CN101735353B - N-vinyl amides polymer and laponite composite hydrogel and preparation method - Google Patents

N-vinyl amides polymer and laponite composite hydrogel and preparation method Download PDF

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CN101735353B
CN101735353B CN 201010019233 CN201010019233A CN101735353B CN 101735353 B CN101735353 B CN 101735353B CN 201010019233 CN201010019233 CN 201010019233 CN 201010019233 A CN201010019233 A CN 201010019233A CN 101735353 B CN101735353 B CN 101735353B
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water
laponite
initiator
hydrogel
azo
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CN101735353A (en
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刘新星
童真
裴煜
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

The invention provides a preparation method of high-strength and high-tenacity N-vinyl amides polymer and laponite composite hydrogel, which comprises the following steps of: dispersing laponite in water, stirring to obtain a uniform and transparent dispersing solution, then sequentially adding a N-vinyl amides monomer, an initiator and a water-soluble dye, uniformly stirring, deoxidizing and sealing; heating a reaction system for reacting to obtain laponite cross-linked nano-composite hydrogel; or placing the reaction system in a thermostatic environment, illuminating the obtained laponite cross-linked nanocomposite hydrogel by using an UV (ultraviolet) light. By dispersing the laponite in the water fully, adding the N-vinyl amides monomer and the initiator, selecting a water-bath heating mode or an UV light induced reaction mode, and adopting an in-situ free radical polymerization method, the invention obtains the hydrogel with a high-strength and high-tenacity N-vinyl amides polymer and laponite nano-composite structure.

Description

N-vinylamide polymer and lithium algae soil composite aquogel and preparation method
Technical field
The present invention relates to composite aquogel, particularly a kind of high-strength and high ductility N-vinylamide polymer and lithium algae soil composite aquogel and preparation method.
Background technology
Polyalcohol hydrogel because of its in extensive applications such as petrochemical complex, food and biomedical engineerings; As: crude oil/processed oil dewatering agent, oilwell water shutoff water transfer, foodstuff additive, medicine sustained release and biological tissue's packing material or the like receive people's common concern and research.Yet there is following defective in conventional polymer hydrogel (hereinafter to be referred as the OR gel): the low toughness of intensity is not good enough,, be merely able to be used for gel-strength is required very low field, this has greatly influenced the range of application of polyalcohol hydrogel.
Publish (Adv.Mater. according to document; 2002; 14:1120-1124); Haraguchi etc. are dispersed in lithium algae soil (Laponite) nanoparticle in the water; Make N-NSC 11448 (NIPAm) and the original position radical polymerization in the Laponite dispersion liquid of acrylic amide (AM) monomer; The Laponite nano particle plays the effect of polyfunctionality linking agent, thereby has obtained two kinds of Nanometer composite hydrogels (hereinafter to be referred as the NC gel): poly N-isopropyl acrylamide/Laponite Nanometer composite hydrogel (PNIPAm/Laponite Nanocomposite Hydrogel) and SEPIGEL 305/Laponite Nanometer composite hydrogel (PAm/Laponite Nanocomposite Hydrogel).The NC gel has the mechanical property of high-strength and high ductility, and the transparency is good.Up to now; Only there are these two kinds of acrylic amides can successfully prepare lithium algae soil Nanometer composite hydrogel; And these two kinds of hydrogels (>=80%) or lithium algae soil and monomer content when water ratio is higher be when low (≤10%), and mechanical property still has sizable decline.
Summary of the invention
The objective of the invention is to defective to the prior art existence; A kind of high-strength and high ductility N-vinylamide polymer and lithium algae soil composite aquogel is provided; This Nanometer composite hydrogel (water ratio 50～90%) not only has the high characteristics such as HS of the high H.T. of elongation at break and tensile strength, and (universal testing machine records its elongation at break and intensity respectively between 50%～4000% and 2kPa～1MPa with the rate of extension of 100mm/ second; And common OR gel is very fragile, can not be clamped in and carry out Elongation test on the universal testing machine); And (equilibrium swelling than respectively between 5～120, water ratio 83～99%) can also keep quite high mechanical property (universal testing machine records its elongation at break and tensile strength respectively between 10%～2000% and 5kPa～350kPa) with the rate of extension of 100mm/ second when reaching swelling equilibrium.Simultaneously, high adsorption capacity, bio-toxicity is low, the transparency good (transmittance that the ultraviolet spectrophotometer records hydrogel provided by the invention at the 600nm wavelength is between 40～95%).
