CN115449346A - 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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- CN115449346A CN115449346A CN202211053626.XA CN202211053626A CN115449346A CN 115449346 A CN115449346 A CN 115449346A CN 202211053626 A CN202211053626 A CN 202211053626A CN 115449346 A CN115449346 A CN 115449346A
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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 154
- 238000005498 polishing Methods 0.000 title claims abstract description 68
- 239000011246 composite particle Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- 238000006243 chemical reaction Methods 0.000 claims abstract description 138
- 238000001354 calcination Methods 0.000 claims abstract description 124
- 239000002245 particle Substances 0.000 claims abstract description 66
- 239000000376 reactant Substances 0.000 claims abstract description 55
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000011259 mixed solution Substances 0.000 claims abstract description 39
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 239000002243 precursor Substances 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004202 carbamide Substances 0.000 claims abstract description 20
- 239000012459 cleaning agent Substances 0.000 claims abstract description 20
- 239000011230 binding agent Substances 0.000 claims abstract description 18
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 18
- 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 18
- 238000004140 cleaning Methods 0.000 claims abstract description 16
- 239000011261 inert gas Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000005507 spraying Methods 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 7
- 230000007246 mechanism Effects 0.000 claims description 88
- 238000003860 storage Methods 0.000 claims description 86
- 238000005469 granulation Methods 0.000 claims description 52
- 230000003179 granulation Effects 0.000 claims description 52
- 239000000463 material Substances 0.000 claims description 45
- 238000010438 heat treatment Methods 0.000 claims description 26
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 16
- 238000005485 electric heating Methods 0.000 claims description 14
- 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
- 150000004982 aromatic amines Chemical class 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000004513 sizing Methods 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 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
- 239000000853 adhesive Substances 0.000 claims description 3
- 230000001070 adhesive effect Effects 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
- 238000012545 processing Methods 0.000 abstract description 20
- 238000007517 polishing process Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 18
- 230000008569 process Effects 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 239000006249 magnetic particle Substances 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000010586 diagram Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 230000009471 action Effects 0.000 description 6
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- 238000004519 manufacturing process Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 230000002349 favourable effect Effects 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 2
- 230000000712 assembly Effects 0.000 description 2
- 238000000429 assembly Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 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
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 230000014509 gene expression Effects 0.000 description 1
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- 238000009434 installation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron alkoxide Chemical class 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
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- 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
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- 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 a reactant with a preset shape by using reaction raw materials through a hydrothermal reaction; the reaction raw materials comprise ethylene glycol, urea and ferric chloride hexahydrate, and the preset shapes comprise polygons, flower shapes, hollow circles or solid spheres; 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 a preset shape; 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, which is provided by the scheme, is simple, has strong 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.
Description
Technical Field
The invention relates to the technical field of ultraprecise processing, 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, the viscosity and the yield stress of the magnetorheological fluid can be increased rapidly, the magnetorheological fluid has solid-like mechanical properties, and the rheological process of the magnetorheological fluid has reversibility and controllability. Polishing hard and brittle materials by utilizing the rheological property of the magnetorheological fluid has become one of the hot spots of the research of the advanced processing technology. With the development of science and technology, people have higher and higher requirements on the processing precision of materials, such as the surface precision of crystal faces, parts of precision instruments and the like, and the higher requirements are also provided for the magnetorheological processing. Compared with conventional polishing, magnetorheological polishing has the advantage of not introducing new subsurface damage during polishing.
The performance of the magnetorheological polishing solution has a crucial influence on the magnetorheological polishing effect, and the traditional magnetorheological polishing solution mainly comprises base carrier liquid, magnetosensitive particles, an abrasive and an additive. In magnetorheological polishing, the abrasive acts as a "tool," while the magnetic particle chains act as a polishing pad. In other words, the chain structure of magnetic particles "entrains" the abrasive for polishing. Therefore, the processing using the conventional magnetorheological polishing fluid has the following disadvantages: (1) The magnetic particles of the traditional magnetorheological polishing solution are spherical carbonyl iron powder, so that the holding effect on the grinding materials in the processing process is limited, and the magnetorheological polishing efficiency is influenced. (2) The magnetic particles and the abrasive are randomly mixed and distributed in the base carrier liquid in the processing process, and when the abrasive particles act on a workpiece, the magnetic particles also have a certain removing effect on the workpiece, so that the magnetic particles are easily abraded, the service life of the magnetorheological polishing liquid is further shortened, and the polishing effect is even influenced. (3) The abrasive material is clamped by the magnetic particles for polishing, the action of the abrasive material on a workpiece is random, and the polishing uniformity cannot be ensured. (4) When the size of the abrasive in the magnetorheological polishing solution is not uniform, the abrasive with smaller size is easier to be held by the magnetic particles, so that a part of the abrasive cannot be fully utilized, the polishing efficiency is reduced, and the magnetorheological polishing effect is even influenced.
