CN115449346B - Preparation method and device of ferroferric oxide composite particles for magnetorheological polishing - Google Patents
Preparation method and device of ferroferric oxide composite particles for magnetorheological polishing Download PDFInfo
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- CN115449346B CN115449346B CN202211053626.XA CN202211053626A CN115449346B CN 115449346 B CN115449346 B CN 115449346B CN 202211053626 A CN202211053626 A CN 202211053626A CN 115449346 B CN115449346 B CN 115449346B
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 153
- 239000011246 composite particle Substances 0.000 title claims abstract description 67
- 238000005498 polishing Methods 0.000 title claims abstract description 64
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 137
- 238000001354 calcination Methods 0.000 claims abstract description 126
- 239000002245 particle Substances 0.000 claims abstract description 66
- 239000000376 reactant Substances 0.000 claims abstract description 56
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000011259 mixed solution Substances 0.000 claims abstract description 40
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 30
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 239000012459 cleaning agent Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000004202 carbamide Substances 0.000 claims abstract description 18
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 238000004140 cleaning Methods 0.000 claims abstract description 17
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 17
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 238000005507 spraying Methods 0.000 claims abstract description 12
- 230000007246 mechanism Effects 0.000 claims description 88
- 238000003860 storage Methods 0.000 claims description 86
- 239000000463 material Substances 0.000 claims description 41
- 238000005469 granulation Methods 0.000 claims description 28
- 230000003179 granulation Effects 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 22
- 238000005485 electric heating Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 238000009413 insulation Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 229920000768 polyamine Polymers 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 9
- 238000004513 sizing Methods 0.000 claims description 9
- 150000004982 aromatic amines Chemical class 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- 125000002723 alicyclic group Chemical group 0.000 claims description 3
- 125000001931 aliphatic group Chemical class 0.000 claims description 3
- 125000003118 aryl group Chemical group 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 abstract description 19
- 238000007517 polishing process Methods 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 7
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 13
- 239000007788 liquid Substances 0.000 description 12
- 239000006249 magnetic particle Substances 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 238000000227 grinding Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 230000009471 action Effects 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003082 abrasive agent Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 229910001868 water Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 238000011949 advanced processing technology Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron alkoxide Chemical class 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide [Fe3O4]
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Composite Materials (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a preparation method and a device of ferroferric oxide composite particles for magnetorheological polishing, wherein the preparation method comprises the following steps: A. preparing reactants with preset shapes by utilizing reaction raw materials through hydrothermal reaction; the reaction raw materials comprise glycol, urea and ferric chloride hexahydrate, and the preset shape comprises a polygon, a flower shape, a hollow round shape or a solid sphere; B. cleaning and drying by using a cleaning agent reactant; C. calcining the ferroferric oxide precursor in an inert gas environment to obtain ferroferric oxide particles with preset shapes; D. mixing an abrasive with a binder to obtain a mixed solution; E. and spraying the mixed solution to the ferroferric oxide particles to obtain the ferroferric oxide composite particles. The preparation method of the ferroferric oxide composite particles for magnetorheological polishing is simple, high in operability and beneficial to improving the processing quality and the processing efficiency of the surface of a polished workpiece in the magnetorheological polishing process.
Description
Technical Field
The invention relates to the technical field of ultra-precise machining, in particular to a preparation method and a device of ferroferric oxide composite particles for magnetorheological polishing.
Background
The magnetorheological fluid belongs to an intelligent material, generates a rheological effect under the action of an external field, and has the advantages that the viscosity and yield stress can be increased sharply, the magnetorheological fluid is similar to the mechanical property of solid, and the rheological process of the material has reversibility and controllability. Polishing of hard and brittle materials by utilizing the rheological properties of magnetorheological fluids has become one of the hot spots in advanced processing technology research. Along with the development of scientific technology, the requirements of people on the processing precision of materials are higher and higher, such as the surface precision of crystal faces, parts of precise instruments and the like, and the requirements on magneto-rheological processing are also higher and higher. Magnetorheological polishing has the advantage over conventional polishing that no new subsurface damage is introduced during the polishing process.
The performance of the magnetorheological polishing liquid has a critical influence on the magnetorheological polishing effect, and the traditional magnetorheological polishing liquid mainly comprises a base carrier liquid, magnetically sensitive particles, abrasive materials and additives. In magnetorheological polishing, the abrasive acts as a "cutter" and the chains of magnetic particles act as a polishing pad. In other words, the chain structure of magnetic particles "entraps" the abrasive for polishing. Thus, processing using conventional magnetorheological polishing fluids has the following drawbacks: (1) The magnetic particles of the traditional magnetorheological polishing liquid are spherical carbonyl iron powder, so that the holding effect on the abrasive is very limited in the processing process, and the magnetorheological polishing efficiency is affected. (2) The magnetic particles and the abrasive are randomly mixed and distributed in the base carrier liquid in the processing process, and the abrasive particles act on the workpiece and simultaneously have a certain removing effect on the workpiece, so that the magnetic particles are easily worn, the service life of the magnetorheological polishing liquid is further shortened, and even the polishing effect is influenced. (3) The abrasive polishes under the centre gripping of magnetic particle, and the abrasive has randomness to the effect of work piece, can't guarantee the homogeneity of polishing. (4) When the sizes of the abrasive materials in the magnetorheological polishing liquid are not uniform, the abrasive materials with smaller sizes are easier to hold by the magnetic particles, so that a part of the abrasive materials cannot be fully utilized, the polishing efficiency is reduced, and even the magnetorheological polishing effect is affected.
Disclosure of Invention
The invention aims to provide a preparation method of ferroferric oxide composite particles for magnetorheological polishing, which is simple and strong in operability, and is beneficial to improving the processing quality and the processing efficiency of the surface of a polished workpiece in the magnetorheological polishing process so as to overcome the defects in the prior art.
The invention further aims at providing a device for realizing the preparation method of the ferroferric oxide composite particles for magnetorheological polishing, which has the advantages of simple structure, convenient use and convenient preparation of the ferroferric oxide composite particles, so as to improve the processing quality and the processing efficiency of the surface of a polished workpiece in the magnetorheological polishing process.
