CN103964659A - Method for solidifying lead-containing sludge by utilizing iron-containing sludge generated by Fenton reagent method - Google Patents
Method for solidifying lead-containing sludge by utilizing iron-containing sludge generated by Fenton reagent method Download PDFInfo
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- CN103964659A CN103964659A CN201410192244.4A CN201410192244A CN103964659A CN 103964659 A CN103964659 A CN 103964659A CN 201410192244 A CN201410192244 A CN 201410192244A CN 103964659 A CN103964659 A CN 103964659A
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- Prior art keywords
- sludge
- containing sludge
- iron containing
- fenton reagent
- utilizing
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 239000010802 sludge Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 48
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 37
- 239000012028 Fenton's reagent Substances 0.000 title claims abstract description 18
- 238000009713 electroplating Methods 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims description 15
- 238000001238 wet grinding Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000002386 leaching Methods 0.000 abstract description 6
- 239000003513 alkali Substances 0.000 abstract description 4
- 230000003628 erosive effect Effects 0.000 abstract description 2
- 229910021514 lead(II) hydroxide Inorganic materials 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract 1
- FLTRNWIFKITPIO-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe] FLTRNWIFKITPIO-UHFFFAOYSA-N 0.000 abstract 1
- 239000002910 solid waste Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 239000004568 cement Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 208000014644 Brain disease Diseases 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 208000032274 Encephalopathy Diseases 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000010801 sewage sludge Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Treatment Of Sludge (AREA)
Abstract
The invention discloses a method for solidifying lead-containing sludge by utilizing iron-containing sludge generated by a Fenton reagent method, and ensures that the iron-containing sludge is subjected to resource utilization while lead-containing electroplating sludge is immobilized, so that the leaching of lead is greatly reduced. The method comprises the following specific process steps: (1) grinding after the iron-containing sludge and the lead-containing sludge are dried and uniformly mixing; (2) calcining at a high temperature after the two kinds of uniformly-mixed sludge are pressed. The method has the benefits that as Fe(OH)3 in the iron-containing sludge can react with Pb(OH)2 at a high temperature to generate stable PbFe12O19, the erosion of an acid-alkali solution can be resisted, the leaching of the lead is effectively prevented, and the purpose of safely solidifying the lead-containing sludge is achieved; the method has the advantages of good economy, large alkali capacity and the like.
Description
Technical field
The present invention relates to solid waste resource recovery and utilize field, be specifically related to a kind of iron containing sludge of the Fenton of employing reagent method generation as the method for the curing leaded electroplating sludge of solidifying agent.
Background technology
Electroplating sludge is the solid waste that the electroplating wastewater that produces in plating production process and waste and old electroplate liquid produce in treating processes, has that moisture content is high, heavy metal content is high, easily by spies such as leachings.Lead and compound thereof are poisonous to human body, easily in human body inner accumulated, are mainly stored in bone after picked-up, and part replaces the calcium in calcium phosphate, are difficult for discharging, and poisoningly can cause system damage when darker, when serious, can cause lead encephalopathy.Because plumbous mobility is larger, in by the process of banking up, easily the environment of periphery is produced to serious threat, therefore how the leaded mud of safe disposal is the focus of field of environment engineering always.
