CN110314687A - Fe3+Load composite catalyst and its preparation method and class Fenton sludge dewatering preprocess method - Google Patents
Fe3+Load composite catalyst and its preparation method and class Fenton sludge dewatering preprocess method Download PDFInfo
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- CN110314687A CN110314687A CN201910689794.XA CN201910689794A CN110314687A CN 110314687 A CN110314687 A CN 110314687A CN 201910689794 A CN201910689794 A CN 201910689794A CN 110314687 A CN110314687 A CN 110314687A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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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
- C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
- C02F11/14—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
- C02F11/143—Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents using inorganic substances
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
A kind of Fe3+Composite catalyst and its preparation method and class Fenton sludge dewatering preprocess method are loaded, cities and towns disposition of solid waste and resource utilization field are belonged to.The Fe3+The carrier for loading composite catalyst is mud granule and clay mineral, wherein in mass ratio, mud granule: clay mineral=(3~5): 1；Fe3+Load Fe in composite catalyst3+Average load amount be 5~10mmol/g.Its preparation method are as follows: after mixing carrier, FeCl is added3Solution is granulated, and drying and calcining is made.By the Fe3+It loads in composite catalyst, with Fe3+Substitute Fe2+, with H2O2Class Fenton's reaction occurs under the conditions of raw sewage pH, to carry out sludge reinforcing dehydration pre-process efficiently, economic to sludge.Fe3+Load composite catalyst can recycle.This method can make sludge achieve the purpose that quickly and efficiently to be dehydrated, and reduce sludge subsequent treatment cost, realize the treatment of wastes with processes of wastes against one another, economical and effective.
Description
Technical field
The invention belongs to the technical field of cities and towns disposition of solid waste and resource utilization, specifically a kind of Fe3+
Load composite catalyst and its preparation method and class Fenton sludge dewatering preprocess method.
Background technique
China increasingly payes attention to sewage treatment, and sewage treatment has reached quite high level, and specific resistance to filtration
It is horizontal to be improved.Currently, most cities sewage treatment plant handles sewage using biochemical process, will necessarily produce in the process
Raw a large amount of biochemical sludge, the usual complicated components of sludge, variability is big, and moisture content is high (usually >=99% or more), concentrated
Treated sludge, for moisture content still 90% or more, the scale of construction is huge, makes troubles to transport, storage and use, and is possible to
Cause the secondary pollution of environment.Therefore, sludge dewatering has become the important link during specific resistance to filtration.To improve sludge
Filtering means dehydration performance, need to improve sludge.Common sludge conditioning technology is broadly divided into physical method (freeze thawing, machinery
Energy, heating, microwave, HIGH PRESSURE TREATMENT etc.), chemical method (soda acid, addition flocculant, Fenton processing etc.) and bioanalysis (sludge it is good
Oxygen and Anaerobic Digestion) three classes.Above method has an application in practice, but because chemical method have easy to operate, operation at
The advantages such as this is lower, conditioning effect is stable are current most popular methods.In chemical method, Fenton processing has convenient fast
Victory, it is easily operated the advantages that be widely used in industrial processes.But strong acid environment is needed in traditional Fenton's reaction,
PH narrow scope of application, and Fe2+Addition be easy to produce iron cement and cannot recycle, therefore limit tradition to a certain degree
The application of Fenton's reaction.
Summary of the invention
The problem to be solved in the present invention is just to provide a kind of Fe3+It loads composite catalyst and its preparation method and class Fenton sludge is de-
Water pretreatment process, this method are the methods based on advanced oxidation, and this method is equipped with using excess sludge as catalyst support material
Clay mineral prepares loaded catalyst, with Fe3+Substitute Fe2+, with H2O2Class Fenton's reaction occurs under the conditions of raw sewage pH,
To carry out sludge reinforcing dehydration pre-process efficiently, economic to sludge.Sludge can be made to reach quick and high using the present invention
The purpose of dehydration is imitated, reduces sludge subsequent treatment cost, while catalyst preparation embodies the thought of the treatment of wastes with processes of wastes against one another, the present invention is
A kind of economy, actual effect sludge strengthen dehydration pre-process method.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of Fe of the invention3+Load the preparation method of composite catalyst, comprising the following steps:
Step 1: sludge pretreatment
Sludge is dehydrated, dried, is ground up, sieved, the mud granule of >=60 mesh is obtained；
Step 2:
Mud granule is mixed with clay mineral, obtains mixture；Wherein, in mass ratio, mud granule: clay mineral=
(3~5): 1；
Into mixture, the FeCl that substance withdrawl syndrome is 20~40mmol/L is added3Solution, while EDTA- is added
2Na is stirred evenly, and is granulated, is obtained haydite；Wherein, by volume, mixture: FeCl3Solution=1:(1~1.5)；EDTA-
The mass percent that the additional amount of 2Na accounts for mud granule is 0~0.5%；
Step 3: drying and calcining
By haydite, naturally dry, the haydite dried；After the haydite dried is placed in 100~110 DEG C of dryings completely,
It is immediately placed in 450~600 DEG C again, keeps the temperature 3~6min, be continuously heating to 900~1100 DEG C, keep the temperature 10~20min, it is cold with furnace
But it to room temperature, takes out, obtains Fe3+Load composite catalyst.
