CN109603820A - The monatomic method for preparing catalyst of room temperature degradation of formaldehyde under a kind of Oxygen Condition - Google Patents
The monatomic method for preparing catalyst of room temperature degradation of formaldehyde under a kind of Oxygen Condition Download PDFInfo
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Abstract
The invention discloses a kind of monatomic method for preparing catalyst of room temperature degradation of formaldehyde under Oxygen Condition, comprising the following steps: (1) hydrogen reducing obtains the defective TiO with surface Lacking oxygen2Carrier；(2) sediment Au/ defect TiO is prepared in deposition-precipitation method2；(3) dry, calcining obtains the monatomic Au/ defect TiO of final product2Catalyst.Compared with existing catalyst, present invention has an advantage that catalyst Au/ defect TiO2High-efficient, the service life is long, and monatomic catalyst has stronger anti-poisoning capability, has very big advantage in degradation of formaldehyde reaction；Using Au/ defect TiO2Monatomic catalyst, being built with conducive to the dispersion between metallic atom for defect, can be realized O2Under the conditions of be detached from ozone auxiliary room-temperature catalytic oxidation.
Description
Technical field
The present invention relates to method for preparing catalyst more particularly to a kind of monatomic catalyst systems of room-temperature catalytic oxidation formaldehyde
Preparation Method.
Background technique
Aldehydes is that one of maximum component of content, formaldehyde are one of the most common type aldehydes in global reactivity VOCs in atmosphere
VOCs, it is one of the main source for controlling the new free radical that ozone is formed.Formaldehyde is mainly derived from VOCs (alcohols and other carbon
Hydrogen compound) oxidative degradation during multiple.In either indoor or outdoor air, formaldehyde is all a kind of preferential pollution
Object, with toxicity and irritation.
Using active carbon, the adsorbents such as aluminium oxide can effectively remove HCHO, but adsorb usually by the limit of adsorption capacity
System, room-temperature catalytic oxidation technology are the most effective technologies of VOCs degradation, which is usually catalysis with metal, metal oxide
Agent is oxidized the formaldehyde under normal temperature conditions in conjunction with strong oxidizing property free radical as CO2、H2O.Compared with conventional catalyst combustion method, often
Warm catalytic oxidation technologies may be implemented in efficient, safety, VOCs exhaust gas of degrading to low energy consumption under the conditions of room temperature (20-50 DEG C).Currently,
The research for having document report room-temperature catalytic oxidation processing formaldehyde, benzene, toluene etc. proposes monatomic urge on this basis
The concept of change, monatomic catalysis, which refers to, is carried on isolated monatomic active site on carrier, realizes that active site is high
Spend a kind of emerging catalysis concept of dispersion.Existing research show monatomic catalysis can significantly reduce catalysis needed for reaction temperature with
Pressure, it is most likely that realize the VOCs constant temperature catalyzing degradation without additional ozone auxiliary.
Currently used various VOCs processing techniques cannot degradation of formaldehyde gas well, be on the one hand easier to cause to urge
Agent inactivation, on the other hand may cause secondary pollution.The monatomic catalytic oxidation technologies of room temperature utilize monatomic work at normal temperature
Property site and O2Double action exhaustive oxidation formaldehyde gas, have easy to operate, safe, high-efficient, catalyst persistently etc. excellent
Point.Compared to carrier nanometer catalyst, monatomic catalyst has many unique advantages, for example, active bit architecture it is uniform,
Metallic atom utilization efficiency can realize maximization, have unique high activity, can link up homogeneously with multiphase etc., these advantages are equal
Be confirmed in early-stage study, the fields such as CO oxidation reaction, Water gas shift/WGS, hydrogenation reaction and electrochemical catalysis all
It is widely used.Experiment and theoretical research show that monatomic high activity of catalyst and selectivity are attributable to active metal original
Interaction and thus caused electronic structure change between son and carrier.Monatomic catalyst surface with higher
Can, it is monatomic more liquid, tend to assemble in catalytic reaction process, influence catalytic activity, currently, existing monatomic
Catalyst, such as Ag/TiO2Also need to realize the degradation of formaldehyde under higher temperature conditions, and easy in inactivation, stability are poor.
