CN100551654C - A kind of method of preparing ceramic microball by injection-condensation and device thereof - Google Patents
A kind of method of preparing ceramic microball by injection-condensation and device thereof Download PDFInfo
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Abstract
A kind of method of preparing ceramic microball by injection-condensation and device thereof belong to technical field of ceramic material.Method the present invention of the present invention is with the stable slurry of certain solid concentration, becomes droplet by vibration, is distributed in the oil medium with uniform temperature, droplet balling-up under the effect of interfacial tension, gelation reaction takes place in the polymer monomer polymerization of drop inside, solidifies balling-up.Then through technical process such as washing, drying, roasting and sintering, the ceramic microsphere that finally obtains high finished product rate and adhere to specification.Provide the device of implementation method, comprised pressurized tank (1), glue flowmeter (2), electromagnetic vibrator (3), nozzle (4) disperses post (5), thermal source (6), ventilation equipment (7), signal generator (8), power amplifier (9).Of the present inventionly be a little, the thus obtained microsphere good sphericity, internal structure is even.Do not need mould, cost is low, helps producing in batches.
Description
Technical field
The invention belongs to technical field of ceramic material, particularly a kind of method of preparing ceramic microball by injection-condensation and device thereof.Propose slurry and be dispersed into new method of dripping and the new formula that calculates the slurry scattering parameter, also proposed the new mode that the gel reaction catalyst adds, disclose the key equipment of this method simultaneously.
Technical background
Ceramic microsphere is widely used in dyestuff, coating, printing ink, the paint production grinding agent as the chemical industry raw material, also at automobile, shipbuilding, internal combustion engine, military project, metal die, universal machine parts, instrument device, even become indispensable polishing agent in the heavy industry such as spaceship, space shuttle.Ceramic microsphere also can be made the reinforcing filler in plastics, rubber, the nylon products, can make to fill evenly.Oil exploitation industry selects for use ceramic microsphere to use as a kind of special kollag, mixes mud when drilling an oil well, and drill bit is bored down rapidly, has played effects such as reducing resistance, reduction bit wear; Ceramic microsphere can also stress on underground oil field layer as proppant, can obviously improve oil exploitation efficient.Ceramic microsphere with certain porosity can also be as the transmuting material of catalyst carrier or nuclear waste disposal.And different application backgrounds also proposes different requirements to the material of ceramic microsphere, density, sphere diameter, sphericity etc.
Liu Yongxian discloses a kind of preparation method of foam ceramic spherulite in patent (CN 1285335A).This method is to be primary raw material with the different material of melt temperatures such as glass waste residue, flyash, bentonite and pore former, binding agent, make by steps such as batching, rotating granulation, drying, calcining, autogenous grindings, can be used for the less demanding operating mode of sphericity.Yang Jinlong etc. disclose a kind of method that the method that adopts colloidal formation prepares ceramic bead in patent (ZL 02125221.1).This method is that the suspended substance that will add initator injects the funnel that can regulate diameter, enters the heated liquid oil medium from the funnel liquid bead that drips, and forms ceramic bead, and the diameter of bead is regulated by the diameter of regulating funnel.
Technology contents:
The method and the device thereof that the purpose of this invention is to provide a kind of preparing ceramic microball by injection-condensation can obtain sphere diameter by this method and can establish at the 50-2000 micron, or the ceramic microsphere of the adjustable high quality and low cost of high densification or the porosity.
The present invention has provided the computing formula that slurry disperses, and has designed homodisperse control parameter.The invention allows for the new mode that the gel reaction catalyst adds, provided the key device of realizing target simultaneously.
