CN103252340B - Resource utilization method of Fenton iron sludge - Google Patents
Resource utilization method of Fenton iron sludge Download PDFInfo
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- CN103252340B CN103252340B CN201310184249.8A CN201310184249A CN103252340B CN 103252340 B CN103252340 B CN 103252340B CN 201310184249 A CN201310184249 A CN 201310184249A CN 103252340 B CN103252340 B CN 103252340B
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- fenton
- iron
- iron mud
- mud
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Abstract
The invention discloses a resource utilization method of Fenton iron sludge. The method comprises the following steps of: (1) treating Fenton; adding the rest of ferrum into concentrated sulfuric acid; and controlling the temperature to be between 70 and 75 DEG C to stir for 30 minutes; (2) adding excessive quantities of scrap iron chips into an iron sludge solution obtained in the step (1) to reduce; detecting Fe3<+> by using a phenol solution until Fe<3+> is totally reduced into Fe<2+>; and (3) after the reduction is finished, standing for precipitating for 30 minutes; extracting supernate; adding ethanol according to the proportion that V(supernate)/V(ethanol) is equal to 10 to 1 and shortening the crystallizing time of ferrous sulfate; and after the crystallization is finished, obtaining an industrial FeSO4.7H2O finished product. According to the method, the bottle neck problem of Fenton technology promotion can be solved, the resource utilization of solid wastes is realized, and Fenton iron sludge is turned from waste into treasure, so that sustainable development of human society is facilitated.
Description
Technical field
The present invention relates to the resource treatment technique field of solid waste, particularly relate to the resource utilization method that a kind of Fenton treatment technology produces iron mud.
Technical background
Within 1894, French scientist H.J.Fenton has found Fe
2+by H
2o
2the oxidation of catalysis malic acid effectively, later research shows that the combination of the two is all a kind of effective oxidant to the organic matter of numerous species.Descendant is this great scientist in honor of, by Fe
2+and H
2o
2the reagent called after Fenton reagent of composition, uses the reaction of this reagent to claim Fenton to react.1964, Fenton reagent is successfully applied in wastewater treatment by Canada scholar H.R.Eisenhaner, in the research of nearly more than ten years Fenton reagent Successful utilization in the process of various industrial sewage, become most widely used general, technique that technology is the most ripe in Sewage advanced treatment technology at present.
Why Fenton reagent has very strong oxidability, is because of H in Fenton reagent
2o
2by Fe
2+catalytic decomposition generates hydroxyl radical free radical (OH), and hydroxyl radical free radical (OH) has following critical nature:
(1) oxidability is strong
Its oxidizing electrode current potential (E) is 2.80V, in known oxidant, be only second to F
2, this means that hydroxyl radical free radical (OH) oxidability is considerably beyond common chemical oxidizing agent.Therefore, it is possible to be oxidized most organic matter.
(2) hydroxyl radical free radical (OH) has very high electrophilicity or electronegativity
There is higher electronegativity or electron affinity energy (569.3kJ), easy attack height cloud density point, hydroxyl radical free radical (OH) this electrophilicity, determines Fenton reagent and has unique advantage in process containing organic matters such as chloro, sulfonic group, nitros.
(3) hydroxyl radical free radical (OH) has addition
When there being carbon-carbon double bond to exist, unless be there is highly active C-H bond by the molecule of attack, otherwise, will addition reaction be there is.
The organic essence of Fenton reagent process is exactly that hydroxyl radical free radical and organic matter react, until organic matter is thoroughly mineralized into CO
2and H
2o
2.
During Fenton method process organic wastewater with difficult degradation thereby, there is the advantage that additive method is incomparable, so far Successful utilization in the process of various industrial wastewater.But Fenton oxidation method can produce a certain amount of chemical sludge in processing procedure, conduct oneself well if improper to comprehend to produce and much endanger, such as: take a large amount of soil; Mud is stacked can produce high temperature or other chemical reaction through wind and weather, the structure of meeting spoiled soil; Directly discharge alluvial riverbed, severe contamination water body; Mud discharges pernicious gas, dust etc. after being decomposed by microbiological oxidation, can increase the weight of the pollution of air; After a large amount of stacking, containing enteric bacteria, parasite and virus etc. in mud, serious harm is to the health of the mankind.Therefore the process of Fenton iron mud has become the key of restriction Fenton Technique Popularizing.
The performance of inventor to Fenton iron mud is studied analysis, and in Fenton iron mud, the content of iron is more than 50%, and wherein main exist with the form of ferric ion, so have very large using value to the recycling of ferro element.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that Fenton iron mud resource utilizes, and produces ferrous sulfate and iron mud is turned waste into wealth, thus make Fenton iron mud obtain abundant recycling by utilizing Fenton iron mud.