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 also aims to provide a device for realizing the preparation method of the ferroferric oxide composite particles for magnetorheological polishing, which has the advantages of simple structure and convenient use, and is convenient for preparing 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.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of ferroferric oxide composite particles for magnetorheological polishing comprises the following steps:
A. preparing a reactant with a preset shape by using reaction raw materials through a hydrothermal reaction; 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;
B. cleaning the reactant obtained 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 obtained in the step D to the ferroferric oxide particles obtained in the step C, and enabling the mixed solution to wrap the ferroferric oxide particles to obtain the ferroferric oxide composite particles.
Preferably, in the step a, the adding ratio of the ferric chloride hexahydrate and 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 in the drying step is 60-80 ℃, and the drying time is 480-720 min.
Preferably, in the step C, the calcining temperature in the calcining step is 400-500 ℃, and the calcining 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 rubber powder and acrylic acid powder, and the curing agent is any one of modified arylamine, aliphatic polyamine, alicyclic polyamine and aromatic polyamine.
Preferably, in the step E, the wrapping temperature in the wrapping step is 70-90 ℃.
A preparation device of 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 calcining and granulating mechanism and a collecting mechanism;
the reaction seat is internally provided with a reaction chamber, a calcining granulation chamber and a storage chamber, the reaction mechanism is arranged inside the reaction chamber and is used for preparing a reactant with a preset shape by using a reaction raw material through a hydrothermal reaction and cleaning the reactant; the calcining and granulating mechanism is arranged in the calcining and granulating chamber, and is used for drying reactants, providing an inert gas environment to calcine the ferroferric oxide precursor, and spraying the mixed solution to the ferroferric oxide particles to wrap the ferroferric oxide particles with the mixed solution; the collecting mechanism is arranged in the storage chamber 13, the calcining granulation 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 1 and is used for conveying reactants and cleaning agents to the reaction mechanism and also used for transferring the cleaned reactants to the calcining and 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 at 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 and 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 calcining and granulating mechanism.
Preferably, the reaction mechanism comprises a rotating seat, a reaction kettle and a heating assembly; the rotating seat is rotatably arranged in the reaction chamber, a plurality of reaction kettles are arranged on the top of the rotating seat, and the reaction kettles are uniformly distributed around the edge of the mounting base at intervals;
heating element includes heating safety cover, first electrothermal tube and first thermodetector, the heating safety cover install in the inner wall of reaction chamber, just the heating safety cover from interior to exterior includes first high temperature resistant layer, first heat preservation and first insulating layer, first electrothermal tube centers on the inner wall setting of heating safety cover, first thermodetector install in the inside of reaction chamber, just first thermodetector is used for detecting the temperature of reaction chamber.
Preferably, the calcining and granulating mechanism comprises an air pressure adjusting assembly, an air supply assembly and a calcining assembly; the air pressure adjusting assembly is arranged inside the calcining granulation chamber and is used for adjusting the air pressure of the calcining granulation chamber, the air supply assembly is arranged outside the calcining granulation chamber and is communicated with the calcining granulation chamber, and the air supply assembly is used for conveying inert gas to the calcining granulation chamber;
the calcining assembly comprises a calcining protection cover, a second electric heating pipe and a second temperature detector, the calcining protection cover is installed on the inner wall of the calcining granulation chamber and 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 pipe is arranged around the inner wall of the calcining protection cover, the second temperature detector is installed 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 assembly, a second storage assembly and a third storage assembly which are sequentially arranged, the first storage assembly, the second storage assembly and the third storage assembly are respectively communicated with the calcining and granulating chamber through pipelines, the first storage assembly is used for storing ferroferric oxide particles, the second storage assembly is used for storing ferroferric oxide composite particles, and the third storage assembly is used for storing mixed solution;
the first storage assembly and the second storage assembly 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 granulation chamber through a pipeline, the first switch valve is arranged on the pipeline and 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 on-off valve, the third storage box is communicated with the calcination and granulation chamber through a pipeline, the third on-off valve is arranged in the pipeline, and the third on-off 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:
1. through the compounding of the ferroferric oxide particles with the preset shapes and the grinding materials, on one hand, 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, and the service life of the magnetorheological polishing solution is prolonged.
2. The preparation device integrates a plurality of functions of the material conveying mechanism, the reaction mechanism, the calcining granulation mechanism and the collection mechanism, and the occupied space of the preparation device is greatly saved. The reaction mechanism works through a plurality of reaction kettles simultaneously, so that the preparation efficiency of the ferroferric oxide composite particles is greatly improved, the final composite product can be output by charging once, 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 diagram of a device for preparing ferroferric oxide composite particles for magnetorheological polishing, according to the invention.
FIG. 2 is a schematic flow chart of the working states of a calcining granulation mechanism and a collecting mechanism in the preparation device of ferroferric oxide composite particles for magnetorheological polishing.
Fig. 3 is a schematic structural diagram of the ferroferric oxide composite particles of example 1 in a preparation method of the ferroferric oxide composite particles for magnetorheological polishing according to the present invention.
Fig. 4 is a schematic structural diagram of the ferroferric oxide composite particles of example 2 in a method for preparing ferroferric oxide composite particles for magnetorheological polishing according to the present invention.