The present invention is with the stable slurry of certain solid concentration (water base), becomes droplet by vibration, is distributed in the oil medium with uniform temperature, droplet balling-up under the effect of interfacial tension, gelation reaction takes place in the polymer monomer polymerization of drop inside, solidifies balling-up.Then through technical process such as washing, drying, roasting and sintering, the ceramic microsphere that finally obtains high finished product rate and adhere to specification.Its method is:
1, the preparation of slurry:
The organic matter monomer and the crosslinking agent that will have free radical activity mix with water, are mixed with premixed liquid, and organic monomer and crosslinking agent account for premixed liquid quality 2～30%, and the mass ratio of monomer and crosslinking agent is 10～20: 0～1.Add ceramic powder and dispersant, wherein the solid concentration of ceramic powder in slurry is 40～60%, and dispersant dosage is 0.2～2% of a ceramic powder.
2, the preparation of suspended nitride:
Above-mentioned slurry is handled by the mode of mechanical agitation or ball milling, obtained the stable suspersion slurry of high solid loading, again by the bubble in the degassing processing elimination slurry.Stir and add initator.Initiator amount accounts for the 0.5～10wt ‰ of slip gross mass.
3, the dispersion of slurry:
Gained slurry in 2 is transferred in the pressurized tank,, adjusts the pressure and the dispersion frequency of slurry according to the size and the density requirements of design microballoon.The slurry droplet balling-up in oil medium that disperses.
If the radius of required product ceramic microsphere is R, the density of ceramic microsphere is D, and the solid concentration of ceramic powder is V in the slurry, and the density of ceramic powder is Dp,, the flow L of single injector per second, the frequency of establishing electromagnetic vibrator be f then:
The quality percentage composition of ceramic powder is in the slurry:
Then can set up equation by ceramic powder:
With (1) substitution (2), can get
Because R, D, V, Dp are known quantity, and L can survey, so can determine scattering parameter.
4, the washing of microballoon, drying, roasting and sintering
The bead of collecting is placed the Rotary drying stove that can vacuumize, wash and drying.Carry out roasting and sintering according to the corresponding system of the character of ceramic powder then, obtain the ceramic microsphere of the design size and the porosity.
The device that the above-mentioned method for preparing gel micro-ball relates to comprises the pressurized tank of placing slurry, the dispersing nozzle that is connected with pressurized tank, the electromagnetic vibrator of fixed nozzle and signal thereof take place and control device, the dispersion post of oiliness decentralized medium is housed, disperse the outer thermal source of post, with the washing that disperses post to link to each other, drying device etc.
Porcelain powder of the present invention is ZrO
2, Al
2O
3, Si
3N
4, SiC, tourmaline, cordierite, or add carbon dust as pore former; Monomer is the acrylamide with free radical activity, Methacrylamide, in N hydroxymethyl acrylamide, the acrylate 1～4 kind; Crosslinking agent is the N-N-methylene-bisacrylamide; Dispersant is ammonium polyacrylate, ammonium citrate, polyacrylic 1～3 kind.
Degassing processing of the present invention comprises and vacuumizes or add 1～2 kind of defoamer; Vacuumize and be meant that slurry vacuumizes 10～30min under the operating mode of vibration or stirring; Defoamer comprises different new ester, aliphatic acid 1～2 kind, and consumption is 0.05～2% of a ceramic powder quality.
Initator of the present invention is an ammonium persulfate, and the adding method is: with a certain amount of ammonium persulfate dissolving, the stirring arm gob adds ammonium persulfate aqueous solution then earlier.
Of the present invention catalyst n-N-N-N-tetramethylethylenediamine is joined in the oil medium, add volume ratio than being oil medium: catalyst=100: 2～4.
Oil medium of the present invention can be a kind of of methyl-silicone oil, paraffin oil, kerosene or edible oil, and oily temperature control is between 50～90 ℃.
External thermal source of the present invention is water-bath, oil bath, outward around the heating tape or microwave.
