CN106552617A - A kind of Pd/TiO2- C nano pipe catalyst and preparation method thereof - Google Patents
A kind of Pd/TiO2- C nano pipe catalyst and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Pd/TiO2- C nano pipe catalyst, is counted with the gross mass of catalyst as 100%, wherein, TiO2Weight/mass percentage composition be 85-98%, Pd weight/mass percentage compositions be 0.1-5.5%, carbon weight/mass percentage composition be 0.5-12%；Average caliber is 4-13nm, and the carbon of 93-98% is covered in TiO2The inner surface of nanotube.Its preparation method simple possible, with it is with low cost and environmentally friendly the characteristics of, with prior art, TiO2Nano tube supported Pd catalyst is compared, Pd/TiO prepared by the inventive method2- C nano pipe catalyst adhesive property is good, it is not necessary to add machine-shaping by organic binder bond, and than conventional TiO2Nano tube supported Pd catalyst has more preferable aldehyde hydrogenation activity.
Description
Technical field
The present invention relates to a kind of Pd/TiO2The preparation method of-C nano pipe, the Pd/TiO for preparing2- C nano pipe is used to contain
Aldehyde compound is hydrogenated with.
Background technology
Since the Japanese Scientists Lijima discoveries nineties in last century CNT, as the TiO of semi-conducting material2Nanometer
Pipe receives the extensive concern of academia and industrial quarters due to surface electron rich structure, and the emphasis of concern essentially consists in preparation technology
Improvement and surface-functionalized imparting its catalysis, absorption and photoelectric properties (D.V.Bavykin, J.M.Friedrich, F.C.Walsh,
Protonated Titanates and TiO2Nanostructured Materials:Synthesis,Properties,and
Applications, Advanced Materials, 2006 2807-2824 page of volume 18).TiO2The preparation technology master of nanotube
To include the method such as Hydrothermal Synthesiss under anodic oxidation electrochemical process, template and alkalescence condition.Wherein, proposed by Kasuga
Alkaline Hydrothermal Synthesiss be considered as method a kind of simple to operate, cheap (B Poudel, W Z Wang, C Dames,
J Y Huang,S Kunwar,D Z Wang,D Banerjee,G Chen,Z F Ren,Formation of crystallized
Volume 16 of titania nanotubes and their transformation into nanowires, Nanotechnology, 2005 year
Page 1935-1940).
Relevant TiO2Nanotube surface functionalization gives its catalytic performance and has reported in many documents.For example, middle promulgated by the State Council
Bright patent ZL200710024369.6 discloses TiO2The preparation method of nanotube, and further supported V2O5Component is used for
Selective oxidation of methanol synthesizing dimethoxym ethane.Hu et al. is with TiO2Nano tube supported Pd catalyst is for methyl orange photocatalysis point
Solution shows good activity (catalysis journal, 2015 221-228 page of volume 36).TiO2Nano tube supported catalyst
Although with good activity, which is difficult to molding, and intensity is poor, is also possible to impact activity after addition auxiliary agent.
SiO is adopted for problem above, Yang et al.2To TiO2Nanotube is modified, and loads Pd for hydrogenation on cinnamic aldehyde,
As a result show the modified catalyst than non-SiO2Modified catalyst has preferably activity, and catalyst is due to SiO2Mix
Enter to be also easy to processing and forming (RSC Advances, 2014 63062-63069 page of volume 4).
The content of the invention
For single TiO2Nano-tube support is difficult to molding, and the problems such as introduce other components and may result in activity and reduce,
The present invention is by TiO2In nanotube, modification carbon-coating, increases its caking property, then further supported palladium, for containing aldehyde radical
Compound is hydrogenated with, and thus completes the present invention.
Technical scheme
A kind of Pd/TiO2- C nano pipe catalyst, is counted with the gross mass of catalyst as 100%, wherein, TiO2Quality hundred
Content is divided to be 85-98%, Pd weight/mass percentage compositions are 0.1-5.5%, and carbon weight/mass percentage composition is 0.5-12%；Average caliber
For 4-13nm, the carbon of 93-98% is covered in TiO2The inner surface of nanotube.