Fig. 5 is a schematic structural diagram of the ferroferric oxide composite particles of example 3 in a preparation method of the ferroferric oxide composite particles for magnetorheological polishing according to the present invention.
Wherein: a reaction seat 1, a reaction chamber 11, a calcining granulation chamber 12 and a storage chamber 13;
the device comprises a material conveying mechanism 2, a mounting base 21, a feeding assembly 22 and a transferring assembly 23;
the reaction mechanism 3, the rotary base 31, the reaction kettle 32, the heating component 33, the first electric heating tube 331, the first temperature detector 332, and the heating protective cover 333;
a calcining granulation mechanism 4, a calcining component 41, a calcining protection cover 413, a second electric heating tube 411 and a second temperature detector 412;
a collecting mechanism 5, a first storage component 51, a first storage box 511, a first switch valve 512, a filter screen 513, a second storage component 52, a third storage component 53, a third storage box 531 and a third switch valve 532.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
The technical scheme provides a preparation method of ferroferric oxide composite particles for magnetorheological polishing, which comprises the following steps:
A. preparing a reactant with a preset shape by using reaction raw materials through a 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;
B. 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 obtained in the step D to the ferroferric oxide particles obtained in the step C, and enabling the mixed solution to wrap 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 scheme firstly passes through BGlycol, urea and hexahydrated iron chloride are subjected to hydrothermal reaction to generate a reactant (namely ferroferric oxide) with a preset shape, and compared with the traditional process in which carbonyl iron powder is used as magnetic particles, the scheme utilizes the ferroferric oxide generated by the hydrothermal reaction as the magnetic particles, so that the hardness of the ferroferric oxide is higher, and the ferroferric oxide is more beneficial to effectively grinding the surface of a polished workpiece in the polishing process. Specifically, the reaction principle is as follows: ethylene glycol is used as a solution and a raw material in hydrothermal reaction, and with the increase of temperature, urea in the solution can be slowly hydrolyzed to obtain OH - Ions to make OH in solution - The ion concentration gradually increases to form an alkaline environment. Fe under high temperature and alkaline environment 3+ Will combine with ethylene glycol to generate iron alkoxide precursor crystal nucleus, and the crystal nucleus grows continuously to finally form reactant with certain shape.
It should be noted that 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 above factors can be adjusted according to actual polishing needs to meet the polishing needs. In a preferred embodiment of the present invention, the shape of the reactant is preferably polygonal (especially irregular polygonal), flower, hollow round or solid sphere: the irregular polygonal ferroferric oxide has larger friction force between the surface of the irregular polygonal ferroferric oxide and the base carrier liquid, so the sedimentation stability of the magnetorheological polishing liquid is facilitated, and the normal and efficient polishing function of the magnetorheological polishing liquid is facilitated. Due to the structural particularity of the flower-shaped ferroferric oxide, when the magnetic chain string is formed, blade structures among particles can be mutually staggered, so that the connection strength of the magnetic chain string is improved, the holding force of the magnetic chain string on the grinding materials is further improved, and the polishing efficiency is improved. The density of the hollow round ferroferric oxide is lower, and the stability of the magnetorheological polishing solution is improved, so that the normal magnetorheological polishing and the efficient polishing function can be ensured. The solid spherical ferroferric oxide has good magnetic induction intensity, so that the high efficiency of the polishing process can be effectively ensured.
And then, cleaning the reactant obtained in the step A, removing reaction impurities remained on the surface of the reactant, and drying to obtain the ferroferric oxide precursor. And D, calcining the ferroferric oxide precursor in the step B in an inert gas (such as argon, nitrogen and the like) environment, so that the ferroferric oxide precursor is decomposed under the action of high temperature and reduced into ferroferric oxide particles with a preset shape. Specifically, the process for preparing the ferroferric oxide particles through the hydrothermal reaction in the scheme comprises the following reaction stages:
(1)CO(NH 2 ) 2 +H 2 O→2NH 3 ·H 2 O↑+CO 2
(2)
(3)
(4)
and finally, spraying a mixed solution obtained by mixing the grinding material and the binder to the ferroferric oxide particles to wrap the ferroferric oxide particles with the mixed solution to obtain the ferroferric oxide composite particles.
The scheme provides a preparation method of ferroferric oxide composite particles for magnetorheological polishing aiming at the problems of the traditional magnetorheological polishing solution, and the grinding material is coated on the outer layer of the ferroferric oxide particles, so that the efficiency and uniformity of the magnetorheological polishing are improved, the holding effect of the ferroferric oxide particles on the grinding material is improved, 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 cost of the magnetorheological polishing is reduced.
It should be noted that the abrasive in this embodiment may be a diamond abrasive.
In step a, the addition ratio of the ferric chloride hexahydrate and 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 the ferric chloride hexahydrate and the urea in the reaction raw materials, and the temperature and the time of the hydrothermal reaction, and the glycol in the preparation process is sufficient, and is not limited herein.