Device of the present invention comprises: pressurized tank (1), and glue flowmeter (2), electromagnetic vibrator (3), nozzle (4) disperses post (5), thermal source (6), signal generator (7), power amplifier (8), air compressor machine (9).Air compressor machine is connected by steel pipe, pressure pipe with pressurized tank, under pressure slip is injected sebific duct.Store slip in the pressurized tank, be connected with flowmeter, nozzle by sebific duct, flowmeter is controlled the flow of slip at spray nozzle front end.Electromagnetic vibrator is connected with nozzle, and power amplifier is connected with electromagnetic vibrator by holding wire, power line with signal generation apparatus.Nozzle is disperseing post top.
Major advantage of the present invention is:
1, can design the ceramic microsphere size and the porosity, and be met good sphericity, the uniformity height of designing requirement, high-quality, the high ceramic microsphere of yield rate are particularly suitable for the preparation of small size microballoon.
2, form the macromolecule network structure behind the monomer polymerization, combine densification, the bead intensity height after the moulding, good toughness, difficult broken with ceramic powder.
3, the moulding of ceramic microsphere relies on the slurry surface tension balling-up different with decentralized medium, and the gelatification of monomer is solidified, the thus obtained microsphere good sphericity, and internal structure is even.Do not need mould, cost is low, helps producing in batches.
4, the gel reaction catalyst is joined in the oil medium, when promoting microballoon to solidify, can also reduce the temperature of gel reaction greatly, reduced production cost and be beneficial to safety in production.
Description of drawings:
Accompanying drawing 1 is the equipment schematic diagram of glue dispersion and gelling.Wherein, pressurized tank 1, glue flowmeter 2, electromagnetic vibrator 3, nozzle 4 disperses post 5, thermal source 6, signal generator 7, power amplifier 8, air compressor machine 9.
Specific implementation
The preparation of embodiment 1, transmuting material zirconia ceramic ball
Raw material is commercially available ZrO
2Powder, average grain diameter are 0.5 micron.Preparation 100ml premixed liquid, mass ratio is: 82%H
2O:16% acrylamide: 2%N-N-methylene-bisacrylamide.Add ZrO
2Powder, the configuration solid concentration is 50% slurry, adds the dispersant ammonium polyacrylate, the dispersant quality is ZrO
20.5% of powder quality.Mechanical agitation 2 hours, froth in vacuum 15～30min.Add the aqueous solution (mass concentration 2%) 0.8ml of initiator ammonium persulfate, transfer to after the stirring and leave standstill 10min in the pressurized tank.The catalyst n that disperses canned an amount of methyl-silicone oil (viscosity 50mPaS, density 0.8g/ml) adding silicone oil quality 2% in the post, N, N, the N-tetramethylethylenediamine is connected and is disperseed the outer thermal source of post, and silicone oil is heated to 50 ℃ of constant temperature.Slurry pressurization 0.35MPa, single mouth flow is 1ml/s, dispersion frequency is 120S
-1, microballoon collected and transfer to wash in the Rotary drying stove and dry, (900 ℃, 2h) obtaining density is 5.3g/cm to pass through roasting and low-temperature sintering then
3, pore volume is 0.08ml/g, and specific surface is 12, and sphere diameter is 500 ± 20 μ m, the zirconia ceramic ball transmuting material of out-of-roundness＜0.02.
The preparation of embodiment 2, abrasive material zirconia ceramic ball
Raw material is commercially available Y
2O
3Stable ZrO
2Powder, average grain diameter are 1 micron.Preparation 100ml premixed liquid, mass ratio is: 92%H
2O: 7.2% acrylamide: 0.8%N-N-methylene-bisacrylamide.Add ZrO
2Powder, the configuration solid concentration is 58% slurry, adds the dispersant ammonium polyacrylate, the dispersant quality is ZrO
21.5% of powder quality.Ball milling 8 hours adds the defoamer isooctanol, and consumption is ZrO
20.7% of powder stirs a little.10 of the aqueous solution (mass concentration 5%) of adding initiator ammonium persulfate are transferred to after the stirring and are left standstill 10min in the pressurized tank.Disperse canned an amount of paraffin oil (viscosity mPaS, density g/ml) in the post, connect and disperse the outer thermal source of post, paraffin oil is heated to 80 ℃ of constant temperature.The slurry pressurization, single mouth flow is that dispersion frequency is 120S
-1, microballoon collected and transfer to wash in the Rotary drying stove and dry, behind roasting and sintering, obtain density 6.2g/cm
3, sphere diameter is 80 ± 10 μ m, out-of-roundness＜0.02, microhardness 19.12GPa, the zirconia ceramic microballoon abrasive material of any surface finish.
