CN114835356A - Preparation method of sludge-based iron-carbon micro-electrolysis biological filler - Google Patents
Preparation method of sludge-based iron-carbon micro-electrolysis biological filler Download PDFInfo
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a preparation method of a sludge-based iron-carbon micro-electrolysis biological filler, which has the advantages of low heavy metal content, high product quality and stable quality. The method comprises the following steps: s1, treating municipal sludge by electroosmosis: carrying out electroosmosis deep dehydration on municipal sludge, and crushing by using a sludge crusher; s2, crushing sludge biological tempering: uniformly mixing the crushed sludge and a biological modulator to obtain a sludge-based raw material with a required content ratio of organic matters to ash; s3, chemically activating the sludge-based raw material: spraying an activating agent on a sludge-based raw material, then carrying out chemical activation, cleaning, drying and grinding to obtain sludge charcoal powder; s4, granulating the biological filler: uniformly mixing the sludge charcoal powder with iron powder and attapulgite clay powder, adding water, ball-milling to prepare water-containing raw material pellets, and drying to obtain dry raw material pellets; s5, calcining and solidifying the biological filler: calcining the dried raw material pellets to be solid to obtain the sludge-based iron-carbon micro-electrolysis biological filler.
Description
Technical Field
The invention belongs to the technical field of sewage treatment and sludge recycling treatment, and particularly relates to a preparation method of a sludge-based iron-carbon micro-electrolysis biological filler.
Background
The biological filler has the advantages of large specific surface area, light weight, high strength, corrosion resistance and the like, and is widely applied to the sewage treatment process.
In order to reduce the secondary pollution of municipal sludge to the environment and improve the resource utilization efficiency of organic wastes, the industry starts to try to prepare water treatment biological fillers by using sludge.
At present, a method for preparing a biological filler by using sludge is described in a paper ' preparation of sludge-based biological filler and research on urban runoff pollution control ' (Huang Yi, Master thesis of Ningbo university, academic grant date, 2017-01-01) ', and the process is that sludge, fly ash and river sludge are used as main raw materials, and goldenrod and calcium carbonate are added as auxiliary materials to fire the biological filler, so that an optimal filler formula and roasting process conditions are determined. The result shows that the optimal formula of the sludge-based biological filler is that the sludge, the fly ash and the river sludge are 3: 5: 4.5, and 9 percent of goldenrod and 5 percent of calcium carbonate are doped; the optimal process is that the sintering temperature is 950 ℃, the sintering time is 10min, the preheating temperature is 500 ℃, and the heating speed is 7 ℃/min; under the condition, the water absorption of the filler is 65% apparent density 630kg/m 3 Cylinder pressure 0.42MPa, specific surface 0.2m 2 (ii) in terms of/g. As seen by SEM, the sludge-based biological filler has a rough surface, has rich pore structures and is mostly provided with open pores; from XRD analysis, it is known that the filler is mainly composed of ionic crystals, and the most predominant crystal structures are an oxide structure and a silicate structure. The paper also performs heavy metal adsorption studies on sludge-based biological fillers. Researches on the adsorption of heavy metal Pb in water by the sludge-based biological filler 2+ 、Cd 2+ 、Ni 2+ 、Cr 3+ And with Cr 3+ For example, the adsorption mechanism of heavy metals was studied. The result shows that the addition of calcium carbonate in the raw materials is beneficial to improving the Cr content of the sludge-based biological filler 3+ 、Pb 2+ The adsorption capacity of (c); the competitive power of the four heavy metals is Cr 3+ >Pb 2+ >Ni 2+ >Cd 2+ (ii) a Sludge-based biological filler pair Cr 3+ The maximum adsorption amount of (a) is 4.32 mg/g; the adsorption isotherms were in accordance with Langmuir and Freundlich models; the adsorption mechanism mainly comprises: the oxygen-containing functional group anion is combined with chromium ions to form insoluble compounds for sedimentation; chromium ions are hydrolyzed to generate chromium hydroxide precipitate which is then absorbed by the filler; the negative potential on the surface of the adsorbent is combined with positive-valence chromium ions to generate electrostatic adsorption; displacement reaction of chromium ions with cations.
However, since the domestic sewage and the industrial wastewater are mixed to be treated, the sludge of a sewage plant contains a large amount of heavy metals, and the problem is not considered when the sludge is prepared into the biological filler in the prior art, so that the prepared sludge biological filler has the risk of secondary pollution caused by heavy metal precipitation;
secondly, the quality of the biological filler prepared by the existing sludge is poor mainly due to two reasons: firstly, due to the difference of sewage sources and sewage sludge treatment processes, the property difference of sludge is large; secondly, the organic matter content of the sludge is low (less than 50 percent), and the proportion of the organic matter and the ash content is unbalanced.