The present invention also aims to provide the preparation method of said hydrogel.
The preparation method of a kind of high-strength and high ductility N-vinylamide polymer of the present invention and lithium algae soil composite aquogel may further comprise the steps:
The first step is scattered in lithium algae soil in the water, stirs the dispersion liquid that obtains homogeneous transparent, adds N-vinyl amide monomer, initiator then successively, and back deoxygenation sealing stirs; Each composition weight umber is following:
Lithium algae soil 0.5～20
Water 49～94.5
N-vinyl amide monomer 5～30
Initiator 0.01～1;
Second step placed 30-60 ℃ of water-bath to heat reaction system, and reaction 12-72h promptly obtains the crosslinked Nanometer composite hydrogel of lithium algae soil; Perhaps
Reaction system is placed 0-30 ℃ of isoperibol, select the UV lamp of 100-400nm wave band for use, apart from reaction system 1-100cm, irradiation 0.1-8h promptly obtains the crosslinked Nanometer composite hydrogel of lithium algae soil;
The present invention also can comprise for the 3rd step, and the hydrogel in the reaction system is taken out, and can obtain high-strength and high ductility, and the transparency is good, chromatophilous Nanometer composite hydrogel.Or will be not the gel of adding water soluble dyestuff place the water-soluble dye 0.1～10 hour of 0.01～1mg/L, can get painted Nanometer composite hydrogel; The consumption of water-soluble dye is 0～0.01 weight.
In the first step, stir the dispersion liquid that 0.1-10h obtains homogeneous transparent
Lithium algae mount of the present invention is drawn together natural and synthetic lithium algae soil, four kinds of product: Laponite series that preferred especially Rockwood company produces, and its product and molecular formula are respectively:
XLS type: [Mg 5.34Li 0.66Si 8O 20(OH) 4] Na 0.66, Na 4P 2O 7Modification
RDS type: Na + 0.7[(Si 8Mg 5.5Li 0.3) O 20(OH) 4] - 0.7, Na 4P 2O 7Modification
XLG type: [Mg 5.34Li 0.66Si 8O 20(OH) 4] Na 0.66
RD type: Na + 0.7[(Si 8Mg 5.5Li 0.3) O 20(OH) 4] - 0.7
Monomer of the present invention is the N-vinyl amide monomer, preferred especially N-vinyl acetamide, and N-methyl-N-vinyl acetamide, preferable amount is the 10-20% of reaction mass total amount.
Initiator of the present invention comprises water-soluble azo initiator, as 2,2 '-azo diisobutyl amidine dihydrochloride (being called for short V-50); 2,2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride (being called for short VA-044), 4; 4 '-azo two (4-cyanopentanoic acid) (being called for short V-501); Azo di-isopropyl tetrahydroglyoxaline (be called for short VA-061) etc., preferred especially 2,2 '-azo diisobutyl amidine dihydrochloride (being called for short V-50) or 2; 2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride (being called for short VA-044), preferable amount is the 0.05-0.5% of reaction mass total amount.Initiator of the present invention can be dissolved in the deoxidation high purity water in advance, makes things convenient for weighing to calculate.
Water-soluble dye of the present invention comprises and preferred cationic water-soluble dye such as cationic blue, rhodamine B etc.
The present invention compared with prior art has following advantage:
1, through lithium algae soil is well dispersed in the water; Add N-vinyl amide monomer and initiator; Select heating in water bath or UV Photoinitiated reactions mode; Adopt the method for original position radical polymerization, thereby obtain the hydrogel of high-strength and high ductility N-vinylamide polymer and lithium algae soil nano composite structure.
