CN109603895B - Air purification material - Google Patents
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- CN109603895B CN109603895B CN201811637798.5A CN201811637798A CN109603895B CN 109603895 B CN109603895 B CN 109603895B CN 201811637798 A CN201811637798 A CN 201811637798A CN 109603895 B CN109603895 B CN 109603895B
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- B01J29/00—Catalysts comprising molecular sieves
- B01J29/03—Catalysts comprising molecular sieves not having base-exchange properties
- B01J29/0308—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41
- B01J29/0316—Mesoporous materials not having base exchange properties, e.g. Si-MCM-41 containing iron group metals, noble metals or copper
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- 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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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Abstract
The invention provides an air purification material, which is characterized by comprising a formaldehyde decomposition layer positioned at the upstream and an auxiliary adsorption layer positioned at the downstream; the formaldehyde decomposition layer comprises a formaldehyde decomposition material for decomposing formaldehyde, and the auxiliary adsorption layer is used for adsorbing other polluting gases in the air; the formaldehyde decomposition material consists of a DD3R molecular sieve and a noble metal active component. The invention selects the adsorption materials of the formaldehyde hierarchical layer, ensures that the formaldehyde in the gas is preferentially catalyzed and decomposed, and assists the downstream adsorption layer to ensure the applicability of the purification material in the air.
Description
Technical Field
The application relates to an air purification material, in particular to an air purification material for preferentially purifying formaldehyde in airflow.
Background
Harmful substances such as formaldehyde, benzene, toluene, xylene and the like can be released in newly-decorated houses, are particularly harmful to human bodies, and can cause serious influence on human health and even endanger life after long-term contact. The release period of formaldehyde is longer, or as long as 3-15 years, compared to the release period of other types of pollutant gases as low as 6 months. So that after several months of ventilation and odor removal after house decoration, the formaldehyde in the room needs to be preferentially purified. The commonly used formaldehyde pollutants can be removed by physical adsorption (such as activated carbon, molecular sieve, etc.), biological method, ozone oxidation method, plant degradation method, catalytic oxidation method, etc. The physical method for removing formaldehyde by using a porous material is easily influenced by the absorption pore diameter and has limited absorption capacity; although the biological method has good effect of removing formaldehyde, once microorganisms are leaked, the danger is larger; the ozone oxidation method is easy to cause secondary pollution; the plant degradation method can degrade formaldehyde to a certain extent but has limited formaldehyde absorption capacity, and the method can be used as an auxiliary method for removing formaldehyde; catalytic oxidation is currently the best method used to remove formaldehyde.
The catalyst used in the conventional catalytic oxidation method usually employs a porous material such as a molecular sieve (e.g., ZSM-5, HY, MCM-41, MCM-48, NaY, SBA-15, etc.), titanium oxide, etc. as a catalyst support. However, in practical application, formaldehyde is found to be catalytically decomposed into water and carbon dioxide, wherein the water can lead to the deactivation of the catalyst, and the carbon dioxide can be adsorbed by the porous material, so that the formaldehyde catalytic decomposition performance of the catalyst is lower and lower. Moreover, the prepared catalyst material has great effect difference between the laboratory measurement effect and the actual application, because a single formaldehyde gas is often adopted in the laboratory for effect measurement, and the actually applied gas contains various types of gases such as benzene, toluene, xylene, acetone, water and the like besides formaldehyde, and generates competitive adsorption with formaldehyde in the catalysis process, so that the final formaldehyde purification effect has great difference with the laboratory effect.
Disclosure of Invention
For this purpose, the invention designs an air purification material aiming at formaldehyde in polluted gas, wherein the material comprises a formaldehyde decomposition layer positioned at the upstream and an auxiliary adsorption layer positioned at the downstream; the formaldehyde decomposition layer comprises a formaldehyde decomposition material for decomposing formaldehyde, and the auxiliary adsorption layer is used for adsorbing other polluting gases in the air; the formaldehyde decomposition material consists of a DD3R molecular sieve and a noble metal active component.
