CN105013322B - A kind of manganese oxide catalyst is used for the purposes of catalysis oxidation formaldehyde - Google Patents

A kind of manganese oxide catalyst is used for the purposes of catalysis oxidation formaldehyde Download PDF

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CN105013322B
CN105013322B CN201510359133.2A CN201510359133A CN105013322B CN 105013322 B CN105013322 B CN 105013322B CN 201510359133 A CN201510359133 A CN 201510359133A CN 105013322 B CN105013322 B CN 105013322B
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formaldehyde
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oxide
manganese dioxide
catalysis oxidation
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CN105013322A (en
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贺泓
张江浩
张长斌
李要彬
王莲
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Research Center for Eco Environmental Sciences of CAS
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Abstract

The invention provides the purposes that a kind of manganese oxide catalyst is used for catalysis oxidation formaldehyde, the Mn oxide is the manganese dioxide of γ or/and δ crystal formations.The present invention has to be had the following advantages that using the manganese dioxide of δ crystal formations as catalyst oxidation of formaldehyde:(1) initiation temperature of catalysis oxidation formaldehyde is low, conversion ratio at high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)) at 50 DEG C has reached 37%, converted completely at 80 DEG C, its activity is located at prostatitis in non-precious metal catalyst;(2) its crystal formation keeps stable before and after excellent in stability, one side catalytic reaction, and another aspect catalytic conversion keeps constant in long-time active testing.