It is the Main Means of heavy metal sewage sludge that curing/stabilizing is processed always, mainly comprises that cement, glass etc. are coated curing.Thermal treatment causes people's concern gradually owing to having the advantage such as significantly minimizing, recovery energy wherein; And the cost of heat treatment for solidification is low compared with cement, vitrification cost, the means using thermal treatment as main processing solid waste in future in Europe.Fenton reagent method is widely used in the processing of high concentrated organic wastewater, but its main drawback is easily to produce the mud that contains a large amount of ironic hydroxides, in mud, the content of ironic hydroxide is even up to 50%, conventionally iron containing sludge dehydration is returned to stove ironmaking, if but efficiently utilize iron containing sludge will the popularization of Fenton reagent method be produced to important meaning.A Chinese patent (CN 200910198271.1) discloses a kind of method of pickling iron containing sludge recycling, concrete steps are after iron containing sludge is dried, directly to utilize high pressure compacting balling-up, send in 1100 DEG C of High Temperature Furnaces Heating Apparatuss and be no less than 1h, the flammable CO Gas recovery producing in heat-processed, liberated heat is entering the heating of stokehold for pressure ball, remaining the dry of mud that can be used for, this method has solved the problem of the high energy gamma source consumption of pyroprocessing.Another Chinese patent (publication number CN 201010023054.1) has proposed a kind ofly to adopt iron containing sludge to add to meet the method that sizing agent is prepared cooled agglomerated pellet, produce the good cohesiveness to iron containing sludge by adding organic sizing agent (vinyl acetate, vinylformic acid, Xylo-Mucine, polyvinyl alcohol etc.) and inorganic additives (wilkinite, calcium oxide, alkaline flower bulb alkali etc.), but shortcoming is to add complicated components, and each component must strictly be controlled proportioning in certain sequence.More than open invention has related to the recycling of iron containing sludge, but has the problem such as operation steps complexity, technical process length.Have not been reported as for the research that utilizes iron containing sludge to solidify electroplating sludge.
Summary of the invention
Problem to be solved by this invention is to be difficult to processing problem for the leaded mud producing in the iron containing sludge recycling of Fenton reagent method generation and plating production process, both are solidified to leaded mud in conjunction with the iron containing sludge that forms a kind of Fenton of utilization reagent method generation method by means of calcination.
A kind of method of utilizing the iron containing sludge of Fenton reagent method generation to solidify leaded electroplating sludge of the present invention, comprises the following steps:
1) by Fenton reagent method produce iron containing sludge and electroplating sludge dry respectively, by dry iron containing sludge and electroplating sludge respectively as in ball mill pulverize, levigate;
2) by two kinds of levigate mud Fe/Pb=12-15 mixing in molar ratio, mixed mud is placed in to ball mill again and adopts wet-milling mode levigate;
3) by step 2) ball milling mix finish mixing sludge slurries dry, then the mixing sludge of oven dry is pressed into block mud through tabletting machine,
4) block mud is placed in to 800-1000 DEG C of calcining 2.5-4h of the inherent temperature of retort furnace, cooling after, realized iron containing sludge and solidified leaded electroplating sludge.
The bake out temperature of step 1) is 105 DEG C, and drying time is 24-48h.
The drum's speed of rotation 50-100r/min of step 1), Ball-milling Time 0.5-2h.
Step 2) in, the solid-to-liquid ratio that wet-milling mode adopts is 5-2, Ball-milling Time 12-18h.
The bake out temperature of step 3) is 105-200 DEG C.
When step 3) compressing tablet, pressure range is 500-1000kg/cm
2.
The principle of solidification of the present invention is by pyroprocessing, and first the lead hydroxide in the ironic hydroxide in iron containing sludge and leaded mud dewaters and form ferric oxide and plumbous oxide, generates PbFe through further reacting
12o
19, due to PbFe
12o
19there is good chemical stability and physical strength, after solidifying, can resist the erosion of acid, alkali and other undesirable elements in environment, prevent solvable plumbous the inflow in environment in mud.
Embodiment
Below in conjunction with example, the invention will be further described, and following examples are intended to illustrate the present invention instead of limitation of the invention further.
