CN102068987A - Rare earth modified activated carbon-supported nanogold catalytic material and preparation method thereof - Google Patents
Rare earth modified activated carbon-supported nanogold catalytic material and preparation method thereof Download PDFInfo
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- CN102068987A CN102068987A CN2010105836721A CN201010583672A CN102068987A CN 102068987 A CN102068987 A CN 102068987A CN 2010105836721 A CN2010105836721 A CN 2010105836721A CN 201010583672 A CN201010583672 A CN 201010583672A CN 102068987 A CN102068987 A CN 102068987A
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Abstract
The invention discloses a rare earth modified activated carbon-supported nanogold catalytic material and a preparation method thereof. The catalytic material comprises the following components by weight percent: 0.1-2% of gold used as active component, 1-25% of rare earth oxide and 73-98.9% of activated carbon used as carrier, wherein rare earth oxide contains one or two of lanthanide oxide, thorium oxide, terbium oxide, dysprosium oxide, cerium oxide, neodymium oxide, gadolinium oxide and yttrium oxide. The catalytic material of the invention uses the activated carbon which is treated by strong oxidizer, as carrier and is prepared by modifying with rare earth oxide and supporting with nanogold. The catalytic material has double functions of adsorption and room temperature catalytic oxidation for the elimination of CO; when the air speed is 10000h<-1> at the room temperature, the CO conversion rate of the catalytic material is 99.99%; when the catalytic material is used continuously for 600h, the catalytic activity still reaches 99.6%; and the catalyst has low active component gold content, simple production process and lower production cost.
Description
Technical field
That the present invention relates to is a kind of catalysis material and preparation method, particularly relates to a kind of rare earth modified activated carbon supported nano gold catalysis material and preparation method.
Background technology
Carbon monoxide (CO) is colourless, tasteless and non-irritating gas, and coal gas manufacturing, coking, metallurgy, hydrocarbon fuel and partial oxidation, vehicular emission etc. all contain CO gas.Human body sucks carbon monoxide can cause acute poisoning and chronic lesion.For reducing pollution emissions, must purify carbon monoxide.The normal temperature removal method of micro CO mainly contains absorption process, absorption method and catalytic oxidation.
Load type gold catalyst demonstrates very high catalytic activity to carbon monoxide room-temperature catalytic oxidation, also generates N at nitric oxide reduction
2Reaction, Water gas shift/WGS, photocatalysis hydrolysis produce the completing combustion of hydrogen and volatile organic matter and react the medium good catalytic performance that shows.And nano catalyst has the performance that nano effect has improved catalyst because of its gold grain size at 2～5nm, becomes the research focus.Studies show that not only the size of gold grain has appreciable impact to catalyst activity, and kind of carrier also there is tangible influence to catalyst activity.Carrier commonly used has transition metal oxide, alkaline earth oxide and hydroxide, active carbon etc.
Active carbon has flourishing pore structure, specific area can be up to 2000m
2/ g and good absorption property and cheap can resistance to acids and bases matter stablizing, load noble metal thereon more easily reclaims by the burning of charcoal carrier, so active carbon is often used as the carrier of catalyst.Thereby one of effect of absorbent charcoal carrier be exactly improve dispersion degree of active components and stability make catalyst that more active sites can be provided.The surface area pore structure of active carbon and surface functional group all can influence the character of catalyst, and these parameters of absorbent charcoal carrier can be handled by strong oxidizer, carried metal in addition modification to improve the performance of catalyst.
Find through the retrieval to prior art: document discloses a kind of preparation method of activated carbon-carried nano-gold catalyst; preparation adds the protectant dipping solution of a kind of organic acid at least; the activated carbon carrier is put into maceration extract carry out mechanical agitation or ultrasonic mixing; leaving standstill the back filters; carrier is washed; dry; roasting reduction obtains the activated carbon carried nano-gold catalyst; the ozone and the volatile organic matter of low concentration in the air can be effectively decomposed in the little and even distribution of this activity of such catalysts component gold grain size.
