CN107597197A - A kind of preparation method of high-porosity alumina Ceramic Balls - Google Patents
A kind of preparation method of high-porosity alumina Ceramic Balls Download PDFInfo
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- CN107597197A CN107597197A CN201710965145.9A CN201710965145A CN107597197A CN 107597197 A CN107597197 A CN 107597197A CN 201710965145 A CN201710965145 A CN 201710965145A CN 107597197 A CN107597197 A CN 107597197A
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Abstract
A kind of preparation method of high-porosity alumina Ceramic Balls disclosed by the invention, comprises the following steps：Step 1, ethanol mixed aqueous solution is prepared；Step 2, suspended underflow is prepared；Step 3, thick embryo is prepared；Step 4, by gradient sintering in the thick embryo implantation roaster of step 3, air cooling obtains the aluminium oxide ceramic ball of high porosity after taking-up.Preparation method step of the invention is simple to operation, cost is relatively low, and stability is higher in the reaction；Wherein by the way of gradient sintering, heat can be slowly discharged, prevents ceramic ball fractured；Stable pore structure is formd as pore-foaming agent using urea simultaneously；The aluminium oxide ceramic ball resistance to pressure of preparation is good, weatherability is strong, adapts to a variety of reaction environments, and aluminium oxide ceramic ball hole is uniform and porosity is high, good dispersion and bigger than surface, expands application on a catalyst support.
Description
Technical field
The invention belongs to catalyst carrier preparation method technical field, and in particular to a kind of high-porosity alumina Ceramic Balls
Preparation method.
Background technology
Catalyst carrier is also known as carrier (support), is one of composition of loaded catalyst.Catalytic active component supports
On carrier surface, carrier is mainly used in supporting active component, catalyst is had a specific physical behavior, and carrier in itself one
As and do not have a catalytic activity.
Majority carrier is the product in Catalyst, it is conventional have alumina support, silica-gel carrier, absorbent charcoal carrier and
Some natural products such as float stone, diatomite etc..Carrier can make manufactured catalyst have suitable shape, size and machinery strong
Degree, to meet the operation requirement of industrial reactor；Carrier can be such that active component is dispersed on carrier surface, obtain higher ratio table
Area, improve the catalytic efficiency of unit mass active component.Such as platinum is carried on activated carbon, if being carrier with molecular sieve, platinum
It can reach the decentralization close to atom level.Carrier can also prevent active component from sintering in use, improve catalyst
Heat resistance.For some strong exothermal reactions, carrier dilutes the active component in catalyst, to meet thermal balance requirement；Well
The carrier of thermal conductivity, such as metal, carborundum；Help to remove reaction heat, avoid catalyst surface hot-spot.Carrier again may be used
Some catalyst being originally used in homogeneous reaction are carried on solid carrier solid catalyst is made, if phosphate adsorption is in silicon
Manufactured solid acid catalyst in diatomaceous earth, enzyme are supported on manufactured immobilised enzymes on carrier.
Aluminium oxide ceramic ball is presently the most conventional catalyst carrier, is widely used in noble metal catalyst.Your gold
Metal catalyst belongs to solid-liquid contact catalyst, can just play catalytic effect by contact, with the increase of catalyst specific surface, urge
Changing performance can also steadily improve, therefore the demand more and more higher of the carrier for Large ratio surface.At present, the preparation of aluminium oxide ceramic ball
Method is because step is complicated, cost is higher, the aluminium oxide ceramic ball porosity of preparation and more relatively low than surface, constrain significantly its
Application in catalyst carrier.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high-porosity alumina Ceramic Balls, solves existing aluminum oxide
The preparation method of Ceramic Balls is because step is complicated, cost is higher, the aluminium oxide ceramic ball porosity of preparation and more relatively low than surface
Problem.
