CN106732577B - A kind of itrogenous organic substance catalyst for catalytic combustion and its preparation method and application - Google Patents
A kind of itrogenous organic substance catalyst for catalytic combustion and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of itrogenous organic substance catalyst for catalytic combustion and its preparation method and application, with Al2O3For carrier, active component Ir, one or more of adjuvant component Sm, In, Sn oxide.With Al2O3Carrier meter, active component Ir load capacity are 0.1wt%-1wt%, and auxiliary agent load capacity is 1wt%-10wt%.Preparation method includes: (1) first by carrier Al2O3It is impregnated in the precursor solution of auxiliary agent, the complex carrier Al of load auxiliary agent is obtained after drying and roasting2O3, the auxiliary agent is one or more of Sm, In, Sn oxide；(2) the complex carrier Al for obtaining step (1)2O3It is impregnated in the salting liquid containing active component, catalyst is made through dry and roasting, the active component is Ir.The method of the present invention preparation process is simple, and the catalyst of preparation has good catalytic combustion activity, selectivity and stability to nitrogenous organic exhaust gas, especially suitable for handling the organic exhaust gas containing propylene and acrylonitrile.
Description
Technical field
The present invention relates to a kind of catalyst for catalytic combustion and its preparation method and application more particularly to a kind of itrogenous organic substances
Catalyst for catalytic combustion and its preparation method and application.
Background technique
Nitrogenous volatile organic matter is widely present in the production or use process of amine, amide, nitrile etc., as acrylonitrile synthesizes
The ammoxidation of propylene technique that technique mostly uses greatly BP company to develop, mainly contain in technology waste gas propylene, propane, carbon monoxide and
Acrylonitrile.Catalysis burning is to handle the effective means of volatile organic compounds, the final production of the nitrogen in itrogenous organic substance
It is possible that there are two types of objects, and one is N2, one is NOx.Consider from environmental angle, Ying Jinliang avoids generating NOx.
CN1034867 discloses a kind of nitrogenous catalyst for purifying organic waste gas, which is to carry with natural mordenite zeolite
Body, active component are composed with iron, copper, manganese, cerium, the two or more of chromated oxide, the weight ratio of active component and carrier
For 1%-10%.The catalyst to the itrogenous organic substances such as n-butylamine, dinethylformamide, aniline all have good catalytic activity and
Stronger control NOx ability.But the catalyst need to be used cooperatively when implementing with Pt-Pd noble metal catalyst, in air speed 5000-
15000h-1, 280-400 DEG C of temperature, concentration 2000-5000mg/m3When, conversion ratio is greater than 98%, and control NOx efficiency is greater than 90%.But
It is that the catalyst is not directed to stability problem.
CN103212419 discloses a kind of for catalyst and preparation method and application containing acrylonitrile waste gas, catalyst
Using Ca-Ti ore type crystalline form (ABO3) metal oxide as catalyst, wherein A is rare earth metal, and B is transition metal, is passed through
A, the screening of B metal ions with combine, using benzyl alcohol it is legal synthesize be suitable for the catalysis that removes containing acrylonitrile waste gas
Agent, and by control catalytic combustion process condition, make the product that acrylonitrile conversion is nontoxic, i.e. N2, H2O and CO2, especially
It is that can prevent the generation of other nitrogen oxides in hot stage.Reaction temperature needed for the catalyst is high, and N2Poor selectivity.
LaCu0.2Fe0.8O3It is wherein active highest catalyst, when reacting 300 DEG C, the yield of nitrogen is lower than 80%.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of itrogenous organic substance catalyst for catalytic combustion and its preparation sides
Method and application.The method of the present invention preparation process is simple, and the catalyst of preparation burns to nitrogenous organic exhaust gas with good catalysis
Activity, selectivity and stability, particularly suitable for handling the organic exhaust gas containing propylene and acrylonitrile.
Itrogenous organic substance catalyst for catalytic combustion provided by the invention, with Al2O3For carrier, active component Ir, auxiliary agent group
It is divided into one or more of Sm, In, Sn oxide, preferably Sm.With Al2O3Carrier meter, active component Ir load capacity are
0.1wt%-1wt%, adjuvant component load capacity are 1wt%-10wt%.It further, further include micro- in catalyst provided by the invention
The load capacity of Pt the and/or Pd active component of amount, Pt and/or Pd are 0.01wt%-0.1wt%.