To achieve the purpose, the invention adopts the following technical scheme:
The preparation method of the ferroferric oxide composite particles for magnetorheological polishing comprises the following steps:
A. Preparing reactants with preset shapes by utilizing reaction raw materials through hydrothermal reaction; wherein the reaction raw materials comprise ethylene glycol, urea and ferric chloride hexahydrate, and the preset shape comprises a polygon, a flower shape, a hollow round shape or a solid sphere shape;
B. cleaning the reactant in the step A by using a cleaning agent, and drying to obtain a ferroferric oxide precursor;
C. Calcining the ferroferric oxide precursor in the step B in an inert gas environment to obtain ferroferric oxide particles with a preset shape;
D. mixing an abrasive with a binder to obtain a mixed solution;
E. And D, spraying the mixed solution in the step C to the ferroferric oxide particles so that the mixed solution wraps the ferroferric oxide particles to obtain the ferroferric oxide composite particles.
Preferably, in the step a, the adding ratio of the ferric chloride hexahydrate to the urea is 1: (0.5-2);
The reaction temperature of the hydrothermal reaction is 160-230 ℃ and the reaction time is 350-1000 min.
Preferably, in the step B, the cleaning agent comprises deionized water and absolute ethyl alcohol, the drying temperature is 60-80 ℃, and the drying time is 480-720 min.
Preferably, in the step C, the calcination temperature is 400-500 ℃ and the calcination time is 150-200 min.
Preferably, in the step D, the mixing ratio of the abrasive to the binder is 3: (0.5-1.5);
the grain diameter of the abrasive is 10-800 nm;
According to the mass ratio, the adhesive comprises 1-2 parts of sizing material, 8-10 parts of deionized water and 1-2 parts of curing agent, wherein the sizing material is any one of metallographic sizing powder and acrylic acid powder, and the curing agent is any one of modified aromatic amine, aliphatic polyamine, alicyclic polyamine and aromatic polyamine.
Preferably, in step E, the coating temperature is 70-90 ℃.
The preparation device for the ferroferric oxide composite particles for magnetorheological polishing is used for realizing the preparation method of the ferroferric oxide composite particles for magnetorheological polishing, and comprises a reaction seat, a material conveying mechanism, a reaction mechanism, a calcination granulating mechanism and a collecting mechanism;
The reaction seat is internally provided with a reaction chamber, a calcination granulating chamber and a storage chamber, the reaction mechanism is arranged in the reaction chamber and is used for preparing reactants with preset shapes by utilizing reaction raw materials through hydrothermal reaction and cleaning the reactants; the calcining and granulating mechanism is arranged in the calcining and granulating chamber and is used for drying reactants, providing an inert gas environment for calcining the ferroferric oxide precursor and spraying the mixed solution to the ferroferric oxide particles so that the mixed solution wraps the ferroferric oxide particles; the collecting mechanism is arranged in the storage chamber, the calcining and granulating chamber is communicated with the collecting mechanism, and the collecting mechanism is used for collecting and storing ferroferric oxide particles, mixed solution and ferroferric oxide composite particles;
The material conveying mechanism is arranged at the top of the reaction seat and is used for conveying reactants and cleaning agents to the reaction mechanism and transferring the cleaned reactants to the calcination granulating mechanism.
Preferably, the material conveying mechanism comprises a mounting base, a feeding component and a transferring component, wherein the mounting base is rotatably mounted on the top of the reaction seat, the feeding component and the transferring component are distributed at intervals around the edge of the mounting base, and both the feeding component and the transferring component can move up and down relative to the mounting base;
The feeding assembly is at least provided with five groups, the feeding assembly is used for conveying reactants and cleaning agents to the reaction mechanism, and the transferring assembly is used for transferring the cleaned reactants in the reaction mechanism to the calcination granulation mechanism.
Preferably, the reaction mechanism comprises a rotating seat, a reaction kettle and a heating component; the rotary seat is rotatably arranged in the reaction chamber, a plurality of reaction kettles are arranged at the top of the rotary seat, and the reaction kettles are uniformly distributed around the edge of the mounting base at intervals;
The heating assembly comprises a heating protection cover, a first electric heating tube and a first temperature detector, wherein the heating protection cover is installed on the inner wall of the reaction chamber, the heating protection cover comprises a first high-temperature resistant layer, a first heat-preserving layer and a first heat-insulating layer from inside to outside, the first electric heating tube surrounds the inner wall of the heating protection cover, the first temperature detector is installed inside the reaction chamber, and the first temperature detector is used for detecting the temperature of the reaction chamber.
Preferably, the calcination granulating mechanism comprises an air pressure adjusting component, an air supply component and a calcination component; the air pressure adjusting component is arranged in the calcining and granulating chamber and used for adjusting the air pressure of the calcining and granulating chamber, the air supply component is arranged outside the calcining and granulating chamber and communicated with the calcining and granulating chamber, and the air supply component is used for conveying inert gas to the calcining and granulating chamber;
the calcining assembly comprises a calcining protective cover, a second electric heating tube and a second temperature detector, wherein the calcining protective cover is arranged on the inner wall of the calcining granulation chamber, the calcining protective cover comprises a second high-temperature resistant layer, a second heat preservation layer and a second heat insulation layer from inside to outside, the second electric heating tube is arranged around the inner wall of the calcining protective cover, the second temperature detector is arranged inside the calcining granulation chamber, and the second temperature detector is used for detecting the temperature of the calcining granulation chamber;
The collecting mechanism comprises a first storage component, a second storage component and a third storage component which are sequentially arranged, the first storage component, the second storage component and the third storage component are respectively communicated with the calcining granulation chamber through pipelines, the first storage component is used for storing ferroferric oxide particles, the second storage component is used for storing ferroferric oxide composite particles, and the third storage component is used for storing mixed solution;
The first storage component and the second storage component have the same structure; the first storage component comprises a first storage box, a first switch valve and a filter screen, the first storage box is communicated with the calcination granulating chamber through a pipeline, the first switch valve is arranged on the pipeline and is used for opening and closing the pipeline, and the filter screen is horizontally arranged in the first storage box;
The third storage component comprises a third storage box and a third switch valve, the third storage box is communicated with the calcination granulating chamber through a pipeline, the third switch valve is arranged in the pipeline, and the third switch valve is used for opening and closing the pipeline.
The technical scheme provided by the embodiment of the application can have the following beneficial effects:
Through the compounding of the ferroferric oxide particles with the preset shape and the abrasive, the holding effect of the ferroferric oxide particles on the abrasive is improved, the abrasion of the ferroferric oxide particles in the processing process is reduced, and the service life of the magnetorheological polishing liquid is prolonged.