The technical solution adopted in the present invention is a kind of preparation method of high-porosity alumina Ceramic Balls, including following
Step：
Step 1, ethanol mixed aqueous solution is prepared
Polyvinylpyrrolidone is dissolved in ethanol water, is stirred by ultrasonic to being completely dissolved, obtains ethanol mixing water
Solution；
Step 2, suspended underflow is prepared
Nano-sized Alumina Powder is added in the ethanol mixed aqueous solution of step 1, ultrasonic agitation forms white slurry；With
Nano grade silica particles and nanometer aluminium powder are sequentially added in backward white slurry, twice ultrasonic obtains suspended dense after stirring
Slurry；
Step 3, thick embryo is prepared
Urea and curing agent are added dropwise in the suspended underflow of step 2 successively, form suspended dispersion, then will be suspended
Dispersion is inserted and microwave reaction is carried out in spherical die, quick cooling in atmosphere after reaction terminates, obtains thick embryo；
Step 4, by gradient sintering 6h in the thick embryo implantation roaster of step 3, air cooling obtains high porosity after taking-up
Aluminium oxide ceramic ball.
It is of the invention to be further characterized in that,
Ethanol volumetric concentration is 40%-70% in step 1 ethanol water, polyvinylpyrrolidine in ethanol mixed aqueous solution
The mass concentration of ketone is 2-5g/L.
The frequency being stirred by ultrasonic in step 1 is 2.5-5.5kHz.
Nano-sized Alumina Powder mass concentration is 70-100g/L, nano grade silica particles quality in the suspended underflow of step 2
Concentration is 3-8g/L, nanometer aluminium powder mass concentration is 3-10g/L.
In step 2 particle diameter of Nano-sized Alumina Powder be 100-500nm, nano grade silica particles particle diameter be 20-
150nm, the particle diameter of nanometer aluminium powder are 200-500nm.
Parameter is stirred by ultrasonic in step 2 is：Supersonic frequency 7.5-13.5kHz, ultrasonic time 20-40min；
Twice ultrasonic stirring parameter be：Supersonic frequency 20-40kHz, ultrasonic time 20-40min.
Curing agent is m-phenylene diamine (MPD) in step 3, and its mass concentration in suspended dispersion is 1-3g/L, and urea is outstanding
Mass concentration in turbid dispersion is 3-6g/L.
Microwave reaction parameter in step 3 is：Microwave wattage 100-300w, 140-250 DEG C of temperature, reaction time 20-
30min。
Rate of addition in step 3 is 0.1-0.5g/min.
Gradient sintering in step 4 is specially：300-500 DEG C, insulation 1h are warming up to first, are continuously heating to 600-900
DEG C, insulation 2h, be continuously heating to 1300-1500 DEG C, be incubated 3h.
The present invention preparation method beneficial effect be：
(1) preparation method of the invention obtains aluminium oxide ceramic ball resistance to pressure is good, weatherability is strong, adapts to a variety of reactions
Environment；
(2) the aluminium oxide ceramic ball porosity that preparation method of the invention obtains is high, bigger than surface, expands in catalyst
Application on carrier；
(3) preparation method step of the invention is simple, cost is relatively low, stability is high, obtained aluminium oxide ceramic ball hole
Uniformly, good dispersion；
(4) preparation method of the invention can slowly be discharged heat, be prevented Ceramic Balls from breaking by the way of gradient sintering
Split；
(5) preparation method of the invention forms stable pore structure, there is good reality using urea as pore-foaming agent
With value.
Embodiment
Below by embodiment, the present invention is described in detail.
A kind of preparation method of high-porosity alumina Ceramic Balls of the present invention, comprises the following steps：
Step 1, ethanol mixed aqueous solution is prepared
Polyvinylpyrrolidone is dissolved in ethanol water, is stirred by ultrasonic to being completely dissolved, obtains ethanol mixing water
Ethanol volumetric concentration is 40%-70% in solution, wherein ethanol water, polyvinylpyrrolidone in ethanol mixed aqueous solution
Mass concentration is 2-5g/L, and the frequency of ultrasonic agitation is 2.5-5.5kHz.Polyvinylpyrrolidone is as dispersant, for improving
The dispersiveness of Nano-sized Alumina Powder, nano grade silica particles and nanometer aluminium powder in system in subsequent step.
Good directionality is stirred by ultrasonic, penetration capacity is strong, is not very big liquid or solidliquid mixture suitable for viscosity,
The principle of magnetic field and whirlpool is make use of, so as to reach the purpose of agitated liquid.
