CN108579743A - A kind of preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation - Google Patents
A kind of preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation Download PDFInfo
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- CN108579743A CN108579743A CN201810250404.4A CN201810250404A CN108579743A CN 108579743 A CN108579743 A CN 108579743A CN 201810250404 A CN201810250404 A CN 201810250404A CN 108579743 A CN108579743 A CN 108579743A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G2209/00—Specific waste
- F23G2209/14—Gaseous waste or fumes
Abstract
The invention discloses a kind of preparation methods of the low temperature high activity catalyst of catalysis benzene complete oxidation, carrier is first added in the solution, fully heating reduction is carried out again after absorption chloroplatinic acid, specific method includes quantitatively weighing carrier, it immerses in ethylene glycol, then chloroplatinic acid aqueous solution is added, add NaOH aqueous solutions adjustment solution pH, stir under room temperature, allow in the solution chloroplatinic acid reach on carrier saturation absorption and etc.；Additional inorganic reducing agent need not be added in process of the present invention need not also add macromolecule stabilizer, and the content of precious metals pt is low in catalyst, catalyst preparation process is simple, and catalyst is easy to carry out and implement without high-temperature roasting and hydrogen reducing；Catalyst activity is high, stability is good.
Description
Technical field
A kind of preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation of the disclosure of the invention, belongs to low
Concentration volatile organism benzene is catalyzed completely burned processing technology field.
Background technology
Benzene is a kind of typical VOCs (volatile organism), and the chemical constitution of benzene is sufficiently stable, in natural environmental condition
Under it is not degradable, to soil, water body and air can result in persistently and seriously pollute, the harm of animals and plants and the mankind are not allowed
Ignore.If humans and animals Long Term Contact benzene can cause great damage to blood, causes slow poisoning, even result in death.
The discharge of wastewater containing benzene or exhaust gas is frequently encountered in industrial production and daily life, in order to avoid these harmful substances are largely arranged
Environment be rivals in a contest with ecological destruction, National Environmental Protection Agency has formulated relevant discharge standard (GB16297-1996《Atmosphere pollution
Comprehensive discharge standard》).
Processing for waste gas containing benzene, there are many methods at present, such as condensation method, absorption method, biotransformation method, heating power combustion
Burning method and Production by Catalytic Combustion Process etc., wherein catalytic oxidation are acknowledged as one of most effective means, and ([1] Li Weibin, Gong Hao, is urged
Change the latest developments [J] of burning removal VOCs pollutants, Acta PhySico-Chimica Sinica, 2010,26 (4):885-894.).Catalysis burning
Method is lower than heating power combustion method reaction temperature, usually within 400 DEG C, therefore the secondary pollution that not will produce nitrogen oxides etc..
Crucial technology is the preparation method of high activity and high stability catalyst in Production by Catalytic Combustion Process application process.Usually
It uses Pt as active component, but is differed greatly with the catalyst performance obtained by different carriers or different preparation methods.
For example, using tin oxide as carrier loaded Pt, for Pt/SnO2, to the catalytic activity of benzene oxidatoin, when benzene conversion ratio is up to 90%
Temperature is 320 DEG C, adds suitable CeO2This temperature value is reduced to 256 DEG C afterwards.(such as [2] kingly way, stannic oxide are carrier
Rare earth oxide is to the catalytic activity rare earths of benzene complete oxidation, and 1989, (04):32-35)Pt/Al2O3It is that preferable benzene purification is urged
Agent, when Pt contents are 0.01%, range of reaction temperature is 360-400 DEG C of ([3] Jin Yun etc., in Pt/Al2O3Benzene on catalyst
Dynamic (dynamical) influence [J] the Chemical Journal of Chinese Universities of minus 0.9 grade of interior diffusion couple, 1991 (01):84-88.)
