CN108676121A - A kind of magnetism hemicellulose based aquagel - Google Patents
A kind of magnetism hemicellulose based aquagel Download PDFInfo
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- CN108676121A CN108676121A CN201810338454.8A CN201810338454A CN108676121A CN 108676121 A CN108676121 A CN 108676121A CN 201810338454 A CN201810338454 A CN 201810338454A CN 108676121 A CN108676121 A CN 108676121A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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Abstract
The present invention relates to a kind of preparation methods of magnetic high-molecular hydrogel, belong to hydrogel preparing technical field.A kind of magnetism hemicellulose based aquagel, to be modified hemicellulose, acrylic acid and MODIFIED Fe3O4For raw material, with H2O2Vc redox systems are initiator, are made by graft copolymerization under the action of crosslinking agent.The present invention is with nontoxic H2O2Vc redox systems are initiator, extract hemicellulose, ionizable acrylic acid with economic obsolescences objects such as oil tea shell, chestnut shell, chinquapin shell, walnut shell, pecan shells and with the Fe of magnetic field responsiveness3O4For raw material, hydrogel is prepared by graft copolymerization, the application field of hemicellulose has not only been expanded, but also the water absorbing properties and tensile strength of gel can be controlled by adjusting the amount of crosslinking agent and acrylic acid, has also substantially reduced the time of gel-forming.
Description
Technical field
The present invention relates to a kind of preparation methods of magnetic high-molecular hydrogel, belong to hydrogel preparing technical field.
Background technology
Magnetic natural polymer hydrogel is three-dimensional net structure, and magnetic hydrogel can show to stretch under magnetic fields
The various deformations such as long, contraction or bending, but gel network structure will not destroy, and magnetic gel is with its unique flexibility and infiltration
Property adsorb in targeted drug release, cell separation and label, protein and have a wide range of applications with detaching etc..With natural high
Molecule is the progress in Intelligent Hydrogel of Material synthesis because of good biocompatibility and to the sensibility of environmental stimuli, is cured in biology
The application in field is also more and more extensive.
Currently, the raw material for making hydrogel is mostly polymer chemistry ingredient, in face of scarcity of raw material, higher price or carry
The limitation of all many conditions such as toxicity, the type of hydrogel is less, and the field of application has limitation, limits the market of hydrogel
Development.Economic forest waste makees a kind of environmentally friendly, green, sustainable development biomass.It is currently used primarily in matrix, fertilizer etc. is low
Value application field, results in waste of resources.
The synthetic method of magnetic high-molecular hydrogel material can be divided into two classes, and one type investment is by magnetic Fe3O4Grain
Son is distributed to by the method for physical blending in the solution of high-molecular gel monomer, then reacts to form magnetic by high molecular crosslink
Property hydrogel.Another kind is in-situ synthesis, and it is molten that the macromolecule hydrogel material prepared is soaked in magnetic material presoma
In liquid, inorganic magnetic nano-particle is then formed in situ in hydrogel material by next step chemical reaction, though this method is right
The case where magnetism is unevenly distributed makes moderate progress.It is solidifying that these methods are all that the single method by magnetic particle physics is added to
It in glue, affects to the performance of gel itself, such as reduces its water imbibition, the tensile strength of gel.
Invention content
The purpose of the present invention is being directed to the above-mentioned problems in the prior art, provide a kind of water imbibition and tensile strength compared with
High magnetic hemicellulose based aquagel.
Object of the invention can be realized by the following technical scheme：A kind of magnetism hemicellulose based aquagel, it is described
Hydrogel is to be modified hemicellulose, acrylic acid and MODIFIED Fe3O4For raw material, with H2O2- Vc redox systems are initiator,
It is made by graft copolymerization under the action of crosslinking agent.
The present invention is with H2O2- Vc redox systems are initiator, and modified hemicellulose is made to form network knot with acrylic acid
Structure, and will have magnetic MODIFIED Fe3O4Doping in the network architecture, forms and has magnetic gel, and then improve the suction of gel
Aqueous and tensile strength, while greatly shortening the time of plastic.
