CN109666252A - A kind of high-intensitive double-network hydrogel and preparation method thereof with magnetic responsiveness - Google Patents
A kind of high-intensitive double-network hydrogel and preparation method thereof with magnetic responsiveness Download PDFInfo
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Abstract
The invention discloses one kind to be based on Fe3O4High-intensitive magnetic response double-network hydrogel of nano particle and preparation method thereof.The hydrogel is by by Fe3O4Nano particle is introduced into prepare in dual network (DN) hydrogel and be formed, double-network hydrogel constructs first network using the carboxyl and ferric ion formation ligand complex on natural anion polysaccharide pectin molecule chain, using the polyacrylamide network of covalent cross-linking as the second network.The hydrogel can be by adjusting Fe3O4Content make its tensile strength up to 1.20 ± 0.07MPa, elongation strain is 1600 ± 232%, elasticity modulus 1.10MPa ± 0.08MPa.More importantly hydrogel is in addition to also having good magnetic responsiveness, different degrees of bending can be realized under externally-applied magnetic field, can be applied to software brake field with preferable mechanical performance.
Description
Technical field
The present invention relates to one kind to be based on Fe3O4The preparation side of the magnetic responsiveness of nano particle, high-intensitive double-network hydrogel
Method belongs to field of functional materials.
Background technique
Magnetic responsiveness brake has the characteristics that accurate controllability, fast response time, stability are high, is widely used in electronics
Equipment, Medical Devices, the fields such as biomedicine.Hydrogel is due to distinctive 3D network structure, good flexibility and biofacies
Capacitive, the performances such as higher water content, can be efficiently applied to magnetic responsiveness brake field, to prepare magnetic responsiveness water-setting
Adhesive brake.For magnetic responsiveness hydrogel, mechanical property, sensitivity, anti-fatigue ability are important performance parameter.So
And the mechanical performance of current magnetic responsiveness hydrogel is weaker, intensity is generally less than megapascal, and the biocompatibility of material compared with
Difference, these disadvantages limit their application.Therefore, preparation mechanical property is preferable, and the magnetic responsiveness hydrogel of high sensitivity is made
It is a highly important meaning for magnetic brake.
In recent years, a kind of high-intensitive dual network (DN) hydrogel based on physical crosslinking and covalent cross-linking, becomes and currently grinds
The hot spot studied carefully.Since DN gel has uniform network structure, scatteredload can be effectively arrived, the hair of stress concentration phenomenon is reduced
It is raw, mainly pass through introducing " sacrificing key " concept, there is unique energy dissipation mechanism, to play raising hydrogel intensity
With flexible purpose.And the usual intensity of magnetic hydrogel and flexibility currently reported cannot be met simultaneously, Er Qiening
Colloid system is defective, is easy to be destroyed quickly, these undoubtedly limit it in the application that there are certain requirements mechanical performance in field.
Traditional DN hydrogel have preparation process complexity it is cumbersome, using be related to swelling, diffusion, it is difficult to control two kinds of monomers
Molar ratio and two kinds of networks the disadvantages of being made of covalent cross-linking, cannot restoring after fracture.And polysaccharide based aquagel has
Good biocompatibility, solve artificial-synthetic copolymer's bring raw material sources are limited, product is impure, harmful by-products,
The disadvantages of starting monomer is harmful to the human body, still, simple polysaccharide based aquagel toughness is poor, and gel rubber system is very crisp, can not
Meet the needs of mechanical strength and ductility.And by chemical crosslinking double-network hydrogel have preferable anti-fatigue ability and
Mechanical strength.Therefore, by the way that the polyacrylamide of the polysaccharide based aquagel of physical crosslinking and chemical crosslinking is combined together system
Standby double-network hydrogel can meet the features such as the simple, good biocompatibility of mechanical property, preparation process simultaneously.
Summary of the invention
In order to improve, magnetic responsiveness hydrogel preparation step is cumbersome, process is uncontrollable, poor mechanical property, device bio-compatible
Property it is poor the disadvantages of, we are creative to propose magnetic Fe3O4Nano particle and high-intensitive double-network hydrogel combine, to make
Standby magnetic responsiveness, the high-intensitive double-network hydrogel provided is as magnetic induction brake.Firstly, we select natural polysaccharide fruit
Glue as first network raw material, by and Fe3+Carry out ligand complex and form first network, polyacrylamide as the second network,
To prepare high-intensitive double-network hydrogel.Then by magnetic Fe3O4Nano particle is introduced into polysaccharide-based high intensity dual network water
Gel prepares the high-intensitive double-network hydrogel with magnetic responsiveness as magnetic induction brake.