Embodiment 1
The iron containing sludge that Fenton reagent method is produced and leaded electroplating sludge (leaded 20%) are placed in respectively 105 DEG C and dry 24h, subsequently by dry iron containing sludge and electroplating sludge respectively as in ball mill pulverize, levigate, drum's speed of rotation 50r/min, Ball-milling Time 0.5h.By two kinds of levigate mud Fe/Pb=12 mixing in molar ratio, be again placed in ball mill and be mixed and finely ground, the process that is mixed and finely ground adopts wet-milling mode, solid-to-liquid ratio 5, Ball-milling Time 12h.Ball milling is mixed to the mixing sludge slurries that finish 105 DEG C of oven dry, then the mixing sludge of oven dry is suppressed to tabletting machine pressure range 500kg/cm through tabletting machine
2.Be placed in 800 DEG C of calcining 2.5h of the inherent temperature of retort furnace through the block mud of tabletting machine compacting.After levigate after burnt block mud is pulverized, adopt " leaching toxicity from solid waste method-hac buffer method " of amendment to leach continuously 22d, leach the lead concentration 25mg/L finishing in rear solution.
Embodiment 2
The iron containing sludge that Fenton reagent method is produced and leaded electroplating sludge (leaded 45%) are placed in respectively 105 DEG C and dry 48h, subsequently by dry iron containing sludge and electroplating sludge respectively as in ball mill pulverize, levigate, drum's speed of rotation 100r/min, Ball-milling Time 2h.By two kinds of levigate mud Fe/Pb=15 mixing in molar ratio, be again placed in ball mill and be mixed and finely ground, the process that is mixed and finely ground adopts wet-milling mode, solid-to-liquid ratio 3, Ball-milling Time 18h.Ball milling is mixed to the mixing sludge slurries that finish 200 DEG C of oven dry, then the mixing sludge of oven dry is suppressed to tabletting machine pressure range 1000kg/cm through tabletting machine
2.Be placed in 1000 DEG C of calcining 4h of the inherent temperature of retort furnace through the block mud of tabletting machine compacting.After levigate after burnt block mud is pulverized, adopt " leaching toxicity from solid waste method-hac buffer method " of amendment to leach continuously 22d, leach the lead concentration 12mg/L finishing in rear solution.
Embodiment 3
The iron containing sludge that Fenton reagent method is produced and leaded electroplating sludge (lead concentration 16%) are placed in respectively 105 DEG C and dry 36h, subsequently by dry iron containing sludge and electroplating sludge respectively as in ball mill pulverize, levigate, drum's speed of rotation 75r/min, Ball-milling Time 1h.By two kinds of levigate mud Fe/Pb=14 mixing in molar ratio, be again placed in ball mill and be mixed and finely ground, the process that is mixed and finely ground adopts wet-milling mode, solid-to-liquid ratio 4, Ball-milling Time 15h.Ball milling is mixed to the mixing sludge slurries that finish 200 DEG C of oven dry, then the mixing sludge of oven dry is suppressed to tabletting machine pressure range 750kg/cm through tabletting machine
2.Be placed in 900 DEG C of calcining 3h of the inherent temperature of retort furnace through the block mud of tabletting machine compacting.After levigate after burnt block mud is pulverized, adopt " leaching toxicity from solid waste method-hac buffer method " of amendment to leach continuously 22d, leach the lead concentration 20mg/L finishing in rear solution.
The concrete application approach of the present invention is a lot, and the above is only the preferred embodiment of the present invention, should be understood that; for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvement, these improve and also should be considered as protection scope of the present invention.
Claims (6)
1. a method of utilizing the iron containing sludge of Fenton reagent method generation to solidify leaded electroplating sludge, is characterized in that comprising the following steps:
1) by Fenton reagent method produce iron containing sludge and electroplating sludge dry respectively, by dry iron containing sludge and electroplating sludge respectively as in ball mill pulverize, levigate;
2) by two kinds of levigate mud Fe/Pb=12-15 mixing in molar ratio, mixed mud is placed in to ball mill again and adopts wet-milling mode levigate;
3) by step 2) ball milling mix finish mixing sludge slurries dry, then the mixing sludge of oven dry is pressed into block mud through tabletting machine,
4) block mud is placed in to 800-1000 DEG C of calcining 2.5-4h of the inherent temperature of retort furnace, cooling after, realized iron containing sludge and solidified leaded electroplating sludge.