([4] Kim H S, Kim T W, Koh H L, Lee S H, Min B R, the Complete benzene such as Kim
oxidation over Pt-Pd bimetal catalyst supported onγ-alumina:influence of Pt-
Pd ratio on the catalytic activity[J],Applied Catalysis A:General,2005,280:
Pt-Pd two-component metals 125-131.) are supported on γ-Al2O3On, it is anti-with the catalyst of 0.3wt.%Pt 2wt.%Pd contents
It answers active highest, reaction temperature that can keep benzene complete oxidation, catalyst stability test 32 hours when being 250 DEG C, transports
Row about reduced by 10% to 50 hours catalyst activities, catalytic activity and stability the urging compared with single-activity component of bimetallic component
Agent is good.
([5] Yang P, Li J, Cheng Z, Zuo S, Promoting effects of Ce the and Pt such as Yang Peng
addition on the destructive performances of V2O5/gamma-Al2O3for catalytic
combustion of benzene[J],Applied Catalysis a-General,2017,542:38-46.) report recently
The best catalyst 0.3%Pt/10%Ce-10%V/ γ-Al of performance that they are developed2O3It is 1000ppm in benzene concentration,
Air speed is 20000h-1Under the conditions of, for the T of the treating technology reaction of benzene90%Temperature is 235 DEG C.Catalyst preparation process
Middle carrier is mainly using γ-Al2O3, recycle hydrazine hydrate reduction method to obtain reduction-state by three dipping process respectively
Active component platinum.The shortcomings that its catalyst preparation process is：Step is more, will produce containing nitrogen compound in waste water after reduction.
Current already clear restoring method being affected for Pt particle surface properties, Liu Zhimin et al. ([6] Liu Zhi
It is quick, Li Xiaohong, Chen Zhijian, Ying Pinliang, Feng Zhaochi, Li Can, Pt/Al2O3Shadow of the catalyst reduction method to Pt particle surface properties
Ring [J] chemistry of fuel journals, 2009 (02):205-211.) compare in detail with hydrogen reduction method and sodium formate solution reduction method
The obtained difference on catalyst structure and performance.
Therefore a key technology of the excellent supported Pt catalysts of processability is exactly the restoring method of catalyst.With
The ethylene glycol with stabilization, easily removed is that the reduction method of solvent is to have developed a kind of method in recent years, easily controllable metal
Grain size and dispersion.The NaBH stablized such as Wu Feng et al. spent glycols4Reduction method for preparing nanometer Pt/C catalyst ([7] Wu Feng etc., work(
Energy material, 2009,40 (8) 1381), Sun Xibo et al. is used to prepare Pt/CeO2Catalyst ([8] Sun Xibo, Peng Ruosi, Li Shu
Monarch, beam Xiao Ming, Chen Limin pay fame and gain, and Wu Junliang, Ye Daiqi, Pt particle sizes are to Pt/CeO2Catalysis oxidation toluene performance influences
[J], ACTA Scientiae Circumstantiae, 2016:1-13).The former reduction process also needs that NaBH is added4As reducing agent, Pt that the latter obtains
Particle colloidal sols need to be used as stabilizer, catalyst application with PVP (polyvinylpyrrolidone, Polyvinyl Pyrrolidone)
It also needs to be removed remaining stabilizer with roasting method in the process, then be obtained again with hydrogen reducing.
Invention content
The present invention proposes a kind of Pt/Al for preparing and having high reaction activity and stability to the complete oxidation of benzene2O3And Pt/
CeZrOx catalyst methods.It is first adsorbed onto on carrier by the presoma chloroplatinic acid of Pt, then heating is gone back in ethylene glycol solution
Original adjusts catalyst surface performance by adjusting the pH of solution, and then regulates and controls catalyst reaction activity.
The purpose of the present invention is：Using new preparation method, precious metals pt loaded catalyst is prepared, can be realized in height
Waste gas containing benzene is decomposed in temperature less than the complete catalysts oxidation under 200 degrees celsius under space velocities.
The present invention adopts the following technical scheme that realize
A kind of preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation, is first added and carries in the solution
Body carries out heating reduction again after fully adsorbing chloroplatinic acid, and specific method is：
1) carrier, is quantitatively weighed, immerses in ethylene glycol, chloroplatinic acid aqueous solution is then added, adds NaOH aqueous solution tune
The pH of whole solution, it stirs under room temperature, chloroplatinic acid is allowed to reach saturation absorption on carrier in the solution；
2), above-mentioned solution under nitrogen protection and isothermal condition is heated to reduction, be cooled to room temperature after reduction,
To be separated by solid-liquid separation with the method for centrifugation, and be washed with deionized, obtained powder is vacuum dried, is pressed on tablet press machine
Piece, the particle of screening collection 40-120 mesh, evaluates it in benzene complete oxidation on atmospheric fixed bed catalyst reaction device after grinding
Activity in reaction.