Preferably, the noble metal is one or more of Pt, Pd, Au and Ag.
Preferably, the auxiliary adsorption layer is selected from adsorbents with large specific surface area, such as activated carbon, zeolite, molecular sieve, silica gel and the like.
Preferably, the formaldehyde decomposition layer further comprises a carbon dioxide adsorbing material for adsorbing CO2 in the gas flow and/or carbon dioxide generated by formaldehyde decomposition.
Preferably, the carbon dioxide adsorbing material is composed of an amino functionalized porous material.
Preferably, the distance between the formaldehyde decomposition layer and the auxiliary adsorption layer is not less than 10 cm.
Preferably, the formaldehyde decomposition layer and the auxiliary adsorption layer are separable.
For the carbon dioxide adsorbing material, preferably, the porous material is a composite porous material with a micropore/mesopore structure. Particularly preferably, the composite porous material is HZSM-5/MCM-41.
Preferably, the mass ratio of the carbon dioxide adsorbing material to the amino-functionalized porous material is 1: 0.5-4.
Preferably, the amine modifier used for preparing the amino-functionalized porous material is one or more of hindered amine, alkylamine, amino polymer and organosilane. Particularly preferably, the amine is tetraethylenepentamine.
Preferably, the formaldehyde decomposition material consists of a DD3R molecular sieve and a noble metal active component, wherein the mass fraction of the molecular sieve is 90-95% and the mass fraction of the noble metal active component is 5-10% calculated by 100% of the type of the catalyst; the preparation method of the formaldehyde purification material comprises the following steps:
(1) mixing water, amantadine and a cosolvent, completely dissolving the amantadine through high-frequency ultrasonic treatment, dripping a silicon source and noble metal salt solution under the condition of ice bath stirring, and stirring and aging at high temperature to form amantadine: silicon source: noble metal sources: cosolvent: the water molar ratio is 30-50:100:5-20:100-500:5000-50000 synthetic fluid;
(2) adding the seed crystal prepared in advance into the synthetic liquid according to the mass ratio of 0.2-2%, placing the synthetic liquid into a microwave reaction kettle, and carrying out hydrothermal synthesis for 48-72h under the microwave condition with the stirring temperature of 150-;
(3) after the hydrothermal synthesis is finished, pouring the synthetic liquid in the microwave reaction kettle into an evaporation container to evaporate water in the synthetic liquid and dry the solid material;
(4) and roasting the dried solid material for 3-4h in an ozone environment to prepare the required formaldehyde purification material. In the method, the roasting temperature is 300-400 ℃. The noble metal is one or more of Pt, Pd, Au and Ag. The cosolvent is ethylenediamine. The seed crystal is one of sigma-1, DD3R and ZSM-58. Preferably, the dried solid material is ground prior to firing. The frequency of the high-frequency ultrasonic wave is 20-25kHz, and the power is 500-1800 w. The seed crystal is molecular sieve particles without template agent removal.
Preferably, the carbon dioxide adsorbent material is prepared by an impregnation method.
THE ADVANTAGES OF THE PRESENT INVENTION
1. Firstly, the formaldehyde decomposition layer adopts the all-silicon molecular sieve as the adsorption material, so that the water generated by formaldehyde decomposition and the water molecules in the air are prevented from being absorbed by the molecular sieve, and the possibility of catalyst deactivation is reduced. Because the diameter of the molecular sieve pore canal with the DDR configuration is larger than the kinetic diameter of formaldehyde and smaller than the kinetic diameter of polluted gases such as benzene, toluene, xylene, acetone and the like, other polluted gases can be prevented from entering the DD3R pore canal to be adsorbed, and the relatively single adsorbability of the adsorbing material to the formaldehyde gas is ensured.
