CN103041815A - Preparation method of iron-supported attapulgite heterogeneous fenton catalyst - Google Patents
Preparation method of iron-supported attapulgite heterogeneous fenton catalyst Download PDFInfo
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Abstract
The invention discloses a preparation method of an iron-supported attapulgite heterogeneous fenton catalyst. The method comprises the process steps that A, attapulgite is taken and crushed; B, a right amount of attapulgite is immersed in an acid solution, and uniformly stirred to form a sample; C, the sample is centrifuged; an upper layer suspension is filter and dried; modified attapulgite is obtained; D, the attapulgite is ground and sieved; E, an FeCl3 solution with the concentration of 0.5-2mol/L is adopted; the attapulgite is immersed for 6-24h in a water bath; and F, the attapulgite is centrifuged or filtered, and dried and ground to the original particle size; and a finished product is prepared. The method has the advantages that iron ions are supported to the modified attapulgite through immersion and ion exchange, and the heterogeneous fenton catalyst is prepared, so that nondegradable waste water can be treated efficiently, and the problems that a pH value in homogeneous fenton is low, iron mud can be generated, and secondary pollution is caused are solved. An adsorptive property, an ion exchange property, and a strong oxidizing property of fenton reaction are exerted in waste water treatment.
Description
Technical field
That the present invention relates to is the preparation method of a kind of year heterogeneous Fenton catalyst of iron nonmetallic ore, relates in particular to the preparation method of a kind of year heterogeneous Fenton catalyst of iron attapulgite.
Background technology
The source of hardly degraded organic substance is very extensive in the water, is the difficult problem of water treatment field to its processing always.And high-level oxidation technology is owing to having the characteristics such as the strong and non-secondary pollution of oxidability, is considered to process the method that hardly degraded organic substance in the water has application prospect most.In the advanced oxidation treatment technology, the Fenton technology has the characteristics such as treatment effeciency is high, cost is relatively low, easy industrialization, becomes gradually one of main method in the present high-level oxidation technology.Over past ten years, external many scholars turn to application study with the Fenton technology from laboratory research gradually, for the treatment of actual used water difficult to degradate.But for common homogeneous phase Fenton system, because it only could carry out under lower pH effectively, need to repeatedly reconcile the pH value to waste water, increase on foot processing cost, and the catalyst of homogeneous phase Fenton system is miscible in waste water, reaction also can produce a large amount of iron containing sludges after finishing, and post processing is complicated.
For solving the bottleneck problem of Fenton system applies, the iron ion immobilization is become solid-phase catalyst, consist of heterogeneous Fenton system, not limited by pH value, be the main development direction of present Fenton system.
Attapulgite claims again palygorskite, is a kind of moisture zeopan clay mineral of chain layer structure, all has in a plurality of fields such as environmental protection, chemical industry, light industry, agricultural, building materials extremely widely to use.It is cheap, has larger specific area, stronger absorption property and certain ion-exchange capacity.But the impurity content of natural attapulgite is many, and sour modification can make the attapulgite inner elongate and fine and close orderly crystalline substance bundle is interrupted, disperses, and impurity such as calcium, magnesium, manganese are removed in a large number, and adsorption capacity, ion-exchange capacity obviously increase.
Summary of the invention
That the present invention proposes is the preparation method of a kind of year heterogeneous Fenton catalyst of iron attapulgite, its purpose is intended to firmly be carried on iron ion on the carrier, it is a kind of dipping technique, it also is a kind of ion exchange technique, with firmly being carried on the attapulgite after iron ion process dipping and the ion-exchange, be prepared into a kind of heterogeneous Fenton catalyst, can increase like this pH value scope, and catalyst can be repeatedly used, and avoids producing secondary pollution.Have certain economic worth and practicality.