2, the present invention introduces monomer molecule on the surface of the sub-lamella of lithium algae grogs; And in the presence of initiator; Carry out original position radical polymerization, between lithium algae grogs, form polymer chain, thereby the present invention can be through regulating the ratio between lithium algae soil (linking agent), monomer and the initiator; Obtain different mechanical properties and swelling behavior, also have good transparence and chromatic Nanometer composite hydrogel simultaneously.
3, compared with prior art, the present invention can be under lower lithium algae soil concentration and monomer concentration (≤10%), and the high-strength and high-ductility of realization gel (elongation at break is>=2000%, breaking tenacity>=800KPa); The gel that the present invention obtains is after reaching swelling equilibrium; (water ratio>=90%, elongation at break are>=2000%, breaking tenacity>=170KPa) still to keep preferably mechanical property; Because mechanical property is too poor, can't be used for test behind the gel swelling that other method obtains.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail, but the working of an invention mode is not limited thereto.
Embodiment 1
At first; 2g lithium algae soil Laponte XLS is scattered in the 100g high purity water; Stir the dispersion liquid that 4h obtains homogeneous transparent, add 10g N-vinyl acetamide monomer, 0.04g V-50 initiator then successively, the rear-guard oxygen that stirs is transferred in the glass test tube and is sealed; Reaction initiation mode can obtain strong mechanical performance, good, the chromatophilous Nanometer composite hydrogel of the transparency for placing 40-60 ℃ of water-bath heating 36 hours; One one of the hydrogel of preparation gained is divided to be used for universal testing machine mensuration mechanical property and spectrophotometric determination transmittance; The elongation at break of this part Nanometer composite hydrogel is 1200%; Breaking tenacity 33.0kPa, transmittance 90.0%, water ratio 88.0%; Another part is placed in a large amount of high purity waters and soaked 15-20 days, refreshes the water periodically and to swelling equilibrium, uses the gravimetric determination swelling ratio; The elongation at break of this part Nanometer composite hydrogel is 50% behind the mensuration swelling equilibrium, breaking tenacity 5.0kPa, transmittance 96.0%, swelling ratio 82.0 (water ratio 99%).
Embodiment 2
Present embodiment except that following characteristics with embodiment 1: institute adds lithium algae soil and is 6g.The elongation at break of this Nanometer composite hydrogel is 2400%, breaking tenacity 260kPa, transmittance 65%, water ratio 84%; The elongation at break of this part Nanometer composite hydrogel is 1200% behind the mensuration swelling equilibrium, breaking tenacity 150.0kPa, transmittance 85%, swelling ratio 27.0 (water ratio 96%).
Embodiment 3
Present embodiment except that following characteristics with embodiment 1: institute adds lithium algae soil and is 10g.The elongation at break of this Nanometer composite hydrogel is 2500%, breaking tenacity 830kPa, transmittance 70%, water ratio 80%; The elongation at break of this part Nanometer composite hydrogel is 1800% behind the mensuration swelling equilibrium, breaking tenacity 350.0kPa, transmittance 80%, swelling ratio 13.0 (water ratio 92%).
Embodiment 4
Present embodiment except that following characteristics with embodiment 1: to add monomer be N-methyl-N-vinyl acetamide in institute.The elongation at break of this Nanometer composite hydrogel is 50%, breaking tenacity 2.5kPa, transmittance 43%, water ratio 80%; The elongation at break of this part Nanometer composite hydrogel is 10% behind the mensuration swelling equilibrium, breaking tenacity 1.0kPa, transmittance 75%, swelling ratio 50 (water ratio 98%).
Embodiment 5
Present embodiment except that following characteristics with embodiment 2: to add monomer be N-methyl-N-vinyl acetamide in institute.The elongation at break of this Nanometer composite hydrogel is 2500%, breaking tenacity 230kPa, transmittance 44%, water ratio 84%; The elongation at break of this part Nanometer composite hydrogel is 2200% behind the mensuration swelling equilibrium, breaking tenacity 170.0kPa, transmittance 65%, swelling ratio 11.0 (water ratio 92%).
