CN110391060A - A kind of preparation method of magnetic fluid material - Google Patents
A kind of preparation method of magnetic fluid material Download PDFInfo
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- CN110391060A CN110391060A CN201910506123.5A CN201910506123A CN110391060A CN 110391060 A CN110391060 A CN 110391060A CN 201910506123 A CN201910506123 A CN 201910506123A CN 110391060 A CN110391060 A CN 110391060A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0063—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use in a non-magnetic matrix, e.g. granular solids
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/44—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids
- H01F1/445—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of magnetic liquids, e.g. ferrofluids the magnetic component being a compound, e.g. Fe3O4
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
Abstract
The present invention relates to a kind of preparation methods of magnetic fluid material, belong to magnetic composite preparation technical field.Mixed serum and silica gel are mixed to prepare mixed emulsion by the present invention, mixed emulsion is injected in sodium hydroxide solution, filter residue is obtained by filtration, graphene oxide and ethylene glycol are mixed, with filter residue, reaction solid is made in dopamine mixing oscillation, solid and diethylene-triamine pentaacetic acid will finally be reacted, magnetic fluid material is made in the blended under agitation such as ethylene glycol, chitosan and ferroso-ferric oxide are dispersed stirring by the present invention in acetic acid solution, reinforce the bonding suction-operated between ferroso-ferric oxide and chitosan, the polymer microballoon of formation, the mutual magnetic force of ferroso-ferric oxide can be effectively prevent to attract to form agglomeration, graphene and ferroferric oxide nano granules bonding coat, make graphene, a strata dopamine film is covered on ferriferrous oxide particles, avoid the formation of agglomeration, enhance the dispersion performance of magnetic-particle, with wide application Prospect.
Description
Technical field
The present invention relates to a kind of preparation methods of magnetic fluid material, belong to magnetic composite preparation technical field.
Background technique
Magnetic fluid, also known as magnetic liquid, ferrofluid or magnetic liquid.Magnetic fluid refers to the nano-magnetic for being adsorbed with stabilizer
Grain high degree of dispersion and stable colloidal dispersion for being formed in carrier fluid.Magnetic fluid has both the magnetism of magnet and the mobility of liquid,
When not having externally-applied magnetic field, it has mobility and certain viscosity as common liq, but when there are externally-applied magnetic field,
Magnetic fluid shows paramagnetism.
Magnetic fluid material is mainly magnetic nanoparticle, base load liquid and the surface of nanometer scale (10nm or less) by diameter
Activating agent three parts composition.Nanoparticle forms one by interfacial agent with base load liquid, even if in gravitational field, electric field, magnetic
Can also exist steadily in the long term under field action, not generate and precipitate and separate.Therefore, it is widely used in chemical industry, biology and clinic
The multiple fields such as medicine.
Magnetic fluid has two kinds of forms of oil-based magnetic fluids and water-based magnetic fluid, and different magnetic fluids has in different media
There is different dispersion performances.The magnetic fluid system stable for one must have following condition: (1) ruler of magnetic-particle
Very little necessary sufficiently small, energy of thermal motion prevents particle agglomeration and precipitating.(2) surfactant can prevent particle agglomeration, therefore institute
The surfactant molecule of selection interacts with magnetic-particle, forms close clad in particle surface.
Although existing magnetic fluid bio-compatibility is stronger, generally existing stability is bad, magnetic nanoparticle
It is poor with carrier fluid compatibility, it be easy to cause separation of solid and liquid.It is easy to cause dispersibility poor in use, brings it about reunion
Phenomena such as.Currently, the further impr-vement of magnetic nanoparticle dispersion all concentrates in the selection of dispersing agent, lead to magnetic nanoparticle
Degree of scatter in magnetic fluid is never obviously improved.
It would therefore be highly desirable to develop a kind of stability, good dispersion, being not susceptible to the magnetic fluid material reunited has important meaning
Justice.
