CN106117402B - High-performance magnetorheological nano composite polymeric gel process for preparing - Google Patents

High-performance magnetorheological nano composite polymeric gel process for preparing Download PDF

Info

Publication number
CN106117402B
CN106117402B CN201610515618.0A CN201610515618A CN106117402B CN 106117402 B CN106117402 B CN 106117402B CN 201610515618 A CN201610515618 A CN 201610515618A CN 106117402 B CN106117402 B CN 106117402B
Authority
CN
China
Prior art keywords
magnetic
magnetorheological
acrylamide
deionized water
certain amount
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201610515618.0A
Other languages
Chinese (zh)
Other versions
CN106117402A (en
Inventor
刘亚青
孙友谊
王妍
赵贵哲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
North University of China
Original Assignee
North University of China
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by North University of China filed Critical North University of China
Priority to CN201610515618.0A priority Critical patent/CN106117402B/en
Publication of CN106117402A publication Critical patent/CN106117402A/en
Application granted granted Critical
Publication of CN106117402B publication Critical patent/CN106117402B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08J2333/24—Homopolymers or copolymers of amides or imides
    • C08J2333/26—Homopolymers or copolymers of acrylamide or methacrylamide
    • C—CHEMISTRY; METALLURGY
    • 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)
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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, solves the problem of existing gel dispersion, stability are poor, and mechanical performance and rheomagnetic be able to not can improve simultaneously, scheme is：FeCl2•4H2O、FeCl3•6H2O, surfactant is dissolved in water；Add NaOH, Magneto separate ultrasonic disperse, disperse in deionized water；Hectorite is added in deionized water, adds high polymer monomer；Initiator and catalyst are added, adds dispersion liquid；Vacuumize, sealing reaction.Advantage：1st, magnetic nanoparticle does not settle, and the interaction force increase between magnetic particle and gelatin polymer matrix, improves stability and dispersiveness；2nd, three-dimensional crosslinked network structure is formed, loading is big, controllability is more preferable；3rd, mechanical property and rheomagnetic can be simultaneous excellent, and tensile strength, elongation at break, magnetic rheology effect, relative magnetic rheology effect are high.

