CN106117402A - High-performance magnetorheological nano composite polymeric gel process for preparing - Google Patents
High-performance magnetorheological nano composite polymeric gel process for preparing Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/52—Amides or imides
- C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F120/56—Acrylamide; Methacrylamide
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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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
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- C08K3/34—Silicon-containing compounds
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
- C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
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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
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C08K2201/00—Specific properties of additives
- C08K2201/01—Magnetic additives
Abstract
The present invention relates to magnetorheological materials technical field, specially high-performance magnetorheological nano composite polymeric gel process for preparing, solve the problem that existing gel dispersion, poor stability, mechanical performance and magnetorheological performance cannot improve simultaneously, scheme is: FeCl2•4H2O、FeCl3•6H2O, surfactant are dissolved in water；Adding NaOH, Magneto separate ultrasonic disperse, in dispersion deionized water；Hectorite is added in deionized water, adds high polymer monomer；Add initiator and catalyst, add dispersion liquid；Evacuation, seals reaction.Advantage: 1, magnetic nanoparticle does not settles, the interaction force between magnetic particle and gelatin polymer matrix increases, improves stability and dispersibility；2, forming three-dimensional crosslinked network structure, loading is big, controllability is more preferable；3, mechanical property and magnetorheological performance are held concurrently excellent, and hot strength, elongation at break, magnetic rheology effect, relative magnetic rheology effect are high.
Description
Technical field
The present invention relates to magnetorheological materials technical field, specially high-performance magnetorheological nano composite polymeric gel prepare
Method.
Background technology
Magnetorheological materials is a class new function material, is magnetized under internal magnetization granule outside magnetic field, produces phase interaction
Firmly, when material is by deformation, these magnetic force form opposing torque therein, cause magnetorheological materials to produce modulus and resistance
The change of the mechanics parameters such as Buddhist nun, this effect is referred to as magnetic rheology effect, has continuous field controllable, magnetic response speed fast, reversible
Property the characteristic such as good, be all with a wide range of applications in fields such as Aero-Space, information, machineries.Magnetorheological materials is main at present
There is a three types: (1) magnetic flow liquid, (2) magnetic rheology elastic body, (3) magnetorheological high-molecular gel.Magnetic flow liquid is to occur the earliest
Magnetorheological materials (1948), be made up of liquid and magnetic particle, under the action of a magnetic field, yield stress and apparent viscosity occur
Notable change, has higher magnetic rheology effect (> 300.0%), it is applied in intelligent damping noise reduction field, but, magnetic current
Become liquid and there is the problem such as magnetic particle free settling, stability difference, significantly limit improving further and large area of its performance
Popularization and application.Magnetic rheology elastic body is a kind of New Materials On Magnetorheological Fluids grown up the nineties in 20th century, mainly by elasticity
Body forms with magnetic particle, and magnetic particle is fixed by elastomer, thus there is not the problem of magnetic particle sedimentation, but, magnetic
Property particle be difficult to reset under the action of a magnetic field, thus magnetic rheology effect relatively low (< 300.0%), significantly limiting its through engineering approaches should
With.Magnetorheological high-molecular gel concept is to be proposed first by Nevada ,Usa university professor Gordaninejad at the beginning of 21 century, lotus
Langdell volt Polytechnics Memdes professor further confirms that for 2010, magnetorheological high-molecular gel be between magnetic flow liquid and
A class New Materials On Magnetorheological Fluids between magnetic rheology elastic body, magnetic particle not free settling, and have higher magnetic rheology effect
(ca. 6000.0%).This characteristic is mainly attributed to the three-dimensional crosslinked network knot constructed by macromolecule, liquid and magnetic particle etc.
Structure, wherein three-dimensional crosslink polymer network is that magnetic particle stability provides safeguard, and is present in liquid in crosslink polymer network
Resistance is little, and occurring to reset under the action of a magnetic field for magnetic particle provides environment.
But, existing magnetorheological high-molecular gel, in order to realize high magnetorheological performance, often by simple at magnetic current
Uprise and molecular gel matrix is filled a large amount of magnetic particle, but, the introducing of a large amount of magnetic particles necessarily causes high-molecular gel
Mechanical performance, dispersibility, stability significantly declines.These problems greatly limit the through engineering approaches of magnetorheological high-molecular gel
Application.Therefore, the magnetorheological nano combined high score that a kind of dispersibility, good stability, magnetorheological performance and mechanical performance are high is studied
Sub-gel process for preparing is necessary.
Summary of the invention
The present invention solves existing magnetorheological high-molecular gel dispersibility, poor stability, mechanical performance and magnetorheological performance
The problem that cannot simultaneously improve, it is provided that the magnetorheological nanometer that a kind of dispersibility, good stability, magnetorheological performance and mechanical performance are high
Composite high-molecular gel process for preparing.