Summary of the invention
The technical problems to be solved by the invention: for easily absorption causes to reunite between current magnetic fluid material particle
Phenomenon, while the labile defect of magnetic particle, provide a kind of preparation method of magnetic fluid material.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
The specific preparation step of magnetic fluid material are as follows:
Weigh reaction solid, diethylene-triamine pentaacetic acid, disodium ethylene diamine tetraacetate, gluconic acid, sodium gluconate and second
Glycol is put into high speed disperser, and magnetic current is made in 45~55min of blended under agitation under conditions of revolving speed is 1100~1200r/min
Body material；
React the specific preparation step of solid are as follows:
(1) it by graphene oxide and ethylene glycol investment three-necked flask, is stirred with blender with the revolving speed mixing of 400~420r/min
It mixes 120~140min and dispersion liquid is made, by dispersion liquid and chlorination iron powder investment reaction kettle, temperature of reaction kettle is increased to
160~180 DEG C, 130~150min of isothermal reaction, hydro-thermal reaction liquid is made；
(2) it is filtered hydro-thermal reaction liquid to obtain filter cake, filter cake is placed in baking oven, the condition for being 160~180 DEG C in temperature
5~6h of lower drying, is adsorbed to obtain magnetic product after drying with magnet, weighs cell reaction object, magnetic product, mass fraction
It is placed in a beaker, is placed the beaker in shaking table for 5~7% dopamine solution and aminomethane, the item for being 32~34 DEG C in temperature
2~3h of mixing oscillation, is obtained by filtration modified filter residue under part after oscillation, is adsorbed to obtain reaction solid with magnet；
The specific preparation step of cell reaction object are as follows:
(1) acetic acid solution that chitosan and mass fraction are 6~8% is put into beaker and is uniformly mixed obtained mixed solvent, to burning
Ferroferric oxide powder is added in cup, 45~55min is mixed with the revolving speed of 800~900r/min with blender, is made mixed
Close slurries；
(2) silica gel is added into beaker, 2~3h is mixed with the revolving speed of 900~920r/min with blender, mixing cream is made
Liquid injects mixed emulsion in syringe, and syringe is placed in and fills the hydrogen-oxygen that the mass fraction for accounting for beaker volume 3/4 is 10~12%
On the beaker for changing sodium solution, syringe bottom end and liquid level distance are 7~9cm, are inserted respectively in pin hole and sodium hydroxide solution
Enter positive and negative electrode；
(3) by syringe, into beaker, extrusion mixing lotion, whole close power supply after squeezing out, reaction product are obtained, by reaction product
It is filtered to obtain filter residue, filter residue 4~6 times wash with distilled water to get cell reaction object.
Preferably according to parts by weight, reaction solid is 8~10 parts, diethylene-triamine pentaacetic acid is 1.2~1.4 parts,
Disodium ethylene diamine tetraacetate is 1.6~1.8 parts, gluconic acid is 0.2~0.4 part, sodium gluconate is 0.2~0.4 part, second two
Alcohol is 35~37 parts.
Reacting the mass ratio of graphene oxide and ethylene glycol in the specific preparation step (1) of solid is 1:20.
Reacting dispersion liquid and the mass ratio of chlorination iron powder in the specific preparation step (1) of solid is 18:1.
React in the specific preparation step (2) of solid it is preferred according to parts by weight, cell reaction object is 5~7 parts, magnetic
The dopamine solution that product is 4~6 parts, mass fraction is 5~7% is 20~22 parts, aminomethane is 2.0~2.4 parts.
The quality for the acetic acid solution that chitosan and mass fraction are 6~8% in the specific preparation step (1) of cell reaction object
Than for 1:10, the quality for the ferroferric oxide powder being added dropwise into beaker is the 16~18% of mixed solvent quality.
The quality for the silica gel being added in the specific preparation step (2) of cell reaction object into beaker is mixed serum quality
23~25%.
Voltage in the specific preparation step (3) of cell reaction object between syringe and sodium hydroxide solution be 18~22kV,
Rate of extrusion is 3~5mL/min.