Description

High-performance magnetorheological nano composite polymeric gel process for preparing
Technical field
The present invention relates to magnetorheological materials technical field, prepared by specially high-performance magnetorheological nano composite polymeric gel Method.
Background technology
Magnetorheological materials are a kind of new function materials, and internal magnetization particle is magnetized under external magnetic field, produce phase interaction Firmly, when material is by deformation, these magnetic force are internally formed opposing torque at it, cause magnetorheological materials to produce modulus and resistance The change of the mechanics parameters such as Buddhist nun, the effect are referred to as magnetic rheology effect, have 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 are main at present There are three types：(1) magnetic flow liquid, (2) magnetic rheology elastic body, (3) magnetorheological high-molecular gel.Magnetic flow liquid is that occur earliest Magnetorheological materials（1948）, it is made up of liquid and magnetic particle, under magnetic fields, yield stress and apparent viscosity occur Significant changes, possess higher magnetic rheology effect（>300.0%）, it is applied in intelligent damping noise reduction field, still, magnetic current Become liquid and the problems such as magnetic particle free settling, stability difference be present, limit further raising and the large area of its performance significantly Popularization and application.Magnetic rheology elastic body is a kind of New Materials On Magnetorheological Fluids to grow up the 1990s, mainly by elasticity Body is formed with magnetic particle, and magnetic particle is fixed by elastomer, thus the problem of magnetic particle settles, still, magnetic is not present Property particle is difficult to reset under magnetic fields, thus magnetic rheology effect is relatively low（<300.0%）, limiting its engineering significantly should With.Magnetorheological high-molecular gel concept was proposed first by Nevada ,Usa university professor Gordaninejad at the beginning of 21 century, lotus Langdell volt Polytechnics Memdes teaches and further confirmed that for 2010, magnetorheological high-molecular gel be between magnetic flow liquid and A kind of New Materials On Magnetorheological Fluids between magnetic rheology elastic body, magnetic particle not free settling, and possess 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, provided safeguard wherein three-dimensional crosslink polymer network is magnetic particle stability, be present in liquid in crosslink polymer network Resistance is small, and rearrangement, which occurs, under magnetic fields for magnetic particle provides environment.
But existing magnetorheological high-molecular gel, in order to realize high rheomagnetic energy, often by simply in magnetic current Become in high-molecular gel matrix and fill a large amount of magnetic particles, still, the introducing of a large amount of magnetic particles necessarily causes high-molecular gel Mechanical performance, dispersiveness, stability significantly declines.These problems greatly limit the engineering of magnetorheological high-molecular gel Using.Therefore, a kind of dispersiveness of research, stability are good, and rheomagnetic can be with the high magnetorheological nano combined high score of mechanical performance Sub- gel process for preparing is necessary.
The content of the invention
The existing magnetorheological high-molecular gel dispersiveness of present invention solution, stability are poor, mechanical performance and rheomagnetic energy The problem of can not improving simultaneously, there is provided a kind of dispersiveness, stability are good, and rheomagnetic can be with the high magnetorheological nanometer of mechanical performance 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 deionization In water, the FeCl2•4H2O、 FeCl3•6H2O dosage should ensure that Fe2+Salt and Fe3+The mol ratio of salt is 1:1.2~1:1.5； The surfactant is Dopamine hydrochloride, ethylenediamine tetra-acetic acid, polyvinyl alcohol, polyacrylic acid, polyacrylamide, polyacrylamide One kind in amine copolymer thing, polyvinylpyrrolidone, KH550, KH560, KH570, dosage of surfactant Fe2+Salt and Fe3+ 0.5 ~ 2.5wt% of salt gross mass；The dosage of the deionized water should ensure that Fe2+Salt and Fe3+Saline solution total concentration scope is 5.0wt%~15.0wt%；After stirring and dissolving is uniform at the mechanical agitation that speed is 500r/min and 50.0 DEG C, with 1 drop/sec The NaOH solution that a certain amount of concentration is 1.5mol/L is slowly added dropwise in speed, continues to react 90min afterwards, forms the black of stabilization Color dispersion liquid, the dosage of the NaOH solution should ensure that NaOH solution and Fe2+Salt and Fe3+Saline solution volume ratio is 1:1；Will Stable black dispersion liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, divides again It is scattered in a certain amount of deionized water, Fe is made3O4Magnetic nanoparticle stable dispersions, the dosage of the deionized water should protect Demonstrate,prove Fe3O4The mass concentration of magnetic nanoparticle stable dispersions is 2.0% ~ 6.0%；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 1.0%-15.0% of ion water quality；Stirring adds gross mass to the transparent aqueous solution is formed For the acrylamide of deionized water quality 8.0% ~ 15.0%（AM）；Or 2- acrylamide-2-methyl propane sulfonics（AMPS）And propylene Acid（AA）；Or acrylamide and acrylic acid；Or acrylamide and 2- acrylamide-2-methyl propane sulfonics and acrylic acid, the above three Kind material is referred to as high polymer monomer, the acrylic acid, acrylamide, the mol ratio of 2- acrylamide-2-methyl propane sulfonic threes For 3 ~ 10：0~2.971：0~0.274；It is complete to continue stirring and dissolving under the conditions of 0 ~ 5.0 DEG C, forms the aqueous solution of clear homogeneous； Add the initiator ammonium sulfate of high polymer monomer gross mass 1.0 ~ 2.0%（APS）With high polymer monomer gross mass 0.05% ~ 0.35% Catalyst n, N, N ', N '-tetramethylethylenediamine（TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, finally add Enter a certain amount of step 1）Obtained Fe3O4Magnetic nanoparticle stable dispersions, it is uniformly mixed to obtain Gel Precursor, Add 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 made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumize 30min under the conditions of 0 ~ 5.0 DEG C, seal Outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, and magnetorheological nano composite polymeric is made and coagulates Glue.
