CN103263896A - Cellulose-based polymer/montmorillonite nano composite adsorption material and preparation method thereof - Google Patents
Cellulose-based polymer/montmorillonite nano composite adsorption material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a cellulose-based polymer/montmorillonite nano composite adsorbent and discloses a method for preparing a cellulose-based polymer/montmorillonite composite nano adsorbent through a way of performing graft copolymerization and intercalation polymerization at the same time in a homogeneous-phase ionic liquid system. The montmorillonite piece layers in the cellulose-based polymer/montmorillonite nano composite adsorbent are uniformly dispersed in the cellulose-based polymer in a peeling manner, and the cellulose-based polymer/montmorillonite nano composite adsorbent is an excellent organic/inorganic nano composite adsorption material; and the raw materials are widely available, the preparation technology is green and environment-friendly, the synthesis method is simple, the reaction conditions are mild, the solvent is easy to recycle, and the cellulose-based polymer/montmorillonite nano composite adsorbent can be applied to the field of wastewater treatment.
Description
Technical field
The present invention relates to a kind of functional polymer nano field of compound material, be specifically related to nano composite material of a kind of cellulose-based polymer/imvite and preparation method thereof, it be by function monomer in the graft copolymerization on the cellulose skeleton and function monomer the in-situ inserted polymerization between cheating engaging layer carry out simultaneously and make the functional polymer nano composite, can be widely used in field of waste water treatment
Background technology
Along with the fast development of global economy and society, water pollution problems is constantly aggravated, and serious harm is to ecological environment and human life and health.The improvement that water pollutes is through becoming the focus of domestic and international efforts at environmental protection person's research.In recent years, owing to the developmental research of the whole world to the new forms of energy environment-friendly materials, cellulose attracts tremendous attention as a kind of natural macromolecular material.Characteristics such as that cellulose has is pollution-free, wide material sources, good biocompatibility, physicochemical properties are stable will can be used for fields such as high absorbency material, oil absorbent, heavy metal absorbent and chromatography after its functionalization or the modification.And imvite because its aboundresources, interlayer cation interchangeability, such mineral have the ability of absorption cation and polarity organic molecule, is used as adsorbent and flocculant as the natural inorganic mineral material in the wastewater treatment of being everlasting.With cellulose modified the time and inorganic clay carry out compound preparation organic/inorganic composite material, be one of research direction of cellulose composite material in recent years.
With regard to present document, lot of documents shows that the performance of this organic/inorganic composite material is more excellent than former composition, in particular for water treatment field.(H. Qiu such as Qiu Haixia, J. Yu. Polyacrylate/ (Carboxymethyl cellulose Modified Montmorillonite) Superabsorbent Nanocomposite:Preparation and Water Absorbency. Journal of applied polymer science. 2008,107 (1): 118-123) synthesized polyacrylic acid/carboxymethyl cellulose/montmorillonite composite material, and studied its water absorbing capacity and water holding capacity, studies show that its water absorbing capacity and water holding capacity are better than stock blend.(L. Wang such as Wang Li, J. Zhang, A. Wang. Removal of Methylene Blue from Aqueous Solution Using Chitosan-g-Poly (Acrylic Acid)/Montmorillonite Superadsorbent Nanocomposite. Colloids and Surfaces A:Physicochemical and Engineering Aspects. 2008,322 (1): 47-53) synthesized shitosan-g-acrylic acid/montmorillonite compound adsorbent, studies show that its adsorption capacity to methylene blue is extremely superior.And cellulose is owing to being insoluble in usual vehicle, so few to the research for preparing cellulose-based polymer/montmorillonite composite material in the homogeneous system.
Therefore, research, the development and application to the novel environmental functional composite material will have great science, society and economic implications.So, we will to cellulose and imvite modified after carry out compound, thereby obtain the better composite of adsorptivity.
Summary of the invention
The technical problem to be solved in the present invention is: imvite is how by intercalation or peel off; The polymer of which kind of monomer has excellent adsorption capacity.
For solving the problems of the technologies described above, the following concrete technical scheme that the present invention has adopted.
