CN112354562B - Copper-containing catalyst and preparation method and application thereof - Google Patents

Copper-containing catalyst and preparation method and application thereof Download PDF

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CN112354562B
CN112354562B CN202011337143.3A CN202011337143A CN112354562B CN 112354562 B CN112354562 B CN 112354562B CN 202011337143 A CN202011337143 A CN 202011337143A CN 112354562 B CN112354562 B CN 112354562B
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copper
containing catalyst
carbon monoxide
temperature
preparing
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CN112354562A (en
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陆继长
赵玉慧
罗永明
方健
张哲玮
黄子君
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Kunming University of Science and Technology
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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
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/864—Removing carbon monoxide or hydrocarbons
    • 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
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72—Copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/22—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/502—Carbon monoxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/06—Polluted air
    • 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
    • B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
    • B01J2231/70—Oxidation reactions, e.g. epoxidation, (di)hydroxylation, dehydrogenation and analogues
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

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Abstract

The invention discloses a copper-containing catalyst and a preparation method and application thereof, wherein the preparation method comprises the following steps: and loading soluble copper salt on the silicon-based material by adopting an isometric impregnation method, drying, roasting, sieving, putting into a reactor, introducing flowing gas, and heating to obtain the copper-containing catalyst. When the prepared copper-containing catalyst is used for low-temperature catalytic oxidation of carbon monoxide, the conversion rate of the carbon monoxide can be obviously improved. The catalyst with high dispersion and high activity component is obtained by a simple treatment method, and has good application prospect.