The method have the benefit that:
(1) present invention first mixes chitosan with acetic acid solution, ferroferric oxide powder is added after mixing, mixed serum is made,
Mixed serum and silica gel are mixed to prepare mixed emulsion again and are fitted into syringe, infuses mixed emulsion under conditions of logical high-voltage electricity
Enter in sodium hydroxide solution, filter residue is obtained by filtration after injection, then graphene oxide and ethylene glycol are mixed, adds after stirring
Enter iron chloride and carry out high temperature hydro-thermal reaction, filtered after reaction, is dry, is made with filter residue, dopamine mixing oscillating reactions and reacts solid
Body, finally will reaction solid and the obtained magnetic fluid material of diethylene-triamine pentaacetic acid, ethylene glycol and other auxiliary agent blended under agitation
Chitosan and ferroso-ferric oxide are dispersed stirring in acetic acid solution, silica gel are added after stirring, has in chitosan by material, the present invention
A large amount of hydroxyl radical free radical can make to generate between ferroso-ferric oxide and chitosan using Hydrogen Binding Adsorption and intermolecular force
Suction-operated is bonded, then by way of high-pressure electrolysis, forms chitosan, silica gel and ferroso-ferric oxide three porous poly-
Object microballoon is closed, the dispersibility of chitosan and ferroso-ferric oxide in magnetic fluid material, Neng Gouyou can be improved in this micro-sphere structure
Effect prevents the mutual magnetic force of ferroso-ferric oxide from attracting to form agglomeration, at the same using silica gel and chitosan to ferroso-ferric oxide shape into
Row cladding, makes ferroso-ferric oxide itself be difficult to be corroded by external environment, has good chemical stability；
(2) graphene oxide and iron chloride are carried out high temperature hydro-thermal reaction by the present invention in ethylene glycol solution, make graphene and tool
Magnetic ferroferric oxide nano granules bonding cladding, dry after hydro-thermal reaction and with dopamine solution hybrid reaction, make stone
A strata dopamine film is covered on black alkene, ferriferrous oxide particles, makes to be difficult to adsorb mutually by magnetic force between ferroso-ferric oxide,
Agglomeration is avoided the formation of, the dispersion performance of magnetic-particle is enhanced, while using the stability of graphene itself, being aoxidized with four
After three-iron combines, makes ferroso-ferric oxide avoid being corroded by external environment, have broad application prospects.
Specific embodiment
The acetic acid solution 1:10 in mass ratio that chitosan and mass fraction are 6~8% is put into be uniformly mixed in beaker and is made
Mixed solvent the ferroferric oxide powder of mixed solvent quality 16~18% is added into beaker, with blender with 800~900r/
45~55min is mixed in the revolving speed of min, and mixed serum is made；Mixed serum quality 23~25% is added into above-mentioned beaker
Silica gel is mixed 2~3h with blender with the revolving speed of 900~920r/min and mixed emulsion is made, by mixed emulsion injection needle
In cylinder, syringe is placed on the beaker for filling the sodium hydroxide solution that the mass fraction for accounting for beaker volume 3/4 is 10~12%,
Syringe bottom end and liquid level distance are 7~9cm, are inserted into positive and negative electrode respectively in pin hole and sodium hydroxide solution；By above-mentioned needle
Cylinder extrusion mixing lotion into beaker under conditions of voltage is 18~22kV, rate of extrusion is 3~5mL/min, all squeezes out
After close power supply, obtain reaction product, reaction product be filtered to obtain filter residue, wash with distilled water filter residue 4~6 times, i.e.,
Cell reaction object is obtained, it is spare；By graphene oxide and ethylene glycol 1:20 in mass ratio investment three-necked flask in, with blender with
The revolving speed of 400~420r/min is mixed 120~140min and dispersion liquid is made, in mass ratio with chlorination iron powder by dispersion liquid
18:1 is put into reaction kettle, and temperature of reaction kettle is increased to 160~180 DEG C, 130~150min of isothermal reaction, and it is anti-that hydro-thermal is made
Answer liquid；It is filtered above-mentioned hydro-thermal reaction liquid to obtain filter cake, filter cake is placed in baking oven, the item for being 160~180 DEG C in temperature
Dry 5~6h, is adsorbed to obtain magnetic product after drying with magnet under part, according to parts by weight, weigh 5~7 parts it is spare
The dopamine solution and 2.0~2.4 parts of amino that cell reaction object, 4~6 parts of magnetic products, 20~22 parts of mass fractions are 5~7%
Methane is placed in a beaker, and is placed the beaker in shaking table, 2~3h of mixing oscillation under conditions of temperature is 32~34 DEG C, after oscillation
Modified filter residue is obtained by filtration, is adsorbed to obtain reaction solid with magnet；According to parts by weight, weigh 8~10 parts of above-mentioned reaction solids,
1.2~1.4 parts of diethylene-triamine pentaacetic acids, 1.6~1.8 parts of disodium ethylene diamine tetraacetates, 0.2~0.4 part of gluconic acid,
It is 1100~1200r/min in revolving speed in 0.2~0.4 part of sodium gluconate and 35~37 parts of ethylene glycol investment high speed dispersers
Under conditions of 45~55min of blended under agitation be made magnetic fluid material.