Summary of the invention
The object of the present invention is to provide a kind of rare earth modified activated carbon supported nano gold catalysis material and preparation method thereof.The present invention is achieved by the following technical solutions:
The invention provides a kind of rare earth modified activated carbon supported nano gold catalysis material, it is characterized in that its mass percent consists of: the active component gold is 0.1～2%, rare earth oxide is 1～25%, and surplus was for to handle absorbent charcoal carrier through strong oxidizer.
Described strong oxidizer is the mixed solution that the hydrogen peroxide of 10% nitric acid and 10% is made into.
Described rare earth oxide is lanthana or dysprosia or cerium oxide or neodymia or yittrium oxide, or cerium oxide and neodymia.
The invention provides a kind of rare earth modified activated carbon supported nano gold catalysis preparation methods, it is characterized in that may further comprise the steps:
The first step, active carbon pre-treatment: the nitric acid of preparation 10% and 10% hydrogen peroxide solution mix, and active carbon was flooded wherein 1 hour, take out in 100～120 ℃ of oven dry 4 hours;
Second step, rare earth modified active carbon: the active carbon incipient impregnation after the first step handled in rare-earth metal nitrate solution 1 hour, took out in 80～120 ℃ of baking ovens dry 2 hours, under vacuum or nitrogen protection,, make rare earth modified active carbon in 300 ℃ of roastings 4 hours;
The 3rd step, supported nano-gold: go on foot the modified activated carbon that makes with 60 ℃ of following incipient impregnations second of chlorauric acid solution and take out after 2 hours; Use sodium borohydride solution, 20 ℃ of following active carbons of taking out of reduction 2 hours spend deionised water, filter, and 100～150 ℃ of dryings 4 hours make the rare earth modified activated carbon supported nano gold catalysis material of finished product catalysis material.
Described rare-earth metal nitrate is lanthanum nitrate or dysprosium nitrate or cerous nitrate or neodymium nitrate or yttrium nitrate, or cerous nitrate and neodymium nitrate.
Catalysis material of the present invention carries out performance evaluation to the purifying property of CO in Φ 16mm, the straight type glass tube of long 300mm reactor, catalyst amount is 6mL, and it is 20～200ppm that unstripped gas consists of CO content, and all the other are air.Be reflected under the normal temperature and pressure environment and carry out, reaction gas volume air speed (GHSV) is 10000h
-1, obtain the CO conversion ratio by gas chromatographic analysis.
Compared with prior art, catalysis material of the present invention is a carrier with the strong oxidizer processed active carbon, is prepared from through rare-earth oxide modified back loading nm of gold.The present invention has the following advantages: this catalysis material is eliminated the dual-use function with absorption and room-temperature catalytic oxidation to CO, and at room temperature air speed is 10000h
-1The time, catalysis material is 99.99% to the initial conversion of CO, use 600h continuously after, catalytic activity still reaches 99.6%, and activity of such catalysts component gold content is low, production technology is easy, the Preparation of Catalyst cost is lower.
The specific embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Active carbon after Comparative Examples 1 pre-treatment
Compound concentration is 10% nitric acid and 10% hydrogen peroxide mixed solution 10mL, and Φ 15mm, long 50mm active carbon are flooded wherein 1h, takes out the back in 100 ℃ of dry 4h, makes the active carbon after the pre-treatment.
Made active carbon is carried out the CO catalytic performance test according to the afore-mentioned test condition, and active carbon is 93.7% to the initial conversion of micro CO in the time of 20 ℃, and the conversion ratio of carbon monoxide reduces to 54.8% behind the 2h.
Embodiment 1
Compound concentration is 10% nitric acid and 10% hydrogen peroxide mixed solution 10mL, and Φ 15mm, long 50mm active carbon are flooded wherein 1h, takes out the back in 100 ℃ of dry 4h, makes the active carbon after the pre-treatment.Take by weighing the 0.08g lanthanum nitrate and be dissolved in wiring solution-forming in the 6mL deionized water, the active carbon of pre-treatment is placed the medium volume dipping of solution 1h after, dry 2h in 100 ℃ of baking ovens.Dried active carbon under vacuum (or nitrogen protection), in 300 ℃ of calcining 3h, is made rare earth modified active carbon.
