CN106040230A - Method for preparing integrated catalyst for low-temperature catalytic oxidation of formaldehyde - Google Patents
Method for preparing integrated catalyst for low-temperature catalytic oxidation of formaldehyde Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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Abstract
The invention relates to a method for preparing an integrated catalyst for low-temperature catalytic oxidation of formaldehyde. The method comprises the steps of conducting hydration on an aluminum sheet subjected to anodic oxidation in deionized water which is 30-95 DEG C for 5-70 min, so that a Boehm system is obtained; placing the Boehm system in a chloroplatinic acid solution with the concentration of 0.1-0.8 g/L for dipping lasting 1-8 h at 25 DEG C, and conducting drying for 12 h at normal temperature; conducting reduction for 0.5-3 h at 25 DEG C in a sodium borohydride solution with the concentration of 0.05-1 mol/L, and conducting drying for 12 h at normal temperature, so that the integrated catalyst is obtained. The catalyst prepared with the method can well adsorb methanol when applied to a methanol catalytic combustion system, and can oxidize part of methanol at normal temperature, methanol conversion rate reaches 72% at normal temperature when platinum content is 2-2.5 wt%, and complete conversion can be achieved at 60 DEG C.
Description
Technical field
The present invention relates to the preparation method of a kind of integrated catalyst for formaldehyde low-temperature catalytic oxidation, be specifically related to one
Plant the novel preparation method rich in hydroxyl integration catalyst for formaldehyde treated.Belong in catalytic oxidation process air and wave
The property sent out organic compound (VOCs) field.
Background technology
Along with the raising of people's living standard, various organic polymers are widely used in daily life, such as indoor
Urea aldehyde tree commonly used in the artificial boards such as finishing plywood, core-board, medium density fibre board (MDF) and particieboard and furniture
Fat adhesive；The membrane material that wallpaper coating etc. are used；The auxiliary agent added in the laundry care agent of daily use, detergent etc.
Such as the VOCs (Volatile Organic Compounds, VOCs) such as formaldehyde and benzene class can be discharged Deng all, make
People live in an environment the most unsound.About kind more than 300 has been detected at present according to statistics in indoor air
VOCs is wherein the highest with content of formaldehyde.Formaldehyde is in second in China's priority acccess control toxic chemical, is defended by the world
Raw tissue is defined as carcinogenic and causes deformed material, and the allergen being well recognized as, is also one of potential strong mutagen, for a long time
Contact low dosage formaldehyde can cause the diseases such as chronic respiratory tract disease, nasopharyngeal carcinoma, nuclear gene mutation, leukemia, human body
Health causes serious threat.Therefore effectively administering of indoor environmental pollution is extremely urgent.
The method being presently used for purifying indoor formaldehyde mainly has adsorption technology, photocatalysis technology, lower temperature plasma technology
And catalytic oxidation technologies.Formaldehyde the most just can be completely decomposed into harmless H by catalytic oxidation technologies2O and
CO2, thus the method becoming the purifying formaldehyde having most application prospect.Noble metal with its excellent catalytic oxidation activity frequently as urging
Change the catalyst of oxidation of organic compounds.In formaldehyde through catalytic oxidation catalyst preparation process, typically by noble metal (Pt, Pd, Rh, Au
Deng) load on graininess or powdery metal oxide carrier, such as the Publication No. of ecological Studies institute of Chinese Academy of Sciences He Hong
The patent of 1795970, is supported on TiO by precious metals pt2On.But due to graininess or powder catalyst have pressure drop high,
Resistance to mass tranfer is poor, be difficult to the shortcomings such as plastotype (such as Chinese patent CN201410642073), is difficult to apply it to industrial treatment first
During aldehyde, use metallic matrix integration catalyst that these problems can be made to have been resolved；Additionally, the oxidation of formaldehyde is steamed with water
There is close relationship in gas, under steam atmosphere, the oxidation of formaldehyde is more effective, therefore, seek one can with self provide water or
The carrier of hydroxyl, more effectively processes inherently to formaldehyde and brings unprecedented rosy prospect.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of integrated catalyst for formaldehyde low-temperature catalytic oxidation, should
Catalyst preparation process is simple, pressure drop is low, heat and mass transfer performance is good, be prone to plastotype, has good industrial prospect.