In summary, the prior art has the following problems: the sludge-based iron-carbon micro-electrolysis biological filler prepared by the existing method has high heavy metal content and low product quality, and the biological filler prepared by sludge with different properties has large production batch difference.
Disclosure of Invention
The invention aims to provide a preparation method of a sludge-based iron-carbon micro-electrolysis biological filler, which has the advantages of low heavy metal content, high product quality and stable quality.
The technical solution for realizing the purpose of the invention is as follows:
a preparation method of a sludge-based iron-carbon micro-electrolysis biological filler comprises the following steps:
s1, treating municipal sludge by electroosmosis: carrying out electroosmosis deep dehydration on municipal sludge with the water content of 75-85%, and crushing by using a sludge crusher;
s2, crushing sludge biological tempering: uniformly mixing the crushed sludge and a biological modulator to obtain a sludge-based raw material with the required content ratio of organic matters to ash;
s3, chemically activating the sludge-based raw material: spraying an activating agent on the sludge-based raw material, then carrying out chemical activation, cleaning, drying and grinding to obtain sludge charcoal powder;
s4, granulating the biological filler: uniformly mixing the sludge charcoal powder, iron powder and attapulgite clay powder, adding clear water, preparing into water-containing raw material pellets by a ball mill, and drying the water-containing raw material pellets in an air atmosphere at 105 ℃ to obtain dried raw material pellets;
s5, calcining and solidifying the biological filler: and transferring the dried raw material pellets to a fixed bed tubular furnace for calcining and solidifying to obtain the sludge-based iron-carbon micro-electrolysis biological filler.
Preferably, in the step of chemically activating the sludge-based raw material, the chemical activation process of S3 includes:
placing the sludge-based raw material sprayed with the activating agent in drying equipment for low-temperature drying;
and transferring the sludge-based raw material after low-temperature drying to a rotary tube furnace for direct pyrolysis.
Further preferably, the drying apparatus is one of a flash dryer, a drum dryer, a belt dryer, a film dryer or a disc dryer;
the low-temperature drying temperature is controlled to be 120-150 ℃;
the direct pyrolysis temperature is controlled at 500-600 ℃, and 6-12% of oxygen-containing nitrogen is introduced in the direct pyrolysis process.
Preferably, the chemically activated sludge-based raw material is washed with 10% hydrochloric acid and tap water until the pH is neutral, and then dried and ground to obtain sludge charcoal powder.
Preferably, the activating agent is a zinc chloride solution, the concentration is 3-4 mol/L, and the solid-to-liquid ratio of the sludge-based raw material to the activating agent is 1: 2-1: 2.5.
preferably, in the municipal sludge electroosmosis treatment step, electroosmosis deep dehydration conditions are as follows:
the mechanical pressure is 80-100 kPa, the voltage gradient is 30-50V/cm, the sludge thickness is 0.5-1 cm, and the sludge water content after electroosmotic dehydration treatment is 50-60%.
Preferably, in S2, in the step of crushing sludge and biologically modifying, the content ratio a of organic matter to ash content of the sludge-based raw material is determined according to the following formula:
A＝0.00304B-4.66355C+2.95633D-0.51155E+2.33806，
in the formula, B is the specific surface area, C is the total pore volume, D is the micropore volume, and E is the micropore ratio.
According to the BET theory, the larger the specific surface area, the larger the amount of adsorption.
When the specific surface area is less than 600m 2 When per gram, the filler is common iron-carbon micro-electrolysis biological filler,
when 600m 2 Specific surface area is not more than 900m and is not more than g 2 When per gram, the product is good iron-carbon micro-electrolysis biological filler,
when the specific surface area is more than 900m 2 In terms of/g, the product is a superior iron-carbon micro-electrolysis biological filler.
The empirical formula of the content ratio A of the organic matters to the ash content of the sludge-based raw material is obtained by measuring the specific surface area, the total pore volume, the micropore volume and the micropore ratio of the biological filler prepared by mixing the organic matters with the ash content in the ratio A and then performing linear fitting on the measured result and the A. The filler produced subsequently can be substituted into an empirical formula according to the requirements of customers or actual production batches on the comparison surface area, the total pore volume, the micropore volume and the micropore ratio to obtain the sludge-based raw material organic matter and ash content ratio A.