Step 2, suspended underflow is prepared
The Nano-sized Alumina Powder that particle diameter is 100-500nm is added in the ethanol mixed aqueous solution of step 1, ultrasound is stirred
Mix to form white slurry；It is that 20-150nm nano grade silica particles are with particle diameter then to particle diameter is sequentially added in white slurry
200-500nm nanometer aluminium powders, twice ultrasonic obtain suspended underflow after stirring；Nano-sized Alumina Powder quality in suspended underflow
Concentration is 70-100g/L, nano grade silica particles mass concentration is 3-8g/L, nanometer aluminium powder mass concentration is 3-10g/L.
Parameter, which is stirred by ultrasonic, is：Supersonic frequency 7.5-13.5kHz, ultrasonic time 20-40min；The ginseng of twice ultrasonic stirring
Number is：Supersonic frequency 20-40kHz, ultrasonic time 20-40min.
Step 3, thick embryo is prepared
Urea and curing agent m-phenylene diamine (MPD) are added dropwise to the suspended underflow of step 2 with 0.1-0.5g/min speed successively
It is interior, suspended dispersion is formed, wherein mass concentration of the m-phenylene diamine (MPD) in suspended dispersion is 1-3g/L, and urea is suspended
Mass concentration in dispersion is 3-6g/L；Then suspended dispersion is inserted microwave reaction is carried out in spherical die, instead
After should terminating in atmosphere, quickly cooled down by modes such as fan blowings, obtain thick embryo, microwave reaction parameter is：Microwave wattage
100-300w, 140-250 DEG C of temperature, reaction time 20-30min.
Step 4, by gradient sintering 6h in the thick embryo implantation roaster of step 3, normal temperature is air-cooled to after taking-up and obtains high hole
The aluminium oxide ceramic ball of gap rate；Wherein gradient sintering is specially：300-500 DEG C, insulation 1h are warming up to first, are continuously heating to
600-900 DEG C, insulation 2h, are continuously heating to 1300-1500 DEG C, are incubated 3h.
Preparation method step of the invention is simple to operation, cost is relatively low, and stability is higher in the reaction；Wherein using ladder
The mode of sintering is spent, heat can be slowly discharged, prevent ceramic ball fractured；Formd steady as pore-foaming agent using urea simultaneously
Fixed pore structure；The aluminium oxide ceramic ball resistance to pressure of preparation is good, weatherability is strong, adapts to a variety of reaction environments, aluminum oxide pottery
Porcelain ball gap is uniform and porosity is high, good dispersion and bigger than surface, expands application on a catalyst support.
Embodiment 1
(1) polyethylene of dispersing agent pyrrolidones is dissolved in ethanol water, is stirred by ultrasonic to being completely dissolved, obtains second
Ethanol volumetric concentration is 40% in alcohol mixed aqueous solution, wherein ethanol water, polyvinylpyrrolidine in ethanol mixed aqueous solution
The mass concentration of ketone is 2g/L, and the frequency of ultrasonic agitation is 2.5kHz.
(2) particle diameter 100nm Nano-sized Alumina Powder is added in ethanol mixed aqueous solution, ultrasonic agitation forms white
Slurry；It is secondary then to sequentially adding particle diameter 20nm nano grade silica particles and particle diameter 200nm nanometer aluminium powders in white slurry
Suspended underflow is obtained after ultrasonic agitation is uniform；Nano-sized Alumina Powder mass concentration is 70g/L, nanometer titanium dioxide in suspended underflow
Silicon powder mass concentration is 3g/L, nanometer aluminium powder mass concentration is 3g/L.
Parameter, which is stirred by ultrasonic, is：Supersonic frequency 7.5kHz, ultrasonic time 20min；Twice ultrasonic mixing parametric is：Supersonic frequency
Rate 20kHz, ultrasonic time 20min.
(3) urea and curing agent m-phenylene diamine (MPD) are added dropwise in suspended underflow with 0.1g/min speed successively, formed outstanding
The mass concentration of turbid dispersion, wherein m-phenylene diamine (MPD) is 1g/L, and the mass concentration of urea is 3g/L；Then by suspended dispersion
System, which inserts, carries out microwave reaction in spherical die, reaction quick cooling after terminating, obtain thick embryo, microwave reaction parameter is：Microwave
Wattage 100w, 140 DEG C of temperature, reaction time 30min.