Example 1
The preparation of mixed serum:
It is molten that the acetic acid solution 1:10 in mass ratio that chitosan and mass fraction are 6% is put into uniformly mixed obtained mixing in beaker
The ferroferric oxide powder of mixed solvent quality 16% is added into beaker for agent, is stirred with blender with the revolving speed mixing of 800r/min
45min is mixed, mixed serum is made.
The preparation of cell reaction object:
The silica gel of mixed serum quality 23% is added into above-mentioned beaker, 2h is mixed with the revolving speed of 900r/min with blender
Mixed emulsion is made, mixed emulsion is injected in syringe, it is 10% that syringe, which is placed in, and fills the mass fraction for accounting for beaker volume 3/4
Sodium hydroxide solution beaker on, syringe bottom end and liquid level distance be 7cm, in pin hole and sodium hydroxide solution respectively
It is inserted into positive and negative electrode；By above-mentioned syringe under conditions of voltage is 18kV, rate of extrusion is 3mL/min the extrusion mixing into beaker
Lotion closes power supply after all squeezing out, obtains reaction product, reaction product is filtered to obtain filter residue, wash with distilled water
Filter residue 4 times to get cell reaction object, it is spare.
The preparation of hydro-thermal reaction liquid:
By in graphene oxide and ethylene glycol 1:20 in mass ratio investment three-necked flask, mixed with blender with the revolving speed of 400r/min
It closes stirring 120min and dispersion liquid is made, dispersion liquid and chlorination iron powder 18:1 in mass ratio are put into reaction kettle, by reaction kettle
Temperature is increased to 160 DEG C, isothermal reaction 130min, and hydro-thermal reaction liquid is made.
React the preparation of solid:
It is filtered above-mentioned hydro-thermal reaction liquid to obtain filter cake, filter cake is placed in baking oven, it is dry under conditions of temperature is 160 DEG C
Dry 5h is adsorbed to obtain magnetic product after drying with magnet, according to parts by weight, weighs 5 parts of spare cell reaction objects, 4
The dopamine solution and 2.0 parts of aminomethanes that part magnetic product, 20 parts of mass fractions are 5% are placed in a beaker, and are placed the beaker and are shaken
In bed, mixing oscillation 2h, is obtained by filtration modified filter residue, is adsorbed and reacted with magnet under conditions of temperature is 32 DEG C after oscillation
Solid.
The preparation of magnetic fluid material:
According to parts by weight, 8 parts of above-mentioned reaction solids, 1.2 parts of diethylene-triamine pentaacetic acids, 1.6 parts of ethylenediamine tetrems are weighed
In acid disodium, 0.2 part of gluconic acid, 0.2 part of sodium gluconate and 35 parts of ethylene glycol investment high speed dispersers, it is in revolving speed
Magnetic fluid material is made in blended under agitation 45min under conditions of 1100r/min.
Example 2
The preparation of mixed serum:
It is molten that the acetic acid solution 1:10 in mass ratio that chitosan and mass fraction are 7% is put into uniformly mixed obtained mixing in beaker
The ferroferric oxide powder of mixed solvent quality 17% is added into beaker for agent, is stirred with blender with the revolving speed mixing of 850r/min
50min is mixed, mixed serum is made.
The preparation of cell reaction object:
The silica gel of mixed serum quality 24% is added into above-mentioned beaker, 2h is mixed with the revolving speed of 910r/min with blender
Mixed emulsion is made, mixed emulsion is injected in syringe, it is 11% that syringe, which is placed in, and fills the mass fraction for accounting for beaker volume 3/4
Sodium hydroxide solution beaker on, syringe bottom end and liquid level distance be 8cm, in pin hole and sodium hydroxide solution respectively
It is inserted into positive and negative electrode；By above-mentioned syringe under conditions of voltage is 20kV, rate of extrusion is 4mL/min the extrusion mixing into beaker
Lotion closes power supply after all squeezing out, obtains reaction product, reaction product is filtered to obtain filter residue, wash with distilled water
Filter residue 5 times to get cell reaction object, it is spare.
