CN110314687B - Fe 3+ Load composite catalyst and preparation method thereof and Fenton-like sludge dehydration pretreatment method - Google Patents
Fe 3+ Load composite catalyst and preparation method thereof and Fenton-like sludge dehydration pretreatment method Download PDFInfo
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- CN110314687B CN110314687B CN201910689794.XA CN201910689794A CN110314687B CN 110314687 B CN110314687 B CN 110314687B CN 201910689794 A CN201910689794 A CN 201910689794A CN 110314687 B CN110314687 B CN 110314687B
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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
Abstract
Fe 3+ A supported composite catalyst, a preparation method thereof and a Fenton-like sludge dewatering pretreatment method belong to the field of urban solid waste disposal and resource utilization. The Fe 3+ The carrier of the loaded composite catalyst is sludge particles and clay minerals, wherein the mass ratio of the sludge particles: clay mineral = (3 to 5): 1; fe 3+ Fe in supported composite catalyst 3+ The average loading amount of (B) is 5 to 10mmol/g. The preparation method comprises the following steps: mixing the carriers, adding FeCl 3 The solution is prepared by granulation, drying and calcination. Adding the Fe 3+ In a supported composite catalyst, with Fe 3+ Substituted for Fe 2+ And H 2 O 2 The Fenton-like reaction is carried out under the condition of the pH value of the original sludge, so that the sludge is subjected to efficient and economic sludge enhanced dehydration pretreatment. Fe 3+ The supported composite catalyst can be recycled. The method can achieve the purpose of rapid and efficient dehydration of the sludge, reduce the subsequent treatment cost of the sludge, realize the treatment of waste by waste, and has economical efficiency and effectiveness.
Description
Technical Field
The invention belongs to the technical field of town solid waste disposal and resource utilization, and particularly relates to Fe 3+ A loaded composite catalyst, a preparation method thereof and a Fenton-like sludge dehydration pretreatment method.
Background
China pays more and more attention to sewage treatment, the sewage treatment reaches a quite high level, and the sludge treatment level needs to be improved. At present, most municipal sewage treatment plants adopt a biochemical process to treat sewage, a large amount of biochemical sludge is inevitably generated in the process, the sludge usually has complex components, great variability and high water content (usually more than or equal to 99 percent), the water content of the sludge after concentration treatment is still more than 90 percent, the sludge has large volume, the transportation, the storage and the use are inconvenient, and rings are possibly formedSecondary environmental pollution. Therefore, sludge dewatering becomes an important link in the sludge treatment and disposal process. In order to improve the filtration and dehydration performance of the sludge, the sludge needs to be conditioned. The conventional sludge conditioning techniques are mainly classified into physical methods (freeze thawing, mechanical energy, heating, microwave, high-pressure treatment, etc.), chemical methods (acid-base, flocculant addition, fenton treatment, etc.), and biological methods (aerobic and anaerobic digestion treatment of sludge). The methods are applied in practice, but the chemical method has the advantages of simple operation, low operation cost, stable conditioning effect and the like, and is the most widely used method at present. In the chemical method, fenton treatment has the advantages of convenience, rapidness, easy operation and the like and is widely applied in the industrial process. However, the traditional Fenton reaction needs a strong acid environment, the pH application range is narrow, and Fe 2+ The addition of (a) easily produces iron mud and cannot be recycled, thus limiting the application of the traditional fenton reaction to a certain extent.
Disclosure of Invention
The invention aims to provide Fe 3+ A supported composite catalyst and its preparing process and Fenton-like sludge dewatering pretreatment method based on advanced oxidation are disclosed, which includes such steps as preparing supported catalyst from residual sludge as supporting material and clay minerals, and using Fe as carrier 3+ Substitution of Fe 2+ And H 2 O 2 The Fenton-like reaction is carried out under the condition of the pH value of the original sludge, so that the sludge is subjected to efficient and economic sludge enhanced dehydration pretreatment. The invention can realize the purpose of quick and efficient dehydration of the sludge, reduce the subsequent treatment cost of the sludge, and simultaneously the preparation of the catalyst reflects the idea of treating waste by waste.