The preparation device integrates a plurality of functions of the material conveying mechanism, the reaction mechanism, the calcination granulating mechanism and the collecting mechanism, and the occupied space of the preparation device is greatly saved. The reaction mechanism works simultaneously through the reaction kettles, so that the preparation efficiency of the ferroferric oxide composite particles is greatly improved, the final composite product can be output after one-time charging according to the scheme, the one-time automatic production from the preparation to the coating and the final collection of the magnetic particles is realized, the time cost for preparing the composite particles is greatly reduced, and the production efficiency of the ferroferric oxide composite particles is improved.
Drawings
FIG. 1 is a schematic structural view of a preparation apparatus of ferroferric oxide composite particles for magnetorheological polishing according to the present invention.
FIG. 2 is a schematic diagram showing the working states of the calcining and granulating mechanism and the collecting mechanism in the preparation device of the ferroferric oxide composite particles for magnetorheological polishing.
Fig. 3 is a schematic structural view of the ferroferric oxide composite particle of example 1 in a preparation method of the ferroferric oxide composite particle for magnetorheological polishing according to the present invention.
Fig. 4 is a schematic structural view of the ferroferric oxide composite particle of example 2 in a preparation method of the ferroferric oxide composite particle for magnetorheological polishing according to the present invention.
Fig. 5 is a schematic structural view of the ferroferric oxide composite particle of example 3 in a preparation method of the ferroferric oxide composite particle for magnetorheological polishing according to the present invention.
Wherein: reaction seat 1, reaction chamber 11, calcining granulation chamber 12 and storage chamber 13;
a material conveying mechanism 2, a mounting base 21, a feeding assembly 22 and a transferring assembly 23;
The reaction mechanism 3, the rotating seat 31, the reaction kettle 32, the heating component 33, the first electric heating tube 331, the first temperature detector 332 and the heating protection cover 333;
The calcination granulation mechanism 4, the calcination assembly 41, the calcination protective cover 413, the second electric heating tube 411, and the second temperature detector 412;
The collection mechanism 5, the first storage unit 51, the first storage box 511, the first switching valve 512, the filter screen 513, the second storage unit 52, the third storage unit 53, the third storage box 531, and the third switching valve 532.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention.
The technical scheme provides a preparation method of ferroferric oxide composite particles for magnetorheological polishing, which comprises the following steps:
A. Preparing reactants with preset shapes by utilizing reaction raw materials through hydrothermal reaction; wherein the reaction raw materials comprise ethylene glycol, urea and ferric chloride hexahydrate, and the preset shape comprises a polygon, a flower shape, a hollow round shape or a solid sphere shape;
B. cleaning the reactant in the step A by using a cleaning agent, and drying to obtain a ferroferric oxide precursor;
C. Calcining the ferroferric oxide precursor in the step B in an inert gas environment to obtain ferroferric oxide particles with a preset shape;
D. mixing an abrasive with a binder to obtain a mixed solution;
E. And D, spraying the mixed solution in the step C to the ferroferric oxide particles so that the mixed solution wraps the ferroferric oxide particles to obtain the ferroferric oxide composite particles.
In order to improve the processing quality and the processing efficiency of the surface of a polished workpiece in the magnetorheological polishing process, the technical scheme provides a preparation method of ferroferric oxide composite particles for magnetorheological polishing, which comprises five steps of A (reaction), B (cleaning), C (calcination), D (liquid preparation) and E (granulation).
Specifically, the reactant (namely, ferroferric oxide) with a preset shape is generated by carrying out hydrothermal reaction on ethylene glycol, urea and ferric chloride hexahydrate, and compared with the traditional process that carbonyl iron powder is used as magnetic particles, the ferroferric oxide generated by the hydrothermal reaction is used as the magnetic particles, so that the hardness is higher, and the method is more beneficial to effectively grinding the surface of a polished workpiece in the polishing process. Specifically, the reaction principle is as follows: the ethylene glycol is used as a solution and a raw material in the hydrothermal reaction, and as the temperature is increased, the urea in the solution slowly hydrolyzes OH - ions, so that the concentration of OH - ions in the solution is gradually increased to form an alkaline environment. Fe 3+ can be combined with ethylene glycol under high temperature and alkaline environment to generate iron alkoxide precursor crystal nucleus, and the crystal nucleus continuously grows to finally form a reactant with a certain shape.
It should be noted that, the reactants with different shapes can be prepared according to different mixing ratios of the reactants in the hydrothermal reaction and different temperatures and times of the hydrothermal reaction, and the factors can be adjusted according to actual polishing requirements to meet polishing requirements. In preferred embodiments of the present embodiment, the shape of the reactants is preferably polygonal (in particular irregular polygonal), flower-shaped, hollow circular or solid spherical: the irregular polygonal ferroferric oxide has larger friction force between the surface of the ferroferric oxide and the base carrier liquid, so that the sedimentation stability of the magnetorheological polishing liquid is facilitated, and the normal and efficient polishing function of the magnetorheological polishing is facilitated. Because of the structural specificity of the flower-shaped ferroferric oxide, the 'blade' structures among particles can be mutually staggered when the magnetic linkage strings are formed, so that the connection strength of the magnetic linkage strings is improved, and the holding force of the magnetic linkage strings on the abrasive is further improved, so that the polishing efficiency is improved. The hollow round ferroferric oxide has lower density, is beneficial to improving the stability of the magnetorheological polishing liquid, and can ensure the normal and efficient realization of the polishing function of the magnetorheological polishing. The solid spherical ferroferric oxide has good magnetic induction intensity, so that the high-efficiency performance of the polishing process can be effectively ensured.
And (c) cleaning the reactant in the step A, removing reaction impurities remained on the surface of the reactant, and drying to obtain the ferroferric oxide precursor. Next, the ferroferric oxide precursor in the step B is calcined in an inert gas (such as argon, nitrogen, etc.) environment, so that the ferroferric oxide precursor is decomposed under the action of high temperature and reduced into ferroferric oxide particles with preset shapes. Specifically, the process for preparing the ferroferric oxide particles through hydrothermal reaction in the scheme comprises the following reaction stages:
（1）CO(NH2)2+H2O→2NH3·H2O↑+CO2
（2）NH3·H2O NH4++OH-
（3）2Fe3++3HOCH2CH2OH+6OH- Fe2(OCH2CH2O)3+6H2O
（4）3Fe2(OCH2CH2O)3 2Fe3O4+10H2O↑+15C+3CH4↑
and finally, spraying the mixed solution obtained by mixing the abrasive and the binder to the ferroferric oxide particles, so that the ferroferric oxide particles are wrapped by the mixed solution, and the ferroferric oxide composite particles are obtained.