More specifically, when polygonal ferroferric oxide granules are prepared, the addition ratio of the ferric chloride hexahydrate and the 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 the ferric chloride hexahydrate and the urea is preferably 1:2, the reaction temperature of the hydrothermal reaction is 160-180 ℃, and the reaction time is 350-400 min; when hollow round ferroferric oxide particles are prepared, the addition ratio of the ferric chloride hexahydrate and the urea is preferably 1:2, the reaction temperature of the hydrothermal reaction is 160-180 ℃, and the reaction time is 500-550 min; when preparing solid spherical ferroferric oxide particles, the addition ratio of the ferric chloride hexahydrate and the urea is preferably 1:2, the reaction temperature of the hydrothermal reaction is 180-230 ℃, and the reaction time is 900-1000 min.
In step B, the cleaning agent comprises deionized water and absolute ethyl alcohol, the drying temperature in the drying step is 60-80 ℃, and the drying time is 480-720 min.
In a preferred embodiment of the present technical solution, the residual impurities and reaction raw materials on the surface of the reactant can be cleaned by using absolute ethanol and deionized water, and the specific steps are firstly removing the reaction impurities from the deionized water, then dissolving the residual ethylene glycol in the reactant in the absolute ethanol, and simultaneously removing the deionized water in the previous step from the absolute ethanol to perform a double cleaning function. And the drying step is to remove the residual deionized water and absolute ethyl alcohol in the cleaning process, so as to ensure that the milled powder effectively wraps the ferroferric oxide particles in the subsequent steps.
In step C, the calcining temperature in the calcining step is 400 to 500 ℃, and the calcining time is 150 to 200min.
The aim of calcination is 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 scheme controls the temperature and time of the calcining step, and is favorable for preparing ideal ferroferric oxide particles.
In step D, the mixing ratio of the abrasive to the binder is 3: (0.5 to 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 rubber powder and acrylic acid powder, and the curing agent is any one of modified arylamine, aliphatic polyamine, alicyclic polyamine and aromatic polyamine.
In one embodiment of the present disclosure, the mixing mass ratio of the abrasive to the binder is 3: (0.5-1.5) is favorable for uniformly coating the grinding material on the surfaces of the ferroferric oxide particles in the granulation step. The grain size of the grinding material is 10-800 nm, so that the grinding material can be more uniformly coated on the surface of ferroferric oxide grains; on the other hand, in magnetorheological polishing, the polishing effect of the abrasive in the particle size range is better.
The scheme also provides a raw material and a proportion of the binder for wrapping abrasive particles on the surfaces of the ferroferric oxide particles, and when the raw materials are mixed according to the proportion of the scheme, the raw materials are favorable for fast reaction with air at a certain temperature to be condensed.
In step E, the wrapping temperature in the wrapping step is 70 to 90 ℃.
In a more preferred embodiment of the technical scheme, the wrapping temperature in the wrapping step is 70-90 ℃, which is beneficial to quickly bonding the ferroferric oxide particles and the grinding material under the action of the binder to form the composite particles.
A preparation device of ferroferric oxide composite particles for magnetorheological polishing is used for realizing the preparation method of the ferroferric oxide composite particles for the magnetorheological polishing, and comprises a reaction seat 1, a material conveying mechanism 2, a reaction mechanism 3, a calcining and granulating mechanism 4 and a collecting mechanism 5;
the reaction seat 1 is internally provided with a reaction chamber 11, a calcining granulation chamber 12 and a storage chamber 13, the reaction mechanism 3 is arranged inside the reaction chamber 11, and the reaction mechanism 3 is used for preparing a reactant with a preset shape by using a reaction raw material through a hydrothermal reaction and cleaning the reactant; the calcining and granulating mechanism 4 is arranged inside the calcining and granulating chamber 12, and the calcining and granulating mechanism 4 is used for drying reactants, providing an inert gas environment for calcining a ferroferric oxide precursor, and spraying a mixed solution to ferroferric oxide particles to wrap the ferroferric oxide particles with the mixed solution; the collecting mechanism 5 is arranged in the storage chamber 13, the calcining granulation chamber 12 is communicated with the collecting mechanism 5, and the collecting mechanism 5 is used for collecting and storing ferroferric oxide particles, mixed solution and 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 calcining and granulating mechanism 4.
The scheme also provides a device for realizing the preparation method of the ferroferric oxide composite particles for magnetorheological polishing, as shown in the figure 1-2, the device is simple in structure and convenient to use, and the ferroferric oxide composite particles are convenient to prepare, so that the processing quality and the processing efficiency of the surface of a polished workpiece are improved in the magnetorheological polishing process.
More specifically, the material conveying mechanism 2 comprises a mounting base 21, a feeding assembly 22 and a transferring assembly 23, 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 both the feeding assembly 22 and the transferring assembly 23 can move up and down relative to the mounting base 21;
the feeding assembly 22 is provided with at least five groups, the feeding assembly 22 is used for conveying reactants and cleaning agents to the reaction mechanism 3, and the transferring assembly 23 is used for transferring the cleaned reactants in the reaction mechanism 3 to the calcining and granulating mechanism 4.
The material conveying mechanism 2 is used for injecting raw materials of hydrothermal reaction into the reaction mechanism 3, so that the preparation of reactants is realized; used for injecting the cleaning agent into the reaction mechanism 3, thus realize the cleaning of reactant; and the device is also used for transferring the cleaned reactant to the calcining and granulating mechanism 4, so that the subsequent preparation process is convenient to carry out.