The specific surface area of catalyst of the present invention is greater than 150m2/ g, Kong Rong 0.3-0.6ml/g, acid amount is with NH3The side-TPD
Method is calculated as 0.6-0.8mmol/g.Al in catalyst of the present invention2O3For commercially available or homemade γ-Al2O3。
The preparation method of itrogenous organic substance catalyst for catalytic combustion of the present invention, comprising the following steps:
(1) first by carrier Al2O3It is impregnated in the precursor solution of auxiliary agent, load auxiliary agent is obtained after drying and roasting
Complex carrier Al2O3, the auxiliary agent is one or more of Sm, In, Sn oxide；
(2) the complex carrier Al for obtaining step (1)2O3It is impregnated in the salting liquid containing active component, through dry and roasting
It is fired into catalyst, the active component is Ir.
In the present invention, Al described in step (1)2O3It is commercially available or self-control, it is preferable to use γ-Al2O3。
In the present invention, the precursor solution of step (1) described auxiliary agent is containing in samaric nitrate, indium nitrate, tin tetrachloride
One or more of aqueous solutions, preferably samaric nitrate.Wherein, the mass concentration of samarium nitrate solution is 5-50g/L, the quality of indium nitrate
Concentration is 5.5-55g/L, and the mass concentration of tin tetrachloride is 4-40g/L, dip time 1-10min.In catalyst, with Al2O3It carries
Body meter, adjuvant component load capacity are 1wt%-10wt%.
In the present invention, the salting liquid of active component is the nitrate or chlorination salting liquid of Ir in step (2).Active component
In salting liquid, in terms of metal, Ir concentration is 0.2-2g/L.In catalyst, with Al2O3Carrier meter, the load capacity of Ir are 0.1wt%-
1wt%.It further, further include Pt and/or Pd in the salting liquid of active component, in terms of metal, Pt concentration is 0-0.2g/L, Pd
Concentration is 0-0.2g/L.In catalyst, with Al2O3The load capacity of carrier meter, Pt and/or Pd are 0.01wt%-0.1wt%.Dipping
Before, the pH for needing to control active component salt solution is 3-5.
In the present invention, a certain amount of ionic liquid can be added in the salting liquid of active component in step (2), described
Cation is [emim] in ionic liquid+Or [bmim]+One of, anion BF4 -, PF6 -, F-, OH-One of；Ion
The concentration of liquid is 1-10g/L.
In the present invention, drying temperature described in step (1) and step (2) is 100-120 DEG C, and drying time is that 6-12 is small
When；The maturing temperature is 400-600 DEG C, and calcining time is 2-5 hours.
The application of itrogenous organic substance catalyst for catalytic combustion prepared by the present invention mainly contains propylene and third in exhaust gas to be processed
Alkene nitrile, concentration 1000-5000mg/m3, 200-400 DEG C of reaction temperature, air speed 5000-20000h-1.After processing, propylene and
The conversion ratio of acrylonitrile is all larger than 95%, N2Yield be greater than 90%.
Compared with prior art, the present invention has the advantage that
(1) using adjuvant components such as Sm, In, Sn to γ-Al2O3It is modified, makes it have suitable cellular structure and acid
Intensity is conducive to the diffusion and absorption of itrogenous organic substance molecule on a catalyst, improves removal of the catalyst to itrogenous organic substance
Effect.
(2) Ir and adjuvant component Sm, In, Sn act synergistically, and not only there is good catalysis burning to live itrogenous organic substance
Property and selectivity, especially help avoid the loss of active component, improve the stability of catalyst.
(3) Ir and Pt and/or Pd active component act synergistically, and increase catalyst significantly to the removal effect of itrogenous organic substance
Add, avoids generating NOx, N2Yield dramatically increase.
(4) in catalyst preparation process, ionic liquid is added, contributes to form suitable cellular structure, it not only can be with
The load capacity and dispersion degree of active component are improved, and helps avoid the loss of active component, improves the stabilization of catalyst
Property.
Specific embodiment
Illustrative explanation is carried out in more detail to the present invention below by embodiment, but the embodiment should not manage
Solution is limitation of the scope of the invention.In the present invention, wt% is mass fraction.
Embodiment 1
First by γ-Al2O3It is impregnated 5 minutes in the samaric nitrate aqueous solution of 5g/L, it is 12 hours, 500 DEG C dry through 100 DEG C
Roasting obtained Sm after 5 hours2O3-Al2O3Complex carrier.By Sm2O3-Al2O3It is dense that complex carrier is impregnated in Ir concentration 0.2g/L, Pt
It spends in the chloro-iridic acid, chloroplatinic acid and chlorine palladium aqueous acid of 0.1g/L, Pd concentration 0.1g/L, the pH of solution is 4, through 120 DEG C dry 6
Hour, 600 DEG C roasting 3 hours after obtain load Ir-Pt-Pd catalyst.