The present invention is realized by following operating procedure: magnetorheological nano composite polymeric gel process for preparing, including
Following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By a certain amount of FeCl2•4H2O、FeCl3•6H2O and a certain amount of surfactant are dissolved in a certain amount of deionized water,
Described FeCl2•4H2O、 FeCl3•6H2The consumption of O should ensure that Fe2+Salt and Fe3+The mol ratio of salt is 1:1.2 ~ 1:1.5；Described table
Face activating agent be dopamine hydrochloride, ethylenediaminetetraacetic acid, polyvinyl alcohol, polyacrylic acid, polyacrylamide, polyacrylic acid, poly-third
One in acrylamide copolymer, polyvinylpyrrolidone, KH550, KH560, KH570, dosage of surfactant is Fe2+Salt with
Fe3+0.5 ~ 2.5wt% of salt gross mass；The consumption of described deionized water should ensure that Fe2+Salt and Fe3+Saline solution total concentration scope
For 5.0wt% ~ 15.0wt%；After at the mechanical agitation that speed is 500r/min and 50.0 DEG C, stirring and dissolving is uniform, with 1 drop/sec
Speed be slowly added dropwise the NaOH solution that a certain amount of concentration is 1.5mol/L, continue reaction 90min afterwards, formed stable
Black dispersion liquid, the consumption of described NaOH solution should ensure that NaOH solution and Fe2+Salt and Fe3+Saline solution volume ratio is 1:1；
Magnetic separation method is used to isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, again stable black dispersion liquid
It is distributed in a certain amount of deionized water, prepares Fe3O4Magnetic nanoparticle stable dispersions, the consumption of described deionized water should
Ensure Fe3O4The mass concentration of magnetic nanoparticle stable dispersions is 2.0% ~ 6.0%；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 1.0%-15.0% of ionized water quality；Stirring, to forming transparent aqueous solution, adds gross mass for going
The acrylamide (AM) of ionized water quality 8.0% ~ 15.0%；Or 2-acrylamide-2 methyl propane sulfonic acid (AMPS) and acrylic acid
(AA)；Or acrylamide and acrylic acid；Or acrylamide and 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid, three of the above thing
Matter is referred to as high polymer monomer, and described acrylic acid, acrylamide, the mol ratio of 2-acrylamide-2 methyl propane sulfonic acid three be 3 ~
10:0 ~ 2.971:0 ~ 0.274；Under the conditions of 0 ~ 5.0 DEG C, continue stirring and dissolving complete, form the aqueous solution of clear homogeneous；Add
The initiator ammonium sulfate (APS) of high polymer monomer gross mass 1.0 ~ 2.0% and urging of high polymer monomer gross mass 0.05% ~ 0.35%
Agent N, N, N ', N '-tetramethylethylenediamine (TEMED), at N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding one
The Fe that quantitative step 1) prepares3O4Magnetic nanoparticle stable dispersions, is uniformly mixed and obtains Gel Precursor, adds
Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality account for water, hectorite and high polymer monomer raw material gross mass
0.1%-10.0%；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 0 ~ 5.0 DEG C, evacuation 30min, seals outlet,
Under the conditions of sealed environment and 40.0 DEG C, react 24h, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
It is various different that described magnetorheological nano composite polymeric gel can be prepared as including film, block, column
Shape.It is prepared as multiple difformity, is applicable to various uses.
The invention have the advantages that 1, use Fe3O4Magnetic nanoparticle substitutes traditional micron order carbon-based iron or ferromagnetism
Particle, and use surfactant to Fe3O4Magnetic nanoparticle modifying surface, not only makes Fe3O4Magnetic nanoparticle
In position polymerization process does not settles, and add Fe3O4Phase interaction between magnetic nanoparticle with gelatin polymer matrix
Firmly, improve Fe3O4Magnetic nanoparticle stability in high-molecular gel and dispersibility；2, replaced by situ aggregation method
Prepare magnetorheological high-molecular gel for blending method, form three-dimensional crosslinked network structure, and Fe3O4The loading of magnetic nanoparticle
More preferable with three-dimensional net structure controllability；3, using hectorite as the physical crosslinking agent of formation polymer three-dimensional network structure, high
Molecule monomer as polymer monomers, is prepared mechanical property by in-situ polymerization and magnetorheological performance is held concurrently excellent magnetorheological macromolecule
Nano composite polymeric gel, the most remote super existing skill of hot strength, elongation at break, magnetic rheology effect, relative magnetic rheology effect
Art level, is the peak of the most magnetorheological high-molecular gel properties.
