CN101108343A - Pd carried iolite honeycomb ceramic catalyze material and method of manufacturing the same - Google Patents
Pd carried iolite honeycomb ceramic catalyze material and method of manufacturing the same Download PDFInfo
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- CN101108343A CN101108343A CNA2007100291990A CN200710029199A CN101108343A CN 101108343 A CN101108343 A CN 101108343A CN A2007100291990 A CNA2007100291990 A CN A2007100291990A CN 200710029199 A CN200710029199 A CN 200710029199A CN 101108343 A CN101108343 A CN 101108343A
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- reducing solution
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- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 27
- 239000011020 iolite Substances 0.000 title claims description 13
- 238000004519 manufacturing process Methods 0.000 title description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 87
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 26
- 229910052878 cordierite Inorganic materials 0.000 claims abstract description 23
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000007747 plating Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000002791 soaking Methods 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000006555 catalytic reaction Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 101150003085 Pdcl gene Proteins 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000003599 detergent Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000012805 post-processing Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 8
- 229910021529 ammonia Inorganic materials 0.000 claims 4
- 239000012153 distilled water Substances 0.000 claims 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- 229910052684 Cerium Inorganic materials 0.000 abstract description 6
- 229910052759 nickel Inorganic materials 0.000 abstract description 6
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000006479 redox reaction Methods 0.000 abstract description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract 5
- 230000003197 catalytic effect Effects 0.000 abstract 3
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 12
- 239000007788 liquid Substances 0.000 description 5
- 238000005844 autocatalytic reaction Methods 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000000921 elemental analysis Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007664 blowing Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000011946 reduction process Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000004630 mental health Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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Abstract
The invention relates to a Pd-carried cordierite honeycomb ceramic catalytic material and a preparation method for the material. The Pd-carried cordierite honeycomb ceramic catalytic material comprises a cordierite honeycomb ceramic substrate and a palladium loaded on the surface of the substrate by a chemical plating method. The ceramic catalytic material is prepared by the chemical plating method and taking use of the oxidation reduction reaction between sodium hypophosphite and palladium chloride as well as the autocatalytic action of the palladium, hence the metal Pd is deposited on the cordierite honeycomb ceramic substrate. The surface area of the cordierite honeycomb ceramic substrate used in the invention is substantially increased after being eroded by alkali. The chemical Pd plating by using the improved new method has not only simplified the operation process, but also can obviously improve the loaded quantity of Pd on the ceramic substrate and the dispersing evenness if adding assistant Ce and Ni.
Description
Technical field
The present invention relates to a kind of honeycomb ceramic catalyze material and preparation method thereof, particularly relate to a kind of Pd carried iolite honeycomb ceramic catalyze material and preparation method thereof.
Background technology
Along with automobile more and more widely use in social life, vehicle exhaust is also more and more serious to the pollution that atmospheric environment causes, and is endangering people's physical and mental health deeply, influences the raising of people's quality of life.Utilizing catalyst technology to administer tail gas pollution of motor-driven vehicle is the most effective, the most practical at present, method the most widely.
The process of traditional preparation process iolite honeycomb ceramic catalyze material is loaded down with trivial details, the conditional request harshness.Therefore it is significant to probe into the new method for preparing the purifying vehicle exhaust catalysis material.
Summary of the invention
The purpose of this invention is to provide a kind of Pd carried iolite honeycomb ceramic catalyze material and preparation method thereof.
The present invention adopts the method for chemical plating Pd on cordierite honeycomb ceramic, utilize the redox reaction between sodium hypophosphite and the palladium bichloride and the autocatalysis of palladium, make Metal Palladium be deposited on the cordierite honeycomb ceramic matrix, carry palladium cordierite honeycomb ceramic automotive exhaust catalysis material thereby make.Its preparation technology is simple, greatly reduces production cost of products.Find simultaneously that on new preparation method basis the interpolation of auxiliary agent Ce and Ni can improve adsorbance and the dispersed uniform of Pd on matrix to a great extent, and good prospects for application is arranged.
Of the present invention year palladium iolite honeycomb ceramic catalyze material is by the cordierite honeycomb ceramic matrix and is carried on its surperficial palladium and constitutes that described palladium is carried on the cordierite honeycomb ceramic primary surface by chemical plating method.
Of the present invention year palladium iolite honeycomb ceramic catalyze material is the method by chemical palladium-plating on the cordierite honeycomb ceramic matrix, utilize the redox reaction between sodium hypophosphite and the palladium bichloride and the autocatalysis of palladium, make Metal Palladium be deposited on the cordierite honeycomb ceramic matrix and make.