Summary of the invention
The purpose of the present invention is to overcome the disadvantages of the prior art, provides room-temperature catalytic oxidation formaldehyde under a kind of Oxygen Condition
Method for preparing catalyst, this method can prepare catalyst at normal temperature, with monatomic catalyst prepared by this method have compared with
Strong monatomic stability, the Degradation Formaldehyde reaction temperature carried out with the monatomic catalyst is low, greatly reduces reaction activation
Can, catalytic efficiency is significantly promoted.
The technical scheme is that
The monatomic method for preparing catalyst of room temperature degradation of formaldehyde under a kind of Oxygen Condition of the invention, including following step
It is rapid:
Step 1: the TiO for being 40-60nm by diameter2Nanometer powder is placed in tube furnace, and gas stream is passed through in tube furnace
Speed is the H of 50-100mL/min2And N2Gaseous mixture, the H2And N2Volume ratio is 1:(18-20), tubular type furnace temperature is adjusted to
200-400 DEG C of heat treatment TiO2Nanometer powder 1.5-2.5h obtains the defective TiO with surface Lacking oxygen2Carrier；
Step 2: firstly, will be the defective TiO of 1:(45-55) with deionized water quality ratio2Carrier suspends
In deionized water, 12-16min is stirred with glass bar, the sal volatile of 0.8-1.2mol/L is added into suspension, obtains
Solution A；
It then, will be the HAuCl of 1:(9.2-11.7) with deionized water quality ratio4·4H2O is dissolved in deionized water, so
After be added dropwise in solution A, obtain solution B, in the solution B, ammonium carbonate and HAuCl4·4H2The ratio between the amount of O substance is
(2-3): 1, the defective TiO2Carrier and HAuCl4·4H2The mass ratio of O is (10-50): 1；
Finally, solution B is stirred 0.8-1.1h at a temperature of -10-50 DEG C, it is collected by filtration with funnel and is formed by precipitating
Precipitating is washed with deionized in object；
Step 3: by the sediment after washing in drying box at 60-80 DEG C dry 3-5h, then in tube furnace in
H is passed through at 200-400 DEG C2And N2Gaseous mixture calcines 1.5-2.5h, wherein H2And N2Volume ratio is 1:(18-20), gas flow rate is
50-100mL/min obtains monatomic Au/ defect TiO2Catalyst.
Present invention has an advantage that catalyst Au/ defect TiO2High-efficient, the service life is long, and monatomic catalyst has stronger
Anti- poisoning capability has very big advantage in degradation of formaldehyde reaction；TiO2As carrier, except having, nontoxic, performance is stable, price
Outside the advantages that cheap, anticorrosive, also as aluminium oxide, there are polymolecularity, high porosity；Using Au/ defect TiO2It is monatomic
Catalyst, being built with conducive to the dispersion between metallic atom for defect, can be realized O2Under the conditions of be detached from ozone auxiliary room temperature
Catalysis oxidation.
Detailed description of the invention
Fig. 1 is that deposition-precipitation method of the present invention prepares Au/ defect TiO2Catalyst process schematic diagram.
Specific embodiment
Below in conjunction with case study on implementation of the present invention, the technical solution in case study on implementation of the present invention is carried out clear, complete
Description, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, shall fall within the protection scope of the present invention.
Of the invention the reaction mechanism is as follows: compared to complete TiO2Nano particle, the TiO of aerobic vacancy defect2Nanometer
Grain surface forms Ti-Au-Ti structure, has better stability, and due to steric hindrance and electrostatic effect, O2Primary attachment in
HCHO is adsorbed in the site Ti in the site Au, adjacent bit, and this absorption mechanism alleviates HCHO and O2Competition on the same site Au
Absorption, Au is monatomic due to its raised d track center of gravity energy level, to the O of absorption2It is activated, the drop of energy barrier needed for oxidation of formaldehyde
It is low, promote the progress of catalytic process.