2. In addition, the auxiliary adsorption layer is arranged at the downstream of the formaldehyde decomposition layer to adsorb other pollution components in the gas and formaldehyde which is not catalytically decomposed by the formaldehyde decomposition layer, so that the applicability of the formaldehyde purifier in purifying air is improved. In addition, because the upstream formaldehyde decomposition layer does not need to be regenerated, and the downstream auxiliary adsorption layer needs to be regenerated, the invention designs a separable two-layer structure, and only needs to regenerate the auxiliary adsorption layer, thereby simplifying the working efficiency of the purifier.
3. In addition, because formaldehyde is decomposed to generate carbon dioxide gas, and a certain amount of carbon dioxide also exists in the air, the salt solution of the noble metal is mixed with the synthesis solution of the DD3R molecular sieve, the noble metal is loaded on the molecular sieve particles by adopting an in-situ synthesis method, part of the noble metal enters a framework of the molecular sieve to replace silicon element, and the ionic radius of the noble metal is larger than that of silicon, so that the aperture of the molecular sieve is relatively reduced, the carbon dioxide adsorption between dynamics close to the aperture of DDR is reduced, and the relatively single adsorption of the adsorption material to the formaldehyde gas is also ensured. The formaldehyde decomposition material is compounded with the CO2 adsorption material, and the amino modified porous adsorption material ensures that the CO2 adsorption material preferentially adsorbs CO2 gas, reduces the degree of CO2 adsorption of the formaldehyde decomposition material, and further ensures the formaldehyde decomposition capacity of the composite material.
Detailed Description
Example 1
(1) Crushing amantadine into particles, putting the particles into a beaker, adding a proper amount of ethylenediamine and water, and then carrying out ultrasonic treatment on the particles for 15min by using an ultrasonic cell crusher, wherein the set frequency is 20kHz and the power is 900 w. And (3) placing the beaker into an ice-water mixture after ultrasonic treatment, adding a rotor after the beaker is cooled, and sequentially dropwise adding a proper amount of silica sol and H2PtCl4 solution under a stirring state. After the end of the dropwise addition, the beaker was heated to 90 ℃ with stirring and held for 30min to form amantadine: silicon source: noble metal sources: ethylene diamine: the water molar ratio is 47: 100: 10:400: 11240.
(2) Ball-milling pre-prepared DD3R molecular sieve particles (the particle size is 300 nm), adding the ball-milled particles into the synthetic solution according to the mass ratio of 0.5%, placing the synthetic solution into a microwave reaction kettle, and stirring under the microwave condition for hydrothermal synthesis for 72 hours to ensure that a silicon source in the synthetic solution is fully utilized, wherein the synthesis temperature is 160 ℃.
(3) And after the hydrothermal synthesis is finished, pouring the synthetic liquid in the microwave reaction kettle into an evaporation container, evaporating and drying water in the synthetic liquid at high temperature, and grinding the solid particles agglomerated together to disperse the solid particles.
(4) The dried solid material is roasted for 3-4h in an ozone environment to prepare the required air purification material A1, and the set temperature is 300 ℃.
Example 2
(1) Crushing amantadine into particles, putting the particles into a beaker, adding a proper amount of ethylenediamine and water, and then carrying out ultrasonic treatment on the particles for 15min by using an ultrasonic cell crusher, wherein the set frequency is 20kHz and the power is 900 w. And (3) placing the beaker into an ice-water mixture after ultrasonic treatment, adding a rotor after the beaker is cooled, and sequentially dropwise adding a proper amount of silica sol and H2PtCl4 solution under a stirring state. After the end of the dropwise addition, the beaker was heated to 90 ℃ with stirring and held for 30min to form amantadine: silicon source: noble metal sources: ethylene diamine: the water molar ratio is 47: 100: 10:400: 11240.
(2) Ball-milling pre-prepared DD3R molecular sieve particles (the particle size is 300 nm), adding the ball-milled particles into the synthetic solution according to the mass ratio of 0.5%, placing the synthetic solution into a microwave reaction kettle, and stirring under the microwave condition for hydrothermal synthesis for 72 hours to ensure that a silicon source in the synthetic solution is fully utilized, wherein the synthesis temperature is 160 ℃.
