CN105013322A - Use of manganite catalyst in catalytic oxidation of formaldehyde - Google Patents
Use of manganite catalyst in catalytic oxidation of formaldehyde Download PDFInfo
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- CN105013322A CN105013322A CN201510359133.2A CN201510359133A CN105013322A CN 105013322 A CN105013322 A CN 105013322A CN 201510359133 A CN201510359133 A CN 201510359133A CN 105013322 A CN105013322 A CN 105013322A
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Abstract
The invention provides a use of a manganite catalyst in catalytic oxidation of formaldehyde. The manganite is gamma or/and delta crystal form manganese dioxide. The delta crystal form manganese dioxide as a formaldehyde catalytic oxidation catalyst has the advantages of 1, a formaldehyde catalytic oxidation ignition temperature is low, a conversion ratio is 37% under conditions of a high formaldehyde concentration of 170ppm, a high airspeed of 100000mL/(g.h) and a temperature of 50 DEG C, conversion is complete at a temperature of 80 DEG C and the activity of the unprecious metal catalyst is high on the list, and 2, stability is excellent, the crystal form before and after catalytic reaction is stable and a catalytic conversion rate is kept in a long-term activity test.
Description
Technical field
The invention belongs to formaldehyde catalysis technical field, be specifically related to the purposes of a kind of manganese oxide catalyst for catalyze oxidation of formaldehyde.
Background technology
Formaldehyde has as adhesive strengthens artificial floor hardness, insect protected, corrosion-resistant function, is thus widely used in furniture and fixtures material.On the other hand, formaldehyde also can be discharged into gradually in surrounding environment from adhesive, and this just result in the severe contamination of room air.The testing result of interior decoration association Indoor Environment Detection Working Committee of China also shows: formaldehyde become Chinese new clothes repair the house in major pollutants.Be exposed in the formaldehyde gas of certain content for a long time, gently then can the organ such as exciting eye, nose, larynx, heavy then cause fatigue and allergic reaction, even cause tumour, be detrimental to health.Thus, the Exploration & stu dy for the minimizing technology of formaldehyde high-efficiency is very urgent.
At present, the method removing indoor formaldehyde mainly contains photocatalysis method, plasma decomposition, absorption method and catalytic oxidation.Wherein formaldehyde exhaustive oxidation can be carbon dioxide and water by catalysed oxidation processes under low temperature even room temperature condition, catalyst is excited without the need to illumination or plasma, there is no the restriction of the saturated adsorption of adsorbent, thus breach many limitations of first three methods yet.The catalyst of current removal formaldehyde is mainly loaded noble metal catalyst and catalyst of transition metal oxide, and formaldehyde can be removed in room temperature by noble metal catalyst completely, but expensive, and this causes the attention gradually to transition metal oxide research.
CN 103691461A discloses the method for a kind of application load gold hydroxyapatite catalyst, with calcium nitrate and diammonium hydrogen phosphate for presoma, adopts liquid phase deposition to obtain carrier hydroxyapatite; Being presoma with gold chloride, take hydroxyapatite as carrier, adopts Powder by Homogenous Precipitation, prepares gold-supported hydroxyapatite catalyst.This catalyst can at room temperature catalytic elimination formaldehyde, but its shortcoming is active material is gold, and its price changes the commercial applications of catalyst by hindering.
CN 103962163A discloses the preparation method of transient metal doped hydroxyapatite and the catalytic oxidation of PARA FORMALDEHYDE PRILLS(91,95) thereof, and the method step is simple, the cycle is short, but compared to noble metal catalyst, its catalytic activity is not high.Thus the non-precious metal catalyst studying highly active catalyze oxidation of formaldehyde will have far-reaching realistic meaning.
Prior art (Tian Hua, He Junhui, the progress of manganese oxide catalyze oxidation of formaldehyde, chemistry circular the 76th volume the 2nd phase in 2013,100th ~ 106 pages) only discloses the manganese dioxide of α and beta crystal for purifying formaldehyde.They are at high load capacity, namely high-speed height concentration of formaldehyde condition (100000mL/ (gh) and 170ppm) under remove the temperature required height of formaldehyde completely, cannot practical application be met.
Summary of the invention
Based on this, the object of the present invention is to provide a kind of method of catalyze oxidation of formaldehyde, described method adopts the Mn oxide of different crystal forms as catalyst, achieves the efficient oxidation of formaldehyde.
In order to achieve the above object, present invention employs following technical scheme:
Manganese oxide catalyst is used for a purposes for catalyze oxidation of formaldehyde, and described Mn oxide is that γ is or/and the manganese dioxide of δ crystal formation.