According to the scheme, aiming at the problems existing in the conventional magnetorheological polishing solution, the preparation method of the ferroferric oxide composite particles for magnetorheological polishing is provided, and the grinding materials are coated on the outer layers of the ferroferric oxide particles, so that on one hand, the efficiency and uniformity of magnetorheological polishing are improved, the holding effect of the ferroferric oxide particles on the grinding materials is improved, on the other hand, the abrasion of the ferroferric oxide particles in the processing process is reduced, the service life of the magnetorheological polishing solution is prolonged, and the magnetorheological polishing cost is reduced.
It should be noted that the abrasive in this embodiment may be a diamond abrasive.
Further described, in the step a, the adding ratio of the ferric chloride hexahydrate to the urea is 1: (0.5-2);
The reaction temperature of the hydrothermal reaction is 160-230 ℃ and the reaction time is 350-1000 min.
In order to ensure that the hydrothermal reaction of the scheme can prepare ferroferric oxide particles with ideal shapes, the scheme also limits the adding proportion of ferric chloride hexahydrate and urea in the reaction raw materials, the temperature and the time of the hydrothermal reaction, and the sufficient amount of glycol in the preparation process is not limited.
More specifically, when preparing polygonal ferroferric oxide particles, the addition ratio of ferric chloride hexahydrate and urea is preferably 2:1, the reaction temperature of the hydrothermal reaction is 160-180 ℃ and the reaction time is 500-550 min; when preparing flower-shaped ferroferric oxide particles, the addition ratio of ferric chloride hexahydrate to urea is preferably 1:2, the reaction temperature of the hydrothermal reaction is 160-180 ℃ and the reaction time is 350-400 min; when preparing hollow round ferroferric oxide particles, the addition ratio of ferric chloride hexahydrate to urea is preferably 1:2, the reaction temperature of the hydrothermal reaction is 160-180 ℃ and the reaction time is 500-550 min; when solid spherical ferroferric oxide particles are prepared, the addition ratio of ferric chloride hexahydrate to urea is preferably 1:2, the reaction temperature of the hydrothermal reaction is 180-230 ℃ and the reaction time is 900-1000 min.
Further more, in the step B, the cleaning agent comprises deionized water and absolute ethyl alcohol, the drying temperature of the drying step is 60-80 ℃, and the drying time is 480-720 min.
In a preferred embodiment of the present disclosure, the method may use absolute ethanol and deionized water to clean impurities and reaction raw materials remaining on the surface of the reactant, specifically, the steps include removing reaction impurities by deionized water, dissolving ethylene glycol remaining in the reactant in the absolute ethanol, and removing deionized water in the previous step by the absolute ethanol to perform a double cleaning function. The drying step is to remove the deionized water and absolute ethyl alcohol remained in the cleaning process, so as to ensure the effective encapsulation of the ferroferric oxide particles by the grinding powder in the subsequent step.
Further, in the step C, the calcination temperature of the calcination step is 400-500 ℃ and the calcination time is 150-200 min.
The calcination aims to decompose the ferroferric oxide precursor under the action of high temperature to form ferroferric oxide particles with different shapes so as to improve the processing efficiency and the processing quality of the composite particles. The method controls the temperature and time of the calcination step, and is beneficial to preparing ideal ferroferric oxide particles.
Further, in the step D, the mixing ratio of the abrasive to the binder is 3: (0.5-1.5);
the grain diameter of the abrasive is 10-800 nm;
According to the mass ratio, the adhesive comprises 1-2 parts of sizing material, 8-10 parts of deionized water and 1-2 parts of curing agent, wherein the sizing material is any one of metallographic sizing powder and acrylic acid powder, and the curing agent is any one of modified aromatic amine, aliphatic polyamine, alicyclic polyamine and aromatic polyamine.
In one embodiment of the present disclosure, the mixing mass ratio of the abrasive and the binder is 3: (0.5-1.5), which is favorable for evenly coating the grinding material on the surface of the ferroferric oxide particles in the granulating step. The grain diameter of the abrasive is 10-800 nm, so that the abrasive can be more uniformly coated on the surface of the ferroferric oxide particles; on the other hand, in magnetorheological polishing, the polishing effect of the abrasive in this particle size range is good.
The proposal also provides a raw material and a proportion of the adhesive for wrapping the abrasive particles on the surface of the ferroferric oxide particles, and the raw material is favorable for fast reaction with air to coagulate at a certain temperature when being mixed according to the proportion of the proposal.
Further, in the step E, the wrapping temperature of the wrapping step is 70-90 ℃.
In a more preferred embodiment of the present disclosure, the wrapping step is performed at a wrapping temperature of 70-90 ℃, which is advantageous for rapidly bonding the ferroferric oxide particles and the abrasive to form composite particles under the action of the binder.
The preparation device for the ferroferric oxide composite particles for magnetorheological polishing is used for realizing the preparation method of the ferroferric oxide composite particles for magnetorheological polishing, and comprises a reaction seat 1, a material conveying mechanism 2, a reaction mechanism 3, a calcination granulating mechanism 4 and a collecting mechanism 5;
The reaction seat 1 is internally provided with a reaction chamber 11, a calcination granulating chamber 12 and a storage chamber 13, the reaction mechanism 3 is arranged in the reaction chamber 11, and the reaction mechanism 3 is used for preparing reactants with preset shapes by utilizing reaction raw materials through hydrothermal reaction and cleaning the reactants; the calcining and granulating mechanism 4 is arranged in the calcining and granulating chamber 12, the calcining and granulating mechanism 4 is used for drying reactants, providing an inert gas environment for calcining the ferroferric oxide precursor, and spraying the mixed solution to the ferroferric oxide particles to enable the mixed solution to wrap the ferroferric oxide particles; the collecting mechanism 5 is arranged in the storage chamber 13, the calcining and granulating chamber 12 and the collecting mechanism 5 are communicated with each other, and the collecting mechanism 5 is used for collecting and storing the ferroferric oxide particles, the mixed solution and the ferroferric oxide composite particles;
The material conveying mechanism 2 is arranged at the top of the reaction seat 1, and the material conveying mechanism 2 is used for conveying reactants and cleaning agents to the reaction mechanism 3 and also used for transferring the cleaned reactants to the calcination granulating mechanism 4.