(3) And after the hydrothermal synthesis is finished, pouring the synthetic liquid in the microwave reaction kettle into an evaporation container, evaporating and drying water in the synthetic liquid at high temperature, and grinding the solid particles agglomerated together to disperse the solid particles.
(4) The dried solid material is roasted for 3-4h in an ozone environment to prepare the required formaldehyde decomposition material, and the set temperature is 300 ℃.
(5) And uniformly mixing commercial HZSM-5 and MCM-41 molecular sieves with the same mass, and then placing the mixture in an oven for 6 hours.
(6) Weighing tetraethylenepentamine with the mass of 30% of that of the composite molecular sieve, adding absolute ethyl alcohol, ultrasonically stirring for 10min to completely dissolve the tetraethylenepentamine, adding the composite molecular sieve in the step (5), ultrasonically treating for 6h, and drying in a vacuum drying oven at 80 ℃ for a whole day to obtain the CO2 adsorbing material.
(7) And (3) uniformly mixing the formaldehyde decomposition material prepared in the step (4) and the CO2 adsorption material prepared in the step (6) in equal mass, thereby obtaining the air purification composite material A2.
Example 3
An air cleaning material a3 was prepared by using the formaldehyde cleaning material prepared in example 1 as an upstream formaldehyde decomposition layer and commercial activated carbon (767 type) as an auxiliary adsorption layer.
Example 4
An air cleaning material a4 was prepared by using the formaldehyde cleaning material prepared in example 2 as an upstream formaldehyde decomposition layer and commercial activated carbon (767 type) as an auxiliary adsorption layer.
Comparative example 1
(1) Silica sol is used as a silicon source, TPAOH is used as a template agent, and the silica sol and deionized water are prepared into the silica sol-based composite material with the molar ratio of SiO2 to H2PtCl 4: TPAOH: H2O = 100: 10: 5: 1000.
(2) Adding a prepared silicalite-1 molecular sieve into the synthetic solution according to the mass ratio of 0.5% after ball milling (the particle size is 300 nm), placing the synthetic solution into a microwave reaction kettle, and carrying out hydrothermal synthesis for 72 hours under the microwave condition by stirring, wherein the synthesis temperature is 160 ℃.
(3) And after the hydrothermal synthesis is finished, pouring the synthetic liquid in the microwave reaction kettle into an evaporation container, evaporating and drying water in the synthetic liquid at high temperature, and grinding the solid particles agglomerated together to disperse the solid particles.
(4) The dried solid material is roasted for 3-4h in an ozone environment to prepare the required air purification material D1, and the set temperature is 300 ℃.
Reference document 2
(1) Crushing amantadine into particles, putting the particles into a beaker, adding a proper amount of ethylenediamine and water, and then carrying out ultrasonic treatment on the particles for 15min by using an ultrasonic cell crusher, wherein the set frequency is 20kHz and the power is 900 w. After ultrasonic treatment, the beaker is placed in an ice-water mixture, after the beaker is cooled, a rotor is added, and a proper amount of silica sol is added dropwise under the stirring state. After the end of the dropwise addition, the beaker was heated to 90 ℃ with stirring and held for 30min to form amantadine: silicon source: ethylene diamine: the water molar ratio is 47: 100: 400:11240 of the synthetic liquid.
(2) Ball-milling pre-prepared DD3R molecular sieve particles (the particle size is 300 nm), adding the ball-milled particles into the synthetic solution according to the mass ratio of 0.5%, placing the synthetic solution into a microwave reaction kettle, and stirring under the microwave condition for hydrothermal synthesis for 72 hours to ensure that a silicon source in the synthetic solution is fully utilized, wherein the synthesis temperature is 160 ℃.
(3) And after the hydrothermal synthesis is finished, centrifuging, cleaning and drying the synthetic liquid in the microwave reaction kettle to obtain the DD3R molecular sieve particles. Dispersing the molecular sieve particles in H2PtCl4 solution, stirring for a while, evaporating to remove water at 80 deg.C, and drying.