Description

Copper-containing catalyst and preparation method and application thereof
Technical Field
The invention relates to the field of catalysts, and particularly relates to a copper-containing catalyst, and a preparation method and application thereof.
Background
Nowadays, air pollution is receiving increasing attention, and various toxic and harmful gases in the air are becoming hot topics, and carbon monoxide is one of them. Research shows that the affinity of carbon monoxide and hemoglobin is 200-300 times that of oxygen, and carbon monoxide and hemoglobin easily form carboxyhemoglobin after inhalation, so that the combination of oxygen and hemoglobin is prevented, the oxygen carrying capacity of blood is reduced, strong toxic reaction is caused, and great harm is caused to a human body. Meanwhile, with the development of economy and society, the annual increase of fossil energy consumption and the number of motor vehicles leads to the annual increase of carbon monoxide emission. Carbon monoxide has extremely high stability, is not easy to react with other substances, is not easy to dissolve in water, has poor hygroscopicity, and is difficult to reduce the amount of carbon monoxide under the action of natural conditions, so that the removal of carbon monoxide has important significance for ensuring the health of human bodies and treating atmospheric pollution.
Copper has been extensively studied in the direction of low temperature oxidation of carbon monoxide. Compared with noble metals, the copper-based catalyst has the advantages of low price, high reserves on the earth, and good activity and stability. In the current research, the main research on copper focuses on valence-change performance, degree of dispersion, exploration of active ingredients, interaction of active ingredients with carriers, and the like. In the current research, there are many conventional methods for obtaining highly dispersed catalyst, such as sol-gel method, hydrothermal method, deposition precipitation method, etc., but these methods are complicated and time-consuming to prepare.
Disclosure of Invention
The invention aims to provide a copper-containing catalyst, and a preparation method and application thereof. Loading copper on a base material by an isometric impregnation method, and then carrying out in-situ treatment on the base material loaded with the copper by flowing gas to obtain the copper-containing catalyst.
In order to achieve the purpose, the invention provides the following technical scheme:
one of the technical schemes of the invention is as follows: a preparation method of a copper-containing catalyst is provided, which comprises the following steps:
and (3) putting the base material into a copper precursor solution for dipping, drying, roasting, sieving, introducing flowing gas, and heating to obtain the copper-containing catalyst.
Preferably, the copper precursor is a soluble copper salt; the substrate material is a silicon-based material or an aluminum-based material.
Preferably, the soluble copper salt is copper nitrate.
Preferably, the concentration of the copper precursor solution is 0-0.6 g/mL but not 0 g/mL; the impregnation adopts an isometric impregnation method; the drying temperature is 80-140 ℃, and the drying time is 6-16 h.
Preferably, the silicon-based material is silicon dioxide powder or microsphere silica gel; the aluminum-based material is alumina.
Preferably, the sieving is to sieve the materials by 20-120 meshes, and the materials with the sieve size of 20-120 meshes are taken.
Preferably, the flow rate of the introduced flowing gas is 10-120 mL/min, the catalytic activity of the copper-containing catalyst obtained by treatment cannot be improved when the flow rate is too low, and resource waste can be caused when the flow rate is too high; the temperature rise treatment condition is that the temperature rise rate is increased to 200-900 ℃ at 1-10 ℃/min, if the temperature rise rate is too high, Cu substances are easy to sinter, the Cu dispersibility of the copper-containing catalyst is poor, and the catalytic activity is influenced.
More preferably, the temperature is maintained for 0.5 hour after the temperature is raised to the maximum temperature.
Preferably, the gas may be any gas.
The second technical scheme of the invention is as follows: provides a copper-containing catalyst prepared by the preparation method.
The third technical scheme of the invention is as follows: the copper-containing catalyst is applied to the low-temperature catalytic oxidation of carbon monoxide.
The specific steps of the copper-containing catalyst for catalytic oxidation of carbon monoxide are as follows: filling a copper-containing catalyst into a reactor, purging by inert gas, introducing 10000ppm of carbon monoxide, and feeding at a total space velocity of 15000h-1The reaction temperature is 40-260 ℃.
The beneficial technical effects of the invention are as follows:
the invention can lead the surface of the copper-containing catalyst to be reconstructed by carrying out simple flowing gas in-situ treatment on the copper-containing catalyst, greatly improve the activity of the copper-containing catalyst, and lead the conversion rate of carbon monoxide to reach 100 percent at 240 ℃ of the prepared copper-containing catalyst; can also promote active substances and disperse on the carrier well at the same time, and the active substances can pass through H2TPR test, the Cu-containing catalyst prepared according to the invention in H2The TPR spectrum has obvious reduction peaks of Cu with high dispersion and low reduction temperature.
The silicon-based material is used for preparing the copper-containing catalyst, the silicon content is 80-99.9 percent, and the copper content is more than 0 percent. The preparation method of the copper-containing catalyst provided by the invention has great industrial practicability in the preparation of the catalyst in a factory.
Drawings
FIG. 1 is a graph comparing the activity of copper-containing catalysts obtained in example 1 and comparative example 1;
FIG. 2 is a graph comparing the activity of copper-containing catalysts prepared in example 2 and comparative example 2;
FIG. 3 is a graph comparing the activity of copper-containing catalysts obtained in example 3 and comparative example 3;
FIG. 4 is a graph comparing the activity of copper-containing catalysts obtained in examples 4-5 and comparative example 4;
FIG. 5 is a graph comparing the activity of copper-containing catalysts prepared in example 8 with that of comparative example 1;
FIG. 6 is a graph comparing the activity of copper-containing catalysts prepared in example 9 and comparative example 1;
FIG. 7 is a TPR plot of copper-containing catalysts prepared in examples 1, 2, 3 and comparative example 1;
FIG. 8 is a TPR plot of the copper-containing catalysts prepared in examples 4-5 and comparative example 4.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the present invention, examples of which are illustrated in the accompanying drawings, and this detailed description should not be taken to be limiting of the invention, but is rather a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
Dissolving 0.60g of copper nitrate in 2mL of deionized water, adding 2g of mesoporous microsphere silica gel, stirring until the mixture is fully mixed, drying at 110 ℃ for 12h, roasting at 500 ℃ in a muffle furnace, cooling, sieving with a 20-120 mesh sieve, taking materials of 20-120 meshes, putting the materials into a fixed bed reactor, and carrying out programmed heating to 500 ℃ at the speed of 8 ℃/min for 0.5h under the atmosphere of helium gas of 30mL/min to obtain the copper-containing catalyst.
Example 2
Dissolving 1.20g of copper nitrate in 2mL of deionized water, adding 2g of mesoporous microsphere silica gel, stirring until the mixture is fully mixed, drying at 90 ℃ for 10 hours, roasting at 500 ℃ in a muffle furnace, cooling, sieving with a 20-120-mesh sieve, taking materials of 20-120 meshes, putting the materials into a fixed bed reactor, and carrying out temperature programming to 500 ℃ at the speed of 5 ℃/min for 0.5 hour under the atmosphere of 15mL/min helium gas to obtain the copper-containing catalyst.