Above-mentioned Pd/TiO2The preparation method of-C nano pipe catalyst, comprises the following steps：
(1) take TiO2During powder adds the alkali liquor of 5-40wt%, at 100-180 DEG C, hydro-thermal reaction 12-48h obtains hydro-thermal
Product；
(2), after by hydrothermal product filtration, washing, it is dried, obtains the solid containing metatitanic acid；
(3) solid containing metatitanic acid in step (2) is contacted with organic polymer, obtains product of contact；
(4) by the roasting under the noble gases of entrainment Organic Alcohol of the product of contact of step (3), obtain TiO2- C is compound to be received
Mitron；
(5) by the TiO of step (4)2- C composite nano tubes are contacted with the aqueous solution containing palladium, are dried, are subsequently placed in lazy
Roasting under property gas, obtains final product.
In step (1), the alkali liquor is NaOH aqueous solutions or KOH aqueous solutions.
In step (2), the baking temperature is 40-85 DEG C.
In step (3), the organic polymer is selected from any one in glucose, sucrose, phenolic resin or furfural.
In step (3), in order to ensure that the solid of metatitanic acid and organic polymer are fully contacted, organic solvent or water is selected to make
For solvent.Organic solvent is any in methanol, ethanol, normal propyl alcohol, isopropanol, n-butyl alcohol, isobutanol or the tert-butyl alcohol
It is a kind of.
In step (4), the Organic Alcohol is any in normal propyl alcohol, isopropanol, n-butyl alcohol, isobutanol or the tert-butyl alcohol
It is a kind of.
In step (4), carry secretly in the noble gases of Organic Alcohol, the amount of the Organic Alcohol of entrainment with the mass ratio of noble gases is
1:100-1:800。
In step (4), sintering temperature is 350-550 DEG C.
In step (5), sintering temperature is 100-350 DEG C.
In step (4) and (5), the noble gases are selected from N2, He or Ar gas.
In step (5), the aqueous solution containing palladium refers to Palladous chloride., Palladous nitrate. or acetic acid aqueous palladium, wherein water and metal
The mass ratio of salt is 300:1-50:1.
According to the present invention, aforesaid Pd/TiO is further related to2- C nano pipe catalyst or according to aforesaid preparation method of the present invention
The Pd/TiO of preparation2Application of-C nano pipe the catalyst in containing aldehyde compound hydrogenation.
Above-mentioned Pd/TiO2Application of-the C catalyst in containing aldehyde compound hydrogenation, will be the catalyst warm at 100-300 DEG C
The lower hydrogen reducing 1-3h of degree, is passed through aldehyde compound, then carries out hydrogenation reaction under 40-300 DEG C of reaction temperature, produce
Thing adopts gas chromatogram and liquid-phase chromatographic analysis.Wherein, aldehyde compound refers to the aldehyde containing alkyl group, aromatic hydrocarbon group,
Including formaldehyde, acetaldehyde, propionic aldehyde, benzaldehyde, 4- carboxyl benzaldehydes, terephthalaldehyde.
Technique effect
Pd/TiO of the invention2- C nano pipe catalyst, its preparation method simple possible, with low cost and to ring
The characteristics of border is friendly, and the carbon-coating of 93%-98% is attached to TiO2The inner surface of nanotube.With the conventional TiO of prior art2
Nano tube supported Pd catalyst is compared, Pd/TiO prepared by the inventive method2- C nano pipe catalyst adhesive property is good,
Machine-shaping by organic binder bond need not be added, and than conventional TiO2Nano tube supported Pd catalyst has more preferable
Aldehyde hydrogenation activity.
Specific embodiment
With reference to specific embodiment, the invention will be further described.In the present invention, the transmitting of Pd contents using plasma
Spectrum analyses, C content determine that using thermogravimetric method the inside and outside distribution in hole adopts tem observation.