The scheme also provides a device for realizing the preparation method of the ferroferric oxide composite particles for magnetorheological polishing, which is shown in fig. 1-2, and has the advantages of simple structure, convenient use and convenient preparation of the ferroferric oxide composite particles, so that the processing quality and the processing efficiency of the surface of a polished workpiece are improved in the magnetorheological polishing process.
To further illustrate, the material conveying mechanism 2 includes a mounting base 21, a feeding assembly 22 and a transferring assembly 23, wherein the mounting base 21 is rotatably mounted on the top of the reaction seat 1, the feeding assembly 22 and the transferring assembly 23 are spaced around the edge of the mounting base 21, and the feeding assembly 22 and the transferring assembly 23 can move up and down relative to the mounting base 21;
The feeding components 22 are provided with at least five groups, the feeding components 22 are used for conveying reactants and cleaning agents to the reaction mechanism 3, and the transferring components 23 are used for transferring the cleaned reactants in the reaction mechanism 3 to the calcination granulating mechanism 4.
The material conveying mechanism 2 of the scheme is used for injecting the raw materials of the hydrothermal reaction into the reaction mechanism 3, so that the preparation of reactants is realized; for injecting a cleaning agent into the reaction mechanism 3, thereby achieving cleaning of the reactants; and the method is also used for transferring the cleaned reactant to a calcination granulating mechanism 4, so that the subsequent preparation process is convenient.
Specifically, the material conveying mechanism 2 comprises a mounting base 21, a feeding component 22 and a transferring component 23, wherein the feeding component 22 and the transferring component 23 are mounted on the mounting base 21 and rotate along with the rotation of the mounting base 21, so that the feeding component 22 and the transferring component 23 can move to the upper part of the reaction chamber 11 or the calcining granulation chamber 12 as required. The feeding component 22 and the transferring component 23 can move up and down relative to the mounting base 21, and the feeding component 22 moves up and down, so that the reaction raw materials and the cleaning agent can be accurately conveyed to the reaction mechanism 3, and waste is avoided; the up and down movement of the transfer assembly 23 facilitates complete removal of the reactants from the reaction mechanism 3, thereby ensuring the amount of reactants produced.
More specifically, the feed assemblies 22 are provided with at least five sets, and the five sets of feed assemblies 22 may be used to deliver ethylene glycol, urea, ferric chloride hexahydrate, deionized water, and absolute ethanol, respectively, without limitation.
It should be noted that the feeding assembly 22 in this embodiment may be a conventional feeding device in the field, such as a feeding piston, and the transferring assembly 23 is a conventional material conveying device in the field, which can perform material taking and discharging, and is not limited herein.
Further describing, the reaction mechanism 3 includes a rotating base 31, a reaction kettle 32 and a heating component 33; the rotating seat 31 is rotatably installed in the reaction chamber 11, a plurality of reaction kettles 32 are provided, the plurality of reaction kettles 32 are arranged at the top of the rotating seat 31, and the reaction kettles 32 are uniformly distributed around the edge of the installation base 21 at intervals;
The heating assembly 33 includes a heating protection cover 333, a first electrothermal tube 331 and a first temperature detector 332, the heating protection cover 333 is mounted on the inner wall of the reaction chamber 11, and the heating protection cover 333 includes a first high temperature resistant layer, a first heat insulation layer and a first heat insulation layer from inside to outside, the first electrothermal tube 331 is disposed around the inner wall of the heating protection cover 333, the first temperature detector 332 is mounted inside the reaction chamber 11, and the first temperature detector 332 is used for detecting the temperature of the reaction chamber 11.
The reaction mechanism 3 of the scheme is used for preparing reactants with preset shapes by utilizing reaction raw materials through hydrothermal reaction and cleaning the reactants.
Specifically, the reaction mechanism 3 includes a rotary base 31, a reaction kettle 32, and a heating assembly 33; the reaction kettle 32 is arranged at the top of the mounting base 21 and rotates along with the rotation of the rotating seat 31, so that the reaction kettle 32 moves to the lower part of the feeding component 22 or the transferring component 23, the accurate addition of reaction raw materials and cleaning agents is facilitated, and meanwhile, the transferring component 23 is also convenient for taking out the cleaned reactants from the reaction kettle 32; in addition, in the hydrothermal reaction process and the cleaning process, the rotating seat 31 can drive the reaction kettle 32 to centrifugally rotate, so that the uniform mixing of the reaction raw materials in the reaction kettle 32 is quickened, and the cleaning efficiency is quickened. The heating component 33 is mainly used for providing a heating temperature required in the hydrothermal reaction (specifically realized by the first electric heating tube 331); in addition, the heating component 33 is further provided with a first temperature detector 332 for detecting the temperature of the reaction chamber 11, so as to facilitate the improvement of the controllability of technicians in the preparation process of the composite particles, and ensure that accurate temperature control is realized; the heating protection cover 333 includes, from inside to outside, a first high temperature resistant layer, a first heat preservation layer, and a first heat insulation layer, where the first high temperature resistant layer is used to prevent the high temperature generated by the first electric heating tube 331 from damaging the external mechanical and circuit structure; the first heat-preserving layer is wrapped outside the first high-temperature-resistant layer so as to reduce temperature loss; the first heat insulation layer wraps the first heat insulation layer, so that the loss of temperature is further prevented, the high temperature in the reaction chamber 11 is not conducted to other places of the reaction seat 1, and the normal progress of other reactions is avoided.
It should be noted that, the rotating speed of the rotating seat 31 in the scheme in the hydrothermal reaction process is preferably 50-100 r/min, and the rotating speed in the centrifugal cleaning process is preferably 5000-10000 r/min, so that the precursor and the cleaning agent are layered under the action of centrifugal force, the precursor with heavier mass is deposited at the bottom, and the cleaning agent is on the upper layer, thereby being convenient for separating the ferroferric oxide precursor from the cleaning agent. The layers of the heating protection cover 333 in this embodiment are made of conventional materials that can perform related functions, for example, the first heat insulation layer may be made of materials such as heat insulation cotton, which is not limited herein.