In order to achieve the purpose, the invention adopts the following technical scheme:
fe of the invention 3+ The preparation method of the supported composite catalyst comprises the following steps:
step 1: sludge pretreatment
Dehydrating, drying, grinding and sieving the sludge to obtain sludge particles with the particle size of more than or equal to 60 meshes;
step 2:
mixing the sludge particles with clay minerals to obtain a mixture; wherein, according to the mass ratio, the sludge particles: clay mineral = (3 to 5): 1;
FeCl with the mass concentration of 20-40 mmol/L is added into the mixture 3 Adding EDTA-2Na into the solution, uniformly stirring, and granulating to obtain ceramsite; wherein, according to the volume ratio, the mixture: feCl 3 Solution =1: (1-1.5); the addition amount of EDTA-2Na accounts for 0 to 0.5 percent of the mass percentage of the sludge particles;
and step 3: dry calcination of
Naturally drying the ceramsite to obtain dried ceramsite; drying the dried ceramsite at 100-110 ℃, immediately placing the dried ceramsite at 450-600 ℃, preserving heat for 3-6 min, continuously heating to 900-1100 ℃, preserving heat for 10-20 min, cooling to room temperature along with the furnace, and taking out the ceramsite to obtain Fe 3+ And (3) loading the composite catalyst.
In the step 1, the dehydration is physical dehydration or chemical dehydration, and the physical dehydration is one or more of filter pressing, suction filtration, filtration and centrifugation.
In the step 2, the average diameter of the ceramsite is 4-6 mm.
In the step 3, the drying is complete, and preferably for 4 to 6 hours.
Said Fe 3+ In the preparation method of the supported composite catalyst, the EDTA-2Na is added for the purpose of preventing Fe 3+ Precipitation occurs.
Fe 3+ The supported composite catalyst is prepared by the preparation method.
Fe 3+ The carrier of the supported composite catalyst is sludge particles and clay minerals, wherein the mass ratio of the sludge particles: clay mineral = (3-5): 1; fe 3+ Fe in supported composite catalyst 3+ The average loading amount of (B) is 5 to 10mmol/g.
Fe 3+ Including Fe 3+ Supported composite catalyst and H 2 O 2 Reagent, in molar ratio, fe 3+ Fe in supported composite catalyst 3+ ：H 2 O 2 In the reagent H 2 O 2 ＝1：(2～3)；
Said H 2 O 2 The reagent is preferably H with the mass percentage of 30% 2 O 2 An aqueous solution.
Based on Fe 3+ The method for sludge dewatering pretreatment of Fenton-like reagent, which adopts the Fe 3+ The Fenton-like reagent realizes the intensified dehydration pretreatment of the sludge through the Fenton-like oxidation process of the sludge.
The Fe base 3+ The method for sludge dewatering pretreatment of Fenton reagent comprises the following steps:
adding Fe into the sludge to be treated after the sludge concentration treatment in the sludge regulating tank 3+ Supported composite catalyst and H 2 O 2 Stirring the reagent to obtain sludge subjected to dehydration pretreatment; wherein, fe 3+ The quantity concentration of the load composite catalyst in the sludge to be treated is 30-50 mmol/L, H 2 O 2 The reagent accounts for 60 to 150mmol/L of the substance of the sludge to be treated; the stirring pretreatment is carried out, the stirring rotating speed is 30-50 r/min, and the pretreatment time is 60-90 min;
the sludge to be treated comes from residual sludge in a sludge concentration tank, and the water content is more than or equal to 90 percent.
The sludge after dehydration pretreatment prepared by the method can be used for the Fe-based catalyst of the invention 3+ A sludge raw material loaded with the composite catalyst.
One kind of Fe of the present invention 3+ A supported composite catalyst of Fe capable of being recycled 3+ And (3) loading the composite catalyst.