Embodiment 6
Present embodiment except that following characteristics with embodiment 3: to add monomer be N-methyl-N-vinyl acetamide in institute.The elongation at break of this Nanometer composite hydrogel is 3100%, breaking tenacity 530kPa, transmittance 45%, water ratio 80%; The elongation at break of this part Nanometer composite hydrogel is 3000% behind the mensuration swelling equilibrium, breaking tenacity 350.0kPa, transmittance 60%, swelling ratio 9.5 (water ratio 90%).
Embodiment 7
Present embodiment except that following characteristics with embodiment 1: institute adds lithium algae soil and is Laponite XLG.The elongation at break of this Nanometer composite hydrogel is 1400%, breaking tenacity 60kPa, transmittance 89%, water ratio 88%; The elongation at break of this part Nanometer composite hydrogel is 80% behind the mensuration swelling equilibrium, breaking tenacity 8.5kPa, transmittance 95%, swelling ratio 60.0 (water ratio 98%).
Embodiment 8
Present embodiment except that following characteristics with embodiment 1: institute adds lithium algae soil and is Laponite RD.The elongation at break of this Nanometer composite hydrogel is 1600%, breaking tenacity 80kPa, transmittance 90%, water ratio 88%; The elongation at break of this part Nanometer composite hydrogel is 100% behind the mensuration swelling equilibrium, breaking tenacity 15.0kPa, transmittance 93%, swelling ratio 55.0 (water ratio 99%).
Embodiment 9
Present embodiment except that following characteristics with embodiment 2: institute adds lithium algae soil and is Laponite RDS.The elongation at break of this Nanometer composite hydrogel is 2600%, breaking tenacity 330kPa, transmittance 62%, water ratio 84%; The elongation at break of this part Nanometer composite hydrogel is 1500% behind the mensuration swelling equilibrium, breaking tenacity 180.0kPa, transmittance 85%, swelling ratio 20.0 (water ratio 95%).
Embodiment 10
Present embodiment except that following characteristics with embodiment 4: institute adds lithium algae soil and is Laponite XLG.The elongation at break of this Nanometer composite hydrogel is 130%, breaking tenacity 11.0kPa, transmittance 40%, water ratio 88%; The elongation at break of this part Nanometer composite hydrogel is 40% behind the mensuration swelling equilibrium, breaking tenacity 3.5kPa, transmittance 65%, swelling ratio 48.0 (water ratio 98%).
Embodiment 11
Present embodiment except that following characteristics with embodiment 4: institute adds lithium algae soil and is Laponite RD.The elongation at break of this Nanometer composite hydrogel is 150%, breaking tenacity 18kPa, transmittance 42%, water ratio 88%; The elongation at break of this part Nanometer composite hydrogel is 60% behind the mensuration swelling equilibrium, breaking tenacity 5.0kPa, transmittance 60%, swelling ratio 44.0 (water ratio 98%).
Embodiment 12
Present embodiment except that following characteristics with embodiment 5: institute adds lithium algae soil and is Laponite RDS.The elongation at break of this Nanometer composite hydrogel is 2800%, breaking tenacity 300kPa, transmittance 45%, water ratio 84%; The elongation at break of this part Nanometer composite hydrogel is 2000% behind the mensuration swelling equilibrium, breaking tenacity 200.0kPa, transmittance 66%, swelling ratio 11.0 (water ratio 91%).
Embodiment 13
Present embodiment except that following characteristics with embodiment 1-12: reactive mode is a UV illumination initiated polymerization, and the 245nmUV lamp shone 20-60 minute apart from Glass tubing 5cm.The basically identical of gained gel each item performance and embodiment 1-12.
Embodiment 14
Present embodiment except that following characteristics with embodiment 1-13: to add initiator be VA-044 in institute.The basically identical of gained gel each item performance and embodiment 1-13.