Example 3
Dissolving 0.80g of copper nitrate in 2mL of deionized water, adding 2g of mesoporous microsphere silica gel, stirring until the mixture is fully mixed, drying at 110 ℃ for 12h, roasting at 500 ℃ in a muffle furnace, cooling, sieving with a 20-120 mesh sieve, taking a material of 20-120 meshes, putting the material into a fixed bed reactor, and carrying out temperature programming to 500 ℃ at a speed of 10 ℃/min for 0.5h under a nitrogen atmosphere of 30mL/min to obtain the copper-containing catalyst.
Example 4
Dissolving 0.30g of copper nitrate in 2mL of deionized water, adding 2g of alumina, stirring until the mixture is fully mixed, drying at 100 ℃ for 12h, roasting at 500 ℃ in a muffle furnace, cooling, sieving with a 20-120 mesh sieve, taking materials of 20-120 meshes, putting the materials into a fixed bed reactor, and carrying out temperature programming to 500 ℃ at the speed of 5 ℃/min under the atmosphere of helium gas of 30mL/min for 0.5h to obtain the copper-containing catalyst.
Example 5
Dissolving 0.30g of copper nitrate in 2mL of deionized water, adding 2g of alumina, stirring until the mixture is fully mixed, drying at 100 ℃ for 12 hours, roasting at 500 ℃ in a muffle furnace, cooling, sieving with a 20-120 mesh sieve, taking a material of 20-120 meshes, putting the material into a fixed bed reactor, and carrying out temperature programming to 500 ℃ at a speed of 5 ℃/min for 0.5 hour under a nitrogen atmosphere of 30mL/min to obtain the copper-containing catalyst.
Example 6
Dissolving 0.10g of copper nitrate in 2mL of deionized water, adding 2g of mesoporous microsphere silica gel, stirring until the mixture is fully mixed, drying for 6h at 140 ℃, roasting at 500 ℃ in a muffle furnace, cooling, sieving with a 20-120 mesh sieve, taking a material of 20-120 meshes, putting the material into a fixed bed reactor, and carrying out temperature programming to 900 ℃ at the speed of 10 ℃/min for 0.5h under the air atmosphere of 10mL/min to obtain the copper-containing catalyst.
Example 7
Dissolving 0.05g of copper nitrate into 2mL of deionized water, adding 2g of silicon dioxide powder, stirring until the mixture is fully mixed, drying for 16h at 80 ℃, roasting at 500 ℃ in a muffle furnace, cooling, sieving with a 20-120 mesh sieve, taking a material of 20-120 meshes, putting the material into a fixed bed reactor, and carrying out programmed heating to 200 ℃ at the speed of 1 ℃/min for 0.5h under the atmosphere of helium gas of 120mL/min to obtain the copper-containing catalyst.
Example 8
The gas flow rate was adjusted to 5mL/min as compared with example 1, and other treatment conditions were the same.
Example 9
The temperature increase rate was adjusted to 20 ℃/min as compared with example 1, and other treatment conditions were the same.
Comparative example 1
Compared with example 1, the method is not put into a solid bed reactor for flowing gas treatment and temperature rise treatment.
Comparative example 2
Compared with the example 2, the method is not put into a solid bed reactor for flowing gas treatment and temperature rise treatment.
Comparative example 3
Compared with example 3, the reactor is not placed in a solid bed reactor for flowing gas treatment and temperature rise treatment.
Comparative example 4
Compared with example 4, the method is not put into a solid bed reactor for flowing gas treatment and temperature rise treatment.
And (4) testing results:
(1) the activity of the copper-containing catalysts obtained in examples 1 to 5, examples 8 to 9 and comparative examples 1 to 4 was measured by the following method:
filling a copper-containing catalyst into a fixed bed reactor, wherein the filling mass is 0.1g, firstly purging with helium gas, and then introducing 1% O 22% of CO and 97% of He, the concentration of carbon monoxide is 20000ppm, and the total space velocity of feeding is 15000h-1The reaction system pressure is normal pressure, and the carbon monoxide low-temperature oxidation reaction is carried out under the condition that the reaction temperature is increased from 40 ℃ to 360 ℃, and the results are shown in figures 1-4.
FIG. 1 is a graph comparing the activity of the copper-containing catalysts of example 1 with that of comparative example 1. from FIG. 1, it can be seen that the copper-containing catalyst of example 1 achieves a carbon monoxide conversion of 85% at 260 ℃; the copper-containing catalyst of comparative example 1 had a carbon monoxide conversion of 35% at 260 c and only reached 85% at 360 c.
FIG. 2 is a graph comparing the activity of the copper-containing catalysts of example 2 with that of comparative example 2. from FIG. 2, it can be seen that the copper-containing catalyst of example 2 achieves a carbon monoxide conversion of 85% at 260 deg.C; the copper-containing catalyst of comparative example 2 had a carbon monoxide conversion of 50% at 260 c and only reached 85% at 360 c.
FIG. 3 is a graph comparing the activity of the copper-containing catalysts of example 3 with that of comparative example 3. from FIG. 3, it can be seen that the copper-containing catalyst of example 3 achieves 85% carbon monoxide conversion at 260 deg.C; the copper-containing catalyst of comparative example 3 had a carbon monoxide conversion of 35% at 260 c and only reached 85% at 360 c.
FIG. 4 is a graph comparing the activity of the copper-containing catalysts of examples 4-5 with that of comparative example 4. from FIG. 4, it can be seen that the copper-containing catalysts of examples 4-5 can achieve 85% carbon monoxide conversion at 200 deg.C, and the copper-containing catalysts of example 4 can achieve 100% carbon monoxide conversion at 240 deg.C; the copper-containing catalyst of comparative example 4 had a carbon monoxide conversion of 35% at 200 c and only achieved 85% at 240 c.
FIG. 5 is a graph comparing the activity of the copper-containing catalysts of example 8 with that of comparative example 1, and it can be seen from FIG. 5 that the copper-containing catalyst of example 8 has almost no improvement in activity at a treat rate of 5 mL/min.
FIG. 6 is a graph comparing the activity of the copper-containing catalysts of example 9 with that of comparative example 1, and it can be seen from FIG. 6 that the copper-containing catalyst of example 9 even has a somewhat decreased activity at a temperature ramp rate of 20 deg.C/min.
As can be seen from fig. 1-6, the activity of the copper-containing catalyst treated in situ with flowing gas under specific conditions is significantly higher than that of the untreated copper-containing catalyst, the copper-containing catalyst treated in situ with flowing gas starts to convert carbon monoxide at 140 ℃, and the conversion rate of carbon monoxide in each example can reach more than 85% at 260 ℃.
(2) H was carried out on the copper-containing catalysts obtained in examples 1 to 3 and comparative example 12TPR test, results are shown in FIG. 7.
As can be seen from FIG. 7, the He and N are used2And after the treatment at different flow rates, the reduction peak of the highly dispersed Cu is obvious, which proves that the treatment process promotes the dispersion of Cu species, the reduction peak of the highly dispersed Cu is at 150 ℃, and the reduction peak of the untreated Cu is at 230 ℃.
From the above results, it can be seen that the copper-containing catalyst, when treated in situ with flowing gas, has a significantly higher dispersed active species present than the untreated sample.
(3) H was performed on the copper-containing catalysts obtained in examples 4 to 5 and comparative example 42TPR test, the results are shown in FIG. 8.
As can be seen from FIG. 8, the He and N are used2After treatment, the reduction peak of high dispersion Cu is obvious, and the treatment process proves that the dispersion of Cu species is promoted, the reduction peak of the high dispersion Cu is at 150 ℃, and the reduction peak of the untreated Cu is at 230 ℃.
From the above results, it can be seen that the copper-containing catalyst, when treated in situ with flowing gas, has a significantly higher dispersed active species present than the untreated sample.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (8)

