CN106552617B - A kind of Pd/TiO2C nano pipe catalyst and preparation method thereof - Google Patents
A kind of Pd/TiO2C nano pipe catalyst and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of Pd/TiO2C nano pipe catalyst is in terms of 100% by the gross mass of catalyst, wherein TiO2Mass percentage be 85-98%, Pd mass percentage be 0.1-5.5%, carbon mass percentage be 0.5-12%；Average caliber is 4-13nm, and the carbon of 93-98% is covered in TiO2The inner surface of nanotube.Preparation method simple possible, have the characteristics that it is low in cost and environmentally friendly, with the prior art, TiO2Nano tube supported Pd catalyst is compared, the Pd/TiO of the method for the present invention preparation2C nano pipe catalyst adhesive property is good, do not need to be added organic binder can machine-shaping, and than conventional TiO2Nano tube supported Pd catalyst has better 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 being prepared2C nano pipe is used for
Containing aldehyde compound plus hydrogen.
Background technique
TiO since the Japanese Scientists Lijima nineties in last century has found carbon nanotube, as semiconductor material2It receives
For mitron since surface electron rich structure receives the extensive concern of academia and industry, the emphasis of concern essentially consists in preparation work
The improvement of skill and it is surface-functionalized assign 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 pages of volume 18).TiO2It receives
The preparation process of mitron mainly includes the methods of hydrothermal synthesis under anodic oxidation electrochemical process, template and alkaline condition.Wherein,
It is considered as a kind of method (B Poudel, W Z easy to operate, cheap by the alkaline hydrothermal synthesis that Kasuga is proposed
Wang,C Dames, J Y Huang,S Kunwar,D Z Wang,D Banerjee,G Chen,Z F Ren,Formation
of crystallized titania nanotubes and their transformation into nanowires,
Nanotechnology, 2005 volume 16 page 1935-1940).
Related TiO2Nanotube surface functionalization assigns its catalytic performance and is reported in many documents.For example, Chinese
Patent of invention ZL200710024369.6 discloses TiO2The preparation method of nanotube, and further supported V2O5Component is used for first
Alcohol selective oxidation synthesizing dimethoxym ethane.Hu et al. is with TiO2Nano tube supported Pd catalyst shows for methyl orange photocatalysis Decomposition
Good activity (catalysis journal, 2015 221-228 pages of volume 36) out.TiO2Nano tube supported catalyst is although have good
Activity, but it is difficult to form, and intensity is poor, is also possible to impact activity after adding auxiliary agent.In view of the above problems,
Yang et al. uses SiO2To TiO2Nanotube is modified, and loads Pd for hydrogenation on cinnamic aldehyde, the results showed that the Modified catalytic
Agent is than non-SiO2Modified catalyst has preferably activity, and catalyst is due to SiO2Incorporation be also easy to processing and forming (RSC
Advances, 2014 63062-63069 pages of volume 4).
Summary of the invention
For single TiO2Nano-tube support is difficult to form, and introducing other components may result in activity reduction etc. and ask
Topic, the present invention pass through in TiO2Carbon-coating is modified in nanotube, increases its caking property, then further supported palladium, for containing aldehyde radical
Compound adds hydrogen, thus completes the present invention.
Technical solution
A kind of Pd/TiO2C nano pipe catalyst is in terms of 100% by the gross mass of catalyst, wherein TiO2Quality hundred
Dividing content is 85-98%, and Pd mass percentage is 0.1-5.5%, and carbon mass percentage is 0.5-12%；Average caliber is
The carbon of 4-13nm, 93-98% are covered in TiO2The inner surface of nanotube.
Above-mentioned Pd/TiO2The preparation method of C nano pipe catalyst, comprising the following steps:
(1) TiO is taken2Powder is added in the lye of 5-40wt%, and hydro-thermal reaction 12-48h obtains hydro-thermal at 100-180 DEG C
Product；
(2) it after being filtered, washed hydrothermal product, 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) product of contact of step (3) is roasted under the inert gas of entrainment Organic Alcohol, obtains TiO2- C composite Nano
Pipe；
(5) by the TiO of step (4)2- C composite nano tube is contacted with aqueous solution containing palladium, dry, is subsequently placed in inertia
Under gas roast to get.
In step (1), the lye is NaOH aqueous solution or KOH aqueous solution.
In step (2), the drying temperature is 40-85 DEG C.
In step (3), any one of the organic polymer in glucose, sucrose, phenolic resin or furfural.
In step (3), in order to guarantee that the solid of metatitanic acid comes into full contact with organic polymer, organic solvent or water is selected to make
For solvent.Any one of organic solvent in methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol or the tert-butyl alcohol.
In step (4), the Organic Alcohol is any one in normal propyl alcohol, isopropanol, n-butanol, isobutanol or the tert-butyl alcohol
Kind.
