CN109603894B - Preparation method of formaldehyde purification material - Google Patents
Preparation method of formaldehyde purification material Download PDFInfo
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- CN109603894B CN109603894B CN201811637769.9A CN201811637769A CN109603894B CN 109603894 B CN109603894 B CN 109603894B CN 201811637769 A CN201811637769 A CN 201811637769A CN 109603894 B CN109603894 B CN 109603894B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J29/0325—Noble metals
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- 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
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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Abstract
The invention provides a preparation method of a formaldehyde purification material, which comprises 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 a catalyst. The invention selects the adsorption carrier of the noble metal active component, thereby ensuring that the adsorption carrier preferentially adsorbs and decomposes the formaldehyde in the gas, and ensuring the decomposition and purification rate of the formaldehyde.
Description
Technical Field
The application relates to a preparation method of an air purification material, in particular to a preparation method of a special purification material for formaldehyde containing various types of pollution gases at room temperature.
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
Aiming at the problems, the invention provides a purification material for purifying formaldehyde gas in indoor air, which solves the technical problem of low formaldehyde purification rate caused by competitive adsorption of various polluted gases on an adsorption material.
The invention provides a preparation method of a formaldehyde purification material, which 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.
Preferably, the calcination temperature is 300-400 ℃.
Preferably, the noble metal is one or more of Pt, Pd, Au and Ag.
Preferably, the cosolvent is ethylenediamine.
Preferably, the seed crystal is one of sigma-1, DD3R and ZSM-58.
Preferably, the dried solid material is ground prior to firing.
Preferably, the frequency of the high-frequency ultrasound is 20-25kHz, and the power is 500-1800 w.
Preferably, the seed crystal is molecular sieve particles without template removal.
The invention has the advantages that:
1. firstly, the invention adopts the all-silicon molecular sieve as the adsorption material, thereby avoiding the water generated by the decomposition of formaldehyde and the water molecules in the air from being absorbed by the molecular sieve, and reducing the possibility of catalyst deactivation.
2. Secondly, the DD3R molecular sieve is adopted as the adsorption material, and the diameter of the molecular sieve pore channel 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 and acetone, so that other polluted gases can be prevented from entering the DD3R pore channel to be adsorbed, and the relatively single adsorbability of the adsorption material to formaldehyde gas is ensured.
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.
4. For the DD3R molecular sieve adsorbing material, the synthesis method is optimized, such as ensuring the dissolution of amantadine by adopting a high-power high-frequency ultrasonic instrument, reducing the specific surface area of the material by adopting a microwave matching stirring mode and the like to ensure that the finally prepared material has excellent formaldehyde purification capacity.
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 formaldehyde purification material A, and the set temperature is 300 ℃.
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 formaldehyde 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 formaldehyde 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 formaldehyde 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 formaldehyde 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 in a common high-temperature environment to prepare the required formaldehyde purification material D5, and the set temperature is 700 ℃.
Comparative test
500mg of each of the purified materials prepared in the above examples and comparative examples 1 to 3 was placed in a tubular fixed bed reactor to conduct experiments, the protection was carried out at room temperature, a mixed contaminated gas (40% formaldehyde, 20% toluene, 20% xylene and 20% acetone) was bubbled through with nitrogen gas and 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 in table 1, it can be seen that the purifying material provided by the present invention has the best purifying ability for 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. The preparation method of the formaldehyde purification material is characterized by comprising 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) roasting the dried solid material for 3-4h in an ozone environment to prepare the required formaldehyde purification material; the roasting temperature is 300-400 ℃; the noble metal is one or more of Pt, Pd, Au and Ag; the frequency of the high-frequency ultrasonic wave is 20-25kHz, and the power is 500-1800 w.
2. The method of claim 1, wherein the co-solvent is ethylenediamine.
3. The method of claim 1, wherein the seed crystal is one of sigma-1, DD3R, and ZSM-58.
4. The method of claim 1, wherein the dried solid material is ground prior to firing.
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