The preparation of hydro-thermal reaction liquid:
By in graphene oxide and ethylene glycol 1:20 in mass ratio investment three-necked flask, mixed with blender with the revolving speed of 410r/min
It closes stirring 130min and dispersion liquid is made, dispersion liquid and chlorination iron powder 18:1 in mass ratio are put into reaction kettle, by reaction kettle
Temperature is increased to 170 DEG C, isothermal reaction 140min, and hydro-thermal reaction liquid is made.
React the preparation of solid:
It is filtered above-mentioned hydro-thermal reaction liquid to obtain filter cake, filter cake is placed in baking oven, it is dry under conditions of temperature is 170 DEG C
Dry 5h is adsorbed to obtain magnetic product after drying with magnet, according to parts by weight, weighs 6 parts of spare cell reaction objects, 5
The dopamine solution and 2.2 parts of aminomethanes that part magnetic product, 21 parts of mass fractions are 6% are placed in a beaker, and are placed the beaker and are shaken
In bed, mixing oscillation 2h, is obtained by filtration modified filter residue, is adsorbed and reacted with magnet under conditions of temperature is 33 DEG C after oscillation
Solid.
The preparation of magnetic fluid material:
According to parts by weight, 9 parts of above-mentioned reaction solids, 1.3 parts of diethylene-triamine pentaacetic acids, 1.7 parts of ethylenediamine tetrems are weighed
In acid disodium, 0.3 part of gluconic acid, 0.3 part of sodium gluconate and 36 parts of ethylene glycol investment high speed dispersers, it is in revolving speed
Magnetic fluid material is made in blended under agitation 50min under conditions of 1150r/min.
Example 3
The preparation of mixed serum:
It is molten that the acetic acid solution 1:10 in mass ratio that chitosan and mass fraction are 8% is put into uniformly mixed obtained mixing in beaker
The ferroferric oxide powder of mixed solvent quality 18% is added into beaker for agent, is stirred with blender with the revolving speed mixing of 900r/min
55min is mixed, mixed serum is made.
The preparation of cell reaction object:
The silica gel of mixed serum quality 25% is added into above-mentioned beaker, 3h is mixed with the revolving speed of 920r/min with blender
Mixed emulsion is made, mixed emulsion is injected in syringe, it is 12% that syringe, which is placed in, and fills the mass fraction for accounting for beaker volume 3/4
Sodium hydroxide solution beaker on, syringe bottom end and liquid level distance be 9cm, in pin hole and sodium hydroxide solution respectively
It is inserted into positive and negative electrode；By above-mentioned syringe under conditions of voltage is 22kV, rate of extrusion is 5mL/min the extrusion mixing into beaker
Lotion closes power supply after all squeezing out, obtains reaction product, reaction product is filtered to obtain filter residue, wash with distilled water
Filter residue 6 times to get cell reaction object, it is spare.
The preparation of hydro-thermal reaction liquid:
By in graphene oxide and ethylene glycol 1:20 in mass ratio investment three-necked flask, mixed with blender with the revolving speed of 420r/min
It closes stirring 140min and dispersion liquid is made, dispersion liquid and chlorination iron powder 18:1 in mass ratio are put into reaction kettle, by reaction kettle
Temperature is increased to 180 DEG C, isothermal reaction 150min, and hydro-thermal reaction liquid is made.
React the preparation of solid:
It is filtered above-mentioned hydro-thermal reaction liquid to obtain filter cake, filter cake is placed in baking oven, it is dry under conditions of temperature is 180 DEG C
Dry 6h is adsorbed to obtain magnetic product after drying with magnet, according to parts by weight, weighs 7 parts of spare cell reaction objects, 6
The dopamine solution and 2.4 parts of aminomethanes that part magnetic product, 22 parts of mass fractions are 7% are placed in a beaker, and are placed the beaker and are shaken
In bed, mixing oscillation 3h, is obtained by filtration modified filter residue, is adsorbed and reacted with magnet under conditions of temperature is 34 DEG C after oscillation
Solid.
