CN109020134A - A kind of method of two steps annealing method recycling Fenton sludge - Google Patents
A kind of method of two steps annealing method recycling Fenton sludge Download PDFInfo
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- CN109020134A CN109020134A CN201811079168.0A CN201811079168A CN109020134A CN 109020134 A CN109020134 A CN 109020134A CN 201811079168 A CN201811079168 A CN 201811079168A CN 109020134 A CN109020134 A CN 109020134A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
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Abstract
The invention discloses a kind of methods of two steps annealing method recycling Fenton sludge, solve in the prior art that Fenton Treatment of Sludge is at high cost, secondary pollution are also easy to produce, to the disagreeableness problem of environment.The method of the present invention includes the following steps: by Fenton sludge dewatering；It calcines for the first time, obtains the first calcined product；Carbon dust is added into first calcined product, after mixing, carries out second and calcines, obtain the second calcined product；Second calcined product is separated with magnetic separation, respectively obtains Fe3O4And clout.Design science of the present invention, method is simple, easy to operate, is able to achieve the recycling of iron resource in Fenton sludge, environmentally friendly.
Description
Technical field
The invention belongs to technical field of water pollution control, and in particular to a kind of side of two steps annealing method recycling Fenton sludge
Method.
Background technique
Fenton's reaction was chanced on by Fenton HJ in 1893, had there is more than 100 years history till now.Period
Research about Fenton process also emerges one after another, but just starts to start to answer on a large scale inside sewage treatment field in nearly 10 years
With.In recent years in China's field of waste water treatment, standard is increasingly strict, and many types waste water cannot use traditional biological method
Processing is gone, Fenton technology is most mature, simplest technique, gradually in sewage treatment industry inside advanced oxidation processes because of it
The inside comes into vogue.But Fenton technology produces a large amount of iron containing sludge during running.Not due to Fenton technology application time
It is long, lack corresponding sludge treatment experience and method.Currently, China is the standard using danger wastes for this sludge
Processing is gone, which not only adds processing costs, the problem of even more producing secondary pollution, cause huge danger to environment
Evil.
Therefore it provides a kind of method for the iron containing sludge that processing Fenton technology generates, at low cost, and it is pollution-free, become this
Field technical staff's urgent problem to be solved.
Summary of the invention
Technical problem solved by the present invention is a kind of method of two steps annealing method recycling Fenton sludge, solves the prior art
Middle Fenton Treatment of Sludge is at high cost, is also easy to produce secondary pollution, to the disagreeableness problem of environment.
The technical solution adopted by the invention is as follows:
A kind of method of two steps annealing method recycling Fenton sludge of the present invention, comprising the following steps:
Step 1. is by Fenton sludge dewatering；
Step 2. will treated that Fenton sludge is calcined for the first time through step 1, obtains the first calcined product；
Carbon dust is added into first calcined product in step 3., after mixing, carries out second and calcines, obtain second
Calcined product；
Step 4. separates second calcined product with magnetic separation, respectively obtains Fe3O4And clout.
It further, is 0~35wt% by Fenton sludge dewatering to moisture content in the step 1.
Further, in the step 2, the temperature calcined for the first time is 500 DEG C~1500 DEG C, and calcination time is 3h~5h.
Further, in the step 3, the quality of the mixture of first calcined product and carbon dust is based on 100%, carbon
Powder mass content is 1%~20%.
Further, in the step 3,500 DEG C~800 DEG C of temperature of second of calcining, calcination time is 2h~5h.
Further, it in the step 2, calcines carried out in Muffle furnace for the first time.
Further, in the step 3, second of calcining carries out in tube furnace.
Further, the resulting clout of the step 4 is carbon dust or carbon dust and Fe2O3Mixture or carbon dust with
The mixture of FeO.
Further, it in the clout return step 3, mixes, reuses with the first calcined product.
Further, the Fenton sludge is to add FeSO in organic wastewater4And H2O2, after Fenton's reaction, then add
Lye, gained sediment.
Compared with prior art, the invention has the following advantages:
Design science of the present invention, method is simple, easy to operate, the recycling of iron resource in Fenton sludge is able to achieve, to environment
It is friendly.
