CN103263933A - Noble metal-doped active carbon catalyst - Google Patents
Noble metal-doped active carbon catalyst Download PDFInfo
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- CN103263933A CN103263933A CN2013102235990A CN201310223599A CN103263933A CN 103263933 A CN103263933 A CN 103263933A CN 2013102235990 A CN2013102235990 A CN 2013102235990A CN 201310223599 A CN201310223599 A CN 201310223599A CN 103263933 A CN103263933 A CN 103263933A
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Abstract
The invention relates to a noble metal-doped active carbon catalyst which can be used for effectively solving the problem that an existing wastewater catalyst is poor in use effect. The catalyst is prepared by mixing carbon and noble metals palladium Pd, platinum pt, ruthenium Ru and nickel Ni, wherein the weight ratio of Pd, pt, Ru and Ni is (90-96):(1-3):1:3:(1-3). The preparation method comprises the following steps: soaking active carbon in an ethylene diamine tetraacetic acid sodium salt liquid for soaking and pre-treatment, and filtering after soaking for 1-2 hours; then, preparing carbon slurry till no precipitate is generated; adding the novel metals into a nitrate liquor or a chloride salt liquor according to the weight ratio of carbon and noble metals; then, adding the liquor to the carbon slurry; stirring for 3-5 hours at 25-80 DEG C; then, adding an alkaline aqueous liquor at 25-70 DEG V; adjusting the pH value of the reaction liquid to 7-8; insulating and stirring for 1-2 hours at 25-70 DEG C to obtain slurry; and then calcining to obtain the active carbon-loaded noble metal catalyst which is novel and unique, and strong in dirt-removing power to wastewater and high in efficiency.
Description
One, technical field
The present invention relates to catalyst, particularly a kind of activated-carbon catalyst of doped precious metal.
Two, background technology
In use there is following problem in the catalyst that uses in sewage disposal at present, and the amount of reagent of use is many, and excessive use can increase the COD in the processed waste water, and may produce secondary pollution; Mineralization of organic material is insufficient, and the intermediate product of formation often toxicity is bigger; For eliminating the bigger intermediate product of some toxicity, need carry out the process that first acidifying is alkalized again, in fact this process has added salt, reduces biodegradability; The operating cost of system is higher; Service life is short; Power of regeneration is very poor, and therefore, improvement and the innovation of disposing of sewage with catalyst are the problems of needing solution badly.
Three, summary of the invention
At above-mentioned situation, for overcoming the defective of prior art, the present invention's purpose just provides a kind of activated-carbon catalyst of doped precious metal, can effectively solve the bad problem of existing waste water catalyst result of use.
The technical scheme of its solution is, the present invention is by charcoal and precious metal palladium Pd, platinum pt, ruthenium Ru and nickel mix, charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel is 90-96: 1-3: 1-3: 1-3: 1-3, the preparation method is, active carbon is immersed in the disodium EDTA aqueous solution soaks preliminary treatment, soak time is 1-2 hour, afterwards active carbon is leached, then pretreated absorbent charcoal carrier and water are mixed and made into the charcoal slurries, reach not take place to be precipitated as standard, be saturation state, according to charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel adds above-mentioned noble metal in nitrate solution or the chlorate aqueous solution, nitrate solution or the chlorate aqueous solution that will contain noble metal afterwards join in the charcoal slurries, stir 3～5h down at 25～80 ℃, under 25～70 ℃ of conditions, add alkaline aqueous solution again, conditioned reaction liquid pH value to 7～8, at 25～70 ℃ of insulated and stirred 1～2h, obtain slurries, calcining obtains activated carbon supported noble metal catalyst then.
The present invention is novel unique, and is strong to the dirt-removing power of waste water, the efficient height.
Four, the specific embodiment
Be described in further details below in conjunction with the specific embodiment of the present invention of embodiment.
