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CN109589977A - One kind is for VOCs argentum-based catalyzer preparation method of degrading - Google Patents

One kind is for VOCs argentum-based catalyzer preparation method of degrading Download PDF

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CN109589977A
CN109589977A CN201811474307.XA CN201811474307A CN109589977A CN 109589977 A CN109589977 A CN 109589977A CN 201811474307 A CN201811474307 A CN 201811474307A CN 109589977 A CN109589977 A CN 109589977A
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agno
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丁辉
刘强
赵丹
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Tianjin University
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Abstract

本发明公开了一种用于降解VOCs银基催化剂制备方法，包括以下步骤：将活性炭纤维片浸泡在甲醇溶液，洗涤，烘干后浸泡在NaOH溶液，再烘干。将所得活性炭纤维片放入到(NH4)2C2O4·H2O与KMnO4的混合溶液中并添加盐酸调节混合体系pH，然后将混合体系置于恒温油浴锅中搅拌反应，反应完毕后将活性炭纤维片取出洗涤，烘干。将氨水溶液加入到AgNO3溶液中，并搅拌直到溶液变透明。将所得活性炭纤维片浸泡到透明溶液中并加入H2O2溶液，搅拌。最后将活性炭纤维取出，洗涤，烘干，煅烧获得Ag/MnO2‑ACF催化剂。本方法在实现较强VOCs吸附的同时，极大提高了VOCs的降解率以及矿化率，稳定性也增强。

The invention discloses a preparation method of a silver-based catalyst for degrading VOCs, comprising the following steps: soaking activated carbon fiber sheets in methanol solution, washing, drying, soaking in NaOH solution, and drying again. The obtained activated carbon fiber sheet is put into the mixed solution of (NH 4 ) 2 C 2 O 4 ·H 2 O and KMnO 4 and hydrochloric acid is added to adjust the pH of the mixed system, and then the mixed system is placed in a constant temperature oil bath to stir and react, After the reaction is completed, the activated carbon fiber sheet is taken out, washed, and dried. The aqueous ammonia solution was added to the AgNO3 solution and stirred until the solution became transparent. Soak the obtained activated carbon fiber sheet into the transparent solution and add the H2O2 solution , stirring. Finally, the activated carbon fibers are taken out, washed, dried, and calcined to obtain an Ag/MnO 2 -ACF catalyst. This method greatly improves the degradation rate and mineralization rate of VOCs while achieving strong VOCs adsorption, and the stability is also enhanced.

Description

One kind is for VOCs argentum-based catalyzer preparation method of degrading
Technical field
The invention belongs to catalyst technical fields, and in particular to one kind is for degrade VOCs argentum-based catalyzer and its preparation side Method.
Background technique
As air environmental pollution is got worse, there is a growing awareness that air environment prestige caused by human health The side of body, and VOCs, that is, volatile organic contaminant is a kind of very harmful pollutant in atmosphere, it not only can be with the coup injury mankind Respiratory mucosa causes surface skin allergy, and further secondary response forms photochemical fog and ozone pair in an atmosphere Human health causes bigger harm.The discharge of VOCs is included in Con trolling index by national departments concerned, therefore efficient The exploitation of VOCs degradation technique just seems more important.By using Ag/MnO2- ACF catalyst degradation VOCs is highest One of method of effect is translated into CO while efficient degradation realizes that VOCs content reduces again2And H2O realizes innoxious Discharge.
Most of effective catalyst is based on nano crystals catalyst now, and reaction temperature it is generally higher (110 DEG C with On), and noble metal catalyst is using more in loaded catalyst, since noble metal is expensive, industrial application is difficult, Noble metal utilisation is improved, while carrying out catalysis reaction under normal temperature conditions, realizes the economy and safety of catalytic degradation VOCs Property become important research direction.In Ag/MnO2Atom level is realized by reducing the size of Ag active site in-ACF catalyst Load, makes Ag active site high degree of dispersion, the utilization rate of precious metals ag, while MnO is improved while improving catalytic activity2 The carrier of the stronger adsorption function constituted with ACF carrier not only increases the monoatomic load stability of Ag, and plays and inhale The attached synergistic effect with catalysis greatly improves catalytic activity.
