of environmental stimuli (such as temperature, pH value) can be perceived, realizes it to stimulation with shrinking by swelling
Response, excellent characteristic makes hydrogel cause the interest of vast environmental project researcher, and has been widely used for ring
The improvement field of border pollution, such as absorption heavy metal, processing dyeing waste water.PVA gel rubber material is due to its high-moisture, high-elastic
Property, hypotoxicity, high-biocompatibility and it is machined the features such as, have been to be concerned by more and more people, and industry, agricultural, biology,
The fields such as environment are widely used.And it is internal containing a large amount of hydroxyl, itself can mix with macromolecule, pass through physics
The approach such as winding, Hydrogenbond prepare high-strength composite hydrogel.
Nanoparticle is blended with polymeric matrix, the nanometer size effect of nanoparticle itself can be played, by nanoparticle
Mechanical property, optical property, electrical property and magnetic property that son has itself etc. assigns polymeric matrix, and composite material is made to compare phase
The composite material of the macroscopic view or micron level answered has bigger raising on macro property, while being able to maintain polymeric matrix sheet again
The features such as processability possessed by body is good, light-weight, stability is good.In recent years, many researchers are attempting nanometer
Material is introduced into gel rubber material, and functionality macroscopic material is made, and provides greatly reference meaning for the application of multifunctional material
Justice.Wherein most study is three-dimensional grapheme based nano composite material.Xu et al. has prepared three-dimensional using one step hydro thermal method
The Graphene gel of porous network structure, research find its with good electric conductivity (Xu et al., Acs Nano, 2010.4
(7): 4324-4330.)；Shao et al. uses solid liquid interface self-assembly method, utilizes the hydroxyl and graphene oxide of oxidation aluminium surface
Interaction between the functional group abundant of surface prepares graphene oxide hydrogel material (Shaoet al., Chemical
Communications, 2011.47 (20): 5771-3.).Yang et al. is prepared for PVA/GO by simple sol-gel method
Hydrogel material, discovery have good absorption property (Yanget al., Journal of to methylene blue dye
Nanoscience and Nanotechnology, 2016.16 (2): 1775-1782.).Polymer based nanocomposites
Preparation greatly expands the potential application space of two-dimension nano materials.
Summary of the invention
Goal of the invention: it is directed to Ti3C2Material limits existing for adsorbing domain practical application, skill to be solved by this invention
There is provided a kind of three-dimensional Ti for art problem3C2The preparation method of hydrogel material.The hydrogel material hole prepared by this method
Rate is high, and size is big between aperture and hole, large specific surface area, has preferable absorption property and biocompatibility, is expected to be applied to dye
The fields such as material, heavy metal, waste oil absorption, have broad application prospects.
There is provided three-dimensional Ti for the last technical problems to be solved of the present invention3C2Hydrogel material and its application.
Technical solution: in order to solve the above technical problems, the present invention adopts the following technical scheme: the present invention provides one kind three
Tie up Ti3C2The preparation method of hydrogel material, it the following steps are included:
(1) polyvinyl alcohol is add to deionized water, 2~3h of mechanical stirring obtains PVA water under the conditions of 85~95 DEG C
Solution；
(2) a certain amount of two dimension Ti is added in the PVA aqueous solution obtained to step (1)3C2Nano material, at 85~95 DEG C
Under continue 1~3h of stirring until be uniformly mixed obtain mixture；
(3) mixture that step (2) obtains is cast in mold, is put into freeze forming in refrigerator, obtains sample；
(4) sample for obtaining step (3) takes out, and is placed in and thaws at room temperature, and continues freeze-thaw and recycle 3~10 times；
(5) sample that step (4) obtains low temperature in vacuum freeze drier is placed in be lyophilized to obtain three-dimensional Ti3C2Hydrogel
Material.
Wherein, in the step (1), the mass ratio of PVA and deionized water is 1: 9~24.
Wherein, in the step (2), Ti in the aqueous solution3C2The mass ratio of nano material and PVA are Ti3C2: PVA=
1~6: 20.
Wherein, cooling time is 8~16h in the step (3), and cryogenic temperature is -15~25 DEG C.
Wherein, in the step (4), sample is placed in thaw at room temperature, and thawing time is 4~8h.