(4) The dried solid material is roasted for 3-4h in an ozone environment to prepare the required air purification material D2, and the set temperature is 300 ℃.
Comparative example 3
(1) Crushing amantadine into particles, putting the particles into a beaker, adding a proper amount of ethylenediamine and water, and then carrying out ultrasonic treatment on the particles for 15min by using an ultrasonic cell crusher, wherein the set frequency is 20kHz and the power is 900 w. And (3) placing the beaker into an ice-water mixture after ultrasonic treatment, adding a rotor after the beaker is cooled, and sequentially dropwise adding a proper amount of silica sol and H2PtCl4 solution under a stirring state. After the end of the dropwise addition, the beaker was heated to 90 ℃ with stirring and held for 30min to form amantadine: silicon source: noble metal sources: ethylene diamine: the water molar ratio is 47: 100: 10:400: 11240.
(2) Ball-milling pre-prepared DD3R molecular sieve particles (the particle size is 300 nm), adding the ball-milled particles into the synthetic solution according to the mass ratio of 0.5%, placing the synthetic solution into a microwave reaction kettle, and stirring under the microwave condition for hydrothermal synthesis for 72 hours to ensure that a silicon source in the synthetic solution is fully utilized, wherein the synthesis temperature is 160 ℃.
(3) After the hydrothermal synthesis is finished, the synthetic fluid in the microwave reaction kettle is centrifugally cleaned and dried to obtain a solid material, and the agglomerated solid particles are ground to be dispersed.
(4) The dried solid material is roasted for 3-4h in an ozone environment to prepare the required air purification material D3, and the set temperature is 300 ℃.
Reference 4
(1) Crushing amantadine into particles, putting the particles into a beaker, adding a proper amount of ethylenediamine and water, and then carrying out ultrasonic treatment on the particles for 15min by using an ultrasonic cell crusher, wherein the set frequency is 20kHz and the power is 900 w. And (3) placing the beaker into an ice-water mixture after ultrasonic treatment, adding a rotor after the beaker is cooled, and sequentially dropwise adding a proper amount of silica sol and H2PtCl4 solution under a stirring state. After the end of the dropwise addition, the beaker was heated to 90 ℃ with stirring and held for 30min to form amantadine: silicon source: noble metal sources: ethylene diamine: the water molar ratio is 47: 100: 10:400: 11240.
(2) Ball-milling pre-prepared DD3R molecular sieve particles (the particle size is 300 nm), adding the ball-milled particles into the synthetic liquid according to the mass ratio of 0.5%, placing the synthetic liquid into a common reaction kettle, stirring in an oven, and carrying out hydrothermal synthesis for 72 hours to ensure that a silicon source in the synthetic liquid is fully utilized, wherein the synthesis temperature is 160 ℃.
(3) And after the hydrothermal synthesis is finished, pouring the synthetic liquid in the microwave reaction kettle into an evaporation container, evaporating and drying water in the synthetic liquid at high temperature, and grinding the solid particles agglomerated together to disperse the solid particles.
(4) The dried solid material is roasted for 3-4h in an ozone environment to prepare the required air purification material D4, and the set temperature is 300 ℃.
Comparative example 5
(1) Crushing amantadine into particles, putting the particles into a beaker, adding a proper amount of ethylenediamine and water, and then carrying out ultrasonic treatment on the particles for 15min by using an ultrasonic cell crusher, wherein the set frequency is 20kHz and the power is 900 w. And (3) placing the beaker into an ice-water mixture after ultrasonic treatment, adding a rotor after the beaker is cooled, and sequentially dropwise adding a proper amount of silica sol and H2PtCl4 solution under a stirring state. After the end of the dropwise addition, the beaker was heated to 90 ℃ with stirring and held for 30min to form amantadine: silicon source: noble metal sources: ethylene diamine: the water molar ratio is 47: 100: 10:400: 11240.