It is an object of the invention to overcome existing hydrogel mechanical property and poor biocompatibility, preparation process cumbersome, anti-
The disadvantages of poor fatigue properties, provide that a kind of preparation process is simple, mechanical performance is high, the high intensity hydrogel of good biocompatibility.
Technical scheme is as follows:
A kind of high-intensitive double-network hydrogel with magnetic responsiveness；By magnetic Fe3O4Nano particle and high-intensitive dual network
Hydrogel combines；Natural polysaccharide pectin as first network raw material, by and Fe3+It carries out ligand complex and forms the first net
Network, polyacrylamide are the second network, obtain high-intensitive double-network hydrogel；Magnetic Fe3O4Nano particle is introduced into polysaccharide-based height
Intensity double-network hydrogel obtains the high-intensitive double-network hydrogel with magnetic responsiveness.
The preparation method of high-intensitive double-network hydrogel with magnetic responsiveness of the invention；Include the following steps:
(1) by Fe3O4Nano particle is added in ionized water, and ultrasonic disperse obtains magnetic fluid；Pectin and acrylamide are rubbed
You for 1:1~11 than being dissolved in above-mentioned deionized water, after mixing evenly, photoinitiator, crosslinking agent is then added, temperature is risen to
50-80 DEG C, solution is obtained after stirring；
(2) step (1) acquired solution is vacuumized, and fills N2To remove the O in solution2；Then solution is transferred to
It in mold, is placed under ultraviolet lamp and irradiates, form pectin/polyacrylamide list network aqueous gel of magnetic responsiveness；
(3) pectin/polyacrylamide list network aqueous gel that step (2) obtains is soaked in FeCl3Magnetic is obtained in solution
The Fe of responsiveness3+The pectin of crosslinking/polyacrylamide DN hydrogel.
In the step (1), pectin mass fraction is 1-30wt%, and acrylamide concentration is 0.1-5wt% mixed solution.
It is preferred that Fe3O4Nano particle is added to the Fe being configured in ionized water3O4Nanoparticle mass score is 1%-
11wt%.
Preferred photoinitiator is Iracure 2959, and additional amount is that the percentage of the sum of pectin and acrylamide mole is
0.05-2mol%.
It is preferred that crosslinking agent N, N- methylene-bisacrylamide, additional amount are the percentages of the sum of pectin and acrylamide mole
Than for 0.01-0.1mol%.
Being placed in irradiation condition under ultraviolet lamp in the step (2) is: intensity 5-10W, and wavelength is under the ultraviolet lamp of 365nm
Irradiate 1-5h.
Step (3) FeCl3Solution concentration is 0.01-2M, soaking time 0.5-12h.
High-intensitive double-network hydrogel with magnetic responsiveness of the invention is as cantilever beam flexure actuator.
Compared with prior art, the invention has the following beneficial effects: be prepared for Fe using " one pot of two-step method "3+Crosslinking
Pectin/polyacrylamide high intensity double-network hydrogel, overcomes that preparation process is cumbersome, uncontrollable disadvantage.Prepared is more
Glycosyl double-network hydrogel has preferable toughness, anti-fatigue performance and biocompatibility.
Meanwhile in order to solve the problems, such as that current magnetic responsiveness brake mechanical property is weak, pass through the Fe that will be prepared3O4Nanometer
Particle introduces above-mentioned high-intensitive double-network hydrogel, is prepared into magnetic responsiveness, high-intensitive double-network hydrogel, and with higher
Sensitivity, so that the DN hydrogel can be used as magnetic responsiveness brake under magnetic drive.The double-network hydrogel can pass through tune
Save Fe3O4Content make its tensile strength up to 1.20 ± 0.07MPa, elongation strain is 1600 ± 232% (Fig. 2 a), springform
It measures 1.10MPa ± 0.1MPa (Fig. 2 b).Hydrogel, can in addition to also having good magnetic responsiveness with preferable mechanical performance
To realize different degrees of bending (Fig. 4) under externally-applied magnetic field.