Ag/MnO2The stable dispersion of monatomic Ag and the vacancy of catalyst surface are closely related in-ACF catalyst, foundation Carrier surface vacancy is conducive to the realization of monatomic steady load.Tang Xingfu seminar etc. carries out to silver nano-grain catalyst Discovery catalysis reaction occurs mainly in the neighboring atom of carrier and metal contact during research, reduces the partial size pair of noble metal It is very desirable in improving metallic atom utilization rate.Long Liping etc. uses NiO/AL respectively2O3、CoO/AL2O3、MnO2/ AL2O3、Fe2O3/AL2O3And CuO/AL2O3Its O3 catalytic oxidation toluene performance is probed into, catalytic performance is best under normal temperature conditions The degradation of toluene rate of catalyst be only 40%.Si Macong etc. uses Cu-Mn-Ce-O/ γ-AL2O3Catalyst is in 110-130 DEG C decline solution toluene in certain ozone concentration, toluene conversion is up to 83.9%.Nm-class catalyst still remains under normal low temperature The lower disadvantage of catalytic performance.The size for reducing active site, can not only improve the utilization rate of noble metal, while also to a certain degree On improve catalytic activity.MinLi etc. loads TiO2In in activated carbon fibre, under ultraviolet light conditions, the height of toluene is realized Effect degradation.But article of the monatomic steady load on activated carbon fibre (ACF) be yet there are no into relevant report.
Summary of the invention
The purpose of the present invention is to overcome the disadvantages of the prior art, provides a kind of preparation of catalyst for VOCs degradation Method, this method be not only able to achieve efficient degradation VOCs at normal temperature, but also can give full play to noble metal utilisation and realize monatomic bear A possibility that carrying, enhancing catalyst industrial application.
The technical proposal for solving the technical problem of the invention are as follows:
A kind of preparation method of catalyst for VOCs degradation of the invention, comprising the following steps:
(1) activated carbon fibre piece is immersed in concentration is 0.1-0.2mol/L methanol solution 3-5min, uses deionization later Water cleans 3-5min and removes the possible residue in surface, and taking-up is put into beaker and is placed in 55-65 DEG C of baking oven 20-30min, further takes out and put Enter 2-3min in the NaOH solution that concentration is 0.5-1mol/L, then the activated carbon fibre piece for speckling with NaOH solution is placed into beaker In, it is placed in 100-120 DEG C of baking oven and heats the hydrolysis that 30-40min promotes activated carbon fibre surface；
(2) taking mass ratio is (1-1.5): 4 (NH4)2C2O4·H2O and KMnO4It is molten to be dissolved in formation mixing in deionized water Liquid, the KMnO4Solid-to-liquid ratio with deionized water is (0.015g-0.020g): 1ml；
Activated carbon fibre piece obtained by step (1), which will be put into mixed solution, and adds 0.2-0.5mol/L hydrochloric acid to mix The pH of system is adjusted to 7-7.3, then mixed system is placed in the stirring in 90-110 DEG C of thermostatical oil bath with 140-160rpm Speed is stirred to react 9-11h, and the taking-up of activated carbon fibre piece is washed with deionized 3-5 times after completion of the reaction, is put into 60-80 DEG C Baking oven in dry 40-60min；The activated carbon fibre piece and KMnO4Mass ratio be 1:(0.3-0.6)；
(3) ammonia spirit that mass fraction is 25%-30% is slowly added into AgNO3In solution, and stir until molten Liquid bleach；The AgNO3AgNO in solution3It is (0.005-0.010) with taken activated carbon fibre tablet quality ratio in step (1): 1；
(4) H for being 30-35% by mass fraction2O2Solution is added in step (3) in clear solution and soaking step (2) Gained activated carbon fiber piece stirs 30-40min at 0-10 DEG C, finally filters mixture in beaker, by filtrate deionization Water cleans 3-5 times, the H2O2H in solution2O2With AgNO3Mass ratio (1.5-2): 1；
(5) filtrate dry 10-12h at 60-80 DEG C is obtained later by it in 300-400 DEG C of calcining 3-5h after washing Obtain Ag/MnO2-ACF。
The invention has the benefit that in Ag/MnO2It is realized in-ACF catalyst by reducing the size of Ag active site Atom level load, makes Ag active site high degree of dispersion, the utilization rate of precious metals ag is improved while improving catalytic activity, together When MnO2The carrier of the stronger adsorption function constituted with ACF carrier not only increases the monoatomic load stability of Ag, and The synergistic effect for playing absorption and catalysis greatly improves catalytic activity.