A kind of organic/inorganic nano composite adsorbing material, synthetic by the following method: the organo montmorillonite after the former organ-mmt modification is dispersed in the organic solvent, adds function monomer then, high-speed stirred is prepared into and disperses uniform mixed solution; Mixed solution is joined in the cellulosic ionic liquid solution then, after mixing, add a certain amount of crosslinking agent and initator, at 40-120 ℃ of lower seal reaction 0.1-48 h, after separation, washing, drying, make cellulose-based polymer/montmorillonite composite material.Wherein the organic degree of imvite is 0-30%, and the mass ratio of cellulose, organo montmorillonite, initator, crosslinking agent, monomer is 1:(0.1-3): (0.001-1): (0.001-1): (5-300).
Described cellulose-based polymer/montmorillonite Composite sorbing material, its feature is described, and to be cellulose from cotton, fiber crops, straw, straw, the bagasse a kind of, its degree of polymerization≤1000.
Described imvite is sodium-based montmorillonite, calcium-base montmorillonite, magnesium base montmorillonite or the imvite through organising.
Described cellulose-based polymer/montmorillonite Composite sorbing material, the described grafted monomers of its feature are wherein a kind of such as acrylic acid, substitutional crylic acid, acrylamide, substituted acrylamide, acrylate, substituted acrylate, vinylpyridine, vinyl imidazole, vinyl-pyrrolidinone, VCz.
Described organic imvite modified dose be organic quaternary ammonium salt, organic season phosphonium salt, organic imidazole salts, the organ-mmt degree is 0-30%.
Described organic solvent is dimethyl formamide, dimethyl sulfoxide (DMSO), oxolane, pyridine, chloroform.
Described ionic liquid is 1-pi-allyl-3-methylimidazole chlorine, 1-butyl-3-methylimidazole chlorine, 1-(2-ethoxy)-3-methylimidazole chlorine, bromo N-ethylpyridine, 1-ethyl-3-methylimidazole methyl phosphonate salt.
Described initator is ammonium persulfate, ammonium ceric nitrate, potassium peroxydisulfate, azodiisobutyronitrile etc., and crosslinking agent is N, N-dimethyl bisacrylamide, benzoyl peroxide, N hydroxymethyl acrylamide, DAAM etc.
Described compound adsorbent be applied to wastewater treatment etc.
Cellulose-based polymer of the present invention/montmorillonite Composite adsorbent has the following advantages.
1. the present invention is raw material with cellulose and imvite, and that the composite adsorbing material of preparation has is cheap, raw material sources abundant, environment is not caused secondary pollution, advantage such as reusable, and the used recyclable recycling of solvent in the building-up process.
2. cellulose-based polymer/montmorillonite Composite the sorbing material of the present invention's preparation has realized carrying out simultaneously in the homogeneous system guess of graft copolymerization and intercalation polymeric, and composite structure superior performance, and synthesis condition gentleness, operating procedure is simple, production cost is low, easy operating.
3. the absorption property of Zhi Bei cellulose-based polymer/montmorillonite Composite adsorbent is superior, and heavy metal ion, organic pollution, dyestuff etc. are had good absorption property, in field of waste water treatment good prospect is arranged.
Description of drawings
Fig. 1 is the XRD spectra of imvite (a), organo montmorillonite (b), poly-(the 4-vinylpridine)/organo montmorillonite (c) of cellulose-g-.
Fig. 2 is the infrared spectrum of fibrillation element (d), imvite (e), organo montmorillonite (f), cellulose-g-polymethyl methacrylate/organo montmorillonite (g).
Fig. 3 is the TEM spectrogram of poly-(the 4-vinylpridine)/organo montmorillonite of cellulose-g-.
The specific embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is described further, but protection scope of the present invention is not limited to this.