The preparation of magnetic fluid material:
According to parts by weight, 10 parts of above-mentioned reaction solids, 1.4 parts of diethylene-triamine pentaacetic acids, 1.8 parts of ethylenediamine tetrems are weighed
In acid disodium, 0.4 part of gluconic acid, 0.4 part of sodium gluconate and 37 parts of ethylene glycol investment high speed dispersers, it is in revolving speed
Magnetic fluid material is made in blended under agitation 55min under conditions of 1200r/min.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that cell reaction object is not added.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that hydro-thermal reaction liquid is not added.
Comparative example 3: the magnetic fluid material of company, Daliang City production.
Magnetic fluid material in magnetic fluid material produced by the present invention and comparative example is detected, testing result such as table 1
It is shown:
Suspension test
Magnetic fluid material in magnetic fluid material produced by the present invention and comparative example is suspended in alcohol solvent, the above suspension
It after being ultrasonically treated 30min, stands, records the time of every kind of magnetic fluid sedimentation.
1 performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Average grain diameter (nm) | 7 | 7 | 6 | 11 | 12 | 10 |
| Clad ratio (%) | 5.6 | 5.9 | 6.0 | 4.2 | 4.5 | 5.1 |
| Molar susceptibility (cm3/ moL) | 436 | 440 | 443 | 369 | 374 | 389 |
| Particle concentration (wt%) | 21.1 | 21.4 | 21.7 | 18.9 | 19.5 | 17.2 |
| Sedimentation time (h) | 2.5 | 2.7 | 3.0 | 1.6 | 1.3 | 2.2 |
| Stability | Without obvious layering after one month | Without obvious layering after one month | Without obvious layering after one month | There are a large amount of layerings after one month | Without obvious layering after one month | There is obvious layering after one month |
From the data in table 1, it can be seen that magnetic fluid material particle produced by the present invention exists without obvious aggregate, particle diameter distribution is uniform, tool
There are good stability and biocompatibility.Magnetic response efficiency and rheological behavior can by the type of the coating of magnetic particle,
Structure and clad ratio are regulated and controled, and preparation method is simple, and product cost is low, are suitable for industrialized production, have good city
Field prospect.
Claims (8)
1. a kind of preparation method of magnetic fluid material, it is characterised in that specific preparation step are as follows:
Weigh reaction solid, diethylene-triamine pentaacetic acid, disodium ethylene diamine tetraacetate, gluconic acid, sodium gluconate and second
Glycol is put into high speed disperser, and magnetic current is made in 45~55min of blended under agitation under conditions of revolving speed is 1100~1200r/min
Body material；
The specific preparation step of the reaction solid are as follows:
(1) it by graphene oxide and ethylene glycol investment three-necked flask, is stirred with blender with the revolving speed mixing of 400~420r/min
It mixes 120~140min and dispersion liquid is made, by dispersion liquid and chlorination iron powder investment reaction kettle, temperature of reaction kettle is increased to
160~180 DEG C, 130~150min of isothermal reaction, hydro-thermal reaction liquid is made；
(2) it is filtered hydro-thermal reaction liquid to obtain filter cake, filter cake is placed in baking oven, the condition for being 160~180 DEG C in temperature
5~6h of lower drying, is adsorbed to obtain magnetic product after drying with magnet, weighs cell reaction object, magnetic product, mass fraction
It is placed in a beaker, is placed the beaker in shaking table for 5~7% dopamine solution and aminomethane, the item for being 32~34 DEG C in temperature
2~3h of mixing oscillation, is obtained by filtration modified filter residue under part after oscillation, is adsorbed to obtain reaction solid with magnet；
The specific preparation step of the cell reaction object are as follows:
(1) acetic acid solution that chitosan and mass fraction are 6~8% is put into beaker and is uniformly mixed obtained mixed solvent, to burning
Ferroferric oxide powder is added in cup, 45~55min is mixed with the revolving speed of 800~900r/min with blender, is made mixed
Close slurries；
(2) silica gel is added into beaker, 2~3h is mixed with the revolving speed of 900~920r/min with blender, mixing cream is made
Liquid injects mixed emulsion in syringe, and syringe is placed in and fills the hydrogen-oxygen that the mass fraction for accounting for beaker volume 3/4 is 10~12%
On the beaker for changing sodium solution, syringe bottom end and liquid level distance are 7~9cm, are inserted respectively in pin hole and sodium hydroxide solution
Enter positive and negative electrode；
(3) by syringe, into beaker, extrusion mixing lotion, whole close power supply after squeezing out, reaction product are obtained, by reaction product
It is filtered to obtain filter residue, filter residue 4~6 times wash with distilled water to get cell reaction object.
