CN103212419B - Preparation method and application of catalyst for treating acrylonitrile contained waste gas - Google Patents
Preparation method and application of catalyst for treating acrylonitrile contained waste gas Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a catalyst for treating acrylonitrile contained waste gas. The catalyst is characterized in that a metallic oxide with a perovskite crystal form (ABO3) is used as a catalyst, the catalyst suitable for removing the acrylonitrile contained waste gas is synthesized by using a benzoic alcohol synthesis method and through sieving and combining A-site and B-site metal ions, acrylonitrile is converted into nontoxic and harmless products including N2, H2O and CO2 through controlling catalytic combustion process conditions, and particularly, other nitrogen oxides such as NO2, NO and other secondary pollution gases can be prevented from being generated at a high-temperature stage. The catalyst can be applied to the treatment for the acrylonitrile contained waste gas discharged by an acrylonitrile factory and a carbon fiber factory.
Description
Technical field
The invention belongs to a kind of for containing the method for preparing catalyst of acrylonitrile waste gas process and application, relate in particular to the method for preparing catalyst of a kind of composite oxide of metal catalytic combustion with perovskite crystal formation containing acrylonitrile waste gas and the type.Can be used for acrylonitrile plant, the discharge of carbon fiber factory containing acrylonitrile waste gas process.
Background technology
Due in current synthesis of acrylonitrile technique, what have the employing of 95% is the ammoxidation of propylene technique that BP company develops.The tail gas of the waste gas of this production technology mainly absorption tower discharge, the poisonous components such as the acrylonitrile containing propylene, propane, carbon monoxide and trace, if do not added process, will certainly damage human body and environment.The volatilizable organic method of current process low concentration has absorption method, biological treatment, directly burning method and Production by Catalytic Combustion Process.And catalytic combustion is acknowledged as efficient, the most energy-conservation method.At present in HCN-containing gases, HCN catalytic combustion research more (as CN1511615A, CN101269297A, CN1462652A).Although noble metal catalyst proves effectively, limit its application due to expensive.Transition metal is adopted to be carried on mesoporous material, Al
2o
3or SiO
2deng on carrier, effectively can deviate from HCN waste gas, but have no report for the process of acrylonitrile off-gas.Although patent CN101138699A and CN101362051A all reports acrylonitrile off-gas treatment process, the catalyst adopted is noble metal catalyst.At present, the method with the composite oxide of metal catalytic combustion acrylonitrile waste gas of perovskite crystal formation is utilized to have no report.For the synthetic method of perovskite, be divided into solid-phase synthesis and wet chemistry method.Citric acid complex method is exactly a kind of conventional method preparing perovskite, and perovskite specific area is low is a great problem always perplexing its application.How to solve this difficult problem, forefathers it is also proposed a lot of way, as mechanical ball milling, and flame injection etc., but DeGrain.For this difficult problem, have employed a kind of novel non-aqueous solvent method in the present invention, prepared the perovskite of Nano grade particle, had high-specific surface area, anti-sintering, spheric granules disperses good feature.
Summary of the invention
The object of the invention is to solve the pollution problem containing acrylonitrile waste gas, propose a kind of novel method for preparing catalyst, select best catalyst, and adopt the method for catalytic combustion, can by acrylonitrile at a lower temperature directly selective catalysis combustion decomposition be carbon dioxide, nitrogen and water.It is alternative that this catalyst has higher catalytic activity, and raw material is simple, and with low cost, no coupling product, has industrial application value.
