CN105153438A - Preparation method of high-strength high-swelling nanocellulose and polyving akohol composite hydrogel - Google Patents
Preparation method of high-strength high-swelling nanocellulose and polyving akohol composite hydrogel Download PDFInfo
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Abstract
The invention discloses a preparation method of high-strength high-swelling nanocellulose and polyving akohol composite hydrogel. The method comprises the following steps that nanocellulose suspension is added in dimethyl sulfoxide solvent, and magnetic stirring is conducted to prepare mixed dispersion liquid; polyving akohol is added, and magnetic stirring is conducted for 3 h on the condition that the temperature is 95 DEG C; standing is conducted for 30 min at the constant temperature of 60 DEG C, the dispersion liquid is placed at the constant temperature after being frozen at low temperature, and freezing and thawing circulation is conducted for 5-8 times; obtained hydrogel is put in deionized water to swap out the dimethyl sulfoxide solvent in the gel, and the nanocellulose and polyving akohol composite gel is obtained. According to the preparation method of the high-strength high-swelling nanocellulose and polyving akohol composite hydrogel, reactions are physical reactions, and pollution to the environment in the preparation process is extremely low; by means of a mixed solvent system of dimethyl sulfoxide and water, formation of a uniform network structure of the nanocellulose and polyving akohol gel can be effectively facilitated, the formed three-dimensional interpenetrating network structure can effectively improve the strength and the swelling degree of the gel, the dimethyl sulfoxide can be directly swapped out from the gel after the reaction is completed, and the obtained biomass gel is free of toxicity and pollution.
Description
Technical field
The present invention relates to the preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel, belong to bioengineering field.
Background technology
Hydrogel, as a kind of desirable bio-medical material, has attracted increasing research interest.Polyvinyl alcohol (PVA) is a kind of water-soluble polymeric macromolecular material, and it has extraordinary biocompatibility, hypotoxicity simultaneously.The application of PVA hydrogel in biomedical sector is more and more subject to people's attention.Methyl-sulphoxide is a kind of well thin protic, utilizes it and water mixed solvent as solvent system, polyvinyl alcohol gel can be made to form the cross-linked network structure of homogeneous dispersion, thus can form homogeneous aperture in formation gelation process.Therefore, the gel obtained by the mixed solvent system of methyl-sulphoxide and water is utilized to have the better mechanical strength of the polyvinyl alcohol gel more obtained than pure water.
And nano-cellulose is a kind of novel polymer reinforcing material, have the advantage of light weight, excellent in mechanical performance, biological degradability, its recyclability is also that other strongtheners cannot be by comparison.But, the mechanics of simple polyvinyl alcohol gel, swelling and thermomechanical property also cannot meet the requirement of biomedical material, therefore, fully in conjunction with the advantage performance of polyvinyl alcohol, nano-cellulose and methyl-sulphoxide, a kind of both there is high strength for preparation, the gelatinous material of high swelling and excellent thermomechanical property had been the thinking having very much scientific meaning and application prospect.
Polyvinyl alcohol be a kind of be widely used in gel research polymkeric substance, the positive active research of recent domestic its in bionic application.(the EuropeanPolymerJournal such as current StevenSpoljaric, 2014,56 phases, 105-117 page), composite aquogel is prepared by fibrillated fibre element, polyvinyl alcohol and borax, obtain the hydrogel of certain self-healing ability, but the swelling property of this performance to gel has had restriction, the swelling capacity of gel is not high.(the ArabianJournalofChemistry such as El-RefaieKenawy, 2014,7th phase, 372-280 page), obtained by polyvinyl alcohol and hydroxyethylamyle compound and the gel film significantly improved is adsorbed to protein mass, expanded its application at biomedical sector, but the introducing of hydroxyethylamyle reduces the intensity of gel.
Because biomass are cheap, it is wide, environmentally friendly to originate, therefore preparing gelatinous material by biomass is a kind of desirable method.Therefore, nano-cellulose is a kind of desirable strongthener preparing nanofiber hydrogels.But, there is no the report using nano-cellulose to prepare high strength, high swelling nano-cellulose/polyvinyl alcohol hydrogel in methyl-sulphoxide/aqueous solvent at present.