Fe 3+ The recycling method of the load composite catalyst comprises the following steps: in sludge after dehydration pretreatment, fe is filtered by adopting a filtering mode 3+ Separating the load composite catalyst from the sludge after dehydration pretreatment, and separating the separated Fe 3+ The loaded composite catalyst is washed and dried for repeated use.
One kind of Fe of the present invention 3+ The loaded composite catalyst, the preparation method thereof and the sludge dewatering pretreatment method have the following principles: the sludge is dehydrated by utilizing a high-grade oxidation method, and the generated strong oxidant intermediate hydroxyl free radical (. OH) is utilized to destroy the sludge structure, release more bound water in the sludge and strengthen the sludge dehydration effect.
Fe of the invention 3+ The loaded composite catalyst, the preparation method thereof and the sludge dewatering pretreatment method have the advantages and beneficial effects that:
1. the invention adopts a high-grade oxidation method to strengthen the sludge dehydration and uses Fe 3+ Replacing Fe in traditional Fenton reaction 2 + ，Fe 3+ Supported composite catalyst and H 2 O 2 The Fenton-like reaction is formed, the dehydration can be enhanced under the original pH condition of the sewage, the defect that the traditional Fenton reaction needs to be carried out under the strong acid condition is overcome, and the enhanced dehydration of the sludge is realized.
2. The invention takes sludge as Fe 3+ Preparation of Fe from support material of loaded composite catalyst 3+ The supported composite catalyst embodies the concept of 'treating waste by waste'.
3. Fe of the invention 3+ The supported composite catalyst can be recycled, and is an economic and effective sludge enhanced dehydration pretreatment method.
4. Fe prepared by the invention 3+ The supported composite catalyst is prepared by using residual sludge as a supporting material and matching with clay minerals to prepare Fe 3+ The supported composite catalyst is added with EDTA-2Na in the preparation process to prevent Fe 3+ Precipitation occurs.
Detailed Description
The present invention will be described in further detail with reference to examples.
In the present invention, unless otherwise specified, the solution is an aqueous solution thereof. The concentration is mass concentration.
In the following examples, the dehydration pretreatment reaction apparatus used was: the reaction apparatus of this example was a cylindrical PVC tank (diameter: 10 cm) of 1L volume, and sludge and Fe to be treated were stirred by an electric stirrer 3+ The Fenton-like reagent (2) is mixed and stirred.
In the following examples, test sludges were used: the sludge comes from a concentration tank of a certain sewage treatment plant in Fushun city, and the basic parameters are shown in table 1:
based on Fe 3+ The method for dewatering and pretreating Fenton reagent-like sludge comprises the following steps:
1) The residual sludge is used as a supporting material and is matched with Fe of clay minerals 3+ Loading composite catalyst, adding EDTA-2Na to prevent Fe 3+ Precipitation occurs;
2)Fe 3+ replacing Fe in traditional Fenton reaction 2+ ，Fe 3+ Supported composite catalyst and H 2 O 2 The Fenton-like reaction is formed, and the dehydration can be enhanced under the original pH condition of the sludge;
3) The composite catalyst can be recycled.
Example 1
(1) Fe 3+ The preparation method of the supported composite catalyst comprises the following steps:
step 1: sludge pretreatment
The sludge is residual sludge with the water content of 80 percent obtained by filter pressing of a plate-and-frame filter press, and is dried, ground and sieved by a 60-mesh sieve to obtain sludge particles;
and 2, step:
the kaolin adopted in the embodiment is clay mineral; according to the mass ratio, the sludge particles are: kaolin =5:1, mixing sludge particles with kaolin to obtain a mixture;
FeCl is added to the mixture in a concentration of 30mmol/L of the substance 3 Simultaneously adding EDTA-2Na which accounts for 0.5 percent of the mass of the sludge particles into the solution, uniformly stirring, and granulating to prepare ceramsite with the diameter of 5 mm; wherein, according to the volume ratio, the mixture: feCl 3 Solution = 1.5;
and step 3: dry calcination
And drying the prepared ceramsite. Then drying the mixture in an oven at 100 ℃ for 5 hoursImmediately moving to a muffle furnace with the initial temperature set to 500 ℃, preserving the heat at 500 ℃ for 5min, continuing to increase the temperature to 1000 ℃, and preserving the heat at 1000 ℃ for 15min. Then naturally cooling the furnace to room temperature, taking out the furnace to obtain Fe 3+ And loading the composite catalyst for later use. Preparation of Fe 3+ Fe in supported composite catalyst 3+ The average loading of (2) was 6mmol/g.