The magnetorheological nano composite polymeric gel can prepare film forming, block, column.A variety of different shapes are prepared into, It is applicable to various uses.
The present invention has advantages below：1st, Fe is used3O4Magnetic nanoparticle substitutes traditional carbon-based iron of micron order or ferromagnetism Particle, and using surfactant to Fe3O4Magnetic nanoparticle surface is modified, and not only causes Fe3O4Magnetic nanoparticle Do not settled in polymerization process in the original location, and add Fe3O4Phase interaction between magnetic nanoparticle and gelatin polymer matrix Firmly, Fe is improved3O4Stability and dispersiveness of the magnetic nanoparticle in high-molecular gel；2nd, replaced by situ aggregation method Magnetorheological high-molecular gel is prepared for blending method, forms three-dimensional crosslinked network structure, and Fe3O4The loading of magnetic nanoparticle It is more preferable with three-dimensional net structure controllability；3rd, it is high using hectorite as the Physical crosslinking agent for forming polymer three-dimensional network structure Molecule monomer prepares mechanical property by in-situ polymerization and rheomagnetic can simultaneous excellent magnetorheological macromolecule as polymer monomers Nano composite polymeric gel, the remote super existing skill of tensile strength, elongation at break, magnetic rheology effect, relative magnetic rheology effect Art is horizontal, is the peak of high-molecular gel properties magnetorheological so far.
Brief description of the drawings
Fig. 1 is that nano composite polymeric gel prepared by the present invention prepares the pictorial diagram after January；There is figure to can be seen that this Still stable homogeneous after nano composite polymeric gel January, illustrate nano composite polymeric gel prepared by the present invention have compared with Good dispersiveness and stability；
Fig. 2 is any local SEM figures of nano composite polymeric gel prepared by the present invention；By in figure it may be clearly seen that Nano composite polymeric gel has three-dimensional crosslinked network structure；
Fig. 3 is the VSM figures of nano composite polymeric gel prepared by the present invention；The nanometer that as seen from the figure prepared by the present invention is answered High-molecular gel magnetic saturation intensity is closed up to 19.10emu/g；
Fig. 4 is the stress-strain diagram of nano composite polymeric gel prepared by the present invention；As seen from the figure prepared by the present invention Nano composite polymeric gel tensile strength up to 75.0kPa；
Fig. 5 is the storage modulus of nano composite polymeric gel prepared by the present invention（a）Absolute value is bent with changes of magnetic field Line；As seen from the figure, the absolute magnetic rheology effect of nano composite polymeric gel prepared by the present invention is 4.8Mpa；
Fig. 6 is the storage modulus of nano composite polymeric gel prepared by the present invention（b）Relative value is bent with changes of magnetic field Line；As seen from the figure, the relative magnetic rheology effect of nano composite polymeric gel prepared by the present invention is 7000%.
Embodiment
Embodiment one：Magnetorheological nano composite polymeric gel process for preparing, including following operating procedure：
1）Coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions：
By 3.58g FeCl2•4H2O, 6.08g FeCl3•6H2O and Fe2+Salt and Fe3+The 0.5wt% of salt gross mass table Face activating agent Dopamine hydrochloride is dissolved in 90ml deionized water；Stir in the mechanical agitation that speed is 500r/min and at 50.0 DEG C Mix after being uniformly dissolved, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio is 1:1st, concentration is 1.5mol/L NaOH solution, continue to react 90min afterwards, form stable black dispersion liquid；By stable black dispersion liquid Magnetic-particle, ultrasonic disperse, then Magneto separate are isolated using magnetic separation method, after being repeated 3 times, be re-dispersed into it is a certain amount of go from Fe is formed in sub- water3O4Magnetic nanoparticle mass concentration is 3.0% Fe3O4Magnetic nanoparticle stable dispersions；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 1.0% of ion water quality；Stirring adds deionized water quality to the transparent aqueous solution is formed 9.5% acrylamide（AM）；It is complete to continue stirring and dissolving under the conditions of 2 DEG C, forms the aqueous solution of clear homogeneous；Add propylene The initiator ammonium sulfate of acid amides gross mass 2.0%（APS）With the catalyst n of acrylamide quality 0.2%, N, N ', N '-tetramethyl second Diamines（TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of step 1）Obtained Fe3O4 Magnetic nanoparticle stable dispersions, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4Stable point of magnetic nanoparticle Fe in dispersion liquid3O4Quality account for the 5% of water, hectorite and acrylamide quality；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 5 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
Embodiment two：Magnetorheological nano composite polymeric gel process for preparing, including following operating procedure：
1）Coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions：
By 3.58g FeCl2•4H2O, 7.3g FeCl3•6H2O and Fe2+Salt and Fe3+Live on the 2wt% of salt gross mass surface Property agent ethylenediamine tetra-acetic acid is dissolved in 90ml deionized water；Stir in the mechanical agitation that speed is 500r/min and at 50.0 DEG C After being uniformly dissolved, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio is 1:1st, concentration 1.5mol/ L NaOH solution, continue to react 90min afterwards, form stable black dispersion liquid；Stable black dispersion liquid is used into magnetic Partition method isolates magnetic-particle, ultrasonic disperse, then Magneto separate, after being repeated 3 times, is re-dispersed into a certain amount of deionized water Form Fe3O4Magnetic nanoparticle mass concentration is 2% Fe3O4Magnetic nanoparticle stable dispersions；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 2.5% of ion water quality；Stirring to the transparent aqueous solution is formed, add gross mass for go from The 2- acrylamide-2-methyl propane sulfonics of sub- water quality 11%（AMPS）And acrylic