Specifically, the material conveying mechanism 2 comprises a mounting base 21, a feeding assembly 22 and a transferring assembly 23, wherein the feeding assembly 22 and the transferring assembly 23 are mounted on the mounting base 21 and rotate along with the rotation of the mounting base 21, so that the feeding assembly 22 and the transferring assembly 23 can move to the upper part of the reaction chamber 11 or the calcining and pelletizing chamber 12 according to the requirement. 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 reaction raw materials and cleaning agents can be accurately conveyed to the reaction mechanism 3, and waste is avoided; the up-and-down movement of the rotating assembly 23 facilitates the complete extraction of the reactant from the reaction mechanism 3, thereby ensuring the production amount of the reactant.
More specifically, the feed assembly 22 is provided with at least five groups, and the five groups of feed assemblies 22 can be used for conveying ethylene glycol, urea, ferric chloride hexahydrate, deionized water and absolute ethyl alcohol, respectively, and are not limited herein.
It should be noted that the feeding assembly 22 in the present embodiment may be a feeding piston or other conventional feeding device in the art, and the transferring assembly 23 is a material conveying device capable of taking and discharging materials in the conventional art, and is not limited herein.
To explain further, the reaction mechanism 3 includes a rotary base 31, a reaction kettle 32 and a heating assembly 33; the rotary base 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 on the top of the rotary base 31, and the reaction kettles 32 are uniformly distributed around the edge of the installation base 21 at intervals;
heating element 33 includes heating safety cover 333, first electrothermal tube 331 and first thermodetector 332, heating safety cover 333 install in the inner wall of reaction chamber 11, just heating safety cover 333 from interior to exterior includes first high temperature resistant layer, first heat preservation and first insulating layer, first electrothermal tube 331 centers on the inner wall setting of heating safety cover 333, first thermodetector 332 install in the inside of reaction chamber 11, just first thermodetector 332 is used for detecting the temperature of reaction chamber 11.
The reaction mechanism 3 of the present embodiment is used for preparing a reactant in a preset shape by hydrothermal reaction using reaction raw materials, and cleaning the reactant.
Specifically, the reaction mechanism 3 includes a rotary base 31, a reaction kettle 32 and a heating assembly 33; the reaction kettle 32 is mounted at the top of the mounting base 21 and rotates along with the rotation of the rotary seat 31, so that the reaction kettle 32 moves to the position below the feeding component 22 or the transferring component 23, accurate addition of reaction raw materials and cleaning agents is facilitated, and meanwhile, cleaned reactants can be conveniently taken out of the reaction kettle 32 by the transferring component 23; in addition, in the hydrothermal reaction process and the cleaning process, the rotary seat 31 can drive the reaction kettle 32 to rotate centrifugally, so that the uniform mixing of the reaction raw materials in the reaction kettle 32 is accelerated, and the cleaning efficiency is accelerated. The heating element 33 is mainly used to provide the heating temperature required in the hydrothermal reaction (specifically, the first electrothermal tube 331); in addition, the heating assembly 33 is further provided with a first temperature detector 332 for detecting the temperature of the reaction chamber 11, so that the controllability of a technician in the preparation process of the composite particles is improved, and accurate temperature control is ensured; the heating protective cover 333 comprises a first high temperature resistant layer, a first heat preservation layer and a first heat insulation layer from inside to outside, wherein the first high temperature resistant layer is used for preventing the high temperature generated by the first electric heating tube 331 from damaging external mechanical and circuit structures; the first heat-preservation layer wraps the outer surface of the first high-temperature-resistant layer to reduce temperature loss; the first heat insulation layer wraps the outside of the first heat insulation layer, so that the temperature loss is further prevented, the high temperature in the reaction chamber 11 cannot be conducted to other places of the reaction seat 1, and the influence on the normal operation of other reactions is avoided.
It should be noted that the rotation speed of the rotating seat 31 in the present embodiment is preferably 50 to 100r/min in the hydrothermal reaction process, and the rotation speed in the centrifugal cleaning process is preferably 5000 to 10000r/min, so that the precursor and the cleaning agent are layered under the action of centrifugal force, the precursor with heavy mass is precipitated at the bottom, and the cleaning agent is on the upper layer, which facilitates the separation of the ferroferric oxide precursor and the cleaning agent. In the present embodiment, each layer of the heating protection cover 333 is made of a conventional material that can achieve the relevant function, for example, the first thermal insulation layer may be made of a material such as thermal insulation cotton, which is not limited herein.