2. the method for utilizing the iron containing sludge of Fenton reagent method generation to solidify leaded electroplating sludge according to claim 1, is characterized in that: the bake out temperature of step 1) is 105 DEG C, and drying time is 24-48.
3. the method for utilizing the iron containing sludge of Fenton reagent method generation to solidify leaded electroplating sludge according to claim 1 and 2, is characterized in that: the drum's speed of rotation 50-100r/min of step 1), Ball-milling Time 0.5-2h.
4. the method for utilizing the iron containing sludge of Fenton reagent method generation to solidify leaded electroplating sludge according to claim 1 and 2, is characterized in that: step 2) in, the solid-to-liquid ratio that wet-milling mode adopts is 5-2, Ball-milling Time 12-18h.
5. the method for utilizing the iron containing sludge of Fenton reagent method generation to solidify leaded electroplating sludge according to claim 1 and 2, is characterized in that: the bake out temperature of step 3) is 105-200 DEG C.
6. the method for utilizing the iron containing sludge of Fenton reagent method generation to solidify leaded electroplating sludge according to claim 1 and 2, is characterized in that: when step 3) compressing tablet, pressure range is 500-1000kg/cm
2.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410192244.4A CN103964659B (en) | 2014-05-08 | 2014-05-08 | A kind of iron containing sludge utilizing Fenton reagent method to produce solidifies the method for leaded mud |
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| CN201410192244.4A CN103964659B (en) | 2014-05-08 | 2014-05-08 | A kind of iron containing sludge utilizing Fenton reagent method to produce solidifies the method for leaded mud |
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| CN103964659A true CN103964659A (en) | 2014-08-06 |
| CN103964659B CN103964659B (en) | 2015-09-16 |
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| CN201410192244.4A Expired - Fee Related CN103964659B (en) | 2014-05-08 | 2014-05-08 | A kind of iron containing sludge utilizing Fenton reagent method to produce solidifies the method for leaded mud |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554140A (en) * | 2015-09-29 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of residual active sludge cracks decrement method |
| CN107381993A (en) * | 2017-09-05 | 2017-11-24 | 常州大学 | A kind of method using steel plant's pickling iron containing sludge hot setting electroplating sludge |
| CN109293177A (en) * | 2018-09-21 | 2019-02-01 | 德兴市益丰再生有色金属有限责任公司 | One kind being used for the cured method of leaded sludge high temperature |
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2014
- 2014-05-08 CN CN201410192244.4A patent/CN103964659B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102531301A (en) * | 2011-12-31 | 2012-07-04 | 同济大学 | Bottom sediment stabilizing agent and application thereof |
| CN103073166A (en) * | 2013-02-05 | 2013-05-01 | 上海市环境科学研究院 | Method for simultaneously stabilizing heavy metals and deeply dewatering municipal sludge for municipal sludge |
| CN103663920A (en) * | 2013-10-18 | 2014-03-26 | 广州泰历盟环保科技有限公司 | Ferric salt sludge dehydrating agent and sludge dehydrating method |
Non-Patent Citations (1)
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| 沈瑾等: "铁氧体法稳定污泥中重金属的试验方法", 《中国优秀硕士学位论文全文数据库（电子期刊）》, vol. 2, 15 February 2014 (2014-02-15), pages 027 - 454 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106554140A (en) * | 2015-09-29 | 2017-04-05 | 中国石油化工股份有限公司 | A kind of residual active sludge cracks decrement method |
| CN107381993A (en) * | 2017-09-05 | 2017-11-24 | 常州大学 | A kind of method using steel plant's pickling iron containing sludge hot setting electroplating sludge |
| CN109293177A (en) * | 2018-09-21 | 2019-02-01 | 德兴市益丰再生有色金属有限责任公司 | One kind being used for the cured method of leaded sludge high temperature |
| CN109293177B (en) * | 2018-09-21 | 2021-11-23 | 德兴市益丰再生有色金属有限责任公司 | Method for high-temperature solidification of lead-containing sludge |
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| CN103964659B (en) | 2015-09-16 |
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