Based on the above mechanism, the monatomic catalyst preparation side of room temperature degradation of formaldehyde under a kind of Oxygen Condition of the invention
Method, comprising the following steps:
Step 1: the TiO for being 40-60nm by diameter2Nanometer powder is placed in tube furnace, and gas stream is passed through in tube furnace
Speed is the H of 50-100mL/min2And N2Gaseous mixture, the H2And N2Volume ratio is 1:(18-20), tubular type furnace temperature is adjusted to
200-400 DEG C of heat treatment TiO2Nanometer powder 1.5-2.5h obtains the defective TiO with surface Lacking oxygen2Carrier；
Step 2: firstly, will be the defective TiO of 1:(45-55) with deionized water quality ratio2Carrier suspends
In deionized water, 12-16min is stirred with glass bar, the sal volatile of 0.8-1.2mol/L is added into suspension, obtains
Solution A；
It then, will be the HAuCl of 1:(9.2-11.7) with deionized water quality ratio4·4H2O is dissolved in deionized water, so
After be added dropwise in solution A, obtain solution B, in the solution B, ammonium carbonate and HAuCl4·4H2The ratio between the amount of O substance is
(2-3): 1, the defective TiO2Carrier and HAuCl4·4H2The mass ratio of O is (10-50): 1；
Finally, solution B is stirred 0.8-1.1h at a temperature of -10-50 DEG C, it is collected by filtration with funnel and is formed by precipitating
Precipitating is washed with deionized in object；
Step 3: by the sediment after washing in drying box at 60-80 DEG C dry 3-5h, then in tube furnace in
H is passed through at 200-400 DEG C2And N2Gaseous mixture calcines 1.5-2.5h, wherein H2And N2Volume ratio is 1:(18-20), gas flow rate is
50-100mL/min obtains monatomic Au/ defect TiO2Catalyst.
Embodiment 1
Step 1: the TiO for being 40nm by diameter2Nanometer powder is placed in tube furnace, and gas flow rate is passed through in tube furnace
For the H of 50mL/min2And N2Gaseous mixture, the H2And N2Volume ratio is 1:18, and tubular type furnace temperature is adjusted to 200 DEG C of heat treatments
TiO2Nanometer powder 1.5h obtains the defective TiO with surface Lacking oxygen2Carrier；
Step 2: firstly, by with deionized water quality than the defective TiO for 1:452Carrier is suspended in
In ionized water, 12min is stirred with glass bar, the sal volatile of 0.8mol/L is added into suspension, obtains solution A；
Then, by with deionized water quality than the HAuCl for 1:9.24·4H2O is dissolved in deionized water, is then added dropwise
Enter in solution A, obtains solution B, in the solution B, ammonium carbonate and HAuCl4·4H2The ratio between amount of O substance is 2:1, described
Defective TiO2Carrier and HAuCl4·4H2The mass ratio of O is 10:1；
Finally, solution B is stirred 0.8h at a temperature of -10 DEG C, be collected by filtration with funnel and be formed by sediment, spend from
Sub- water washing precipitating；
Step 3: the sediment after washing to be dried to 3h in drying box at 60 DEG C, then in 200 DEG C in tube furnace
Under be passed through H2And N2Gaseous mixture calcines 1.5h, wherein H2And N2Volume ratio is 1:18, and gas flow rate 50mL/min obtains single original
Sub- Au/ defect TiO2Catalyst.
The evaluation of catalyst oxidation effectiveness carries out in Degradation Formaldehyde reaction unit, and the present embodiment is packed into reactor and is made
Catalyst 1g to be measured, for the reaction of room-temperature catalytic oxidation formaldehyde under Oxygen Condition, reaction condition are as follows: concentration of formaldehyde is
1000mg/m3, air speed 20000h-1, with the concentration of gas chromatograph detection reactants and products.The catalysis of monatomic catalyst
Performance is shown in Table 1.