CN102786642A discloses a kind of preparation method of Nanometer cellulose/polyvinyl alcohol gel composite material, add Potassium Persulphate (KPS), sodium bisulfite (SBS) and vinylformic acid (AA), linking agent (NMBA) promotes nano-cellulose and polyvinyl alcohol crosslinked, but gel prepared by the method employs a large amount of chemical reagent and is cross-linked, not only cost is high, can produce toxicity in contaminate environment and use procedure, these deficiencies significantly limit the application at bioengineering field of gel.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel, comprises the following steps:
(1) nano-cellulose suspension adds in dimethylsulfoxide solvent, and magnetic agitation is mixed with mixed dispersion liquid;
(2) polyvinyl alcohol adds in the dispersion liquid in step (1), and heating condition lower magnetic force is stirred to evenly;
(3) the dispersion liquid constant temperature of step (2) is left standstill, obtain nano-cellulose and polyvinyl alcohol mixing dispersion liquid;
(4) dispersion liquid that step (3) obtains is poured in mould, leave standstill;
(5) after step (4) being obtained mixed dispersion liquid cryogenic freezing, constant temperature is placed again, multigelation, circulation 5-8 time;
(6) hydrogel that step (5) obtains is put into the dimethylsulfoxide solvent that deionized water displaces gel, obtain nano-cellulose/polyvinyl alcohol plural gel.
As preferred technical scheme, described nano-cellulose is the nano-cellulose of plant origin, and the concentration of the nano-cellulose in nano-cellulose suspension is 0.8 ~ 1.2wt%, and diameter is 10 ~ 30nm, length 500nm ~ 2 μm.
As preferred technical scheme, the polymerization degree 1750 ± 50 of described polyvinyl alcohol.
As preferred technical scheme, each components by weight nano-cellulose suspension: dimethylsulfoxide solvent: polyvinyl alcohol=20:80:7.5.
As preferred technical scheme, in step (2), magnetic agitation temperature is 95 DEG C, and in step (3), dwell temperature is 60 DEG C.
As preferred technical scheme, in step (5), the cryogenic freezing temperature of each freeze thawing is-20 DEG C, freezing time 12h; Constant temperature laying temperature be 25 DEG C storage period 4h.
As preferred technical scheme, described nano-cellulose by mechanical mill, enzymic hydrolysis, acid hydrolysis or oxidizing in any one method to prepare or at least two or more methods is combined and prepared.
As preferred technical scheme, the preparation method of described nano-cellulose suspension is as follows:
A, sieve get 40 ~ 60 object bamboo powder raw materials, use electronic balance accurately to take 10g filter paper packet and wrap and put into Soxhlet extraction device, prepare the Benzene-ethanol extraction liquid of 450ml after being dried, 90 DEG C are carried out extracting 6h, filtration washing is directly neutral, wherein benzene 300ml in Benzene-ethanol extraction liquid, ethanol 150ml;
B, the raw material after filter wash is put into beaker, add 400ml deionized water, process in acid condition with the Textone of 1 ~ 1.25wt%, again adding with measuring Textone after 1h, processing equally in acid condition, repeating interpolation 5 ~ 7 times, to remove most of xylogen, obtained holocellulose;
The potassium hydroxide solution of C, preparation 2 ~ 3wt%, processes holocellulose 2 ~ 3h that the 1st step obtains, to remove most of hemicellulose wherein at 90 DEG C;
D, with 1 ~ 1.25wt% Textone treatment step (C) gained solution 1 ~ 2h in acid condition, and at 90 DEG C, purification process 2 ~ 4h is carried out to gained Mierocrystalline cellulose with the potassium hydroxide of 4 ~ 7wt% further, to remove delignification and hemicellulose, thus obtain the Mierocrystalline cellulose of purifying;
The hydrochloric acid soln of E, employing 1 ~ 1.5wt%, the purifying cellulose 2 ~ 3h obtained in treatment step (D) at 80 ~ 90 DEG C;
F, the purifying cellulose that step e obtains is made into the aqueous suspension that concentration is 0.8 ~ 1.2wt%, milled processed 15 ~ 20 minutes, obtains Fibre diameter at 10 ~ 30nm, the nano-cellulose suspension liquid of staple length in 500nm ~ 2 μm.