It in step (4), carries secretly in the inert gas of Organic Alcohol, the amount of the Organic Alcohol of entrainment and the mass ratio of inert gas are
1:100-1:800。
In step (4), maturing temperature is 350-550 DEG C.
In step (5), maturing temperature is 100-350 DEG C.
In step (4) and (5), the inert gas is selected from N2, He or Ar gas.
In step (5), aqueous solution containing palladium refers to palladium chloride, palladium 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, Pd/TiO above-mentioned is further related to2C nano pipe catalyst is prepared according to the present invention above-mentioned
The Pd/TiO of method preparation2C nano pipe catalyst is adding the application in hydrogen containing aldehyde compound.
Above-mentioned Pd/TiO2C catalyst is adding the application in hydrogen containing aldehyde compound, by the catalyst at 100-300 DEG C
At a temperature of hydrogen reducing 1-3h, be passed through aldehyde compound, hydrogenation reaction, product then carried out under 40-300 DEG C of reaction temperature
Using gas-chromatography 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 benzaldehyde, terephthalaldehyde.
Technical effect
Pd/TiO according to the present invention2C nano pipe catalyst, preparation method simple possible have low in cost and right
Environmental-friendly feature, and the carbon-coating of 93%-98% is attached to TiO2The inner surface of nanotube.With the routine of the prior art
TiO2Nano tube supported Pd catalyst is compared, the Pd/TiO of the method for the present invention preparation2C nano pipe catalyst adhesive property is good,
Do not need to be added organic binder can machine-shaping, and than conventional TiO2Nano tube supported Pd catalyst has better
Aldehyde hydrogenation activity.
Specific embodiment
The present invention is further explained in the light of specific embodiments.In the present invention, Pd content using plasma hair
Spectrum analysis is penetrated, C content is determined using thermogravimetric method, and the inside and outside distribution in hole uses tem observation.
Embodiment 1
Take TiO2100 mass parts of powder are added to the NaOH aqueous solution that 500 mass parts mass fractions are 10%, at 120 DEG C
Lower hydro-thermal reaction obtains hydrothermal product for 24 hours, and the product after hydro-thermal reaction is filtered, washed, and 60 DEG C of dry 5h are obtained containing metatitanic acid
Solid.100 mass parts of solid after taking drying are mixed with the aqueous solution of 60 mass parts glucose, are stirred, 40 DEG C of dryings, in N2
The lower 400 DEG C of roastings of mixed atmosphere with normal propyl alcohol obtain TiO2C nano pipe.By upper TiO210 mass parts of C nano pipe, which are scattered in, to be contained
0.05 mass parts PdCl2Aqueous solution in, stirring, 50 DEG C of dryings, 400 DEG C roast up to Pd/TiO2C nano pipe A, measures it
Middle Pd mass percentage is 0.3%, and carbon mass percentage is 4.1%, and carbon 98% is covered in TiO2The inner surface of nanotube,
Average caliber is 9.5nm.
Embodiment 2
Take TiO2100 mass parts of powder add 400 mass parts mass fractions to be 20% KOH aqueous solution, the hydro-thermal at 130 DEG C
Reaction 48h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, washed, 70 DEG C of dry 5h obtain the solid containing metatitanic acid.
100 mass parts of solid after taking drying are mixed with the water-methanol solution of 80 mass parts phenolic resin, are stirred, 50 DEG C of dryings, in N2
The lower 420 DEG C of roastings of mixed atmosphere with n-butanol obtain TiO2C nano pipe.By upper TiO210 mass parts of C nano pipe are scattered in
Containing 0.2 mass parts PdCl2Aqueous solution in, stirring, 50 DEG C of dryings, 450 DEG C roast up to Pd/TiO2C nano pipe B, measures it
Middle Pd mass percentage is 1.1%, and carbon mass percentage is 6.0%, and carbon 97.5% is covered in TiO2The interior table of nanotube
Face, average caliber are 9.0nm.
Embodiment 3
Take TiO2100 mass parts of powder add 400 mass parts mass fractions to be 20% KOH aqueous solution, the hydro-thermal at 110 DEG C
Reaction 48h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, washed, 65 DEG C of dry 5h obtain the solid containing metatitanic acid.
100 mass parts of solid after taking drying are mixed with the butanol solution of 90 mass parts furfurals, are stirred, 50 DEG C of dryings, in N2With it is different
The lower 380 DEG C of roastings of the mixed atmosphere of butanol obtain TiO2C nano pipe.By upper TiO210 mass parts of C nano pipe are scattered in containing 0.2
Mass parts PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 500 DEG C roast up to Pd/TiO2- C nanotube C, measures wherein Pd
Mass percentage is 2.3%, and carbon mass percentage is 8.3%, and carbon 96.5% is covered in TiO2The inner surface of nanotube,
Average caliber is 7.1nm.