(2) Ball-milling pre-prepared DD3R molecular sieve particles (the particle size is 300 nm), adding the ball-milled particles into the synthetic solution according to the mass ratio of 0.5%, placing the synthetic solution into a microwave reaction kettle, and stirring under the microwave condition for hydrothermal synthesis for 72 hours to ensure that a silicon source in the synthetic solution is fully utilized, wherein the synthesis temperature is 160 ℃.
(3) And after the hydrothermal synthesis is finished, pouring the synthetic liquid in the microwave reaction kettle into an evaporation container, evaporating and drying water in the synthetic liquid at high temperature, and grinding the solid particles agglomerated together to disperse the solid particles.
(4) The dried solid material is roasted for 3-4h under the common high-temperature environment to prepare the required air purification material D5, and the set temperature is 700 ℃.
Comparative test
500mg of each of the air-purifying materials prepared in the above examples and comparative examples 1 to 3 was placed in a tubular fixed-bed reactor to conduct experiments, the atmosphere was protected at room temperature, a mixed contaminated gas (40% formaldehyde, 20% toluene, 20% xylene and 20% acetone) was bubbled through, nitrogen was blown into the reaction system, the concentration of formaldehyde at the inlet of the reactor was controlled to be 50mg/m3, the reaction space velocity (GHSV) was 30000mlg-1h-1, and the activity evaluation results are shown in Table 1.
TABLE 1 evaluation results of the purification Material
From the results of table 1, it can be seen that the purification composite material provided by the present invention has the best ability to purify formaldehyde in exhaust gas containing various pollutants.
The above description is for the purpose of illustrating embodiments of the invention and is not intended to limit the invention, and it will be understood by those skilled in the art that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. An air cleaning material, characterized in that the material comprises a formaldehyde decomposition layer at the upstream and an auxiliary adsorption layer at the downstream; the formaldehyde decomposition layer comprises a formaldehyde decomposition material for decomposing formaldehyde, and the auxiliary adsorption layer is used for adsorbing other polluting gases in the air; the formaldehyde decomposition material consists of DD3R molecular sieve and noble metal active component, and the mass of the molecular sieve is calculated by 100 percent of the weight of the catalystThe mass fraction is 90-95%, and the mass fraction of the noble metal active component is 5-10%; the auxiliary adsorption layer is selected from activated carbon, zeolite, molecular sieve or silica gel, and the formaldehyde decomposition layer also comprises a catalyst for CO in the gas flow2And/or a carbon dioxide adsorbing material for adsorbing carbon dioxide generated by formaldehyde decomposition; the carbon dioxide adsorbing material is composed of an amino functionalized porous material; the preparation method of the formaldehyde purification material comprises the following steps:
(1) mixing water, amantadine and a cosolvent, completely dissolving the amantadine through high-frequency ultrasonic treatment, dripping a silicon source and noble metal salt solution under the condition of ice bath stirring, and stirring and aging at high temperature to form amantadine: silicon source: noble metal sources: cosolvent: the water molar ratio is 30-50:100:5-20: 100-;
(2) adding the seed crystal prepared in advance into the synthetic liquid according to the mass ratio of 0.2-2%, placing the synthetic liquid into a microwave reaction kettle, and carrying out hydrothermal synthesis for 48-72h under the condition of microwave stirring, wherein the synthesis temperature is 150-180 ℃;
(3) after the hydrothermal synthesis is finished, pouring the synthetic liquid in the microwave reaction kettle into an evaporation container to evaporate water in the synthetic liquid and dry the solid material;
(4) and roasting the dried solid material for 3-4h in an ozone environment to prepare the required formaldehyde purification material.
2. The material of claim 1, wherein the noble metal is one or more of Pt, Pd, Au and Ag.
3. The material according to claim 1, wherein the formaldehyde decomposition layer and the auxiliary adsorption layer are spaced from each other by a distance of not less than 10 cm.
4. The material of claim 1, wherein the formaldehyde decomposition layer and the auxiliary absorbent layer are separable.
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