Ingredient in the dewatered Fenton sludge of step 1 of the present invention is mainly FeOOH and organic matter；It passes it through and forges for the first time
After burning, organic matter is oxidized to carbon dioxide and water discharge, and the main component of the first calcined product of gained is Fe2O3.First is forged
It burns after carbon dust is added in product and carries out second of calcining, the quality of carbon dust is slightly larger than Fe2O3Fe is generated under the action of carbon dust3O4, obtain
The main component of the second calcined product arrived is Fe3O4And carbon dust；By the second calcined product through magnetic separation, Fe is realized3O4With carbon dust
Separation.Fe3O4It utilizes as iron resource, in the resulting carbon dust return step 3 of step 4, is mixed with the first calcined product, repeat benefit
With.The quality of carbon dust is slightly larger than Fe in the present invention2O3Generate Fe3O4Required carbon dust amount, to guarantee Fe2O3It can generate completely
Fe3O4.Low, resulting Fe is put into using the method for the present invention3O4As iron resource, production cost can not only be offsetted, moreover it is possible to realize
Profit.
Detailed description of the invention
Attached drawing 1 is that the temperature and time that the present invention calcines for the first time investigates result figure.
Attached drawing 2 is that the temperature of second of calcining of the present invention investigates result figure.
Specific embodiment
Following specific embodiments can make more detailed description, but subject of the present invention range to the contents of the present invention
Following specific embodiments are not limited to, all technologies realized based on the content of present invention, technique are all belonged to the scope of the present invention.
Embodiment 1
The investigation for the temperature and time that the present invention calcines for the first time is present embodiments provided, specific as follows:
Simulation urotropine wastewater is handled using Fenton process: the pH of waste water being transferred to 4, sequentially adds the FeSO of 5g/L4With
The H of 15g/L2O2, alkali is added after reaction, adjusts pH value to 7, staticly settles, gained sediment is Fenton sludge, main component
For FeOOH and organic matter；It is 15wt% by Fenton sludge dewatering to water content.
Five parts of the dewatered Fenton sludge is taken, is weighed, is placed in Muffle furnace, is forged under conditions of different temperature respectively
After burning the different time, weighing.With calcined Fenton sludge weight divided by the Fenton sludge weight before calcining, before obtaining calcining
Weight ratio afterwards investigates the oxidization condition of organic matter in Fenton sludge with this, as a result as shown in Fig. 1, it may be assumed that
When calcination temperature is set as 100 DEG C, 1 hour to 5 hours after calcining, calcining front and back weight ratio is unchanged；
When calcination temperature is set as 200 DEG C, 0 hour to 5 hours after calcining, calcining front and back weight ratio becomes in decline
Gesture tends towards stability for 5-6 hours；
When calcination temperature is set as 300 DEG C, 0 hour to 4 hours after calcining, calcining front and back weight ratio becomes in decline
Gesture tends towards stability for 4-6 hours；
When calcination temperature is set as 400 DEG C, 0 hour to 3 hours after calcining, calcining front and back weight ratio becomes in decline
Gesture tends towards stability for 3-6 hours；
When calcination temperature is set as 500 DEG C, 0 hour to 3 hours after calcining, calcining front and back weight ratio becomes in decline
Gesture tends towards stability for 3-6 hours；
And calcination temperature, when being 400 DEG C -500 DEG C, weight ratio is consistent before and after final calcining, shows calcination temperature not
Less than 400 DEG C up to the organic matter in complete oxidation Fenton sludge.
It can be seen that calcined temperature is not less than 400 DEG C for the first time, calcination time is not less than 3 hours, can complete oxidation sweet smell
Organic matter in sludge.
Embodiment 2
The investigation of the temperature and time of second of calcining of the present invention is present embodiments provided, specific as follows:
The first calcined product for calcining 5 hours through 500 DEG C and the carbon dust ratio of 84:16 in mass ratio in Example 1
After mixing, it is divided into 5 parts, is respectively put into tube furnace, calcines the different time under conditions of different temperature respectively, obtain
To the second calcined product, which is analyzed by X-ray diffractometer respectively, as a result as shown in Fig. 2, it may be assumed that
When calcination temperature is lower than 500 DEG C, the iron of the second calcined product is with Fe2O3Form exist；
When calcination temperature is 500 DEG C, start the Fe for having occurred a small amount of in the second calcined product3O4；
When calcination temperature is greater than 500 DEG C and when less than 700 DEG C, Fe in the second calcined product3O4Amount gradually increase；
When calcination temperature is 700 DEG C, the iron of the second calcined product is with Fe3O4Form exist；
When calcination temperature is greater than 700 DEG C and less than 800 DEG C, the second calcined product begins with FeO generation；
When calcination temperature is 900 DEG C or more, start to generate Fe in the second calcined product.
When the iron of the second calcined product is with Fe3O4Form in the presence of, have magnetism, can be using magnetic separation by itself and carbon dust point
From therefore, the temperature of second of calcining selects 500 DEG C -800 DEG C.