Accompanying drawing explanation
Fig. 1 is the pictorial diagram after January prepared by nano composite polymeric gel prepared by the present invention；Figure is had to can be seen that this
Still stable homogeneous after nano composite polymeric gel January, illustrates that nano composite polymeric gel prepared by the present invention has relatively
Good dispersibility and stability；
Fig. 2 is the SEM figure of nano composite polymeric gel arbitrarily local prepared by the present invention；By in figure it may be clearly seen that nanometer
Composite high-molecular gel has three-dimensional crosslinked network structure；
Fig. 3 is the VSM figure of nano composite polymeric gel prepared by the present invention；The nano combined height that as seen from the figure prepared by the present invention
Molecular gel magnetic saturation intensity is up to 19.10emu/g；
Fig. 4 is the stress-strain diagram of nano composite polymeric gel prepared by the present invention；What as seen from the figure prepared by the present invention receives
The hot strength of rice composite high-molecular gel is up to 75.0kPa；
Fig. 5 is that storage modulus (a) absolute value of nano composite polymeric gel prepared by the present invention is along with changes of magnetic field curve；By
Figure understands, and the absolute magnetic rheological effect of nano composite polymeric gel prepared by the present invention is 4.8Mpa；
Fig. 6 is that storage modulus (b) relative value of nano composite polymeric gel prepared by the present invention is along with changes of magnetic field curve；By
Figure understands, and the relative magnetic rheology effect of nano composite polymeric gel prepared by the present invention is 7000%.
Detailed description of the invention
Embodiment one: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By the FeCl of 3.58g2•4H2The FeCl of O, 6.08g3•6H2O and Fe2+Salt and Fe3+Live in the surface of the 0.5wt% of salt gross mass
Property agent dopamine hydrochloride is dissolved in the deionized water of 90ml；Stir molten at the mechanical agitation that speed is 500r/min and 50.0 DEG C
After solving uniformly, it is slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is 1:1, concentration is 1.5mol/L
NaOH solution, afterwards continue reaction 90min, form stable black dispersion liquid；Magnetic is used to divide stable black dispersion liquid
Isolate magnetic-particle, ultrasonic disperse, then Magneto separate from method, after being repeated 3 times, be re-dispersed into shape in a certain amount of deionized water
Become Fe3O4Magnetic nanoparticle mass concentration is the Fe of 3.0%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 1.0% of ionized water quality；Stirring, to forming transparent aqueous solution, adds deionized water quality 9.5%
Acrylamide (AM)；Under the conditions of 2 DEG C, continue stirring and dissolving complete, form the aqueous solution of clear homogeneous；Add acrylamide
The initiator ammonium sulfate (APS) of gross mass 2.0% and the catalyst n of acrylamide quality 0.2%, N, N ', N '-tetramethylethylenediamine
(TEMED), at N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding the Fe that a certain amount of step 1) prepares3O4Nanometer
Magnetic particle stable dispersions, is uniformly mixed and obtains Gel Precursor, adds Fe3O4Magnetic nanoparticle stable dispersions
Middle Fe3O4Quality account for water, hectorite and the 5% of acrylamide quality；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 5 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment two: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By the FeCl of 3.58g2•4H2The FeCl of O, 7.3g3•6H2O and Fe2+Salt and Fe3+The surface activity of the 2wt% of salt gross mass
Agent ethylenediaminetetraacetic acid is dissolved in the deionized water of 90ml；Stir molten at the mechanical agitation that speed is 500r/min and 50.0 DEG C
After solving uniformly, it is slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is 1:1, concentration is 1.5mol/L
NaOH solution, afterwards continue reaction 90min, form stable black dispersion liquid；Magnetic is used to divide stable black dispersion liquid
Isolate magnetic-particle, ultrasonic disperse, then Magneto separate from method, after being repeated 3 times, be re-dispersed into shape in a certain amount of deionized water
Become Fe3O4Magnetic nanoparticle mass concentration is the Fe of 2%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 2.5% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
The 2-acrylamide-2 methyl propane sulfonic acid (AMPS) of quality 11% and acrylic acid (AA), described 2-acrylamide-2 methyl propane sulfonic acid
It is that 0.001:6(2-acrylamide-2 methyl propane sulfonic acid value levels off to 0 but is not 0 with acrylic acid mol ratio)；0 DEG C of condition
Lower continuation stirring and dissolving is complete, forms the aqueous solution of clear homogeneous；Add 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid is total
The initiator ammonium sulfate (APS) of quality 1.0% and 2-acrylamide-2 methyl propane sulfonic acid and the catalysis of acrylic acid gross mass 0.25%
Agent N, N, N ', N '-tetramethylethylenediamine (TEMED), at N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding certain