Compound concentration is the chlorauric acid solution 6mL of 0.008g/mL, and 60 ℃ flood rare earth modified active carbon 2h down; Compound concentration is the NaBH of 0.05g/mL
4Solution 10mL, 20 ℃ of following reducing activity charcoal 2h spend deionised water, filter, and 100 ℃ of dry 4h make the finished product catalysis material.Au: La wherein
2O
3: active carbon=1: 2: 100.
Made active carbon is carried out the CO catalytic performance test according to the afore-mentioned test condition, and active carbon is 99.1% to the initial conversion of micro CO in the time of 20 ℃, and the conversion ratio of carbon monoxide reduces to 91.6% behind the 2h.
Embodiment 2
Compound concentration is 10% nitric acid and 10% hydrogen peroxide mixed solution 10mL, and Φ 15mm, long 50mm active carbon are flooded wherein 1h, takes out the back in 100 ℃ of dry 4h, makes the active carbon after the pre-treatment.Take by weighing the 0.078g neodymium nitrate and be dissolved in wiring solution-forming in the 6mL deionized water, the active carbon of pre-treatment is placed the medium volume dipping of solution 1h after, dry 2h in 100 ℃ of baking ovens.Dried active carbon under vacuum (or nitrogen protection), in 300 ℃ of calcining 3h, is made rare earth modified active carbon.
Compound concentration is the chlorauric acid solution 6mL of 0.008g/mL, and 60 ℃ flood rare earth modified active carbon 2h down; Compound concentration is the NaBH of 0.05g/mL
4Solution 10mL, 20 ℃ of following reducing activity charcoal 2h spend deionised water, filter, and 100 ℃ of dry 4h make the finished product catalysis material.Au: Nd wherein
2O
3: active carbon=1: 2: 100.
Made active carbon is carried out the CO catalytic performance test according to the afore-mentioned test condition, and active carbon is 98.9% to the initial conversion of micro CO in the time of 20 ℃, and the conversion ratio of carbon monoxide reduces to 96.8% behind the 2h.
Embodiment 3
Compound concentration is 10% nitric acid and 10% hydrogen peroxide mixed solution 10mL, and Φ 15mm, long 50mm active carbon are flooded wherein 1h, takes out the back in 100 ℃ of dry 4h, makes the active carbon after the pre-treatment.Take by weighing the 0.056g dysprosium nitrate and be dissolved in wiring solution-forming in the 6mL deionized water, the active carbon of pre-treatment is placed the medium volume dipping of solution 1h after, dry 2h in 100 ℃ of baking ovens.Dried active carbon under vacuum (or nitrogen protection), in 300 ℃ of calcining 3h, is made rare earth modified active carbon.
Compound concentration is the chlorauric acid solution 6mL of 0.008g/mL, and 60 ℃ flood rare earth modified active carbon 2h down; Compound concentration is the NaBH of 0.05g/mL
4Solution 10mL, 20 ℃ of following reducing activity charcoal 2h spend deionised water, filter, and 100 ℃ of dry 4h make the finished product catalysis material.Au: Dy wherein
2O
3: active carbon=1: 2: 100.
Made active carbon is carried out the CO catalytic performance test according to the afore-mentioned test condition, and active carbon is 99.4% to the initial conversion of micro CO in the time of 20 ℃, and the conversion ratio of carbon monoxide reduces to 82.9% behind the 2h.