Embodiment 3
The method for present embodiments providing two steps annealing method recycling Fenton sludge of the invention, specifically:
Simulation urotropine wastewater is handled using Fenton process: the pH of waste water being transferred to 4, sequentially adds the FeSO of 5g/L4With
The H of 15g/L2O2, alkali is added after reaction, adjusts pH value to 7, staticly settles, gained sediment is Fenton sludge, main component
For FeOOH and organic matter；
It is 15wt% by Fenton sludge dewatering to water content；
Dewatered Fenton sludge is placed in Muffle furnace, calcines 3h under conditions of 500 DEG C, the carbon dioxide of calcining and
Water discharge, the solid calcined are the first calcined product.After calcining for the first time, the organic matter in Fenton sludge is basic
It is oxidized completely, generates carbon dioxide and water discharge, the main component of the first calcined product of gained is to be generated by FeOOH
Fe2O3；
First calcined product and the carbon dust ratio of 84:16 in mass ratio are uniformly mixed, are put into tube furnace, at 700 DEG C
Under conditions of calcine 2h, obtain the second calcined product.The main component of second calcined product is by Fe2O3The Fe being transformed into3O4,Carbon
Powder and a small amount of Fe2O3。
Due to Fe3O4With magnetism, the second calcined product is passed through into magnetic separating, realizes Fe3O4With carbon dust, a small amount of Fe2O3
Separation.Fe3O4It is utilized as iron resource, carbon dust and a small amount of Fe2O3It can mix, repeat with the first calcined product again as clout
It utilizes.Fe3O4Magnetic separation with carbon dust is separated into the prior art, effectively realizes Fe using iron powder magnetic separation function3O4With point of carbon dust
From.
Embodiment 4
The method for present embodiments providing two steps annealing method recycling Fenton sludge of the invention, specifically:
Simulation urotropine wastewater is handled using Fenton process: the pH of waste water being transferred to 3, sequentially adds the FeSO of 5g/L4With
The H of 15g/L2O2, be added alkali after reaction, adjust pH value to 7.5, staticly settle, gained sediment is Fenton sludge, mainly at
It is divided into FeOOH and organic matter；
It is 0wt% by Fenton sludge dewatering to water content；
Dewatered Fenton sludge is placed in Muffle furnace, calcines 3h under conditions of 400 DEG C, the carbon dioxide of calcining and
Water discharge, the solid calcined are the first calcined product.After calcining for the first time, the organic matter in Fenton sludge is basic
It is oxidized completely, generates carbon dioxide and water discharge, the main component of the first calcined product of gained is to be generated by FeOOH
Fe2O3；
First calcined product and the carbon dust ratio of 9:1 in mass ratio are uniformly mixed, are put into tube furnace, at 700 DEG C
Under the conditions of calcine 2h, obtain the second calcined product.The main component of second calcined product is by Fe2O3The Fe being transformed into3O4, with
And carbon dust.
Due to Fe3O4With magnetism, the second calcined product is passed through into magnetic separating, realizes Fe3O4With the separation of carbon dust.
Fe3O4It is utilized as iron resource, carbon dust can be mixed with the first calcined product again, be reused.
Embodiment 5
The method for present embodiments providing two steps annealing method recycling Fenton sludge of the invention, specifically:
Simulation urotropine wastewater is handled using Fenton process: the pH of waste water being transferred to 3.5, sequentially adds the FeSO of 5g/L4
With the H of 15g/L2O2, alkali is added after reaction, adjusts pH value to 7.5, staticly settles, gained sediment is Fenton sludge, main
Ingredient is FeOOH and organic matter；
It is 35wt% by Fenton sludge dewatering to water content；
Dewatered Fenton sludge is placed in Muffle furnace, calcines 5h under conditions of 600 DEG C, the carbon dioxide of calcining and
Water discharge, the solid calcined are the first calcined product.After calcining for the first time, the organic matter in Fenton sludge is basic
It is oxidized completely, generates carbon dioxide and water discharge, the main component of the first calcined product of gained is to be generated by FeOOH
Fe2O3；
First calcined product and the carbon dust ratio of 85:15 in mass ratio are uniformly mixed, are put into tube furnace, at 800 DEG C
Under conditions of calcine 2h, obtain the second calcined product.The main component of second calcined product is by Fe2O3The Fe being transformed into3O4、
Carbon dust and on a small quantity by Fe3O4The FeO being transformed into.
Due to Fe3O4With magnetism, the second calcined product is passed through into magnetic separating, realizes Fe3O4With carbon dust, a small amount of FeO
Separation.Fe3O4It is utilized as iron resource, carbon dust and a small amount of FeO can be mixed with the first calcined product again as clout, be reused.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit protection model of the invention
It encloses, as long as that in body design thought of the invention and mentally makes has no the change of essential meaning or polishing, is solved
The technical issues of it is still consistent with the present invention, should all be included within protection scope of the present invention.