Preferably, the method for graft copolymerization includes the following steps：
Modified hemicellulose is substantially dissolved in distilled water, modified hemicellulose solution is obtained；
Vitamin C is weighed in reaction vessel, hydrogen peroxide is added, then modified hemicellulose solution is added thereto, fills
MODIFIED Fe is added after dividing mixing3O4Particle is added acrylic acid, then hot water soluble crosslinking agent is added thereto after being sufficiently mixed, stir
It mixes to solution temperature and increases, stop stirring, stand form gel at room temperature；
It takes out gel to be impregnated with deionized water at room temperature, removes unreacted reagent, finally freeze-drying obtains water-setting
Glue.
Further preferably, the addition of acrylic acid is 2.5-10ml in every gram of modified hemicellulose.Although acrylic acid is added
Hydroxy radical content can be increased, and then increase net charge density and electrostatic repulsion, but the increase of acrylic acid dosage also improves
The network density of hydrogel limits the expansion of network, reduces the swelling ratio of hydrogel.
Further preferably, MODIFIED Fe3O4The mass ratio of particle and modified hemicellulose is (0.3-0.6):1.It is added and is modified
Fe3O4Particle can make Fe3O4Particle is complexed together well with hemicellulose, while hydrogel being made to have magnetism, if being added
Fe3O4Particle is non-modified, then material dispersion is uneven, cannot be merged well, and has been easy sediment precipitation.
And if MODIFIED Fe3O4The amount that particle is added is very little, and hydrogel magnetic property is small, and MODIFIED Fe3O4The too big complexing of the amount that particle is added is anti-
Should be incomplete, ferroso-ferric oxide can be caused to be unevenly distributed in hydrogel, and then influence swelling and magnetic behavior and appearance.
Further preferably, the addition of crosslinking agent is 0.05-0.2g in every gram of modified hemicellulose, and the crosslinking agent is
N, N '-methylene-bisacrylamide.Swelling ratio is one of the important parameter for characterizing hydrogel performance, a large amount of micropores in hydrogel
So that hydrone is very easy to spread and adsorb in hydrogel, the moisture more much bigger than own wt can be stored.In aqueous solution
In, negatively charged COO- make hydrogel network generate electrostatic repulsion cause structure expand and so that hydrogel have it is very high molten
Swollen rate.Crosslinking agent plays an important role in hydrogel three-dimensional network structure, and dosage of crosslinking agent is very little, the crosslink density of product
It is low, good three-dimensional structure cannot be formed, the water-soluble of hydrogel increases, and is easily deformed and ineffective；The dosage of crosslinking agent
When excessive, the three-dimensional structure crosslink density of hydrogel is excessively high, reduces the network swelling behavior of hydrogel, limits the suction of hydrogel
Water-swellable rate.
Further preferably, the mass ratio of vitamin C and modified hemicellulose is (0.08-0.2):1.
Further preferably, 5-20mL hydrogen peroxide is added in every gram of vitamin C.Vitamin C is unified into oxygen with hydrogen peroxide
Change reduction system, redox system generates Atomic oxygen radical anion, and Atomic oxygen radical anion causes on hemicellulose derivative
Double bond.
Further preferably, the hydrogel is impregnated 1-3 days with deionized water, is freeze-dried 12-48h.
Preferably, the modification hemicellulose is made by acrylated modification.
Further preferably, modified hemicellulose is especially by following method acylation modification：Hemicellulose is completely dissolved in
Then distilled water is added N, N- dimethylformamides, and carries out magnetic agitation, then revolving remove moisture, finally into solution according to
Secondary addition LiCl, 4-dimethylaminopyridine, N, N- dimethylformamides and acryloyl chloride, react 30-60min at 50-90 DEG C, cold
But precipitated in ethanol after, wash discoloration repeatedly with ethyl alcohol and acetone when filtering, be dried to obtain it is acrylated after modification half fiber
Dimension element.