Embodiment 4
Compound concentration is 10% nitric acid and 10% hydrogen peroxide mixed solution 10mL, and Φ 15mm, long 50mm active carbon are flooded wherein 1h, takes out the back in 100 ℃ of dry 4h, makes the active carbon after the pre-treatment.Take by weighing the 0.151g cerous nitrate and be dissolved in wiring solution-forming in the 6mL deionized water, the active carbon of pre-treatment is placed the medium volume dipping of solution 1h after, dry 2h in 100 ℃ of baking ovens.Dried active carbon under vacuum (or nitrogen protection), in 300 ℃ of calcining 3h, is made rare earth modified active carbon.
Compound concentration is the chlorauric acid solution 6mL of 0.008g/mL, and 60 ℃ flood rare earth modified active carbon 2h down; Compound concentration is the NaBH of 0.05g/mL
4Solution 10mL, 20 ℃ of following reducing activity charcoal 2h spend deionised water, filter, and 100 ℃ of dry 4h make the finished product catalysis material.Au: CeO wherein
2: active carbon=1: 2: 100.
Made active carbon is carried out the CO catalytic performance test according to the afore-mentioned test condition, and active carbon is 98.5% to the initial conversion of micro CO in the time of 20 ℃, and the conversion ratio of carbon monoxide reduces to 91.3% behind the 2h.
Embodiment 5
Compound concentration is 10% nitric acid and 10% hydrogen peroxide mixed solution 10mL, and Φ 15mm, long 50mm active carbon are flooded wherein 1h, takes out the back in 100 ℃ of dry 4h, makes the active carbon after the pre-treatment.Take by weighing the 0.102g yttrium nitrate and be dissolved in wiring solution-forming in the 6mL deionized water, the active carbon of pre-treatment is placed the medium volume dipping of solution 1h after, dry 2h in 100 ℃ of baking ovens.Dried active carbon under vacuum (or nitrogen protection), in 300 ℃ of calcining 3h, is made rare earth modified active carbon.
Compound concentration is the chlorauric acid solution 6mL of 0.008g/mL, and 60 ℃ flood rare earth modified active carbon 2h down; Compound concentration is the NaBH of 0.05g/mL
4Solution 10mL, 20 ℃ of following reducing activity charcoal 2h spend deionised water, filter, and 100 ℃ of dry 4h make the finished product catalysis material.Au: Y wherein
2O
3: active carbon=1: 2: 100.
Made active carbon is carried out the CO catalytic performance test according to the afore-mentioned test condition, and active carbon is 99.99% to the initial conversion of micro CO in the time of 20 ℃, and the conversion ratio of carbon monoxide reduces to 73.4% behind the 2h.
Embodiment 6
Compound concentration is 10% nitric acid and 10% hydrogen peroxide mixed solution 10mL, and Φ 15mm, long 50mm active carbon are flooded wherein 1h, takes out the back in 100 ℃ of dry 4h, makes the active carbon after the pre-treatment.Take by weighing the 0.151g cerous nitrate and the 0.078g neodymium nitrate is dissolved in wiring solution-forming in the 6mL deionized water, the active carbon of pre-treatment is placed the medium volume dipping of solution 1h after, dry 2h in 100 ℃ of baking ovens.Dried active carbon under vacuum (or nitrogen protection), in 300 ℃ of calcining 3h, is made rare earth modified active carbon.
Compound concentration is the chlorauric acid solution 6mL of 0.004g/mL, and 60 ℃ flood rare earth modified active carbon 2h down; Compound concentration is the NaBH of 0.05g/mL
4Solution 10mL, 20 ℃ of following reducing activity charcoal 2h spend deionised water, filter, and 100 ℃ of dry 4h make the finished product catalysis material.Au: CeO wherein
2: Nd
2O
3: active carbon=0.5: 2: 2: 100.
Made active carbon is carried out the CO catalytic performance test according to the afore-mentioned test condition, and active carbon is 99.99% to the initial conversion of micro CO in the time of 20 ℃, use 600h continuously after, the conversion ratio of carbon monoxide still reaches 99.6%.
Claims (5)
1. rare earth modified activated carbon supported nano gold catalysis material is characterized in that its mass percent consists of: the active component gold is 0.1～2%, rare earth oxide is 1～25%, and surplus was for to handle absorbent charcoal carrier through strong oxidizer.