Embodiment 2
Step 1: the TiO for being 50nm by diameter2Nanometer powder is placed in tube furnace, and gas flow rate is passed through in tube furnace
For the H of 75mL/min2And N2Gaseous mixture, the H2And N2Volume ratio is 1:19, and tubular type furnace temperature is adjusted to 300 DEG C of heat treatments
TiO2Nanometer powder 2h obtains the defective TiO with surface Lacking oxygen2Carrier；
Step 2: firstly, by with deionized water quality than the defective TiO for 1:502Carrier is suspended in
In ionized water, 15min is stirred with glass bar, the sal volatile of 1mol/L is added into suspension, obtains solution A；
Then, by with deionized water quality than the HAuCl for 1:10.54·4H2O is dissolved in deionized water, is then added dropwise
Enter in solution A, obtains solution B, in the solution B, ammonium carbonate and HAuCl4·4H2The ratio between amount of O substance is 2.5:1, institute
The defective TiO stated2Carrier and HAuCl4·4H2The mass ratio of O is 30:1；
Finally, solution B is stirred 1h at a temperature of 20 DEG C, it is collected by filtration with funnel and is formed by sediment, use deionization
Water washing precipitating；
Step 3: the sediment after washing to be dried to 4h in drying box at 70 DEG C, then in 300 DEG C in tube furnace
Under be passed through H2And N2Gaseous mixture calcines 2h, wherein H2And N2Volume ratio is 1:19, and gas flow rate 75mL/min is obtained monatomic
Au/ defect TiO2Catalyst.
The evaluation of catalyst oxidation effectiveness carries out in Degradation Formaldehyde reaction unit, and the present embodiment is packed into reactor and is made
Catalyst 1g to be measured, for the reaction of room-temperature catalytic oxidation formaldehyde under Oxygen Condition, reaction condition are as follows: concentration of formaldehyde is
1000mg/m3, air speed 20000h-1, with the concentration of gas chromatograph detection reactants and products.The catalysis of monatomic catalyst
Performance is shown in Table 1.
Embodiment 3
Step 1: the TiO for being 50nm by diameter2Nanometer powder is placed in tube furnace, and gas flow rate is passed through in tube furnace
For the H of 75mL/min2And N2Gaseous mixture, the H2And N2Volume ratio is 1:18, and tubular type furnace temperature is adjusted to 300 DEG C of heat treatments
TiO2Nanometer powder 2h obtains the defective TiO with surface Lacking oxygen2Carrier；
Step 2: firstly, by with deionized water quality than the defective TiO for 1:502Carrier is suspended in
In ionized water, 15min is stirred with glass bar, the sal volatile of 1mol/L is added into suspension, obtains solution A；
Then, by with deionized water quality than the HAuCl for 1:10.54·4H2O is dissolved in deionized water, is then added dropwise
Enter in solution A, obtains solution B, in the solution B, ammonium carbonate and HAuCl4·4H2The ratio between amount of O substance is 2:1, described
Defective TiO2Carrier and HAuCl4·4H2The mass ratio of O is 30:1；
Finally, solution B is stirred 1h at a temperature of 20 DEG C, it is collected by filtration with funnel and is formed by sediment, use deionization
Water washing precipitating；
Step 3: the sediment after washing to be dried to 4h in drying box at 70 DEG C, then in 300 DEG C in tube furnace
Under be passed through H2And N2Gaseous mixture calcines 2h, wherein H2And N2Volume ratio is 1:18, and gas flow rate 80mL/min is obtained monatomic
Au/ defect TiO2Catalyst.
The evaluation of catalyst oxidation effectiveness carries out in Degradation Formaldehyde reaction unit, and the present embodiment is packed into reactor and is made
Catalyst 1g to be measured, for the reaction of room-temperature catalytic oxidation formaldehyde under Oxygen Condition, reaction condition are as follows: concentration of formaldehyde is
1000mg/m3, air speed 20000h-1, with the concentration of gas chromatograph detection reactants and products.The catalysis of monatomic catalyst
Performance is shown in Table 1.