2. a kind of preparation method of magnetic fluid material according to claim 1, it is characterised in that: preferably in parts by weight
Meter, the reaction solid is 8~10 parts, diethylene-triamine pentaacetic acid is 1.2~1.4 parts, disodium ethylene diamine tetraacetate is
1.6~1.8 parts, gluconic acid be 0.2~0.4 part, sodium gluconate is 0.2~0.4 part, ethylene glycol is 35~37 parts.
3. a kind of preparation method of magnetic fluid material according to claim 1, it is characterised in that: react the specific system of solid
The mass ratio of standby graphene oxide as described in step (1) and ethylene glycol is 1:20.
4. a kind of preparation method of magnetic fluid material according to claim 1, it is characterised in that: react the specific system of solid
Standby dispersion liquid as described in step (1) and the mass ratio of chlorination iron powder are 18:1.
5. a kind of preparation method of magnetic fluid material according to claim 1, it is characterised in that: react the specific system of solid
In standby step (2) preferably according to parts by weight, the cell reaction object is 5~7 parts, magnetic product is 4~6 parts, quality
The dopamine solution that score is 5~7% is 20~22 parts, aminomethane is 2.0~2.4 parts.
6. a kind of preparation method of magnetic fluid material according to claim 1, it is characterised in that: cell reaction object it is specific
The mass ratio for the acetic acid solution that chitosan described in preparation step (1) and mass fraction are 6~8% is 1:10, is dripped into beaker
The quality of the ferroferric oxide powder added is the 16~18% of mixed solvent quality.
7. a kind of preparation method of magnetic fluid material according to claim 1, it is characterised in that: cell reaction object it is specific
The quality for the silica gel being added described in preparation step (2) into beaker is the 23~25% of mixed serum quality.
8. a kind of preparation method of magnetic fluid material according to claim 1, it is characterised in that: cell reaction object it is specific
Voltage described in preparation step (3) between syringe and sodium hydroxide solution is 18~22kV, rate of extrusion is 3~5mL/
min。
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Cited By (3)
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| CN113372106A (en) * | 2021-08-16 | 2021-09-10 | 绵阳和一磁电有限公司 | Multi-pole magnetic ring pressed compact and manufacturing method thereof |
| CN113913056A (en) * | 2021-11-16 | 2022-01-11 | 海南红杉科创实业有限公司 | Anti-radiation water-based damping coating for strong radiation area and application thereof |
| CN115646470A (en) * | 2022-12-27 | 2023-01-31 | 杭州德海艾科能源科技有限公司 | Magnetic composite material for treating vanadium-containing wastewater and preparation method and application thereof |
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| US20150014572A1 (en) * | 2013-07-09 | 2015-01-15 | National Taipei of University of Technology | Magnetorheological fluid composition and method for forming the same |
| CN105823847A (en) * | 2016-03-16 | 2016-08-03 | 复旦大学 | Glycopeptide enriching and detecting method of amphoteric hydrophilic composite nano material |
| CN106243281A (en) * | 2016-07-25 | 2016-12-21 | 北京农学院 | A kind of with chitosan as substrate, surface is covered with the novel nano magnetic bead preparation method of acrylamide molecules imprinted material |
| CN107376867A (en) * | 2017-06-28 | 2017-11-24 | 西北大学 | A kind of molecule bottle brush type reverse phase absorption agent and preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113372106A (en) * | 2021-08-16 | 2021-09-10 | 绵阳和一磁电有限公司 | Multi-pole magnetic ring pressed compact and manufacturing method thereof |
| CN113913056A (en) * | 2021-11-16 | 2022-01-11 | 海南红杉科创实业有限公司 | Anti-radiation water-based damping coating for strong radiation area and application thereof |
| CN115646470A (en) * | 2022-12-27 | 2023-01-31 | 杭州德海艾科能源科技有限公司 | Magnetic composite material for treating vanadium-containing wastewater and preparation method and application thereof |
| CN115646470B (en) * | 2022-12-27 | 2023-04-07 | 杭州德海艾科能源科技有限公司 | Magnetic composite material for treating vanadium-containing wastewater and preparation method and application thereof |
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