(2) Fe 3+ Including Fe prepared in this example 3+ Supported composite catalyst and H 2 O 2 Reagent, in molar ratio, fe 3+ Fe in supported composite catalyst 3+ ：H 2 O 2 In the reagent H 2 O 2 ＝1：3；
(3) Based on Fe 3+ The method for sludge dewatering pretreatment of Fenton-like reagent specifically comprises the following steps:
adding Fe to the sludge to be tested 3+ The loading composite catalyst has the following addition amount: in terms of the wet sludge volume of the test sludge, in which Fe was added 3+ Fe in supported composite catalyst 3+ The amount concentration of the substance(s) of (1) is 30mmol/L, H 2 O 2 (30%) the amount of the substances accounting for the volume of the wet sludge is 90mmol/L, and the sludge is pretreated for 90min at 40r/min under the condition of the original pH (about 6.9) of the sludge, so that the sludge after the dehydration pretreatment is obtained.
(4) The treatment effect is as follows: in the sludge after the dehydration pretreatment, the water content of a sludge cake can be reduced to 60 percent, CST is reduced to 1696s, SRF and MLSS are respectively reduced by 50 percent, and the sludge dehydration property is obviously enhanced.
(5) Fe 3+ The recycling method of the load composite catalyst comprises the following steps: in sludge after dehydration pretreatment, fe is filtered 3+ Separating the load composite catalyst from the sludge after dehydration pretreatment, and separating the separated Fe 3+ And (4) cleaning and drying the loaded composite catalyst, and then recycling. Removal of Fe 3+ And (4) recycling the sludge loaded with the composite catalyst.
Example 2
(1) Fe 3+ The preparation method of the supported composite catalyst comprises the following steps:
step 1: sludge pretreatment
Sludge removal of Fe in example 1 3+ Dewatering pretreated sludge loaded with composite catalyst, the sludge being Fe-treated 3+ Supported composite catalyst and H 2 O 2 After pretreatment of the formed Fenton-like reagent, fe is removed 3+ The composite catalyst is loaded, and the water content of the mud cake is 62.7% after suction filtration and dehydration. Drying and grinding the sludge, and then sieving the sludge with a 60-mesh sieve to obtain sludge particles;
step 2:
the attapulgite adopted in the embodiment is a viscosity mineral; according to the mass ratio, the sludge particles are: attapulgite =5:1, mixing sludge particles with attapulgite to obtain a mixture;
FeCl is added to the mixture in a concentration of 40mmol/L of the substance 3 Simultaneously adding EDTA-2Na accounting for 0.5 percent of the mass of the sludge particles into the solution, uniformly stirring, and granulating to prepare the ceramsite with the average diameter of 5 mm. Wherein, according to the volume ratio, the mixture: feCl 3 Solution =1:1;
and step 3: dry calcination
And naturally drying the prepared ceramsite. And then placing the mixture in an oven for drying at 110 ℃ for 5h until the drying is complete, and immediately moving the mixture to a muffle furnace with the initial temperature set to 500 ℃ and keeping the temperature at 500 ℃ for 5min, raising the temperature to 1000 ℃ and keeping the temperature at 1000 ℃ for 15min. Then naturally cooling the furnace to room temperature, taking out the furnace to obtain Fe 3+ And loading the composite catalyst for later use. Prepared Fe 3+ Fe in supported composite catalyst 3+ The average loading of (2) was 8mmol/g.