The Fe that the step 1) of amount prepares3O4Magnetic nanoparticle stable dispersions, is uniformly mixed and obtains Gel Precursor, adds
Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality account for water, hectorite and 2-acrylamide-2 methyl propane sulfonic acid and
The 8.5% of acrylic acid gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 0 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment three: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By the FeCl of 3.58g2•4H2The FeCl of O, 7.3g3•6H2O and Fe2+Salt and Fe3+The surface activity of the 2wt% of salt gross mass
Agent polyvinyl alcohol is dissolved in a certain amount of deionized water, and the consumption of described deionized water ensures Fe2+Salt and Fe3+Saline solution is total
Concentration is 5.0wt%；After at the mechanical agitation that speed is 500r/min and 50.0 DEG C, stirring and dissolving is uniform, with the speed of 1 drop/sec
Degree is slowly added dropwise Fe2+Salt and Fe3+Saline solution volume ratio is 1:1, concentration is the NaOH solution of 1.5mol/L, continues anti-afterwards
Answer 90min, form stable black dispersion liquid；Magnetic separation method is used to isolate magnetic-particle stable black dispersion liquid, super
Sound disperses, then Magneto separate, after being repeated 3 times, is re-dispersed in a certain amount of deionized water formation Fe3O4Magnetic nanoparticle matter
Amount concentration is the Fe of 6%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 7% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
Amount 13% 2-acrylamide-2 methyl propane sulfonic acid (AMPS) and acrylic acid (AA), described 2-acrylamide-2 methyl propane sulfonic acid with
Acrylic acid mol ratio is 0.15:10；Under the conditions of 5 DEG C, continue stirring and dissolving complete, form the aqueous solution of clear homogeneous；Add
The initiator ammonium sulfate (APS) of 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid gross mass 1.6% and 2-acrylamide-2 methyl
Propane sulfonic acid and the catalyst n of acrylic acid gross mass 0.05%, N, N ', N '-tetramethylethylenediamine (TEMED), at N2Continue under atmosphere
Stirring 30min dissolves completely, is eventually adding the Fe that a certain amount of step 1) prepares3O4Magnetic nanoparticle stable dispersions, stirring
Mix homogeneously obtains Gel Precursor, adds Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality account for water, hectorite
With 2-acrylamide-2 methyl propane sulfonic acid and the 0.1% of acrylic acid gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 3 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment four: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By FeCl2•4H2O and FeCl3•6H2O is according to Fe2+Salt and Fe3+The mol ratio of salt is the ratio mixing of 1:1.5, with Fe2+
Salt and Fe3+The surfactant polyacrylic acid of the 1wt% of salt gross mass is dissolved in a certain amount of deionized water, described deionized water
Consumption ensure Fe2+Salt and Fe3+Saline solution total concentration is 15wt%；The mechanical agitation that speed is 500r/min and 50.0 DEG C
After lower stirring and dissolving is uniform, it is slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is 1:1, concentration is
The NaOH solution of 1.5mol/L, continues reaction 90min afterwards, forms stable black dispersion liquid；By stable black dispersion liquid
Use magnetic separation method isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, be re-dispersed into a certain amount of go from
Sub-water is formed Fe3O4Magnetic nanoparticle mass concentration is the Fe of 3.5%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 11.5% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
The 2-acrylamide-2 methyl propane sulfonic acid (AMPS) of quality 8% and acrylic acid (AA), described 2-acrylamide-2 methyl propane sulfonic acid and
Acrylic acid mol ratio is 0.274:3；Under the conditions of 3 DEG C, continue stirring and dissolving complete, form the aqueous solution of clear homogeneous；Add
The initiator ammonium sulfate (APS) of 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid gross mass 1.4% and 2-acrylamide-2 methyl
Propane sulfonic acid and the catalyst n of acrylic acid gross mass 0.35%, N, N ', N '-tetramethylethylenediamine (TEMED), at N2Continue under atmosphere
Stirring 30min dissolves completely, is eventually adding the Fe that a certain amount of step 1) prepares3O4Magnetic nanoparticle stable dispersions, stirring
Mix homogeneously obtains Gel Precursor, adds Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality account for water, hectorite
With 2-acrylamide-2 methyl propane sulfonic acid and the 7% of acrylic acid gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 1 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment five: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By FeCl2•4H2O and FeCl3•6H2O is according to Fe2+Salt and Fe3+The mol ratio of salt is the ratio mixing of 1:1.2, with Fe2+
Salt and Fe3+The surfactant polyacrylamide of the 2.5wt% of salt gross mass is dissolved in a certain amount of deionized water, described in go from
The consumption of sub-water ensures Fe2+Salt and Fe3+Saline solution total concentration is 13wt%；In the mechanical agitation that speed is 500r/min and