acid（AA）, the 2- acrylamides -2- methyl The mol ratio of propane sulfonic acid and acrylic acid is 0.001：6（2- acrylamide-2-methyl propane sulfonic values level off to 0 but be 0）； It is complete to continue stirring and dissolving under the conditions of 0 DEG C, forms the aqueous solution of clear homogeneous；Add 2- acrylamide-2-methyl propane sulfonics and The initiator ammonium sulfate of acrylic acid gross mass 1.0%（APS）With 2- acrylamide-2-methyl propane sulfonics and acrylic acid gross mass 0.25% catalyst n, N, N ', N '-tetramethylethylenediamine（TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, most After add a certain amount of step 1）Obtained Fe3O4Magnetic nanoparticle stable dispersions, it is uniformly mixed to obtain gel forerunner Body, add Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality account for water, hectorite and the methyl-prop of 2- acrylamides -2 The 8.5% of sulfonic acid and acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 0 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
Embodiment three：Magnetorheological nano composite polymeric gel process for preparing, including following operating procedure：
1）Coprecipitation prepares Fe3O4Magnetic nanoparticle stable dispersions：
By 3.58g FeCl2•4H2O, 7.3g FeCl3•6H2O and Fe2+Salt and Fe3+Live on the 2wt% of salt gross mass surface Property agent polyvinyl alcohol be dissolved in a certain amount of deionized water, the dosage of the deionized water ensures Fe2+Salt and Fe3+Saline solution Total concentration is 5.0wt%；After stirring and dissolving is uniform at the mechanical agitation that speed is 500r/min and 50.0 DEG C, with 1 drop/sec Fe is slowly added dropwise in speed2+Salt and Fe3+Saline solution volume ratio is 1:1st, concentration is 1.5mol/L NaOH solution, is continued afterwards 90min is reacted, forms stable black dispersion liquid；Stable black dispersion liquid is isolated into magnetic-particle using magnetic separation method, Ultrasonic disperse, then Magneto separate, after being repeated 3 times, it is re-dispersed into a certain amount of deionized water and forms Fe3O4Magnetic nanoparticle Mass concentration is 6% Fe3O4Magnetic nanoparticle stable dispersions；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 7% of ion water quality；To the transparent aqueous solution is formed, addition gross mass is deionization for stirring The 2- acrylamide-2-methyl propane sulfonics of water quality 13%（AMPS）And acrylic acid（AA）, the 2- acrylamides -2- methyl-props The mol ratio of sulfonic acid and acrylic acid is 0.15：10；It is complete to continue stirring and dissolving under the conditions of 5 DEG C, forms the water-soluble of clear homogeneous Liquid；Add 2- acrylamide-2-methyl propane sulfonics and the initiator ammonium sulfate of acrylic acid gross mass 1.6%（APS）With 2- acryloyls The catalyst n of amine -2- methyl propane sulfonic acids and acrylic acid gross mass 0.05%, N, N ', N '-tetramethylethylenediamine（TEMED）, in N2 Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of step 1）Obtained Fe3O4Magnetic nanoparticle is stable Dispersion liquid, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality Account for the 0.1% of water, hectorite and 2- acrylamide-2-methyl propane sulfonics and acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 3 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
Example IV：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 1:1.5 ratio mixing, with Fe2+Salt and Fe3+The 1wt% of salt gross mass surfactant polyacrylic acid is dissolved in a certain amount of deionized water, it is described go from The dosage of sub- water ensures Fe2+Salt and Fe3+Saline solution total concentration is 15wt%；Speed be 500r/min mechanical agitation and After stirring and dissolving is uniform at 50.0 DEG C, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio is 1:1、 Concentration is 1.5mol/L NaOH solution, continues to react 90min afterwards, forms stable black dispersion liquid；By stable black Dispersion liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, is re-dispersed into a certain amount of Deionized water in form Fe3O4Magnetic nanoparticle mass concentration is 3.5% Fe3O4Magnetic nanoparticle stable dispersions；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 11.5% of ion water quality；Stirring to the transparent aqueous solution is formed, add gross mass for go from The 2- acrylamide-2-methyl propane sulfonics of sub- water quality 8%（AMPS）And acrylic acid（AA）, the 2- acrylamides -2- methyl-props The mol ratio of sulfonic acid and acrylic acid is 0.274：3；It is complete to continue stirring and dissolving under the conditions of 3 DEG C, forms the water-soluble of clear homogeneous Liquid；Add 2- acrylamide-2-methyl propane sulfonics and the initiator ammonium sulfate of acrylic acid gross mass 1.4%（APS）With 2- acryloyls The catalyst n of amine -2- methyl propane sulfonic acids and acrylic acid gross mass 0.35%, N, N ', N '-tetramethylethylenediamine（TEMED）, in N2 Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of step 1）Obtained Fe3O4Magnetic nanoparticle is stable Dispersion liquid, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality Account for the 7% of water, hectorite and the methyl propane sulfonic acid of 2- acrylamides -2 and acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 1 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
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 1:1.2 ratio mixing, with Fe2+Salt and Fe3+The 2.5wt% of salt gross mass surfactant polyacrylamide is dissolved in a certain amount of deionized water, described The dosage of deionized water ensures Fe2+Salt and Fe3+Saline solution total concentration is 13wt%；In the mechanical agitation that speed is 500r/min With 50.0 DEG C at stirring and dissolving it is uniform after, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio is 1: 1st, concentration is 1.5mol/L NaOH solution, continues to react 90min afterwards, forms stable black dispersion liquid；By the black of stabilization Color dispersion liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, is re-dispersed into certain Fe is formed in the deionized water of amount3O4Magnetic nanoparticle mass concentration is 4.5% Fe3O4Magnetic nanoparticle stable dispersion Liquid；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 15% of ion water quality；To the transparent aqueous solution is formed, addition gross mass is deionization for stirring The acrylamide and acrylic acid of water quality 10%, the mol ratio of the acrylamide and acrylic acid is 2.971:6；Under the conditions of 4 DEG C It is complete to continue stirring and dissolving, forms the aqueous solution of clear homogeneous；Add acrylamide and the initiator of acrylic acid gross mass 1.2% Ammonium sulfate（APS）With acrylamide and the catalyst n of acrylic acid gross mass 0.35%, N, N ', N '-tetramethylethylenediamine （TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of step 1）Obtained Fe3O4Nanometer Magnetic particle stable dispersions, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4Magnetic nanoparticle stable dispersions Middle Fe3O4Quality account for the 10% of water, hectorite and acrylamide and acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 2 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