Further describing, the calcining granulation mechanism 4 includes an air pressure adjusting component, an air supply component and a calcining component 41; the air pressure adjusting component is arranged in the calcining and granulating chamber 12 and is used for adjusting the air pressure of the calcining and granulating chamber 12, the air supply component is arranged outside the calcining and granulating chamber 12 and is communicated with the calcining and granulating chamber 12, and the air supply component is used for conveying inert gas to the calcining and granulating chamber 12;
The calcination assembly 41 comprises a calcination protecting cover 413, a second electric heating tube 411 and a second temperature detector 412, wherein the calcination protecting cover 413 is installed on the inner wall of the calcination granulating chamber 12, the calcination protecting cover 413 comprises a second high temperature resistant layer, a second heat insulation layer and a second heat insulation layer from inside to outside, the second electric heating tube 411 is arranged around the inner wall of the calcination protecting cover 413, the second temperature detector 412 is installed inside the calcination granulating chamber 12, and the second temperature detector 412 is used for detecting the temperature of the calcination granulating chamber 12;
The collecting mechanism 5 comprises a first storage component 51, a second storage component 52 and a third storage component 53 which are sequentially arranged, wherein the first storage component 51, the second storage component 52 and the third storage component 53 are respectively communicated with the calcining and granulating chamber 12 through pipelines, the first storage component 51 is used for storing ferroferric oxide particles, the second storage component 52 is used for storing ferroferric oxide composite particles, and the third storage component 53 is used for storing a mixed solution;
the first storage assembly 51 and the second storage assembly 52 have the same structure; the first storage assembly 51 includes a first storage box 511, a first switch valve 512 and a filter screen 513, wherein the first storage box 511 is mutually communicated with the calcination and granulation chamber 12 through a pipeline, the first switch valve 512 is arranged on the pipeline, the first switch valve 512 is used for opening and closing the pipeline, and the filter screen 513 is horizontally arranged inside the first storage box 511;
The third storage assembly 53 includes a third storage box 531 and a third switching valve 532, the third storage box 531 is communicated with the calcination granulating chamber 12 through a pipeline, the third switching valve 532 is disposed on the pipeline, and the third switching valve 532 is used for opening and closing the pipeline.
The calcining and granulating mechanism 4 in this embodiment is used for calcining the precursor of ferroferric oxide in an inert gas (such as argon, nitrogen, etc.), and spraying the mixed solution onto the ferroferric oxide particles in the step C, so that the mixed solution wraps the ferroferric oxide particles.
Specifically, the calcination granulation mechanism 4 includes an air pressure adjusting assembly (not shown), an air supply assembly (not shown), and a calcination assembly 41; the internal air pressure of the calcining granulation chamber 12 can be regulated according to the requirement in the preparation process by the air pressure regulating component so as to achieve the purpose of preparation; the gas supply assembly is used for providing an inert environment for the calcination process of the precursor; the calcination assembly 41 is mainly used for providing the reaction temperature (specifically realized by the second electric heating tube 411) required in the drying step, the calcination step and the granulation step; in addition, a second temperature detector 412 for detecting the temperature of the calcining granulation chamber 12 is further disposed in the calcining assembly 41, so as to facilitate the improvement of the controllability of technicians in the preparation process of the composite particles, so as to ensure the realization of accurate temperature control; the calcination protecting cover 413 comprises a second high temperature resistant layer, a second heat insulating layer and a second heat insulating layer from inside to outside, wherein the second high temperature resistant layer is used for preventing the high temperature generated by the second electric heating tube 411 from damaging external machinery and circuit structures; the second heat-insulating layer is wrapped outside the second high-temperature-resistant layer so as to reduce the loss of temperature; the second heat insulation layer is wrapped outside the second heat insulation layer, so that the loss of temperature is further prevented, the high temperature in the calcining granulation chamber 12 is not conducted to other places of the reaction seat 1, and the influence on the normal progress of other reactions is avoided.
It should be noted that, in this embodiment, each layer of the calcination protecting cover 413 is made of a conventional material capable of performing the relevant function, for example, the second insulating layer may be made of a material such as heat insulating cotton, which is not limited herein.
In addition, the first storage component 51 of the collecting mechanism 5 is used for collecting and storing the ferroferric oxide particles, the second storage component 52 is used for mixing the solution, and the third storage component 53 is used for the ferroferric oxide composite particles in this embodiment. Wherein, three storage components are respectively provided with a switch valve connected with the respective storage box pipeline, and the communication between the storage box and the calcining granulation chamber 12 can be controlled by the switch valve, thereby flexibly realizing the preparation process of the ferroferric oxide composite particles. Further, the first storage component 51 and the second storage component 52 of the present embodiment are further provided with a filter screen 513, and the arrangement of the filter screen 513 is also beneficial to the collection of the particulate products and the collection purity of the particulate products is improved.
More specifically, the working process of the preparation device of the ferroferric oxide composite particles for magnetorheological polishing in the scheme is as follows: (1) The reaction raw materials are conveyed to the reaction kettle 32 through the feeding component 22, and the rotating seat 31 is opened to uniformly mix the reaction raw materials in the reaction kettle 32; the first electric heating tube 331 is turned on, so that the reactant in the reaction kettle 32 is reacted by water heat to generate reactant with a preset shape, and the first electric heating tube 331 is turned off after the reaction is finished. (2) The cleaning agent is conveyed to the reaction kettle 32 through the feeding component 22, the rotating seat 31 is opened, and the reaction raw materials in the reaction kettle 32 are centrifugally cleaned; after the cleaning, the cleaned reactant is transferred to the calcining and granulating chamber 12 through the transfer assembly 23, and the second electric heating tube 411 is started to dry the cleaned reactant, so as to obtain the ferroferric oxide precursor. (3) The air supply assembly is used for continuously introducing inert gas into the calcining and granulating chamber 12, discharging air in the calcining and granulating chamber 12, adjusting the temperature of the second electric heating tube 411, calcining and decomposing the ferroferric oxide precursor in the calcining and granulating chamber 12 to obtain ferroferric oxide particles, and opening the first switch valve 512 of the first storage assembly 51 to store the ferroferric oxide particles in the first storage box 511, as shown in a state A in fig. 2. (4) The abrasive is mixed with the binder to obtain a mixed solution and stored in the third storage member 53. (5) The first switch valve 512 of the first storage module 51 is opened, and the third switch valve 532 of the third storage module 53 is opened, and the air pressure adjusting module is activated to make the calcination and granulation chamber 12 form negative pressure, while the mixed solution of the ferroferric oxide particles in the first storage box 511 and the mixed solution in the third storage box 531 is flushed into the calcination and granulation chamber 12 under the negative pressure, as shown in state B in fig. 2. Then, the first switch valve 512 of the first storage component 51 and the third switch valve 532 of the third storage component 53 are closed, and the temperature of the second electric heating tube 411 and the inert gas inlet rate of the gas supply component are adjusted, so that the mixed solution in the calcining granulation chamber 12 fully wraps the ferroferric oxide particles, and thereby the ferroferric oxide composite particles are obtained. After the granulation is completed, the first switch valve of the second storage assembly 52 is opened, so that the ferroferric oxide composite particles are collected and stored in the first storage box of the second storage assembly 52, as shown in state C in fig. 2, to complete the preparation of the ferroferric oxide composite particles.