For example, in order to produce a bio-filler having a specific surface area of 600, a total pore volume of 0.35, a pore volume of 0.15, and a pore ratio of 0.35, the above data is substituted into the formula to obtain a ═ 2.8965. According to the proportion, the product actually produced has the specific surface area of 606.44, the total pore volume of 0.37, the micropore volume of 0.14 and the micropore ratio of 0.38, and meets the production requirement.
Preferably, the biological modifying agent is one of straw powder, rice hull powder, peanut hull powder and edible fungus matrix powder.
Preferably, in the step of S4, in the step of granulating the biological filler, the mixing ratio of the sludge charcoal powder to the iron powder is 2: 1, the addition amount of the attapulgite clay powder is 20 percent of the total amount of the sludge charcoal powder and the iron powder, and the diameter of a water-containing raw material pellet prepared by a ball mill is controlled to be 0.5-1 cm.
Preferably, in S5, the step of calcining and solidifying the biological filler specifically includes:
and transferring the dried raw material pellets to a fixed bed tube furnace for calcining and solidifying, wherein the heating speed is 2-4 ℃/min, the temperature is maintained for 90-150 min after reaching the final temperature of 700 ℃, and pure nitrogen is filled in the cooling process to maintain an anaerobic environment.
Compared with the prior art, the invention has the following remarkable advantages:
1. the heavy metal content is low: according to the method, heavy metals in the raw sludge are enriched on the negative plate of the electroosmosis dehydration equipment and removed in the pretreatment stage, and heavy metal ions in the sludge biological filler are effectively reduced through sludge electroosmosis pretreatment, so that the problem that the heavy metals in the sludge biological filler are easy to separate out is fundamentally solved.
2. The product quality is stable: according to the invention, the accurate tempering of sludge with different properties is realized through the empirical formula of the organic matter content and the ash ratio of the sludge-based raw material, multiple tests are not needed, the product difference of different production batches is small, the product quality is stable, the test workload is small, and the problems of blindness and complex work of the tempering treatment of the sludge in the prior art are solved.
3. The product quality is high: according to the invention, the biological modulator with high organic matter content is used for supplementing, so that the organic matter content of the sludge-based raw material is increased, and the problem of unbalance of the ratio of organic matter to ash in the production process of the iron-carbon micro-electrolysis biological filler is effectively solved; meanwhile, by utilizing the characteristic of metal corrosion, an iron-carbon micro-electrolysis environment is constructed by the iron-carbon micro-electrolysis primary battery formed by a solution system, and the quality of the iron-carbon biological filler is further improved.
The invention is described in further detail below with reference to the figures and the detailed description.
Drawings
FIG. 1 is a main flow chart of the preparation method of the sludge-based iron-carbon micro-electrolysis biological filler.
Detailed Description
Example one
S1, treating municipal sludge by electroosmosis: and (3) performing electro-osmotic deep dehydration on the municipal sludge with the water content of 80.12%, wherein the electro-osmotic dehydration conditions are that the mechanical pressure is 80kPa, the voltage gradient is 30V/cm, the sludge thickness is 1cm, and the water content of the dehydrated sludge is 56.27%. The dewatered sludge having a water content of 56.27% was crushed by a sludge crusher. Table 1 shows the agricultural heavy metal concentration limit of sludge and the heavy metal content before and after electroosmotic dehydration.
TABLE 1 limit values of concentration of heavy metals in sludge for agricultural use and heavy metal content before and after electroosmotic dehydration
As can be seen from Table 1, the sludge-based iron-carbon micro-electrolysis biological filler prepared by the method of the invention further removes heavy metals in the electroosmosis dehydration pretreatment stage, and meets the A-grade standard of agricultural sludge.
S2, crushing sludge biological tempering: mixing and tempering the crushed sludge and the straw powder to prepare the high-quality iron-carbon micro-electrolysis biological filler with the specific surface area B of 1000, the total pore volume C of 0.60, the micropore volume D of 0.55 and the micropore ratio E of 0.9. According to empirical formula
A＝0.00304*B-4.66355*C+2.95633*D-0.51155*E+2.33806，
The content ratio A of organic matter to ash content of the sludge-based raw material was controlled to 3.75.
In the formula, B is the specific surface area, C is the total pore volume, D is the micropore volume, and E is the micropore ratio.