As a further improvement, the weight content 0.1~1% of Pt of the present invention, the carrier is aluminium oxide
Or Ce-Zr solid solution.
As a further improvement, mass ratio ZrO of the present invention2/CeO2=2.
As a further improvement, it is neutral or alkalinity that alumina support of the present invention, which is surface,.
As a further improvement, pH=7~12 of the present invention.
As a further improvement, reaction temperature when benzene conversion ratio of the present invention reaches 99% is 145~195 degrees Celsius,
Catalytic reaction condition is：Catalyst particle size is 40-120 mesh, and a concentration of 1200-7800ppm of benzene, air is oxidant,
Reaction velocity is 6000-42000h-1。
It is characteristic of the invention that：The present invention proposes that a kind of prepare has high reaction activity and stability to the complete oxidation of benzene
Pt/Al2O3With Pt/CeZrOx catalyst methods, need not add additional inorganic reducing agent in the process need not also add height
Stabilizer molecule, the content of precious metals pt is low in catalyst, catalyst preparation process is simple, and catalyst is without high-temperature roasting and hydrogen
Gas restores, and is easy to carry out and implement；Catalyst activity is high, stability is good.Prepared Pt/Al2O3With Pt/CeZrOx catalyst energy
Realize that complete catalysts oxidation under the conditions of high-speed for waste gas containing benzene under 145~195 degrees celsius of temperature decomposes.
Description of the drawings
Fig. 1 is 0.5%Pt/Al2O3(N) catalyst is for benzene complete oxidation long-play result schematic diagram；
Fig. 2 .0.5%Pt/Al2O3(B11) catalyst is for benzene complete oxidation long-play result schematic diagram.
Specific implementation mode
Technical scheme of the present invention is further described below by specific embodiment：
Embodiment 1
Weigh the ground Al of 2.0g2O3Surface is in alkalinity (pH=8.6, La2O3(4.1%)), it is added to 50mL ethylene glycol
In solution, magnetic agitation pipettes 2mL H2PtCl4(1gPt/100mL), theoretical negative carrying capacity are 1.0wt%.3h is stirred at room temperature.Body
Be pH value be 7.It is heated to 160 DEG C of reflux 8h in the case of nitrogen protection, is cooled to room temperature.Reaction was completed that bottom portion has is yellowish-brown for reaction
Color precipitates, and reaction solution is yellowish-brown suspension.Water washing is added to centrifuge four times, no Cl-In the solution, ethyl alcohol washs 1 time, is put into
100 DEG C of oven drying 8h, obtain grey powder.Again by powder tabletting, crushing, screening, certain granules degree (such as 40-60 is collected
Mesh, 60-80 mesh or 80-120 mesh) Sample storage is spare.Catalyst is denoted as Pt/Al2O3(B7)。
Embodiment 2~4
Other conditions are with embodiment 1, except that H is added2PtCl4NaOH solution is added after solution, when being stirred at room temperature will
The pH value of solution adjusts separately to the catalyst obtained by 9,11,12 and is denoted as Pt/Al respectively2O3(B9)、Pt/Al2O3(B11)、
Pt/Al2O3(B12)。
Embodiment 5~7
Other conditions are with embodiment 3, except that the content of Pt is respectively 0.1%, 0.3% and 0.5%, it is obtained
Catalyst is denoted as 0.1%Pt/Al respectively2O3(B11), 0.3%Pt/Al2O3(B11), 0.5%Pt/Al2O3(B11)。
Embodiment 8
Other conditions are with embodiment 3, except that using CeO2-ZrO2 solid solution CeZrOx (ZrO2/CeO2=2 (matter
Measure ratio)) it is used as carrier, obtained catalyst to be denoted as 1%Pt/CeZrOx.