The present invention is achieved through the following technical solutions:
The preparation method of a kind of integrated catalyst for formaldehyde low-temperature catalytic oxidation, it is characterised in that described method
Comprise the steps:
1) anodic oxidation of aluminium sheet: it is 50A/m that pretreated aluminium sheet is placed at 20 DEG C electric current density2, 0.1-
0.8mol/L oxalic acid solution Anodic Oxidation 8-16h, air-dry after at 350-550 DEG C roasting 1-3h；
2) by hot hydration, it is thus achieved that rich in the integrated carrier the most vigorous nurse body (AlOOH) of hydroxyl: i.e., by step 1)
Anodic oxidation aluminium sheet in 30-95 DEG C of deionized water, be hydrated 5min-70min, under room temperature be dried 12h；
3) active component load: vigorous nurse body is placed in the platinum acid chloride solution that concentration is 0.1g/L-0.8g/L, at 25 DEG C
Dipping 1-8h, is dried 12h under room temperature；
4) chemical method reduction: by through step 3) the vigorous nurse body that loaded is placed in the sodium borohydride that concentration is 0.05-1mol/L
In solution at 25 DEG C reduce 0.5-3h, under room temperature be dried 12h, obtain described integrated catalyst.
Described step 1) described in aluminium sheet pretreatment be: respectively with 10wt%NaOH solution and 10wt%HNO3Solution pair
Aluminium sheet carries out pre-treatment 4min and 2min.
Described step 2) in, preferred 80-95 DEG C of hydration temperature, hydration time is preferably 60-70min.
Described step 3) in, the concentration of platinum acid chloride solution is preferably 0.4g/L.
Described step 3) in, dip time is preferably 4 hours.
The platinum content of described catalyst is 0.05-2.5wt%, and its applicating evaluating condition is: by the integration catalysis of preparation
When agent is applied in formaldehyde catalytic combustion system, the catalyst being calculated as 0.05-2.5wt% with platinum constituent mass percentage composition is
0.3g, concentration of formaldehyde is 200ppm, and air speed is 3000-150,000L/ (g h).
Compared with the prior art, advantages of the present invention is as follows:
The present invention uses anodizing technology to be prepared for a kind of novel vigorous nurse of integrated catalyst carrier rich in hydroxyl
Body, relative to commonly used graininess or powder carrier, it has, and pressure drop is low, heat and mass good, be prone to the excellent of plastotype
Point, it is possible to the air purifier well and on market carries out miniature combination, it is easy to industrialization；It addition, make by oneself relative to other
Vigorous nurse body, it has the advantage that preparation technology is simple to operation.During tradition vigorous nurse body preparation, it is necessary to add forerunner
Body, precipitant, structure regulating agent etc., condition is wayward, and the vigorous nurse body structure prepared is uneven, and is graininess or flower pattern
Scatter shape, although having possessed rich in this characteristic of hydroxyl, PARA FORMALDEHYDE PRILLS(91,95) has good absorption property, but still do not has during industrialization
Solve the deficiency that pressure drop is high, heat transfer property is poor, structure is single.The present invention had both applied the advantage of integrated carrier, the most successfully made
Obtaining the vigorous nurse body rich in hydroxyl, this is a sizable breakthrough for the low-temperature catalytic oxidation of formaldehyde, empty to micro high efficiency
The extensively application of gas purifier provides possibility.
Accompanying drawing explanation
Fig. 1. the integrated catalyst preparation flow of the present invention；
Fig. 2. Fig. 2-a is 10, the catalyst surface aspect graph under 000 times, and Fig. 2-b is 20, the catalyst surface under 000 times
Aspect graph.
Fig. 3. under different hydration temperatures, vigorous nurse body weight gains is over time；
Fig. 4. blank experiment；
Fig. 5. the impact on catalyst activity of the co-impregnation solution concentration；
Fig. 6. the impact on catalyst activity of the co-impregnation time.
Detailed description of the invention
Below by drawings and Examples, the present invention is further elaborated.
According to Fig. 1, prepare catalyst, the aluminium sheet crossed through acid-alkali treatment is carried out in oxalic acid solution anodic oxidation,
Roasting, hydration, be dried to obtain carrier vigorous nurse body under room temperature, by carrier impregnation to platinum acid chloride solution, after dipping terminates, will be dried
After catalyst be submerged in sodium borohydride solution and reduce, drying at room temperature i.e. obtains Pt/AlOOH catalyst, its surface shape
State figure is as in figure 2 it is shown, the catalyst that can prepare has the nanostructured of porous.