Beneficial effect of the present invention is as follows:
1) between nano-cellulose of the present invention and polyvinyl alcohol be physical reaction, preparation process environmental pollution is extremely low, the mixed solvent system of methyl-sulphoxide and water effectively can promote that nano-cellulose/polyvinyl alcohol gel forms homogeneous network structure, the three-dimensional interpenetrating polymer network structure formed effectively can improve intensity and the swelling capacity of gel, and reacted rear methyl-sulphoxide and can directly cement out from gel, the biomass gel nontoxic pollution-free obtained.
2) adopt freeze-thaw cycle legal system for nano-cellulose/polyvinyl alcohol plural gel, preparation process is simple, obtains high-strength composite gel, improves gel thermostability.
3) the nano-cellulose diameter range prepared of the present invention is at 10 ~ 30nm, fiber length ranges is between 500nm ~ 2 μm, and its length-to-diameter ratio and specific surface area improve a lot, and the plural gel of preparation has high strength, high swelling degree, can be applicable to biomedicine, the fields such as organizational project.
Embodiment
Embodiment 1
The step of preparation process of nano-cellulose:
A, sieve get 40 ~ 60 object bamboo powder raw materials, use electronic balance accurately to take 10g filter paper packet and wrap and put into Soxhlet extraction device, prepare the Benzene-ethanol extraction liquid of 450ml after being dried, 90 DEG C are carried out extracting 6h, filtration washing is directly neutral, wherein benzene 300ml in Benzene-ethanol extraction liquid, ethanol 150ml;
B, the raw material after filter wash is put into beaker, add 400ml deionized water, process in acid condition with the Textone of 1 ~ 1.25wt%, again adding with measuring Textone after 1h, processing equally in acid condition, repeating interpolation 5 ~ 7 times, to remove most of xylogen, obtained holocellulose;
The potassium hydroxide solution of C, preparation 2 ~ 3wt%, processes holocellulose 2 ~ 3h that the 1st step obtains, to remove most of hemicellulose wherein at 90 DEG C;
D, with 1 ~ 1.25wt% Textone treatment step (C) gained solution 1 ~ 2h in acid condition, and at 90 DEG C, purification process 2 ~ 4h is carried out to gained Mierocrystalline cellulose with the potassium hydroxide of 4 ~ 7wt% further, to remove delignification and hemicellulose, thus obtain the Mierocrystalline cellulose of purifying;
The hydrochloric acid soln of E, employing 1 ~ 1.5wt%, the purifying cellulose 2 ~ 3h obtained in treatment step (D) at 80 ~ 90 DEG C;
F, the purifying cellulose that step e obtains is made into the aqueous suspension that concentration is 0.8 ~ 1.2wt%, milled processed 15 ~ 20 minutes, obtains diameter at 10 ~ 30nm, the nano-cellulose suspension liquid of length in 500nm ~ 2 μm.
Embodiment 2
The preparation method of this high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel, comprises the following steps:
(1) take the nano-cellulose suspension of 5g, drip a certain amount of deionized water and keep the water-content in suspension to be 20g, add in 80g dimethyl sulfoxide solution, magnetic agitation is mixed with mixed dispersion liquid;
(2) weighing polyvinyl alcohol 7.5g, adds in the dispersion liquid in step (1), and 95 DEG C of condition lower magnetic forces stir 3h;
(3) step (2) dispersion liquid constant temperature is left standstill 30min, dwell temperature is 60 DEG C, obtains nano-cellulose and polyvinyl alcohol mixing dispersion liquid;
(4) dispersion liquid that step (3) obtains is poured in mould, leave standstill 10min;
(5) step (4) is obtained mixed dispersion liquid cryogenic freezing 12h, freezing temp is-20 DEG C, and after taking out, constant temperature places 4h, and laying temperature is 25 DEG C, has repeated 5 freeze-thaw cycle;
(6) hydrogel that step (5) obtains is put into the dimethylsulfoxide solvent that deionized water displaces gel, obtain nano-cellulose/polyvinyl alcohol plural gel.
Performance test is carried out to obtained nano-cellulose/polyvinyl alcohol plural gel.Test result is in table 1.