Embodiment 1
The present invention is by charcoal and precious metal palladium Pd, platinum pt, ruthenium Ru and nickel mix, charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel is 90: 1: 1: 1: 1, the preparation method is, active carbon is immersed in carries out preliminary treatment in the disodium EDTA aqueous solution, soak time is 1-2 hour, afterwards active carbon is leached, then pretreated absorbent charcoal carrier and water are mixed and made into the charcoal slurries, reach not take place to be precipitated as standard, it is saturation state, according to charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel, add above-mentioned noble metal in nitrate solution or the chlorate aqueous solution, nitrate solution or the chlorate aqueous solution that will contain noble metal afterwards join in the charcoal slurries, stir 3～5h down at 25～80 ℃, under 25～70 ℃ of conditions, add alkaline aqueous solution again, conditioned reaction liquid pH value to 7～8 at 25～70 ℃ of insulated and stirred 1～2h, obtain slurries, calcining obtains activated carbon supported noble metal catalyst then.
Embodiment 2
The present invention is by charcoal and precious metal palladium Pd, platinum pt, ruthenium Ru and nickel mix, charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel is 93: 2: 2: 2: 2, the preparation method is, active carbon is immersed in carries out preliminary treatment in the disodium EDTA aqueous solution, soak time is 1-2 hour, afterwards active carbon is leached, then pretreated absorbent charcoal carrier and water are mixed and made into the charcoal slurries, reach not take place to be precipitated as standard, it is saturation state, according to charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel, add above-mentioned noble metal in nitrate solution or the chlorate aqueous solution, nitrate solution or the chlorate aqueous solution that will contain noble metal afterwards join in the charcoal slurries, stir 3～5h down at 25～80 ℃, under 25～70 ℃ of conditions, add alkaline aqueous solution again, conditioned reaction liquid pH value to 7～8 at 25～70 ℃ of insulated and stirred 1～2h, obtain slurries, calcining obtains activated carbon supported noble metal catalyst then.
Embodiment 3
The present invention is by charcoal and precious metal palladium Pd, platinum pt, ruthenium Ru and nickel mix, charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel is 96: 3: 3: 3: 3, the preparation method is, active carbon is immersed in the disodium EDTA aqueous solution soaks preliminary treatment, soak time is 1-2 hour, afterwards active carbon is leached, then pretreated active carbon and water are mixed and made into the charcoal slurries, reach not take place to be precipitated as standard, state namely reaches capacity, according to charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel, add above-mentioned noble metal in nitrate solution or the chlorate aqueous solution, nitrate solution or the chlorate aqueous solution that will contain noble metal afterwards join in the charcoal slurries, stir 3～5h down at 25～80 ℃, under 25～70 ℃ of conditions, add alkaline aqueous solution again, conditioned reaction liquid pH value to 7～8 at 25～70 ℃ of insulated and stirred 1～2h, obtain slurries, calcining obtains activated carbon supported noble metal catalyst then.
The processing procedure of active carbon of the present invention is:
1, drying stage
At first timber is placed in the dryer; under temperature 120-150 degree centigrade, pyrolysis rate is very slow, mainly is that contained humidity relies on the outside heat of supplying with to evaporate in the timber; making its water content is 0.1%-1%, and the chemical composition of wood materials does not change.
2, the pre-charing stage
In retort, be under the 150-275 ℃ of condition in temperature, heated 2-3 hour, the wood materials pyrolysis is apparent in view, the wood materials chemical composition begins to change, wherein unstable components is decomposed materials such as generating carbon dioxide, carbon monoxide and little acetic acid as hemicellulose, reaches the state that a large amount of impurity separate;
More than two stages all want the extraneous heat of supplying with to guarantee the rising of pyrolysis temperature, so be called the endothermic decomposition stage again.
3, the charing stage
In retort, be under the 275-400 degrees celsius in temperature, 2-3 hour heat time heating time, in this stage, wood materials carries out thermal decomposition sharp, generates a large amount of catabolites; Contain a large amount of acetic acid, methyl alcohol and wood tar in the product liquid that generates, carbon dioxide content reduces gradually in the gaseous product that generates, and imflammable gas such as methane, ethene increase gradually, and this stage is emitted a large amount of reaction heat, so be called the exothermic reaction stage again.
4, calcination stage
In calcining kiln, under temperature 450-500 ℃ condition, to heat 4-5 hour, this stage relies on the outside heat of supplying with to carry out the calcining of charcoal, discharges the volatile materials that remains in the charcoal, improves the fixed carbon content of charcoal, contains charcoal purity more than 95%.