S3, chemically activating the sludge-based raw material: spraying zinc chloride solution with the concentration of 3mol/L on the sludge-based raw material for chemical activation, wherein the solid-liquid ratio of the sludge-based raw material to the activating agent is 1: 2.
placing the activated sludge-based raw material in a 120 ℃ disc type dryer for low-temperature drying for 30min, transferring the sludge-based raw material after low-temperature drying to a rotary tube furnace for direct pyrolysis for 60min, wherein the pyrolysis temperature is 500 ℃, and 8% oxygen-containing nitrogen is introduced in the pyrolysis process.
After pyrolysis and activation of the sludge-based raw material, washing the sludge-based raw material by using 10% hydrochloric acid and tap water until the pH value is neutral, drying and grinding the sludge-based raw material to prepare the sludge charcoal powder.
S4, granulating the biological filler: mixing sludge charcoal powder, iron powder and attapulgite clay powder according to the weight ratio of 2: 1: 0.6 proportion, adding clean water, preparing the raw material balls containing water by a ball mill when the mixed materials have better forming effect, drying the raw material balls in the air atmosphere of 105 ℃, removing the redundant water in the raw material balls, and obtaining the raw material balls with the diameter of 1 cm.
S5, calcining and solidifying the biological filler: transferring the dried raw material pellets to a fixed bed tubular furnace for calcining and solidifying, filling pure nitrogen into the fixed bed tubular furnace in the calcining process, raising the temperature to 700 ℃ at the heating rate of 2 ℃/min, maintaining for 90min to prepare the sludge-based iron-carbon micro-electrolysis biological filler, and filling pure nitrogen protective gas in the cooling process to maintain an oxygen-free environment.
And (3) carrying out adsorption performance determination, specific surface area characterization and pore size analysis on the prepared sludge-based iron-carbon micro-electrolysis biological filler according to a BET method. According to the BET equation:
specific surface area S BET The larger the adsorption n is;
wherein n is the adsorption amount, S BET Is a specific surface area, delta is N 2 The cross section area of the nitrogen molecules in hexagonal accumulation at the temperature of 77K is in a liquid state, p0 is saturated vapor pressure, p is adsorption pressure, and the application range of p/p0 is 0.05-0.35. The specific surface area characterization and pore size analysis results of the superior sludge-based iron-carbon micro-electrolysis biological filler are shown in table 2.
TABLE 2 high-quality sludge-based iron-carbon micro-electrolysis biological filler specific surface area characterization and pore size analysis results
As can be seen from Table 2, the error rate of the indexes of the actual specific surface area B, the total pore volume C, the micropore volume D, the micropore ratio E and the demand index of the sludge-based iron-carbon micro-electrolysis biological filler prepared by the method is less than 5%, the sludge with different properties can be accurately quenched and tempered, and the difference of production batches is small.
The test results of the adsorption performance of the superior sludge-based iron-carbon micro-electrolysis biological filler on the total phosphorus in the sewage plant are shown in table 3.
As can be seen from Table 3, the sludge-based iron-carbon micro-electrolysis biological filler S prepared by the method of the invention BET Compared with the traditional sludge biological filler, the total phosphorus removal efficiency is improved by 3.48-10.45 times, compared with the commercial biological filler, the total phosphorus removal efficiency is improved by 1.05-2.61 times, after the total phosphorus removal efficiency is added at the advanced treatment section of a sewage plant, the maximum total phosphorus removal efficiency reaches 68.75%, the effluent quality reaches the standard IV-class standard, the standard improvement and transformation requirements of the sewage plant are met, and the product quality is high.
Table 3 superior product sludge-based iron-carbon micro-electrolysis biological filler to sewage plant total phosphorus adsorption performance test table
Claims (10)
1. A preparation method of a sludge-based iron-carbon micro-electrolysis biological filler is characterized by comprising the following steps:
s1, treating municipal sludge by electroosmosis: carrying out electroosmosis deep dehydration on municipal sludge with the water content of 75-85%, and crushing by using a sludge crusher;
s2, crushing sludge biological tempering: uniformly mixing the crushed sludge and a biological modulator to obtain a sludge-based raw material with the required content ratio of organic matters to ash;
s3, chemically activating the sludge-based raw material: spraying an activating agent on the sludge-based raw material, then carrying out chemical activation, cleaning, drying and grinding to obtain sludge charcoal powder;
s4, granulating biological filler: uniformly mixing the sludge charcoal powder with iron powder and attapulgite clay powder, adding clear water, preparing into water-containing raw material pellets by a ball mill, and drying the water-containing raw material pellets in an air atmosphere at 105 ℃ to obtain dried raw material pellets;
s5, calcining and solidifying the biological filler: and transferring the dried raw material pellets to a fixed bed tubular furnace for calcining and solidifying to obtain the sludge-based iron-carbon micro-electrolysis biological filler.