The invention described above is carried the preparation method of palladium iolite honeycomb ceramic catalyze material, generally comprises following steps:
(1) to the surface preparation of cordierite honeycomb ceramic matrix: cordierite honeycomb ceramic matrix (being designated hereinafter simply as matrix) surfaces externally and internally is cleaned 30～40min with detergent solution and ultrasonic wave, taking out the matrix water rinses well, then this matrix being soaked in concentration is 25～30min in the 50g/L NaOH solution again, the etched the matrix surfaces externally and internally, take out the back with 1: in the 1HCl solution and remove the NaOH of remnants, be washed till neutral with deionized water again and continuation immersion 4～5h, then pull oven for drying out;
(2) preparation chemical palladium-plating solution:
The solution of Pd: 1.5～3.0g/L PdCl
2+ 30.0～40.0g/L NH
4(best proportioning is the ammoniacal liquor of Cl+160～200ml/L (25%): 2.4g/L PdCl
2+ 37.7g/L NH
4The ammoniacal liquor of Cl+192ml/L (25%));
Reducing solution: 9.0～15.0g/L NaH
2PO
2+ 30.0～40.0g/L NH
4(best proportioning is the ammoniacal liquor of Cl+160～200ml/L (25%): 12.0g/L NaH
2PO
2+ 37.7g/L NH
4The ammoniacal liquor of Cl+192ml/L (25%)).
Ready above-mentioned two kinds of reaction solutions are placed thermostat respectively, and the heating temperature control is at 40.0 ± 0.2 ℃;
(3) chemical palladium-plating: the matrix that step (1) was handled is put into reducing solution, and solution will not have matrix, and the control stir speed (S.S.) is 300～400rpm, soaked 3～7min; Take out matrix, dry, put it in the solution of Pd, operation requires with identical in reducing solution, take out after soaking 4～5min, blow with cold wind and to no longer include drop to the aperture and (can guarantee the uniformity of loaded liquid on the matrix like this, avoid the uneven distribution that causes owing to the liquid gravity settlement action in its reduction process), then blowing with hot blast (can allow a part of Pd restore under the effect of heat earlier like this, then utilizing the autocatalysis of Pd can make Pd reduce more thoroughly, thereby improve the utilization rate of Pd) black (black is represented matrix Pd in the load) appears relatively uniformly to matrix surface; The matrix of the above Pd of having is put into the solution of reducing solution and Pd successively respectively again, repeat aforesaid operations 1～3 time;
(4) post processing of plating palladium catalysis material: the plating palladium catalysis material that step (3) obtains is rinsed well with deionized water earlier, soaked 3～5min in the deionized water, take out, dry up, obtain carrying the palladium iolite honeycomb ceramic catalyze material and be placed on.
According to above-mentioned method, can also be in step (3) for the second time during soaking and reducing solution, in reducing solution, add the CeO of 0.12～0.81g/L again
2, or add the CeO of 0.12～0.81g/L in the reducing solution again
2NiCl with 0.15～0.82g/L
2.6H
2O.
Of the present invention year palladium iolite honeycomb ceramic catalyze material preparation method, employed cordierite honeycomb ceramic matrix surface is comparatively smooth, and its surface area has increase greatly after alkali corrosion.Use method of the present invention and carry out chemical palladium-plating, not only simplified operation sequence, and after adding auxiliary agent Ce, Ni, can obviously improve load capacity and the dispersed uniform of Pd on ceramic matrix.
Description of drawings
Fig. 1 is the SEM photo of the surperficial microstructure of blank sample (through the cordierite honeycomb ceramic matrix of the inventive method step 1 processing).
Fig. 2 is the SEM photo of the embodiment 1 surperficial microstructure that makes sample.
Fig. 3 is the SEM photo of the embodiment 3 surperficial microstructure that makes sample.
Fig. 4 is the SEM photo of the embodiment 7 surperficial microstructure that makes sample.
The specific embodiment
In order to further specify the present invention, enumerate following examples, but do not limit the scope of the invention.
Embodiment 1:
(1) to the surface preparation of cordierite honeycomb ceramic matrix: cordierite honeycomb ceramic matrix (being designated hereinafter simply as matrix) is soaked in the supersonic generator that fills liquid detergent solution, start supersonic generator, clean 30min, to remove the impurity such as greasy dirt of matrix surface.Taking out matrix rinses well successively with clear water and deionized water.Then this matrix being soaked in concentration again is about 30min in the 50g/LNaOH solution, with the etched the matrix surfaces externally and internally, takes out the back with 1: in the 1HCl solution and remove the NaOH of remnants.Take out surface matrix after treatment, be washed till neutral and continue with deionized water and soak about 4h, then pull out, put into oven drying 1h.Matrix after handling is cut into the specification of 4.0cm * 4.0cm.