Claims (10)
1. a kind of method of two steps annealing method recycling Fenton sludge, which comprises the following steps:
Step 1. is by Fenton sludge dewatering；
Step 2. will treated that Fenton sludge is calcined for the first time through step 1, obtains the first calcined product；
Carbon dust is added into first calcined product in step 3., after mixing, carries out second and calcines, obtain the second calcining
Product；
Step 4. separates second calcined product with magnetic separation, respectively obtains Fe3O4And clout.
2. the method according to claim 1, wherein being by Fenton sludge dewatering to moisture content in the step 1
0~35wt%.
3. according to the method described in claim 2, it is characterized in that, in the step 2, the temperature calcined for the first time is 500 DEG C~
1500 DEG C, calcination time is 3h~5h.
4. the method according to claim 1, wherein in the step 3, first calcined product and carbon dust
For the quality of mixture based on 100%, carbon dust mass content is 1%~20%.
5. according to the method described in claim 4, it is characterized in that, in the step 3,500 DEG C of the temperature of second of calcining~
800 DEG C, calcination time is 2h~5h.
6. according to the method described in claim 5, it is characterized in that, calcining carried out in Muffle furnace for the first time in the step 2.
7. according to the method described in claim 6, it is characterized in that, in the step 3, second of calcining in tube furnace into
Row.
8. the method according to the description of claim 7 is characterized in that the resulting clout of the step 4 be carbon dust or carbon dust with
Fe2O3Mixture or carbon dust and FeO mixture.
9. according to the method described in claim 8, it is characterized in that, being mixed in the clout return step 3 with the first calcined product
It closes, recycling.
10. method described in -9 any one according to claim 1, which is characterized in that the Fenton sludge is in organic wastewater
Add FeSO4And H2O2, after Fenton's reaction, then lye is added, gained sediment.
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| CN201811079168.0A CN109020134A (en) | 2018-09-17 | 2018-09-17 | A kind of method of two steps annealing method recycling Fenton sludge |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994022772A1 (en) * | 1993-04-01 | 1994-10-13 | Solvay Interox Gmbh | Oxidative method of purifying highly contaminated waste water |
| CN101491771A (en) * | 2009-03-02 | 2009-07-29 | 华东理工大学 | Fenton and Fenton-like reaction catalyst regeneration and reclamation method |
| CN104437502A (en) * | 2014-12-15 | 2015-03-25 | 南京理工大学 | Magnetic fenton catalyst spinel ferrite employing fenton iron sludge as iron source and application of magnetic fenton catalyst spinel ferrite |
| CN104818381A (en) * | 2015-05-26 | 2015-08-05 | 长安大学 | Method for recovering iron from Bayer process red mud |
| CN105254067A (en) * | 2015-10-28 | 2016-01-20 | 同济大学 | Resource utilization method for advanced wastewater treatment Fenton method sludge |
| CN106946330A (en) * | 2017-03-31 | 2017-07-14 | 华南理工大学 | A kind of method that chemical oxidation iron cement prepares water treatment agent |
| CN107760862A (en) * | 2017-10-19 | 2018-03-06 | 东北大学 | A kind of method from recovering iron from red mud |
-
2018
- 2018-09-17 CN CN201811079168.0A patent/CN109020134A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994022772A1 (en) * | 1993-04-01 | 1994-10-13 | Solvay Interox Gmbh | Oxidative method of purifying highly contaminated waste water |
| CN101491771A (en) * | 2009-03-02 | 2009-07-29 | 华东理工大学 | Fenton and Fenton-like reaction catalyst regeneration and reclamation method |
| CN104437502A (en) * | 2014-12-15 | 2015-03-25 | 南京理工大学 | Magnetic fenton catalyst spinel ferrite employing fenton iron sludge as iron source and application of magnetic fenton catalyst spinel ferrite |
| CN104818381A (en) * | 2015-05-26 | 2015-08-05 | 长安大学 | Method for recovering iron from Bayer process red mud |
| CN105254067A (en) * | 2015-10-28 | 2016-01-20 | 同济大学 | Resource utilization method for advanced wastewater treatment Fenton method sludge |
| CN106946330A (en) * | 2017-03-31 | 2017-07-14 | 华南理工大学 | A kind of method that chemical oxidation iron cement prepares water treatment agent |
| CN107760862A (en) * | 2017-10-19 | 2018-03-06 | 东北大学 | A kind of method from recovering iron from red mud |
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