In the step 1, the dehydration is that physics is dehydrated or filters pressing, suction filtration, mistake are selected in chemical dehydration, physics dehydration
One or more of filter, centrifugation.
In the step 2, the average diameter of the haydite is 4~6mm.
In the step 3, the drying is complete, preferably 4~6h.
The Fe3+In the preparation method for loading composite catalyst, the addition of the EDTA-2Na, the purpose is to prevent
Fe3+It precipitates.
A kind of Fe3+Composite catalyst is loaded, is made using above-mentioned preparation method.
A kind of Fe3+Composite catalyst is loaded, carrier is mud granule and clay mineral, wherein in mass ratio, sludge
Grain: clay mineral=(3~5): 1；Fe3+Load Fe in composite catalyst3+Average load amount be 5~10mmol/g.
A kind of Fe3+Fenton-type reagent, including Fe3+Load composite catalyst and H2O2Reagent, in molar ratio, Fe3+Load
Fe in composite catalyst3+: H2O2H in reagent2O2=1:(2~3)；
The H2O2Reagent is preferably the H that mass percentage is 30%2O2Aqueous solution.
One kind being based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, using above-mentioned Fe3+Class Fenton examination
Agent realizes the reinforcing dehydration pre-process of sludge by carrying out class Fenton oxidation process to sludge.
It is described based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, specifically includes the following steps:
Into sludge conditioning pond by sludge condensation treated sludge to be processed, Fe is added3+Load composite catalyst
With H2O2Reagent is stirred, the sludge after obtaining dehydration pre-process；Wherein, Fe3+Load composite catalyst accounts for dirt to be processed
The substance withdrawl syndrome of mud is 30~50mmol/L, H2O2Reagent account for sludge to be processed substance withdrawl syndrome be 60~
150mmol/L；The stirring pretreatment, speed of agitator are 30~50r/min, and pretreatment time is 60~90min；
The excess sludge of sludge to be processed from sludge concentration tank, moisture content >=90%.
Using method of the invention, sludge after the dehydration pre-process of preparation can be used for Fe of the present invention3+Load compound urge
The sludge raw material of agent.
A kind of Fe of the invention3+Composite catalyst is loaded, for the Fe that can be recycled3+Load composite catalyst.
A kind of Fe3+Load the recoverying and utilizing method of composite catalyst are as follows: in the sludge after dehydration pre-process, using filtering
Mode is by Fe3+Sludge separation after loading composite catalyst and dehydration pre-process, by the Fe after separation3+Load composite catalyst
After cleaning, drying, reused.
A kind of Fe of the invention3+Composite catalyst and its preparation method and the pretreated method of sludge dewatering are loaded, principle is:
Make sludge dewatering using the method for advanced oxidation, is destroyed using the strong oxidizer intermediate product hydroxyl radical free radical (OH) of generation dirty
Mud structure discharges and combines water, reinforcement sludge dehydrating effect in more sludge.
A kind of Fe of the invention3+Load composite catalyst and its preparation method and the pretreated method of sludge dewatering, advantage and
Beneficial effect is:
1, the present invention is dehydrated using the method reinforcement sludge of advanced oxidation, and with Fe3+Substitute the Fe in traditional Fenton's reaction2 +, Fe3+Load composite catalyst and H2O2Class Fenton's reaction is formed, dehydration can be strengthened under the conditions of sewage original pH, it is fragrant to solve tradition
The drawbacks of reaction of pausing must carry out under strongly acidic conditions realizes the reinforcing dehydration of sludge.
2, the present invention is Fe with sludge3+The backing material for loading composite catalyst prepares Fe3+Load composite catalyst, body
The theory of existing " treatment of wastes with processes of wastes against one another ".
3, Fe of the invention3+Load composite catalyst can recycle and reuse, and be the sludge reinforcing of a kind of economy, actual effect
Dehydration pre-process method.
