CN102189007B - Alumina coating slurry and preparation method thereof - Google Patents
Alumina coating slurry and preparation method thereof Download PDFInfo
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- CN102189007B CN102189007B CN2010101162772A CN201010116277A CN102189007B CN 102189007 B CN102189007 B CN 102189007B CN 2010101162772 A CN2010101162772 A CN 2010101162772A CN 201010116277 A CN201010116277 A CN 201010116277A CN 102189007 B CN102189007 B CN 102189007B
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Abstract
The invention relates to foam alumina slurry and a preparation method thereof, which mainly solve the problems that production efficiency is low and the prepared coating has low uniformity and firmness because alumina slurry has a large particle size and low uniformity and stability, is easy to precipitate and greatly changes when stored for a long time in the prior art. The foam alumina slurry comprises water, alumina sol, alumina, a coating property auxiliary agent, an anionic-cationic conditioning agent and a foaming agent. The preparation method comprises the following steps of: dissolving the alumina sol, the alumina, the coating property auxiliary agent and the anionic-cationic conditioning agent in the water with stirring, and fully mixing to obtain slurry I; foaming a certain amount of foaming agent and water by using a foaming machine, and adding foam into the slurry I; and quickly emulsifying and grinding the slurry added with the foam in a colloid mill. Through the technical scheme, the problems are well solved, and the invention can be used for preparing the alumina slurry in the process of producing a layered composite carrier.
Description
Technical field
The present invention relates to a kind of foamed alumina slurry and preparation method thereof.
Background technology
Noble metal is widely used in chemical industry, oil refining and vehicle exhaust processing as the loaded catalyst of active component at present.Active component non-uniform Distribution in carrier can reduce the consumption of noble metal, improves the utilization rate of noble metal; Simultaneously, the catalyst of non-uniform Distribution also showed than better active, the selective and life-span of equally distributed catalyst in many reactions.Often reach the effect of non-uniform Distribution by the control to dipping in early days, but often be difficult to control the distribution of catalyst.This just need to provide a kind of special carrier, and this carrier is comprised of inert core and coating, only has coating adsorbing metal and coating layer thickness controlled, Here it is lamellar composite carrier.Flood catalyst at this carrier and just made thickness and the controlled heterogeneity catalyst of distribution, ZL02100598.2 has reported cleaning catalyst for tail gases of automobiles such as patent.This invention cleaning catalyst for tail gases of automobiles is take the cordierite honeycomb ceramic matrix as the first carrier, take aluminum oxide coating layer slurries (salic, noble metal) as Second support.By with the first carrier impregnation in the coating slurries, disposable spray finishing is made catalyst.In ethylbenzene catalytic dehydrogenation～H 2 selective oxidation process, patent US6177381 and CN1479649A have reported lamellar composite carrier for another example.Carrier has for example coating gama-alumina for example of Alpha-alumina and an inorganic oxide of a kernel.And for example patent US6858769 and CN1705510A have reported a kind of H 2 selective oxidation catalyst take lithium aluminate as carrier.This catalyst is take cordierite as kernel, take lithium aluminate as coating.
The common feature of above-mentioned catalyst is to use an inert material on the one hand, is the kernel of carrier such as ceramic honey comb, cordierite, α～aluminium oxide, applies the coating material of one deck bigger serface to enlarge the carrier effective surface area at carrier on the other hand.But the figure layer carrier rate of wear of prior art preparation is larger, strength of coating and coating and carrier relatively poor in conjunction with firmness, and coating is easy to wear or come off, thereby affects catalyst performance, has limited the long period use of catalyst.Influence factor during the preparation coating is a lot, but slurry is undoubtedly one of crucial influence factor.Patent CN101491776A provides a kind of prescription and preparation method who prepares coating paste, and this slurry is comprised of in aluminium colloidal sol, activated alumina, organic adhesive, inorganic adhesive, surfactant, pH adjusting agent below 10 microns particle mean size.The preparation method is dissolved in aluminium colloidal sol, organic adhesive, surfactant, pH adjusting agent in the water, under 500～5000 rev/mins high-speed stirred, mix, then add inorganic binder, active oxidation aluminium powder, high speed dispersion 10～180 minutes, the gained alumina slurry ground 10 minutes～10 hours in ball mill, sand mill, ball mill or colloid mill again, made alumina coats pulp.The slurry that makes has improved the stability of coating to a certain extent, has reduced rate of wear, and complicated but the method prepares the slurry preparation process, the cycle is long; The slurry that is worth disperses not fully so that the slurry granularity is larger; Slurry is stable poor, places for a long time the granularity variation greatly even produces precipitation, and in addition, with the coated carrier that this slurry makes, rate of wear is bigger than normal, and the firmness of coating is also relatively poor.Need to improve formula of size and preparation method, obtain when enhancing productivity one scattered, the slurry of the little and good stability of granularity, thus improve the firmness of the coating of preparation, reduce the rate of wear of coating.