Should be pointed out that because each position received heat difference of charing equipment, the thermal conductivity factor of wood materials is less again, therefore, the residing position of wood materials difference in the equipment, even bolt timber is inside and outside, also may be in different pyrolysis phase.
Advantage of the present invention is:
1, the noble metal active Pd/carbon catalyst that mixed can have good effect of removing to the larger molecular organics in the waste water;
2, doped precious metal activated-carbon catalyst, course of reaction have HO to generate, and be almost not selective to organic matter degradation, and the pollutant levels scope is not required yet;
3, doped precious metal activated-carbon catalyst, reaction speed is fast, most organic matters in this process oxidation rate up to 106-109m-1s-1;
4, doped precious metal activated-carbon catalyst, the HO that reaction generates can bring out chain reaction, under appropriate reaction conditions, the thorough mineralising of organic matter can not produced new pollutant;
5, doped precious metal activated-carbon catalyst, can with the mutual coupling of other high-level oxidation technologies, also can with technology couplings such as biology, materialization; Particularly as the preliminary treatment of biological treatment, can significantly improve the biodegradability of waste water, improve the degradation efficiency of subsequent treatment greatly;
6, doped precious metal activated-carbon catalyst, operating process is controlled easily, can operate adjustment according to handling needs;
7, doped precious metal activated-carbon catalyst, can reach 3-5 service life, can remain higher removal efficient;
8, doped precious metal activated-carbon catalyst can reclaiming, and long-range consideration greatly reduces the operating cost of wastewater treatment;
9, doped precious metal activated-carbon catalyst device therefor floor space is little, covert saving the cost of wastewater treatment drop into.
Claims (4)
1. the activated-carbon catalyst of a doped precious metal, by charcoal and precious metal palladium Pd, platinum pt, ruthenium Ru and nickel mix, charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel is 90-96: 1-3: 1-3: 1-3: 1-3, the preparation method is, active carbon is immersed in the disodium EDTA aqueous solution soaks preliminary treatment, soak time is 1-2 hour, afterwards active carbon is leached, then pretreated absorbent charcoal carrier and water are mixed and made into the charcoal slurries, reach not take place to be precipitated as standard, be saturation state, according to charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel adds above-mentioned noble metal in nitrate solution or the chlorate aqueous solution, nitrate solution or the chlorate aqueous solution that will contain noble metal afterwards join in the charcoal slurries, stir 3～5h down at 25～80 ℃, under 25～70 ℃ of conditions, add alkaline aqueous solution again, conditioned reaction liquid pH value to 7～8, at 25～70 ℃ of insulated and stirred 1～2h, obtain slurries, calcining obtains activated carbon supported noble metal catalyst then.
2. the present invention is by charcoal and precious metal palladium Pd, platinum pt, ruthenium Ru and nickel mix, charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel is 90: 1: 1: 1: 1, the preparation method is, active carbon is immersed in carries out preliminary treatment in the disodium EDTA aqueous solution, soak time is 1-2 hour, afterwards active carbon is leached, then pretreated absorbent charcoal carrier and water are mixed and made into the charcoal slurries, reach not take place to be precipitated as standard, it is saturation state, according to charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel, add above-mentioned noble metal in nitrate solution or the chlorate aqueous solution, nitrate solution or the chlorate aqueous solution that will contain noble metal afterwards join in the charcoal slurries, stir 3～5h down at 25～80 ℃, under 25～70 ℃ of conditions, add alkaline aqueous solution again, conditioned reaction liquid pH value to 7～8 at 25～70 ℃ of insulated and stirred 1～2h, obtain slurries, calcining obtains activated carbon supported noble metal catalyst then.
3. the present invention is by charcoal and precious metal palladium Pd, platinum pt, ruthenium Ru and nickel mix, charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel is 93: 2: 2: 2: 2, the preparation method is, active carbon is immersed in carries out preliminary treatment in the disodium EDTA aqueous solution, soak time is 1-2 hour, afterwards active carbon is leached, then pretreated absorbent charcoal carrier and water are mixed and made into the charcoal slurries, reach not take place to be precipitated as standard, it is saturation state, according to charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel, add above-mentioned noble metal in nitrate solution or the chlorate aqueous solution, nitrate solution or the chlorate aqueous solution that will contain noble metal afterwards join in the charcoal slurries, stir 3～5h down at 25～80 ℃, under 25～70 ℃ of conditions, add alkaline aqueous solution again, conditioned reaction liquid pH value to 7～8 at 25～70 ℃ of insulated and stirred 1～2h, obtain slurries, calcining obtains activated carbon supported noble metal catalyst then.