A kind of method for preparing catalyst and application for containing acrylonitrile waste gas process that the present invention proposes comprises the following steps:
(1) preparation of perovskite type metal oxide catalyst, perovskite type metal oxide can be expressed as: ABO
3, wherein A is generally alkaline-earth metal, and B is generally transition metal, can be a kind of metal also can be various metals.By the acetylacetonate of the nitrate of A position metallic element and B position metallic element, be that (wherein metal ion molar concentration rate in A, B position is A:B=1:1 or A:B for the ratio of 1:100 ~ 120 according to the mol ratio of slaine and phenmethylol
1: B
2=1:0.2:0.8) be dissolved in benzyl alcohol solution and be made into mixed solution, fully dissolve under 70 DEG C ~ 80 DEG C conditions, and be transferred to after keeping 20 minutes in static reaction still, reactor is placed in the baking oven of 200 DEG C, maintain 24 hours, rear centrifugation is taken out in room temperature cooling, obtains solid matter, and with absolute ethanol washing 3 ~ 5 times, until phenmethylol removes completely.The solid matter obtained is transferred to 100 DEG C of baking oven inner dryings 24 hours, calcines in Muffle furnace, heating rate is 2 DEG C/min, calcines 6 hours, be naturally down to room temperature, namely obtain desired perovskite type metal oxide under 450 DEG C ~ 550 DEG C conditions.
(2) by catalyst prepared by step (1), be placed in fixed bed quartz tube reactor, at ambient pressure, reaction temperature rises to 600 DEG C from 100 DEG C, and gather a secondary data every 50 DEG C, by acrylonitrile, the gaseous mixture of oxygen and nitrogen is with volume space velocity 80000h
-1~ 120000 h
-1pass in reacting furnace, through catalytic combustion, waste gas is removed.Wherein, the volume of gaseous mixture consists of acrylonitrile: oxygen=0.3:1 ~ 10, and nitrogen is as Balance Air;
In method of the present invention, selected solvent is phenmethylol, A position Metal Ion Selective Electrode lanthanum nitrate, and B is Metal Ion Selective Electrode ferric acetyl acetonade, acetylacetone copper, acetylacetone cobalt, chromium acetylacetonate, these organic salts such as manganese acetylacetonate one or more.Dissolving mixing temperature is 80 DEG C, maintains 20 minutes.The mol ratio of metal ion and phenmethylol is 1:120, and metal ion molar concentration is A:B=1:1 and A:B
1: B
2=1:0.2:0.8.
In the inventive method, selected synthetic method is the synthesis of static reaction still, and temperature conditions selects 200 DEG C, maintains 24 hours.Calcining heat is 450 ~ 550 DEG C, maintains 6 hours.
In the inventive method, selected catalyst has LaFeO
3, LaCoO
3, LaMnO
3, La
2cuO
3, LaCrO
3, LaCu
0.2co
0.8o
3, LaCu
0.2fe
0.8o
3, LaCu
0.2mn
0.8o
3and LaCu
0.2cr
0.8o
3.
In the inventive method, step (2) is applied to acrylonitrile (C
3h
3n) process of waste gas, the condition of catalytic combustion acrylonitrile waste gas is, air speed is 120000h
-1, while guarantee catalytic effect, increase treating capacity, reduce catalyst amount.Acrylonitrile and oxygen volume ratio are preferably 0.3:1.2.Optimal reaction temperature interval is 350 DEG C ~ 550 DEG C.
Feature of the present invention is:
(1) adopt phenmethylol as solvent first, under cryogenic high pressure, prepared the composite oxide of metal with perovskite crystal formation, improve its specific area (56m
2/ g), and the perovskite specific area that citric acid complex method (conventional method) is prepared is on average lower than 15m
2/ g.By the catalyst that the method is prepared, improve the selective of its catalyst.
(2) combined by the screening of B position metal ion, successfully obtain the catalyst that can be applicable to acrylonitrile off-gas and remove.The operating condition controlling reaction carries out selective catalyst combustion, and acrylonitrile conversion can be made to be harmless N
2, H
2o and CO
2and it is selective higher.
(3) in the present invention, the initiation temperature of catalyst is low, and can avoid nitrogen unit procatarxis over oxidation in high temperature section, forms another kind of pollutant NO
x, this reaction is exothermic reaction, and energy consumption is lower.
Accompanying drawing illustrates:
Fig. 1 is the LaFeO that the inventive method and conventional method are prepared
3x-ray diffractogram (XRD), the XRD that wherein (a) prepares products therefrom for phenmethylol method (method in the present invention) schemes, b () is prepared products therefrom XRD for citric acid complex method (conventional method) and is schemed, by contrasting (no.74-2203) with standard diagram, product prepared by two kinds of methods all has perovskite crystal structure, illustrates that new method also can prepare the good perovskite type metal oxide of crystal structure.