Detailed description of the invention
Fig. 1 is present invention preparation Ag/MnO2- ACF catalyst process schematic diagram.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
The present invention prepares reaction equation about the monatomic catalyst of Ag/Mn2-ACF:
KMnO4+(NH4)2C2O4·H2O+-OH→MnO2-
NH3·H2O+AgNO3→Ag(NH3)2OH+H2O
Ag(NH3)2OH+H2O2+MnO2-→AgMnO2-
There are also hydroxyl groups abundant in activated carbon fibre (ACF), can be formed by potassium permanganate oxidation and ACF is with chemical bond Connected MnO2, and then with MnO2As young brilliant, promote in the liquid phase potassium permanganate the MnO to be formed is reacted with ammonium oxalate2Stablize The surface ACF is formed with the MnO compared with multi-hole2- ACF carrier, so using anti-Ostwald method by Ag it is monatomic you load to MnO2On-ACF carrier, to obtain monatomic Ag/MnO2- ACF catalyst.
Based on principles above, a kind of preparation method of catalyst for VOCs absorption degradation of the invention, including it is following Step:
(1) activated carbon fibre piece is immersed in concentration is 0.1-0.2mol/L methanol solution 3-5min, uses deionization later Water cleans 3-5min and removes the possible residue in surface, and taking-up is put into beaker and is placed in 55-65 DEG C of baking oven 20-30min, further takes out and put Enter 2-3min in the NaOH solution that concentration is 0.5-1mol/L, then the activated carbon fibre piece for speckling with NaOH solution is placed into beaker In, it is placed in 100-120 DEG C of baking oven and heats the hydrolysis that 30-40min promotes activated carbon fibre surface.
(2) taking mass ratio is (1-1.5): 4 (NH4)2C2O4·H2O and KMnO4It is molten to be dissolved in formation mixing in deionized water Liquid, the KMnO4Solid-to-liquid ratio with deionized water is (0.015g-0.020g): 1ml.By activated carbon fibre piece obtained by step (1) It is put into mixed solution and adds 0.2-0.5mol/L hydrochloric acid and adjust the pH of mixed system to 7-7.3, then by mixture It is that the mixing speed being placed in 90-110 DEG C of thermostatical oil bath with 140-160rpm is stirred to react 9-11h, will lives after completion of the reaction Property Carbon fibe piece taking-up be washed with deionized 3-5 time, be put into 60-80 DEG C of baking oven dry 40-60min.The active carbon Fibre plate and KMnO4Mass ratio be 1:(0.3-0.6).
(3) ammonia spirit that mass fraction is 25%-30% is slowly added into AgNO3In solution, and stir until molten Liquid bleach.The AgNO3AgNO in solution3It is (0.005-0.010) with taken activated carbon fibre tablet quality ratio in step (1): 1。
(4) H for being 30-35% by mass fraction2O2Solution is added in step (3) in clear solution and soaking step (2) Gained activated carbon fiber piece stirs 30-40min at 0-10 DEG C, finally filters mixture in beaker, by filtrate deionization Water cleans 3-5 times, the H2O2H in solution2O2With AgNO3Mass ratio (1.5-2): 1.