4, Fe prepared by the present invention3+Composite catalyst is loaded, is and to be equipped with clay mineral using excess sludge as backing material
Prepare Fe3+Composite catalyst is loaded, EDTA-2Na is added in preparation process, prevents Fe3+It precipitates.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
In the present invention, specified otherwise is removed, solution is its aqueous solution.Concentration is mass concentration.
In following embodiment, the dehydration pre-process reaction unit of use are as follows: the reaction unit of the present embodiment is that volume is 1L
Column PVC tank (diameter 10cm), by electric mixer to sludge and Fe to be processed3+Fenton-type reagent mixed
Stirring.
In following embodiment, use for try sludge: sludge come from sewage treatment plant, Fushun City concentration basin, basic parameter
It is shown in Table 1:
One kind being based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, including following measures:
1) excess sludge is backing material and the Fe for being equipped with clay mineral3+Composite catalyst is loaded, EDTA-2Na is added,
Prevent Fe3+It precipitates；
2)Fe3+Substitute the Fe in traditional Fenton's reaction2+, Fe3+Load composite catalyst and H2O2Class Fenton's reaction is formed, it can
Strengthen dehydration under the conditions of sludge original pH；
3) the recyclable recycling of composite catalyst.
Embodiment 1
(1) a kind of Fe3+Load the preparation method of composite catalyst, comprising the following steps:
Step 1: sludge pretreatment
Sludge is the excess sludge of the moisture content 80% obtained after plate and frame filter press filters pressing, drying, grinding
Afterwards, 60 meshes are crossed, mud granule is obtained；
Step 2:
The kaolin that the present embodiment uses is clay mineral；In mass ratio, mud granule: kaolin=5:1, by sludge
Grain is mixed with kaolin, obtains mixture；
Into mixture, the FeCl that substance withdrawl syndrome is 30mmol/L is added3Solution, while adding mud granule quality
0.5% EDTA-2Na is granulated after mixing evenly, prepares the haydite that diameter is 5mm；Wherein, by volume, mixture:
FeCl3Solution=1:1.5；
Step 3: drying and calcining
The haydite of preparation is dried.It is placed in 100 DEG C of drying 5h of baking oven again, is immediately moved into initial temperature later and is set as 500
In DEG C Muffle furnace, in 500 DEG C of heat preservation 5min, continues temperature and rise to 1000 DEG C, and in 1000 DEG C of heat preservation 15min.In furnace certainly later
It is so cooled to room temperature, takes out, obtains Fe3+It is stand-by to load composite catalyst.The Fe of preparation3+Load Fe in composite catalyst3+It is flat
Equal load capacity is 6mmol/g.
(2) a kind of Fe3+Fenton-type reagent, including Fe manufactured in the present embodiment3+Load composite catalyst and H2O2Reagent,
In molar ratio, Fe3+Load Fe in composite catalyst3+: H2O2H in reagent2O2=1:3；
(3) a kind of to be based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, specifically includes the following steps:
Fe is first added in for examination sludge3+Load composite catalyst, additive amount are as follows: for trying the wet mud volume of sludge
Meter, wherein the Fe of addition3+Load Fe in composite catalyst3+Substance withdrawl syndrome be 30mmol/L, H2O2(30%) dosage
The substance withdrawl syndrome of wet mud volume is accounted for as 90mmol/L, under the conditions of sludge original pH (about 6.9), 40r/min locates sludge in advance
Manage 90min, the sludge after obtaining dehydration pre-process.
(4) treatment effect: in the sludge after dehydration pre-process, moisture content of the cake can be down to 60%, CST and be decreased to 16s,
SRF and MLSS reduce by 50% respectively, and dehydration property significantly increases.
(5) a kind of Fe3+Load the recoverying and utilizing method of composite catalyst are as follows: in the sludge after dehydration pre-process, use
Filter type is by Fe3+Sludge separation after loading composite catalyst and dehydration pre-process, by the Fe after separation3+Load compound urge
After agent cleaning, drying, reused.Remove Fe3+The sludge of load composite catalyst is recycled.