Fig. 2 is in the inventive method, the LaFeO that phenmethylol method synthesizes
3electron-microscope scanning (SEM) figure, it is coccoid that pattern is class, and Granular composite is comparatively obvious.
Fig. 3 is in the present invention, the LaFeO adopting two kinds of distinct methods to prepare in embodiment 1 and comparative example 1
3activity rating figure, acrylonitrile conversion rate and product carbon dioxide and nitrogen vary with temperature curve map.Wherein (a) represents the catalyst acquired results in embodiment 1, and (b) represents the catalyst acquired results in comparative example 1.As seen from the figure, the catalyst that new method synthesizes can significantly improve N
2productive rate.
Fig. 4 is in the inventive method, adopts LaFeO
3catalyst is under different acrylonitrile and oxygen volume ratio the most, the yield with temperature change curve of nitrogen.In figure, 1%, 1.2%, 8% what represent respectively is different oxygen concentrations, and the concentration of acrylonitrile is 0.3%.Can find out in this figure that in oxygen concentration be 1.2%, catalyst is to selective the best of nitrogen.
Fig. 5 is under oxygen concentration is 1.2% condition, when B position is Co, Cu, Cr, Mn and Fe element respectively, dissimilar perovskite type metal composite oxide catalytic burning acrylonitrile activity rating figure, wherein (a) varies with temperature curve for acrylonitrile conversion rate, and (b) is N
2yield with temperature change curve.
Fig. 6 is under oxygen concentration is 1.2% condition, B position is bimetallic and Cu:M(Co, Cr, Mn, Fe)=0.2:0.8 time, dissimilar perovskite type metal composite oxide catalytic burning acrylonitrile activity rating figure, wherein (a) varies with temperature curve for acrylonitrile conversion rate, and (b) is N
2yield with temperature change curve.
Detailed description of the invention
Embodiment 1: the phenmethylol measuring 60ml is poured in 100ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 2.209 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the ferric acetyl acetonade of 1.802 grams, after 20 minutes, is proceeded to by mixed solution in high pressure static reactor.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 450 DEG C of roastings 6 hours.Finally obtain the metal oxide LaFeO with perovskite crystal formation
3.
By the metal dust compressing tablet of preparation, and sift out 40-60 object particle, take the catalyst granules of 0.2g, be placed in miniature fixed-bed quartz reactor, then simulate acrylonitrile off-gas situation at ambient pressure and carry out active appraisal experiment.Will containing acrylonitrile (0.3 vol%), O
2and N (1.2%)
2the gaseous mixture of (as Balance Air) take air speed as 120000h
-1be incorporated in reacting furnace, temperature is from 100 DEG C, and every 50 DEG C of tests once, reaction temperature is: 100 ~ 600 DEG C.Adopt the U.S. Nicolet Nexus 470 class infrared spectrometric analyzer with 2.4m light path gas analysis pool to carry out online gasometric analysis, thus obtain the conversion ratio of acrylonitrile and the productive rate of each product.Experimental results is shown in Fig. 3.
Embodiment 2: the LaFeO obtained by the preparation method of catalyst in embodiment 1
3, under acrylonitrile and oxygen volume ratio are 0.3:1.0 condition, carry out activity rating, other condition is all with embodiment 1, and experimental results is shown in Fig. 4.
Embodiment 3: the LaFeO obtained by the preparation method of catalyst in embodiment 1
3, under acrylonitrile and oxygen volume ratio are 0.3:8.0 condition, carry out activity rating, other condition is all with embodiment 1, and experimental results is shown in Fig. 4.
Embodiment 4: the phenmethylol measuring 60ml is poured in 100ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 2.209 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the acetylacetone copper of 1.336 grams, after 20 minutes, is proceeded to by mixed solution in high pressure static reactor.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 550 DEG C of roastings 6 hours.Finally obtain the metal oxide La with perovskite crystal formation
2cuO
4.All the other steps are with embodiment 1.Experimental results is shown in Fig. 5 (a) and Fig. 5 (b).