In gained catalyst, Sm2O3Load capacity is 1wt%, and Ir load capacity is 0.1wt%, and Pt load capacity is 0.05wt%, and Pd is negative
Carrying capacity is 0.05wt%.The specific surface area 190m of gained catalyst2/ g, Kong Rong 0.5ml/g, acid amount is with NH3- TPD method is calculated as
0.6mmol/g。
Embodiment 2
First by γ-Al2O3It is impregnated 5 minutes in the indium nitrate aqueous solution of 5.5g/L, it is 12 hours dry through 100 DEG C, 500
DEG C roasting 5 hours after obtain In2O3-Al2O3Complex carrier.By In2O3-Al2O3Complex carrier is impregnated in Ir concentration 0.2g/L, Pt
In the chloro-iridic acid of concentration 0.1g/L, Pd concentration 0.1g/L, chloroplatinic acid and chlorine palladium aqueous acid, the pH of solution is 4, dry through 120 DEG C
Dry 6 hours, 600 DEG C roasting 3 hours after obtain load Ir-Pt-Pd catalyst.
In gained catalyst, In2O3Load capacity is 1wt%, and Ir load capacity is 0.1wt%, and Pt load capacity is 0.05wt%, and Pd is negative
Carrying capacity is 0.05wt%.The specific surface area 188m of gained catalyst2/ g, Kong Rong 0.55ml/g, acid amount is with NH3- TPD method is calculated as
0.65mmol/g。
Embodiment 3
First by γ-Al2O3It is impregnated 5 minutes in the tin tetrachloride aqueous solution of 4g/L, it is 12 hours dry through 100 DEG C, 500
DEG C roasting 5 hours after obtain SnO2-Al2O3Complex carrier.By SnO2-Al2O3It is dense that complex carrier is impregnated in Ir concentration 0.2g/L, Pt
It spends in the chloro-iridic acid, chloroplatinic acid and chlorine palladium aqueous acid of 0.1g/L, Pd concentration 0.1g/L, the pH of solution is 4, through 120 DEG C dry 6
Hour, 600 DEG C roasting 3 hours after obtain load Ir-Pt-Pd catalyst.
In gained catalyst, SnO2Load capacity is 1wt%, and Ir load capacity is 0.1wt%, and Pt load capacity is 0.05wt%, and Pd is negative
Carrying capacity is 0.05wt%.The specific surface area 191m of gained catalyst2/ g, Kong Rong 0.6ml/g, acid amount is with NH3- TPD method is calculated as
0.7mmol/g。
Embodiment 4
First by γ-Al2O3After being impregnated 3 minutes in the samaric nitrate of 26g/L and the indium nitrate aqueous solution of 30g/L, through 100
DEG C dry 12 hours, 500 DEG C obtained Sm after roasting 4 hours2O3-In2O3-Al2O3Complex carrier.By Sm2O3-In2O3-Al2O3It is multiple
Carrier impregnation is closed in the chloro-iridic acid and chloroplatinic acid aqueous solution of Ir concentration 1g/L, Pt concentration 0.1g/L, the pH of solution is 3, through 110
DEG C dry 12 hours, 500 DEG C of roastings obtained the catalyst of load Ir-Pt for 2 hours.
In gained catalyst, Sm2O3Load capacity is 5wt%, In2O3Load capacity is 5wt%, and Ir load capacity is 0.5wt%, and Pt is negative
Carrying capacity is 0.05wt%.The specific surface area 167m of gained catalyst2/ g, Kong Rong 0.4ml/g, acid amount is with NH3- TPD method is calculated as
0.7mmol/g。
Embodiment 5
First by γ-Al2O3After being impregnated 3 minutes in the samaric nitrate of 26g/L and the tin tetrachloride aqueous solution of 6g/L, through 120
DEG C dry 6 hours, 400 DEG C obtained Sm after roasting 5 hours2O3-SnO2-Al2O3Complex carrier.By Sm2O3-SnO2-Al2O3It is compound
Carrier impregnation is in the chloro-iridic acid and chlorine palladium aqueous acid of Ir concentration 0.4g/L, Pd concentration 0.02g/L, and the pH of solution is 5, warp