Further, the calcining granulation mechanism 4 comprises an air pressure adjusting component, an air supply component and a calcining component 41; the air pressure adjusting component is installed inside the calcination granulation chamber 12, and is used for adjusting the air pressure of the calcination granulation chamber 12, the air supply component is arranged outside the calcination granulation chamber 12, and is communicated with the calcination granulation chamber 12, and is used for conveying inert gas to the calcination granulation chamber 12;
the calcining assembly 41 comprises a calcining protection cover 413, a second electric heating tube 411 and a second temperature detector 412, the calcining protection cover 413 is installed on the inner wall of the calcining granulation chamber 12, the calcining protection 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 calcining protection cover 413, the second temperature detector 412 is installed inside the calcining granulation chamber 12, and the second temperature detector 412 is used for detecting the temperature of the calcining granulation chamber 12;
the collecting mechanism 5 comprises a first storage assembly 51, a second storage assembly 52 and a third storage assembly 53 which are sequentially arranged, the first storage assembly 51, the second storage assembly 52 and the third storage assembly 53 are respectively communicated with the calcining and granulating chamber 12 through pipelines, the first storage assembly 51 is used for storing ferroferric oxide particles, the second storage assembly 52 is used for storing ferroferric oxide composite particles, and the third storage assembly 53 is used for storing mixed solution;
the first storage assembly 51 and the second storage assembly 52 have the same structure; the first storage module 51 comprises a first storage box 511, a first switch valve 512 and a filter screen 513, wherein the first storage box 511 is communicated with the calcination 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 module 53 includes a third storage box 531 and a third open/close valve 532, the third storage box 531 is communicated with the calcination granulation chamber 12 through a pipeline, the third open/close valve 532 is disposed in the pipeline, and the third open/close valve 532 is used for opening and closing the pipeline.
The calcining and granulating mechanism 4 in the scheme is used for calcining the ferroferric oxide precursor in the environment of inert gas (such as argon, nitrogen and the like), and the mixed solution is sprayed to the ferroferric oxide particles in the step C, so that the mixed solution wraps the ferroferric oxide particles.
Specifically, the calcining granulation mechanism 4 includes an air pressure adjusting assembly (not shown), an air supply assembly (not shown), and a calcining assembly 41; the internal air pressure of the calcining and granulating chamber 12 can be adjusted according to the requirements in the preparation process through the air pressure adjusting component so as to achieve the preparation purpose; the gas supply assembly is used for providing an inert environment for the calcination process of the precursor; the calcination component 41 is mainly used to provide the reaction temperature required in the drying step, the calcination step and the granulation step (specifically realized by the second electrothermal tube 411); in addition, the calcining assembly 41 is further provided with a second temperature detector 412 for detecting the temperature of the calcining granulation chamber 12, so that the controllability of technicians in the preparation process of the composite particles is improved, and accurate temperature control is ensured; the calcination protecting cover 413 comprises a second high temperature resistant layer, a second 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 electrothermal tube 411 from damaging external machinery and circuit structures; the second heat-insulating layer wraps the second high-temperature-resistant layer to reduce temperature loss; the second heat insulating layer wraps the outside of the second heat insulating layer, so that the temperature loss is further prevented, the high temperature in the calcining granulation chamber 12 cannot be conducted to other places of the reaction seat 1, and the influence on the normal operation of other reactions is avoided.
In the present embodiment, each layer of the calcined protective cover 413 is made of a conventional material that can perform the relevant function, for example, the second thermal insulation layer can be made of a material such as thermal insulation cotton, and the invention is not limited thereto.
In addition, in the scheme, the first storage component 51 of the collecting mechanism 5 is used for collecting and storing 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. Wherein, the three storage assemblies 51 are respectively provided with a switch valve connected with the pipeline of each storage box, and the communication between the storage box and the calcining and granulating chamber 12 can be controlled by the switch valve, so that the preparation process of the ferroferric oxide composite particles can be flexibly realized. Further, the first storage subassembly 51 and the second storage subassembly 53 of this scheme still are provided with filter screen 513, and filter screen 513's setting is still favorable to the collection to granule class result, promotes it and collects the purity.
More specifically, the working process of the device for preparing the ferroferric oxide composite particles for magnetorheological polishing comprises the following steps: (1) The reaction raw materials are conveyed to the reaction kettle 32 through the feeding assembly 22, and the rotary 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 to make the reaction raw materials in the reaction kettle 32 generate a reactant with a preset shape through a hydrothermal reaction, and the first electric heating tube 331 is turned off after the reaction is finished. (2) Conveying the cleaning agent to the reaction kettle 32 through the feeding assembly 22, and starting the rotary seat 31 to centrifugally clean the reaction raw materials in the reaction kettle 32; after the washing, the washed reactant is transferred to the calcining granulation chamber 12 through the transfer assembly 23, and the second electric heating tube 411 is opened to dry the washed reactant, so as to obtain the ferroferric oxide precursor. (3) Continuously introducing inert gas into the calcining and granulating chamber 12 by using the gas supply assembly, exhausting the air in the calcining and granulating chamber 12, adjusting the temperature of the second electric heating tube 411, so that the ferroferric oxide precursor is calcined and decomposed 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 state a in fig. 2. (4) The abrasive is mixed with the binder to obtain a mixed solution and stored in the third storage unit 53. (5) The first on-off valve 512 of the first storage module 51 is opened, and the third on-off valve 532 of the third storage module 53 is opened, the air pressure regulating module is started, so that the calcination and granulation chamber 12 is under negative pressure, and the ferroferric oxide granules in the first storage box 511 and the mixed solution in the third storage box 531 are flushed into the calcination and granulation chamber 12 under the negative pressure, as shown in state B in fig. 2. Then, the first on-off valve 512 of the first storage assembly 51 and the third on-off valve 532 of the third storage assembly 53 are closed, the temperature of the second electric heating tube 411 and the inert gas introducing rate of the gas supply assembly are adjusted, and the mixed solution in the calcining and granulating chamber 12 is made to fully wrap the ferroferric oxide particles, so that the ferroferric oxide composite particles are obtained. After the granulation is completed, the first on-off 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, and the preparation of the ferroferric oxide composite particles is completed.