Embodiment 4
Take TiO2100 mass parts of powder add 500 mass parts mass fractions to be 5% NaOH aqueous solution, the hydro-thermal at 150 DEG C
Reaction 20h obtains hydrothermal product, the product after hydro-thermal reaction is filtered, washed, 60 DEG C of dry 8h obtain the solid containing metatitanic acid.
100 mass parts of solid after taking drying are mixed with the aqueous solution of 50 mass parts glucose, are stirred, 50 DEG C of dryings, in N2With positive third
The lower 530 DEG C of roastings of the mixed atmosphere of alcohol obtain TiO2C nano pipe.By upper TiO210 mass parts of C nano pipe are scattered in 0.9 mass
Part PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 480 DEG C roast up to Pd/TiO2C nano pipe D measures wherein Pd mass hundred
Dividing content is 5.0%, and carbon mass percentage is 6.6%, and sulfate radical mass percentage is 0.9%, and 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 300 mass parts mass fractions to be 40% NaOH aqueous solution, are lauched at 140 DEG C
Thermal response 30h obtains hydrothermal product, and the product after hydro-thermal reaction is filtered, washed, and 80 DEG C of dry 5h obtain consolidating containing metatitanic acid
Body.100 mass parts of solid after taking drying are mixed with the ethanol solution of 50 mass parts phenolic resin, are stirred, 50 DEG C of dryings, in N2
The lower 380 DEG C of roastings of mixed atmosphere with n-butanol obtain TiO2C nano pipe.By upper TiO210 mass parts of C nano pipe are scattered in
0.6 mass parts PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 460 DEG C roast up to Pd/TiO2- C nanotube E, measures wherein
Pd mass percentage is 3.3%, and carbon mass percentage is 10.9%, and carbon 95.3% is covered in TiO2The interior table of nanotube
Face, average caliber are 6.1nm.
Embodiment 6
Take TiO2100 mass parts of powder add 400 mass parts mass fractions to be 20% NaOH aqueous solution, are lauched at 140 DEG C
Thermal response 30h obtains hydrothermal product, and the product after hydro-thermal reaction is filtered, washed, and 75 DEG C of dry 5h obtain consolidating containing metatitanic acid
Body.100 mass parts of solid after taking drying are mixed with the aqueous solution of 60 mass parts phenolic resin, are stirred, 50 DEG C of dryings, in N2With
The lower 450 DEG C of roastings of the mixed atmosphere of n-butanol obtain TiO2C nano pipe.By upper TiO210 mass parts of C nano pipe are scattered in
0.003 mass parts PdCl2Aqueous solution in, stirring, 60 DEG C of dryings, 400 DEG C roast up to Pd/TiO2C nano pipe F, measures it
Middle Pd mass percentage is 0.1%, and carbon mass percentage is 12.2%, and carbon 93.1% is covered in TiO2Nanotube it is interior
Surface, average caliber are 12nm.
Comparative example 1
Take TiO2100 mass parts of powder add 400 mass parts mass fractions to be 20% NaOH aqueous solution, are lauched at 140 DEG C
Thermal response 30h obtains hydrothermal product, and the product after hydro-thermal reaction is filtered, washed, and 75 DEG C of dry 5h obtain consolidating containing metatitanic acid
Body, in N2TiO is obtained with 450 DEG C of roastings2Nanotube.By upper TiO211 mass parts of nanotube are scattered in 0.003 mass parts PdCl2
Aqueous solution in, stirring, 60 DEG C of dryings, 400 DEG C roast up to Pd/TiO2Nanotube G measures wherein Pd mass percentage
It is 0.1%, average caliber is 14nm.
1. the strength test of preformed catalyst
The Pd/TiO in 100 mass parts embodiments 5 is taken respectively2Pd/ in C nano pipe E and 100 mass parts comparative examples 1
TiO2Nanotube G is respectively added 1 part of nitric acid that mass concentration is 63%, the water of 8 mass parts is added, mediates, extrusion, 450 DEG C of roastings
It burns, tests the intensity of preformed catalyst.
Test measures: the intensity of the preformed catalyst of embodiment 5 is 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 is tested
(1) catalyst in embodiment 1-6 and comparative example 1 is weighed into 1 mass parts respectively, under 250 DEG C of hydrogen atmospheres also
Original is then transferred in reaction kettle, and the 4- carboxyl benzaldehyde of 9 mass parts is added in a kettle, is added under the conditions of 4MPa and 280 DEG C
Hydrogen 1h, conversion results are shown in Table 1.