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 1:1.3 ratio mixing, with Fe2+Salt and Fe3+The 1.5wt% of salt gross mass surfactant polyacrylic acid is dissolved in a certain amount of deionized water, described to go The dosage of ionized water ensures Fe2+Salt and Fe3+Saline solution total concentration is 7wt%；Speed be 500r/min mechanical agitation and After stirring and dissolving is uniform at 50.0 DEG C, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio is 1:1、 Concentration is 1.5mol/L NaOH solution, continues to react 90min afterwards, forms stable black dispersion liquid；By stable black Dispersion liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, is re-dispersed into a certain amount of Deionized water in form Fe3O4Magnetic nanoparticle mass concentration is 2.5% Fe3O4Magnetic nanoparticle stable dispersions；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 5.5% of ion water quality；Stirring to the transparent aqueous solution is formed, add gross mass for go from The acrylamide and acrylic acid of sub- water quality 15%, the mol ratio of the acrylamide and acrylic acid is 1.5:10；In 1 DEG C of condition Lower continuation stirring and dissolving is complete, forms the aqueous solution of clear homogeneous；Add the initiation of acrylamide and acrylic acid gross mass 1.8% Agent ammonium sulfate（APS）With acrylamide and the catalyst n of acrylic acid gross mass 0.05%, N, N ', N '-tetramethylethylenediamine （TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of step 1）Obtained Fe3O4Nanometer Magnetic particle stable dispersions, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4Magnetic nanoparticle stable dispersions Middle Fe3O4Quality account for the 3% of water, hectorite and acrylamide and acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 4 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
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 1:1.4 ratio mixing, with Fe2+Salt and Fe3+The 2.5wt% of salt gross mass surfactant polyacrylamide copolymer is dissolved in a certain amount of deionized water In, the dosage of the deionized water ensures Fe2+Salt and Fe3+Saline solution total concentration is 9wt%；In the machine that speed is 500r/min Tool stir and 50.0 DEG C at stirring and dissolving it is uniform after, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume Than for 1:1st, concentration is 1.5mol/L NaOH solution, continues to react 90min afterwards, forms stable black dispersion liquid；Will be steady Fixed black dispersion liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, disperses again Fe is formed into a certain amount of deionized water3O4Magnetic nanoparticle mass concentration is 5.5% Fe3O4Magnetic nanoparticle is stable Dispersion liquid；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 13% of ion water quality；To the transparent aqueous solution is formed, addition gross mass is deionization for stirring The acrylamide and acrylic acid of water quality 12%, the mol ratio of the acrylamide and acrylic acid is 0.001:3；Under the conditions of 4 DEG C It is complete to continue stirring and dissolving, forms the aqueous solution of clear homogeneous；Add acrylamide and the initiator sulphur of acrylic acid gross mass 1% Sour ammonium（APS）With acrylamide and the catalyst n of acrylic acid gross mass 0.3%, N, N ', N '-tetramethylethylenediamine（TEMED）, N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of step 1）Obtained Fe3O4Magnetic nanoparticle is steady Determine dispersion liquid, be uniformly mixed to obtain Gel Precursor, add Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Matter Amount accounts for the 6% of water, hectorite and acrylamide and acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 1 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
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 1:1.5 ratio mixing, with Fe2+Salt and Fe3+The 0.5wt% of salt gross mass surfactant polyvinylpyrrolidone is dissolved in a certain amount of deionized water, The dosage of the deionized water ensures Fe2+Salt and Fe3+Saline solution total concentration is 14wt%；In the machinery that speed is 500r/min Stirring and 50.0 DEG C at stirring and dissolving it is uniform after, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio For 1:1st, concentration is 1.5mol/L NaOH solution, continues to react 90min afterwards, forms stable black dispersion liquid；Will be stable Black dispersion liquid magnetic-particle, ultrasonic disperse, then Magneto separate are isolated using magnetic separation method, after being repeated 3 times, be re-dispersed into Fe is formed in a certain amount of deionized water3O4Magnetic nanoparticle mass concentration is 2% Fe3O4Magnetic nanoparticle stable dispersion Liquid；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 1.5% of ion water quality；Stirring to the transparent aqueous solution is formed, add gross mass for go from The acrylamide and 2- acrylamide-2-methyl propane sulfonics and acrylic acid of sub- water quality 14%, acrylamide and the 2- acryloyl The mol ratio of amine -2- methyl propane sulfonic acids and acrylic acid is 0.001:0.15:10；It is complete to continue stirring and dissolving under the conditions of 0 DEG C, shape Into the aqueous solution of clear homogeneous；Add acrylamide and 2- acrylamide-2-methyl propane sulfonics and acrylic acid gross mass 1.8% Initiator ammonium sulfate（APS）With the catalysis of acrylamide and 2- acrylamide-2-methyl propane sulfonics and acrylic acid gross mass 0.05% Agent N, N, N ', N '-tetramethylethylenediamine（TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding certain The step 1 of amount）Obtained Fe3O4Magnetic nanoparticle stable dispersions, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality account for water, hectorite, acrylamide, the methyl of 2- acrylamides -2 The 10% of propane sulfonic acid, acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 3 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