The preparation device in the scheme integrates a plurality of functions of the material conveying mechanism 2, the reaction mechanism 3, the calcining granulation mechanism 4 and the collection mechanism 5, and the occupied space of the preparation device is greatly saved. The reaction mechanism 3 works through a plurality of reaction kettles 32 simultaneously, so that the preparation efficiency of the ferroferric oxide composite particles is greatly improved, the final composite product can be output by feeding once, 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 hydrothermal reaction by using reaction raw materials; the method comprises the following steps of preparing reaction raw materials of ferric chloride hexahydrate, urea and glycol, wherein the adding proportion of the ferric chloride hexahydrate and the urea is 2:1, enough ethylene glycol is added, the reaction temperature of the hydrothermal reaction is 160 ℃, and the reaction time is 500min;
B. washing reactants by using deionized water and absolute ethyl alcohol in sequence, and drying at the temperature of 60 ℃ for 480min to obtain a ferroferric oxide precursor;
C. calcining the ferroferric oxide precursor for 150min at the temperature of 400 ℃ in an argon environment to obtain polygonal ferroferric oxide particles;
D. grinding materials with the particle size of 10-800 nm and a binder are mixed according to the proportion of 3:1 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 arylamine;
E. and (3) spraying the mixed solution to the ferroferric oxide particles at the temperature of 70 ℃ to enable the mixed solution to wrap the ferroferric oxide particles to obtain the ferroferric oxide composite particles, wherein the structural schematic diagram is shown in figure 3.
Example 2
A. Preparing a flower-shaped reactant by using reaction raw materials through a hydrothermal reaction; the reaction raw materials of ferric chloride hexahydrate, urea and ethylene glycol are mixed according to a mass ratio of 1:2, enough glycol is added, the reaction temperature of the hydrothermal reaction is 170 ℃, and the reaction time is 400min;
B. washing reactants by using deionized water and absolute ethyl alcohol in sequence, and drying at the temperature of 70 ℃ for 560min to obtain a ferroferric oxide precursor;
C. calcining the ferroferric oxide precursor for 180min at 450 ℃ in an argon environment to obtain flower-shaped ferroferric oxide particles;
D. grinding materials with the particle size of 10-800 nm and a binder are mixed according to the proportion of 3:1 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 arylamine;
E. and (3) spraying the mixed solution to the ferroferric oxide particles at the temperature 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 is shown in figure 4.
Example 3
A. Preparing a hollow round reactant by using reaction raw materials through a hydrothermal reaction; the method comprises the following steps of preparing reaction raw materials of ferric chloride hexahydrate, urea and glycol, wherein the adding proportion of the ferric chloride hexahydrate and the urea is 1:2, enough ethylene glycol is added, the reaction temperature of the hydrothermal reaction is 180 ℃, and the reaction time is 550min;
B. washing reactants by using deionized water and absolute ethyl alcohol in sequence, and drying at the temperature of 80 ℃ for 720min to obtain a ferroferric oxide precursor;
C. calcining the ferroferric oxide precursor for 200min at the temperature of 500 ℃ in an argon environment to obtain hollow round ferroferric oxide particles;
D. grinding materials with the particle size of 10-800 nm and a binder are mixed according to the proportion of 3:1 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 arylamine;
E. and (3) spraying the mixed solution to the ferroferric oxide particles at the temperature of 90 ℃ to enable the mixed solution to wrap the ferroferric oxide particles to obtain the ferroferric oxide composite particles, wherein the structural schematic diagram is shown in fig. 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 example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The relative arrangement of the components and steps, the 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 portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as exemplary only and not as limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.
In the description of the present invention, it is to be understood that the orientation or positional relationship indicated by the orientation words such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal" and "top, bottom", etc. are usually based on the orientation or positional relationship shown in the drawings, and are only for convenience of description and simplicity of description, and in the case of not making a reverse description, these orientation words do not indicate and imply that the device or element being referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore, should not be considered as limiting the scope of the present invention; the terms "inner and outer" refer to the inner and outer relative to the profile of the respective component itself.
For ease of description, spatially relative terms such as "over 8230 \ 8230;,"' over 8230;, \8230; upper surface "," above ", etc. may be used herein to describe the spatial relationship of one device or feature to another device or feature as shown in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary terms "at 8230; \8230; above" may include both orientations "at 8230; \8230; above" and "at 8230; \8230; below". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
It should be noted that the terms "first", "second", and the like are used to define the components, and are only used for convenience of distinguishing the corresponding components, and unless otherwise stated, the terms have no special meaning, and therefore, the scope of the present invention should not be construed as being limited.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the application described herein are capable of operation in sequences other than those illustrated or described herein.