4- carboxyl benzaldehyde adds hydrogen 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 also
Original, is then passed through acetaldehyde 0.05ml/min, hydrogen 10ml/min, and under the conditions of normal pressure and 40 DEG C plus hydrogen 1h, conversion results are shown in Table 2
It is shown.
Acetaldehyde adds hydrogen result in 2 different catalysts of table
It can be seen that from the test result of Tables 1 and 2 and aldehyde compound carried out using catalyst of the invention to add hydrogen,
With better hydrogenation activity, conversion ratio is higher.
Claims (9)
1. a kind of Pd/TiO2C nano pipe catalyst, which is characterized in that by the gross mass of catalyst be 100% in terms of, wherein TiO2
Mass percentage be 85-98%, Pd mass percentage be 0.1-5.5%, carbon mass percentage be 0.5-12%；It is flat
Equal caliber is 4-13nm, and the carbon of 93-98% is covered in TiO2The inner surface of nanotube；The Pd/TiO2C nano pipe catalyst by
Following methods are prepared:
1) according to above-mentioned mass percentage ratio, TiO is taken2Powder is added in the lye of 5-40wt%, is lauched at 100-180 DEG C
Thermal response 12-48h obtains hydrothermal product；
2) it after being filtered, washed hydrothermal product, is dried, obtains the solid containing metatitanic acid；
3) solid in step 2) containing metatitanic acid is contacted with organic polymer, obtains product of contact；
4) product of contact of step 3) is roasted under the inert gas of entrainment Organic Alcohol, obtains TiO2- C composite nano tube；
5) by the TiO of step 4)2- C composite nano tube is contacted with aqueous solution containing palladium, dry, is subsequently placed under inert gas and is roasted
Burn to get.
2. Pd/TiO as described in claim 12C nano pipe catalyst, which is characterized in that the lye be NaOH aqueous solution or
KOH aqueous solution.
3. Pd/TiO as described in claim 12C nano pipe catalyst, which is characterized in that in step 2), the drying temperature
It is 40-85 DEG C.
4. Pd/TiO as described in claim 12C nano pipe catalyst, which is characterized in that in step 3), organic high score
Any one of son in glucose, sucrose, phenolic resin or furfural.
5. Pd/TiO as described in claim 12C nano pipe catalyst, which is characterized in that in step 4), the Organic Alcohol choosing
From any one in normal propyl alcohol, isopropanol, n-butanol, isobutanol or the tert-butyl alcohol.
6. Pd/TiO as described in claim 12C nano pipe catalyst, which is characterized in that in step 4), carry Organic Alcohol secretly
In inert gas, the amount of the Organic Alcohol of entrainment and the mass ratio of inert gas are 1:100-1:800.
7. Pd/TiO as described in claim 12C nano pipe catalyst, which is characterized in that in step 4), maturing temperature is
350-550℃。
8. Pd/TiO as described in claim 12C nano pipe catalyst, which is characterized in that in step 5), maturing temperature is
100-350℃。
9. Pd/TiO as claimed in any one of claims 1 to 82C nano pipe catalyst, which is characterized in that in step 5), contain
The aqueous solution of palladium refers to palladium chloride, palladium nitrate or acetic acid aqueous palladium, and wherein the mass ratio of water and metal salt is 300:1-50:1.
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| 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 |
| 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 |
| 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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| CN101249429A (en) * | 2007-11-12 | 2008-08-27 | 浙江理工大学 | Preparation of titanic oxide nano pipe light catalyst with hollow protection layer |
| CN102139211A (en) * | 2010-02-02 | 2011-08-03 | 中国石油化工股份有限公司 | Method for preparing noble metal/TiO2-C catalyst for hydrofining of crude terephthalic acid |
| CN102139230A (en) * | 2010-02-02 | 2011-08-03 | 中国石油化工股份有限公司 | Method for preparing TiO2-C composite carrier for p-carboxybenzaldehyde hydrogenation process |
| CN102157732A (en) * | 2011-03-24 | 2011-08-17 | 河南大学 | Titanium dioxide/carbon composite nanotube and preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101249429A (en) * | 2007-11-12 | 2008-08-27 | 浙江理工大学 | Preparation of titanic oxide nano pipe light catalyst with hollow protection layer |
| CN102139211A (en) * | 2010-02-02 | 2011-08-03 | 中国石油化工股份有限公司 | Method for preparing noble metal/TiO2-C catalyst for hydrofining of crude terephthalic acid |
| CN102139230A (en) * | 2010-02-02 | 2011-08-03 | 中国石油化工股份有限公司 | Method for preparing TiO2-C composite carrier for p-carboxybenzaldehyde hydrogenation process |
| CN102157732A (en) * | 2011-03-24 | 2011-08-17 | 河南大学 | Titanium dioxide/carbon composite nanotube and preparation and application thereof |
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