Embodiment 1
Getting and obtaining concentration in ionic liquid 1-pi-allyl-3-methylimidazole chlorine that 0.2000 g cotton fiber adds 10 g is 20% cellulosic ionic liquid solution.Getting 0.15 g organo montmorillonite in addition adds among the 5.00 ml DMF, after being uniformly dispersed in DMF to organo montmorillonite, add 2.0 g methyl methacrylate monomers more respectively, behind magnetic agitation 6 h, scattered mixed solution is dropwise joined in the cellulosic ionic liquid solution, after mixing, add 0.001 g ammonium persulfate and 0.200 g N, N-dimethyl bisacrylamide heats up 60 ℃, after reacting 50 min, obtain white block solid product.The product that obtains is at room temperature spent deionised water for several times, wash dry 12 h in 60 ℃ of following air dry ovens, dry 12 h in 60 ℃ vacuum drying chamber after the drying again with acetone.Characterize through IR, XRD and TEM, methyl methacrylate not only successfully is grafted on the cellulose skeleton, and intercalation between cheating engaging layer.And studied it to the adsorption capacity of 2,4-chlorophenesic acid, its maximal absorptive capacity is 410 mg/g.
Getting and obtaining concentration in ionic liquid 1-pi-allyl-3-methylimidazole chlorine that 0.1000 g stalk cellulose adds 10 g is 10% cellulosic ionic liquid solution.Getting 0.10 g organo montmorillonite in addition respectively adds among the 5.00 ml DMF, after being uniformly dispersed in DMF to organo montmorillonite, add 1.5 g 4-vinylpridine monomers more respectively, behind magnetic agitation 6 h, scattered mixed solution is dropwise joined in the cellulosic ionic liquid solution, after mixing, add 0.02 g azodiisobutyronitrile and 0.25 g N, N-dimethyl bisacrylamide heats up 80 ℃, after reacting 50 min, obtain milky blocks of solid product.The product that obtains is at room temperature spent deionised water for several times, wash dry 12 h in 60 ℃ of following air dry ovens, dry 12 h in 60 ℃ vacuum drying chamber after the drying again with acetone.Characterize through IR, XRD and TEM, 4-vinylpyridine not only successfully is grafted on the cellulose skeleton, and intercalation between cheating engaging layer.And studied it to the adsorption capacity of 2,4-chlorophenesic acid, its maximal absorptive capacity is 890 mg/g.
Embodiment 3
Getting and obtaining concentration in ionic liquid 1-pi-allyl-3-methylimidazole chlorine that 0.1500 g flaxen fiber adds 10 g is 15% cellulosic ionic liquid solution.Getting 0.10 g sodium-based montmorillonite in addition respectively adds among the 5.00 ml DMF, after being uniformly dispersed in DMF to sodium-based montmorillonite, add 3.0 g acrylamide monomers more respectively, behind magnetic agitation 6 h, scattered mixed solution is dropwise joined in the cellulosic ionic liquid solution, after mixing, add 0.02 g potassium peroxydisulfate and 0.25 g N hydroxymethyl acrylamide, heat up 65 ℃, react 50 min after, obtain the colorless transparent gel product.The product that obtains is at room temperature spent deionised water for several times, wash dry 12 h in 60 ℃ of following air dry ovens, dry 12 h in 60 ℃ vacuum drying chamber after the drying again with acetone.Characterize through IR, XRD and TEM, acrylamide not only successfully is grafted on the cellulose skeleton, and intercalation between cheating engaging layer.And studied its adsorption capacity to methylene blue, its maximal absorptive capacity is 420 mg/g.
Getting and obtaining concentration in ionic liquid 1-pi-allyl-3-methylimidazole chlorine that 0.1500 g cotton fiber adds 10 g is 15% cellulosic ionic liquid solution.Getting 0.10 g sodium-based montmorillonite in addition respectively adds among the 5.00 ml DMF, after being uniformly dispersed in DMF to sodium-based montmorillonite, add 3.0 g acrylic monomers more respectively, behind magnetic agitation 6 h, scattered mixed solution is dropwise joined in the cellulosic ionic liquid solution, after mixing, add 0.05 g potassium peroxydisulfate and 0.05 g DAAM, heat up 60 ℃, react 50 min after, obtain the colorless transparent gel product.The product that obtains is at room temperature spent deionised water for several times, wash dry 12 h in 60 ℃ of following air dry ovens, dry 12 h in 60 ℃ vacuum drying chamber after the drying again with acetone.Characterize through IR, XRD and TEM, acrylic acid not only successfully is grafted on the cellulose skeleton, and intercalation between cheating engaging layer.And studied its adsorption capacity to methylene blue, its maximal absorptive capacity is 1700 mg/g.