(2) preparation chemical palladium-plating solution:
The solution of Pd: weighing 0.24g PdCl
2With 3.77g NH
4Cl is measured the 100mL deionized water in same beaker, will be wherein about 1/3rd add beakers, stirs.Ammoniacal liquor with 19.2mL adds beaker again, then pours remaining water into, stirs.
Reducing solution: weighing 1.20g NaH
2PO
2.H
2O and 3.77g NH
4Cl is measured the 100mL deionized water in same beaker, will be wherein about 1/3rd add beakers, stirs.Ammoniacal liquor with 19.2mL adds beaker again, then pours remaining water into, stirs.
Ready above-mentioned two kinds of reaction solutions are placed thermostat respectively, heating temperature control to 40.0 ± 0.2 ℃.
(3) chemical palladium-plating: the matrix that will handle is put into reducing solution (making solution not have matrix), and the control stir speed (S.S.) is 400rpm, soaks about 5min.Take out matrix, dry, put it in the solution of Pd, operation requires with identical in reducing solution, take out after soaking about 5min, to aperture, no longer include the drop (uniformity of loaded liquid on the assurance matrix with the cold blowing of hair dryer elder generation, avoid the uneven distribution that causes owing to the liquid gravity settlement action in its reduction process), then hot blow (allows a part of Pd restore under the effect of heat earlier, then the autocatalysis owing to Pd can make Pd reduce more thoroughly, thereby improves the utilization rate of Pd) to the relatively more uniform black of matrix surface appearance.Matrix after drying up is put into the solution of reducing solution and Pd successively respectively again, repeat aforesaid operations twice.
(4) post processing of plating palladium catalysis material: the sample that obtains is rinsed well with deionized water earlier, then in deionized water, soaked about 5min, take out, dry up.
The SEM photo of the surperficial microstructure of obtained sample as shown in Figure 2.
Embodiment 2:
With embodiment 1, just for the second time during soaking and reducing solution, in reducing solution, add 0.12g CeO
2
Embodiment 3:
With embodiment 1, just for the second time during soaking and reducing solution, in reducing solution, add 0.30g CeO
2
The surperficial microstructure of obtained sample as shown in Figure 3, the sample surfaces results of elemental analyses is as shown in table 1.
Embodiment 4:
With embodiment 1, just for the second time during soaking and reducing solution, in reducing solution, add 0.51g CeO
2
Embodiment 5:
With embodiment 1, just for the second time during soaking and reducing solution, in reducing solution, add 0.81g CeO
2
Embodiment 6:
With embodiment 1, just for the second time during soaking and reducing solution, in reducing solution, add 0.30g CeO
2And 0.15gNiCl
2.6H
2O.
Embodiment 7:
With embodiment 1, just for the second time during soaking and reducing solution, in reducing solution, add 0.30g CeO
2And 0.36gNiCl
2.6H
2O.
The surperficial microstructure of obtained sample as shown in Figure 4, the sample surfaces results of elemental analyses is as shown in table 1.
Embodiment 8:
With embodiment 1, just for the second time during soaking and reducing solution, in reducing solution, add 0.30g CeO
2And 0.50gNiCl
2.6H
2O.
Embodiment 9:
With embodiment 1, just for the second time during soaking and reducing solution, in reducing solution, add 0.30g CeO
2And 0.82gNiCl
2.6H
2O.
(white velvet-like granule is the material that contains Pd among the figure more as can be seen by gained sample electromicroscopic photograph among each embodiment, the rule blockage is the material that contains Ce), preparation method of the present invention can make Pd be carried on (Fig. 2) on the cordierite honeycomb ceramic matrix really, interpolation by auxiliary agent Ce and Ni simultaneously can improve the load capacity of Pd on matrix and the uniformity of distribution (Fig. 3, Fig. 4).
The elementary analysis of table 1. sample surfaces
| Embodiment | Pd | Ce | Ni | |||
| Weight％ | Atomic％ | Weight％ | Atomic％ | Weight％ | Atomic％ | |
| 3 | 13.45 | 4.02 | 5.56 | 1.26 | 0.00 | 0.00 |
| 7 | 18.91 | 5.81 | 3.44 | 0.80 | 0.50 | 0.28 |
By results of elemental analyses in the table as can be known, according to plating palladium method of the present invention, Pd, Ni and Ce all can load on matrix surface securely, and the interpolation of Ce, Ni simultaneously can improve load capacity and the dispersed uniform of Pd at matrix surface.
Claims (5)
1. Pd carried iolite honeycomb ceramic catalyze material by the cordierite honeycomb ceramic matrix and be carried on its surperficial palladium and constitute, is characterized in that described palladium is carried on the cordierite honeycomb ceramic matrix surface by chemical plating method.