Preferably, in the present invention, described Mn oxide is the manganese dioxide of δ crystal formation.The present invention is used for catalyze oxidation of formaldehyde by adopting the manganese dioxide of δ crystal formation, there is the advantage that conversion ratio is high and catalytic temperature is low, higher catalytic activity is shown 50 DEG C time, it still shows higher catalytic conversion under the test condition of high concentration (170ppm) high-speed (100000mL/ (gh)), and complete (100%) that still can realize formaldehyde at 80 DEG C transforms.
Preferably, in the present invention, in catalyze oxidation of formaldehyde process, the initial concentration of formaldehyde is 0-170ppm and does not comprise 0, such as 10ppm, 30ppm, 50ppm, 70ppm, 90ppm, 110ppm, 130ppm, 150ppm or 170ppm.Adopt the manganese dioxide of δ crystal formation of the present invention, under can realizing high concentration, during (high to 170ppm) 80 DEG C, formaldehyde 100% transforms.
Preferably, in the present invention, in catalyze oxidation of formaldehyde process, air speed is 0-100000mL/ (gh) and does not comprise 0, and described air speed is such as 100000mL/ (gh).Adopt the manganese dioxide of δ crystal formation of the present invention, under can realizing high-speed, during (100000mL/ (gh)) 80 DEG C, formaldehyde 100% transforms.
In the present invention, in catalyze oxidation of formaldehyde process, the consumption of Mn oxide is any amount.
Preferably, the manganese dioxide of described δ crystal formation take manganese sulfate as reducing agent, and potassium permanganate or ammonium persulfate are oxidant, adopts water heat transfer, specific as follows:
Requisite oxygen agent, reducing agent and deionized water is added in hydrothermal reaction kettle, by stirring, Oxidizing and Reducing Agents is thoroughly dissolved, and be placed in the insulating box of 200 ~ 240 DEG C and react, after reaction terminates, material in reactor to be filtered, washing and dry, roasting in atmosphere afterwards.
The manganese dioxide of the present invention by adopting specific hydrothermal temperature 200 ~ 240 DEG C (such as 205 DEG C, 210 DEG C, 215 DEG C, 220 DEG C, 225 DEG C, 230 DEG C or 235 DEG C) to prepare δ crystal formation, the manganese dioxide of the δ crystal formation obtained is made to have excellent formaldehyde catalytic activity, and higher catalytic activity is still shown under the test condition of high concentration (170ppm) high-speed (100000mL/ (gh)), complete (100%) that still can realize formaldehyde at 80 DEG C transforms.
Preferably, insulating box reaction 18 ~ 30h, such as 19h, 20h, 21h, 22h, 23h, 24h, 25h, 26h, 27h, 28h or 29h of 200 ~ 240 DEG C is placed in, preferred 24h.Time can not form sufficient δ crystal formation lower than catalyst during 18h, then can cause the waste of heat higher than 30h.
Preferably, described drying time is 12 ~ 24h, such as 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h or 23h.
Preferably, the temperature of described roasting is 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 lower than 300 DEG C, and catalyst can not be in abundant stable state, and higher than 450 DEG C, then easily causes the sintering of Ag.Roasting time is 3-6 hour, such as 3.3h, 3.6h, 3.9h, 4.2h, 4.5h, 4.8h, 5.1h, 5.4h or 5.7h, and lower than 3h, catalyst can not obtain roasting, then easily sinters and increase production cost higher than 6h.
Preferably, described Mn oxide area load has active component elemental silver.Load active component elemental silver, can improve the catalytic activity of catalyst significantly.