Embodiment 5
Getting and obtaining concentration in ionic liquid 1-pi-allyl-3-methylimidazole chlorine of plain 10 g of adding of 0.2000 g bagasse fibre is 20% cellulosic ionic liquid solution.Getting 0.15 g organo montmorillonite in addition respectively adds among the 5.00 ml DMF, after being uniformly dispersed in DMF to organo montmorillonite, add 2.5 g 2-vinylpyridine monomers more respectively, behind magnetic agitation 6 h, scattered mixed solution is dropwise joined in the cellulosic ionic liquid solution, after mixing, add 0.05 g azodiisobutyronitrile and 0.05 g DAAM, heat up 80 ℃, react 50 min after, obtain the colorless transparent gel product.The product that obtains is at room temperature spent deionised water for several times, wash dry 12 h in 60 ℃ of following air dry ovens, dry 12 h in 60 ℃ vacuum drying chamber after the drying again with acetone.Characterize through IR, XRD and TEM, the 2-vinylpyridine not only successfully is grafted on the cellulose skeleton, and intercalation between cheating engaging layer.And studied its Pyrogentisinic Acid's adsorption capacity, its maximal absorptive capacity is 120 mg/g.
Getting and obtaining concentration in ionic liquid 1-pi-allyl-3-methylimidazole chlorine that 0.1500 g straw cellulose adds 10 g is 15% cellulosic ionic liquid solution.Getting 0.10 g organo montmorillonite in addition respectively adds among the 5.00 ml DMF, after being uniformly dispersed in DMF to organo montmorillonite, add 2.0 g l-vinyl-2-pyrrolidone monomers more respectively, behind magnetic agitation 6 h, scattered mixed solution is dropwise joined in the cellulosic ionic liquid solution, after mixing, add 0.05 g azodiisobutyronitrile and 0.05 g DAAM, heat up 70 ℃, react 50 min after, obtain the yellow transparent solid product.The product that obtains is at room temperature spent deionised water for several times, wash dry 12 h in 60 ℃ of following air dry ovens, dry 12 h in 60 ℃ vacuum drying chamber after the drying again with acetone.Characterize through IR, XRD and TEM, l-vinyl-2-pyrrolidone not only successfully is grafted on the cellulose skeleton, and intercalation between cheating engaging layer.And studied it to the adsorption capacity of 2,4-chlorophenesic acid, its maximal absorptive capacity is 650 mg/g.
Embodiment 7
Getting and obtaining concentration in ionic liquid 1-pi-allyl-3-methylimidazole chlorine that 0.2500 g flaxen fiber adds 10 g is 25% cellulosic ionic liquid solution.Getting 0.15 g organo montmorillonite in addition respectively adds among the 5.00 ml DMF, after being uniformly dispersed in DMF to organo montmorillonite, add 2.5 g 9-vinyl carbazole monomers more respectively, behind magnetic agitation 6 h, scattered mixed solution is dropwise joined in the cellulosic ionic liquid solution, after mixing, add 0.02 g azodiisobutyronitrile and 0.25 g DAAM, heat up 65 ℃, react 120 min after, obtain milky blocks of solid product.The product that obtains is at room temperature spent deionised water for several times, wash dry 12 h in 60 ℃ of following air dry ovens, dry 12 h in 60 ℃ vacuum drying chamber after the drying again with acetone.Characterize through IR, XRD and TEM, the 9-vinyl carbazole not only successfully is grafted on the cellulose skeleton, and intercalation between cheating engaging layer.And studied its Pyrogentisinic Acid's adsorption capacity, its maximal absorptive capacity is 250 mg/g.