Technical solution of the present invention: the preparation method of a kind of year heterogeneous Fenton catalyst of iron attapulgite comprises following processing step:
A, get attapulgite and pulverize, cross 5-20 orders after pulverizing;
B, to get the amount that the attapulgite that has filtered out in right amount is immersed in 5-20 times of attapulgite quality be in the hydrochloric acid solution of 2-10mol/L; Uniform stirring, mixing speed is 60-300r/min, gets sample;
C, with the centrifugal 10-60min of step B sample, the rotating speed of described centrifuge is 1500-1800 r/min, centrifugal after with upper strata suspension through filtering or without centrifugal direct filtration available quick filter paper, sample obtains attapulgite modified at 103-105 ° of C oven dry 2-3h after will filtering;
D, step C gained attapulgite was ground 40-200 mesh sieves;
E, employing concentration are the FeCl of 0.5-2mol/L
3Solution is pressed FeCl
3Solution: the ratio of attapulgite 5:1-20:1, step D gained attapulgite was soaked in water-bath 6-24 hour;
F, with the attapulgite that makes in the step e rotating speed with 1500-1800 r/min, centrifugal 10-60min, or use quick Filter paper filtering is dried 2-3h, and is ground to the described granule size of step D under 103-105 ° of C condition, the catalyst preparation is finished.
Beneficial effect of the present invention: the present invention on attapulgite, is prepared into catalyst with the iron firm attachment, forms heterogeneous Fenton system, can high efficiency must process used water difficult to degradate.This process can reach more than 95% removal of pollutants rates such as phenol in wastewater.Take full advantage of the strong oxidizing property of ion exchangeable, adsorptivity and the Fenton's reaction of attapulgite, do not produce secondary pollution, and catalyst can be repeatedly used, create considerable economic benefit and good social benefit.
The specific embodiment
Embodiment 1
A, get attapulgite and pulverize, cross 5 orders after pulverizing;
B, to get the amount that the attapulgite that has filtered out in right amount is immersed in 10 times of attapulgite quality be in the hydrochloric acid solution of 6mol/L; Uniform stirring, mixing speed is 80r/min, gets sample;
C, step B sample is centrifugal as 1500 r/min take rotating speed, 10min, behind described centrifuge centrifugal with upper strata suspension through filtering; Perhaps without centrifugal direct filtration, available quick filter paper will filter rear sample and dry 2h under 103 ° of C condition, obtain attapulgite modified;
D, step C gained attapulgite was ground 100 mesh sieves;
E, employing concentration are the FeCl of 1 mol/L
3Solution is pressed FeCl
3Solution: attapulgite is 5:1, and step D gained attapulgite was soaked in water-bath 6 hours;
F, with the attapulgite that makes in the step e rotating speed with 1500 r/min, centrifugal 10min, or use quick Filter paper filtering is dried 2h, and is ground to the described granule size of step D under 103 ° of C conditions, the catalyst preparation is finished;
G, the attapulgite for preparing is used for the experiment of phenol synthetic water, clearance can reach 99%.
Embodiment 2
A, get attapulgite and pulverize, cross 15 orders after pulverizing;
B, to get the amount that the attapulgite that has filtered out in right amount is immersed in 15 times of attapulgite quality be in the hydrochloric acid solution of 2mol/L; Uniform stirring, mixing speed is 60r/min, gets sample;
C, with the centrifugal 35min of step B sample, the rotating speed of described centrifuge is 1600r/min, centrifugal after with upper strata suspension through filtering; Perhaps without centrifugal direct filtration, available quick filter paper will filter rear sample and dry 2.5h under 105 ° of C condition, obtain attapulgite modified;
D, step C gained attapulgite was ground 200 mesh sieves;
E, employing concentration are the FeCl of 2 mol/L
3Solution is pressed FeCl
3Solution: the ratio of attapulgite 20:1, step D gained attapulgite was soaked in water-bath 24 hours;
F, with the attapulgite that makes in the step e with centrifugal rotational speed 1800r/min, 60min, or use quick Filter paper filtering is dried 3h, and is ground to the described granule size of step D under 105 ° of C conditions, the catalyst preparation is finished;
G, the attapulgite for preparing is used for the experiment of phenol synthetic water, clearance can reach 99%.