Embodiment 15
Present embodiment except that following characteristics with embodiment 1-13.It is V-501 that institute adds initiator.The basically identical of gained gel each item performance and embodiment 1-13.
Embodiment 16
Present embodiment except that following characteristics with embodiment 1-13.It is VA-061 that institute adds initiator.The basically identical of gained gel each item performance and embodiment 1-13.
Embodiment 17
Present embodiment except that following characteristics with embodiment 1-15.In lithium algae soil dispersion liquid, add water-soluble dye cationic blue 0.001g.It is blue that the gained gel is, the basically identical of each item performance and embodiment 1-15 except that transmittance.
Embodiment 18
Present embodiment except that following characteristics with embodiment 1-15.In lithium algae soil dispersion liquid, add water-soluble dye rhodamine B 0.001g.The gained gel is red-purple, the basically identical of each item performance and embodiment 1-15 except that transmittance.
Embodiment 19
Place the 0.1mg/ml dyestuff rhodamine B aqueous solution to take out after 1 hour embodiment 1-16 gained Nanometer composite hydrogel, hydrogel and dye solution are homochromy, place three monthly phenomenons of fading that do not occur.
Embodiment 20
Place the blue aqueous solution of 0.1mg/ml dye cations to take out after 1 hour embodiment 1-16 gained Nanometer composite hydrogel, hydrogel and dye solution are homochromy, place three monthly phenomenons of fading that do not occur.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (9)

1. the preparation method of N-vinylamide polymer and lithium algae soil composite aquogel is characterized in that may further comprise the steps:
The first step is scattered in lithium algae soil in the water, stirs the dispersion liquid that obtains homogeneous transparent, adds N-vinyl amide monomer, initiator then successively, and back deoxygenation sealing stirs; Each composition weight umber is following:
Second step placed 30-60 ℃ of water-bath to heat reaction system, reaction 12-72h; Perhaps
Reaction system is placed 0-30 ℃ of isoperibol, select the UV lamp of 100-400nm wave band for use, apart from reaction system 1-100cm, irradiation 0.1-8h; Take out hydrogel.
2. method according to claim 1 is characterized in that, in the first step, stirs the dispersion liquid that 0.1-10h obtains homogeneous transparent.
3. method according to claim 2 is characterized in that four kinds of products of Laponite series that described lithium algae soil is produced for Rockwood company, and its molecular formula is respectively:
XLS type: [Mg 5.34Li 0.66Si 8O 20(OH) 4] Na 0.66, Na 4P 2O 7Modification;
RDS type: Na + 0.7[(Si 8Mg 5.5Li 0.3) O 20(OH) 4] - 0.7, Na 4P 2O 7Modification;
XLG type: [Mg 5.34Li 0.66Si 8O 20(OH) 4] Na 0.66
RD type: Na + 0.7[(Si 8Mg 5.5Li 0.3) O 20(OH) 4] - 0.7
4. method according to claim 3 is characterized in that described N-vinyl amide monomer comprises N-vinyl acetamide and/or N-methyl-N-vinyl acetamide.
5. method according to claim 4 is characterized in that described initiator comprises water-soluble azo initiator.
6. method according to claim 5 is characterized in that described initiator comprises water-soluble azo initiator.
7. method according to claim 6; It is characterized in that described water-soluble azo initiator comprises 2; 2 '-azo diisobutyl amidine dihydrochloride, 2; 2 '-azo [2-(2-tetrahydroglyoxaline-2-yl) propane] dihydrochloride, 4,4 '-in the azo two (4-cyanopentanoic acids), azo di-isopropyl tetrahydroglyoxaline one or more, consumption is the 0.05-0.5% of reaction mass total amount.
8. method according to claim 7 is characterized in that described water-soluble dye is the cation water-soluble dyestuff.
9. the N-vinylamide polymer of the said method of one of claim 1-8 preparation and the native composite aquogel of lithium algae.
CN 201010019233 2010-01-07 2010-01-07 N-vinyl amides polymer and laponite composite hydrogel and preparation method Expired - Fee Related CN101735353B (en)

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