(4) thick embryo is implanted into gradient sintering 6h in roaster, the oxidation that normal temperature obtains high porosity is air-cooled to after taking-up
Aluminium Ceramic Balls；Wherein gradient sintering is specially：300 DEG C, insulation 1h are warming up to first, are continuously heating to 600 DEG C, insulation 2h, after
It is continuous to be warming up to 1300 DEG C, it is incubated 3h.
Embodiment 2
(1) polyethylene of dispersing agent pyrrolidones is dissolved in ethanol water, is stirred by ultrasonic to being completely dissolved, obtains second
Ethanol volumetric concentration is 60% in alcohol mixed aqueous solution, wherein ethanol water, polyvinylpyrrolidine in ethanol mixed aqueous solution
The mass concentration of ketone is 3g/L, and the frequency of ultrasonic agitation is 4.5kHz.
(2) particle diameter 300nm Nano-sized Alumina Powder is added in ethanol mixed aqueous solution, ultrasonic agitation forms white
Slurry；It is 300nm nanometer aluminium powders then to particle diameter 100nm nano grade silica particles are sequentially added in white slurry with particle diameter,
Twice ultrasonic obtains suspended underflow after stirring；Nano-sized Alumina Powder mass concentration is 80g/L, nanometer two in suspended underflow
Silicon oxide powder mass concentration is 6g/L, nanometer aluminium powder mass concentration is 7g/L.
Parameter, which is stirred by ultrasonic, is：Supersonic frequency 10kHz, ultrasonic time 30min；Twice ultrasonic stirring parameter be：Ultrasound
Frequency 30kHz, ultrasonic time 30min.
(3) urea and curing agent m-phenylene diamine (MPD) are added dropwise in suspended underflow with 0.3g/min speed successively, formed outstanding
The mass concentration of turbid dispersion, wherein m-phenylene diamine (MPD) is 2g/L, and the mass concentration of urea is 5g/L；Then by suspended dispersion
System, which inserts, carries out microwave reaction in spherical die, reaction quick cooling after terminating, obtain thick embryo, microwave reaction parameter is：Microwave
Wattage 200w, 200 DEG C of temperature, reaction time 25min.
(4) thick embryo is implanted into gradient sintering 6h in roaster, the oxidation that normal temperature obtains high porosity is air-cooled to after taking-up
Aluminium Ceramic Balls；Wherein gradient sintering is specially：400 DEG C, insulation 1h are warming up to first, are continuously heating to 700 DEG C, insulation 2h, after
It is continuous to be warming up to 1400 DEG C, it is incubated 3h.
Embodiment 3
(1) polyethylene of dispersing agent pyrrolidones is dissolved in ethanol water, is stirred by ultrasonic to being completely dissolved, obtains second
Ethanol volumetric concentration is 70% in alcohol mixed aqueous solution, wherein ethanol water, polyvinylpyrrolidine in ethanol mixed aqueous solution
The mass concentration of ketone is 5g/L, and the frequency of ultrasonic agitation is 5.5kHz.
(2) particle diameter 500nm Nano-sized Alumina Powder is added in ethanol mixed aqueous solution, ultrasonic agitation forms white
Slurry；Then to sequentially adding particle diameter 150nm nano grade silica particles and particle diameter 500nm nanometer aluminium powders in white slurry, two
Suspended underflow is obtained after secondary ultrasonic agitation is uniform；Nano-sized Alumina Powder mass concentration is 100g/L, nanometer two in suspended underflow
Silicon oxide powder mass concentration is 8g/L, nanometer aluminium powder mass concentration is 10g/L.
Parameter, which is stirred by ultrasonic, is：Supersonic frequency 13.5kHz, ultrasonic time 40min；Twice ultrasonic mixing parametric is：Ultrasound
Frequency 40kHz, ultrasonic time 40min.
(3) urea and curing agent m-phenylene diamine (MPD) are added dropwise in suspended underflow with 0.5g/min speed successively, formed outstanding
The mass concentration of turbid dispersion, wherein m-phenylene diamine (MPD) is 3g/L, and the mass concentration of urea is 6g/L；Then by suspended dispersion
System, which inserts, carries out microwave reaction in spherical die, reaction quick cooling after terminating, obtain thick embryo, microwave reaction parameter is：Microwave
Wattage 300w, 250 DEG C of temperature, reaction time 20min.