Preferably, the mass percent of quality sum that described active component elemental silver accounts for 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 catalyze oxidation of formaldehyde, described method adopts the manganese dioxide of δ crystal formation as catalyst.Preferably, under high concentration (concentration of formaldehyde 170ppm) high-speed (100000mL/ (gh)) condition, catalyze oxidation of formaldehyde is carried out.Under this concentration and space velocities, complete (100%) that can realize formaldehyde at 80 DEG C transforms.That is, when concentration of formaldehyde 170ppm, air speed be 100000mL/ (gh) and temperature are 80 DEG C, formaldehyde 100% transforms completely.Further preferably, the manganese dioxide of described δ crystal formation take manganese sulfate as reducing agent, potassium permanganate or ammonium persulfate are oxidant, adopt water heat transfer, specific as follows: in hydrothermal reaction kettle, to add requisite oxygen agent, reducing agent and deionized water, by stirring, Oxidizing and Reducing Agents is thoroughly dissolved, and be placed in the insulating box of 200 ~ 240 DEG C and react, after reaction terminates, material in reactor filtered, wash and drying, roasting in atmosphere afterwards.Further preferably, insulating box reaction 18 ~ 30h, such as 19h, 20h, 21h, 22h, 23h, 24h, 25h, 26h, 27h, 28h or 29h of 200 ~ 240 DEG C is placed in, preferred 24h.Time can not form sufficient δ crystal formation lower than catalyst during 18h, then can cause the waste of heat higher than 30h.Further preferably, the temperature of described roasting is 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 lower than 300 DEG C, and catalyst can not be in abundant stable state, and higher than 450 DEG C, then easily causes the sintering of Ag.Roasting time is 3-6 hour, such as 3.3h, 3.6h, 3.9h, 4.2h, 4.5h, 4.8h, 5.1h, 5.4h or 5.7h, and lower than 3h, catalyst can not obtain roasting, then easily sinters and increase production cost higher than 6h.Further preferably, described Mn oxide area load has active component elemental silver.Load active component elemental silver, can improve the catalytic activity of catalyst significantly.Preferably, the mass percent of quality sum that described active component elemental silver accounts for silver and Mn oxide is 2-10%, such as 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9% or 10%, preferably 8%.
The manganese dioxide of the present invention by adopting specific hydrothermal temperature 200 ~ 240 DEG C (such as 205 DEG C, 210 DEG C, 215 DEG C, 220 DEG C, 225 DEG C, 230 DEG C or 235 DEG C) to prepare δ crystal formation, the manganese dioxide of the δ crystal formation obtained is made to have excellent formaldehyde catalytic activity, and higher catalytic activity is still shown under the test condition of high concentration (170ppm) high-speed (100000mL/ (gh)), complete (100%) that still can realize formaldehyde at 80 DEG C transforms.
Compared with the prior art, the present invention has and adopts the manganese dioxide of δ crystal formation to have the following advantages as catalyst oxidation of formaldehyde tool:
(1) initiation temperature of catalyze oxidation of formaldehyde is low, conversion ratio when high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)) at 50 DEG C reaches 37%, transform completely at 80 DEG C, in non-precious metal catalyst, its activity is positioned at prostatitis;
(2) excellent in stability, before and after catalytic reaction, its crystal formation keeps stable on the one hand, and catalytic conversion remains unchanged in long-time (50h) active testing on the other hand, at concentration 170ppm, air speed 100,000mL/ (gh), during temperature 80 DEG C, all the time the conversion ratio of 100% is maintained, at concentration 170ppm, more high-speed 150,000mL/ (gh), under temperature 75 DEG C of conditions, maintain the conversion ratio of 60% all the time;
(3) adopt nontoxic component, decrease the harm to health and ecological environment, preparation process is simple, with low cost, easily realizes industrialization.
Detailed description of the invention
Technical scheme of the present invention is further illustrated below by detailed description of the invention.
Embodiment 1
Method as follows is adopted to prepare α, the manganese dioxide of β, γ and δ crystal formation:
Take manganese sulfate as reducing agent, potassium permanganate or ammonium persulfate are oxidant, adopt water heat transfer to prepare α, the manganese dioxide-catalyst of β, γ and δ crystal formation, specific as follows:
Required precursor (i.e. Oxidizing and Reducing Agents) (X) and 80mL deionized water is added in the hydrothermal reaction kettle of 100mL, by stirring, precursor is thoroughly dissolved, and be placed in the insulating box of certain reaction temperature (Y) and react certain hour (Z), then material in reactor is filtered, washing, dried overnight, afterwards with roasting at 300 DEG C in air.Following table is classified as X, the particular value of Y, Z.
| X | Y | Z | |
| α-MnO 2 | MnSO 4·H 2O+KMnO 4 | 160℃ | 24h |
| β-MnO 2 | MnSO 4·H 2O+(NH 4) 2S 2O 8 | 140℃ | 12h |
| γ-MnO 2 | MnSO 4·H 2O+(NH 4) 2S 2O 8 | 90℃ | 24h |
| δ-MnO 2 | MnSO 4·H 2O+KMnO 4 | 200-240℃ | 24h |
In four kinds of manganese dioxide, the activity of δ crystal formation manganese dioxide catalysis formaldehyde exhaustive oxidation, far above other crystal formation, illustrates the crystal formation advantage that it is huge.The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table, and arranges from high to low according to activity.Test condition: concentration 170ppm, air speed 100,000mL/ (gh).