After stirring and dissolving is uniform at 50.0 DEG C, it is slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio be 1:1,
Concentration is the NaOH solution of 1.5mol/L, continues reaction 90min afterwards, forms stable black dispersion liquid；By stable black
Dispersion liquid uses magnetic separation method to isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, is re-dispersed into a certain amount of
Deionized water in formed Fe3O4Magnetic nanoparticle mass concentration is the Fe of 4.5%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 15% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
Acrylamide and acrylic acid, described acrylamide and acrylic acid mol ratio of amount 10% are 2.971:6；Continue under the conditions of 4 DEG C
Stirring and dissolving is complete, forms the aqueous solution of clear homogeneous；Add acrylamide and the initiator sulphuric acid of acrylic acid gross mass 1.2%
Ammonium (APS) and acrylamide and the catalyst n of acrylic acid gross mass 0.35%, N, N ', N '-tetramethylethylenediamine (TEMED),
N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding the Fe that a certain amount of step 1) prepares3O4Magnetic nanoparticle is steady
Determine dispersion liquid, be uniformly mixed and obtain Gel Precursor, add Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Matter
Amount accounts for water, hectorite and acrylamide and the 10% of acrylic acid gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 2 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment six: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By FeCl2•4H2O and FeCl3•6H2O is according to Fe2+Salt and Fe3+The mol ratio of salt is the ratio mixing of 1:1.3, with Fe2+
Salt and Fe3+The surfactant polyacrylic acid of the 1.5wt% of salt gross mass is dissolved in a certain amount of deionized water, described deionization
The consumption of water ensures Fe2+Salt and Fe3+Saline solution total concentration is 7wt%；In the mechanical agitation and 50.0 that speed is 500r/min
After stirring and dissolving is uniform at DEG C, it is slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is 1:1, concentration
For the NaOH solution of 1.5mol/L, continue reaction 90min afterwards, form stable black dispersion liquid；By stable black dispersion
Liquid uses magnetic separation method to isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, is re-dispersed into a certain amount of going
Ionized water is formed Fe3O4Magnetic nanoparticle mass concentration is the Fe of 2.5%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 5.5% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
The acrylamide of quality 15% and acrylic acid, described acrylamide and acrylic acid mol ratio are 1.5:10；Continue under the conditions of 1 DEG C
Continuous stirring and dissolving is complete, forms the aqueous solution of clear homogeneous；Add acrylamide and the initiator sulfur of acrylic acid gross mass 1.8%
Acid ammonium (APS) and acrylamide and the catalyst n of acrylic acid gross mass 0.05%, N, N ', N '-tetramethylethylenediamine (TEMED),
At N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding the Fe that a certain amount of step 1) prepares3O4Magnetic nanoparticle
Stable dispersions, is uniformly mixed and obtains Gel Precursor, adds Fe3O4Fe in magnetic nanoparticle stable dispersions3O4's
Quality accounts for water, hectorite and acrylamide and the 3% of acrylic acid gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 4 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment seven: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By FeCl2•4H2O and FeCl3•6H2O is according to Fe2+Salt and Fe3+The mol ratio of salt is the ratio mixing of 1:1.4, with Fe2+
Salt and Fe3+The surfactant polyacrylamide copolymer of the 2.5wt% of salt gross mass is dissolved in a certain amount of deionized water, institute
The consumption stating deionized water ensures Fe2+Salt and Fe3+Saline solution total concentration is 9wt%；Stir at the machinery that speed is 500r/min
Mix and stir at 50.0 DEG C stirring and dissolving uniformly after, be slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is
1:1, concentration are the NaOH solution of 1.5mol/L, continue reaction 90min afterwards, form stable black dispersion liquid；By stable
Black dispersion liquid uses magnetic separation method to isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, is re-dispersed into one
Quantitative deionized water is formed Fe3O4Magnetic nanoparticle mass concentration is the Fe of 5.5%3O4Magnetic nanoparticle stable dispersion
Liquid；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 13% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
Acrylamide and acrylic acid, described acrylamide and acrylic acid mol ratio of amount 12% are 0.001:3；Continue under the conditions of 4 DEG C
Stirring and dissolving is complete, forms the aqueous solution of clear homogeneous；Add acrylamide and the initiator ammonium sulfate of acrylic acid gross mass 1%
(APS) and acrylamide and the catalyst n of acrylic acid gross mass 0.3%, N, N ', N '-tetramethylethylenediamine (TEMED), at N2Atmosphere