The present invention solves the problems of the technologies described above with following technical scheme:
The method that a kind of Fenton iron mud resource of the present invention utilizes, comprises the following steps:
(1) after getting Fenton process, the chemical iron mud of residue adds the concentrated sulfuric acid, and volume ratio=10 ︰ 1 of the chemical Tie Ni ︰ concentrated sulfuric acid, is heated to temperature and stirs 30min at 70 ~ 75 DEG C, obtain iron mud solution;
(2) add excessive waste iron filing in the iron mud solution obtained to step (1) to reduce, detect Fe by phenol solution
3+, until Fe
3+be reduced into Fe completely
2+, quiescent setting 30min after completing, extracts supernatant, lower sediment dehydration landfill disposal;
(3) by supernatant: the volume ratio=10:1 of ethanol adds ethanol, shorten the crystallization time of ferrous sulfate, to be crystallized completely after to get product industrial FeSO
47H
2o.
The moisture control of the residue chemistry iron mud of described step (1), 93 ~ 96%, can adopt dilution or concentrated method to make its moisture content reach this value.
Described step (2) is 60 ~ 70min with the time that waste iron filing carries out reducing.
The present invention produces ferrous sulfate by utilizing Fenton iron mud, iron mud is turned waste into wealth, thus makes Fenton iron mud obtain abundant recycling.
Accompanying drawing explanation
Fig. 1 is the process chart of the inventive method.
Detailed description of the invention
Embodiment 1:
Raw material: Fenton technology advanced treating paper pulp papermaking waste water residue iron mud, Fe
2o
3content 53.2%, the content of organic matter 28.5%.
Treatment step:
(1) above-mentioned Fenton iron mud is got through the concentrated chemical iron mud 1m obtaining moisture content 95.5%
3, add the industrial concentrated sulfuric acid of mass concentration 98% by volume ratio=10 ︰ 1 of chemical Tie Ni ︰ sulfuric acid, and be heated to 70 DEG C, fully stir 30min, form iron mud solution;
(2) to the 1.1m that step (1) obtains
3add 24kg waste iron filing in iron mud solution to reduce, after recovery time 70min, detect Fe by phenol solution
3+, Fe
3+be reduced into Fe completely
2+, quiescent setting 30min after completing, extracts supernatant, lower sediment dehydration landfill disposal;
(3) in supernatant, add the industrial alcohol of purity 99% effectively to shorten the crystallization time of ferrous sulfate by V (supernatant)/V (ethanol)=10:1, after crystallization completely, obtain FeSO
47H
2o.FeSO after testing
47H
2o content reaches 98.34%, and other indexs also all reach GB10531-89 water treatment agent ferrous sulfate high-class product standard.Ferrous sulfate can be back to Fenton system or be used as other purposes.
Embodiment 2:
Raw material: Fenton technology advanced treating alcohol waste water residue iron mud, Fe
2o
3content 55.8%, the content of organic matter 25.4%.
Treatment step:
(1) get above-mentioned Fenton iron soiled ends and concentrate the chemical iron mud 1m obtaining moisture content 94.8%
3, add the industrial concentrated sulfuric acid of mass concentration 98% by volume ratio=10 ︰ 1 of chemical Tie Ni ︰ sulfuric acid, temperature controls, at 75 DEG C, fully to stir 30min, forms iron mud solution;
(2) to the 1.1m that step (1) obtains
3add 22kg waste iron filing in iron mud solution to reduce, after reduction 60min, detect Fe by phenol solution
3+, Fe
3+be reduced into Fe completely
2+, quiescent setting 30min after completing, extracts supernatant, lower sediment dehydration landfill disposal;
(3) in supernatant, add the industrial alcohol of purity 99% effectively to shorten the crystallization time of ferrous sulfate by V (supernatant)/V (ethanol)=10:1, after crystallization completely, obtain FeSO
47H
2o.FeSO after testing
47H
2o content reaches 98.52%, and other indexs also all reach GB10531-89 water treatment agent ferrous sulfate high-class product standard.
Embodiment 3:
Raw material: Fenton technology deep treatment of pharmaceutical waste water residue iron mud, Fe
2o
3content 55.1%, the content of organic matter 26.9%.
Treatment step:
(1) the chemical iron mud 1m that above-mentioned Fenton iron mud obtains moisture content 93.5% after concentration is got
3, add the industrial concentrated sulfuric acid of mass concentration 98% by volume ratio=10 ︰ 1 of chemical Tie Ni ︰ sulfuric acid, temperature controls, at 73 DEG C, fully to stir 30min, forms iron mud solution;
(2) to the 1.1m that step (1) obtains
3add 23kg waste iron filing in iron mud solution to reduce, after reduction 65min, detect Fe by phenol solution
3+, Fe
3+be reduced into Fe completely
2+, quiescent setting 30min after completing, extracts supernatant, lower sediment dehydration landfill disposal;
(3) in supernatant, add the industrial alcohol of purity 99% effectively to shorten the crystallization time of ferrous sulfate by V (supernatant)/V (ethanol)=10:1, after crystallization completely, obtain FeSO
47H
2o.FeSO after testing
47H
2o content reaches 98.47%, and other indexs also all reach GB10531-89 water treatment agent ferrous sulfate high-class product standard.