Embodiment 2
(1) a kind of Fe3+Load the preparation method of composite catalyst, comprising the following steps:
Step 1: sludge pretreatment
Sludge is to remove Fe in embodiment 13+Sludge after loading the dehydration pre-process of composite catalyst, this sludge pass through
Fe3+Load composite catalyst and H2O2After the Fenton-type reagent pretreatment of composition, using removal Fe3+Composite catalyst is loaded,
It is dehydrated through filtering, moisture content of the cake 62.7%.Sludge crosses 60 meshes after drying, grinding, obtains mud granule；
Step 2:
The attapulgite that the present embodiment uses is viscosity mineral；In mass ratio, mud granule: attapulgite=5:1, it will be dirty
Mud particle is mixed with attapulgite, obtains mixture；
Into mixture, the FeCl that substance withdrawl syndrome is 40mmol/L is added3Solution, while addition accounts for mud granule matter
The EDTA-2Na that percentage is 0.5% is measured, after mixing evenly, is granulated, the haydite that preparation average diameter is 5mm.Wherein, by volume
Than mixture: FeCl3Solution=1:1；
Step 3: drying and calcining
By the haydite naturally dry of preparation.It is complete to drying that it is placed in 110 DEG C of drying 5h of baking oven again, is immediately moved into later initial
Temperature setting is in 500 DEG C of Muffle furnaces, and 5min is kept at 500 DEG C, and temperature rises to 1000 DEG C, and keeps at 1000 DEG C
15min.Cooled to room temperature in furnace later is taken out, obtains Fe3+It is stand-by to load composite catalyst.The Fe of preparation3+Load is multiple
Close Fe in catalyst3+Average load amount be 8mmol/g.
(2) a kind of Fe3+Fenton-type reagent, including Fe manufactured in the present embodiment3+Load composite catalyst and H2O2Reagent,
In molar ratio, Fe3+Load Fe in composite catalyst3+: H2O2H in reagent2O2=1:3；
(3) a kind of to be based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, specifically includes the following steps:
Load composite catalyst is added in for examination sludge, additive amount is 5g/L (wherein, Fe3+It loads in composite catalyst
Fe3+Substance withdrawl syndrome be 40mmol/L), H2O2(30%) dosage accounts for the substance withdrawl syndrome of wet mud volume and is
Under the conditions of 120mmol/L, sludge original pH (about 6.9), dirt of the 40r/min to sludge pretreatment 90min, after obtaining dehydration pre-process
Mud.
(4) treatment effect: the sludge after dehydration pre-process, moisture content of the cake are down to 60% hereinafter, dewatering performance of sludge
It improves.
Embodiment 3
The Fe that will be recycled in embodiment 13+Load composite catalyst recycling, and H2O2The Fe that reagent is formed3+Class
The pretreated method of the sludge dewatering of Fenton reagent, specifically includes the following steps:
(1) used Fe in embodiment 13+Composite catalyst is loaded, by filtering and the sludge point after dehydration pre-process
From being sent into next group of sludge dewatering Pretreatment Test (experiment condition is with embodiment 1) after deionized water is washed and is dried；
(2) Fe of recovered processing is first added in for examination sludge3+Composite catalyst is loaded, wherein H2O2(30%) it adds
The substance withdrawl syndrome that amount accounts for wet mud volume is still 90mmol/L, and under the conditions of sludge original pH (about 6.9), 40r/min is to sludge
Pre-process 90min, the sludge after obtaining dehydration pre-process.
(3) treatment effect: in the sludge after dehydration pre-process, moisture content of the cake can be down to 64.8%, under dehydration rate slightly has
Drop, dewatering performance of sludge are still remarkably reinforced, Fe3+Loading composite catalyst has good recycling property.
Embodiment 4
A kind of Fe3+Load the preparation method of composite catalyst, comprising the following steps:
Step 1: sludge pretreatment
Sludge is the excess sludge of the moisture content 80% obtained after plate and frame filter press filters pressing, drying, grinding
Afterwards, 60 meshes are crossed, mud granule is obtained；
Step 2:
The kaolin that the present embodiment uses is clay mineral；In mass ratio, mud granule: kaolin=3:1, by sludge
Grain is mixed with kaolin, obtains mixture；
Into mixture, the FeCl that substance withdrawl syndrome is 40mmol/L is added3Solution is granulated after mixing evenly, preparation
Diameter is the haydite of 6mm；Wherein, by volume, mixture: FeCl3Solution=1:1.2；
Step 3: drying and calcining
The haydite of preparation is dried.It is placed in 110 DEG C of drying 5h of baking oven again, is immediately moved into initial temperature later and is set as 500
In DEG C Muffle furnace, in 550 DEG C of heat preservation 5min, continues temperature and rise to 1100 DEG C, and in 1100 DEG C of heat preservation 15min.In furnace certainly later
It is so cooled to room temperature, takes out, obtains Fe3+It is stand-by to load composite catalyst.The Fe of preparation3+Load Fe in composite catalyst3+It is flat
Equal load capacity is 6mmol/g.