Enclose the lower stirring 30min that continues to dissolve completely, be eventually adding the Fe that a certain amount of step 1) prepares3O4Magnetic nanoparticle stably divides
Dissipate liquid, be uniformly mixed and obtain Gel Precursor, add Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality account for
Water, hectorite and acrylamide and the 6% of acrylic acid gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 1 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment eight: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By FeCl2•4H2O and FeCl3•6H2O is according to Fe2+Salt and Fe3+The mol ratio of salt is the ratio mixing of 1:1.5, with Fe2+
Salt and Fe3+The surfactant polyvinylpyrrolidone of the 0.5wt% of salt gross mass is dissolved in a certain amount of deionized water, described
The consumption of deionized water ensures Fe2+Salt and Fe3+Saline solution total concentration is 14wt%；It is the mechanical agitation of 500r/min in speed
With 50.0 DEG C at stirring and dissolving uniformly after, be slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is 1:
1, concentration is the NaOH solution of 1.5mol/L, continues reaction 90min afterwards, forms stable black dispersion liquid；By stable black
Color dispersion liquid uses magnetic separation method to isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, is re-dispersed into certain
The deionized water of amount is formed Fe3O4Magnetic nanoparticle mass concentration is the Fe of 2%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 1.5% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
The acrylamide of quality 14% and 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid, described acrylamide and 2-acrylamide-2
Methyl propane sulfonic acid and acrylic acid mol ratio are 0.001:0.15:10；Under the conditions of 0 DEG C, continue stirring and dissolving complete, formed thoroughly
Bright uniform aqueous solution；Add acrylamide and 2-acrylamide-2 methyl propane sulfonic acid and the initiator of acrylic acid gross mass 1.8%
Ammonium sulfate (APS) and acrylamide and 2-acrylamide-2 methyl propane sulfonic acid and the catalyst n of acrylic acid gross mass 0.05%, N,
N ', N '-tetramethylethylenediamine (TEMED), at N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding a certain amount of step
Rapid 1) Fe prepared3O4Magnetic nanoparticle stable dispersions, is uniformly mixed and obtains Gel Precursor, adds Fe3O4Nanometer
Fe in magnetic particle stable dispersions3O4Quality account for water, hectorite, acrylamide, 2-acrylamide-2 methyl propane sulfonic acid, third
The 10% of olefin(e) acid gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 3 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment nine: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By FeCl2•4H2O and FeCl3•6H2O is according to Fe2+Salt and Fe3+The mol ratio of salt is the ratio mixing of 1:1.2, with Fe2+
Salt and Fe3+The surfactant KH550 of the 2.5wt% of salt gross mass is dissolved in a certain amount of deionized water, described deionized water
Consumption ensures Fe2+Salt and Fe3+Saline solution total concentration is 15wt%；At the mechanical agitation that speed is 500r/min and 50.0 DEG C
After stirring and dissolving is uniform, it is slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is 1:1, concentration is
The NaOH solution of 1.5mol/L, continues reaction 90min afterwards, forms stable black dispersion liquid；By stable black dispersion liquid
Use magnetic separation method isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, be re-dispersed into a certain amount of go from
Sub-water is formed Fe3O4Magnetic nanoparticle mass concentration is the Fe of 6%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 10% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
The acrylamide of amount 8% and 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid, described acrylamide and 2-acrylamide-2 methyl
Propane sulfonic acid and acrylic acid mol ratio are 1.5:0.001:7；Under the conditions of 3 DEG C, continue stirring and dissolving complete, form clear homogeneous
Aqueous solution；Add acrylamide and the initiator ammonium sulfate of 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid gross mass 2%
(APS) and acrylamide and 2-acrylamide-2 methyl propane sulfonic acid and the catalyst n of acrylic acid gross mass 0.15%, N, N ', N '-
Tetramethylethylenediamine (TEMED), at N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding a certain amount of step 1) system
The Fe obtained3O4Magnetic nanoparticle stable dispersions, is uniformly mixed and obtains Gel Precursor, adds Fe3O4Nano-magnetic grain
Fe in sub-stable dispersions3O4Quality to account for water, hectorite, acrylamide, 2-acrylamide-2 methyl propane sulfonic acid, acrylic acid total
The 6% of quality；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 0 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment ten: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By FeCl2•4H2O and FeCl3•6H2O is according to Fe2+Salt and Fe3+The mol ratio of salt is the ratio mixing of 1:1.3, with Fe2+
Salt and Fe3+The surfactant KH560 of the 1.0wt% of salt gross mass is dissolved in a certain amount of deionized water, described deionized water