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 1:1.2 ratio mixing, with Fe2+Salt and Fe3+The 2.5wt% of salt gross mass surfactant KH550 is dissolved in a certain amount of deionized water, the deionization The dosage of water ensures Fe2+Salt and Fe3+Saline solution total concentration is 15wt%；In the mechanical agitation and 50.0 that speed is 500r/min After stirring and dissolving is uniform at DEG C, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio is 1:1st, concentration For 1.5mol/L NaOH solution, continue to react 90min afterwards, form stable black dispersion liquid；Stable black is disperseed Liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, is re-dispersed into a certain amount of go Fe is formed in ionized water3O4Magnetic nanoparticle mass concentration is 6% Fe3O4Magnetic nanoparticle stable dispersions；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 10% of ion water quality；To the transparent aqueous solution is formed, addition gross mass is deionization for stirring The acrylamide and 2- acrylamide-2-methyl propane sulfonics and acrylic acid of water quality 8%, acrylamide and the 2- acrylamide- The mol ratio of 2- methyl propane sulfonic acids and acrylic acid is 1.5:0.001:7；It is complete to continue stirring and dissolving under the conditions of 3 DEG C, is formed saturating The bright uniform aqueous solution；Add acrylamide and 2- acrylamide-2-methyl propane sulfonics and the initiator of acrylic acid gross mass 2% Ammonium sulfate（APS）With acrylamide and 2- acrylamide-2-methyl propane sulfonics and the catalyst n of acrylic acid gross mass 0.15%, N, N ', N '-tetramethylethylenediamine（TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of step Rapid 1）Obtained Fe3O4Magnetic nanoparticle stable dispersions, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4Nanometer Fe in magnetic particle stable dispersions3O4Quality account for water, hectorite, acrylamide, the methyl propane sulfonic acid of 2- acrylamides -2, third The 6% of olefin(e) acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 0 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
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 1:1.3 ratio mixing, with Fe2+Salt and Fe3+The 1.0wt% of salt gross mass surfactant KH560 is dissolved in a certain amount of deionized water, the deionization The dosage of water ensures Fe2+Salt and Fe3+Saline solution total concentration is 5wt%；In the mechanical agitation and 50.0 that speed is 500r/min After stirring and dissolving is uniform at DEG C, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio is 1:1st, concentration For 1.5mol/L NaOH solution, continue to react 90min afterwards, form stable black dispersion liquid；Stable black is disperseed Liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, is re-dispersed into a certain amount of go Fe is formed in ionized water3O4Magnetic nanoparticle mass concentration is 4% Fe3O4Magnetic nanoparticle stable dispersions；
2）Situ aggregation method prepares Gel Precursor
By a certain amount of hectorite（LT-HS）It is added in a certain amount of deionized water, the hectorite and deionized water Dosage should ensure that hectorite accounts for the 1% of ion water quality；To the transparent aqueous solution is formed, addition gross mass is deionization for stirring The acrylamide and 2- acrylamide-2-methyl propane sulfonics and acrylic acid of water quality 12%, acrylamide and the 2- acryloyl The mol ratio of amine -2- methyl propane sulfonic acids and acrylic acid is 2.971:0.274:3；It is complete to continue stirring and dissolving under the conditions of 5 DEG C, shape Into the aqueous solution of clear homogeneous；Add drawing for acrylamide and 2- acrylamide-2-methyl propane sulfonics and acrylic acid gross mass 1% Send out agent ammonium sulfate（APS）With acrylamide and 2- acrylamide-2-methyl propane sulfonics and the catalyst of acrylic acid gross mass 0.35% N, N, N ', N '-tetramethylethylenediamine（TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of Step 1）Obtained Fe3O4Magnetic nanoparticle stable dispersions, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4 Fe in magnetic nanoparticle stable dispersions3O4Quality account for water, hectorite, acrylamide, the methyl-prop sulphur of 2- acrylamides -2 Acid, the 0.1% of acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 5 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
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 1:1.5 ratio mixing, with Fe2+Salt and Fe3+The 2.0wt% of salt gross mass surfactant KH570 is dissolved in a certain amount of deionized water, the deionization The dosage of water ensures Fe2+Salt and Fe3+Saline solution total concentration is 11wt%；In the mechanical agitation and 50.0 that speed is 500r/min After stirring and dissolving is uniform at DEG C, Fe is slowly added dropwise with 1 drop/sec of speed2+Salt and Fe3+Saline solution volume ratio is 1:1st, concentration For 1.5mol/L NaOH solution, continue to react 90min afterwards, form stable black dispersion liquid；Stable black is disperseed Liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, is re-dispersed into a certain amount of go Fe is formed in ionized water3O4Magnetic nanoparticle mass concentration is 6% Fe3O4Magnetic nanoparticle stable dispersions；
2）Situ aggregation method prepares Gel Precursor
By 0.48g hectorite（LT-HS）It is added in 8ml deionized waters, stirring adds to the transparent aqueous solution is formed 1.00g acrylamide, the 0.0795g methyl propane sulfonic acid of 2- acrylamides -2,0.30g acrylic acid；Continue under the conditions of 5 DEG C Stirring and dissolving is complete, forms the aqueous solution of clear homogeneous；Add 0.0256g initiator ammonium sulfate（APS）With 30 μ l catalysis Agent N, N, N ', N '-tetramethylethylenediamine（TEMED）, in N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding certain The step 1 of amount）Obtained Fe3O4Magnetic nanoparticle stable dispersions, it is uniformly mixed to obtain Gel Precursor, adds Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Quality account for water, hectorite, acrylamide, the methyl of 2- acrylamides -2 The 1% of propane sulfonic acid, acrylic acid gross mass；
3）Magnetorheological nano composite polymeric gel is made
Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 2 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.