Embodiment 1
Take TiO2100 mass parts of powder are added to the NaOH aqueous solutions that 500 mass parts mass fractions are 10%, at 120 DEG C
Lower hydro-thermal reaction 24h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, is washed, and 60 DEG C are dried 5h and are contained
The solid of metatitanic acid.The aqueous solution of 100 mass parts of dried solid and 60 mass parts glucoses is taken, is stirred, 40 DEG C
It is dried, in N2400 DEG C of roastings lower with the mixed atmosphere of normal propyl alcohol obtain TiO2- C nano pipe.By upper TiO2- C nano pipe
10 mass parts are scattered in containing 0.05 mass parts PdCl2Aqueous solution in, stirring, 50 DEG C of dryings, 400 DEG C of roastings are obtained final product
Pd/TiO2- C nano pipe A, it is 0.3% to measure wherein Pd weight/mass percentage compositions, and carbon weight/mass percentage composition is 4.1%, carbon 98%
It is covered in TiO2The inner surface of nanotube, average caliber are 9.5nm.
Embodiment 2
Take TiO2100 mass parts of powder add the KOH aqueous solutions that 400 mass parts mass fractions are 20%, the water at 130 DEG C
Thermal response 48h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, is washed, and 70 DEG C are dried 5h and obtain containing metatitanic acid
Solid.The water-methanol solution that 100 mass parts of dried solid are taken with 80 mass parts phenolic resin mixes, stirring, 50 DEG C
It is dried, in N2420 DEG C of roastings lower with the mixed atmosphere of n-butyl alcohol obtain TiO2- C nano pipe.By upper TiO2- C nano pipe
10 mass parts are scattered in containing 0.2 mass parts PdCl2Aqueous solution in, stirring, 50 DEG C of dryings, 450 DEG C of roastings are obtained final product
Pd/TiO2- C nano pipe B, it is 1.1% to measure wherein Pd weight/mass percentage compositions, and carbon weight/mass percentage composition is 6.0%, carbon 97.5%
It is covered in TiO2The inner surface of nanotube, average caliber are 9.0nm.
Embodiment 3
Take TiO2100 mass parts of powder add the KOH aqueous solutions that 400 mass parts mass fractions are 20%, the water at 110 DEG C
Thermal response 48h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, is washed, and 65 DEG C are dried 5h and obtain containing metatitanic acid
Solid.The butanol solution that 100 mass parts of dried solid are taken with 90 mass parts furfurals mixes, stirring, and 50 DEG C are done
It is dry, in N2380 DEG C of roastings lower with the mixed atmosphere of isobutanol obtain TiO2- C nano pipe.By upper TiO2- C nano pipe 10
Mass parts are scattered in containing 0.2 mass parts PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 500 DEG C of roastings obtain final product Pd/TiO2-C
Nanotube C, it is 2.3% to measure wherein Pd weight/mass percentage compositions, and carbon weight/mass percentage composition is 8.3%, and carbon 96.5% is covered in
TiO2The inner surface of nanotube, average caliber are 7.1nm.
Embodiment 4
Take TiO2100 mass parts of powder add the NaOH aqueous solutions that 500 mass parts mass fractions are 5%, the water at 150 DEG C
Thermal response 20h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, is washed, and 60 DEG C are dried 8h and obtain containing metatitanic acid
Solid.The aqueous solution of 100 mass parts of dried solid and 50 mass parts glucoses is taken, is stirred, 50 DEG C of dryings,
In N2530 DEG C of roastings lower with the mixed atmosphere of normal propyl alcohol obtain TiO2- C nano pipe.By upper TiO210 mass of-C nano pipe
Part is scattered in 0.9 mass parts PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 480 DEG C of roastings obtain final product Pd/TiO2- C nano
Pipe D, it is 5.0% to measure wherein Pd weight/mass percentage compositions, and carbon weight/mass percentage composition is 6.6%, and sulfate radical quality percentage contains
Measure as 0.9%, carbon 97.3% is covered in TiO2The inner surface of nanotube, average caliber are 4.8nm.
Embodiment 5
Take TiO2100 mass parts of powder add the NaOH aqueous solutions that 300 mass parts mass fractions are 40%, at 140 DEG C
Hydro-thermal reaction 30h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, is washed, and 80 DEG C are dried 5h and obtain containing titanium
The solid of acid.The ethanol solution that 100 mass parts of dried solid are taken with 50 mass parts phenolic resin mixes, stirring, 50 DEG C
It is dried, in N2380 DEG C of roastings lower with the mixed atmosphere of n-butyl alcohol obtain TiO2- C nano pipe.By upper TiO2- C nano pipe
10 mass parts are scattered in 0.6 mass parts PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 460 DEG C of roastings obtain final product Pd/TiO2-C
Nanotube E, it is 3.3% to measure wherein Pd weight/mass percentage compositions, and carbon weight/mass percentage composition is 10.9%, and carbon 95.3% is covered
In TiO2The inner surface of nanotube, average caliber are 6.1nm.