1. A method for preparing a copper-containing catalyst, comprising the steps of:
putting the base material into a copper precursor solution for dipping, drying, roasting, sieving, introducing flowing gas, and heating to prepare a copper-containing catalyst;
the flowing gas is nitrogen, helium or air, and the flow rate of the flowing gas is 10-120 mL/min; the temperature rise treatment is carried out under the condition that the temperature rise rate is 1-10 ℃/min until the temperature rises to 200-900 ℃.
2. The method of claim 1, wherein the copper precursor is a soluble copper salt; the substrate material is a silicon-based material or an aluminum-based material.
3. The method for preparing the copper-containing catalyst according to claim 1, wherein the concentration of the copper precursor solution is 0 to 0.6g/mL and is not 0 g/mL; the impregnation adopts an impregnation method; the drying temperature is 80-140 ℃, and the drying time is 6-16 h.
4. The method for preparing the copper-containing catalyst according to claim 2, wherein the silicon-based material is silica powder or microspherical silica gel; the aluminum-based material is alumina.
5. The method for preparing the copper-containing catalyst according to claim 1, wherein the sieving is 20-120 mesh sieving.
6. A copper-containing catalyst prepared according to the method for preparing a copper-containing catalyst of any one of claims 1 to 5.
7. Use of the copper-containing catalyst of claim 6 in the low temperature catalytic oxidation of carbon monoxide.
8. Use of a copper-containing catalyst in the low-temperature catalytic oxidation of carbon monoxide according to claim 7, characterized in that the copper-containing catalyst is charged into the reactor, purged with an inert gas and charged with 10000ppm of carbon monoxide at a total space velocity of 15000h-1The reaction temperature is 40-260 ℃.
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