CN103861611A - Preparation method and application of Cu-Mn catalyst loaded on aluminum-pillared montmorillonite - Google Patents
Preparation method and application of Cu-Mn catalyst loaded on aluminum-pillared montmorillonite Download PDFInfo
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- CN103861611A CN103861611A CN201410099382.8A CN201410099382A CN103861611A CN 103861611 A CN103861611 A CN 103861611A CN 201410099382 A CN201410099382 A CN 201410099382A CN 103861611 A CN103861611 A CN 103861611A
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Abstract
The invention relates to a preparation method and the application of a Cu-Mn catalyst loaded on aluminium-pillared montmorillonite, belonging to the field of catalytic oxidation of CO. The montmorillonite which is widespread in the natural world is taken as a raw material; the preparation method comprises the steps of modifying the montmorillonite raw ore by sodium treatment and aluminum-pillaring, and loading Cu and Mn onto the aluminum-pillared montmorillonite to prepare the catalyst, wherein the loading amounts of Cu and Mn are respectively 4.8-9wt%. The Cu-Mn catalyst is suitable for the catalytic oxidation of CO with high space velocity (60, 000h<-1>-100, 000h<-1>). After the load-type Cu-Mn catalyst is adopted, CO is completely converted into CO2 (the conversion rate is 100%) at 180 DEG C, and the conversion rate of about 100% of CO can be maintained within 100h at 180 DEG C.
Description
Technical field
The present invention relates to a kind of aluminium pillared montmorillonite load type Catalysts and its preparation method and application for CO catalytic oxidation.
Background technology
CO is one of main air pollutants, is seriously endangering people's Health and Living.CO catalytic oxidation has practical application widely, as: in fuel cell, the hydrogen-rich gas that utilizes methanol recapitalization to produce, and the CO containing in common this mixture can cause Pt catalyst poisoning, effectively selectively removes H
2in a small amount of CO gas of mixing, for the normal work of fuel cell, be very important.The various aspects such as the CO elimination in CO sensor, breathing mask and closed system all relate to the catalytic oxidation problem of CO.Therefore, efficient, the low cost CO catalyst for catalytic oxidation of research and development has wide industrial prospect.
For realizing the catalytic oxidation of CO, the selection of catalyst and preparation are vital.Before the eighties in last century, it is mainly the noble metal catalyst taking Pt, Pd as active component that CO is oxidized catalyst used, but can only be applicable to the catalytic oxidation that CO concentration is lower.Manganese and Cu oxide, inexpensive because of its cost, the many merits such as high activity and durability, are widely used in various important reactions, and China has compared with the manganese of horn of plenty and copper resource.In view of the catalytic activity that manganese and copper catalyst possess, develop can continuous and effective CO catalytic oxidation effective catalyst have great importance.
This project implementation obtains project of national nature science fund project (21277008); Project of national nature science fund project (20777005); The subsidy of Education Commission of Beijing development in science and technology plan general project (KM2013100050010) is also the research contents of these projects.
Summary of the invention
The object of this invention is to provide a kind of preparation of aluminium pillared montmorillonite load Cu-Mn catalyst and for CO catalytic oxidation pollutant, the catalyst providing can be oxidized CO being less than under 300 DEG C of reaction temperatures, and obtain higher CO conversion ratio, catalyst stability is high, and preparation technology is simple, raw material extensively exist at nature.
The preparation of aluminium pillared montmorillonite provided by the invention is catalyst carrier, and Cu-Mn is carried on aluminium pillared montmorillonite carrier and makes catalyst.With imvite and aluminium chloride be raw material, use copolymerization method prepare aluminium pillared montmorillonite carrier, utilize improved infusion process loaded Cu-Mn catalyst.Concrete preparation is achieved through the following technical solutions:
The preparation method of above-mentioned catalyst provided by the present invention, comprises the steps:
According to a certain percentage the imvite of purification is joined and in distilled water, stir into thick shape solution, wherein water: imvite (mass ratio)=(5～10): 1, taking subsequently a certain proportion of NaCl is added in above-mentioned slurries, wherein slurries: NaCl(mass ratio)=(90～100): 1, under 60～80 DEG C of conditions, react 1～3 hour, centrifuge washing 8～12 times subsequently, until without Cl
-detect, product is placed in to 120～140 DEG C and is dried 24～48 hours, make sodium imvite.
Under 60～80 DEG C of conditions of temperature, the NaOH solution of 0.1～0.3mol/L is added to the AlCl of 0.1～0.3mol/L with the speed of 1～2ml/min
3in solution, wherein ([Al
3+]: [OH
-] (mol ratio)=(1～3): 1), continue to stir 1～3 hour, put 22～26 hours gentle and quiet solution chamber subsequently, obtain aluminium pillaring agent.
By a certain percentage above-mentioned sodium imvite is joined in distilled water, in distilled water: sodium imvite (mass ratio)=100:(1～3)) ratio makes sodium imvite suspension slurry, at ambient temperature, above aluminium post liquid is dropwise dropped in sodium imvite suspension slurry to wherein sodium imvite (mass number): [Al
3+] (molal quantity)=1g:(3～7) mmol, under 50～70 DEG C of temperature conditions, sustained response 1～3 hour, at room temperature leaves standstill 22～26 hours, and centrifuge washing 4～7 times detects until without Cl
-, 120～140 DEG C of dry 20～24h, take out dried product and grind and sieve, and put it into subsequently in muffle furnace, rise to 300～500 DEG C with 1～2 DEG C/min heating rate, keep this temperature to calcine 1～3 hour, and gained sample is aluminium pillared montmorillonite.
2, immerse stain legal system for aluminium pillared montmorillonite load Cu and Mn catalyst
By Mn (NO
3)
24H
2o and Cu (NO
3)
26H
2o is dissolved in distilled water, is made into molar concentration and is respectively 7～9mol/L solution, and wherein the mol ratio of Mn and Cu is 1:1.Above manganese nitrate and copper nitrate mixed solution are added to aluminium pillared montmorillonite, wherein the mass ratio of MnO and aluminium pillared montmorillonite is (0.05～0.1): 1, stir 1～2 hour, at room temperature leave standstill 24～48 hours subsequently, 120～140 DEG C are dried 24～48 hours, then in Muffle furnace, are warming up to 400 DEG C～500 DEG C with 1～3 DEG C/min, and keep this temperature calcining 4～6 hours, obtain MnO-CuO/ montmorillonite catalyst.
(3) catalyst of the present invention, (60,000h under high-speed
-1～100,000h
-1), 1%CO concentration is had to higher catalytic oxidation activity: 1) MnO-CuO/ montmorillonite catalyst is completely oxidized to CO by CO in the time of 180 DEG C～270 DEG C
2, in 100 hours, keep ≈ 100%CO oxygenation efficiency; 2) raw material that Kaolinite Preparation of Catalyst uses and preparation process is simple to operation, low price.The present invention does not need additional any fuel, directly utilizes O in air
2for oxidant, have that raw material are economical and practical, use procedure energy consumption is low, easy and simple to handle, reaction condition is gentle, can reduce secondary pollution and can continuous operation etc. advantage.
Imvite is a kind of natural silicate clay mineral, there is large specific area, the commutative performance of good absorption property and interlayer cation, it is a kind of good catalyst carrier, aluminium pillared montmorillonite is that hydroxy Al ion is inserted into a kind of duct composite between cheating engaging layer, utilize its table specific area large, heat resistance high, it is carried out to Cu-Mn Metal Supported, obtain Cu-Mn support type aluminium pillared montmorillonite, this catalyst has larger specific area and pore structure equally, the features such as higher heat resistance, aspect processing atmosphere pollution especially benzo pollutants, showing good application prospect as catalyst.
Brief description of the drawings
The XRD figure of M, Na-M, Al-PILC, Cu/PILC, Mn/PILC and the Cu-Mn/PILC of Fig. 1 embodiment 1,2 and 3 preparations
Fig. 2 is the CO catalytic combustion activity figure of the Cu-Mn/PILC for preparing of the embodiment of the present invention 3
Fig. 3 is the CO stability of the Cu-Mn/PILC for preparing of the embodiment of the present invention 3
Detailed description of the invention
Embodiment 1
(1) preparation of aluminium pillared montmorillonite carrier
According to a certain percentage the imvite of purification is joined and in distilled water, stir into thick shape solution, water: imvite (mass ratio)=5:1, taking subsequently a certain proportion of NaCl is added in above-mentioned slurries, wherein slurries: NaCl(mass ratio)=90:1,60 DEG C of reactions 1 hour, centrifuge washing 8 times subsequently, until without Cl
-detect, product is placed in to 120 DEG C and is dried 24 hours, make sodium imvite.
In the time of 60 DEG C, the NaOH solution of 0.1mol/L is added to the AlCl of 0.1mol/L with the speed of 1ml/min
3in solution, wherein [Al
3+]: [OH
-] (mol ratio)=1:1, continue to stir 1 hour, put 22 hours gentle and quiet solution chamber subsequently, obtain aluminium pillaring agent.
By a certain percentage above-mentioned sodium imvite is joined in distilled water, in distilled water: sodium imvite (mass ratio)=100:1) ratio makes sodium imvite suspension slurry, at ambient temperature, above aluminium post liquid is dropwise dropped in sodium imvite suspension slurry to wherein sodium imvite (mass number): [Al
3+] (molal quantity)=1g:3mmol, sustained response 1 hour at 50 DEG C, at room temperature leaves standstill 22 hours, and centrifuge washing 4 times detects until without Cl
-, 120 DEG C of dry 20h, take out dried product and grind and sieve, and put it into subsequently in muffle furnace, rise to 300 DEG C with 1 DEG C/min heating rate, keep this temperature calcining 1 hour, and gained sample is aluminium pillared montmorillonite.
(2) immerse stain legal system for aluminium pillared montmorillonite load Mn catalyst
By Mn (NO
3)
24H
2o is dissolved in distilled water, is made into 7mol/L solution.In the situation that stirring, above manganese nitrate solution is added to aluminium pillared montmorillonite, wherein the mass ratio of MnO and aluminium pillared montmorillonite is 0.05:1, stir 1 hour, at room temperature leave standstill 24 hours subsequently, 120 DEG C are dried 24 hours, again in Muffle furnace, be warming up to 400 DEG C with 1 DEG C/min, and keep this temperature calcining 4 hours, obtain MnO/ montmorillonite catalyst.
(3) catalyst activity evaluation.The concentration of CO is 1%, and air speed is 60,000h
-1.Gas-chromatography TCD detection reaction tail gas CO content.100% of the obtained catalyst of the embodiment of the present invention 1 oxidation CO(CO transforms) temperature be 240 DEG C, when temperature is in the scope of 100 DEG C～200 DEG C, CO conversion ratio straight line raises until reach 100%.
Embodiment 2
(1) preparation of aluminium pillared montmorillonite carrier
According to a certain percentage the imvite of purification is joined and in distilled water, stir into thick shape solution, wherein water: imvite (mass ratio)=8:1, taking subsequently a certain proportion of NaCl is added in above-mentioned slurries, wherein slurries: NaCl(mass ratio)=95:1,70 DEG C of reactions 2 hours, centrifuge washing 10 times subsequently, until without Cl
-detect, product is placed in to 130 DEG C and is dried 36 hours, make sodium imvite.
Under temperature 70 C condition, the NaOH solution of 0.2mol/L is added in the extreme to the AlCl of 0.2mol/L with the speed of 1.5ml/min
3in solution, wherein [Al
3+]/[OH
-] (mol ratio)=2:1, continue to stir 2 hours, put 24 hours gentle and quiet solution chamber subsequently, obtain aluminium pillaring agent.
By a certain percentage above-mentioned sodium imvite is joined in distilled water, in distilled water: sodium imvite (mass ratio)=100:2 ratio is made sodium imvite suspension slurry, at ambient temperature, above aluminium post liquid is dropwise dropped in sodium imvite suspension slurry to wherein sodium imvite (mass number): [Al
3+] (molal quantity)=1g:5mmol, under 60 DEG C of temperature conditions, sustained response 2 hours, at room temperature leaves standstill 24 hours, and centrifuge washing 5 times detects until without Cl
-, 130 DEG C of dry 22h, take out dried product and grind and sieve, and put it into subsequently in muffle furnace, rise to 400 DEG C with 1.5 DEG C/min heating rate, keep this temperature calcining 2 hours, and gained sample is aluminium pillared montmorillonite.
(2) immerse stain legal system for aluminium pillared montmorillonite load Cu-Mn catalyst
By Mn (NO
3)
24H
2o and Cu (NO
3)
26H
2o is dissolved in distilled water, is made into molar concentration and is respectively 8mol/L solution, and wherein the mol ratio of Mn and Cu is 1.5:1.5.In the situation that stirring, above manganese nitrate and copper nitrate mixed solution are added to aluminium pillared montmorillonite, wherein the mass ratio of MnO and aluminium pillared montmorillonite is 0.08:1, stir 1.5 hours, at room temperature leave standstill 36 hours subsequently, 130 DEG C are dried 36 hours, again in Muffle furnace, be warming up to 450 DEG C with 2 DEG C/min, and keep this temperature calcining 5 hours, obtain MnO-CuO/ montmorillonite catalyst.
(3) catalyst activity evaluation.The concentration of CO is 1%, and air speed is 80,000h
-1.Gas-chromatography TCD detection reaction tail gas CO content.100% of the obtained catalyst of the embodiment of the present invention 1 oxidation CO(CO transforms) temperature be 180 DEG C, when temperature is in the scope of 100 DEG C～160 DEG C, CO conversion ratio straight line raises until reach 100%.
Embodiment 3
(1) preparation of aluminium pillared montmorillonite carrier
According to a certain percentage the imvite of purification is joined and in distilled water, stir into thick shape solution, water: imvite (mass ratio)=10:1, taking subsequently a certain proportion of NaCl is added in above-mentioned slurries, wherein slurries: NaCl(mass ratio)=100:1, under 80 DEG C of conditions, react 3 hours, centrifuge washing 12 times subsequently, until without Cl
-detect, product is placed in to 140 DEG C and is dried 48 hours, make sodium imvite.
Under 80 DEG C of conditions of temperature, the NaOH solution of 0.3mol/L is added in the extreme to the AlCl of 0.1～0.3mol/L with the speed of 2ml/min
3in solution, wherein [Al
3+]/[OH
-] (mol ratio)=3, continue to stir 3 hours, put 26 hours gentle and quiet solution chamber subsequently, obtain aluminium pillaring agent.
By a certain percentage above-mentioned sodium imvite is joined in distilled water, in distilled water: sodium imvite (mass ratio)=100:3 ratio is made sodium imvite suspension slurry, at ambient temperature, above aluminium post liquid is dropwise dropped in sodium imvite suspension slurry to wherein sodium imvite (mass number): [Al
3+] (molal quantity)=1g:7mmol, under 70 DEG C of temperature conditions, sustained response 3 hours, at room temperature leaves standstill 26 hours, and centrifuge washing 7 times detects until without Cl
-, 140 DEG C of dry 24h, take out dried product and grind and sieve, and put it into subsequently in muffle furnace, rise to 500 DEG C with 2 DEG C/min heating rate, keep this temperature calcining 3 hours, and gained sample is aluminium pillared montmorillonite.
(2) immerse stain legal system for aluminium pillared montmorillonite load Cu catalyst
By Cu (NO
3)
26H
2o is dissolved in distilled water, is made into 9mol/L solution.In the situation that stirring, above copper nitrate mixed solution is added to aluminium pillared montmorillonite, wherein the mass ratio of CuO and aluminium pillared montmorillonite is 0.05:1, stir 2 hours, at room temperature leave standstill 48 hours subsequently, 140 DEG C are dried 48 hours, again in Muffle furnace, be warming up to 500 DEG C with 3 DEG C/min, and keep this temperature calcining 6 hours, obtain MnO-CuO/ montmorillonite catalyst.
(3) catalyst activity evaluation.The concentration of CO is 1%, and air speed is 100,000h
-1.Gas-chromatography TCD detection reaction tail gas CO content.100% of the obtained catalyst of the embodiment of the present invention 1 oxidation CO(CO transforms) temperature be 270 DEG C, when temperature is in the scope of 100 DEG C～260 DEG C, CO conversion ratio straight line raises until reach 100%.
Claims (2)
1. a preparation method for aluminium pillared montmorillonite load Cu-Mn catalyst, is characterized in that:
Imvite is joined and in distilled water, stirs into slurries, wherein water: mass ratio=(5～10) of imvite: 1, taking subsequently NaCl is added in above-mentioned slurries, wherein, mass ratio=(90～100) of slurries: NaCl: 1, under 60～80 DEG C of conditions, react 1～3 hour, centrifuge washing 8～12 times subsequently, until without Cl
-detect, product is placed in to 120～140 DEG C and is dried 24～48 hours, make sodium imvite;
Under 60～80 DEG C of conditions of temperature, the NaOH solution of 0.1～0.3mol/L is added to the AlCl of 0.1～0.3mol/L with the speed of 1～2ml/min
3in solution, wherein [Al
3+]: [OH
-] mol ratio=(1～3): 1, continue stir 1～3 hour, put 22～26 hours gentle and quiet solution chamber subsequently, obtain aluminium pillaring agent;
Above-mentioned sodium imvite is joined in distilled water, in distilled water: mass ratio=100:(1～3 of sodium imvite) ratio makes sodium imvite suspension slurry, the drop of above aluminium pillaring agent is added in sodium imvite suspension slurry, wherein, sodium imvite: [Al
3+] add ratio=1g:(3～7) mmol, under 50～70 DEG C of temperature conditions, sustained response 1～3 hour, leaves standstill 22～26 hours, centrifuge washing 4～7 times detects until without Cl
-, 120～140 DEG C of dry 20～24h, take out dried product and grind and sieve, and put it into subsequently in muffle furnace, rise to 300～500 DEG C with 1～2 DEG C/min heating rate, keep this temperature to calcine 1～3 hour, and gained sample is aluminium pillared montmorillonite;
By Mn (NO
3)
24H
2o and Cu (NO
3)
26H
2o is dissolved in distilled water, is made into molar concentration 7～9mol/L solution respectively, and wherein the mol ratio of Mn and Cu is 1:1; In the situation that stirring, above manganese nitrate and copper nitrate mixed solution are added to aluminium pillared montmorillonite, wherein the mass ratio of MnO and aluminium pillared montmorillonite is (0.05～0.1): 1, stir 1～2 hour, leave standstill 24～48 hours subsequently, 120～140 DEG C are dried 24～48 hours, again in Muffle furnace, be warming up to 400 DEG C～500 DEG C with 1～3 DEG C/min, and keep this temperature calcining 4～6 hours, obtain MnO-CuO/ montmorillonite catalyst.
2. the catalyst that according to claim 1 prepared by method, in the application of CO catalytic oxidation, is characterized in that: above-mentioned catalyst is placed on and in continuous-flow fixed bed device, passes into CO and react with air Mixture.Reaction pressure is normal pressure～2MPa, and reaction velocity is 60,000h
-1～100,000h
-1, in air and CO gaseous mixture, the concentration of CO is 1%, 25～300 DEG C of reaction temperatures.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105540542A (en) * | 2015-12-07 | 2016-05-04 | 铜陵市明诚铸造有限责任公司 | Preparation process of Mn-Cu/Al-PILM deoxidizing agent |
| CN105709750A (en) * | 2014-12-04 | 2016-06-29 | 中国石油化工股份有限公司 | Copper pillared montmorillonite catalyst, and preparation method and application thereof |
| CN106861607A (en) * | 2017-03-17 | 2017-06-20 | 武汉理工大学 | A kind of preparation method of the modified carbon/montmorillonite Composite sorbing material of organic-inorganic |
| CN108290142A (en) * | 2015-11-24 | 2018-07-17 | 株式会社世Fa | The complex composition for pernicious gas removal containing copper-manganese catalyst |
| CN109482141A (en) * | 2018-12-22 | 2019-03-19 | 北京工业大学 | The preparation method and application of aluminium pillared montmorillonite load C a-Nb compound adsorbent |
| CN110013826A (en) * | 2018-12-22 | 2019-07-16 | 北京工业大学 | The preparation method and application of aluminium pillared montmorillonite load K-Nb or Mg-Nb compound adsorbent |
| CN115007125A (en) * | 2022-07-08 | 2022-09-06 | 湘潭大学 | Sepiolite-loaded manganese-cerium composite catalyst and preparation method and application thereof |
| CN115301243A (en) * | 2022-07-15 | 2022-11-08 | 西北大学 | Supported perovskite catalyst, preparation method and application thereof |
| CN116116387A (en) * | 2022-11-01 | 2023-05-16 | 邵阳学院 | Soil heavy metal adsorbent and preparation method thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105709750A (en) * | 2014-12-04 | 2016-06-29 | 中国石油化工股份有限公司 | Copper pillared montmorillonite catalyst, and preparation method and application thereof |
| CN105709750B (en) * | 2014-12-04 | 2018-01-16 | 中国石油化工股份有限公司 | A kind of copper pillared montmorillonite catalyst and its preparation method and application |
| CN108290142A (en) * | 2015-11-24 | 2018-07-17 | 株式会社世Fa | The complex composition for pernicious gas removal containing copper-manganese catalyst |
| CN108290142B (en) * | 2015-11-24 | 2021-04-27 | 株式会社世一Fa | Composite composition for harmful gas removal containing copper-manganese catalyst |
| CN105540542A (en) * | 2015-12-07 | 2016-05-04 | 铜陵市明诚铸造有限责任公司 | Preparation process of Mn-Cu/Al-PILM deoxidizing agent |
| CN106861607A (en) * | 2017-03-17 | 2017-06-20 | 武汉理工大学 | A kind of preparation method of the modified carbon/montmorillonite Composite sorbing material of organic-inorganic |
| CN110013826A (en) * | 2018-12-22 | 2019-07-16 | 北京工业大学 | The preparation method and application of aluminium pillared montmorillonite load K-Nb or Mg-Nb compound adsorbent |
| CN109482141A (en) * | 2018-12-22 | 2019-03-19 | 北京工业大学 | The preparation method and application of aluminium pillared montmorillonite load C a-Nb compound adsorbent |
| CN109482141B (en) * | 2018-12-22 | 2021-10-15 | 北京工业大学 | Preparation method and application of aluminum pillared montmorillonite-loaded Ca-Nb composite adsorbent |
| CN110013826B (en) * | 2018-12-22 | 2022-05-24 | 北京工业大学 | Preparation method and application of K-Nb or Mg-Nb composite adsorbent loaded by aluminum pillared montmorillonite |
| CN115007125A (en) * | 2022-07-08 | 2022-09-06 | 湘潭大学 | Sepiolite-loaded manganese-cerium composite catalyst and preparation method and application thereof |
| CN115301243A (en) * | 2022-07-15 | 2022-11-08 | 西北大学 | Supported perovskite catalyst, preparation method and application thereof |
| CN115301243B (en) * | 2022-07-15 | 2024-01-05 | 浙江聚泰新能源材料有限公司 | Supported perovskite catalyst, preparation method and application thereof |
| CN116116387A (en) * | 2022-11-01 | 2023-05-16 | 邵阳学院 | Soil heavy metal adsorbent and preparation method thereof |
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Application publication date: 20140618 |