The preparation device in this scheme collects material conveying mechanism 2, reaction mechanism 3, calcine granulation mechanism 4 and collection mechanism 5a plurality of functions in an organic wholely, has saved preparation device's occupation space greatly. The reaction mechanism 3 works simultaneously through the reaction kettles 32, so that the preparation efficiency of the ferroferric oxide composite particles is greatly improved, the final composite product can be output after one-time charging according to the scheme, the one-time automatic production from the preparation to the coating and the final collection of the magnetic particles is realized, the time cost for preparing the composite particles is greatly reduced, and the production efficiency of the ferroferric oxide composite particles is improved.
Example 1
A. Preparing polygonal reactants by utilizing reaction raw materials through hydrothermal reaction; wherein, the reaction raw materials of ferric chloride hexahydrate, urea and ethylene glycol comprise the following materials in percentage by mass: 1, enough ethylene glycol, the reaction temperature of the hydrothermal reaction is 160 ℃, and the reaction time is 500min;
B. Washing the reactant by deionized water and absolute ethyl alcohol in sequence, and drying at 60 ℃ for 480 minutes to obtain a ferroferric oxide precursor;
C. Calcining the ferroferric oxide precursor in an argon environment at 400 ℃ for 150min to obtain polygonal ferroferric oxide particles;
D. Grinding material with the diameter of 10-800 nm and binder according to the weight ratio of 3:1, mixing the materials in a mass ratio to obtain a mixed solution; wherein, according to the mass ratio, the binder comprises 1 part of metallographic rubber powder, 8 parts of deionized water and 1 part of modified aromatic amine;
E. and spraying the mixed solution to the ferroferric oxide particles in the environment of 70 ℃ to enable the mixed solution to wrap the ferroferric oxide particles, so as to obtain the ferroferric oxide composite particles, wherein the structural schematic diagram of the ferroferric oxide composite particles is shown in figure 3.
Example 2
A. Preparing flower-shaped reactants by utilizing reaction raw materials through hydrothermal reaction; wherein, the reaction raw materials of ferric chloride hexahydrate, urea and ethylene glycol are added according to the mass ratio of 1:2, enough ethylene glycol, the reaction temperature of the hydrothermal reaction is 170 ℃, and the reaction time is 400min;
B. Washing the reactant by deionized water and absolute ethyl alcohol in sequence, and drying for 560 minutes at the temperature of 70 ℃ to obtain a ferroferric oxide precursor;
C. Calcining the ferroferric oxide precursor in an argon environment for 180min at the temperature of 450 ℃ to obtain flower-shaped ferroferric oxide particles;
D. Grinding material with the diameter of 10-800 nm and binder according to the weight ratio of 3:1, mixing the materials in a mass ratio to obtain a mixed solution; wherein, according to the mass ratio, the binder comprises 1 part of metallographic rubber powder, 8 parts of deionized water and 1 part of modified aromatic amine;
E. And spraying the mixed solution to the ferroferric oxide particles in an environment of 80 ℃ to enable the mixed solution to wrap the ferroferric oxide particles, so as to obtain the ferroferric oxide composite particles, wherein the structural schematic diagram of the ferroferric oxide composite particles is shown in figure 4.
Example 3
A. Preparing a hollow round reactant by utilizing reaction raw materials through hydrothermal reaction; wherein, the reaction raw materials of ferric chloride hexahydrate, urea and ethylene glycol are added according to the mass ratio of 1:2, enough ethylene glycol, the reaction temperature of the hydrothermal reaction is 180 ℃, and the reaction time is 550min;
B. Washing the reactant by deionized water and absolute ethyl alcohol in sequence, and drying at 80 ℃ for 720min to obtain a ferroferric oxide precursor;
C. Calcining the ferroferric oxide precursor in an argon environment at the temperature of 500 ℃ for 200min to obtain hollow round ferroferric oxide particles;
D. Grinding material with the diameter of 10-800 nm and binder according to the weight ratio of 3:1, mixing the materials in a mass ratio to obtain a mixed solution; wherein, according to the mass ratio, the binder comprises 1 part of metallographic rubber powder, 8 parts of deionized water and 1 part of modified aromatic amine;
E. And spraying the mixed solution to the ferroferric oxide particles in the environment of 90 ℃ to enable the mixed solution to wrap the ferroferric oxide particles, so as to obtain the ferroferric oxide composite particles, wherein the structural schematic diagram of the ferroferric oxide composite particles is shown in figure 5.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless it is specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective parts shown in the drawings are not drawn in actual scale for convenience of description. Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.
In the description of the present invention, it should be understood that the azimuth or positional relationships indicated by the azimuth terms such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal", and "top, bottom", etc., are generally based on the azimuth or positional relationships shown in the drawings, merely to facilitate description of the present invention and simplify the description, and these azimuth terms do not indicate and imply that the apparatus or elements referred to must have a specific azimuth or be constructed and operated in a specific azimuth, and thus should not be construed as limiting the scope of protection of the present invention; the orientation word "inner and outer" refers to inner and outer relative to the contour of the respective component itself.
Spatially relative terms, such as "above … …," "above … …," "upper surface on … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations "above … …" and "below … …". The device may also be positioned in other different ways (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
In addition, the terms "first", "second", etc. are used to define the components, and are only for convenience of distinguishing the corresponding components, and the terms have no special meaning unless otherwise stated, and therefore should not be construed as limiting the scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and the claims of the present application and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that embodiments of the application described herein may be implemented in sequences other than those illustrated or otherwise described herein.
The technical principle of the present invention is described above in connection with the specific embodiments. The description is made for the purpose of illustrating the general principles of the invention and should not be taken in any way as limiting the scope of the invention. Other embodiments of the invention will be apparent to those skilled in the art from consideration of this specification without undue burden.