4. the present invention is by charcoal and precious metal palladium Pd, platinum pt, ruthenium Ru and nickel mix, charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel is 96: 3: 3: 3: 3, the preparation method is, active carbon is immersed in the disodium EDTA aqueous solution soaks preliminary treatment, soak time is 1-2 hour, afterwards active carbon is leached, then pretreated active carbon and water are mixed and made into the charcoal slurries, reach not take place to be precipitated as standard, state namely reaches capacity, according to charcoal and palladium Pd, platinum pt, the weight ratio of ruthenium Ru and nickel, add above-mentioned noble metal in nitrate solution or the chlorate aqueous solution, nitrate solution or the chlorate aqueous solution that will contain noble metal afterwards join in the charcoal slurries, stir 3～5h down at 25～80 ℃, under 25～70 ℃ of conditions, add alkaline aqueous solution again, conditioned reaction liquid pH value to 7～8 at 25～70 ℃ of insulated and stirred 1～2h, obtain slurries, calcining obtains activated carbon supported noble metal catalyst then.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437361A (en) * | 2014-10-24 | 2015-03-25 | 东华大学 | Method for preparing functional biological carbon by in-situ impregnation |
| CN106219727A (en) * | 2016-08-17 | 2016-12-14 | 河北莫兰斯环境科技股份有限公司 | A kind of technique of efficient catalytic ozonation advanced treating cephalo pharmacy waste water |
| CN108927146A (en) * | 2017-05-23 | 2018-12-04 | 中国石油天然气股份有限公司 | A kind of inferior heavy oil hydrogenation catalyst and preparation method thereof |
| CN108970573B (en) * | 2018-07-24 | 2022-01-07 | 万华化学集团股份有限公司 | Chemical adsorbent and application and method thereof in purification and co-oxidation method for co-production of tert-butyl alcohol |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1050012A (en) * | 1989-08-18 | 1991-03-20 | 大阪瓦斯株式会社 | Handle the method for waste water |
| CN1524613A (en) * | 2003-02-27 | 2004-09-01 | 海云才 | High activity wet oxidation catalyst with carbon material as carrier and its preparation method |
| CN102658133A (en) * | 2012-05-09 | 2012-09-12 | 杭州凯大催化金属材料有限公司 | Method for preparing active carbon carrying precious metal catalyst |
| CN103041811A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Preparation method of catalytic wet oxidation catalyst and treatment method of organic wastewater |
-
2013
- 2013-06-07 CN CN2013102235990A patent/CN103263933A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1050012A (en) * | 1989-08-18 | 1991-03-20 | 大阪瓦斯株式会社 | Handle the method for waste water |
| CN1524613A (en) * | 2003-02-27 | 2004-09-01 | 海云才 | High activity wet oxidation catalyst with carbon material as carrier and its preparation method |
| CN103041811A (en) * | 2011-10-17 | 2013-04-17 | 中国石油化工股份有限公司 | Preparation method of catalytic wet oxidation catalyst and treatment method of organic wastewater |
| CN102658133A (en) * | 2012-05-09 | 2012-09-12 | 杭州凯大催化金属材料有限公司 | Method for preparing active carbon carrying precious metal catalyst |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437361A (en) * | 2014-10-24 | 2015-03-25 | 东华大学 | Method for preparing functional biological carbon by in-situ impregnation |
| CN106219727A (en) * | 2016-08-17 | 2016-12-14 | 河北莫兰斯环境科技股份有限公司 | A kind of technique of efficient catalytic ozonation advanced treating cephalo pharmacy waste water |
| CN108927146A (en) * | 2017-05-23 | 2018-12-04 | 中国石油天然气股份有限公司 | A kind of inferior heavy oil hydrogenation catalyst and preparation method thereof |
| CN108970573B (en) * | 2018-07-24 | 2022-01-07 | 万华化学集团股份有限公司 | Chemical adsorbent and application and method thereof in purification and co-oxidation method for co-production of tert-butyl alcohol |
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Application publication date: 20130828 |