Embodiment 9~10
Other conditions are with embodiment 8, except that the content of Pt is respectively 0.5% and 0.25%, obtained catalysis
Agent is denoted as 0.5%Pt/CeZrOx and 0.25%Pt/CeZrOx respectively.
Embodiment 11
Other conditions are with embodiment 3, except that being in neutrality the chromatography Al of (pH=7.0 ± 0.5) using surface2O3,
The content of Pt is 0.5%, and obtained catalyst is denoted as 0.5%Pt/Al2O3(N)。
Embodiment 12~15
Catalyst (40-60 mesh) 0.14mL prepared by Example 1~4 respectively, is fitted into fixed bed reactors, is used for
The complete oxidation of benzene, reaction condition are：Benzene concentration is 2800ppm, air speed 22000h-1.Gas chromatographic detection analyzes tail
The content of benzene in gas determines reaction conversion ratio by the peak area of benzene before and after reaction, tests and react conversion under condition of different temperatures
Rate.Several characteristic temperatures of benzene oxidatoin are listed in Table 1 below.
Catalysis of the alumina load Pt catalyst for the complete oxidation of benzene under different conditions of 1. solution alkaline of table
Activity
| Example | 12 | 13 | 14 | 15 |
| Catalyst | Pt/Al2O3(B7) | Pt/Al2O3(B9) | Pt/Al2O3(B11) | Pt/Al2O3(B12) |
| T99/℃ | 185 | 155 | 145 | 160 |
| T50/℃ | 174 | 152 | 142 | 157 |
Embodiment 16~18
Catalyst (40-60 mesh) 0.14mL prepared by Example 5~7 respectively, is fitted into fixed bed reactors, is used for
The complete oxidation of benzene, reaction condition are listed in Table 2 below several characteristic temperatures of benzene oxidatoin with example 12.
Catalytic activity of the catalyst of 2. alumina load difference Pt contents of table for the complete oxidation of benzene
| Example | 16 | 17 | 18 |
| Pt contents/% | 0.1 | 0.3 | 0.5 |
| T99/℃ | 195 | 170 | 160 |
| T50/℃ | 192 | 165 | 157 |
| T10/℃ | 190 | 161 | 155 |
Embodiment 19~21
Using 1% made, 0.5% and 0.25%Pt/CeZrOx of embodiment 8~10 (granular size 40-60 mesh)
0.2mL is fitted into as catalyst in fixed bed reactors, is used for the complete oxidation of benzene.Reaction condition is：It is a concentration of
1600ppm benzene, air mass flow 100mL/min, air speed 30000h-1.They distinguish several characteristic temperatures of benzene oxidatoin
It is listed in Table 3 below.Catalytic activity of the Pt/CeZrOx catalyst of 3 difference Pt load capacity of table for the complete oxidation of benzene
| Example | 19 | 20 | 21 |
| Catalyst | 1%Pt/CeZrOx | 0.5%Pt/CeZrOx | 0.25%Pt/CeZrOx |
| T99/℃ | 154 | 161 | 186 |
| T50/℃ | 141 | 144 | 171 |
| T10/℃ | 114 | 130 | 155 |
Embodiment 22~24
Using the 0.5%Pt/Al that embodiment 11 is made2O3(N) it is catalyst, other conditions are different with embodiment 19
It is that concentration in reaction process into catalyst bed benzene adjusts separately as 1200,1500 and 7800ppm, they are for benzene oxidatoin
Several characteristic temperatures be listed in Table 4 below respectively.
4 0.5%Pt/Al of table2O3(N) catalytic activity of the catalyst for the benzene complete oxidation of various concentration
| Example | 22 | 23 | 24 |
| The concentration of benzene | 1200 | 1500 | 7800 |
| T/p99p/℃ | 175 | 160 | 178 |
| T50/℃ | 154 | 148 | 174 |
| T10/℃ | 140 | 100 | 170 |
Embodiment 25~27
Other conditions are with embodiment 23, except that entering the dense of catalyst bed gas space velocity and benzene in reaction process
The difference of degree, conversion temperature when they reach 99% for the conversion ratio of benzene oxidatoin are listed in Table 5 below respectively.