Claims (7)
1. A method for preparing ferroferric oxide composite particles for magnetorheological polishing, which is characterized by comprising the following steps:
A. preparing reactants with preset shapes by utilizing reaction raw materials through hydrothermal reaction; the reaction raw materials comprise ethylene glycol, urea and ferric chloride hexahydrate, and the preset shape is a flower shape;
B. cleaning the reactant in the step A by using a cleaning agent, and drying to obtain a ferroferric oxide precursor;
C. Calcining the ferroferric oxide precursor in the step B in an inert gas environment to obtain ferroferric oxide particles with a preset shape;
D. mixing an abrasive with a binder to obtain a mixed solution;
E. Spraying the mixed solution in the step D to the ferroferric oxide particles in the step C, so that the mixed solution wraps the ferroferric oxide particles to obtain ferroferric oxide composite particles;
In the step A, the adding ratio of the ferric chloride hexahydrate to the urea is 1:2, the reaction temperature of the hydrothermal reaction is 160-180 ℃ and the reaction time is 350-400 min;
In the step C, the calcination temperature is 400-500 ℃ and the calcination time is 150-200 min;
In the step E, the wrapping temperature is 70-90 ℃.
2. The method for preparing ferroferric oxide composite particles for magnetorheological polishing according to claim 1, wherein in the step B, the cleaning agent comprises deionized water and absolute ethyl alcohol, the drying temperature is 60-80 ℃, and the drying time is 480-720 min.
3. The method for preparing ferroferric oxide composite particles for magnetorheological polishing according to claim 1, wherein in the step D, the mixing ratio of the abrasive to the binder is 3: (0.5-1.5);
the grain diameter of the abrasive is 10-800 nm;
According to the mass ratio, the adhesive comprises 1-2 parts of sizing material, 8-10 parts of deionized water and 1-2 parts of curing agent, wherein the sizing material is any one of metallographic sizing powder and acrylic acid powder, and the curing agent is any one of modified aromatic amine, aliphatic polyamine, alicyclic polyamine and aromatic polyamine.
4. A preparation device of ferroferric oxide composite particles for magnetorheological polishing, which is characterized by comprising a reaction seat, a material conveying mechanism, a reaction mechanism, a calcination granulating mechanism and a collecting mechanism, wherein the preparation device is used for realizing the preparation method of ferroferric oxide composite particles for magnetorheological polishing according to any one of claims 1-3;
The reaction seat is internally provided with a reaction chamber, a calcination granulating chamber and a storage chamber, the reaction mechanism is arranged in the reaction chamber and is used for preparing reactants with preset shapes by utilizing reaction raw materials through hydrothermal reaction and cleaning the reactants; the calcining and granulating mechanism is arranged in the calcining and granulating chamber and is used for drying reactants, providing an inert gas environment for calcining the ferroferric oxide precursor and spraying the mixed solution to the ferroferric oxide particles so that the mixed solution wraps the ferroferric oxide particles; the collecting mechanism is arranged in the storage chamber, the calcining and granulating chamber is communicated with the collecting mechanism, and the collecting mechanism is used for collecting and storing ferroferric oxide particles, mixed solution and ferroferric oxide composite particles;
The material conveying mechanism is arranged at the top of the reaction seat and is used for conveying reactants and cleaning agents to the reaction mechanism and transferring the cleaned reactants to the calcination granulating mechanism.
5. The apparatus for preparing ferroferric oxide composite particles for magnetorheological polishing as recited in claim 4, wherein the material conveying mechanism comprises a mounting base, a feeding assembly and a transferring assembly, the mounting base is rotatably mounted on the top of the reaction seat, the feeding assembly and the transferring assembly are spaced around the edge of the mounting base, and the feeding assembly and the transferring assembly can move up and down relative to the mounting base;
The feeding assembly is at least provided with five groups, the feeding assembly is used for conveying reactants and cleaning agents to the reaction mechanism, and the transferring assembly is used for transferring the cleaned reactants in the reaction mechanism to the calcination granulation mechanism.
6. The apparatus for preparing ferroferric oxide composite particles for magnetorheological polishing as recited in claim 5, wherein the reaction mechanism comprises a rotating base, a reaction kettle and a heating assembly; the rotary seat is rotatably arranged in the reaction chamber, a plurality of reaction kettles are arranged at the top of the rotary seat, and the reaction kettles are uniformly distributed around the edge of the mounting base at intervals;
The heating assembly comprises a heating protection cover, a first electric heating tube and a first temperature detector, wherein the heating protection cover is installed on the inner wall of the reaction chamber, the heating protection cover comprises a first high-temperature resistant layer, a first heat-preserving layer and a first heat-insulating layer from inside to outside, the first electric heating tube surrounds the inner wall of the heating protection cover, the first temperature detector is installed inside the reaction chamber, and the first temperature detector is used for detecting the temperature of the reaction chamber.
7. The apparatus for preparing ferroferric oxide composite particles for magneto-rheological polishing according to claim 4, wherein the calcination granulation mechanism comprises an air pressure adjusting component, an air supply component and a calcination component; the air pressure adjusting component is arranged in the calcining and granulating chamber and used for adjusting the air pressure of the calcining and granulating chamber, the air supply component is arranged outside the calcining and granulating chamber and communicated with the calcining and granulating chamber, and the air supply component is used for conveying inert gas to the calcining and granulating chamber;
the calcining assembly comprises a calcining protective cover, a second electric heating tube and a second temperature detector, wherein the calcining protective cover is arranged on the inner wall of the calcining granulation chamber, the calcining protective cover comprises a second high-temperature resistant layer, a second heat preservation layer and a second heat insulation layer from inside to outside, the second electric heating tube is arranged around the inner wall of the calcining protective cover, the second temperature detector is arranged inside the calcining granulation chamber, and the second temperature detector is used for detecting the temperature of the calcining granulation chamber;
The collecting mechanism comprises a first storage component, a second storage component and a third storage component which are sequentially arranged, the first storage component, the second storage component and the third storage component are respectively communicated with the calcining granulation chamber through pipelines, the first storage component is used for storing ferroferric oxide particles, the second storage component is used for storing ferroferric oxide composite particles, and the third storage component is used for storing mixed solution;
The first storage component and the second storage component have the same structure; the first storage component comprises a first storage box, a first switch valve and a filter screen, the first storage box is communicated with the calcination granulating chamber through a pipeline, the first switch valve is arranged on the pipeline and is used for opening and closing the pipeline, and the filter screen is horizontally arranged in the first storage box;
The third storage component comprises a third storage box and a third switch valve, the third storage box is communicated with the calcination granulating chamber through a pipeline, the third switch valve is arranged in the pipeline, and the third switch valve is used for opening and closing the pipeline.
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