(5) filtrate dry 10-12h at 60-80 DEG C is obtained later by it in 300-400 DEG C of calcining 3-5h after washing Obtain Ag/MnO2-ACF。
Embodiment 1
(1) 0.1g activated carbon fibre piece is immersed in concentration is 0.1mol/L methanol solution 3min, uses deionized water later It cleans 3min and removes the possible residue in surface, taking-up is put into beaker and is placed in 55 DEG C of baking oven 20min, further takes out and is put into concentration and is 2min in the NaOH solution of 0.5mol/L, then the activated carbon fibre piece for speckling with NaOH solution is placed in beaker, it is placed in 100 DEG C The hydrolysis that 30min promotes activated carbon fibre surface is heated in baking oven.
(2) taking mass ratio is the (NH of 1:44)2C2O4·H2O and KMnO4It is dissolved in deionized water and forms mixed solution, it is described KMnO4Solid-to-liquid ratio with deionized water is 0.015g:1ml.Activated carbon fibre piece obtained by step (1) is put into mixed solution And add 0.2mol/L hydrochloric acid and adjust the pH of mixed system to 7, then by mixed system be placed in 90 DEG C of thermostatical oil baths with The mixing speed of 140rpm is stirred to react 9h, and the taking-up of activated carbon fibre piece is washed with deionized 3 times after completion of the reaction, is put into Dry 40min in 60 DEG C of baking oven.The activated carbon fibre piece and KMnO4Mass ratio be 1:0.3.
(3) ammonia spirit that mass fraction is 25% is slowly added into AgNO3In solution, and stir until solution becomes saturating It is bright.The AgNO3AgNO in solution3It is 0.005:1 with taken activated carbon fibre tablet quality ratio in step (1).
(4) H for being 30% by mass fraction2O2Solution is added in step (3) in clear solution and soaking step (2) institute Activated carbon fiber piece is obtained, 30min is stirred at 0 DEG C, finally mixture in beaker is filtered, filtrate is cleaned 3 with deionized water It is secondary, the H2O2H in solution2O2With AgNO3Mass ratio 1.5:1.
(5) filtrate dry 10h at 60 DEG C, obtains Ag/MnO in 300 DEG C of calcining 3h for it later after washing2- ACF is denoted as A.
Embodiment 2
(1) 0.1g activated carbon fibre piece is immersed in concentration is 0.15mol/L methanol solution 4min, uses deionized water later It cleans 4min and removes the possible residue in surface, taking-up is put into beaker and is placed in 60 DEG C of baking oven 25min, further takes out and is put into concentration and is 2.5min in the NaOH solution of 0.8mol/L, then the activated carbon fibre piece for speckling with NaOH solution is placed in beaker, it is placed in 110 DEG C Baking oven in heating 35min promote activated carbon fibre surface hydrolysis.
(2) taking mass ratio is the (NH of 1.2:44)2C2O4·H2O and KMnO4It is dissolved in deionized water and forms mixed solution, institute State KMnO4Solid-to-liquid ratio with deionized water is 0.018:1ml.Activated carbon fibre piece obtained by step (1) is put into mixed solution In and add 0.3mol/L hydrochloric acid and adjust the pH of mixed system to 7.2, mixed system is then placed in 100 DEG C of thermostatical oil baths In 10h is stirred to react with the mixing speed of 150rpm, the taking-up of activated carbon fibre piece is washed with deionized 4 after completion of the reaction It is secondary, dry 50min is put into 70 DEG C of baking oven.The activated carbon fibre piece and KMnO4Mass ratio be 1:0.4.
(3) ammonia spirit that mass fraction is 28% is slowly added into AgNO3In solution, and stir until solution becomes saturating It is bright.The AgNO3AgNO in solution3It is 0.008:1 with taken activated carbon fibre tablet quality ratio in step (1).