Summary of the invention
One of technical problem to be solved by this invention is that the slurry that exists in the prior art disperses problem inhomogeneous, poor stability, a kind of new foamed alumina slurry is provided, that this foamed slurry has is scattered, granularity is little, good stability, the coating that makes in conjunction with firmly, advantage that rate of wear is low.Two of technical problem to be solved by this invention provides a kind of preparation method of the slurry corresponding with one of technical solution problem.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of foamed alumina slurry comprises following component by weight percentage:
A) 1～25% aluminium colloidal sol;
B) 5～50% aluminium oxide;
C) 0.1～10% blowing agent;
D) 0.01～1% zwitterion conditioning agent;
E) 0.1～5.0% coating performance auxiliary agent;
F) 10～90% water;
Wherein: the zwitterion conditioning agent is selected from least a in aluminium oxide, aluminum nitrate, lanthanum chloride, stannic chloride, cerous nitrate, magnesium chloride, stannous chloride, lanthanum nitrate, calcium chloride, hydrochloric acid, nitric acid or the ammoniacal liquor; The coating performance auxiliary agent is selected from least a in wollastonite, diopside, perlite, magnesium silicate, calcium silicates, magnesium aluminate, zirconium aluminate or the kaolin; Blowing agent is selected from least two kinds in PVA, HPC, MC, EMC, tween, sapn or the polyethylene glycol.
In the technique scheme, aluminium colloidal sol by weight percentage consumption preferable range is 5～25%, and more preferably scope is 5～20%; The aluminium oxide preferred version is γ-Al
2O
3, δ-Al
2O
3Or θ-Al
2O
3In at least a and granularity be controlled at below 10 microns, consumption is 10%～40% by weight percentage; The blowing agent preferred version is by at least a material I that is selected among PVA, HPC or the EMC, mix with at least a material II that is selected from tween, sapn, the polyethylene glycol, the part by weight of material I and material II is 1: 5～10: 1, and blowing agent by weight percentage consumption is 0.5～10%; The zwitterion conditioning agent is at least a or several in aluminium oxide, lanthanum chloride, stannic chloride, cerous nitrate or the magnesium chloride, and consumption is 0.05～1% by weight percentage; The coating performance auxiliary agent is at least a in wollastonite, diopside, perlite, calcium silicates or the magnesium aluminate, and consumption is 0.5～5% by weight percentage; Water is deionized water, and consumption is 40～70% by weight percentage.
For two of technical solution problem, technical scheme provided by the invention is as follows: a kind of preparation method of the foamed alumina slurry for one of technical solution problem may further comprise the steps:
1) pulverize: by breaking method control aluminium oxide and auxiliary agent particle diameter below 10 microns;
2) mix: with aluminium colloidal sol, aluminium oxide, zwitterion conditioning agent, the coating performance auxiliary agent of aequum, in situation about stirring, be dissolved in the water and fully and mix, obtain slurry I;
3) foaming; After the blowing agent process foaming machine foaming with aequum, join among the slurry I and mix;
4) emulsification and grinding: with alumina slurry emulsification in colloid mill, the grinding of gained, so that the particle mean size of alumina coats pulp below 5 microns, makes foamed alumina slurry II;
Aluminium oxide and performance auxiliary agent are pulverized by comminution by gas stream; With aluminium colloidal sol, aluminium oxide, zwitterion conditioning agent, the coating performance auxiliary agent of aequum, under 2000 rev/mins stirring, be dissolved in the water and mixed 0.5～1 hour, obtain slurry I; Blowing agent and water join in the blowing agent and foam, and obtain the foam of requirement and join to mix 10～30 minutes among the slurry I, then join and carry out colloidal grinding in the colloid mill, and the colloid mill time is controlled at 0.5～1 hour, obtains the slurry that needs.