2. The method for preparing the sludge-based iron-carbon micro-electrolysis biological filler according to claim 1, wherein in the step of chemically activating the sludge-based raw material, the chemical activation process comprises the following steps:
placing the sludge-based raw material sprayed with the activating agent in drying equipment for low-temperature drying;
and transferring the sludge-based raw material after low-temperature drying to a rotary tube furnace for direct pyrolysis.
3. The method for preparing the sludge-based iron-carbon micro-electrolysis biological filler according to claim 2, which is characterized in that:
the drying equipment is one of a flash evaporation type dryer, a rotary drum type dryer, a belt type dryer, a film dryer or a disc type dryer;
the low-temperature drying temperature is controlled to be 120-150 ℃;
the direct pyrolysis temperature is controlled at 500-600 ℃, and 6-12% of oxygen-containing nitrogen is introduced in the direct pyrolysis process.
4. The method for preparing a sludge-based iron-carbon micro-electrolysis biological filler according to one of claims 1 to 3, characterized in that:
and (3) cleaning the chemically activated sludge-based raw material by using 10% hydrochloric acid and tap water until the pH value is neutral, and then drying and grinding to obtain the sludge charcoal powder.
5. The method for preparing a sludge-based iron-carbon micro-electrolysis biological filler according to one of claims 1 to 3, characterized in that:
the activating agent is a zinc chloride solution, the concentration is 3-4 mol/L, and the solid-to-liquid ratio of the sludge-based raw material to the activating agent is 1: 2-1: 2.5.
6. the preparation method of the sludge-based iron-carbon micro-electrolysis biological filler according to claim 1, wherein in the municipal sludge electro-osmosis treatment step, electro-osmosis deep dehydration conditions are as follows:
the mechanical pressure is 80-100 kPa, the voltage gradient is 30-50V/cm, the sludge thickness is 0.5-1 cm, and the sludge water content after electroosmotic dehydration treatment is 50-60%.
7. The method for preparing the sludge-based iron-carbon micro-electrolysis biological filler according to claim 1, wherein in the step of crushing sludge and biologically modifying, the content ratio A of organic matters to ash content of the sludge-based raw material is determined according to the following formula:
A＝0.00304B-4.66355C+2.95633D-0.51155E+2.33806，
in the formula, B is the specific surface area, C is the total pore volume, D is the micropore volume, and E is the micropore ratio.
8. The method for preparing the sludge-based iron-carbon micro-electrolysis biological filler according to claim 7, which is characterized in that:
the biological modifying agent is one of straw powder, rice hull powder, peanut hull powder and edible fungus matrix powder.
9. The method for preparing the sludge-based iron-carbon micro-electrolysis biological filler according to claim 1, which is characterized in that:
in the step of granulating the biological filler, the mixing ratio of the sludge biological carbon powder to the iron powder is 2: 1, the addition amount of the attapulgite clay powder is 20 percent of the total amount of the sludge charcoal powder and the iron powder, and the diameter of a water-containing raw material pellet prepared by a ball mill is controlled to be 0.5-1 cm.
10. The preparation method of the sludge-based iron-carbon micro-electrolysis biological filler according to claim 1, wherein the step of calcining and solidifying the biological filler specifically comprises the following steps:
and transferring the dried raw material pellets to a fixed bed tube furnace for calcining and solidifying, wherein the heating speed is 2-4 ℃/min, the temperature is maintained for 90-150 min after reaching the final temperature of 700 ℃, and pure nitrogen is filled in the cooling process to maintain an anaerobic environment.
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| CN115572023A (en) * | 2022-11-10 | 2023-01-06 | 江苏省环保集团有限公司 | Prevent blockking up high load sewage treatment system |
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| CN109865499A (en) * | 2019-03-22 | 2019-06-11 | 温州大学 | A kind of modified bowl orange peel biological carbon materials and the preparation method and application thereof |
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| JPH09241014A (en) * | 1996-03-08 | 1997-09-16 | Agency Of Ind Science & Technol | Production of activated carbon |
| CN102530941A (en) * | 2011-12-16 | 2012-07-04 | 北京工业大学 | Sludge-based activated carbon and preparation method thereof |
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