Embodiment 5: the phenmethylol measuring 65ml is poured in 100ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 2.209 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the chromium acetylacetonate (III) of 1.782 grams, after 20 minutes, is proceeded to by mixed solution in high pressure static reactor.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 500 DEG C of roastings 6 hours.Finally obtain the metal oxide LaCrO with perovskite crystal formation
3.All the other steps are with embodiment 1.Experimental results is shown in Fig. 5 (a) and Fig. 5 (b).
Embodiment 6: the phenmethylol measuring 60ml is poured in 100ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 2.209 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the acetylacetone cobalt of 1.818 grams, after 20 minutes, is proceeded to by mixed solution in high pressure static reactor.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 550 DEG C of roastings 6 hours.Finally obtain the metal oxide LaCoO with perovskite crystal formation
3.All the other steps are with embodiment 1.Experimental results is shown in Fig. 5 (a) and Fig. 5 (b).
Embodiment 7: the phenmethylol measuring 60ml is poured in 100ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 2.209 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the manganese acetylacetonate (II) of 1.292 grams, after 20 minutes, is proceeded to by mixed solution in high pressure static reactor.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 550 DEG C of roastings 6 hours.Finally obtain the metal oxide LaMnO with perovskite crystal formation
3.All the other steps are with embodiment 1.Experimental results is shown in Fig. 5 (a) and Fig. 5 (b).
Embodiment 8: the phenmethylol measuring 120ml is poured in 200ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 4.418 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the manganese acetylacetonate (II) of 2.067 grams, the acetylacetone copper of 0.534 gram, wherein La:Mn:Cu=1:0.8:0.2, mixed solution, after 20 minutes, proceeds in high pressure static reactor by uniform stirring.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 550 DEG C of roastings 6 hours.Finally obtain the metal oxide LaCu with perovskite crystal formation
0.2mn
0.8o
3.All the other steps are with embodiment 1.Experimental results is shown in Fig. 6 (a) and Fig. 6 (b).
Embodiment 9: the phenmethylol measuring 120ml is poured in 200ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 4.418 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the chromium acetylacetonate (II) of 2.852 grams, the acetylacetone copper of 0.534 gram, wherein La:Cr:Cu=1:0.8:0.2, mixed solution, after 20 minutes, proceeds in high pressure static reactor by uniform stirring.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 550 DEG C of roastings 6 hours.Finally obtain the metal oxide LaCu with perovskite crystal formation
0.2cr
0.8o
3.All the other steps are with embodiment 1.Experimental results is shown in Fig. 6 (a) and Fig. 6 (b).
Embodiment 10: the phenmethylol measuring 120ml is poured in 200ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 4.418 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the acetylacetone cobalt (II) of 2.908 grams, the acetylacetone copper of 0.534 gram, wherein La:Co:Cu=1:0.8:0.2, mixed solution, after 20 minutes, proceeds in high pressure static reactor by uniform stirring.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 500 DEG C of roastings 6 hours.Finally obtain the metal oxide LaCu with perovskite crystal formation
0.2co
0.8o
3.All the other steps are with embodiment 1.Experimental results is shown in Fig. 6 (a) and Fig. 6 (b).
Embodiment 11: the phenmethylol measuring 120ml is poured in 200ml small beaker, adds magnetic stirring bar agitating heating in constant temperature blender with magnetic force, and set temperature is 80
oc.Weighing 4.418 grams of lanthanum nitrates pours in small beaker, after it dissolves completely, adds the ferric acetyl acetonade of 2.883 grams, the acetylacetone copper of 0.534 gram, wherein La:Fe:Cu=1:0.8:0.2, mixed solution, after 20 minutes, proceeds in high pressure static reactor by uniform stirring.Reactor being put into temperature is 200
oin the baking oven of C, maintain 24 hours, take out afterwards.With centrifuge (8000 revs/min, 10 minutes), outwell upper solution, then use absolute ethanol washing, centrifugal twice.Proceed to drying basin after being mixed by gained precipitation absolute ethyl alcohol, put into baking oven dry.This loose powder is ground, makes particle enough thin.Put into Muffle furnace 450 DEG C of roastings 6 hours.Finally obtain the metal oxide LaCu with perovskite crystal formation
0.2fe
0.8o
3.All the other steps are with embodiment 1.Experimental results is shown in Fig. 6 (a) and Fig. 6 (b).