2. the preparation method of a Pd carried iolite honeycomb ceramic catalyze material may further comprise the steps:
(1) to the surface preparation of cordierite honeycomb ceramic matrix: cordierite honeycomb ceramic matrix surfaces externally and internally is cleaned 30～40min with detergent solution and ultrasonic wave, take out matrix, water is rinsed well, then this matrix being soaked in concentration is 25～30min in the 50g/L NaOH solution again, the etched the matrix surfaces externally and internally takes out the back with 1: in the 1HCl solution and remove remaining NaOH, be washed till neutral with deionized water again and continue immersion 4～5h, then pull oven for drying out;
(2) preparation chemical palladium-plating solution:
The solution of Pd: 1.5～3.0g/L PdCl
2+ 30.0～40.0g/L NH
4The ammoniacal liquor of Cl+160～200ml/L, used ammonia concn are 25%;
Reducing solution: 9.0～15.0g/L NaH
2PO
2+ 30.0～40.0g/L NH
4The ammoniacal liquor of Cl+160～200ml/L, used ammonia concn are 25%;
Ready above-mentioned two kinds of solution are placed thermostat respectively, and the heating temperature control is at 40.0 ± 0.2 ℃;
(3) chemical palladium-plating: the matrix that step (1) was handled is put into reducing solution, and solution will not have matrix, and the control stir speed (S.S.) is 300～400rpm, soaked 3～7min; The taking-up matrix, drying puts it in the solution of Pd, and operation requires with identical in reducing solution, takes out behind immersion 4～5min, blows to aperture with cold wind to no longer include drop, then blows to the relatively more uniform black of matrix surface appearance with hot blast; The matrix of the above Pd of having is put into the solution of reducing solution and Pd successively respectively again, repeat aforesaid operations 1～3 time;
(4) post processing of plating palladium catalysis material: the plating palladium catalysis material that step (3) is obtained is earlier clean with distilled water flushing, soaks 3～5min in the distilled water and be placed on, and taking-up dries up, and obtains required year palladium iolite honeycomb ceramic catalyze material.
3. in accordance with the method for claim 2, the proportioning that it is characterized in that the solution of the described Pd of step (2) is: 2.4g/LPdCl
2+ 37.7g/L NH
4The ammoniacal liquor of Cl+192ml/L, used ammonia concn are 25%.
4. in accordance with the method for claim 2, the proportioning that it is characterized in that the described reducing solution of step (2) is: 12.0g/LNaH
2PO
2+ 37.7g/L NH
4The ammoniacal liquor of Cl+192ml/L, used ammonia concn are 25%.
5. according to the described method of claim 2,3 or 4, when it is characterized in that in step (3) for the second time soaking and reducing solution, in reducing solution, add the CeO of 0.12～0.81g/L again
2, or in reducing solution, add the CeO of 0.12～0.81g/L again
2NiCl with 0.15～0.82g/L
26H
2O.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100291990A CN100569361C (en) | 2007-07-18 | 2007-07-18 | Pd carried iolite honeycomb ceramic catalyze material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100291990A CN100569361C (en) | 2007-07-18 | 2007-07-18 | Pd carried iolite honeycomb ceramic catalyze material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101108343A true CN101108343A (en) | 2008-01-23 |
| CN100569361C CN100569361C (en) | 2009-12-16 |
Family
ID=39040719
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|---|---|---|---|
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Cited By (6)
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| CN102872865A (en) * | 2011-07-11 | 2013-01-16 | 中国石油化工股份有限公司 | Method for preparing honeycomb ceramic catalyst |
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| CN1076212C (en) * | 1996-05-08 | 2001-12-19 | 中国科学院大连化学物理研究所 | Method for preparation of extra-thin palladium-ceramic compound film |
| CN1065852C (en) * | 1997-01-31 | 2001-05-16 | 中国科学院大连化学物理研究所 | Gas phase catalytic dehydrogenating and hydrogenation coupled reaction in palladium/ceramic composite membrane reactor |
| CN1101727C (en) * | 1998-11-27 | 2003-02-19 | 华东理工大学 | Rare earth-noble metal catalyst for purifying motor vehicle exhaust and its preparing method |
| ATE326558T1 (en) * | 2001-08-30 | 2006-06-15 | Aktina Ltd | METHOD FOR PRODUCING POROUS CERAMIC-METAL COMPOSITE MATERIALS AND COMPOSITE MATERIALS OBTAINED THEREFROM |
| CN1864897A (en) * | 2005-05-18 | 2006-11-22 | 中国船舶重工集团公司第七二五研究所 | Ceramic microtube based nano metal material and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100569361C (en) | 2009-12-16 |
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