The technical principles of the present invention have been described above with reference to specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive step, and these embodiments will fall within the scope of the present invention.
Claims (10)
1. A preparation method of ferroferric oxide composite particles for magnetorheological polishing is characterized by comprising the following steps:
A. preparing a reactant with a preset shape by using reaction raw materials through a 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;
B. 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 obtained in the step D to the ferroferric oxide particles obtained in the step C, so that the ferroferric oxide particles are wrapped by the mixed solution, and the ferroferric oxide composite particles are obtained.
2. The preparation method of ferroferric oxide composite particles for magnetorheological polishing according to claim 1, wherein 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.
3. The preparation method of 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, and the drying temperature in the drying step is 60-80 ℃ and the drying time is 480-720 min.
4. The preparation method of ferroferric oxide composite particles for magnetorheological polishing according to claim 1, wherein in the step C, the calcining temperature in the calcining step is 400-500 ℃, and the calcining time is 150-200 min.
5. The preparation method of ferroferric oxide composite particles for magnetorheological polishing according to claim 1, wherein in the step D, the mixing ratio of the grinding material to the binder is 3: (0.5 to 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 rubber powder and acrylic acid powder, and the curing agent is any one of modified arylamine, aliphatic polyamine, alicyclic polyamine and aromatic polyamine.
6. The preparation method of ferroferric oxide composite particles for magnetorheological polishing according to claim 1, wherein in the step E, the coating temperature in the coating step is 70-90 ℃.
7. A preparation device of ferroferric oxide composite particles for magnetorheological polishing is characterized in that the preparation device is used for realizing the preparation method of the ferroferric oxide composite particles for magnetorheological polishing in any one of claims 1 to 6, and comprises a reaction seat, a material conveying mechanism, a reaction mechanism, a calcining and granulating mechanism and a collecting mechanism;
the reaction seat is internally provided with a reaction chamber, a calcining granulation chamber and a storage chamber, the reaction mechanism is arranged inside the reaction chamber and is used for preparing a reactant with a preset shape by using a reaction raw material through a hydrothermal reaction and cleaning the reactant; the calcining and granulating mechanism is arranged in the calcining and granulating chamber, and is used for drying reactants, providing an inert gas environment to calcine the ferroferric oxide precursor, and spraying the mixed solution to the ferroferric oxide particles to wrap the ferroferric oxide particles with the mixed solution; the collecting mechanism is arranged in the storage chamber 13, the calcining granulation 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 1 and used for conveying reactants and cleaning agents to the reaction mechanism and transferring the cleaned reactants to the calcining and granulating mechanism.
8. The apparatus according to claim 7, 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 base, the feeding assembly and the transferring assembly are spaced around the edge of the mounting base, and both 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 and 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 calcining and granulating mechanism.
9. The device for preparing the ferroferric oxide composite particles for magnetorheological polishing according to claim 7, wherein 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 on the top of the rotary seat, and the reaction kettles are uniformly distributed around the edge of the mounting base at intervals;
heating element includes heating safety cover, first electrothermal tube and first thermodetector, the heating safety cover install in the inner wall of reaction chamber, just the heating safety cover from interior to exterior includes first high temperature resistant layer, first heat preservation and first insulating layer, first electrothermal tube centers on the inner wall setting of heating safety cover, first thermodetector install in the inside of reaction chamber, just first thermodetector is used for detecting the temperature of reaction chamber.
10. The device for preparing ferroferric oxide composite particles for magnetorheological polishing according to claim 7, wherein the calcining and granulating mechanism comprises an air pressure adjusting component, an air supply component and a calcining component; the air pressure adjusting assembly is arranged inside the calcining granulation chamber and is used for adjusting the air pressure of the calcining granulation chamber, the air supply assembly is arranged outside the calcining granulation chamber and is communicated with the calcining granulation chamber, and the air supply assembly is used for conveying inert gas to the calcining granulation chamber;
the calcining assembly comprises a calcining protection cover, a second electric heating pipe and a second temperature detector, the calcining protection cover is installed on the inner wall of the calcining granulation chamber and 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 pipe is arranged around the inner wall of the calcining protection cover, the second temperature detector is installed 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 assembly, a second storage assembly and a third storage assembly which are sequentially arranged, the first storage assembly, the second storage assembly and the third storage assembly are respectively communicated with the calcining and granulating chamber through pipelines, the first storage assembly is used for storing ferroferric oxide particles, the second storage assembly is used for storing ferroferric oxide composite particles, and the third storage assembly is used for storing mixed solution;
the first storage assembly and the second storage assembly are identical in 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 granulation chamber through a pipeline, the first switch valve is arranged on the pipeline and 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 on-off valve, the third storage box is communicated with the calcination and granulation chamber through a pipeline, the third on-off valve is arranged in the pipeline, and the third on-off valve is used for opening and closing the pipeline.
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