(2) Fe 3+ Including Fe prepared in this example 3+ Supported composite catalyst and H 2 O 2 Reagent, in molar ratio, fe 3+ Fe in supported composite catalyst 3+ ：H 2 O 2 In the reagent H 2 O 2 ＝1：3；
(3) Based on Fe 3+ The method for sludge dewatering pretreatment of Fenton-like reagent specifically comprises the following steps:
adding a loading agent into the test sludgeCatalyst is added in an amount of 5g/L (wherein, fe 3+ Fe in supported composite catalyst 3+ The amount concentration of the substance(s) of (3) is 40 mmol/L), H 2 O 2 (30%) the amount of the substances accounting for the volume of the wet sludge is 120mmol/L, and the sludge is pretreated for 90min at 40r/min under the condition of the original pH (about 6.9) of the sludge, so that the sludge after the dehydration pretreatment is obtained.
(4) The treatment effect is as follows: the water content of the sludge cake of the sludge subjected to dehydration pretreatment is reduced to below 60 percent, and the dehydration performance of the sludge is improved.
Example 3
Fe recovered in example 1 3+ Recycling of the supported composite catalyst, its and H 2 O 2 Fe formed by reagent 3+ The method for sludge dewatering pretreatment of Fenton-like reagent specifically comprises the following steps:
(1) Fe used in example 1 3+ The supported composite catalyst is separated from the sludge after the dehydration pretreatment by filtration, washed by deionized water and dried, and then sent to the next group of sludge dehydration pretreatment experiments (the experimental conditions are the same as those in example 1);
(2) Adding recycled Fe into the tested sludge 3+ Supported composite catalyst in which H 2 O 2 (30%) the amount concentration of the substances accounting for the volume of the wet sludge is still 90mmol/L, and the sludge is pretreated for 90min at 40r/min under the condition of the original pH (about 6.9) of the sludge, so that the sludge after the dehydration pretreatment is obtained.
(3) The treatment effect is as follows: in the sludge after dehydration pretreatment, the water content of sludge cakes can be reduced to 64.8 percent, the dehydration rate is slightly reduced, the sludge dehydration performance is still obviously enhanced, and Fe 3+ The supported composite catalyst has good recycling performance.
Example 4
Fe 3+ The preparation method of the supported composite catalyst comprises the following steps:
step 1: sludge pretreatment
The sludge is residual sludge with the water content of 80 percent obtained by filter pressing of a plate-and-frame filter press, and is dried, ground and sieved by a 60-mesh sieve to obtain sludge particles;
step 2:
the kaolin adopted in the embodiment is clay mineral; according to the mass ratio, sludge particles: kaolin =3:1, mixing sludge particles with kaolin to obtain a mixture;
FeCl was added to the mixture in an amount of 40mmol/L 3 Uniformly stirring the solution, and granulating to prepare ceramsite with the diameter of 6 mm; wherein, according to the volume ratio, the mixture: feCl 3 Solution = 1.2;
and step 3: dry calcination
And drying the prepared ceramsite. And then placing in an oven for drying at 110 ℃ for 5h, immediately moving to a muffle furnace with the initial temperature set to 500 ℃, preserving heat at 550 ℃ for 5min, continuing to heat to 1100 ℃, and preserving heat at 1100 ℃ for 15min. Then naturally cooling the furnace to room temperature, taking out the furnace to obtain Fe 3+ And loading the composite catalyst for later use. Prepared Fe 3+ Fe in supported composite catalyst 3+ The average loading of (2) was 6mmol/g.