Claims (2)

  1. A kind of 1. magnetorheological nano composite polymeric gel process for preparing, it is characterised in that：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, The FeCl2•4H2O、 FeCl3•6H2O dosage should ensure that Fe2+Salt and Fe3+The mol ratio of salt is 1:1.2~1:1.5；The table Face activating agent is Dopamine hydrochloride, ethylenediamine tetra-acetic acid, polyvinyl alcohol, polyacrylic acid, polyacrylamide, polyacrylamide amine copolymer One kind in thing, polyvinylpyrrolidone, KH550, KH560, KH570, dosage of surfactant Fe2+Salt and Fe3+The total matter of salt 0.5 ~ 2.5wt% of amount；The dosage of the deionized water should ensure that Fe2+Salt and Fe3+Saline solution total concentration scope be 5.0wt% ~ 15.0wt%；It is slow with 1 drop/sec of speed after stirring and dissolving is uniform at the mechanical agitation that speed is 500r/min and 50.0 DEG C The NaOH solution that a certain amount of concentration is 1.5mol/L is added dropwise, continues to react 90min afterwards, forms stable black dispersion liquid, The dosage of the NaOH solution should ensure that NaOH solution and Fe2+Salt and Fe3+Saline solution volume ratio is 1:1；By stable black Dispersion liquid isolates magnetic-particle, ultrasonic disperse, then Magneto separate using magnetic separation method, after being repeated 3 times, is re-dispersed into a certain amount of Deionized water in, be made Fe3O4Magnetic nanoparticle stable dispersions, the dosage of the deionized water should ensure that Fe3O4Nanometer The mass concentration of magnetic particle stable dispersions is 2.0% ~ 6.0%；
    2）Situ aggregation method prepares Gel Precursor
    A certain amount of hectorite is added in a certain amount of deionized water, the dosage of the hectorite and deionized water should ensure that lithium Saponite accounts for the 1.0%-15.0% of ion water quality；To the transparent aqueous solution is formed, addition gross mass is deionized water for stirring The acrylamide of amount 8.0% ~ 15.0%；Or 2- acrylamide-2-methyl propane sulfonics and acrylic acid；Or acrylamide and acrylic acid； Or acrylamide and 2- acrylamide-2-methyl propane sulfonics and acrylic acid, three of the above material are referred to as high polymer monomer, described third Olefin(e) acid, acrylamide, the mol ratio of 2- acrylamide-2-methyl propane sulfonic threes are 3 ~ 10：0~2.971：0~0.274；0 ~ It is complete to continue stirring and dissolving under the conditions of 5.0 DEG C, forms the aqueous solution of clear homogeneous；Add high polymer monomer gross mass 1.0 ~ 2.0% Initiator ammonium sulfate and high polymer monomer gross mass 0.05% ~ 0.35% catalyst n, N, N ', N '-tetramethylethylenediamine, N2Continue to stir 30min dissolvings completely under atmosphere, be eventually adding a certain amount of step 1）Obtained Fe3O4Magnetic nanoparticle is steady Determine dispersion liquid, be uniformly mixed to obtain Gel Precursor, add Fe3O4Fe in magnetic nanoparticle stable dispersions3O4Matter Amount accounts for the 0.1%-10.0% of water, hectorite and high polymer monomer raw material gross mass；
    3）Magnetorheological nano composite polymeric gel is made
    Gel Precursor is moved into the glass container of vacuum-pumping, vacuumizes 30min under the conditions of 0 ~ 5.0 DEG C, seal outlet, 24h is reacted under the conditions of sealed environment and 40.0 DEG C, reacts 4h at 60 DEG C, magnetorheological nano composite polymeric gel is made.
  2. 2. magnetorheological nano composite polymeric gel process for preparing according to claim 1, it is characterised in that：The step 3）Obtained magnetorheological nano composite polymeric gel is film, block, column.
CN201610515618.0A 2016-07-04 2016-07-04 High-performance magnetorheological nano composite polymeric gel process for preparing Active CN106117402B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610515618.0A CN106117402B (en) 2016-07-04 2016-07-04 High-performance magnetorheological nano composite polymeric gel process for preparing