The present invention is transformed into the lower ester group of hydrophily by hemicellulose acryloyl chloride acylation modification, by hydrophilic hydroxyl groups.
The hemicellulose for being dissolved in water is not dissolved in water by modified, but is formed gluey.
Further preferably, in every gram of hemicellulose LiCl addition be 0.1-0.2g, 4-dimethylaminopyridine addition
Amount is 0.02-0.05g, the addition of acryloyl chloride is 2.5-5mL.
Further preferably, the time of magnetic agitation is 60-120min.
Further preferably, the hemicellulose is the warp extracted from oil tea shell, chestnut shell, chinquapin shell, walnut shell
Help woods waste base hemicellulose.
Preferably, the MODIFIED Fe3O4It is modified by the following method by vinyltriethoxysilane (A151) and
At：By Fe3O4Particle ultrasonic disperse in a dispersion medium, is slow added into vinyltriethoxysilane (A151), cold after reaction
But, it is washed repeatedly with ethyl alcohol and distilled water, is freeze-dried after magnet separation, obtains the Fe of surface modification3O4Particle.
Further preferably, every gram of Fe3O4The addition of particle medium vinyl triethoxysilane is 2-5mL.
Further preferably, the decentralized medium be second alcohol and water by volume (1-3):1 mixed liquor.
Compared with prior art, the present invention is with nontoxic H2O2- Vc redox systems are initiator, with oil tea shell, Chinese chestnut
The economic obsolescences objects such as shell, chinquapin shell, walnut shell, pecan shell extract hemicellulose, ionizable acrylic acid and have magnetic field
The Fe of response3O4For raw material, hydrogel is prepared by graft copolymerization, has not only expanded the application field of hemicellulose, Er Qieke
To control the water absorbing properties and tensile strength of gel by adjusting the amount of crosslinking agent and acrylic acid, gel-forming is also substantially reduced
Time.
Specific implementation mode
The following is specific embodiments of the present invention, illustrates that technical scheme of the present invention will be further described, but this hair
It is bright to be not limited to these examples.
Embodiment 1
The oil tea shell powder of 50g grindings first uses toluene-ethano (2:1, v/v) it is extracted 6 hours in Soxhlet extractor；It will be without pumping
(75 DEG C) extracting 2h removing water-soluble hemicelluloses in 1000mL water are added in the sample for going out object.Residual substance uses sodium chlorite solution
(5g is dissolved in 500mL water) handles 2 hours (adjusting PH=3.8 with acetic acid) at 75 DEG C and obtains holocellulose.It is 1 in solid-to-liquid ratio:
With 10%KOH extracting holocellulose 10h (23 DEG C) under conditions of 20 (g/mL), obtained filtrate is adjusted into PH with 6mol/L acetic acid
Value, then with 95% ethanol precipitation of 3 times of volumes, filtering, is finally washed with 70% ethyl alcohol of acidification, is air-dried to 5.5
16h is dried after 12h at 60 DEG C, obtains hemicellulose sample.
It weighs 0.66g hemicelluloses to be substantially dissolved in 10mL distilled water, 50 DEG C of magnetic stirring apparatus is heated in cucurbit
It is added 20mLDMF after 5min, after magnetic agitation 10min, rotary evaporation removes distilled water (65 DEG C of 20~30min of revolving), cooling,
0.1g LiCl, 0.033g DMAP, 15mL DMF and 2.437mL acryloyl chlorides is added into solution again, after 70 DEG C are reacted 40min
It is cooled to room temperature, is precipitated in the ethanol solution of 3 times of volumes, when filtering is washed repeatedly with discoloration, so repeatedly with ethyl alcohol and acetone
The dry 12h in 50 DEG C of baking ovens afterwards, obtain it is acrylated after modification hemicellulose.
By 0.2g Fe3O4Particle ultrasonic wave is dispersed in 30mL decentralized media (mixed liquor of 20mL ethyl alcohol and 10mL water)
10min is then moved into three-necked flask, the mechanical agitation in 50 DEG C of water-baths, is slow added into 0.8mL vinyl triethoxyl silicon
Alkane (A151) reacts 7h postcoolings, is washed repeatedly with ethyl alcohol and distilled water, is freeze-dried after magnet separation, obtains surface modification
Fe3O4Particle.
0.2g modification hemicelluloses are substantially dissolved in 9ml distilled water, modified hemicellulose solution is obtained；Weigh 0.02g
In reaction vessel 0.2mL hydrogen peroxide is added, then modified hemicellulose solution is added thereto, after being sufficiently mixed in vitamin C
0.1g MODIFIED Fes are added3O4Particle is added 1mL acrylic acid, then it is added in hot water soluble 0.01g crosslinking agents after being sufficiently mixed
In, stirring to solution temperature increases, and stops stirring, stands form gel at room temperature；It takes out gel and uses deionized water at room temperature
It impregnates 2 days, removes unreacted reagent, be finally freeze-dried 15h and obtain hydrogel.
Embodiment 2
With differing only in for embodiment 1, in graft copolymerization 0.02g crosslinking agents being added in the embodiment 2, (i.e. every gram changes
Property hemicellulose in crosslinking agent addition be 0.1g), other are same as Example 1, are not repeated herein.
Embodiment 3
With differing only in for embodiment 1, in graft copolymerization 0.03g crosslinking agents being added in the embodiment 3, (i.e. every gram changes
Property hemicellulose in crosslinking agent addition be 0.15g), other are same as Example 1, are not repeated herein.
Embodiment 4
With differing only in for embodiment 1, in graft copolymerization 0.04g crosslinking agents being added in the embodiment 4, (i.e. every gram changes
Property hemicellulose in crosslinking agent addition be 0.2g), other are same as Example 1, are not repeated herein.
Embodiment 5
With differing only in for embodiment 2, in the embodiment 5 in graft copolymerization the addition of acrylic acid be 0.5mL (i.e.
The addition of acrylic acid is 2.5mL in every gram of modified hemicellulose, and acrylic acid adds in every gram of modified hemicellulose in embodiment 2
It is 5mL to enter amount), other are same as Example 2, are not repeated herein.
Embodiment 6
With differing only in for embodiment 2, in the embodiment 6 in graft copolymerization the addition of acrylic acid be 1.5mL (i.e.
The addition of acrylic acid is 7.5mL in every gram of modified hemicellulose), other are same as Example 2, are not repeated herein.
Embodiment 7
With differing only in for embodiment 2, in the embodiment 7 in graft copolymerization the addition of acrylic acid be 2mL (i.e. often
The addition of acrylic acid is 10mL in gram modified hemicellulose), other are same as Example 2, are not repeated herein.
Embodiment 8
With differing only in for embodiment 2, which is added 0.08g MODIFIED Fes in graft copolymerization3O4Particle (changes
Property Fe3O4The mass ratio of particle and modified hemicellulose is 0.4:1, MODIFIED Fe in embodiment 23O4Particle and modified hemicellulose
Mass ratio be 0.5：1), other are same as Example 2, are not repeated herein.
Embodiment 9
With differing only in for embodiment 2, which is added 0.06g MODIFIED Fes in graft copolymerization3O4Particle (changes
Property Fe3O4The mass ratio of particle and modified hemicellulose is 0.3:1), other are same as Example 2, are not repeated herein.
Embodiment 10
With differing only in for embodiment 2, which is added 0.12g MODIFIED Fes in graft copolymerization3O4Particle is (i.e.
MODIFIED Fe3O4The mass ratio of particle and modified hemicellulose is 0.6:1), other are same as Example 2, are not repeated herein.
Embodiment 11
With differing only in for embodiment 2, which is added 0.016g vitamin Cs in graft copolymerization, (i.e. dimension life
The mass ratio of plain C and modified hemicellulose is 0.08:1), other are same as Example 2, are not repeated herein.
Embodiment 12
With differing only in for embodiment 2, which is added 0.04g vitamin Cs in graft copolymerization, (i.e. dimension life
The mass ratio of plain C and modified hemicellulose is 0.2:1), other are same as Example 2, are not repeated herein.
Embodiment 13
With differing only in for embodiment 2, the addition of hydrogen peroxide is 0.1mL in graft copolymerization in the embodiment 13
(i.e. the addition of hydrogen peroxide is 5mL in every gram of vitamin C), other are same as Example 2, are not repeated herein.
Embodiment 14
With differing only in for embodiment 2, the addition of hydrogen peroxide is 0.4mL in graft copolymerization in the embodiment 14
(i.e. the addition of hydrogen peroxide is 20mL in every gram of vitamin C), other are same as Example 2, are not repeated herein.
Comparative example 1
With differing only in for embodiment 2, which is added (the i.e. every gram of modification of 0.05g crosslinking agents in graft copolymerization
The addition of crosslinking agent is 0.25g in hemicellulose), other are same as Example 2, are not repeated herein.
Comparative example 2
With differing only in for embodiment 2, in the comparative example 2 in graft copolymerization the addition of acrylic acid be 3mL (i.e. often
The addition of acrylic acid is 15mL in gram modified hemicellulose), other are same as Example 2, are not repeated herein.
Comparative example 3
With differing only in for embodiment 2, in the comparative example 3 in graft copolymerization MODIFIED Fe3O4The addition of particle is
0.04g (i.e. MODIFIED Fes3O4The mass ratio of particle and modified hemicellulose is 0.2:1), other are same as Example 2, herein no longer
It is tired to state.
Comparative example 4
With differing only in for embodiment 2, in the comparative example 4 in graft copolymerization MODIFIED Fe3O4The addition of particle is
0.14g (i.e. MODIFIED Fes3O4The mass ratio of particle and modified hemicellulose is 0.7:1), other are same as Example 2, herein no longer
It is tired to state.
Comparative example 5
With differing only in for embodiment 2, ascorbic addition is 0.012g in graft copolymerization in the comparative example 5
(i.e. the mass ratio of vitamin C and modified hemicellulose is 0.06:1), other are same as Example 2, are not repeated herein.
Comparative example 6
With differing only in for embodiment 2, ascorbic addition is 0.05g in graft copolymerization in the comparative example 6
(i.e. the mass ratio of vitamin C and modified hemicellulose is 0.25:1), other are same as Example 2, are not repeated herein.
Comparative example 7
With differing only in for embodiment 2, the addition of hydrogen peroxide is 0.06mL in graft copolymerization in the comparative example 7
(i.e. the addition of hydrogen peroxide is 3mL in every gram of vitamin C), other are same as Example 2, are not repeated herein.
Comparative example 8
With differing only in for embodiment 2, the addition of hydrogen peroxide is 0.5mL in graft copolymerization in the comparative example 8
(i.e. the addition of hydrogen peroxide is 25mL in every gram of vitamin C), other are same as Example 2, are not repeated herein.
Comparative example 9
With differing only in for embodiment 2, the non-modified processing of hemicellulose in the comparative example 7.
Comparative example 10
With differing only in for embodiment 2, the Fe in the comparative example 83O4The non-modified processing of particle.However the comparative example
In material dispersion it is uneven, cannot be merged well, and be easy sediment precipitation.
Comparative example 11
It, will modified hemicellulose, acrylic acid, MODIFIED Fe in the comparative example 9 with differing only in for embodiment 23O4Particle one
Secondary property, which is added in reaction vessel, to be mixed.However the comparative example can not react, and cannot generate hydrogel.