Embodiment 3Si
3N
4The preparation of bearing ball
Raw material is commercially available α-Si
3N
4, average grain diameter is 2 microns, with Al
2O
3, Y
2O
3Be sintering agent, particle diameter is submicron order, and mass ratio is α-Si
3N
4: Al
2O
3: Y
2O
3=93: 5: 2.Preparation 100ml premixed liquid, mass ratio is: 90%H
2O: 10%N-NMA.Add material powder, the configuration solid concentration is 56% slurry, adds the dispersant ammonium citrate, and the dispersant quality is 2% of a material powder quality.Ball milling 12 hours adds defoamer aliphatic acid, and consumption is 0.2% of a raw meal, stirs a little.Add the aqueous solution (mass concentration 10%) 0.1ml of initiator ammonium persulfate, transfer to after the stirring and leave standstill 30min in the pressurized tank.Disperse canned an amount of kerosene (viscosity mPaS, density g/ml) in the post, connect and disperse the outer thermal source of post, kerosene is heated to 60 ℃ of constant temperature.The slurry pressurization, single mouth flow is that dispersion frequency is 120S
-1, microballoon collected and transfer to wash in the Rotary drying stove and dry, behind roasting and sintering, obtain density 3.13g/cm
3, sphere diameter is 2 ± 0.01mm, out-of-roundness＜0.02, the silicon nitride ceramics bearing ball of microhardness 20.80GPa any surface finish.
The preparation of embodiment 4 tourmaline porous ceramics microballoons
Raw material is commercially available 2MgO2Al
2O
35SiO
2, average grain diameter is 8 microns, is pore creating material with the carbon dust, and its particle diameter is 20 μ m, and the mass ratio of cordierite and carbon dust is 8: 2.Preparation 100ml premixed liquid, mass ratio is: 80%H
2O: 18% hydroxy-ethyl acrylate: 2%N-N-methylene-bisacrylamide.Add material powder, the configuration solid concentration is 45% slurry, adds the dispersant polyacrylic acid, and the dispersant quality is 2% of a material powder quality.Mechanical agitation 6 hours.Add the aqueous solution (mass concentration 8%) 0.15ml of initiator ammonium persulfate, transfer to after the stirring and leave standstill 20min in the pressurized tank.Disperse canned proper amount of edible oil (viscosity mPaS, density g/ml) in the post, connect and disperse the outer thermal source of post, edible oil is heated to 70 ℃ of constant temperature.The slurry pressurization, single mouth flow is that dispersion frequency is 120S
-1, microballoon collected and transfer to wash in the Rotary drying stove and dry, behind roasting and sintering, obtain density g/cm
3, sphere diameter is 1 ± 0.01mm, out-of-roundness＜0.02, and pore volume is 0.1ml/g, and specific surface is 18, and negative ion concentration can reach 1258/cm
3
Claims (9)
1, a kind of method of preparing ceramic microball by injection-condensation is characterized in that, processing step is:
The preparation of a, slurry: the organic matter monomer and the crosslinking agent that will have free radical activity mix with water, are mixed with premixed liquid, and organic monomer and crosslinking agent account for premixed liquid quality 2～30%, and the mass ratio of monomer and crosslinking agent is 10～20: 0～1; Add ceramic powder and dispersant, wherein the solid concentration of ceramic powder in slurry is 40～60%, and dispersant dosage is 0.2～2% of a ceramic powder;
The preparation of b, suspended nitride: above-mentioned slurry is handled by the mode of mechanical agitation or ball milling, obtained the stable suspersion slurry, again by the bubble in the degassing processing elimination slurry; Stir the adding initator, initiator amount accounts for the 0.5～10wt ‰ of slip gross mass;
The dispersion of c, slurry: gained slurry in (2) is transferred in the pressurized tank, leaves standstill 10～30min froth breaking,, adjust the pressure and the dispersion frequency of slurry according to the size and the density requirements of design microballoon; Open the thermal source that disperses post outer, slurry droplet balling-up in oil medium of dispersion;
The washing of d, microballoon, drying, roasting and sintering: the bead of collecting is placed the Rotary drying stove that vacuumizes, wash and drying; Carry out roasting and sintering according to the corresponding system of the character of ceramic powder then, obtain the ceramic microsphere of the design size and the porosity.