Getting and obtaining concentration in ionic liquid 1-pi-allyl-3-methylimidazole chlorine that 0.1000 g stalk cellulose adds 10 g is 10% cellulosic ionic liquid solution.Getting 0.10 g organo montmorillonite in addition respectively adds among the 5.00 ml DMF, after being uniformly dispersed in DMF to organo montmorillonite, add 2.5 g acrylonitrile monemers more respectively, behind magnetic agitation 6 h, scattered mixed solution is dropwise joined in the cellulosic ionic liquid solution, after mixing, add 0.05 g potassium peroxydisulfate and 0.05 g DAAM, heat up 50 ℃, react 180 min after, obtain white block solid product.The product that obtains is at room temperature spent deionised water for several times, wash dry 12 h in 60 ℃ of following air dry ovens, dry 12 h in 60 ℃ vacuum drying chamber after the drying again with acetone.Characterize through IR, XRD and TEM, the 9-vinyl carbazole not only successfully is grafted on the cellulose skeleton, and intercalation between cheating engaging layer.And studied it to Cu
2+Adsorption capacity, its maximal absorptive capacity is 270 mg/g.
Claims (10)
1. the nano combined sorbing material of a cellulose-based polymer/imvite, it is characterized in that, it is the nano combined sorbing material of a kind of cellulose-based polymer/imvite of preparing by the function monomer mode that the in-situ inserted polymerization between cheating engaging layer is carried out simultaneously in the graft copolymerization on the cellulose skeleton and function monomer in the homogeneous phase ion liquid system, and its raw material is formed by following mass percent:
(1) cellulosic matrix, consumption are 0.1-25 %;
(2) functional polymer, consumption are 50-99.8 %;
(3) imvite, consumption are 0.1-25 %.
2. as the described cellulose-based polymer of claim 1/montmorillonite Composite sorbing material, its feature is described, and to be cellulose from cotton, fiber crops, straw, straw, the bagasse a kind of, its degree of polymerization≤1000.
3. imvite as claimed in claim 1 can be any in sodium-based montmorillonite, calcium-base montmorillonite, magnesium base montmorillonite and the process imvite that organises.
4. cellulose-based polymer as claimed in claim 1/montmorillonite Composite sorbing material, the described grafted monomers of its feature are wherein a kind of such as acrylic acid, substitutional crylic acid, acrylamide, substituted acrylamide, acrylate, substituted acrylate, vinylpyridine, vinyl imidazole, vinyl-pyrrolidinone, VCz.
5. as claim 1 described cellulose-based polymer/montmorillonite Composite sorbing material, its preparation process is as follows: the organo montmorillonite after the former organ-mmt modification is dispersed in the organic solvent, add function monomer then, high-speed stirred is prepared into and disperses uniform mixed solution; Mixed solution is joined in the cellulosic ionic liquid solution then, after mixing, add a certain amount of crosslinking agent and initator, at 40-120 ℃ of lower seal reaction 0.1-48 h, make cellulose-based polymer/montmorillonite composite material after separation, washing, drying, the mass ratio of described cellulose, organo montmorillonite, initator, crosslinking agent, polymerisable monomer is 1:(0.1-3): (0.001-1): (0.001-1): (5-300).
As claimed in claim 5 organic imvite modified dose be organic quaternary ammonium salt, organic season phosphonium salt, organic imidazole salts, the organ-mmt degree is 0-30%.
7. as described in the claim 5, described organic solvent is dimethyl formamide, dimethyl sulfoxide (DMSO), oxolane, pyridine, chloroform.
8. be 1-pi-allyl-3-methylimidazole chlorine, 1-butyl-3-methylimidazole chlorine, 1-(2-ethoxy as claim 5 described ionic liquids)-3-methylimidazole chlorine, bromo N-ethylpyridine, 1-ethyl-3-methylimidazole methyl phosphonate salt.
9. as described in the claim 5, initator is ammonium persulfate, ammonium ceric nitrate, potassium peroxydisulfate, azodiisobutyronitrile etc., and crosslinking agent is N, N-dimethyl bisacrylamide, benzoyl peroxide, N hydroxymethyl acrylamide, DAAM etc.
10. the compound adsorbent of preparing as claim 1 or 5 can be applicable to field of waste water treatment etc.
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