Embodiment 3
A, get attapulgite and pulverize, cross 20 orders after pulverizing;
B, to get the amount that the attapulgite that has filtered out in right amount is immersed in 20 times of attapulgite quality be in the hydrochloric acid solution of 10mol/L; Uniform stirring, mixing speed is 300r/min, gets sample;
C, with the centrifugal 60min of step B sample, the rotating speed of described centrifuge is 1800 r/min, centrifugal after with upper strata suspension through filtering; Perhaps without centrifugal direct filtration, available quick filter paper will filter rear sample and dry 2.5h under 105 ° of C condition, obtain attapulgite modified;
D, step C gained attapulgite was ground 40 mesh sieves;
E, employing concentration are the FeCl of 0.5 mol/L
3Solution is pressed FeCl
3Solution: the ratio of attapulgite 10:1, step D gained attapulgite was soaked in water-bath 12 hours;
F, with the attapulgite that makes in the step e with centrifugal rotational speed 1600 r/min, 60min, or use quick Filter paper filtering is dried 2.5h, and is ground to the described granule size of step D under 105 ° of C conditions, the catalyst preparation is finished;
G, the attapulgite for preparing is used for the experiment of phenol synthetic water, clearance can reach 99%.
Embodiment 4
A, get attapulgite and pulverize, cross 10 orders after pulverizing;
B, to get the amount that the attapulgite that has filtered out in right amount is immersed in 5 times of attapulgite quality be in the hydrochloric acid solution of 8mol/L; Uniform stirring, mixing speed is 100r/min, gets sample;
C, with the centrifugal 60min of step B sample, the rotating speed of described centrifuge is 1500r/min, centrifugal after with upper strata suspension through filtering; Perhaps without centrifugal direct filtration, available quick filter paper will filter rear sample and dry 3h under 104 ° of C condition, obtain attapulgite modified;
D, step C gained attapulgite was ground 150 mesh sieves;
E, employing concentration are the FeCl of 2 mol/L
3Solution is pressed FeCl
3Solution: the ratio of attapulgite 15:1, step D gained attapulgite was soaked in water-bath 10 hours;
F, with the attapulgite that makes in the step e with centrifugal rotational speed 1600 r/min, centrifugal 40min, or use quick Filter paper filtering is dried 2h, and is ground to the described granule size of step D under 105 ° of C conditions, the catalyst preparation is finished;
G, the attapulgite for preparing is used for the experiment of phenol synthetic water, clearance can reach 99%.
Embodiment 5
A, get attapulgite and pulverize, cross 18 orders after pulverizing;
B, to get the amount that the attapulgite that has filtered out in right amount is immersed in 5 times of attapulgite quality be in the hydrochloric acid solution of 10mol/L; Uniform stirring, mixing speed is 250r/min, gets sample;
C, with the centrifugal 30min of step B sample, the rotating speed of described centrifuge is 1560 r/min, centrifugal after with upper strata suspension through filtering; Perhaps without centrifugal direct filtration, available quick filter paper will filter rear sample and dry 2.5h under 104 ° of C condition, obtain attapulgite modified;
D, step C gained attapulgite was ground 150 mesh sieves;
E, employing concentration are the FeCl of 2mol/L
3Solution is pressed FeCl
3Solution: the ratio of attapulgite 20:1, step D gained attapulgite was soaked in water-bath 24 hours;
F, with the attapulgite that makes in the step e with centrifugal rotational speed 1800 r/min, centrifugal 60min, or use quick Filter paper filtering is dried 3h, and is ground to the described granule size of step D under 105 ° of C conditions, the catalyst preparation is finished;
G, the attapulgite for preparing is used for the experiment of phenol synthetic water, clearance can reach 99%.
The present invention with iron ion be carried on attapulgite modified on, be prepared into heterogeneous Fenton catalyst, can high efficiency process used water difficult to degradate, solved low pH value in the homogeneous phase Fenton, can produce iron mud, bring the bottleneck problems such as secondary pollution.And the iron ion load capacity is large, adheres to stablely, is not easy to separate out, and catalyst can be repeatedly used.In addition, attapulgite is cheap, have larger specific area, stronger absorption property and certain ion-exchange capacity, with ferropexy on attapulgite, as catalyst, form heterogeneous Fenton system after adding hydrogen peroxide, can finely must bring into play the strong oxidizing property of absorption property and the Fenton's reaction of attapulgite.The heterogeneous Fenton catalyst preparation process that carries the iron attapulgite comprises attapulgite modified, load iron ion two large divisions.After the modification of former concave convex rod mud acid, along with H
+Gradually infiltration to its internal structure octahedral cations ecto-entad, cation progressively even fully is substituted in the octahedron, inner elongate and fine and close orderly crystalline substance bundle is interrupted, disperses, impurity is removed in a large number, and adsorption capacity, ion-exchange capacity obviously increase.The modification purpose is to increase exchange and absorption iron ion amount; The load iron ion adopts dipping and ion-exchange, and part iron ion generation secondary replaces, and enters the attapulgite crystals, and the oxyhydroxide that the part iron ion forms iron is attached to attapulgite's surface.The oxyhydroxide of iron can react with hydrogen peroxide, produces the hydroxyl with strong oxidizing property, hardly degraded organic substance can be carried out oxidation Decomposition.