Description

A kind of manganese oxide catalyst is used for the purposes of catalysis oxidation formaldehyde
Technical field
The invention belongs to formaldehyde catalysis technical field, and in particular to a kind of manganese oxide catalyst is used for catalysis oxidation formaldehyde Purposes.
Background technology
Formaldehyde has as adhesive strengthens artificial floor hardness, insect prevention, corrosion-resistant function, thus is widely used in house Tool and finishing material.On the other hand, formaldehyde can be also gradually released in surrounding environment from adhesive, and this just result in Interior Space The severe contamination of gas.The testing result of Chinese Indoor Environment Detection Working Committee of interior decoration association is also indicated that:Formaldehyde is Repaired the house as Chinese new clothes interior major pollutants.For a long time in the formaldehyde gas of certain content, gently it can then stimulate The organs such as eye, nose, larynx, it is heavy then cause fatigue and allergic reaction, or even trigger tumour, be detrimental to health.Thus, for formaldehyde The exploration of efficient minimizing technology is very urgent with studying.
At present, removing the method for indoor formaldehyde mainly has photocatalysis method, plasma decomposition, absorption method and catalysis oxygen Change method.Wherein formaldehyde exhaustive oxidation even under room temperature condition can be carbon dioxide and water, nothing in low temperature by catalysed oxidation processes Light requirement shines or plasma excites catalyst, the limitation that also saturation without adsorbent is adsorbed, thus breaches first three side Many limitations of method.The catalyst for removing formaldehyde at present is mainly loaded noble metal catalyst and transition metal oxide catalysis Agent, noble metal catalyst can remove formaldehyde completely in room temperature, but expensive, and this causes to grind transition metal oxide The gradually attention studied carefully.
The method that CN 103691461A disclose a kind of golden hydroxyapatite catalyst of application load, with calcium nitrate and phosphorus Sour diammonium hydrogen is presoma, and carrier hydroxyapatite is obtained using liquid phase deposition;Using gold chloride as presoma, with hydroxy-apatite Stone is carrier, using Powder by Homogenous Precipitation, prepares gold-supported hydroxyapatite catalyst.The catalyst can be urged at room temperature Change and remove formaldehyde, but it is gold that its shortcoming, which is active material, its price changes obstruction the commercial applications of catalyst.
CN 103962163A disclose the preparation method of transient metal doped hydroxyapatite and its catalysis oxygen of PARA FORMALDEHYDE PRILLS(91,95) Change, this method step is simple, the cycle is short, but compared to noble metal catalyst, its catalytic activity is not high.Thus study high activity Catalysis oxidation formaldehyde non-precious metal catalyst by with far-reaching realistic meaning.
Prior art (Tian Hua, He Junhui, the progress of manganese oxide catalysis oxidation formaldehyde, chemistry circular 2013 the 76th Rolled up for the 2nd phase, page 100~106) manganese dioxide of α and beta crystal is only disclosed for purifying formaldehyde.They are in high load capacity, i.e. height The high concentration of formaldehyde condition of air speed (100000mL/ (gh) and 170ppm) under remove formaldehyde completely needed for temperature it is high, it is impossible to meet Practical application.
The content of the invention
Based on this, it is an object of the invention to provide a kind of method of catalysis oxidation formaldehyde, methods described is using the not isomorphous The Mn oxide of type realizes the efficient oxidation of formaldehyde as catalyst.
In order to achieve the above object, present invention employs following technical scheme:
A kind of manganese oxide catalyst is used for the purposes of catalysis oxidation formaldehyde, and the Mn oxide is γ or/and δ crystal formations Manganese dioxide.
Preferably, in the present invention, the Mn oxide is the manganese dioxide of δ crystal formations.The present invention is by using δ crystal formations Manganese dioxide be used for catalysis oxidation formaldehyde, with high conversion rate and the low advantage of catalytic temperature, shown at 50 DEG C compared with High catalytic activity, its still shown under high concentration (170ppm) high-speed (100000mL/ (gh)) test condition compared with High catalytic conversion, still can be achieved complete (100%) conversion of formaldehyde at 80 DEG C.
Preferably, in the present invention, during catalysis oxidation formaldehyde, the initial concentration of formaldehyde is 0-170ppm and not included 0, such as 10ppm, 30ppm, 50ppm, 70ppm, 90ppm, 110ppm, 130ppm, 150ppm or 170ppm.Using the present invention's The manganese dioxide of δ crystal formations, it is possible to achieve formaldehyde 100% is converted when 80 DEG C of (up to 170ppm) under high concentration.
Preferably, in the present invention, during catalysis oxidation formaldehyde, air speed is 0-100000mL/ (gh) and not included 0, the air speed is, for example, 100000mL/ (gh).Using the manganese dioxide of the δ crystal formations of the present invention, it is possible to achieve under high-speed Formaldehyde 100% is converted when 80 DEG C of (100000mL/ (gh)).
In the present invention, during catalysis oxidation formaldehyde, the consumption of Mn oxide is any amount.
Preferably, the manganese dioxide of the δ crystal formations is using manganese sulfate as reducing agent, and potassium permanganate or ammonium persulfate are oxidation Agent, is synthesized using hydro-thermal method, specific as follows:
Oxidant, reducing agent and deionized water needed for being added in hydrothermal reaction kettle, make oxidant by stirring and go back Former agent is thoroughly dissolved, and is then placed in 200~240 DEG C of insulating box and is reacted, and material in reactor is filtered, washed by reaction after terminating Wash and dry, be calcined in atmosphere afterwards.
The present invention by using specific 200~240 DEG C of hydrothermal temperature (such as 205 DEG C, 210 DEG C, 215 DEG C, 220 DEG C, 225 DEG C, 230 DEG C or 235 DEG C) prepare the manganese dioxide of δ crystal formations, so as to get the manganese dioxide of δ crystal formations there is excellent first Aldehyde catalytic activity, and still show under high concentration (170ppm) high-speed (100000mL/ (gh)) test condition higher Catalytic activity, still can 80 DEG C i.e. can be achieved formaldehyde complete (100%) conversion.
Preferably, be placed in 200~240 DEG C of insulating box reaction 18~30h, such as 19h, 20h, 21h, 22h, 23h, 24h, 25h, 26h, 27h, 28h or 29h, preferably 24h.Catalyst can not form sufficient δ crystal formations when time is less than 18h, be higher than 30h can then cause the waste of heat.
Preferably, the drying time be 12~24h, such as 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h or 23h.
Preferably, the temperature of the roasting be 300~450 DEG C, such as 310 DEG C, 320 DEG C, 330 DEG C, 340 DEG C, 350 DEG C, 360 DEG C, 370 DEG C, 380 DEG C, 390 DEG C, 400 DEG C, 410 DEG C, 420 DEG C, 430 DEG C or 440 DEG C.Sintering temperature is less than 300 DEG C, catalysis Agent can not be in substantially stabilized state, and higher than 450 DEG C, then easily cause Ag sintering.Roasting time is 3-6 hours, for example 3.3h, 3.6h, 3.9h, 4.2h, 4.5h, 4.8h, 5.1h, 5.4h or 5.7h, less than 3h, catalyst can not be calcined, and high Production cost is then easily sintered and increases in 6h.
Preferably, the active component elemental silver of the Mn oxide area load.Load active component elemental silver, Ke Yixian Write the catalytic activity that ground improves catalyst.
Preferably, the mass percent that the active component elemental silver accounts for the quality sum of silver and Mn oxide is 2- 10%, such as 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%, preferably 8%.