5 0.5%Pt/Al of table2O3(N) catalysis of the catalyst for benzene complete oxidation under various concentration and space velocities
Activity
| Example | 25 | 26 | 27 |
| Concentration/ppm of benzene | 3900 | 3100 | 2200 |
| Air speed/h-1 | 6000 | 15000 | 42000 |
| T99/℃ | 175 | 180 | 175 |
Embodiment 28
Other conditions are with embodiment 23, except that used catalyst granular size is 80-120 mesh, temperature of reactor
Be 170 DEG C, for benzene completely oxidizing catalyst long-play stability result as shown in Figure 1.
Embodiment 29
Other conditions urge the complete oxidation of benzene except that it is 165 DEG C that temperature of reactor is constant with embodiment 18
100 hours continuous operation results of agent are as shown in Figure 2.
The foregoing is merely better embodiments of the present invention, but scope of protection of the present invention is not limited thereto, any ripe
Know those skilled in the art in the technical scope disclosed by the present invention, the technique according to the invention design be subject to equivalent replacement or
The technical solution for changing gained, should all be covered by protection scope of the present invention.
Claims (6)
1. a kind of preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation, it is characterized in that first adding in the solution
Enter carrier, carries out heating reduction again after fully adsorbing chloroplatinic acid, specific method is：
1) carrier, is quantitatively weighed, immerses in ethylene glycol, chloroplatinic acid aqueous solution is then added, it is molten to add the adjustment of NaOH aqueous solutions
The pH of liquid, it stirs under room temperature, chloroplatinic acid is allowed to reach saturation absorption on carrier in the solution；
2), above-mentioned solution under nitrogen protection and isothermal condition is heated to reduction, be cooled to room temperature after reduction, with from
The method of the heart to be separated by solid-liquid separation, and is washed with deionized, and obtained powder is vacuum dried, the tabletting on tablet press machine,
The particle of 40-120 mesh is collected in screening after grinding, it is evaluated on atmospheric fixed bed catalyst reaction device in benzene complete oxidation
In activity.
2. the preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation according to claim 1, special
Sign is the weight content 0.1~1% of the Pt, and the carrier is aluminium oxide or Ce-Zr solid solution.
3. the preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation according to claim 2, special
Sign is mass ratio ZrO2/CeO2=2.
4. the preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation according to claim 2, special
It is surface is neutral or alkalinity that sign, which is the alumina support,.
5. the preparation method of the low temperature high activity catalyst of catalysis benzene complete oxidation according to claim 1, special
Sign is pH=7~12.
6. the system of the low temperature high activity catalyst of the catalysis benzene complete oxidation according to claims 1 or 2 or 3 or 4 or 5
Preparation Method, characterized in that reaction temperature when benzene conversion ratio reaches 99% is 145~195 degrees Celsius, and catalytic reaction condition is：
Catalyst particle size is 40-120 mesh, and a concentration of 1200-7800ppm of benzene, air is oxidant, reaction velocity 6000-
42000h-1。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111545199A (en) * | 2020-05-26 | 2020-08-18 | 北京工业大学 | Supported platinum-tin bimetallic catalyst for efficient oxidation and purification of paraxylene |
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| CN105536777A (en) * | 2015-12-17 | 2016-05-04 | 杭州电子科技大学 | Catalytic combustion active ingredient highly-dispersed catalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105536777A (en) * | 2015-12-17 | 2016-05-04 | 杭州电子科技大学 | Catalytic combustion active ingredient highly-dispersed catalyst and preparation method thereof |
| CN105797720A (en) * | 2016-05-16 | 2016-07-27 | 北京化工大学 | Superfine supported noble metal catalyst prepared through in-situ reduction deposition method and preparing method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111545199A (en) * | 2020-05-26 | 2020-08-18 | 北京工业大学 | Supported platinum-tin bimetallic catalyst for efficient oxidation and purification of paraxylene |
| CN111545199B (en) * | 2020-05-26 | 2022-11-18 | 北京工业大学 | Supported platinum-tin bimetallic catalyst for efficient oxidation and purification of p-xylene |
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