Wherein, in the step (5), sample is placed in vacuum freeze drier and is lyophilized, freeze-drying temperature be -30~-
40 DEG C, freeze-drying time is 12~48h.
The content of present invention further includes the three-dimensional Ti that above-mentioned preparation method obtains3C2Hydrogel material.
The content of present invention further includes three-dimensional Ti3C2Hydrogel material is in terms of dyestuff, heavy metal or waste oil adsorbing domain
Using.
Wherein, the dyestuff is cationic dyes or anionic dye.
Further, the dyestuff is methylene blue or one or both of Congo red.
The invention has the benefit that three-dimensional Ti provided by the invention3C2The preparation method of hydrogel material, technical solution
Easy to operate, cost is relatively low, quickly environmental protection, and the hydrogel material porosity being prepared is high, and large specific surface area is expected to apply
In fields such as dyestuff, heavy metal, waste oil absorption, have broad application prospects.
Detailed description of the invention
Fig. 1 is the PVA/Ti that the embodiment of the present invention 1 obtains3C2The scanning electron microscopic picture of hydrogel material；
Fig. 2 is the PVA/Ti that the embodiment of the present invention 3 obtains3C2Before the absorption of 20mg/L cationic dyes methylene blue
Comparison diagram afterwards；
Fig. 3 is the PVA/Ti that the embodiment of the present invention 4 obtains3C2Before and after the absorption Congo red to 50mg/L anionic dyes
Spectrogram；
Fig. 4 is the scanning electron microscopic picture for the PVA hydrogel material that comparative example of the present invention obtains.
Specific embodiment
The following are the preferred embodiment of the present invention, for explaining only the invention, and is not intended to limit the present invention, and by this
Illustrate that made related improve belongs to the range that appended claims of the present invention are protected.
Embodiment 1
Present embodiments provide a kind of three-dimensional Ti for Dye Adsorption3C2The preparation of hydrogel material, preparation step is such as
Under:
(1) 5g PVA is added in 45g deionized water, mechanical stirring 3h obtains PVA aqueous solution under the conditions of 90 DEG C；
(2) Ti of 1g is added into PVA aqueous solution3C2Material continues to stir 3h at 90 DEG C until uniformly mixed obtain
PVA/Ti3C2Mixture；
(3) by PVA/Ti3C2Mixture is cast in mold, and being put into cooling time in -15 DEG C of refrigerators is 16h freeze forming
Obtain sample；
(4) sample in refrigerator is taken out, is placed in 8h defrosting at room temperature, and continued freeze-thaw and recycle 6 times；
(5) sample of freezing is placed in -40 DEG C of low temperature freeze-dryings in vacuum freeze drier and obtains PVA/Ti for 24 hours3C2Hydrogel
Material.
By the PVA/Ti of taking-up3C2Hydrogel material sample carries out analysis and observation by scanning electron microscope etc., and sample is used for
The Study on adsorption properties of dyestuff.Fig. 1 is the PVA/Ti obtained under affiliated experiment parameter3C2The scanning electron microscope (SEM) photograph of hydrogel material.It is multiple
It closes gel and clearly porous structure is presented, since PVA contains a large amount of-OH base, be easy to and Ti3C2In conjunction with, by covalent cross-linking from
And three-dimensional net structure is formed, porosity is high, large specific surface area.
Embodiment 2
Present embodiments provide a kind of three-dimensional Ti for Dye Adsorption3C2The preparation of hydrogel material, preparation step is such as
Under:
(1) 2g PVA is added in 48g deionized water, mechanical stirring 2h obtains PVA aqueous solution under the conditions of 85 DEG C；
(2) Ti of 0.1g is added into PVA aqueous solution3C2Material continues to stir 1h at 85 DEG C until being uniformly mixed；
(3) by PVA/Ti3C2Mixture is cast in mold, is put into freeze forming in -25 DEG C of refrigerators, time 8h；
(4) sample in refrigerator is taken out, is placed in 4h defrosting at room temperature, and continued freeze-thaw and recycle 10 times；
(5) sample of freezing is placed in -30 DEG C of low temperature freeze-drying 12h in vacuum freeze drier and obtains PVA/Ti3C2Hydrogel
Material.