Present invention also offers a kind of method of catalysis oxidation formaldehyde, methods described uses the manganese dioxide conduct of δ crystal formations Catalyst.Preferably, under the conditions of high concentration (concentration of formaldehyde 170ppm) high-speed (100000mL/ (gh)), it is catalyzed Oxidation of formaldehyde.Under the concentration and space velocities, complete (100%) conversion of formaldehyde can be achieved at 80 DEG C.That is, it is dense in formaldehyde When degree 170ppm, air speed are 100000mL/ (gh) and temperature is 80 DEG C, formaldehyde 100% is converted completely.Further preferably Ground, the manganese dioxide of the δ crystal formations is using manganese sulfate as reducing agent, and potassium permanganate or ammonium persulfate are oxidant, using hydro-thermal method Synthesis, it is specific as follows:Oxidant, reducing agent and deionized water needed for being added in hydrothermal reaction kettle, make oxidation by stirring Agent and reducing agent thoroughly dissolve, and are then placed in 200~240 DEG C of insulating box and react, and react material in reactor after terminating It is filtered, washed and dried, is calcined in atmosphere afterwards.18 are reacted it is further preferred that being placed in 200~240 DEG C of insulating box ~30h, such as 19h, 20h, 21h, 22h, 23h, 24h, 25h, 26h, 27h, 28h or 29h, preferably 24h.When time is less than 18h Catalyst can not form sufficient δ crystal formations, and the waste of heat can be then caused higher than 30h.It is further preferred that the temperature of the roasting Spend for 300~450 DEG C, such as 310 DEG C, 320 DEG C, 330 DEG C, 340 DEG C, 350 DEG C, 360 DEG C, 370 DEG C, 380 DEG C, 390 DEG C, 400 DEG C, 410 DEG C, 420 DEG C, 430 DEG C or 440 DEG C.Sintering temperature is less than 300 DEG C, and catalyst can not be in substantially stabilized state, and high In 450 DEG C, then Ag sintering is easily caused.Roasting time be 3-6 hours, such as 3.3h, 3.6h, 3.9h, 4.2h, 4.5h, 4.8h, 5.1h, 5.4h or 5.7h, less than 3h, catalyst can not be calcined, and then easily sintering and increase are produced into higher than 6h This.It is further preferred that the active component elemental silver of Mn oxide area load.Load active component elemental silver, can be with Significantly increase the catalytic activity of catalyst.Preferably, the active component elemental silver accounts for the quality sum of silver and Mn oxide Mass percent be 2-10%, such as 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%, preferably 8%.
The present invention by using specific 200~240 DEG C of hydrothermal temperature (such as 205 DEG C, 210 DEG C, 215 DEG C, 220 DEG C, 225 DEG C, 230 DEG C or 235 DEG C) prepare the manganese dioxide of δ crystal formations, so as to get the manganese dioxide of δ crystal formations there is excellent first Aldehyde catalytic activity, and still show under high concentration (170ppm) high-speed (100000mL/ (gh)) test condition higher Catalytic activity, still can 80 DEG C i.e. can be achieved formaldehyde complete (100%) conversion.
Compared with the prior art, the present invention has is had using the manganese dioxide of δ crystal formations as catalyst oxidation of formaldehyde Have the following advantages:
(1) initiation temperature of catalysis oxidation formaldehyde is low, high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100, 000mL/ (gh)) when 50 DEG C at conversion ratio reached and converted completely at 37%, 80 DEG C that it is lived in non-precious metal catalyst Property be located at prostatitis;
(2) its crystal formation keeps stable before and after excellent in stability, one side catalytic reaction, and another aspect catalytic conversion is in length Keep constant in time (50h) active testing, in concentration 170ppm, air speed 100,000mL/ (gh), during 80 DEG C of temperature, all the time Maintain 100% conversion ratio, in concentration 170ppm, more high-speed 150,000mL/ (gh) under the conditions of 75 DEG C of temperature, is tieed up all the time Hold 60% conversion ratio;
(3) nontoxic component is used, the harm to health and ecological environment is reduced, preparation process is simple and easy to apply, into This is cheap, easily realizes industrialization.
Embodiment
Technical scheme is further illustrated below by embodiment.
Embodiment 1
α, the manganese dioxide of β, γ and δ crystal formation are prepared using method as follows:
Using manganese sulfate as reducing agent, potassium permanganate or ammonium persulfate are oxidant, and α is obtained using hydro-thermal method is synthetically prepared, The manganese dioxide-catalyst of β, γ and δ crystal formation, it is specific as follows:
Precursor (i.e. Oxidizing and Reducing Agents) (X) and 80mL needed for being added in 100mL hydrothermal reaction kettle go from Sub- water, makes precursor thoroughly dissolve, certain time is reacted in the insulating box for being then placed in certain reaction temperature (Y) by stirring (Z), then material in reactor is filtered, wash, is dried overnight, afterwards with being calcined in air 300 DEG C.Following table is classified as X, Y, Z particular value.
X Y Z
α-MnO2 MnSO4·H2O+KMnO4 160℃ 24h
β-MnO2 MnSO4·H2O+(NH4)2S2O8 140℃ 12h
γ-MnO2 MnSO4·H2O+(NH4)2S2O8 90℃ 24h
δ-MnO2 MnSO4·H2O+KMnO4 200-240℃ 24h
In four kinds of manganese dioxide, the activity of δ crystal formations manganese dioxide catalysis formaldehyde exhaustive oxidation is far above other crystal formations, exhibition Its huge crystal formation advantage is shown.The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table, according to work Property is arranged from high to low.Test condition:Concentration 170ppm, air speed 100,000mL/ (gh).
Embodiment 2
Use and prepare α, the manganese dioxide of β, γ and δ crystal formation in the identical method of embodiment 1.
In concentration 170ppm, air speed 150,000mL/ (gh), under the conditions of 75 DEG C of temperature, the manganese dioxide of δ crystal formations can be with The conversion ratio of maintenance 60% is constant within the 50h times, and α, β, γ are tested under similarity condition, and its activity is gradually reduced from after 5h.
Embodiment 3
α, the manganese dioxide of β, γ and δ crystal formation are prepared using method same as Example 1.
The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table, and is arranged from high to low according to activity Row.Test condition:Concentration 5ppm, air speed 5000mL/ (gh).
Comparative example 1
The manganese dioxide that δ crystal formations are prepared in the identical method of embodiment 1 is used, in addition to hydrothermal temperature is 180 DEG C.
Comparative example 2
The manganese dioxide that δ crystal formations are prepared in the identical method of embodiment 1 is used, in addition to hydrothermal temperature is 260 DEG C.
Under high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)), test comparison example 1 and right The catalytic activity of the catalyst of ratio 2, as a result shows:
The catalyst of comparative example 1 realizes that formaldehyde 50% is converted at 75 DEG C, and 110 DEG C are realized that formaldehyde 100% is converted, comparative example 2 Catalyst realize that formaldehyde 50% is converted at 80 DEG C, realize that formaldehyde 100% is converted at 125 DEG C.
Embodiment 4
Use with the manganese dioxide of identical method α, β, γ and δ crystal formation of embodiment 1, and loaded on the manganese dioxide Active component silver, silver mass fraction 8wt%.
Under the high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)), testing example 4 is urged The catalytic activity of agent.The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table.Test condition:It is dense Spend 170ppm, air speed 100,000mL/ (gh).
Embodiment 5
Remaining is same as Example 4, except silver mass fraction is 2wt%.
Under the high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)), testing example 5 is urged The catalytic activity of agent.The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table.Test condition:It is dense Spend 170ppm, air speed 100,000mL/ (gh).
Embodiment 6
Remaining is same as Example 4, except silver mass fraction is 10wt%.
Under the high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)), testing example 6 is urged The catalytic activity of agent.The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table.Test condition:It is dense Spend 170ppm, air speed 100,000mL/ (gh).
Applicant states that the present invention illustrates the method detailed of the present invention, but not office of the invention by above-described embodiment It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implemented.Art Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and being open.