Claims (5)
1. Based on Fe 3+ The method for sludge dewatering pretreatment of Fenton-like reagent is characterized by comprising the following steps:
adding Fe into the sludge to be treated after the sludge concentration treatment in the sludge regulating tank 3+ Supported composite catalyst and H 2 O 2 Stirring the reagent to obtain sludge subjected to dehydration pretreatment;
in terms of mole ratio, fe 3+ Fe in supported composite catalyst 3+ ：H 2 O 2 In the reagent H 2 O 2 =1：(2~3)；
Wherein, fe 3+ The weight concentration of the load composite catalyst in the sludge to be treated is 30 to 50mmol/L, H 2 O 2 The concentration of the reagent in the matter of the sludge to be treated is 60 to 150mmol/L; stirring and pretreating, wherein the stirring rotation speed is 30 to 50r/min, and the pretreatment time is 60 to 90min;
said Fe 3+ The carrier of the loaded composite catalyst is sludge particles and clay minerals, wherein the mass ratio of the sludge particles:clay mineral = (3~5): 1; fe 3+ Fe in supported composite catalyst 3+ The average load of the catalyst is 5 to 10 mmol/g;
said Fe 3+ The supported composite catalyst is prepared by the following steps:
step 1: sludge pretreatment
Dehydrating, drying, grinding and sieving the sludge to obtain sludge particles with the particle size of more than or equal to 60 meshes;
step 2:
mixing the sludge particles with clay minerals to obtain a mixture; wherein, according to the mass ratio, the sludge particles: clay mineral = (3~5): 1;
FeCl with the concentration of the substance being 20 to 40mmol/L is added to the mixture 3 Adding EDTA-2Na into the solution, uniformly stirring, and granulating to obtain ceramsite; wherein, according to the volume ratio, the mixture: feCl 3 Solution =1: (1 to 1.5); the addition amount of EDTA-2Na accounts for 0 to 0.5 percent of the mass of the sludge granules, and the mass percent of the EDTA-2Na is not equal to 0;
and step 3: dry calcination of
Naturally drying the ceramsite to obtain dried ceramsite; drying the dried ceramsite completely at 100-110 ℃, then immediately placing the ceramsite in a temperature range of 450-600 ℃, preserving heat for 3-6 min, continuously heating to 900-1100 ℃, preserving heat for 10-20min, furnace-cooling to room temperature, and taking out the ceramsite to obtain Fe 3+ And (3) loading the composite catalyst.
2. Fe-based according to claim 1 3+ The method for dewatering and pretreating Fenton-like reagent sludge is characterized in that in the step 1, the dewatering is physical dewatering or chemical dewatering, and the physical dewatering is one or more of filter pressing, suction filtration, filtration and centrifugation.
3. Fe-based alloy according to claim 1 3+ The method for dewatering and pretreating Fenton reagent-like sludge is characterized in that in the step 2, the average diameter of the ceramsite is 4-6 mm.
4. The base of claim 1In Fe 3+ Characterized in that the prepared sludge after dehydration pretreatment is used for preparing Fe 3+ A sludge raw material loaded with the composite catalyst.
5. Fe-based according to claim 1 3+ The method for sludge dehydration pretreatment of Fenton-like reagent is characterized in that Fe is pretreated 3+ The supported composite catalyst is recovered, and the method comprises the following steps: in sludge after dehydration pretreatment, fe is filtered by adopting a filtering mode 3+ Separating the load composite catalyst from the sludge after dehydration pretreatment, and separating the separated Fe 3+ And (4) cleaning and drying the loaded composite catalyst, and then recycling.
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| 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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| CN105417928A (en) * | 2015-12-28 | 2016-03-23 | 南京神克隆科技有限公司 | Method for municipal sludge in-situ detwatering by utilization of Fenton sludge |
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| CN105417928A (en) * | 2015-12-28 | 2016-03-23 | 南京神克隆科技有限公司 | Method for municipal sludge in-situ detwatering by utilization of Fenton sludge |
| CN105688917A (en) * | 2016-02-24 | 2016-06-22 | 湖南永清环保研究院有限责任公司 | Porous ceramsite Fenton catalyst and preparation method thereof |
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