By the PVA/Ti of taking-up3C2Hydrogel material sample carries out analysis and observation by scanning electron microscope etc., and sample is used for
The Study on adsorption properties of dyestuff.Table 1 is the PVA/Ti obtained under affiliated experiment parameter3C2Hydrogel material and Ti3C2Powder for
The maximum adsorption scale of methylene blue solution, it is about Ti that the adsorption capacity of product, which is promoted, after gelation3C23 times of powder.
1 PVA/Ti of table3C2And Ti3C2For the maximum adsorption scale of methylene blue solution
| Adsorbent | Initial concentration | Maximal absorptive capacity (mg/g) |
| PVA/Ti3C2 | 50mg/L | 123.8 |
| Ti3C2 | 50mg/L | 39 |
Embodiment 3
Present embodiments provide a kind of three-dimensional Ti for Dye Adsorption3C2The preparation of hydrogel material, preparation step is such as
Under:
(1) 5g PVA is added in 45g deionized water, mechanical stirring 2.5h obtains PVA aqueous solution under the conditions of 95 DEG C；
(2) Ti of 0.5g is added into PVA aqueous solution3C2Material continues to stir 2h at 95 DEG C until being uniformly mixed；
(3) by PVA/Ti3C2Mixture is cast in mold, is put into freeze forming in -20 DEG C of refrigerators, time 12h；
(4) sample in refrigerator is taken out, is placed in 6h defrosting at room temperature, and continued freeze-thaw and recycle 3 times；
(5) sample of freezing is placed in -35 DEG C of low temperature freeze-dryings in vacuum freeze drier and obtains PVA/Ti for 24 hours3C2Hydrogel
Material sample.
By the PVA/Ti of taking-up3C2Hydrogel material sample carries out analysis and observation by scanning electron microscope etc., and sample is used for
The Study on adsorption properties of dyestuff.Fig. 2 is the PVA/Ti obtained under affiliated experiment parameter3C2To 20mg/L cationic dyes methylene
Comparison diagram before and after the absorption of base indigo plant.
Embodiment 4
Present embodiments provide a kind of three-dimensional Ti for Dye Adsorption3C2The preparation of hydrogel material, preparation step is such as
Under:
(1) 3g PVA is added in 47g deionized water, mechanical stirring 2h obtains PVA aqueous solution under the conditions of 90 DEG C；
(2) Ti of 0.9g is added into PVA aqueous solution3C2Material continues to stir 2h at 90 DEG C until being uniformly mixed；
(3) by PVA/Ti3C2Mixture is cast in mold, is put into freeze forming in -20 DEG C of refrigerators, time 16h；
(4) sample in refrigerator is taken out, is placed in 8h defrosting at room temperature, and continued freeze-thaw and recycle 8 times；
(5) sample of freezing is placed in -40 DEG C of low temperature freeze-drying 48h in vacuum freeze drier and obtains PVA/Ti3C2Hydrogel
Material sample.
By the PVA/Ti of taking-up3C2Hydrogel material sample carries out analysis and observation by scanning electron microscope etc., and sample is used for
The Study on adsorption properties of dyestuff.Fig. 3 is the PVA/Ti obtained under affiliated experiment parameter3C2Hydrogel material is to 50mg/L anion
Picture before and after the Congo red absorption of type dye.
Comparative example
A kind of preparation of three dimensional hydrogel material for Dye Adsorption is present embodiments provided, preparation step is as follows:
(1) 5g PVA is added in 45g deionized water, mechanical stirring 2.5h obtains PVA aqueous solution under the conditions of 95 DEG C；
(2) PVA aqueous solution is cast in mold, is put into freeze forming in -20 DEG C of refrigerators, time 12h；
(3) sample in refrigerator is taken out, is placed in 6h defrosting at room temperature, and continued freeze-thaw and recycle 3 times；
(4) sample of freezing is placed in -35 DEG C of low temperature freeze-dryings in vacuum freeze drier and obtains sample for 24 hours.
The sample of taking-up is subjected to analysis and observation by scanning electron microscope etc., and the absorption property that sample is used for dyestuff is ground
Study carefully.Fig. 4 is the scanning electron microscope (SEM) photograph of the PVA hydrogel material obtained under affiliated experiment parameter.By the PVA hydrogel material and implement
The resulting sample of example 3 carries out absorption property comparison, obtains the PVA/Ti of the embodiment of the present invention 3 Yu comparative example3C2With PVA for rigid
Arnotto solution maximum adsorption scale, as shown in table 2, PVA/Ti3C2Hydrogel material adsorbance has a distinct increment compared with PVA gel.
