CN103964659B - A kind of iron containing sludge utilizing Fenton reagent method to produce solidifies the method for leaded mud - Google Patents

A kind of iron containing sludge utilizing Fenton reagent method to produce solidifies the method for leaded mud Download PDF

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Publication number
CN103964659B
CN103964659B CN201410192244.4A CN201410192244A CN103964659B CN 103964659 B CN103964659 B CN 103964659B CN 201410192244 A CN201410192244 A CN 201410192244A CN 103964659 B CN103964659 B CN 103964659B
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China
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sludge
iron
produce
mud
leaded
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CN201410192244.4A
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Chinese (zh)
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CN103964659A (en
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李琴
毛林强
崔皓
安浩
邓宁
翟建平
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南京大学
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Abstract

The invention discloses a kind of method that iron containing sludge utilizing Fenton reagent method to produce solidifies leaded electroplating sludge, by leaded electroplating sludge immobilization while recycling iron containing sludge, can significantly reduce plumbous leaching.Concrete technology step of the present invention is: (1) is levigate after iron containing sludge and leaded mud being dried, mixing; (2) by mixing two kinds of mud repressed after through high-temperature calcination process.Due to Fe (OH) in iron mud 3can with Pb (OH) 2at high temperature reaction generates stable PbFe 12o 19, be enough to the erosion of resisting acid-base solution, effectively prevent plumbous leaching, reach the object of the plumbous mud of safety solidification; There is good economy performance, subtract the advantages such as capacity is large.

Description

A kind of iron containing sludge utilizing Fenton reagent method to produce solidifies the method for leaded mud

Technical field

The present invention relates to solid waste resource recovery and utilize field, be specifically related to a kind of iron containing sludge adopting Fenton reagent method to produce solidifies leaded electroplating sludge method as 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 the spies such as moisture content is high, heavy metal content is high, easily leached.Plumbous and compound is poisonous to human body, easily accumulated in creatures, after picked-up, major storage is in bone, and part replaces the calcium in calcium phosphate, not easily discharges, poisoning darker time can cause system damage, can lead encephalopathy be caused time serious.Because the mobility of lead is comparatively large, in by the process of banking up, easily produce serious threat to the environment of periphery, therefore how the leaded mud of safe disposal is the focus of field of environment engineering always.

Curing/stabilizing process is the Main Means of heavy metal sewage sludge always, mainly comprises the coated solidification such as cement, glass.Thermal treatment causes the concern of people gradually owing to having the advantage such as significantly minimizing, recovery energy wherein; And the cost of heat treatment for solidification comparatively cement, vitrification cost is low, in Europe using the means of thermal treatment as main process solid waste in future.Fenton reagent method is widely used in the process of high concentrated organic wastewater, but its main drawback is the mud easily produced containing a large amount of ironic hydroxide, in mud, the content of ironic hydroxide is even up to 50%, usually stove ironmaking is returned in iron containing sludge dehydration, but if efficiency utilization iron containing sludge produces important meaning by the popularization of Fenton reagent method.A Chinese patent (CN 200910198271.1) discloses a kind of method of pickling iron containing sludge recycling, concrete steps are that iron containing sludge drying directly utilizes high pressure to suppress balling-up afterwards, send in 1100 DEG C of High Temperature Furnaces Heating Apparatuss and be no less than 1h, the flammable CO Gas recovery produced in heat-processed, liberated heat is used for pressure ball and is entering the heating of stokehold, the remaining drying that can be used for mud, the problem that the high energy gamma source that this solves pyroprocessing consumes.Another Chinese patent (publication number CN 201010023054.1) proposes and a kind ofly adopts iron containing sludge to add to meet the method that sizing agent prepares cooled agglomerated pellet, by adding Organic adhesive (vinyl acetate, vinylformic acid, Xylo-Mucine, polyvinyl alcohol etc.) and the good cohesiveness of inorganic additives (wilkinite, calcium oxide, alkaline sodium silicate etc.) generation to iron containing sludge, but it is complicated that shortcoming is addO-on therapy, and each component strictly must control proportioning in certain sequence.More than open invention relate to the recycling of iron containing sludge, but there is the problem such as operation steps complexity, technical process length.Have not been reported as the research utilizing iron containing sludge to solidify electroplating sludge.

Summary of the invention

Problem to be solved by this invention is that in the iron containing sludge recycling and plating production process produced for Fenton reagent method, the leaded mud that produces is difficult to process problem, both is combined and forms a kind of iron containing sludge utilizing Fenton reagent method to produce solidifies leaded mud method by means of calcination.

A kind of iron containing sludge utilizing Fenton reagent method to produce of the present invention solidifies the method for leaded electroplating sludge, 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 the Fe/Pb=12-15 mixing in molar ratio of levigate two kinds of mud, mixed mud is placed in again ball mill and adopts wet-milling mode levigate;

3) by step 2) ball milling mixing terminate 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 the inherent temperature 800-1000 DEG C of calcining 2.5-4h of retort furnace, after cooling, namely achieves iron containing sludge and solidify 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.