120 DEG C drying 6 hours, 400 DEG C of roastings obtain the catalyst of load Ir-Pd for 5 hours.
In gained catalyst, Sm2O3Load capacity is 5wt%, SnO2Load capacity is 1.5wt%, and Ir load capacity is 0.2wt%, Pd
Load capacity is 0.01wt%.The specific surface area 210m of gained catalyst2/ g, Kong Rong 0.6ml/g, acid amount is with NH3- TPD method is calculated as
0.8mmol/g。
Embodiment 6
First by γ-Al2O3It is impregnated in the tin tetrachloride aqueous solution of 20g/L samaric nitrate, the indium nitrate of 5.5g/L and 6g/L
10 minutes, 8 hours dry through 110 DEG C, 600 DEG C obtain Sm after roasting 2 hours2O3-In2O3- SnO2-Al2O3Complex carrier.It will
Sm2O3-In2O3- SnO2-Al2O3Complex carrier is impregnated in the chlorine of Ir concentration 0.2g/L, Pt concentration 0.1g/L, Pd concentration 0.1g/L
In iridium acid, chloroplatinic acid and chlorine palladium aqueous acid, the pH of solution is 4,6 hours dry through 100 DEG C, and 600 DEG C obtain after roasting 3 hours
Load the catalyst of Ir-Pt-Pd.
In gained catalyst, Sm2O3Load capacity is 4wt%, In2O3Load capacity is 1wt%, SnO2Load capacity is 1.5wt%, Ir
Load capacity is 0.1wt%, and Pt load capacity is 0.05wt%, and Pd load capacity is 0.05wt%.The specific surface area 150m of gained catalyst2/
G, Kong Rong 0.3ml/g, acid amount is with NH3- TPD method is calculated as 0.62mmol/g.
Embodiment 7
First by γ-Al2O3It is impregnated 5 minutes in the samaric nitrate aqueous solution of 5g/L, it is 12 hours, 500 DEG C dry through 100 DEG C
Roasting obtained Sm after 5 hours2O3-Al2O3Complex carrier.By Sm2O3-Al2O3Complex carrier is impregnated in Ir concentration 2g/L chloro-iridic acid water
In solution, the pH of solution is 4,6 hours dry through 120 DEG C, and 600 DEG C obtain the catalyst of load Ir after roasting 3 hours.
In gained catalyst, Sm2O3Load capacity is 1wt%, and Ir load capacity is 1wt%.The specific surface area of gained catalyst
185m2/ g, Kong Rong 0.5ml/g, acid amount is with NH3- TPD method is calculated as 0.57mmol/g.
Embodiment 8
Preparation process and operating condition are the same as embodiment 1.The difference is that: ion is added in the salting liquid of active component
Liquid [emim] BF4, concentration 1g/L.In gained catalyst, Sm2O3Load capacity is 1wt%, and Ir load capacity is 0.1wt%, Pt load
Amount is 0.05wt%, and Pd load capacity is 0.05wt%.The specific surface area 201m of gained catalyst2/ g, Kong Rong 0.58ml/g, acid amount with
NH3- TPD method is calculated as 0.61mmol/g.
Embodiment 9
Preparation process and operating condition are the same as embodiment 4.The difference is that: ion is added in the salting liquid of active component
Liquid [bmim] BF4, concentration 3g/L.In gained catalyst, Sm2O3Load capacity is 5wt%, In2O3Load capacity is 5wt%, Ir load
Amount is 0.5wt%, and Pt load capacity is 0.05wt%.The specific surface area 175m of gained catalyst2/ g, Kong Rong 0.45ml/g, acid amount with
NH3- TPD method is calculated as 0.72mmol/g.
Embodiment 10
Preparation process and operating condition are the same as embodiment 7.The difference is that: ion is added in the salting liquid of active component
Liquid [emim] PF6, concentration 5g/L.In gained catalyst, Sm2O3Load capacity is 1wt%, and Ir load capacity is 1wt%.Gained catalysis
The specific surface area 192m of agent2/ g, Kong Rong 0.54ml/g, acid amount is with NH3- TPD method is calculated as 0.6mmol/g.
Comparative example 1
Preparation process and operating condition are the same as embodiment 4.The difference is that: the auxiliary agent of addition is La and Ce.Gained catalysis
In agent, La2O3Load capacity is 5wt%, Ce2O3Load capacity is 5wt%, and Ir load capacity is 0.5wt%, and Pt load capacity is 0.05wt%.Institute
Obtain the specific surface area 172m of catalyst2/ g, Kong Rong 0.41ml/g, acid amount is with NH3- TPD method is calculated as 0.64mmol/g.
Comparative example 2
Preparation process and operating condition are the same as embodiment 6.The difference is that: it is added without active component Ir.Gained catalyst
In, Sm2O3Load capacity is 4wt%, In2O3Load capacity is 1wt%, SnO2Load capacity is 1.5wt%, and Pt load capacity is 0.05wt%, Pd
Load capacity is 0.05wt%.The specific surface area 153m of gained catalyst2/ g, Kong Rong 0.31ml/g, acid amount is with NH3- TPD method is calculated as
0.63mmol/g。
Comparative example 3
Fe-Cu-Mn catalyst is prepared according to 1 the method for CN1034867 embodiment.