Claims (10)
1. a kind of Fe3+Load the preparation method of composite catalyst, which comprises the following steps:
Step 1: sludge pretreatment
Sludge is dehydrated, dried, is ground up, sieved, the mud granule of >=60 mesh is obtained；
Step 2:
Mud granule is mixed with clay mineral, obtains mixture；Wherein, in mass ratio, mud granule: clay mineral=(3~
5): 1；
Into mixture, the FeCl that substance withdrawl syndrome is 20~40mmol/L is added3Solution, while EDTA-2Na is added, it stirs
Uniformly, it is granulated, obtains haydite；Wherein, by volume, mixture: FeCl3Solution=1:(1~1.5)；The addition of EDTA-2Na
The mass percent that amount accounts for mud granule is 0~0.5%；
Step 3: drying and calcining
By haydite, naturally dry, the haydite dried；After the haydite dried is placed in 100~110 DEG C of dryings completely, then stand
It is placed in 450~600 DEG C, keeps the temperature 3~6min, be continuously heating to 900~1100 DEG C, keep the temperature 10~20min, cool to the furnace
Room temperature is taken out, obtains Fe3+Load composite catalyst.
2. Fe according to claim 13+Load the preparation method of composite catalyst, which is characterized in that the step 1
In, the dehydration is that physics is dehydrated or one of filters pressing, suction filtration, filtering, centrifugation or several are selected in chemical dehydration, physics dehydration
Kind.
3. Fe according to claim 13+Load the preparation method of composite catalyst, which is characterized in that the step 2
In, the average diameter of the haydite is 4~6mm.
4. a kind of Fe3+Load composite catalyst, which is characterized in that be made using preparation method described in claim 1.
5. a kind of Fe3+Load composite catalyst, which is characterized in that the Fe3+Load composite catalyst carrier be mud granule with
Clay mineral, wherein in mass ratio, mud granule: clay mineral=(3~5): 1；Fe3+Load Fe in composite catalyst3+'s
Average load amount is 5~10mmol/g.
6. a kind of Fe3+Fenton-type reagent, which is characterized in that including Fe described in claim 4 or 53+Load composite catalyzing
Agent and H2O2Reagent, in molar ratio, Fe3+Load Fe in composite catalyst3+: H2O2H in reagent2O2=1:(2~3).
7. one kind is based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, which is characterized in that use claim 6
The Fe3+Fenton-type reagent, by sludge carry out class Fenton oxidation process, realize the reinforcing dehydration pre-process of sludge.
8. according to claim 7 be based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, feature exists
In described based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, specifically includes the following steps:
Into sludge conditioning pond by sludge condensation treated sludge to be processed, Fe is added3+Load composite catalyst and H2O2
Reagent is stirred, the sludge after obtaining dehydration pre-process；Wherein, Fe3+Load composite catalyst accounts for the object of sludge to be processed
The amount concentration of matter is 30~50mmol/L, H2O2The substance withdrawl syndrome that reagent accounts for sludge to be processed is 60~150mmol/L；
The stirring pretreatment, speed of agitator are 30~50r/min, and pretreatment time is 60~90min.
9. according to claim 8 be based on Fe3+Fenton-type reagent the pretreated method of sludge dewatering, feature exists
In sludge after the dehydration pre-process of preparation is used for Fe of the present invention3+Load the sludge raw material of composite catalyst.
10. Fe described in claim 4 or 53+Load the recoverying and utilizing method of composite catalyst, which is characterized in that including following
Process: in the sludge after dehydration pre-process, using filter type by Fe3+Dirt after loading composite catalyst and dehydration pre-process
Mud separation, by the Fe after separation3+After loading composite catalyst cleaning, drying, reused.
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| CN112125386A (en) * | 2020-09-02 | 2020-12-25 | 浙江万里学院 | Has the function of removing NH4+-N and CODMnPreparation method of double-function Fenton-like composite material |
| CN114984964A (en) * | 2021-03-01 | 2022-09-02 | 中国石油化工股份有限公司 | Preparation method for preparing ozone oxidation catalyst by using dried drilling mud |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112125386A (en) * | 2020-09-02 | 2020-12-25 | 浙江万里学院 | Has the function of removing NH4+-N and CODMnPreparation method of double-function Fenton-like composite material |
| CN114984964A (en) * | 2021-03-01 | 2022-09-02 | 中国石油化工股份有限公司 | Preparation method for preparing ozone oxidation catalyst by using dried drilling mud |
| CN114984964B (en) * | 2021-03-01 | 2023-07-04 | 中国石油化工股份有限公司 | Preparation method for preparing ozone oxidation catalyst by using dried drilling mud |
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