Embodiment 3
The preparation method of this high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel, comprises the following steps:
(1) take the nano-cellulose suspension of 10g, drip a certain amount of deionized water and keep the water-content in suspension to be 20g, add in 80g dimethyl sulfoxide solution, magnetic agitation is mixed with mixed dispersion liquid;
(2) weighing polyvinyl alcohol 7.5g, adds in the dispersion liquid in step (1), and 95 DEG C of condition lower magnetic forces stir 3h;
(3) step (2) dispersion liquid constant temperature is left standstill 30min, dwell temperature is 60 DEG C, obtains nano-cellulose and polyvinyl alcohol mixing dispersion liquid;
(4) dispersion liquid that step (3) obtains is poured in mould, leave standstill 10min;
(5) step (4) is obtained mixed dispersion liquid cryogenic freezing 12h, freezing temp is-20 DEG C, and after taking out, constant temperature places 4h, and laying temperature is 25 DEG C, has repeated 8 freeze-thaw cycle;
(6) hydrogel that step (5) obtains is put into the dimethylsulfoxide solvent that deionized water displaces gel, obtain nano-cellulose/polyvinyl alcohol plural gel.
Embodiment 4
The preparation method of this high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel, comprises the following steps:
(1) take the nano-cellulose suspension of 20g, drip a certain amount of deionized water and keep the water-content in suspension to be 20g, add in 80g dimethyl sulfoxide solution, magnetic agitation is mixed with mixed dispersion liquid;
(2) weighing polyvinyl alcohol 7.5g, adds in the dispersion liquid in step (1), and 95 DEG C of condition lower magnetic forces stir 3h;
(3) step (2) dispersion liquid constant temperature is left standstill 30min, dwell temperature is 60 DEG C, obtains nano-cellulose and polyvinyl alcohol mixing dispersion liquid;
(4) dispersion liquid that step (3) obtains is poured in mould, leave standstill 10min;
(5) step (4) is obtained mixed dispersion liquid cryogenic freezing 12h, freezing temp is-20 DEG C, and after taking out, constant temperature places 4h, and laying temperature is 25 DEG C, has repeated 6 freeze-thaw cycle;
(6) hydrogel that step (5) obtains is put into the dimethylsulfoxide solvent that deionized water displaces gel, obtain nano-cellulose/polyvinyl alcohol plural gel.
Comparative example 1
The preparation method of this nano-cellulose/polyvinyl alcohol composite hydrogel, comprises the following steps:
(1) take the nano-cellulose suspension of 5g, add a certain amount of deionized water and keep the water-content in whole system to be 100g, magnetic agitation is mixed with mixed dispersion liquid;
(2) weighing polyvinyl alcohol 7.5g, adds in the dispersion liquid in step (1), and 95 DEG C of condition lower magnetic forces stir 3h;
(3) step (2) dispersion liquid constant temperature is left standstill 30min, dwell temperature is 60 DEG C, obtains nano-cellulose and polyvinyl alcohol mixing dispersion liquid;
(4) dispersion liquid that step (3) obtains is poured in mould, leave standstill 10min;
(5) step (4) is obtained mixed dispersion liquid cryogenic freezing 12h, freezing temp is-20 DEG C;
(6) the gel constant temperature after freezing for step (5) is placed 4h, laying temperature is 25 DEG C, counts 1 freeze-thaw cycle together with step (5);
(7) repeating step (5) and (6) complete 5 freeze-thaw cycle, obtain nano-cellulose/polyvinyl alcohol plural gel.
Performance test is carried out to obtained nano-cellulose/polyvinyl alcohol plural gel.Test result is in table 1
The performance synopsis of nano-cellulose/polyvinyl alcohol composite hydrogel that table 1: embodiment 2-4 and comparative example 1 obtain
| Compressive strength (MPa) | Swelling capacity (S%) |
| Embodiment 2 | 0.77 | 580 |
| Embodiment 3 | 1.02 | 740 |
| Embodiment 4 | 1.53 | 760 |
| Comparative example 1 | 0.52 | 470 |
Swelling capacity is tested: obtained gel sample is placed 24h in the deionized water of 25 DEG C and reaches swelling equilibrium, takes out gel sample filter paper and dries gel surface moisture.Swelling capacity
w
sfor weight during swelling equilibrium, W
dfor the weight of xerogel.
Compressive strength is tested: format diameter and the high right cylinder being 12mm of obtained sample, fully swelling gel specimen surface filter paper is dried, carry out compressive strength test with omnipotent mechanics machine (Shenzhen, SANSI), compressive strain rate is set to 5mm/min.Compressive strength when calculating compressive strain is 60%.