Consumption ensures Fe2+Salt and Fe3+Saline solution total concentration is 5wt%；At the mechanical agitation that speed is 500r/min and 50.0 DEG C
After stirring and dissolving is uniform, it is slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is 1:1, concentration is
The NaOH solution of 1.5mol/L, continues reaction 90min afterwards, forms stable black dispersion liquid；By stable black dispersion liquid
Use magnetic separation method isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, be re-dispersed into a certain amount of go from
Sub-water is formed Fe3O4Magnetic nanoparticle mass concentration is the Fe of 4%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
A certain amount of hectorite (LT-HS) is added in a certain amount of deionized water, described hectorite and the consumption of deionized water
Should ensure that hectorite accounts for the 1% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
The acrylamide of amount 12% and 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid, described acrylamide and 2-acrylamide-2 first
Base propane sulfonic acid and acrylic acid mol ratio are 2.971:0.274:3；Under the conditions of 5 DEG C, continue stirring and dissolving complete, formed transparent
Uniform aqueous solution；Add acrylamide and the initiator sulphuric acid of 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid gross mass 1%
Ammonium (APS) and acrylamide and 2-acrylamide-2 methyl propane sulfonic acid and the catalyst n of acrylic acid gross mass 0.35%, N, N ',
N '-tetramethylethylenediamine (TEMED), at N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding a certain amount of step 1)
The Fe prepared3O4Magnetic nanoparticle stable dispersions, is uniformly mixed and obtains Gel Precursor, adds Fe3O4Nano-magnetic
Fe in particle-stabilised dispersion liquid3O4Quality account for water, hectorite, acrylamide, 2-acrylamide-2 methyl propane sulfonic acid, acrylic acid
The 0.1% of gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 5 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Embodiment 11: magnetorheological nano composite polymeric gel process for preparing, including following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By FeCl2•4H2O and FeCl3•6H2O is according to Fe2+Salt and Fe3+The mol ratio of salt is the ratio mixing of 1:1.5, with Fe2+
Salt and Fe3+The surfactant KH570 of the 2.0wt% of salt gross mass is dissolved in a certain amount of deionized water, described deionized water
Consumption ensures Fe2+Salt and Fe3+Saline solution total concentration is 11wt%；At the mechanical agitation that speed is 500r/min and 50.0 DEG C
After stirring and dissolving is uniform, it is slowly added dropwise Fe with the speed of 1 drop/sec2+Salt and Fe3+Saline solution volume ratio is 1:1, concentration is
The NaOH solution of 1.5mol/L, continues reaction 90min afterwards, forms stable black dispersion liquid；By stable black dispersion liquid
Use magnetic separation method isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, be re-dispersed into a certain amount of go from
Sub-water is formed Fe3O4Magnetic nanoparticle mass concentration is the Fe of 6%3O4Magnetic nanoparticle stable dispersions；
2) situ aggregation method prepares Gel Precursor
Being added in 8ml deionized water by the hectorite (LT-HS) of 0.48g, stirring, to forming transparent aqueous solution, adds 1.00g
Acrylamide, 2-acrylamide-2 methyl propane sulfonic acid of 0.0795g, the acrylic acid of 0.30g；Stirring is continued under the conditions of 5 DEG C
Dissolve completely, form the aqueous solution of clear homogeneous；Add initiator ammonium sulfate (APS) and the catalyst n of 30 μ l of 0.0256g,
N, N ', N '-tetramethylethylenediamine (TEMED), at N2Continue stirring 30min under atmosphere to dissolve completely, be eventually adding a certain amount of
The Fe that step 1) prepares3O4Magnetic nanoparticle stable dispersions, is uniformly mixed and obtains Gel Precursor, adds Fe3O4Receive
Fe in rice magnetic particle stable dispersions3O4Quality account for water, hectorite, acrylamide, 2-acrylamide-2 methyl propane sulfonic acid,
The 1% of acrylic acid gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 2 DEG C, evacuation 30min, seals outlet, close
React 24h under the conditions of seal ring border and 40.0 DEG C, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Claims (2)
1. a magnetorheological nano composite polymeric gel process for preparing, it is characterised in that: include following operating procedure:
1) coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions:
By a certain amount of FeCl2•4H2O、FeCl3•6H2O and a certain amount of surfactant are dissolved in a certain amount of deionized water,
Described FeCl2•4H2O、 FeCl3•6H2The consumption of O should ensure that Fe2+Salt and Fe3+The mol ratio of salt is 1:1.2 ~ 1:1.5；Described table
Face activating agent be dopamine hydrochloride, ethylenediaminetetraacetic acid, polyvinyl alcohol, polyacrylic acid, polyacrylamide, polyacrylic acid, poly-third
One in acrylamide copolymer, polyvinylpyrrolidone, KH550, KH560, KH570, dosage of surfactant is Fe2+Salt with
Fe3+0.5 ~ 2.5wt% of salt gross mass；The consumption of described deionized water should ensure that Fe2+Salt and Fe3+Saline solution total concentration scope