Embodiment 2
Adopt and prepare α with the method that embodiment 1 is identical, the manganese dioxide of β, γ and δ crystal formation.
At concentration 170ppm, air speed 150,000mL/ (gh), under temperature 75 DEG C of conditions, the manganese dioxide of δ crystal formation can maintain within the 50h time 60% conversion ratio constant, α, β, γ test under similarity condition, and its activity progressively reduces after 5h.
Embodiment 3
The method identical with embodiment 1 is adopted to prepare α, the manganese dioxide of β, γ and δ crystal formation.
The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table, and arranges from high to low according to activity.Test condition: concentration 5ppm, air speed 5000mL/ (gh).
Comparative example 1
Adopt the manganese dioxide preparing δ crystal formation with the method that embodiment 1 is identical, except hydrothermal temperature is 180 DEG C.
Comparative example 2
Adopt the manganese dioxide preparing δ crystal formation with the method that embodiment 1 is identical, except hydrothermal temperature is 260 DEG C.
Under high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)), the catalytic activity of the catalyst of test comparison example 1 and comparative example 2, result shows:
The catalyst of comparative example 1 realizes formaldehyde 50% at 75 DEG C and transforms, and 110 DEG C realize formaldehyde 100% and transform, and the catalyst of comparative example 2 realizes formaldehyde 50% at 80 DEG C and transforms, and realizes formaldehyde 100% transform at 125 DEG C.
Embodiment 4
Adopt with the identical method α of embodiment 1, the manganese dioxide of β, γ and δ crystal formation, and on this manganese dioxide, load active component is silver-colored, silver-colored mass fraction 8wt%.
Under high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)), the catalytic activity of the catalyst of testing example 4.The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table.Test condition: concentration 170ppm, air speed 100,000mL/ (gh).
Embodiment 5
All the other are identical with embodiment 4, and desilver mass fraction is 2wt%.
Under high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)), the catalytic activity of the catalyst of testing example 5.The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table.Test condition: concentration 170ppm, air speed 100,000mL/ (gh).
Embodiment 6
All the other are identical with embodiment 4, and desilver mass fraction is 10wt%.
Under high concentration of formaldehyde high-speed (concentration 170ppm, air speed 100,000mL/ (gh)), the catalytic activity of the catalyst of testing example 6.The relevant parameter of the manganese dioxide catalysis formaldehyde activity of four kinds of crystal formations is listed in the following table.Test condition: concentration 170ppm, air speed 100,000mL/ (gh).
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of auxiliary element, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. manganese oxide catalyst is used for a purposes for catalyze oxidation of formaldehyde, and described Mn oxide is that γ is or/and the manganese dioxide of δ crystal formation.
2. purposes as claimed in claim 1, it is characterized in that, described Mn oxide is the manganese dioxide of δ crystal formation.
3. purposes as claimed in claim 1 or 2, it is characterized in that, in catalyze oxidation of formaldehyde process, the initial concentration of formaldehyde is 0-170ppm and does not comprise 0.
4. the purposes as described in one of claim 1-3, is characterized in that, in catalyze oxidation of formaldehyde process, air speed is 0-100000mL/ (gh) and does not comprise 0.
5. the purposes as described in one of claim 1-4, is characterized in that, the manganese dioxide of described δ crystal formation take manganese sulfate as reducing agent, and potassium permanganate or ammonium persulfate are oxidant, adopts water heat transfer, specific as follows:
Requisite oxygen agent, reducing agent and deionized water is added in hydrothermal reaction kettle, by stirring, Oxidizing and Reducing Agents is thoroughly dissolved, and be placed in the insulating box of 200 ~ 240 DEG C and react, after reaction terminates, material in reactor to be filtered, washing and dry, roasting in atmosphere afterwards.
6. purposes as claimed in claim 5, is characterized in that, is placed in insulating box reaction 18 ~ 30h, the preferred 24h of 200 ~ 240 DEG C.
7. the purposes as described in claim 5 or 6, is characterized in that, described drying time is 12 ~ 24h.
8. the purposes as described in one of claim 5-7, is characterized in that, the temperature of described roasting is 300 ~ 450 DEG C, and roasting time is 3 ~ 6h.
9. the purposes as described in one of claim 1-8, is characterized in that, described Mn oxide area load has active component elemental silver.
10. purposes as claimed in claim 9, is characterized in that, the mass percent that described active component elemental silver accounts for the quality sum of silver and Mn oxide is 2-10%, preferably 8%.
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