(4) H for being 33% by mass fraction2O2Solution is added in step (3) in clear solution and soaking step (2) institute Activated carbon fiber piece is obtained, 35min is stirred at 5 DEG C, finally mixture in beaker is filtered, filtrate is cleaned 4 with deionized water It is secondary, the H2O2H in solution2O2With AgNO3Mass ratio 1.8:1.
(5) filtrate dry 11h at 70 DEG C, obtains Ag/MnO in 350 DEG C of calcining 4h for it later after washing2- ACF is denoted as B.
Embodiment 3
(1) 0.1g activated carbon fibre piece is immersed in concentration is 0.2mol/L methanol solution 5min, uses deionized water later It cleans 5min and removes the possible residue in surface, taking-up is put into beaker and is placed in 65 DEG C of baking oven 30min, further takes out and is put into concentration and is 3min in the NaOH solution of 1mol/L, then the activated carbon fibre piece for speckling with NaOH solution is placed in beaker, it is placed in 120 DEG C of baking The hydrolysis that 40min promotes activated carbon fibre surface is heated in case.
(2) taking mass ratio is the (NH of 1.5:44)2C2O4·H2O and KMnO4It is dissolved in deionized water and forms mixed solution, institute State KMnO4Solid-to-liquid ratio with deionized water is 0.020g:1ml.Activated carbon fibre piece obtained by step (1) is put into mixed solution In and add 0.5mol/L hydrochloric acid and adjust the pH of mixed system to 7.3, mixed system is then placed in 110 DEG C of thermostatical oil baths In 11h is stirred to react with the mixing speed of 160rpm, the taking-up of activated carbon fibre piece is washed with deionized 5 after completion of the reaction It is secondary, dry 60min is put into 80 DEG C of baking oven.The activated carbon fibre piece and KMnO4Mass ratio be 1:0.6.
(3) ammonia spirit that mass fraction is 30% is slowly added into AgNO3In solution, and stir until solution becomes saturating It is bright.The AgNO3AgNO in solution3It is 0.010:1 with taken activated carbon fibre tablet quality ratio in step (1).
(4) H for being 35% by mass fraction2O2Solution is added in step (3) in clear solution and soaking step (2) institute Activated carbon fiber piece is obtained, 40min is stirred at 10 DEG C, finally mixture in beaker is filtered, filtrate is cleaned 5 with deionized water It is secondary, the H2O2H in solution2O2With AgNO3Mass ratio 2:1.
(5) filtrate dry 12h at 80 DEG C, obtains Ag/MnO in 400 DEG C of calcining 5h for it later after washing2- ACF is denoted as C.
The catalyst of embodiment 1,2,3 is fitted into catalytic evaluation device, for the adsoption catalysis degradation reaction of toluene, Reaction condition is that toluene is 500ppm, and reaction temperature is 65 DEG C, reaction velocity 8000h-1.Catalytic activity is shown in Table 1.
Table 1
, it can be seen that Ag/MnO prepared by the present invention from table 12- ACF catalyst, degradation of toluene rate with higher With mineralization rate.
Although the embodiments of the present invention has been shown and described above, but the invention is not limited to above-mentioned specific Embodiment, the above mentioned embodiment is only schematical, rather than restrictive, and technology belonging to the present invention is led For the those of ordinary skill in domain, without departing from the inventive concept of the premise, several simple deductions can also be made or replaced It changes, all shall be regarded as belonging to the present invention by the claims submitted and determine scope of patent protection.