Embodiment 4
Step 1: the TiO for being 60nm by diameter2Nanometer powder is placed in tube furnace, and gas flow rate is passed through in tube furnace
For the H of 100mL/min2And N2Gaseous mixture, the H2And N2Volume ratio is 1:20, and tubular type furnace temperature is adjusted to 400 DEG C of heat treatments
TiO2Nanometer powder 2.5h obtains the defective TiO with surface Lacking oxygen2Carrier；
Step 2: firstly, by with deionized water quality than the defective TiO for 1:552Carrier is suspended in
In ionized water, 16min is stirred with glass bar, the sal volatile of 1.2mol/L is added into suspension, obtains solution A；
Then, by with deionized water quality than the HAuCl for 1:11.74·4H2O is dissolved in deionized water, is then added dropwise
Enter in solution A, obtains solution B, in the solution B, ammonium carbonate and HAuCl4·4H2The ratio between amount of O substance is 3:1, described
Defective TiO2Carrier and HAuCl4·4H2The mass ratio of O is 50:1；
Finally, solution B is stirred 1.1h at 50 °C, be collected by filtration with funnel and be formed by sediment, spend from
Sub- water washing precipitating；
Step 3: the sediment after washing to be dried to 5h in drying box at 80 DEG C, then in 400 DEG C in tube furnace
Under be passed through H2And N2Gaseous mixture calcines 2.5h, wherein H2And N2Volume ratio is 1:20, and gas flow rate 100mL/min obtains single original
Sub- Au/ defect TiO2Catalyst.
The evaluation of catalyst oxidation effectiveness carries out in Degradation Formaldehyde reaction unit, and the present embodiment is packed into reactor and is made
Catalyst 1g to be measured, for the reaction of room-temperature catalytic oxidation formaldehyde under Oxygen Condition, reaction condition are as follows: concentration of formaldehyde is
1000mg/m3, air speed 20000h-1, with the concentration of gas chromatograph detection reactants and products.The catalysis of monatomic catalyst
Performance is shown in Table 1.
1 Au/ defect TiO of table2Monatomic catalyst oxidation of formaldehyde reactivity worth
Claims (1)
1. the monatomic method for preparing catalyst of room temperature degradation of formaldehyde under a kind of Oxygen Condition, it is characterised in that: including following step
It is rapid:
Step 1: the TiO for being 40-60nm by diameter2Nanometer powder is placed in tube furnace, and gas flow rate is passed through in tube furnace and is
The H of 50-100mL/min2And N2Gaseous mixture, the H2And N2Volume ratio is 1:(18-20), tubular type furnace temperature is adjusted to 200-
400 DEG C of heat treatment TiO2Nanometer powder 1.5-2.5h obtains the defective TiO with surface Lacking oxygen2Carrier；
Step 2: firstly, will be the defective TiO of 1:(45-55) with deionized water quality ratio2Carrier is suspended in
In ionized water, 12-16min is stirred with glass bar, the sal volatile of 0.8-1.2mol/L is added into suspension, obtains solution
A；
It then, will be the HAuCl of 1:(9.2-11.7) with deionized water quality ratio4·4H2O is dissolved in deionized water, is then dripped
It is added in solution A, obtains solution B, in the solution B, ammonium carbonate and HAuCl4·4H2The ratio between amount of O substance is (2-3):
1, the defective TiO2Carrier and HAuCl4·4H2The mass ratio of O is (10-50): 1；
Finally, solution B is stirred 0.8-1.1h at a temperature of -10-50 DEG C, it is collected by filtration with funnel and is formed by sediment, is used
Deionized water washing precipitating；
Step 3: the sediment after washing to be dried to 3-5h in drying box at 60-80 DEG C, then in 200- in tube furnace
H is passed through at 400 DEG C2And N2Gaseous mixture calcines 1.5-2.5h, wherein H2And N2Volume ratio is 1:(18-20), gas flow rate 50-
100mL/min obtains monatomic Au/ defect TiO2Catalyst.
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| CN114162907A (en) * | 2021-11-30 | 2022-03-11 | 上海交通大学 | Monoatomic electrode and preparation method and application thereof |
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