Comparative example 1: the La (NO taking 8.660g
3)
36H
2o(chemically pure reagent) and the Fe (NO of 8.080g
3)
29H
2o (chemically pure reagent), is dissolved in the deionized water of 300ml, and wherein the mol ratio of La and Fe is 1:1, adds 8.403g citric acid (chemically pure reagent) simultaneously, and the mol ratio of citric acid and metal ion summation is that 1:1 dissolves and makes solution.By the mixing material configured, be placed in about 80 DEG C magnetic agitation heating jackets, heat after 3 to 4 hours, form colloidal sol shape, the baking oven inner drying 24 hours of 80 DEG C is transferred to when liquid residual 15 milliliters, 5 milliliters of absolute ethyl alcohols are at room temperature added after grinding, light and burn, by the material transfer after burning in Muffle furnace, in air atmosphere, with 2 DEG C/minute, 650 DEG C are risen to from room temperature, and after maintaining 6 hours, naturally cool to room temperature, finally obtain the metal oxide catalyst powder LaFeO with perovskite crystal formation
3.All the other are with embodiment 1.Experimental results is shown in Fig. 3.
Claims (2)
1. the preparation method for the catalyst containing acrylonitrile waste gas process, it is characterized in that: by phenmethylol as solvent and metal organic salt as metal ion source, adopt static reaction still, be 20 minutes 70 DEG C ~ 80 DEG C and reaction time, then static reaction still be placed in the baking oven of 200 DEG C, maintain 24 hours, rear centrifugation is taken out in room temperature cooling, obtain solid matter, and with absolute ethanol washing, until phenmethylol removes completely; The solid matter obtained is transferred to 100 DEG C of baking oven inner dryings 24 hours, calcines in Muffle furnace, calcine 6 hours under 450 DEG C ~ 550 DEG C conditions, be naturally down to room temperature, namely obtain desired perovskite type metal oxide ABO
3; Wherein A is rare earth metal, and B is transition metal, and A position metal organic salt selects metal nitrate, and B position metal organic salt selects acetylacetonate; The mol ratio of metal organic salt and phenmethylol is 1:100 ~ 120; Synthesized metal oxide has: LaFeO
3, LaCoO
3, LaMnO
3, La
2cuO
3, LaCrO
3, LaCu
0.2co
0.8o
3, LaCu
0.2fe
0.8o
3, LaCu
0.2mn
0.8o
3and LaCu
0.2cr
0.8o
3; Wherein B position metal ion screening be combined as Cu:Fe=0.2:0.8, Cu:Cr=0.2:0.8 and Cu:Mn=0.2:0.8, above ratio is mol ratio.
2. adopt a kind of catalyst application containing acrylonitrile waste gas process prepared by preparation method described in claim 1, it is characterized in that: the process being applied to acrylonitrile waste gas, experiment condition is air speed 80000-120000h
-1, acrylonitrile and oxygen volume ratio are 0.3:1 ~ 10, and reaction temperature is at 350 DEG C ~ 550 DEG C.
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| CN107420917A (en) * | 2016-05-24 | 2017-12-01 | 英尼奥斯欧洲股份公司 | Waste gas combustion furnace controls |
| CN109126804B (en) * | 2018-08-24 | 2021-05-28 | 广东工业大学 | Boron-doped LaCoO3Bifunctional catalyst, preparation method and application thereof |
| CN111468131B (en) * | 2020-05-28 | 2022-05-24 | 福建师范大学 | LaCoO with high catalytic oxidation activity3Method for synthesizing catalyst |
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