Comparative example 4
LaCu is prepared according to 8 the method for embodiment in CN1032124190.2Mn0.8O3Catalyst.
Each catalyst is evaluated on laboratory room small-sized experimental provision, the actual conditions of evaluation are as follows: density of propylene
2000 mg/m3, 1000 mg/m of acrylonitrile concentration3；300 DEG C of reaction temperature；Air speed is 20000h-1, each organic matter removal effect
It is shown in Table 1.
The service performance of each embodiment of table 1 and the catalyst of comparative example preparation
Seen from table 1, catalyst of the present invention is when for processing containing propylene and acrylonitrile waste gas, catalyst
It is active more preferable, and since the catalyst can be to avoid the loss of active component Ir, stability is more preferable.
Claims (8)
1. a kind of preparation method of itrogenous organic substance catalyst for catalytic combustion, it is characterised in that the following steps are included:
(1) first by carrier Al2O3It is impregnated in the precursor solution of auxiliary agent, answering for load auxiliary agent is obtained after drying and roasting
Close carrier Al2O3, the auxiliary agent is one or more of Sm, In, Sn oxide；
(2) the complex carrier Al for obtaining step (1)2O3It is impregnated in the salting liquid containing active component, is made through dry and roasting
At catalyst, the active component is Ir；In the salting liquid of active component, be added a certain amount of ionic liquid, it is described from
Cation is [emim] in sub- liquid+Or [bmim]+One of, anion BF4 -, PF6 -, F-, OH-One of, ionic liquid
The concentration of body is 1-10g/L；Before dipping, the pH for needing to control active component salt solution is 3-5；
In catalyst, with Al2O3Carrier meter, adjuvant component load capacity are 1wt%-10wt%, and the load capacity of Ir is 0.1wt%-1wt%.
2. preparation method according to claim 1, it is characterised in that: Al described in step (1)2O3It is commercially available or homemade
γ-Al2O3。
3. preparation method according to claim 1, it is characterised in that: the precursor solution of step (1) described auxiliary agent is to contain
There is the aqueous solution of one or more of samaric nitrate, indium nitrate, tin tetrachloride；Wherein, the mass concentration of samarium nitrate solution is 5-
50g/L, the mass concentration of indium nitrate are 5.5-55g/L, and the mass concentration of tin tetrachloride is 4-40g/L, dip time 1-
10min。
4. preparation method according to claim 1, it is characterised in that: the salting liquid of active component is Ir's in step (2)
Nitrate or chlorination salting liquid；In the salting liquid of active component, in terms of metal, Ir concentration is 0.2-2g/L.
5. preparation method according to claim 1, it is characterised in that: further include in the salting liquid of step (2) active component
Pt and/or Pd, in terms of metal, Pt concentration is 0.1-0.2g/L, and Pd concentration is 0.02-0.2g/L；In catalyst, with Al2O3Carrier
The load capacity of meter, Pt and/or Pd are 0.01wt%-0.1wt%.
6. preparation method according to claim 1, it is characterised in that: drying temperature described in step (1) and step (2)
It is 100-120 DEG C, drying time is 6-12 hours；The maturing temperature is 400-600 DEG C, and calcining time is 2-5 hours.
7. a kind of itrogenous organic substance catalyst for catalytic combustion, it is characterised in that be using system described in claim 1-6 any one
Preparation Method preparation.
8. the application of itrogenous organic substance catalyst for catalytic combustion according to claim 7, it is characterised in that: exhaust gas to be processed
In mainly contain propylene and acrylonitrile, concentration 1000-5000mg/m3, reaction temperature is 200-400 DEG C, air speed 5000-
20000h-1。
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| CN109569272B (en) * | 2017-09-28 | 2021-11-30 | 中国石油化工股份有限公司 | Cyanogen-containing waste gas treatment method |
| CN109569588B (en) * | 2017-09-28 | 2021-11-30 | 中国石油化工股份有限公司 | Catalyst for catalytic oxidation of waste gas containing cyanogen and preparation method thereof |
| CN110639500A (en) * | 2018-06-27 | 2020-01-03 | 中国石油化工股份有限公司 | Combustion catalyst for cyanogen-containing waste gas and application of combustion catalyst in cyanogen-containing waste gas treatment |
| CN109847746B (en) * | 2019-03-11 | 2021-12-07 | 浙江师范大学 | Catalyst for purifying nitrogen-containing organic matter and preparation method thereof |
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