Above content is in conjunction with concrete preferred embodiment further description made for the present invention, can not assert that implementation of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (3)
1. preparation method of carrying the heterogeneous Fenton catalyst of iron attapulgite is characterized in that the method comprises following processing step:
A, get attapulgite and pulverize, cross 5-20 orders after pulverizing;
B, to get the amount that the attapulgite that has filtered out in right amount is immersed in 5-20 times of attapulgite quality be in the hydrochloric acid solution of 2-10mol/L; Uniform stirring, mixing speed is 60-300r/min, gets sample;
C, with the centrifugal 10-60min of step B sample, the rotating speed of described centrifuge is 1500-1800 r/min, centrifugal after with upper strata suspension through filtering; Perhaps without centrifugal direct filtration, available quick filter paper will filter rear sample and dry 2-3h under 103-105 ° of C condition, obtain attapulgite modified;
D, step C gained attapulgite was ground 40-200 mesh sieves;
E, employing concentration are the FeCl of 0.5-2mol/L
3Solution is pressed FeCl
3Solution: the ratio of attapulgite 5:1-20:1, step D gained attapulgite was soaked in water-bath 6-24 hour;
F, with the attapulgite that makes in the step e rotating speed with 1500-1800 r/min, centrifugal 10-60min, or use quick Filter paper filtering is dried 2-3h, and is ground to the described granule size of step D under 103-105 ° of C condition, the catalyst preparation is finished.
2. the preparation method of a kind of year according to claim 1 heterogeneous Fenton catalyst of iron attapulgite is characterized in that, described step B, and hydrochloric acid solution: the liquid-solid ratio of attapulgite is 5:1-20:1, selected acid solutions is 2-10mol/L.
3. the preparation method of a kind of year according to claim 1 heterogeneous Fenton catalyst of iron attapulgite is characterized in that, the bath temperature in the described step e remains on 50-100 ° of C.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103230796A (en) * | 2013-04-25 | 2013-08-07 | 六安科瑞达新型材料有限公司 | Preparation method of attapulgite supported ferroferric oxide |
| CN103240122A (en) * | 2013-05-17 | 2013-08-14 | 浙江理工大学 | Preparation method of active carbon fiber loaded aminopyridine metal complex |
| CN103551204A (en) * | 2013-10-21 | 2014-02-05 | 中山大学 | Multi-stage hierarchical pore structural Fenton-like catalyst and application thereof |
| CN105268487A (en) * | 2014-07-24 | 2016-01-27 | 艾特克控股集团有限公司 | Preparation method and applications of supported iron oxide catalyst carrier |
| CN106040244A (en) * | 2016-06-01 | 2016-10-26 | 中国科学院过程工程研究所 | Supported solid catalyst for Fenton reaction and preparing method thereof |
| CN106824212A (en) * | 2017-03-10 | 2017-06-13 | 扬州大学 | A kind of CeO2/Fe2O3The preparation method of the nano environment material on load attapulgite |
| CN107335406A (en) * | 2017-06-26 | 2017-11-10 | 东北林业大学 | A kind of water treatment absorbent and preparation method thereof |
| CN108212158A (en) * | 2018-01-17 | 2018-06-29 | 上海交通大学 | A kind of fenton catalyst and its preparation method and application |
| CN108622974A (en) * | 2018-05-04 | 2018-10-09 | 天津工业大学 | A method of using brown mushroom give up bacteria residue handle textile printing and dyeing waste water from dyestuff |
| CN110092505A (en) * | 2019-05-26 | 2019-08-06 | 北京化工大学 | A kind of method of Concave-convex clay rod processing wastewater containing phenol |
| CN110252305A (en) * | 2019-03-05 | 2019-09-20 | 中国科学院生态环境研究中心 | Keep the preparation and application of the iron-carbon micro-electrolytic material of the long-acting catalytic activity of Fenton system |