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610515618.0A CN106117402B (en) 2016-07-04 2016-07-04 High-performance magnetorheological nano composite polymeric gel process for preparing

Publications (2)

Publication Number Publication Date
CN106117402A CN106117402A (en) 2016-11-16
CN106117402B true CN106117402B (en) 2017-11-28

Family

ID=57468207

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610515618.0A Active CN106117402B (en) 2016-07-04 2016-07-04 High-performance magnetorheological nano composite polymeric gel process for preparing

Country Status (1)

Country Link
CN (1) CN106117402B (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
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
CN112812226B (en) * 2020-12-30 2023-05-12 大庆师范学院 Magnetic CPAM water-in-water emulsion and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
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

Also Published As

Publication number Publication date
CN106117402A (en) 2016-11-16

Similar Documents

Publication Publication Date Title
CN104844760B (en) A kind of water-soluble ultrabranching polymer oil-displacing agent and preparation method thereof
CN104710584B (en) macromolecule hydrogel and preparation method thereof
Chen et al. Preparation and characterization of thermosensitive organic–inorganic hybrid microgels with functional Fe3O4 nanoparticles as crosslinker
CN106117402B (en) High-performance magnetorheological nano composite polymeric gel process for preparing
CN104592449B (en) A kind of intelligent aqueous gel and preparation method and application
CN106832113A (en) A kind of temperature-resistant anti-salt flooding polymers containing nano particle
CN103333449A (en) Polymethyl methacrylate-zinc hydroxide nanocomposite and preparation method thereof
CN105733189A (en) High-barrier composite material and preparation method based on two-dimensional nanofiller magnetic induced orientation
Silva et al. Tailoring the morphology of polymer/montmorillonite hybrid latexes by surfactant-free emulsion polymerization mediated by amphipathic MacroRAFT agents
Zhao et al. Efficient removal of cationic and anionic dyes by surfactant modified Fe3O4 nanoparticles
Guimarães et al. Polymer-encapsulation of iron oxide clusters using macroRAFT block copolymers as stabilizers: tuning of the particle morphology and surface functionalization
CN110627969A (en) Method for preparing self-repairing hydrogel by using Janus nano material
WO2014058014A1 (en) Organic-inorganic hybrid silica nanoparticle and production method thereof
CN101336271A (en) Nanoscale superparamagnetic poly(meth)acrylate polymers
CN105001373B (en) Seawater base Instant heatproof fracturing fluid system
CN104465000A (en) Preparation method for ferroferric oxide magnetic mesoporous material wrapped by zinc oxide
CN108231310B (en) Preparation method of modified neodymium iron boron magnetic powder, modified neodymium iron boron magnetic powder and neodymium iron boron sintered body
Paixão et al. Thermoresponsive polymer brushes on magnetic chitosan microspheres: Synthesis, characterization and application in oily water of high salinity
JP6880614B2 (en) How to recover water-insoluble substances
CN104829793A (en) Preparation method of temperature and pH sensitive organic/inorganic hybrid material POSS/PDMAEMA-b-PNIPAM
Gou et al. A novel hybrid hyperbranched nanowire CNTs for enhancing oil recovery through increasing viscoelasticity and high-viscous emulsions to compensate reservoir heterogeneity
CN110643342A (en) Functional material for regulating and controlling ions in liquid
JP2019085435A (en) Organic inorganic composite hydrogel precursor composition, organic inorganic composite hydrogel, and manufacturing method therefor
CN110739110A (en) spherical nanometer magnetons with stable solution dispersibility and preparation method thereof
CN1737956A (en) Magnetic Nano material

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant