CN102240576A - Method for preparing transitional metal/active carbon catalyst - Google Patents
Method for preparing transitional metal/active carbon catalyst Download PDFInfo
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- CN102240576A CN102240576A CN2011101359592A CN201110135959A CN102240576A CN 102240576 A CN102240576 A CN 102240576A CN 2011101359592 A CN2011101359592 A CN 2011101359592A CN 201110135959 A CN201110135959 A CN 201110135959A CN 102240576 A CN102240576 A CN 102240576A
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- ion exchange
- exchange resin
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Abstract
The invention discloses a method for preparing a transitional metal/active carbon catalyst and belongs to the technical field of burnt gas chemical treatment and application. The preparation method comprises a step of loading an ion exchange resin and a step of carbonizing the ion exchange resin. The catalyst preparation method provided by the invention has the advantages of simple, convenient and easy operation, readily available raw material and low cost; and the load rate of the prepared transitional metal/active carbon catalyst is over 50 percent which is 10 to 40 times higher than that of a catalyst prepared by the common immersion method. The transitional metal/active carbon catalyst prepared by the invention, besides retaining the spherical shape of the original ion exchange resin, also has the advantages of uniform particle size distribution, smooth surface, uniform distribution of the transitional metal in and on the surface of the active carbon, and the like.
Description
Technical field
The invention belongs to burnt gas chemical treatment applied technical field, be specifically related to a kind of method for preparing transition metal/activated-carbon catalyst.
Background technology
Because absorbent charcoal carrier has very large specific area and pore volume, and characteristic such as adsorptivity is strong, be applied to PCBs with the field is disposed in the processing of bioxin, metal/activated-carbon catalyst is used for the existing research of decomposition of bioxin, traditional infusion process of preparation metal/active carbon is carried out the excessive dipping dry carbonization in back with metal salt solution to active carbon and is got, but the resulting catalyst loadings of this method is low, its active room for promotion also thereby be restricted, therefore be necessary to explore the catalyst of new metal/activated-carbon catalyst preparation method, further improve the activity of metal/activated-carbon catalyst in order to preparation high capacity amount.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing transition metal/activated-carbon catalyst, improve the load capacity of transition metal, and then improve the catalytic activity of transition metal/activated-carbon catalyst.The preparation method of concrete transition metal/activated-carbon catalyst realizes by following steps:
The first step, the load of ion exchange resin;
Concrete carrying method is: get a certain amount of ion exchange resin and soak 4～6h with deionized water, to remove water-solubility impurity wherein, place within the ion exchange column then, preparation contains the ammonia spirit of a certain amount of transition metal sulfate, flow with 10～50mL/min carries out ion-exchange 1～2h to ion exchange resin, ion exchange resin after exchange finishes is cleaned with deionized water, then at 70 ℃ baking oven inner drying 24h, promptly obtains the ion exchange resin of transition metal in the load.
Second step, the carbonization of ion exchange resin;
The method of described ion exchange resin carbonization is: put into quartz ampoule after containing the ion exchange resin of transition metal in the above-mentioned load in high temperature resistant porcelain boat, first through-current capacity is the N of 300mL/min before the carbonization
2The anaerobic environment of 30min when guaranteeing carbonization, open tube furnace then, with the speed heat temperature raising to 500 of 10 ℃/min ℃, and keep 20min in order to carbonization to resin, quartz ampoule is terminal to absorb processing with absolute ethyl alcohol and active carbon to tail gas, carbonization finishes the back and continues under anaerobic to be cooled to room temperature, can obtain transition metal/activated-carbon catalyst.
Described ion exchange resin is weak-acid ion exchange resin.
The invention has the advantages that:
(1) method for preparing catalyst provided by the invention is easy to operation, and original material is easy to get, and cost is low;
(2) transition metal of gained of the present invention/activated-carbon catalyst load factor reaches more than 50%, and is higher 10～40 times than the resulting catalyst cupport rate of common infusion process;
(3) transition metal/activated-carbon catalyst of the present invention preparation is except the spherical morphology that keeps original ion exchange resin, has also that particle diameter is evenly distributed, catalyst surface is smooth and transition metal is evenly distributed on advantages such as active carbon inside and surface.
Description of drawings
Fig. 1 is the high temperature cabonization device schematic diagram of ion exchange resin;
Fig. 2 a and 2b are 500 times and 10000 times of sem photographs of the zinc/active carbon of novel ion-exchange preparation;
Fig. 2 c and 2d are 500 times and 10000 times of sem photographs of the nickel/active carbon of novel ion-exchange preparation;
Fig. 2 e and 2f are 500 times and 10000 times of sem photographs of the copper/active carbon of novel ion-exchange preparation;
Fig. 3 is the surface and the inner EDAX results of the zinc/active carbon of novel ion-exchange preparation;
Fig. 4 is the inside EDAX results of the nickel/active carbon of novel ion-exchange preparation;
Fig. 5 is the inside EDAX results of the copper/active carbon of novel ion-exchange preparation.
The specific embodiment
Preparation method to transition metal/activated-carbon catalyst provided by the invention is elaborated below in conjunction with accompanying drawing and example.
Described preparation method realizes as follows:
The first step, the load of ion exchange resin;
Get a certain amount of ion exchange resin and soak 4～6h with deionized water, to remove water-solubility impurity wherein, place within the ion exchange column then, preparation contains the ammonia spirit of a certain amount of transition metal sulfate, flow with 10～50mL/min carries out ion-exchange 1～2h to ion exchange resin, ion exchange resin after exchange finishes is cleaned with deionized water, then at 70 ℃ baking oven inner drying 24h, promptly obtains the ion exchange resin of transition metal in the load.
Second step, the carbonization of ion exchange resin;
The carbonization of described ion exchange resin is carried out in the high temperature cabonization device, described high temperature cabonization device comprises high pure nitrogen bottle 1, spinner flowmeter 2, quartz tube furnace 3, quartz ampoule 4 and porcelain boat 5, described high pure nitrogen bottle is arranged on the porch of quartz tube furnace 3, be used to and quartz ampoule 4 be set in the quartz tube furnace 3 high pure nitrogen is provided, quartz ampoule 4 inside are porcelain boat 5, be used to hold the ion exchange resin that needs carbonization in the porcelain boat 5, exit at quartz tube furnace 3 is connected with ice-water bath in turn, absolute ethyl alcohol and active carbon are used for the gas after the carbonization is absorbed.
Put into quartz ampoule 4 after containing the ion exchange resin of transition metal in the above-mentioned load in high temperature resistant porcelain boat 5, as shown in Figure 1, feeding flow earlier in quartz ampoule 4 before the carbonization is the N of 300mL/min
2The anaerobic environment of 30min when guaranteeing carbonization opened quartz tube furnace 3 then, with the speed heat temperature raising to 500 of 10 ℃/min ℃, and keeps 20min in order to the carbonization to ion exchange resin.Gas after the carbonization passes through ice-water bath 6, absolute ethyl alcohol 7 and the active carbon 8 of the end of quartz tube furnace 3 successively, realizes the absorption of tail gas is handled.Carbonization finishes the back and continues under anaerobic to be cooled to room temperature, can obtain transition metal/activated-carbon catalyst.
Described ion exchange resin is weak-acid ion exchange resin.
The invention provides a kind of preparation method of transition metal/activated-carbon catalyst, is example with transition metal zinc/active carbon, mainly comprises the steps to realize:
The first step, the load of ion exchange resin, concrete steps are:
(1) take by weighing 5g weak-acid cation-exchange resin (WK-11, Mitsubishi chemical industry), its structural formula is as follows:
Soak 4h to remove the water-solubility impurity that contains in the resin with the 100mL deionized water.
(2) preparation contains the ammonia spirit of a certain amount of zinc sulfate, comprises 10gZnSO
47H
2O, 100mL deionized water and 100mL mass fraction are 15% ammoniacal liquor.
(3) soaked ion exchange resin is filled in the ion exchange column, the flow of pressing 50mL/min with the ammonia spirit of zinc sulfate is to resin circulation exchange 2h.
(4) exchange finish the back with deionized water with load the resin of zinc clean, place 70 ℃ baking oven inner drying 24h then.
Table one
Annotate: catalyst loadings is represented with the quality of unit mass catalyst cupport transition metal.
Second step, the carbonization of ion exchange resin, concrete grammar is:
(1) good resin is contained in high temperature resistant porcelain boat 5 to get a certain amount of drying, puts into quartz ampoule 4 then and places quartz tube furnace 3, and the control nitrogen flow is 300mL/min, continue to feed nitrogen 30min required anaerobic environment when making carbonization.
(2) open quartz tube furnace 3, with the speed heat temperature raising to 500 of 10 ℃/min ℃, resin is carried out high temperature cabonization 20min, carbonization finishes the back and continues under anaerobic to be cooled to room temperature and get final product.As shown in Table 1, the zinc that obtains/activated carbon supported amount 502.8mg/g is compared catalyst prepared 46.04mg/g and is exceeded more than 50 times.Shown in Fig. 2 a, 2b, the catalyst microscopic pattern is spherical, even particle distribution, and catalyst surface is smooth.The surface and the inner EDAX results of the catalyst that shown in Figure 3 is prepares, the result is presented in catalyst contained three kinds of essential element C, O and the Zn total amount, and the mass ratio of Zn is 59.3%～76.7%, and the Zn content of diverse location is up to more than 50%.
Present embodiment is elaborated with the example that is prepared as of transiting metal nickel/activated-carbon catalyst, mainly realizes as follows:
The first step, the load of ion exchange resin, concrete steps are:
(1) take by weighing 5g weak-acid cation-exchange resin (WK-11, Mitsubishi chemical industry), its structural formula soaks 4h to remove the water-solubility impurity that contains in the resin with embodiment 1 with the 100mL deionized water.
(2) preparation contains the ammonia spirit of a certain amount of nickelous sulfate, comprises 10.5gNiS0
46H
2O, 100mL deionized water and 100mL mass fraction are 15% ammoniacal liquor.
(3) soaked ion exchange resin is filled in the ion exchange column, the flow of pressing 50mL/min with the ammonia spirit of nickelous sulfate is to resin circulation exchange 2h.
(4) exchange finish the back with deionized water with load the resin of nickel clean, place 70 ℃ baking oven inner drying 24h then.
Second step, the carbonization of ion exchange resin, concrete grammar is:
(1) good resin is contained in high temperature resistant porcelain boat 5 to get a certain amount of drying, puts into quartz ampoule 4 then and places quartz tube furnace 3, and the control nitrogen flow is 300mL/min, continue to feed nitrogen 30min required anaerobic environment when making carbonization.
(2) open quartz tube furnace 3, with the speed heat temperature raising to 500 of 10 ℃/min ℃, resin is carried out high temperature cabonization 20min, carbonization finishes the back and continues under anaerobic to be cooled to room temperature and get final product.As shown in Table 1, the nickel that obtains/activated carbon supported amount is up to 542.5mg/g, and the 11.995mg/g that compares infusion process gained nickel/activated-carbon catalyst exceeds nearly 50 times.Shown in Fig. 2 c, 2d, the catalyst microscopic pattern is spherical, even particle distribution, and catalyst surface is smooth.The inside EDAX results of the catalyst that shown in Figure 4 is prepares, result are presented among catalyst contained three kinds of essential element C, the O and Ni, and the mass ratio of Ni is 46.13%～80.6%, and is minimum near 50%, reaches as high as more than 80%.
Present embodiment is elaborated with the example that is prepared as of transition metal copper/activated-carbon catalyst, mainly realizes as follows:
The first step, the load of ion exchange resin, concrete steps are:
(1) take by weighing 5g weak-acid cation-exchange resin (WK-11, Mitsubishi chemical industry), its structural formula soaks 4h to remove the water-solubility impurity that contains in the resin with embodiment 1 with the 100mL deionized water.
(2) preparation contains the ammonia spirit of a certain amount of copper sulphate, comprises 10gCuSO
45H
2O, 100mL deionized water and 100mL mass fraction are 15% ammoniacal liquor.
(3) soaked ion exchange resin is filled in the ion exchange column, the flow of pressing 50mL/min with the ammonia spirit of copper sulphate is to resin circulation exchange 2h.
(4) exchange finish the back with deionized water with load the resin of copper clean, place 70 ℃ baking oven inner drying 24h then.
Second step, the carbonization of ion exchange resin, concrete grammar is:
(1) good resin is contained in high temperature resistant porcelain boat 5 to get a certain amount of drying, puts into quartz ampoule 4 then and places tube furnace 3, and the control nitrogen flow is 300mL/min, continue to feed nitrogen 30min required anaerobic environment when making carbonization.
(2) open quartz tube furnace, with the speed heat temperature raising to 500 of 10 ℃/min ℃, resin is carried out high temperature cabonization 20min, carbonization finishes the back and continues under anaerobic to be cooled to room temperature and get final product.As shown in Table 1, the copper that obtains/activated carbon supported amount is up to 557.3mg/g, and the 12.86mg/g that compares infusion process gained copper/activated-carbon catalyst exceeds nearly 50 times.Shown in Fig. 2 e, 2f, the catalyst microscopic pattern is spherical, even particle distribution, and catalyst surface is smooth.The inside EDAX results of the catalyst that shown in Figure 5 is prepares, the result is presented among contained essential element C of catalyst and the Cu, and the mass ratio of Cu is 57.34%～65.93%, all more than 50%.
In addition, the sulfate of transition metal iron, cobalt and palladium also can be used as the present invention and prepares selection of catalysts.
Claims (6)
1. a method for preparing transition metal/activated-carbon catalyst is characterized in that comprising the steps:
The first step, the load of ion exchange resin;
Get ion exchange resin and soak 4～6h with deionized water, to remove water-solubility impurity wherein, place within the ion exchange column then, the ammonia spirit of preparation transition metal sulfate, flow with 10～50mL/min carries out ion-exchange 1～2h to ion exchange resin, ion exchange resin after exchange finishes is cleaned with deionized water, then at 70 ℃ baking oven inner drying 24h, promptly obtains the ion exchange resin of transition metal in the load;
Second step, the carbonization of ion exchange resin;
Put into quartz ampoule after containing the ion exchange resin of transition metal in the above-mentioned load in high temperature resistant porcelain boat, first through-current capacity is the N of 300mL/min before the carbonization
2The anaerobic environment of 30min when guaranteeing carbonization, open quartz tube furnace then, with the speed heat temperature raising to 500 of 10 ℃/min ℃, and keep 20min in order to carbonization to ion exchange resin, quartz ampoule is terminal to absorb processing with cold bath, absolute ethyl alcohol and active carbon to tail gas, carbonization finishes the back and continues under anaerobic to be cooled to room temperature, promptly obtains transition metal/activated-carbon catalyst.
2. the method for preparing transition metal/activated-carbon catalyst according to claim 1 is characterized in that: described ion exchange resin is weak-acid ion exchange resin.
3. the method for preparing transition metal/activated-carbon catalyst according to claim 1 is characterized in that: described transition metal sulfate is zinc sulfate, copper sulphate, nickelous sulfate, ferric sulfate, cobaltous sulfate or palladium sulfate.
4. the method for preparing transition metal/activated-carbon catalyst according to claim 1 is characterized in that: the ammonia spirit of described sulfate is that 10g sulfate, 100mL deionized water and 100mL mass fraction are 15% ammoniacal liquor.
5. the method for preparing transition metal/activated-carbon catalyst according to claim 1 is characterized in that: described transition metal/activated-carbon catalyst load factor reaches 50%, and ion exchange resin is spherical morphology.
6. high temperature cabonization device that is used to realize the carbonization of the described ion exchange resin of claim 1, it is characterized in that: described high temperature cabonization device comprises the high pure nitrogen bottle, spinner flowmeter, quartz tube furnace, quartz ampoule and porcelain boat, described high pure nitrogen bottle is arranged on the porch of quartz tube furnace, be used to and quartz ampoule be set in the quartz tube furnace high pure nitrogen is provided, quartz ampoule 4 inside are porcelain boat, be used to hold the ion exchange resin that needs carbonization in the porcelain boat, exit at quartz tube furnace is connected with ice-water bath in turn, absolute ethyl alcohol and active carbon are used for the gas after the carbonization is absorbed.
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Cited By (10)
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| CN103100300A (en) * | 2013-01-30 | 2013-05-15 | 北京航空航天大学 | Double-element metal active carbon catalyst thermo-catalytic degradation method for polychlorinated biphenyl in gaseous phase |
| CN103157473A (en) * | 2013-03-27 | 2013-06-19 | 北京林业大学 | Methanol cracking catalyst and preparation method thereof |
| CN103394354A (en) * | 2013-08-22 | 2013-11-20 | 神华集团有限责任公司 | Catalyst loaded on carbon sphere and preparation method of catalyst |
| CN106348280A (en) * | 2016-10-21 | 2017-01-25 | 南通绿业中试技术研究院有限公司 | Preparation method for spherical porous carbon |
| CN108609714A (en) * | 2018-03-21 | 2018-10-02 | 四川大学 | A method of removing incretion interferent in water removal using carbon-based magnetic metal composite material catalyzing activation persulfate |
| CN108640248A (en) * | 2018-03-21 | 2018-10-12 | 四川大学 | A method of removing estrogen in water removal using based on carbon-based Armco magnetic iron cobalt dual-metal material activation peroxy-monosulfate |
| CN110404504A (en) * | 2018-04-26 | 2019-11-05 | 西北大学 | Cu for handling dyeing and printing sewage adulterates walnut shell active carbon and its preparation method and application |
| CN111468093A (en) * | 2020-05-28 | 2020-07-31 | 沈阳师范大学 | Preparation method of carbon nano tube monolithic catalyst |
| CN111715308A (en) * | 2020-06-10 | 2020-09-29 | 安庆师范大学 | ZnO/carbonized ion exchange resin and preparation method thereof |
| CN111790379A (en) * | 2020-07-17 | 2020-10-20 | 安庆师范大学 | Silver-carbonized resin compound and preparation method thereof |
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| CN103100300A (en) * | 2013-01-30 | 2013-05-15 | 北京航空航天大学 | Double-element metal active carbon catalyst thermo-catalytic degradation method for polychlorinated biphenyl in gaseous phase |
| CN103100300B (en) * | 2013-01-30 | 2014-07-30 | 北京航空航天大学 | Double-element metal active carbon catalyst thermo-catalytic degradation method for polychlorinated biphenyl in gaseous phase |
| CN103157473A (en) * | 2013-03-27 | 2013-06-19 | 北京林业大学 | Methanol cracking catalyst and preparation method thereof |
| CN103394354A (en) * | 2013-08-22 | 2013-11-20 | 神华集团有限责任公司 | Catalyst loaded on carbon sphere and preparation method of catalyst |
| CN103394354B (en) * | 2013-08-22 | 2015-08-05 | 神华集团有限责任公司 | A kind of load Synthetic holography Fe-series catalyst on carbon ball and preparation method thereof |
| CN106348280A (en) * | 2016-10-21 | 2017-01-25 | 南通绿业中试技术研究院有限公司 | Preparation method for spherical porous carbon |
| CN108609714A (en) * | 2018-03-21 | 2018-10-02 | 四川大学 | A method of removing incretion interferent in water removal using carbon-based magnetic metal composite material catalyzing activation persulfate |
| CN108640248A (en) * | 2018-03-21 | 2018-10-12 | 四川大学 | A method of removing estrogen in water removal using based on carbon-based Armco magnetic iron cobalt dual-metal material activation peroxy-monosulfate |
| CN108609714B (en) * | 2018-03-21 | 2020-07-24 | 四川大学 | Method for removing endocrine disruptors in water by catalytically activating persulfate through carbon-based magnetic metal composite material |
| CN108640248B (en) * | 2018-03-21 | 2020-11-13 | 四川大学 | Method for removing estrogen in water by activating peroxymonosulfate based on carbon-based magnetic iron-cobalt bimetallic material |
| CN110404504A (en) * | 2018-04-26 | 2019-11-05 | 西北大学 | Cu for handling dyeing and printing sewage adulterates walnut shell active carbon and its preparation method and application |
| CN110404504B (en) * | 2018-04-26 | 2021-09-28 | 西北大学 | Cu-doped walnut shell activated carbon for treating printing and dyeing sewage and preparation method and application thereof |
| CN111468093A (en) * | 2020-05-28 | 2020-07-31 | 沈阳师范大学 | Preparation method of carbon nano tube monolithic catalyst |
| CN111715308A (en) * | 2020-06-10 | 2020-09-29 | 安庆师范大学 | ZnO/carbonized ion exchange resin and preparation method thereof |
| CN111790379A (en) * | 2020-07-17 | 2020-10-20 | 安庆师范大学 | Silver-carbonized resin compound and preparation method thereof |
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