Fig. 3 compares under different hydration temperatures, quality of alumina change and the relation of hydration time.Can from figure
Going out, hydration temperature is the highest, and quality of alumina weightening finish is the most obvious, and increases weight that to reach saturated required time the shortest.30 DEG C of hydrations
Time quality of alumina have almost no change；And mass weight gain has small increase with hydration time when 50 DEG C, this is because low
The lower hydration reaction speed of temperature is low, and hydrated alumina (AlOOH) is formed slowly..When hydration temperature is higher than 65 DEG C, sample weightening finish is bright
Aobvious；And when temperature is higher than 80 DEG C, hydration weightening finish no longer changes over after 60min, has reached saturated.
The activity in catalysis oxidation of formaldehyde of the material present in carrier (AlOOH) and other system is surveyed by Fig. 4
Comment.
Under the effect not having any material, the most not by the dioxygen oxidation in air during 400 DEG C of formaldehyde, add quartz
After sand, formaldehyde has little a part of oxidized when 300 DEG C, and the addition of carrier, greatly reduce the initiation temperature of formaldehyde,
Just having part formaldehyde oxidized when 100 DEG C, when 200 DEG C, formaldehyde conversion has reached 95%.Fully show AlOOH carrier
Advantage.
Embodiment 1
Respectively with 10wt%NaOH solution and 10wt%HNO3After solution carries out pre-treatment 4min and 2min to aluminium sheet, put into
Anodizing tank carries out anodic oxidation, and it is 50A/m that aluminium sheet is placed at 20 DEG C electric current density2, 0.1-0.8mol/L oxalic acid is molten
Liquid Anodic Oxidation 8-16h, air-dry after at 350 DEG C roasting 1h；60-70min it is hydrated, under room temperature in 95 DEG C of deionized waters
Dry 12h obtains vigorous nurse body；
The vigorous nurse body of gained is respectively placed in concentration is 0.1g/L, 0.2g/L, 0.3g/L, 0.4g/L, 0.5g/L, 0.6g/
In the platinum acid chloride solution of L, 0.7g/L, 0.8g/L, at 25 DEG C, impregnate 4h, under room temperature, be dried 12h；The vigorous nurse body loaded is placed in
Concentration be 0.05mol/L sodium borohydride solution at 25 DEG C reduce 1h, under room temperature be dried 12h, obtain integration catalyst.
The catalyst loadings of gained and the chloroplatinic acid concentration impact such as table 1 on platinum load capacity:
The impact on platinum load capacity of the table 1 chloroplatinic acid concentration
When less than 0.4g/L concentration, Pt content increases, at 0.4g/L along with the increase of platinum acid chloride solution concentration
H2PtCl6Time Pt content the highest, reach 2.4wt%, when chloroplatinic acid concentration continue raise, Pt content then presents smooth trend, all exists
2.4wt% fluctuates, and significantly rises, and illustrates that 0.4g/L chloroplatinic acid dipping 4h has already taken up vigorous nurse body carrier and has been provided that
Adsorption potential, continue raise chloroplatinic acid concentration Pt content can not be made to be increased dramatically further.When concentration is less than or equal to
During 0.4g/L, along with the increase of platinum acid chloride solution concentration, the complete conversion temperature of formaldehyde the most gradually migrates to lower temperature, from
90 DEG C of Cat 1 are reduced to 60 DEG C of Cat 4.
The integrated catalyst of preparation is applied in formaldehyde catalytic combustion system, uses with platinum constituent mass percentage composition
The catalyst being calculated as 0.05-2.5wt% is 0.3g, and concentration of formaldehyde is 200ppm, under air speed 3000-150,000L/ (g h),
Carrying out catalyst performance evaluation, corresponding catalyst removes the catalytic efficiency of formaldehyde as shown in Figure 5.
Embodiment 2
Respectively with 10wt%NaOH solution and 10wt%HNO3After solution carries out pre-treatment 4min and 2min to aluminium sheet, put into
Anodizing tank carries out anodic oxidation, and it is 50A/m that aluminium sheet is placed at 20 DEG C electric current density2, in 0.4mol/L oxalic acid solution
Anodic oxidation 12h, air-dry after at 350 DEG C roasting 1h；In 80 DEG C of deionized waters, it is hydrated 60min, is dried 12h under room temperature and obtains
To vigorous nurse body；
The vigorous nurse body of gained is respectively placed in the platinum acid chloride solution that concentration is 0.1g/L, at 25 DEG C, impregnate 1 respectively, 2,
4,6,8 hours, 12h under room temperature, it is dried；The vigorous nurse body loaded is placed in the sodium borohydride solution that concentration is 0.05mol/L 25
Reduction 1h at DEG C, is dried 12h under room temperature, obtain integration catalyst.The dip time of the gained impact such as table 2 on platinum load capacity
Shown in.