2 PVA/Ti of table3C2With PVA for Congo red solution maximum adsorption scale
| Adsorbent | Initial concentration | Maximal absorptive capacity (mg/g) |
| PVA/Ti3C2 | 50mg/L | 107 |
| PVA | 50mg/L | 74.4 |
Claims (10)
1. a kind of three-dimensional Ti3C2The preparation method of hydrogel material, which is characterized in that it the following steps are included:
(1) polyvinyl alcohol is add to deionized water, 2 ~ 3h of mechanical stirring obtains PVA aqueous solution under the conditions of 85 ~ 95 DEG C；
(2) a certain amount of two dimension Ti is added in the PVA aqueous solution obtained to step (1)3C2Nano material continues at 85 ~ 95 DEG C
1 ~ 3h of stirring obtains mixture until being uniformly mixed；
(3) mixture that step (2) obtains is cast in mold, is put into freeze forming in refrigerator and obtains sample；
(4) sample for obtaining step (3) takes out, and is placed in and thaws at room temperature, and continues freeze-thaw and recycle 3 ~ 10 times；
(5) sample that step (4) obtains low temperature in vacuum freeze drier is placed in be lyophilized to obtain three-dimensional Ti3C2Hydrogel material.
2. three-dimensional Ti according to claim 13C2The preparation method of hydrogel material, which is characterized in that in step (1), institute
The mass ratio for stating polyvinyl alcohol and deionized water is 1:9 ~ 24.
3. three-dimensional Ti according to claim 13C2The preparation method of hydrogel material, which is characterized in that in step (2), institute
State Ti in aqueous solution3C2The mass ratio of nano material and PVA are Ti3C2: PVA=1 ~ 6:20.
4. three-dimensional Ti according to claim 13C2The preparation method of hydrogel material, it is characterised in that: the step (3)
Middle cooling time is 8 ~ 16h, and cryogenic temperature is -15 ~ -25 DEG C.
5. three-dimensional Ti according to claim 13C2The preparation method of hydrogel material, it is characterised in that: the step (4)
In, sample is placed in thaw at room temperature, and thawing time is 4 ~ 8h.
6. three-dimensional Ti according to claim 13C2The preparation method of hydrogel material, it is characterised in that: the step (5)
In, sample is placed in vacuum freeze drier and is lyophilized, and freeze-drying temperature is -30 ~ -40 DEG C, and freeze-drying time is 12 ~ 48h.
7. the three-dimensional Ti that the described in any item preparation methods of claim 1 ~ 6 obtain3C2Hydrogel material.
8. three-dimensional Ti as claimed in claim 73C2Hydrogel material answering in terms of dyestuff, heavy metal or waste oil adsorbing domain
With.
9. application according to claim 8, which is characterized in that the dyestuff is cationic dyes or anionic dye.
10. application according to claim 8, which is characterized in that the dyestuff is methylene blue or one of Congo red
Or two kinds.
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Cited By (10)
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| CN110893338A (en) * | 2019-08-26 | 2020-03-20 | 河海大学 | Preparation method of polymer nano composite gel |
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| CN110684510B (en) * | 2019-10-23 | 2021-10-26 | 广东工业大学 | Heat-conduction-enhanced heat-energy-storage shape-stabilized phase-change composite material and preparation method thereof |
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| CN114614112B (en) * | 2022-04-06 | 2024-01-30 | 吉林大学 | Preparation method of solid-state energy storage device with MXene as electrode PVA-based hydrogel as electrolyte |
| CN116786094A (en) * | 2023-07-26 | 2023-09-22 | 山东省煤田地质规划勘察研究院 | Sewage plant tail water advanced nitrogen and phosphorus removal filler based on water supply plant sludge, preparation method and sewage plant tail water advanced treatment system |
| CN116786094B (en) * | 2023-07-26 | 2023-12-29 | 山东省煤田地质规划勘察研究院 | Sewage plant tail water advanced nitrogen and phosphorus removal filler based on water supply plant sludge, preparation method and sewage plant tail water advanced treatment system |
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Application publication date: 20190705 |