Claims (8)

1. a kind of manganese oxide catalyst is used for the purposes of catalysis oxidation formaldehyde, the Mn oxide is the manganese dioxide of δ crystal formations;
The manganese dioxide of the δ crystal formations is using manganese sulfate as reducing agent, and potassium permanganate or ammonium persulfate are oxidant, using hydro-thermal method Synthesis, it is specific as follows:
Oxidant, reducing agent and deionized water needed for being added in hydrothermal reaction kettle, make Oxidizing and Reducing Agents by stirring Thoroughly dissolving, is then placed in 18~30h of reaction in 200~240 DEG C of insulating box, reacts material mistake in reactor after terminating Filter, wash and dry, be calcined in atmosphere afterwards;
The temperature of the roasting is 300~450 DEG C, and roasting time is 3~6h.
2. purposes as claimed in claim 1, it is characterised in that during catalysis oxidation formaldehyde, the initial concentration of formaldehyde is 0- 170ppm and not include 0.
3. purposes as claimed in claim 1, it is characterised in that during catalysis oxidation formaldehyde, air speed is 0-100000mL/ (gh) 0 and is not included.
4. purposes as claimed in claim 1, it is characterised in that react 24h in the insulating box for being placed in 200~240 DEG C.
5. purposes as claimed in claim 1, it is characterised in that the drying time is 12~24h.
6. the purposes as described in one of claim 1-5, it is characterised in that the active component list of Mn oxide area load Matter silver.
7. purposes as claimed in claim 6, it is characterised in that the active component elemental silver accounts for the quality of silver and Mn oxide The mass percent of sum is 2-10%.
8. purposes as claimed in claim 7, it is characterised in that the active component elemental silver accounts for the quality of silver and Mn oxide The mass percent of sum is 8%.
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