Comparative example 12
The first step：By MODIFIED Fe3O4Particle is first dissolved in acrylic acid solution, is uniformly dispersed under ultrasonication；Second step：It will change
Property after hemicellulose be dissolved in distilled water, vitamin C and the initiation reaction of hydrogen peroxide elder generation is added in another rise；After finally causing
Hemicellulose solution be added in acrylic acid mixed solution, be stirring evenly and then adding into crosslinking agent, after it can not stir water
Gel.Table 1：Condition in embodiment 1-14 and comparative example 1-12 graft copolymerizations
Sample parallel determination in Example 1 and embodiment 2 is averaged three times, obtains embodiment 1 and embodiment 2 is made
Fe contents are respectively 180 μ g/mL and 140 μ g/mL in the hydrogel sample obtained, illustrate that the addition of crosslinking agent can be with follow-up magnetism
The complexing effect of ferroso-ferric oxide generates negative interaction.
Hydrogel sample obtained carries out swelling behavior test in Example 1-14 and comparative example 1-11, hydrogel it is molten
Swollen performance test：
The swelling ratio of hydrogel is measured using weight method, and it is 20 DEG C to survey fixed time temperature.Dry hydrogel sample is placed in
In deionized water, weigh after certain time takes out and removes the moisture of excess surface with filter paper.Each embodiment or comparative example
In sample parallel determination three times, be averaged.The calculating of swelling ratio Qeq is as follows：
Qeq=(meq-m0)/m0
In formula, m0 is the quality (g) of dried hydrogel, and meq is quality (g) of the hydrogel in different time.
Swelling behavior of the hydrogel sample obtained in 48h is as shown in table 2 in embodiment 1-14 and comparative example 1-11.
Table 2：Swelling behavior and magnetic effect of the hydrogel sample in 48h in embodiment 1-14 and comparative example 1-11
(saturation magnetization/emu g-1)
It in embodiments of the present invention can be from economic obsolescences such as oil tea shell, chestnut shell, chinquapin shell, walnut shell, pecan shells
Object extracts hemicellulose.
50min can also be reacted at 60 DEG C in hemicellulose acylation modification in embodiments of the present invention, it can also be 50
60min is reacted at DEG C, can also react 30min at 90 DEG C, can also react 35min at 80 DEG C, you can at 50-90 DEG C
Between random time in reaction 30-60min at any temperature.The addition of LiCl can be 0.1- in every gram of hemicellulose simultaneously
Arbitrary value in 0.2g, such as 0.12g, 0.15g, 0.18g, 0.2g；The addition of 4-dimethylaminopyridine can be 0.02-
Arbitrary value in 0.05g, such as 0.02g, 0.03g, 0.04g, 0.05g；The addition of acryloyl chloride can be in 2.5-5mL
Arbitrary value, such as 2.5mL, 3mL, 3.5mL, 4mL, 5mL.
Fe in embodiments of the present invention3O4Modifying process in every gram of Fe3O4Particle medium vinyl triethoxysilane adds
It can be the arbitrary value in 2-5mL, such as 2mL, 3mL, 4mL, 5mL to enter amount；Decentralized medium can be that ethyl alcohol presses volume with water
Than (1-3):The mixed liquor of 1 arbitrary ratio, such as 1：1、2：1、3：1 etc..
In conclusion the present invention is with nontoxic H2O2- Vc redox systems are initiator, with oil tea shell, chestnut shell, cone
The economic obsolescences object such as chestnut shell, walnut shell, pecan shell extracts hemicellulose, ionizable acrylic acid and has magnetic field responsiveness
Fe3O4For raw material, hydrogel is prepared by graft copolymerization, has not only expanded the application field of hemicellulose, but also can pass through
The water absorbing properties and tensile strength for adjusting the amount control gel of crosslinking agent and acrylic acid, also substantially reduce gel-forming when
Between.
This place embodiment is in place of the claimed non-limit of technical scope midrange and in embodiment technology
In scheme to single or multiple technical characteristics it is same replacement be formed by new technical solution, equally all the present invention claims
In the range of protection, and between the parameter that is related to of the present invention program if not otherwise specified, then there is no can not between each other
The unique combinations of replacement.