One aspect of the present invention has been optimized the alumina slurry prescription, the zwitterion conditioning agent that adds provides enough electrolyte and must acid or alkali environment for the stable system of slurry on the one hand, in suspension system, blowing agent and particle can reach high dispersive and stable effect by the repulsive force between the adsorption electric charge, also can be used as on the other hand the auxiliary element of coated carrier or catalyst through playing with the effect of coating oxidation aluminium the effect of stable coatings after the high-temperature roasting; The coating performance auxiliary agent, thus mainly be that the stable composition that utilizes itself and aluminium oxide at high temperature to generate is conducive to coating; On the other hand, blowing agent is by the foaming of blowing agent, can be so that blowing agent disperses more abundant, and the foam quality that obtains is good, bubble diameter is little, the foam yardstick is even, after joining like this among the alumina slurry, a large amount of uniformly vesicle foams have stoped the gathering of alumina particle, and granularity increases because assemble can either to prevent aluminium oxide particles, again can be so that the dispersion of particle is more even, the blowing agent of high dispersive can be at shell of the peripheral formation of particle simultaneously, increase intergranular distance, reduced the effect of Van der Waals force, thereby increased the electro kinetic potential of suspension so that dispersion reaches stable state.In addition, improved the dispersion efficiency of blowing agent by blowing agent foaming, production efficiency also can improve greatly.The slurry that makes is when spraying, because granularity is little, and good dispersion, atomizing effect improves, and can increase the compactness of coating, thereby improves the firmness of coating, the rate of wear of reduction figure layer.The foamed alumina slurry that uses the inventive method to make, slurry granularity d
50All less than 4um, place 15 days disposed slurry granularities and still maintain about 4um, in the time of 30 days, the slurry granularity is still about 5 microns; Make coating 1000 with this slurry and turn rate of wear less than 0.15%, loss late can be controlled at below 0.3% in ultrasonic 30 minutes.It is little to illustrate that slurry that the present invention makes has granularity, and it is low that the advantage of good stability, the coating that makes with this slurry have a rate of wear, and the advantage that firmness is high has obtained preferably technique effect.
The present invention is further elaborated below by embodiment.
The specific embodiment
[embodiment 1]
With 300 gram water, the aluminium colloidal sol of 1200 grams 10%, 40 gram concentration are 20% lanthanum chloride solution, 800 gram gamma oxidation aluminium powders, 8 gram calcium silicates, add successively and mix 60 minutes in the mixer, get 10 gram HPC, 5 gram sapns add water 300 gram and place the foaming machine foaming to make foam, join in the above-mentioned slurry, mixed 30 minutes, add in the colloid mill and ground 40 minutes, make the slurry A that needs.
[embodiment 2]
With 500 gram water, the aluminium colloidal sol of 1000 grams 20%, 70 gram concentration are 50% tin chloride solution, 1200 gram δ-alumina powders, 50 gram magnesium aluminates, 60 gram diopsides add successively and mix 30 minutes in the mixer, get 50 gram PVA, 10 gram tweens add water 600 gram and place the foaming machine foaming to make foam, join in the above-mentioned slurry, mixed 10 minutes, add in the colloid mill and ground 50 minutes, make the slurry B that needs.
[embodiment 3]
With 300 gram water, the aluminium colloidal sol of 2000 grams 40%, 40 gram concentration are 10% magnesium chloride solution, and 40 gram concentration are 20% stannous chloride solution, 300 gram 0-alumina powders, 30 gram wollastonites add successively and mix 40 minutes in the mixer, get 50 gram HPMC, 10 gram polyethylene glycol add water 500 gram and place the foaming machine foaming to make foam, join in the above-mentioned slurry, mixed 20 minutes, add in the colloid mill and ground 30 minutes, make the slurry C that needs.
[embodiment 4]
With 800 gram water, the aluminium colloidal sol of 1000 grams 40%, 50 grams, 10% aluminum nitrate solution, 50 grams, 10% cerous nitrate, 300 gram 0-alumina powders, 300 gram gamma oxidation aluminium powders, 20 gram kyanites once add and mix 50 minutes in the mixer, get 30 gram EMC, molten Sha Mujia water 700 grams of 4 gram pools place the foaming machine foaming to make foam, join and mix 15 minutes in the above-mentioned slurry, add in the colloid mill and ground 60 minutes, make slurry D.
[comparative example 1]
With 1200 gram water, the aluminium colloidal sol of 1000 gram concentration 10%, 10 gram PVA, 7.5 gram CMC, 30 gram sorbester p17s are made slurries, with 2000 rev/mins of high-speed stirred 30 minutes, add 2.5 ml concns again and be 8% nitric acid, 37.5 gram potassic feldspar, 20 gram diatomite, 1000 gram gamma oxidation aluminium powders continue to stir 60 minutes, ball milling 4 hours at room temperature makes alumina slurry E again.