| CN110385129A (en) * | 2019-07-04 | 2019-10-29 | 陕西省土地工程建设集团有限责任公司 | It is a kind of using mud stone as class fenton catalyst, preparation and the application of carrier |
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| CN103230796A (en) * | 2013-04-25 | 2013-08-07 | 六安科瑞达新型材料有限公司 | Preparation method of attapulgite supported ferroferric oxide |
| CN103240122A (en) * | 2013-05-17 | 2013-08-14 | 浙江理工大学 | Preparation method of active carbon fiber loaded aminopyridine metal complex |
| CN103551204A (en) * | 2013-10-21 | 2014-02-05 | 中山大学 | Multi-stage hierarchical pore structural Fenton-like catalyst and application thereof |
| CN103551204B (en) * | 2013-10-21 | 2015-04-22 | 中山大学 | Multi-stage hierarchical pore structural Fenton-like catalyst and application thereof |
| CN105268487B (en) * | 2014-07-24 | 2018-03-02 | 艾特克控股集团有限公司 | A kind of preparation method and applications of loading type ferric oxide catalyst carrier |
| CN105268487A (en) * | 2014-07-24 | 2016-01-27 | 艾特克控股集团有限公司 | Preparation method and applications of supported iron oxide catalyst carrier |
| CN106040244A (en) * | 2016-06-01 | 2016-10-26 | 中国科学院过程工程研究所 | Supported solid catalyst for Fenton reaction and preparing method thereof |
| CN106040244B (en) * | 2016-06-01 | 2018-07-06 | 中国科学院过程工程研究所 | It is a kind of for supported solid catalyst of Fenton's reaction and preparation method thereof |
| CN106824212A (en) * | 2017-03-10 | 2017-06-13 | 扬州大学 | A kind of CeO2/Fe2O3The preparation method of the nano environment material on load attapulgite |
| CN107335406A (en) * | 2017-06-26 | 2017-11-10 | 东北林业大学 | A kind of water treatment absorbent and preparation method thereof |
| CN108212158A (en) * | 2018-01-17 | 2018-06-29 | 上海交通大学 | A kind of fenton catalyst and its preparation method and application |
| CN108212158B (en) * | 2018-01-17 | 2020-08-14 | 上海交通大学 | Fenton catalyst and preparation method and application thereof |
| CN108622974A (en) * | 2018-05-04 | 2018-10-09 | 天津工业大学 | A method of using brown mushroom give up bacteria residue handle textile printing and dyeing waste water from dyestuff |
| CN110252305A (en) * | 2019-03-05 | 2019-09-20 | 中国科学院生态环境研究中心 | Keep the preparation and application of the iron-carbon micro-electrolytic material of the long-acting catalytic activity of Fenton system |
| CN110252305B (en) * | 2019-03-05 | 2020-09-15 | 中国科学院生态环境研究中心 | Preparation and application of iron-carbon micro-electrolysis material capable of maintaining long-acting catalytic activity of Fenton system |
| CN110092505A (en) * | 2019-05-26 | 2019-08-06 | 北京化工大学 | A kind of method of Concave-convex clay rod processing wastewater containing phenol |
| CN110385129A (en) * | 2019-07-04 | 2019-10-29 | 陕西省土地工程建设集团有限责任公司 | It is a kind of using mud stone as class fenton catalyst, preparation and the application of carrier |
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Application publication date: 20130417 Assignee: SHANGHAI RESUN ENVIRONMENTAL TECHNOLOGY CO.,LTD. Assignor: Nanjing Forestry University Contract record no.: 2018320000391 Denomination of invention: Preparation method of iron-supported attapulgite heterogeneous fenton catalyst Granted publication date: 20140625 License type: Common License Record date: 20181214 Application publication date: 20130417 Assignee: MA'ANSHAN SANTA ENVIRONMENTAL PROTECTION TECHNOLOGY CO.,LTD. Assignor: Nanjing Forestry University Contract record no.: 2018320000390 Denomination of invention: Preparation method of iron-supported attapulgite heterogeneous fenton catalyst Granted publication date: 20140625 License type: Common License Record date: 20181214 |
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