Claims (1)

1.一种用于VOCs降解的催化剂的制备方法，其特征在于包括以下步骤：1. a preparation method for the catalyst of VOCs degradation is characterized in that comprising the following steps: (1)将活性炭纤维片浸泡在浓度为0.1-0.2mol/L甲醇溶液3-5min，之后用去离子水清洗3-5min去除表面可能的残留物，取出放入烧杯置于55-65℃烘箱20-30min,再取出放入浓度为0.5-1mol/L的NaOH溶液中2-3min，再将沾有NaOH溶液的活性炭纤维片放置烧杯中，置于100-120℃的烘箱中加热30-40min促进活性炭纤维表面的水解；(1) Soak the activated carbon fiber sheet in methanol solution with a concentration of 0.1-0.2mol/L for 3-5min, then wash it with deionized water for 3-5min to remove possible residues on the surface, take it out and put it in a beaker and place it in an oven at 55-65℃ 20-30min, then take it out and put it in a NaOH solution with a concentration of 0.5-1mol/L for 2-3min, then place the activated carbon fiber sheet stained with the NaOH solution in a beaker and heat it in an oven at 100-120℃ for 30-40min Promote the hydrolysis of activated carbon fiber surface; (2)取质量比为(1-1.5):4的(NH4)2C2O4·H2O与KMnO4溶于去离子水中形成混合溶液，所述KMnO4与去离子水的固液比为(0.015g-0.020g):1ml；将步骤(1)所得活性炭纤维片放入到混合溶液中并添加0.2-0.5mol/L盐酸将混合体系的pH调节到7-7.3，然后将混合体系置于90-110℃恒温油浴锅中以140-160rpm的搅拌速度搅拌反应9-11h，反应完毕后将活性炭纤维片取出用去离子水洗涤3-5次，放入60-80℃的烘箱中干燥40-60min；所述活性炭纤维片与KMnO4的质量比为1:(0.3-0.6)；(2) Dissolve (NH 4 ) 2 C 2 O 4 ·H 2 O and KMnO 4 in deionized water with a mass ratio of (1-1.5):4 to form a mixed solution, and the solid state of the KMnO 4 and deionized water The liquid ratio is (0.015g-0.020g): 1ml; the activated carbon fiber sheet obtained in step (1) is put into the mixed solution and 0.2-0.5mol/L hydrochloric acid is added to adjust the pH of the mixed system to 7-7.3, and then the The mixing system was placed in a constant temperature oil bath at 90-110 °C and stirred for 9-11 hours at a stirring speed of 140-160 rpm. After the reaction was completed, the activated carbon fiber sheet was taken out and washed with deionized water for 3-5 times. Dry 40-60min in the drying oven; The mass ratio of described activated carbon fiber sheet and KMnO is 1 :(0.3-0.6); (3)将质量分数为25％-30％的氨水溶液缓慢加入到AgNO3溶液中，并搅拌直到溶液变透明；所述AgNO3溶液中AgNO3与步骤(1)中所取活性炭纤维片质量比为(0.005-0.010):1；(3) The ammonia solution with a mass fraction of 25%-30% is slowly added to the AgNO 3 solution, and stirred until the solution becomes transparent; the AgNO 3 in the AgNO 3 solution is the same as the mass of the activated carbon fiber sheet taken in step (1). The ratio is (0.005-0.010):1; (4)将质量分数为30-35％的H2O2溶液加入到步骤(3)中透明溶液中并浸泡步骤(2)所得活性碳纤维片，0-10℃下搅拌30-40min,最后将烧杯中混合物过滤，将过滤物用去离子水清洗3-5次，所述H2O2溶液中H2O2与AgNO3的质量比(1.5-2):1；(4) adding the H 2 O 2 solution with a mass fraction of 30-35% into the transparent solution in step (3) and soaking the activated carbon fiber sheet obtained in step (2), stirring at 0-10 ° C for 30-40 min, and finally adding The mixture in the beaker is filtered, and the filtrate is washed 3-5 times with deionized water, and the mass ratio of H 2 O 2 to AgNO 3 in the H 2 O 2 solution is (1.5-2): 1; (5)将洗涤后过滤物在60-80℃下干燥10-12h,之后将其在300-400℃煅烧3-5h，获得Ag/MnO2-ACF。(5) The washed filtrate was dried at 60-80° C. for 10-12 h, and then calcined at 300-400° C. for 3-5 h to obtain Ag/MnO 2 -ACF.
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