Embodiment 6
Take TiO2100 mass parts of powder add the NaOH aqueous solutions that 400 mass parts mass fractions are 20%, at 140 DEG C
Hydro-thermal reaction 30h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, is washed, and 75 DEG C are dried 5h and obtain containing titanium
The solid of acid.The aqueous solution of 100 mass parts of dried solid and 60 mass parts phenolic resin is taken, is stirred, 50 DEG C
It is dried, in N2450 DEG C of roastings lower with the mixed atmosphere of n-butyl alcohol obtain TiO2- C nano pipe.By upper TiO2- C nano pipe
10 mass parts are scattered in 0.003 mass parts PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 400 DEG C of roastings are obtained final product
Pd/TiO2- C nano pipe F, it is 0.1% to measure wherein Pd weight/mass percentage compositions, and carbon weight/mass percentage composition is 12.2%, carbon
93.1% is covered in TiO2The inner surface of nanotube, average caliber are 12nm.
Comparative example 1
Take TiO2100 mass parts of powder add the NaOH aqueous solutions that 400 mass parts mass fractions are 20%, at 140 DEG C
Hydro-thermal reaction 30h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, is washed, and 75 DEG C are dried 5h and obtain containing titanium
The solid of acid, in N2TiO is obtained with 450 DEG C of roastings2Nanotube.By upper TiO211 mass parts of nanotube are scattered in 0.003
Mass parts PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 400 DEG C of roastings obtain final product Pd/TiO2Nanotube G, measures wherein
Pd weight/mass percentage compositions are 0.1%, and average caliber is 14nm.
1. the strength test of preformed catalyst
The Pd/TiO in 100 mass parts embodiments 5 is taken respectively2In-C nano pipe E and 100 mass parts comparative examples 1
Pd/TiO2Nanotube G, each adds 1 part of the nitric acid that mass concentration is 63%, adds the water of 8 mass parts, mediate, squeeze
Bar, 450 DEG C of roastings test the intensity of preformed catalyst.
Test is measured：The intensity of the preformed catalyst of embodiment 5 be 130N/cm, the intensity of the preformed catalyst of comparative example 1
For 60N/cm.The intensity of the preformed catalyst of embodiment 5 is high, more suitable for industrial applications.
2. aldehyde hydrogenation activity test
(1) catalyst in embodiment 1-6 and comparative example 1 is weighed into 1 mass parts respectively, under 250 DEG C of hydrogen atmospheres
Reduction, then proceeds in reactor, adds the 4- carboxyl benzaldehydes of 9 mass parts in a kettle., at 4MPa and 280 DEG C
Under the conditions of be hydrogenated with 1h, conversion results are shown in Table 1.
4- carboxyl benzaldehydes hydrogenation result in 1 different catalysts of table
(2) catalyst in embodiment 1-6 and comparative example 1 is weighed into 1 mass parts respectively, under 250 DEG C of hydrogen atmospheres
Reduction, is then passed through acetaldehyde 0.05ml/min, hydrogen 10ml/min, is hydrogenated with 1h, conversion ratio knot under the conditions of normal pressure and 40 DEG C
Fruit is shown in Table 2.
Acetaldehyde hydrogenation result in 2 different catalysts of table
Can be seen that from the test result of Tables 1 and 2 and aldehyde compound is hydrogenated with using the catalyst of the present invention, have
There is more preferable hydrogenation activity, conversion ratio is higher.
Claims (10)
1. a kind of Pd/TiO2- C nano pipe catalyst, it is characterised in that counted with the gross mass of catalyst as 100%, wherein, TiO2
Weight/mass percentage composition be 85-98%, Pd weight/mass percentage compositions be 0.1-5.5%, carbon weight/mass percentage composition be 0.5-12%；Averagely
Caliber is 4-13nm, and the carbon of 93-98% is covered in TiO2The inner surface of nanotube.