Claims (2)
1. the method that utilizes of Fenton iron mud resource, with iron mud and waste iron filing for raw material, prepares FeSO through acidleach, reduction and Crystallization Procedure
47H
2o, is characterized in that, concrete operation step is as follows:
(1) after getting Fenton process, the chemical iron mud of residue adds the concentrated sulfuric acid, and the moisture control of chemical iron mud is 93 ~ 96%, and volume ratio=10 ︰ 1 of the chemical Tie Ni ︰ concentrated sulfuric acid, is heated to temperature and stirs 30min at 70 ~ 75 DEG C, obtain iron mud solution;
(2) add excessive waste iron filing in the iron mud solution obtained to step (1) to reduce, detect Fe by phenol solution
3+, until Fe
3+be reduced into Fe completely
2+, quiescent setting 30min after completing, extracts supernatant, lower sediment dehydration landfill disposal;
(3) in supernatant, add ethanol by volume ratio=10 ︰ 1 of Shang Qing Ye ︰ ethanol, shorten the crystallization time of ferrous sulfate, to be crystallized completely after to get product industrial FeSO
47H
2o.
2. the method for Fenton iron mud resource utilization according to claim 1, it is characterized in that, described step (2) is 60 ~ 70min with the time that waste iron filing carries out reducing.
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|---|---|---|---|
| CN201310184249.8A CN103252340B (en) | 2013-05-17 | 2013-05-17 | Resource utilization method of Fenton iron sludge |
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|---|---|---|---|
| CN201310184249.8A CN103252340B (en) | 2013-05-17 | 2013-05-17 | Resource utilization method of Fenton iron sludge |
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| CN103252340B true CN103252340B (en) | 2015-04-22 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261622A (en) * | 2014-09-29 | 2015-01-07 | 中国电建集团中南勘测设计研究院有限公司 | Fenton sewage treatment process and equipment thereof |
| CN106986513A (en) * | 2016-01-21 | 2017-07-28 | 上海电气集团股份有限公司 | A kind of method for reclaiming of Fenton iron mud produced by centralized sewage treatment plant |
| CN105664852B (en) * | 2016-01-29 | 2018-05-11 | 南京神克隆科技有限公司 | The recycling processing method of chemical sludge |
| CN106892497A (en) * | 2017-04-14 | 2017-06-27 | 上海电气集团股份有限公司 | Fenton iron mud regeneration device, Fenton methods sewage disposal system and its method |
| CN107902701A (en) * | 2017-11-15 | 2018-04-13 | 成都先进金属材料产业技术研究院有限公司 | The method of purification of byproduct ferrous sulfate of titanium dioxide |
| CN109665568A (en) * | 2019-01-09 | 2019-04-23 | 无锡日月水处理有限公司 | A kind of extraction method of purification of ferrous iron |
| CN110586097A (en) * | 2019-09-03 | 2019-12-20 | 广西大学 | Magnetic ferroferric oxide/graphene oxide nano composite Fenton-like catalytic material and preparation and application thereof |
| CN111072127A (en) * | 2019-12-11 | 2020-04-28 | 东莞道汇环保科技股份有限公司 | Method for recycling ferric salt in Fenton sludge |
| CN114890638A (en) * | 2022-06-02 | 2022-08-12 | 洛阳昊海环保科技有限公司 | Resource utilization method of oil-and organic-containing Fenton iron mud |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5520666A (en) * | 1978-07-31 | 1980-02-14 | Gunze Ltd | Sludge recovery method |
| CN101491771A (en) * | 2009-03-02 | 2009-07-29 | 华东理工大学 | Fenton and Fenton-like reaction catalyst regeneration and reclamation method |
| CN102786099A (en) * | 2012-08-27 | 2012-11-21 | 上海华谊（集团）公司 | Device and method for producing ferrous sulfate solution |
| CN102849803A (en) * | 2011-06-28 | 2013-01-02 | 鞍钢股份有限公司 | A method for recycling Fenton reaction catalyst |
-
2013
- 2013-05-17 CN CN201310184249.8A patent/CN103252340B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5520666A (en) * | 1978-07-31 | 1980-02-14 | Gunze Ltd | Sludge recovery method |
| CN101491771A (en) * | 2009-03-02 | 2009-07-29 | 华东理工大学 | Fenton and Fenton-like reaction catalyst regeneration and reclamation method |
| CN102849803A (en) * | 2011-06-28 | 2013-01-02 | 鞍钢股份有限公司 | A method for recycling Fenton reaction catalyst |
| CN102786099A (en) * | 2012-08-27 | 2012-11-21 | 上海华谊（集团）公司 | Device and method for producing ferrous sulfate solution |
Non-Patent Citations (1)
| Title |
|---|
| 由工业废料铁泥制备FeSO_4•7H_2O的研究;张丽清等;《化学工业与工程》;20110115;第28卷(第01期);35-38,52 * |
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