The impact on platinum load capacity of table 2 dip time
When dip time is less than 4h, along with the prolongation of dip time, Pt content is consequently increased, when dip time is less than
During 4h, along with the prolongation of dip time, Pt load capacity is consequently increased, but 2h only has 0.11wt%Pt；Dip time is more than 4h
After, as time went on to 6h, during 8h, Pt load capacity only has a small amount of lifting, tends towards stability.During this explanation 0.1g/L concentration,
Dip time 4h i.e. reaches Pt adsorption equilibrium on vigorous nurse body carrier, and catalyst activity is directly proportional to Pt content, therefore selects altogether
Dipping 4h is suitable dip time.
The integrated catalyst of preparation is applied in formaldehyde catalytic combustion system, uses with platinum constituent mass percentage composition
The catalyst being calculated as 0.05-2.5wt% is 0.3g, and concentration of formaldehyde is 200ppm, under air speed 3000-150,000L/ (g h),
Carrying out catalyst performance evaluation, corresponding catalyst removes the catalytic efficiency of formaldehyde as shown in Figure 6.
Claims (5)
1. the preparation method for the integrated catalyst of formaldehyde low-temperature catalytic oxidation, it is characterised in that described method bag
Include following steps:
1) anodic oxidation of aluminium sheet: it is 50A/m that pretreated aluminium sheet is placed at 20 DEG C electric current density2, 0.1-0.8mol/L
Oxalic acid solution Anodic Oxidation 8-16h, air-dry after at 350-550 DEG C roasting 1-3h；
2) by hot hydration, it is thus achieved that rich in the integrated carrier the most vigorous nurse body (AlOOH) of hydroxyl: i.e., by step 1) sun
Pole alumina plate is hydrated 5min-70min in 30-95 DEG C of deionized water, is dried 12h under room temperature；
3) active component load: be placed in the platinum acid chloride solution that concentration is 0.1g/L-0.8g/L by vigorous nurse body, impregnates at 25 DEG C
1-8h, is dried 12h under room temperature；
4) chemical method reduction: by through step 3) the vigorous nurse body that loaded is placed in the sodium borohydride solution that concentration is 0.05-1mol/L
In at 25 DEG C reduce 0.5-3h, under room temperature be dried 12h, obtain described integrated catalyst.
2. the preparation method of the integrated catalyst for formaldehyde low-temperature catalytic oxidation as claimed in claim 1, its feature exists
In, described step 1) described in aluminium sheet pretreatment be: respectively with 10wt%NaOH solution and 10wt%HNO3Solution is to aluminium sheet
Carry out pre-treatment 4min and 2min.
3. the preparation method of the integrated catalyst for formaldehyde low-temperature catalytic oxidation as claimed in claim 1, its feature exists
In, described step 2) in, hydration temperature is preferably 80-95 DEG C, and hydration time is 60-70min.
4. the preparation method of the integrated catalyst for formaldehyde low-temperature catalytic oxidation as claimed in claim 1, its feature exists
In, described step 3) in, the concentration of platinum acid chloride solution is 0.4g/L.
5. the preparation method of the integrated catalyst for formaldehyde low-temperature catalytic oxidation as claimed in claim 1, its feature exists
In, described step 3) in, dip time is preferably 4 hours.
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| CN108940265A (en) * | 2018-07-05 | 2018-12-07 | 宁波工程学院 | A kind of catalyst and preparation method thereof of room temperature catalytic oxidation formaldehyde |
| CN109012695A (en) * | 2018-08-17 | 2018-12-18 | 华东理工大学 | A kind of preparation method, thus obtained structural catalyst and its application of the structural catalyst of catalysis oxidation formaldehyde |
| CN112512682A (en) * | 2018-11-30 | 2021-03-16 | 住友化学株式会社 | Catalyst for aldehyde decomposition |
| CN115739113A (en) * | 2022-11-23 | 2023-03-07 | 大气(广东)科技发展有限公司 | Catalyst for catalyzing formaldehyde at room temperature and preparation method thereof |
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