Detailed description of the invention
Fig. 1: different Fe3O4The magnetic strength curve graph of MDN hydrogel under content；
Fig. 2 a): Fe3O4Influence diagram of the content to MDN hydrogel tensile stress and elongation at break；
Fig. 2 b): Fe3O4Influence diagram of the content to MDN hydrogel elastic modulus；
Fig. 3: slant range figure of the hydrogel cantilever beam brake under magnet attraction；
Fig. 4 a: being successively from left to right Fe3O4Answering property of magnetic when content is respectively 1wt%, 2.5wt%, 4wt%, 6wt%,
Optical photograph when high-intensitive double-network hydrogel is as cantilever beam flexure actuator；
Fig. 4 b: being successively from left to right corresponding difference Fe under the action of externally-applied magnetic field3O4The cantilever beam deflection of content
The magnetic response degree figure of brake.
Specific embodiment
Technical solution of the present invention is further illustrated combined with specific embodiments below.
The preparation method of the high-intensitive double-network hydrogel with magnetic responsiveness of invention: it is prepared first with pectin
(pectin) carboxyl and Fe on3+The first network of physical crosslinking is formed by coordination, polyacrylamide (PAAm) passes through covalently
It is cross-linked to form the high-intensitive double-network hydrogel of the second network, then introduces magnetic Fe3O4Nano particle prepares magnetic responsiveness, height
Intensity double-network hydrogel, as magnetic induction brake；The preparation method is as follows:
(1) by Fe3O4Nano particle is added in ionized water, and ultrasonic disperse obtains magnetic fluid, the Fe being configured to3O4Nanometer
Granular mass score is 1%-11wt%, is that 1:1~1:11 is dissolved in above-mentioned deionized water by pectin and acrylamide molar ratio,
After mixing evenly, pectin mass fraction is 1-30wt%, and acrylamide concentration is 0.1-5wt% mixed solution, is then added
Photoinitiator Iracure 2959 and 0.01-0.1mol% the crosslinking agent N,N methylene bis acrylamide of 0.05-2mol%
(MBA) (percentage that the two mole is the sum of pectin and acrylamide mole), rises to 50-80 DEG C, after stirring for temperature
Obtain uniform solution；
(2) step (1) acquired solution is vacuumized, and fills N2To remove the O in solution2；Then solution is transferred to
In mold, being placed in intensity is 5-10W, irradiates 1-5h under the ultraviolet lamp that wavelength is 365nm, forms pectin/poly- third of magnetic responsiveness
Acrylamide list network (SN) hydrogel；
(3) pectin/polyacrylamide list network aqueous gel that step (2) obtains is soaked in the FeCl of 0.01-2M3Solution
In, impregnate the Fe of acquisition magnetic responsiveness after 0.5-12h3+The pectin of crosslinking/polyacrylamide DN hydrogel (abbreviation MDN water-setting
Glue)；
Reagent used in following example mainly includes following several: pectin (pectin), acrylamide (AAm), and three
Ferric chloride hexahydrate (FeCl3·6H2O), ferrous chloride tetrahydrate (FeCl2·4H2O), 2- hydroxyl -4- (2- hydroxyl ethoxy
Base) -2- methyl phenyl ketone (Irgacure 2959), N, N- methylene-bisacrylamide (MBA), concentrated hydrochloric acid, sodium hydroxide is dense
Ammonium hydroxide
Embodiment 1:Fe3O4The preparation of nano particle high intensity magnetic response double-network hydrogel
(1) Fe of 5g preparation is weighed3O4Nano particle is added in 200ml deionized water, and ultrasonic disperse obtains magnetic fluid,
0.05mol pectin and 0.25mol acrylamide is added, then by the photoinitiator 2- hydroxyl of 1mol% (the 1% of AM molar concentration)
Base -4- (2- hydroxy ethoxy) -2- methyl phenyl ketone (Irgacure 2959) and 0.03mol% (3% of AM molar concentration) crosslinking
Agent N, N- methylene-bisacrylamide (MBA) is added thereto, and temperature is risen to 70 DEG C, obtains uniform solution after stirring 2h.
(2) acquired solution is vacuumized twice simultaneously, by filling N2Remove the O in solution2.Then solution is transferred to
In rectangular mould.It is 8W that mold, which is put in intensity, irradiates 2h under the ultraviolet lamp that wavelength is 365nm, it is mono- to form pectin/PAAm
Network (SN) hydrogel.
(3) then the mono- network aqueous gel of pectin/PAAm is soaked in the FeCl of 0.05M3In solution, 4h is impregnated, Fe is made3+
Ligand complex is carried out with carboxyl on pectin, finally obtains pectin/polyacrylamide MDN hydrogel.