For 5.0wt% ~ 15.0wt%；After at the mechanical agitation that speed is 500r/min and 50.0 DEG C, stirring and dissolving is uniform, with 1 drop/sec
Speed be slowly added dropwise the NaOH solution that a certain amount of concentration is 1.5mol/L, continue reaction 90min afterwards, formed stable
Black dispersion liquid, the consumption of described NaOH solution should ensure that NaOH solution and Fe2+Salt and Fe3+Saline solution volume ratio is 1:1；
Magnetic separation method is used to isolate magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, again stable black dispersion liquid
It is distributed in a certain amount of deionized water, prepares Fe3O4Magnetic nanoparticle stable dispersions, the consumption of described deionized water should
Ensure Fe3O4The mass concentration of magnetic nanoparticle stable dispersions is 2.0% ~ 6.0%；
2) situ aggregation method prepares Gel Precursor
Being added in a certain amount of deionized water by a certain amount of hectorite, described hectorite should ensure that lithium with the consumption of deionized water
Saponite accounts for the 1.0%-15.0% of ionized water quality；Stirring is to forming transparent aqueous solution, and addition gross mass is deionized water
The acrylamide of amount 8.0% ~ 15.0%；Or 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid；Or acrylamide and acrylic acid；Or
Acrylamide and 2-acrylamide-2 methyl propane sulfonic acid and acrylic acid, three of the above material is referred to as high polymer monomer, described propylene
Acid, acrylamide, the mol ratio of 2-acrylamide-2 methyl propane sulfonic acid three are 3 ~ 10:0 ~ 2.971:0 ~ 0.274；0 ~ 5.0
Continue stirring and dissolving under the conditions of DEG C complete, form the aqueous solution of clear homogeneous；Add high polymer monomer gross mass 1.0 ~ 2.0%
Initiator ammonium sulfate and the catalyst n of high polymer monomer gross mass 0.05% ~ 0.35%, N, N ', N '-tetramethylethylenediamine, at N2
Continue stirring 30min under atmosphere to dissolve completely, be eventually adding the Fe that a certain amount of step 1) prepares3O4Magnetic nanoparticle is stable
Dispersion liquid, is uniformly mixed and obtains Gel Precursor, adds Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality
Account for water, hectorite and the 0.1%-10.0% of high polymer monomer raw material gross mass；
3) magnetorheological nano composite polymeric gel is prepared
Gel Precursor being moved in the glass container of vacuum-pumping, under the conditions of 0 ~ 5.0 DEG C, evacuation 30min, seals outlet,
Under the conditions of sealed environment and 40.0 DEG C, react 24h, react 4h at 60 DEG C, prepare magnetorheological nano composite polymeric gel.
Magnetorheological nano composite polymeric gel process for preparing the most according to claim 1, it is characterised in that: described step
3) the various different shape including film, block, column of the magnetorheological nano composite polymeric gel obtained by.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108530653A (en) * | 2018-04-18 | 2018-09-14 | 福州大学 | A kind of preparation method of polyvinyl alcohol magnetic hydrogel |
| CN112812226A (en) * | 2020-12-30 | 2021-05-18 | 大庆师范学院 | Magnetic CPAM water-in-water emulsion and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6262129B1 (en) * | 1998-07-31 | 2001-07-17 | International Business Machines Corporation | Method for producing nanoparticles of transition metals |
| CN102041154A (en) * | 2010-12-27 | 2011-05-04 | 昆明理工大学 | Preparation method of water-based magneto rheological hydraulic transmission medium |
| CN102408520A (en) * | 2011-09-22 | 2012-04-11 | 西北工业大学 | Preparation method for nano monodisperse high magnetism response nuclear shell magnetic polymer microsphere |
| CN104861146A (en) * | 2015-05-08 | 2015-08-26 | 中北大学 | Preparation method for high-performance magnetic Fe3O4/polyurethane elastomer composite material |
| CN105153564A (en) * | 2015-10-21 | 2015-12-16 | 山东科技大学 | Graphene-molybdenum oxide nano flame-retardant composite material |
-
2016
- 2016-07-04 CN CN201610515618.0A patent/CN106117402B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6262129B1 (en) * | 1998-07-31 | 2001-07-17 | International Business Machines Corporation | Method for producing nanoparticles of transition metals |
| CN102041154A (en) * | 2010-12-27 | 2011-05-04 | 昆明理工大学 | Preparation method of water-based magneto rheological hydraulic transmission medium |
| CN102408520A (en) * | 2011-09-22 | 2012-04-11 | 西北工业大学 | Preparation method for nano monodisperse high magnetism response nuclear shell magnetic polymer microsphere |
| CN104861146A (en) * | 2015-05-08 | 2015-08-26 | 中北大学 | Preparation method for high-performance magnetic Fe3O4/polyurethane elastomer composite material |
| CN105153564A (en) * | 2015-10-21 | 2015-12-16 | 山东科技大学 | Graphene-molybdenum oxide nano flame-retardant composite material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108530653A (en) * | 2018-04-18 | 2018-09-14 | 福州大学 | A kind of preparation method of polyvinyl alcohol magnetic hydrogel |
| CN112812226A (en) * | 2020-12-30 | 2021-05-18 | 大庆师范学院 | Magnetic CPAM water-in-water emulsion and preparation method thereof |
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