As can be seen from Table 1, the nano-cellulose/polyvinyl alcohol plural gel obtained by preparation method of the present invention has higher intensity and higher swelling capacity.
Claims (8)
1. a preparation method for high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel, is characterized in that: comprise the following steps:
(1) nano-cellulose suspension adds in dimethylsulfoxide solvent, and magnetic agitation is mixed with mixed dispersion liquid;
(2) polyvinyl alcohol adds in the dispersion liquid in step (1), and heating condition lower magnetic force is stirred to evenly;
(3) the dispersion liquid constant temperature of step (2) is left standstill, obtain nano-cellulose and polyvinyl alcohol mixing dispersion liquid;
(4) dispersion liquid that step (3) obtains is poured in mould, leave standstill;
(5) after step (4) being obtained mixed dispersion liquid cryogenic freezing, constant temperature is placed again, multigelation, circulation 5-8 time;
(6) hydrogel that step (5) obtains is put into the dimethylsulfoxide solvent that deionized water displaces gel, obtain nano-cellulose/polyvinyl alcohol plural gel.
2. the preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel according to claim 1, it is characterized in that: described nano-cellulose is the nano-cellulose of plant origin, the concentration of the nano-cellulose in nano-cellulose suspension is 0.8 ~ 1.2wt%, Fibre diameter is 10 ~ 30nm, staple length 500nm ~ 2 μm.
3. the preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel according to claim 2, is characterized in that: the polymerization degree of described polyvinyl alcohol is 1750 ± 50.
4. the preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel according to claim 3, is characterized in that: each components by weight nano-cellulose suspension: dimethylsulfoxide solvent: polyvinyl alcohol=20:80:7.5.
5. the preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel according to claim 4, is characterized in that: in step (2), magnetic agitation temperature is 95 DEG C, and in step (3), dwell temperature is 60 DEG C.
6. the preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel according to claim 5, is characterized in that: in step (5), the cryogenic freezing temperature of each freeze thawing is-20 DEG C, freezing time 12h; Constant temperature laying temperature be 25 DEG C storage period 4h.
7. the preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel according to claim 3, is characterized in that: described nano-cellulose by mechanical mill, enzymic hydrolysis, acid hydrolysis or oxidizing in any one method to prepare or at least two or more methods is combined and prepared.
8. the preparation method of high strength high swelling property nano-cellulose/polyvinyl alcohol composite hydrogel according to claim 7, is characterized in that: the preparation method of described nano-cellulose suspension is as follows:
A, sieve get 40 ~ 60 object bamboo powder raw materials, use electronic balance accurately to take 10g filter paper packet and wrap and put into Soxhlet extraction device, prepare the Benzene-ethanol extraction liquid of 450ml after being dried, 90 DEG C are carried out extracting 6h, filtration washing is directly neutral, wherein benzene 300ml in Benzene-ethanol extraction liquid, ethanol 150ml;
B, the raw material after filter wash is put into beaker, add 400ml deionized water, process in acid condition with the Textone of 1 ~ 1.25wt%, again adding with measuring Textone after 1h, processing equally in acid condition, repeating interpolation 5 ~ 7 times, to remove most of xylogen, obtained holocellulose;
The potassium hydroxide solution of C, preparation 2 ~ 3wt%, processes holocellulose 2 ~ 3h that the 1st step obtains, to remove most of hemicellulose wherein at 90 DEG C;
D, with 1 ~ 1.25wt% Textone treatment step (C) gained solution 1 ~ 2h in acid condition, and at 90 DEG C, purification process 2 ~ 4h is carried out to gained Mierocrystalline cellulose with the potassium hydroxide of 4 ~ 7wt% further, to remove delignification and hemicellulose, thus obtain the Mierocrystalline cellulose of purifying;
The hydrochloric acid soln of E, employing 1 ~ 1.5wt%, the purifying cellulose 2 ~ 3h obtained in treatment step (D) at 80 ~ 90 DEG C;
F, the purifying cellulose that step e obtains is made into the aqueous suspension that concentration is 0.8 ~ 1.2wt%, milled processed 15 ~ 20 minutes, obtains Fibre diameter at 10 ~ 30nm, the nano-cellulose suspension liquid of length in 500nm ~ 2 μm.
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