Specific embodiment described herein is only an example for the spirit of the invention.Technology belonging to the present invention is led
The technical staff in domain can do various modifications or supplement to described specific embodiment or substitute by a similar method, but simultaneously
The spirit or beyond the scope defined by the appended claims of the present invention is not deviated by.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious that can make various changes or correct without departing from the spirit and scope of the present invention.
Claims (10)
1. a kind of magnetism hemicellulose based aquagel, which is characterized in that the hydrogel be modified hemicellulose, acrylic acid and
MODIFIED Fe3O4For raw material, with H2O2- Vc redox systems are initiator, pass through graft copolymerization system under the action of crosslinking agent
.
2. magnetism hemicellulose based aquagel according to claim 1, which is characterized in that the method for graft copolymerization includes such as
Lower step：
Modified hemicellulose is substantially dissolved in distilled water, modified hemicellulose solution is obtained；
Vitamin C is weighed in reaction vessel, hydrogen peroxide is added, then modified hemicellulose solution is added thereto, it is fully mixed
MODIFIED Fe is added after conjunction3O4Particle is added acrylic acid, then hot water soluble crosslinking agent is added thereto after being sufficiently mixed, stirring is extremely
Solution temperature increases, and stops stirring, stands form gel at room temperature；
It takes out gel to be impregnated with deionized water at room temperature, removes unreacted reagent, finally freeze-drying obtains hydrogel.
3. magnetism hemicellulose based aquagel according to claim 1 or 2, which is characterized in that every gram of modified hemicellulose
The addition of middle acrylic acid is 2.5-10mL.
4. magnetism hemicellulose based aquagel according to claim 1 or 2, which is characterized in that MODIFIED Fe3O4Particle with change
Property hemicellulose mass ratio be (0.3-0.6):1.
5. magnetism hemicellulose based aquagel according to claim 1 or 2, which is characterized in that every gram of modified hemicellulose
The addition of middle crosslinking agent is 0.05-0.2g, and the crosslinking agent is N, N '-methylene-bisacrylamides.
6. magnetism hemicellulose based aquagel according to claim 2, which is characterized in that vitamin C and modified hemicellulose
The mass ratio of element is (0.08-0.2):1.
7. magnetism hemicellulose based aquagel according to claim 1 or 2, which is characterized in that the modification hemicellulose
Element is made by acrylated modification：
Modified hemicellulose is especially by following method acylation modification：Hemicellulose is completely dissolved in distilled water, is then added
N, N- dimethylformamide, and magnetic agitation is carried out, then revolving removes moisture, and LiCl, 4- bis- is finally sequentially added into solution
Methylamino pyridine, N, N- dimethylformamides and acryloyl chloride react 30-60min at 50-90 DEG C, sink in ethanol after cooling
Form sediment, wash discoloration repeatedly with ethyl alcohol and acetone when filtering, be dried to obtain it is acrylated after modification hemicellulose.
8. magnetism hemicellulose based aquagel according to claim 7, which is characterized in that LiCl in every gram of hemicellulose
Addition is 0.1-0.2g, the addition of 4-dimethylaminopyridine is 0.02-0.05g, the addition of acryloyl chloride is 2.5-
5mL。
9. magnetism hemicellulose based aquagel according to claim 1 or 2, which is characterized in that the MODIFIED Fe3O4By
Modification forms vinyltriethoxysilane by the following method：By Fe3O4Particle ultrasonic disperse in a dispersion medium, then slowly
Vinyltriethoxysilane is added, reacts postcooling, is washed repeatedly with ethyl alcohol and distilled water, is freeze-dried after magnet separation,
Obtain the Fe of surface modification3O4Particle.
10. magnetism hemicellulose based aquagel according to claim 1 or 2, which is characterized in that every gram of Fe3O4Second in particle
The addition of alkenyl triethoxysilane is 2-5mL.
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