During 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 reaction further 12o 19, due to PbFe 12o 19there is excellent chemical stability and physical strength, the erosion of acid, alkali and other undesirable elements can be resisted in environment after solidification, prevents the solvable lead in mud from flowing in environment.

Embodiment

Below in conjunction with example, the invention will be further described, and following examples are intended to the present invention instead of limitation of the invention further are described.

Embodiment 1

The iron containing sludge produce Fenton reagent method and leaded electroplating sludge (leaded 20%) are placed in 105 DEG C respectively 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 the Fe/Pb=12 mixing in molar ratio of levigate two kinds of mud, 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.The mixing sludge of oven dry, 105 DEG C of oven dry, is then suppressed through tabletting machine, tabletting machine pressure range 500kg/cm by mixing sludge slurries ball milling mixing terminated 2.Block mud through tabletting machine compacting is placed in retort furnace inherent temperature 800 DEG C calcining 2.5h.After levigate after burnt block mud is pulverized, adopt " the leaching toxicity from solid waste method-hac buffer method " of amendment to leach 22d continuously, leach the lead concentration 25mg/L terminated in rear solution.

Embodiment 2

The iron containing sludge produce Fenton reagent method and leaded electroplating sludge (leaded 45%) are placed in 105 DEG C respectively 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 the Fe/Pb=15 mixing in molar ratio of levigate two kinds of mud, 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.The mixing sludge of oven dry, 200 DEG C of oven dry, is then suppressed through tabletting machine, tabletting machine pressure range 1000kg/cm by mixing sludge slurries ball milling mixing terminated 2.Block mud through tabletting machine compacting is placed in retort furnace inherent temperature 1000 DEG C calcining 4h.After levigate after burnt block mud is pulverized, adopt " the leaching toxicity from solid waste method-hac buffer method " of amendment to leach 22d continuously, leach the lead concentration 12mg/L terminated in rear solution.

Embodiment 3

The iron containing sludge produce Fenton reagent method and leaded electroplating sludge (lead concentration 16%) are placed in 105 DEG C respectively 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 the Fe/Pb=14 mixing in molar ratio of levigate two kinds of mud, 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.The mixing sludge of oven dry, 200 DEG C of oven dry, is then suppressed through tabletting machine, tabletting machine pressure range 750kg/cm by mixing sludge slurries ball milling mixing terminated 2.Block mud through tabletting machine compacting is placed in retort furnace inherent temperature 900 DEG C calcining 3h.After levigate after burnt block mud is pulverized, adopt " the leaching toxicity from solid waste method-hac buffer method " of amendment to leach 22d continuously, leach the lead concentration 20mg/L terminated in rear solution.

Embody rule 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 improvement also should be considered as protection scope of the present invention.

Claims (6)

1. the iron containing sludge utilizing Fenton reagent method to produce solidifies a method for leaded electroplating sludge, it is characterized in that comprising the following steps:
1) by Fenton reagent method produce iron containing sludge and electroplating sludge dry respectively, the iron containing sludge of oven dry and electroplating sludge are placed in respectively ball mill pulverize, levigate;
2) by the Fe/Pb=12-15 mixing in molar ratio of levigate two kinds of mud, mixed mud is placed in again ball mill and adopts wet-milling mode levigate;
3) by step 2) ball milling mixing terminate 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 the inherent temperature 800-1000 DEG C of calcining 2.5-4h of retort furnace, after cooling, namely achieves iron containing sludge and solidify leaded electroplating sludge.
2. the iron containing sludge utilizing Fenton reagent method to produce according to claim 1 solidifies the method for leaded electroplating sludge, it is characterized in that: the bake out temperature of step 1) is 105 DEG C, and drying time is 24-48.
3. the iron containing sludge utilizing Fenton reagent method to produce according to claim 1 and 2 solidifies the method for leaded electroplating sludge, it is characterized in that: the drum's speed of rotation 50-100r/min of step 1), Ball-milling Time 0.5-2h.
4. the iron containing sludge utilizing Fenton reagent method to produce according to claim 1 and 2 solidifies the method for leaded electroplating sludge, it 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 iron containing sludge utilizing Fenton reagent method to produce according to claim 1 and 2 solidifies the method for leaded electroplating sludge, it is characterized in that: the bake out temperature of step 3) is 105-200 DEG C.
6. the iron containing sludge utilizing Fenton reagent method to produce according to claim 1 and 2 solidifies the method for leaded electroplating sludge, it is characterized in that: during step 3) compressing tablet, pressure range is 500-1000kg/cm 2.
CN201410192244.4A 2014-05-08 2014-05-08 A kind of iron containing sludge utilizing Fenton reagent method to produce solidifies the method for leaded mud CN103964659B (en)

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CN106554140B (en) * 2015-09-29 2019-04-16 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

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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

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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

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