2. the Pd/TiO described in claim 12The preparation method of-C nano pipe catalyst, it is characterised in that comprise the following steps：
(1) according to above-mentioned weight/mass percentage composition ratio, take TiO2During powder adds the alkali liquor of 5-40wt%, at 100-180 DEG C
Hydro-thermal reaction 12-48h obtains hydrothermal product；
(2), after by hydrothermal product filtration, washing, it is dried, obtains the solid containing metatitanic acid；
(3) solid containing metatitanic acid in step (2) is contacted with organic polymer, obtains product of contact；
(4) by the roasting under the noble gases of entrainment Organic Alcohol of the product of contact of step (3), obtain TiO2- C composite nano tubes；
(5) by the TiO of step (4)2- C composite nano tubes are contacted with the aqueous solution containing palladium, are dried, are subsequently placed in indifferent gas
Roasting under body, obtains final product.
3. Pd/TiO as claimed in claim 22The preparation method of-C nano pipe catalyst, it is characterised in that the alkali liquor is
NaOH aqueous solutions or KOH aqueous solutions.
4. Pd/TiO as claimed in claim 22The preparation method of-C nano pipe catalyst, it is characterised in that in step (2),
The baking temperature is 40-85 DEG C.
5. Pd/TiO as claimed in claim 22The preparation method of-C nano pipe catalyst, it is characterised in that in step (3),
The organic polymer is selected from any one in glucose, sucrose, phenolic resin or furfural.
6. Pd/TiO as claimed in claim 22The preparation method of-C nano pipe catalyst, it is characterised in that in step (4),
The Organic Alcohol is selected from any one in normal propyl alcohol, isopropanol, n-butyl alcohol, isobutanol or the tert-butyl alcohol.
7. Pd/TiO as claimed in claim 22The preparation method of-C nano pipe catalyst, it is characterised in that in step (4),
In the noble gases of entrainment Organic Alcohol, the amount of the Organic Alcohol of entrainment is 1 with the mass ratio of noble gases:100-1:800.
8. Pd/TiO as claimed in claim 22The preparation method of-C nano pipe catalyst, it is characterised in that in step (4),
Sintering temperature is 350-550 DEG C.
9. Pd/TiO as claimed in claim 22The preparation method of-C nano pipe catalyst, it is characterised in that in step (5),
Sintering temperature is 100-350 DEG C.
10. the Pd/TiO as described in any one of claim 2 to 92The preparation method of-C nano pipe catalyst, it is characterised in that
In step (5), the aqueous solution containing palladium refers to Palladous chloride., Palladous nitrate. or acetic acid aqueous palladium, the wherein quality of water and slaine
Than for 300:1-50:1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109395720A (en) * | 2017-08-16 | 2019-03-01 | 中国石化扬子石油化工有限公司 | A kind of Pd/TiO2-SiO2Nano tube catalyst and its preparation method and application |
| CN109395725A (en) * | 2017-08-16 | 2019-03-01 | 中国石化扬子石油化工有限公司 | A kind of Au/TiO2C nano pipe catalyst and its preparation method and application |
| CN110961093A (en) * | 2018-09-28 | 2020-04-07 | 中国石油化工股份有限公司 | Cr-Zr-O/TiO2-C nanotube catalyst, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109395720A (en) * | 2017-08-16 | 2019-03-01 | 中国石化扬子石油化工有限公司 | A kind of Pd/TiO2-SiO2Nano tube catalyst and its preparation method and application |
| CN109395725A (en) * | 2017-08-16 | 2019-03-01 | 中国石化扬子石油化工有限公司 | A kind of Au/TiO2C nano pipe catalyst and its preparation method and application |
| CN109395720B (en) * | 2017-08-16 | 2021-12-03 | 中国石化扬子石油化工有限公司 | Pd/TiO2-SiO2Nanotube catalyst and preparation method and application thereof |
| CN109395725B (en) * | 2017-08-16 | 2021-12-03 | 中国石化扬子石油化工有限公司 | Au/TiO2-C nanotube catalyst, preparation method and application thereof |
| CN110961093A (en) * | 2018-09-28 | 2020-04-07 | 中国石油化工股份有限公司 | Cr-Zr-O/TiO2-C nanotube catalyst, preparation method and application thereof |
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