Fig. 1 is to Fe3O4The magnetic strength of nanometer is characterized and is tested, the experimental results showed that, pure Fe3O4Nanoparticle is satisfied
It can achieve 52.21emu/g with the intensity of magnetization, hysteresis be not present on curve, and remanent magnetism and coercivity are not present, explanation
Using the Fe of coprecipitation preparation3O4Nanoparticle has superparamagnetism.For MDN hydrogel, with Fe3O4Content
Increase, the saturation magnetization of MDN hydrogel is consequently increased, similarly, all MDN samples also without hysteresis,
Coercivity and remanent magnetism are 0, illustrate that prepared MDN hydrogel also has superparamagnetic behavior.
Fig. 2 a is characterized and is tested to the mechanical property of high-intensitive double-network hydrogel, the experimental results showed that, pass through tune
Save Fe3O4The content of nano particle, the tensile strength of double-network hydrogel reach as high as 1.20 ± 0.07MPa, and elongation strain is
1698 ± 119%, elasticity modulus 1.10MPa ± 0.08MPa.It is added after magnetic nano-particle, magnetic double-network hydrogel is still
Apparent yield phenomenon is shown, this is not available for many magnetic hydrogels.Tensile stress-strain curve institute in Fig. 2 b
The elasticity modulus of calculating statistics indicate that: Fe3O4Content from 0wt% to 2.5wt% when, modulus occurs first increasing becoming of successively decreasing again
Gesture, maximum modulus value is in Fe3O4Content reaches when being 1wt%, is 1.20 ± 0.07MPa, and subsequent modulus value tends towards stability, when
Fe3O4When content is 8wt%, modulus minimum is about 0.88MPa, due to Fe3O4Nano particle is rigid, so a small amount of receives
Rice grain content can effectively increase the modulus of MDN hydrogel.
Embodiment 2:Fe3O4The preparation of nano particle high intensity magnetic response double-network hydrogel
(1) 0.5g Fe is weighed3O4Nano particle is added in 20ml deionized water, and ultrasonic disperse obtains magnetic fluid, is added
0.005mol pectin and 0.005mol acrylamide, then by the photoinitiator 2- hydroxyl -4- of the 0.05mol% of raw material total amount
(2- hydroxy ethoxy) -2- methyl phenyl ketone (Irgacure 2959) and 0.01mol% (the 3% of AM molar concentration) crosslinking agent N,
N- methylene-bisacrylamide (MBA) is added thereto, and temperature is risen to 50 DEG C, obtains uniform solution after stirring 1h.
(2) acquired solution is vacuumized twice simultaneously, by filling N2Remove the O in solution2.Then solution is transferred to
In rectangular mould.It is 5W that mold, which is put in intensity, irradiates 1h under the ultraviolet lamp that wavelength is 365nm, it is mono- to form pectin/PAAm
Network (SN) hydrogel.
(3) then the mono- network aqueous gel of pectin/PAAm is soaked in the FeCl of 0.01M3In solution, 0.5h is impregnated, is made
Fe3+Ligand complex is carried out with carboxyl on pectin, finally obtains magnetic responsiveness, the high-intensitive double nets of dual network pectin/polyacrylamide
Network hydrogel.
Embodiment 3:Fe3O4The preparation of nano particle high intensity magnetic response double-network hydrogel
(1) Fe of 50g preparation is weighed3O4Nano particle is added in 2000ml deionized water, and ultrasonic disperse obtains magnetic current
0.5mol pectin and 5.5mol acrylamide is added, then by the photoinitiator 2- hydroxyl of 2mol% (the 1% of AM molar concentration) in body
Base -4- (2- hydroxy ethoxy) -2- methyl phenyl ketone (Irgacure 2959) and 0.1mol% (3% of AM molar concentration) crosslinking
Agent N, N- methylene-bisacrylamide (MBA) is added thereto, and temperature is risen to 80 DEG C, obtains uniform solution after stirring 2h.
(2) acquired solution is vacuumized twice simultaneously, by filling N2Remove the O in solution2.Then solution is transferred to
In rectangular mould.It is 10W that mold, which is put in intensity, irradiates 5h under the ultraviolet lamp that wavelength is 365nm, forms pectin/PAAm
Single network magnetic response hydrogel.
(3) then the mono- network aqueous gel of pectin/PAAm is soaked in the FeCl of 2M3In solution, 12h is impregnated, Fe is made3+With
- COO on pectin-Group carries out ligand complex, and it is double to finally obtain magnetic responsiveness, high-intensitive dual network pectin/polyacrylamide
Network aqueous gel.