[comparative example 2]
Prescription according to patent CN101491776 embodiment 1, with 750 gram water, the aluminium colloidal sol of 1000 gram concentration 10%, 2.5 ml concn is 8% nitric acid, 37.5 gram potassic feldspar, 20 gram diatomite, 1000 gram gamma oxidation aluminium powders once join and mix 30 minutes in the mixer, get 10 gram PVA, 7.5 gram CMC, 30 gram sorbester p17s, foaming makes foam in the 500 gram water adding foaming machines, joins and mixes 10 minutes in the above-mentioned slurry, join in the colloid mill and ground 40 minutes, make slurry F.
[embodiment 5]
With the slurry A of fresh preparation, B, C, D, E, F measures its granule size and distribution with laser particle analyzer, the results are shown in Table 1.Be that 4 millimeters cordierite bead joins in the cylinder with particle diameter, cylinder is heated to 200 ℃, the index drum temperature is 200 rev/mins, slurry A～F is sprayed to respectively on the cordierite bead, dry in the shade under the room temperature, with 80 ℃ of dryings 2 hours, then be warmed up to 120 ℃ dry 2 hours again, 1000 ℃ of roastings 12 hours obtain lamellar composite carrier A
0～F
0The rate of wear of carrier and ultrasonic loss late the results are shown in Table 2.
The particle diameter of table 1 slurry and distribution
| Particle diameter/um | A | B | C | D | E | F |
| d 50 | 3.4 | 3.5 | 3.3 | 3.7 | 8.3 | 5.2 |
| d 90 | 8.9 | 9.1 | 8.6 | 10.2 | 24.5 | 14.9 |
As can be seen from Table 1, the slurry A that adopts prescription of the present invention and preparation technology to obtain, B, C, D and slurry E, F compares, and particle diameter is less, and the particle size distribution of slurry is narrower, illustrates that the slurry that adopts this patent method to make disperses more even.Contrast E and F and F and A～D can find out that this patent and prescription all have facilitation to slurry.
The physical and chemical performance test result of table 2 carrier
| A 0 | B 0 | C 0 | D 0 | E 0 | F 0 | |
| 1000 turn rate of wear/% | 0.11 | 0.13 | 0.13 | 0.12 | 0.28 | 0.16 |
| Ultrasonic 30min loss late a/％ | 0.23 | 0.23 | 0.25 | 0.22 | 0.45 | 0.30 |
A gets carrier 30 as one kind and restrains ultrasonic 30min in the 20kHz ultrasonic wave, and oven dry is weighed, and calculates ultrasonic front and back loss late.
As shown in Table 2, the coating A that adopts the slurry of this patent method to make
0～D
0, its rate of wear and ultrasonic loss late are starkly lower than the E of reference
0, F
0, the coating rate of wear is all below 0.15%, and ultrasonic loss late is all less than 0.3%; Contrast E0 and F0 can find out that in the consistent situation of filling a prescription, its rate of wear of coating and ultrasonic loss late that the slurry that adopts this patent method to obtain prepares are lower, illustrate that coating is more firm; Contrast A
0～D
0With F0, can find out that employing this patent prescription is also more favourable for coating.
[embodiment 6]
Slurry D and slurry E were placed respectively 7 days, and 15 days, after 30 days, laser particle analyzer was measured its granularity, sprayed according to embodiment 5 modes and was prepared into carrier, corresponded to D
1, D
2, D
3And E
1, E
2, E
3The thing of slurry and coating sees Table 2.
Table 3 standing time is on the impact of the coating of slurry and preparation
| Time/sky | Container name | Corresponding slurry d 50/um | 1000 turn rate of wear/% | Ultrasonic 30min loss late/% |
| 0 | D 0 | 3.7 | 0.12 | 0.22 |
| 7 | D 1 | 4.0 | 0.12 | 0.22 |
| 15 | D 2 | 4.3 | 0.12 | 0.23 |
| 30 | D 3 | 5.0 | 0.16 | 0.29 |
| 0 | E 0 | 8.3 | 0.28 | 0.45 |
| 7 | E 1 | 10.0 | 0.32 | 0.47 |
| 15 | E 2 | 13.5 | 0.46 | 0.55 |
| 30 | E 3 | 17.1 | 0.65 | 0.72 |
By table 3, contrast standing time is on the impact of the coating of the slurry of two kinds of methods preparation and preparation thereof, can find out, the foamed slurry and the coating thereof that adopt this method to obtain, prolongation along with standing time, though slurry granularity, coating rate of wear and ultrasonic loss late slightly increase, substantially all control scope in, show that the slurry dispersion that adopts this method to obtain is more stable.