(4) thick embryo is implanted into gradient sintering 6h in roaster, the oxidation that normal temperature obtains high porosity is air-cooled to after taking-up
Aluminium Ceramic Balls；Wherein gradient sintering is specially：500 DEG C, insulation 1h are warming up to first, are continuously heating to 900 DEG C, insulation 2h, after
It is continuous to be warming up to 1500 DEG C, it is incubated 3h.
Claims (10)
1. a kind of preparation method of high-porosity alumina Ceramic Balls, it is characterised in that comprise the following steps：
Step 1, ethanol mixed aqueous solution is prepared
Polyvinylpyrrolidone is dissolved in ethanol water, is stirred by ultrasonic to being completely dissolved, obtains ethanol mixed aqueous solution；
Step 2, suspended underflow is prepared
Nano-sized Alumina Powder is added in the ethanol mixed aqueous solution of step 1, ultrasonic agitation forms white slurry；Then to
Nano grade silica particles and nanometer aluminium powder are sequentially added in white slurry, twice ultrasonic obtains suspended underflow after stirring；
Step 3, thick embryo is prepared
Urea and curing agent are added dropwise in the suspended underflow of step 2 successively, form suspended dispersion, then will be suspended scattered
System is inserted and microwave reaction is carried out in spherical die, quick cooling in atmosphere after reaction terminates, obtains thick embryo；
Step 4, by gradient sintering 6h in the thick embryo implantation roaster of step 3, air cooling obtains the oxidation of high porosity after taking-up
Aluminium Ceramic Balls.
A kind of 2. preparation method of high-porosity alumina Ceramic Balls according to claim 1, it is characterised in that the step
Ethanol volumetric concentration is 40%-70% in rapid 1 ethanol water, and the quality of polyvinylpyrrolidone is dense in ethanol mixed aqueous solution
Spend for 2-5g/L.
A kind of 3. preparation method of high-porosity alumina Ceramic Balls according to claim 1, it is characterised in that the step
The frequency being stirred by ultrasonic in rapid 1 is 2.5-5.5kHz.
A kind of 4. preparation method of high-porosity alumina Ceramic Balls according to claim 1, it is characterised in that the step
In rapid 2 suspended underflow Nano-sized Alumina Powder mass concentration be 70-100g/L, the nano grade silica particles mass concentration be
3-8g/L, the nanometer aluminium powder mass concentration are 3-10g/L.
A kind of 5. preparation method of high-porosity alumina Ceramic Balls according to claim 1 or 4, it is characterised in that institute
The particle diameter for stating Nano-sized Alumina Powder in step 2 is 100-500nm, the nano grade silica particles particle diameter be 20-150nm,
The particle diameter of the nanometer aluminium powder is 200-500nm.
A kind of 6. preparation method of high-porosity alumina Ceramic Balls according to claim 5, it is characterised in that the step
Parameter is stirred by ultrasonic in rapid 2 is：Supersonic frequency 7.5-13.5kHz, ultrasonic time 20-40min；
The parameter of twice ultrasonic stirring is：Supersonic frequency 20-40kHz, ultrasonic time 20-40min.
A kind of 7. preparation method of high-porosity alumina Ceramic Balls according to claim 1, it is characterised in that the step
Curing agent is m-phenylene diamine (MPD) in rapid 3, and its mass concentration in suspended dispersion is 1-3g/L, and urea is in suspended dispersion
In mass concentration be 3-6g/L.
A kind of 8. preparation method of high-porosity alumina Ceramic Balls according to claim 1 or 7, it is characterised in that institute
The microwave reaction parameter stated in step 3 is：Microwave wattage 100-300w, 140-250 DEG C of temperature, reaction time 20-30min.
A kind of 9. preparation method of high-porosity alumina Ceramic Balls according to claim 8, it is characterised in that the step
Rate of addition in rapid 3 is 0.1-0.5g/min.
10. the preparation method of a kind of high-porosity alumina Ceramic Balls according to claim 1, it is characterised in that described
Gradient sintering in step 4 is specially：300-500 DEG C, insulation 1h are warming up to first, are continuously heating to 600-900 DEG C, insulation
2h, 1300-1500 DEG C is continuously heating to, is incubated 3h.
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Cited By (1)
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Application publication date: 20180119 |