2. a kind of rare earth modified activated carbon supported nano gold catalysis material according to claim 1 is characterized in that, described strong oxidizer is the mixed solution that the hydrogen peroxide of 10% nitric acid and 10% is made into.
3. a kind of rare earth modified activated carbon supported nano gold catalysis material according to claim 1 is characterized in that, described rare earth oxide is lanthana or dysprosia or cerium oxide or neodymia or yittrium oxide, or cerium oxide and neodymia.
4. a kind of rare earth modified activated carbon supported nano gold catalysis preparation methods according to claim 1 is characterized in that may further comprise the steps:
The first step, active carbon pre-treatment: the nitric acid of preparation 10% and 10% hydrogen peroxide solution mix, and active carbon was flooded wherein 1 hour, take out in 100～120 ℃ of oven dry 4 hours;
Second step, rare earth modified active carbon: the active carbon incipient impregnation after the first step handled in rare-earth metal nitrate solution 1 hour, took out in 80～120 ℃ of baking ovens dry 2 hours, under vacuum or nitrogen protection,, make rare earth modified active carbon in 300 ℃ of roastings 4 hours;
The 3rd step, supported nano-gold: go on foot the modified activated carbon that makes with 60 ℃ of following incipient impregnations second of chlorauric acid solution and take out after 2 hours; Use sodium borohydride solution, 20 ℃ of following active carbons of taking out of reduction 2 hours spend deionised water, filter, and 100～150 ℃ of dryings 4 hours make the rare earth modified activated carbon supported nano gold catalysis material of finished product catalysis material.
5. a kind of rare earth modified activated carbon supported nano gold catalysis preparation methods according to claim 4, it is characterized in that, described rare-earth metal nitrate is lanthanum nitrate or dysprosium nitrate or cerous nitrate or neodymium nitrate or yttrium nitrate, or cerous nitrate and neodymium nitrate.
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| CN104148083A (en) * | 2014-08-22 | 2014-11-19 | 沈阳三聚凯特催化剂有限公司 | Preparation method of dual-function hydrofining catalyst |
| CN104993155A (en) * | 2015-05-28 | 2015-10-21 | 天能电池集团有限公司 | Preparation method of proton exchange membrane fuel cell anode oxygen reduction electrocatalyst |
| CN105833842A (en) * | 2015-01-13 | 2016-08-10 | 江苏瑞丰科技实业有限公司 | Granular non-noble-metal efficient integrated air purification composite material |
| CN106622229A (en) * | 2017-01-10 | 2017-05-10 | 湘潭大学 | Preparation method of hydrogenation catalyst and method for preparing cyclohexanone through phenol selective hydrogenation |
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2010
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104148083A (en) * | 2014-08-22 | 2014-11-19 | 沈阳三聚凯特催化剂有限公司 | Preparation method of dual-function hydrofining catalyst |
| CN104148083B (en) * | 2014-08-22 | 2016-09-07 | 沈阳三聚凯特催化剂有限公司 | A kind of preparation method of dual-functional hydrogenation catalyst for refining |
| CN105833842A (en) * | 2015-01-13 | 2016-08-10 | 江苏瑞丰科技实业有限公司 | Granular non-noble-metal efficient integrated air purification composite material |
| CN104993155A (en) * | 2015-05-28 | 2015-10-21 | 天能电池集团有限公司 | Preparation method of proton exchange membrane fuel cell anode oxygen reduction electrocatalyst |
| CN106622229A (en) * | 2017-01-10 | 2017-05-10 | 湘潭大学 | Preparation method of hydrogenation catalyst and method for preparing cyclohexanone through phenol selective hydrogenation |
| CN106622229B (en) * | 2017-01-10 | 2019-06-28 | 湘潭大学 | The preparation method and phenol selectivity of hydrogenation catalyst add the method for hydrogen preparing cyclohexanone |
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Application publication date: 20110525 |