Claims (6)
1. foamed alumina slurry comprises following component by weight percentage:
A) 1～25% aluminium colloidal sol;
B) 5～50% aluminium oxide;
C) 0.5～10% blowing agent;
D) 0.01～1% zwitterion conditioning agent;
E) 0.1～5.0% coating performance auxiliary agent;
F) 10～90% water;
Wherein: the zwitterion conditioning agent is selected from least a in aluminum nitrate, lanthanum chloride, stannic chloride, cerous nitrate, magnesium chloride, stannous chloride, lanthanum nitrate, the calcium chloride; The coating performance auxiliary agent is selected from least a in wollastonite, diopside, perlite, magnesium silicate, magnesium aluminate, zirconium aluminate or the kaolin; Blowing agent is mixed with at least a material II that is selected from tween, sapn, the polyethylene glycol by the material I that is selected from EMC, and the part by weight of material I and material II is 1: 10～10: 1.
2. described foamed alumina slurry according to claim 1 is characterized in that aluminium oxide is γ-Al
2O
3, δ-Al
2O
3Or θ-Al
2O
3In at least a and granularity be controlled at below 10 microns.
3. described foamed alumina slurry according to claim 1 is characterized in that the zwitterion conditioning agent is selected from least a in lanthanum chloride, stannic chloride, cerous nitrate, the magnesium chloride, and consumption is 0.05～1% by weight percentage.
4. described foamed alumina slurry according to claim 1 is characterized in that the coating performance auxiliary agent is selected from least a in wollastonite, diopside, perlite, the magnesium aluminate, and consumption is 0.5～5.0% by weight percentage.
5. described foamed alumina slurry according to claim 1 is characterized in that water is deionized water, and consumption is 40～70% by weight percentage.
6. the preparation method of foamed alumina slurry claimed in claim 1 may further comprise the steps:
1) pulverize: by breaking method control aluminium oxide and coating performance auxiliary agent particle diameter below 10 microns;
2) mix: with aluminium colloidal sol, aluminium oxide, zwitterion conditioning agent, the coating performance auxiliary agent of aequum, in situation about stirring, be dissolved in the water and fully and mix, obtain slurry I;
3) foaming; After the blowing agent process foaming machine foaming with aequum, join among the slurry I and mix;
4) emulsification and grinding: with alumina slurry emulsification in colloid mill, the grinding of gained, so that the particle mean size of alumina coats pulp below 5 microns, makes foamed alumina slurry II.
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|---|---|---|---|
| CN2010101162772A CN102189007B (en) | 2010-03-03 | 2010-03-03 | Alumina coating slurry and preparation method thereof |
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|---|---|---|---|
| CN2010101162772A CN102189007B (en) | 2010-03-03 | 2010-03-03 | Alumina coating slurry and preparation method thereof |
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|---|---|
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| CN102189007B true CN102189007B (en) | 2013-01-09 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6177381B1 (en) * | 1998-11-03 | 2001-01-23 | Uop Llc | Layered catalyst composition and processes for preparing and using the composition |
| US6858769B2 (en) * | 2002-10-18 | 2005-02-22 | Uop Llc | Lithium aluminate layered catalyst and a selective oxidation process using the catalyst |
| CN101428216A (en) * | 2007-11-07 | 2009-05-13 | 中国石油化工股份有限公司 | Layered composite carrier for producing shell shaped catalyst |
| CN101491776A (en) * | 2008-01-23 | 2009-07-29 | 中国石油化工股份有限公司 | Alumina coats pulp and preparation method thereof |
-
2010
- 2010-03-03 CN CN2010101162772A patent/CN102189007B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6177381B1 (en) * | 1998-11-03 | 2001-01-23 | Uop Llc | Layered catalyst composition and processes for preparing and using the composition |
| US6858769B2 (en) * | 2002-10-18 | 2005-02-22 | Uop Llc | Lithium aluminate layered catalyst and a selective oxidation process using the catalyst |
| CN1705510A (en) * | 2002-10-18 | 2005-12-07 | 环球油品公司 | A lithium aluminate layered catalyst and a selective oxidation process using the catalyst |
| CN101428216A (en) * | 2007-11-07 | 2009-05-13 | 中国石油化工股份有限公司 | Layered composite carrier for producing shell shaped catalyst |
| CN101491776A (en) * | 2008-01-23 | 2009-07-29 | 中国石油化工股份有限公司 | Alumina coats pulp and preparation method thereof |
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