Embodiment 4: it is based on Fe3O4Test of the high-intensitive magnetic responsiveness double-network hydrogel of nano particle as brake
MDN hydrogel is fabricated to cantilever beam flexure actuator, by observing the brake under the attraction of externally-applied magnetic field
Tilt displacement.As shown in figure 3, tilt displacement is defined as shift length when magnet is separated with MDN brake just.Fig. 4 a from
Left-to-right one is successively Fe3O4Answering property of magnetic, high-intensitive dual network when content is respectively 1wt%, 2.5wt%, 4wt%, 6wt%
Optical photograph when hydrogel is as cantilever beam flexure actuator；Fig. 4 b be successively from left to right under the action of externally-applied magnetic field,
Corresponding difference Fe3O4The magnetic response degree of the cantilever beam flexure actuator of content, the experimental results showed that, work as Fe3O4Content is gradually
When increasing, tilt displacement increases therewith, shows the trend of magnetic enhancement.
Claims (9)
1. a kind of high-intensitive double-network hydrogel with magnetic responsiveness；It is characterized in that by magnetic Fe3O4Nano particle and high intensity
Double-network hydrogel combines；Natural polysaccharide pectin as first network raw material, by and Fe3+It carries out ligand complex and forms the
One network, polyacrylamide are the second network, obtain high-intensitive double-network hydrogel；Magnetic Fe3O4Nano particle is introduced into polysaccharide
Base high intensity double-network hydrogel obtains the high-intensitive double-network hydrogel with magnetic responsiveness.
2. the preparation method of the high-intensitive double-network hydrogel with magnetic responsiveness of claim 1；It is characterized in that including as follows
Step:
(1) by Fe3O4Nano particle is added in ionized water, and ultrasonic disperse obtains magnetic fluid；By pectin and acrylamide molar ratio
It is dissolved in above-mentioned deionized water for 1:1~11, after mixing evenly, photoinitiator, crosslinking agent is then added, temperature is risen into 50-
80 DEG C, solution is obtained after stirring；
(2) step (1) acquired solution is vacuumized, and fills N2To remove the O in solution2；Solution is then transferred to mold
In, it is placed under ultraviolet lamp and irradiates, form pectin/polyacrylamide list network aqueous gel of magnetic responsiveness；
(3) pectin/polyacrylamide list network aqueous gel that step (2) obtains is soaked in FeCl3Magnetic responsiveness is obtained in solution
Fe3+The pectin of crosslinking/polyacrylamide DN hydrogel.
3. method according to claim 2, it is characterized in that pectin mass fraction is 1-30wt%, propylene in the step (1)
Amide concentration is 0.1-5wt% mixed solution.
4. method according to claim 2, it is characterized in that Fe3O4Nano particle is added to the Fe being configured in ionized water3O4It receives
Rice grain mass fraction is 1%-11wt%.
5. method according to claim 2, it is characterized in that photoinitiator is Iracure 2959, additional amount is pectin and propylene
The percentage of the sum of amide mole is 0.05-2mol%.
6. method according to claim 2, it is characterized in that crosslinking agent N, N- methylene-bisacrylamide, additional amount be pectin and
The percentage of the sum of acrylamide mole is 0.01-0.1mol%.
7. method according to claim 2, it is characterized in that being placed in irradiation condition under ultraviolet lamp in the step (2) is: intensity
For 5-10W, 1-5h is irradiated under the ultraviolet lamp that wavelength is 365nm.
8. method according to claim 2, it is characterized in that step (3) FeCl3Solution concentration is 0.01-2M, and soaking time is
0.5-12h。
9. the high-intensitive double-network hydrogel with magnetic responsiveness of claim 1 is as cantilever beam flexure actuator.
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| CN113248742A (en) * | 2021-06-15 | 2021-08-13 | 西华大学 | PH and light dual-response natural polysaccharide hydrogel and preparation method thereof |
| CN113480745A (en) * | 2021-04-16 | 2021-10-08 | 山东师范大学 | Super-stretching magnetic response self-repairing hydrogel and preparation method and application thereof |
| CN114133592A (en) * | 2020-09-04 | 2022-03-04 | 中国水产科学研究院 | Double-network hydrogel, double-network magnetic hydrogel and preparation method and application thereof |
| CN114213680A (en) * | 2021-12-30 | 2022-03-22 | 陕西科技大学 | Magnetic field/temperature dual-response hydrogel and preparation method and application thereof |
| CN115463622A (en) * | 2022-08-03 | 2022-12-13 | 广东纤友朵美生物科技有限公司 | Gel based on oxidized pectin and preparation method thereof |
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