2, method according to claim 1 is characterized in that: the ceramic powder among the step a is ZrO
2, Al
2O
3, Si
3N
4, SiC, tourmaline or cordierite, or add carbon dust as pore former; Monomer is the acrylamide with free radical activity, Methacrylamide, in N hydroxymethyl acrylamide, the acrylate 1～4 kind; Crosslinking agent is the N-N-methylene-bisacrylamide; Dispersant is ammonium polyacrylate, ammonium citrate, polyacrylic 1～3 kind.
3, method according to claim 1 is characterized in that: degassing processing comprises and vacuumizes or add 1～2 kind of defoamer among the step b; Vacuumize and be meant that slurry vacuumizes 10～30min under the operating mode of vibration or stirring; Defoamer comprises different new ester, aliphatic acid, and consumption is 0.05～2% of a ceramic powder quality.
4, method according to claim 1 is characterized in that: the initator among the step b is an ammonium persulfate, and the adding method is: with a certain amount of ammonium persulfate dissolving, the stirring arm gob adds ammonium persulfate aqueous solution then earlier.
5, method according to claim 1 is characterized in that: being calculated as follows of scattering parameter among the step c:
If the radius of required product ceramic microsphere is R, the density of ceramic microsphere is D, and the volumn concentration of ceramic powder is V in the slurry, and the density of ceramic powder is Dp,, the flow L of single injector per second, the frequency of establishing electromagnetic vibrator be f then:
The quality percentage composition of ceramic powder is:
Then can set up equation by ceramic powder:
With (1) substitution (2), can get
6, method according to claim 1 is characterized in that: among the step c catalyst n-N-N-N-tetramethylethylenediamine is joined in the oil medium, add volume ratio than being oil medium: catalyst=100: 2～4.
7, method according to claim 1 is characterized in that: the oil medium among the step c is a kind of of methyl-silicone oil, paraffin oil, kerosene or edible oil, and oily temperature control is between 50～90 ℃.
8, method according to claim 1 is characterized in that: the external thermal source among the step c is water-bath or oil bath, outward around the heating tape or microwave.
9, a kind of device of realizing the described method of claim 1 is characterized in that, this device comprises: pressurized tank (1), and glue flowmeter (2), electromagnetic vibrator (3), nozzle (4) disperses post (5), thermal source (6), signal generator (7), power amplifier (8); Air compressor machine (9); Air compressor machine is connected by steel pipe, pressure pipe with pressurized tank, under pressure slip is injected sebific duct; Store slip in the pressurized tank, be connected with flowmeter, nozzle by sebific duct, flowmeter is controlled the flow of slip at spray nozzle front end; Electromagnetic vibrator is connected with nozzle, and power amplifier is connected with electromagnetic vibrator by holding wire, power line with signal generation apparatus, and nozzle is disperseing post top.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140953A (en) * | 2017-04-18 | 2017-09-08 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
| CN107140953B (en) * | 2017-04-18 | 2019-11-22 | 华中科技大学 | A kind of method that quick extrusion prepares ceramic microsphere |
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