CN110586031A - Preparation method of modified sludge carbon material - Google Patents
Preparation method of modified sludge carbon material Download PDFInfo
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Abstract
The invention discloses a preparation method of a modified sludge carbon material, and belongs to the field of sewage and sludge treatment. The method comprises the following steps: s1, taking a certain amount of activated sludge, adding a flocculating agent, and then physically dehydrating and drying to obtain a sludge dry mud cake; s2, crushing and grinding the sludge dry mud cake prepared in the step S1, and sieving the crushed and ground sludge dry mud cake with a 100-mesh sieve to obtain powdery dry sludge; s3, putting the powdery dry sludge obtained in the step S2 into a tube furnace, pyrolyzing at 800 ℃ for 30min under the anaerobic condition, cooling, taking out a sample, washing away surface ash by deionized water, and drying to obtain powdery sludge carbon; s4, adding the powdered peat obtained in the step S3 into an acid or alkali modifier, soaking for 12-24h, repeatedly washing with deionized water until the washing liquor is neutral, and drying to obtain the modified sludge carbon material. The method realizes the recycling of the solid waste of the sludge, and the prepared modified sludge carbon material has good adsorption effect on soluble organic matters in the sewage.
Description
Technical Field
The invention relates to the field of sewage and sludge treatment, in particular to a preparation method of a modified sludge carbon material, which creates favorable conditions for subsequent treatment and resource utilization of sludge.
Background
With the continuous improvement of the urbanization level of China, the construction of sewage treatment facilities develops at a high speed. In order to further reduce the discharge flux of trace organic pollutants in sewage, the advanced sewage treatment technologies reported at present mainly include membrane separation technology, advanced oxidation technology, electrochemical oxidation technology, adsorption technology and the like. The membrane technology is widely applied to the treatment of the reclaimed water, but the large-scale application of the membrane technology is severely restricted by the membrane pollution; the oxidation technology has the problems of toxic byproducts, high selectivity of the catalyst, difficult separation and recovery, high treatment cost and the like, so that the current practical application is not many; the activated carbon is a porous substance, is easy to automatically control, and has strong adaptability to the change of water quantity, water quality and water temperature, so that the activated carbon adsorption method is a sewage advanced treatment technology with wide application prospect.
The activated sludge method is a common sewage treatment technology of sewage treatment plants, wherein the activated sludge is liquid-solid colloid floccule consisting of different biological groups such as fungi, protozoa and the like, is rich in a large amount of protein, polysaccharide, cellulose, lignin and the like, and can form a porous material with developed pores and various functional groups in the pyrolysis process, so that the obtained sludge carbon material has unique adsorption performance on soluble organic matters in sewage. However, a large amount of flue gas and ash are generated in the pyrolysis process of the activated sludge, and the ash is not converted into gas along with high-temperature pyrolysis, but covers the surface of the sludge carbon material in the cooling process, so that carbon pores on the surface of the sludge carbon material are blocked, and the adsorption performance of the sludge carbon material is influenced; in addition, the sludge contains a plurality of mineral impurities containing silicon, aluminum and phosphorus, and the mineral impurities have extremely high melting points, cannot be melted along with the pyrolysis process, but are better exposed in the process of pyrolyzing the activated sludge into the carbon material, so that the adsorption performance of the sludge carbon material is influenced.
The technology for preparing carbon materials by pyrolyzing activated sludge is not mature at present, and a large part of reasons are that the performance of the carbon materials is different from that of the commercially available activated carbon, and the advantages of the carbon materials in terms of preparation cost are not great. Therefore, the improvement of the adsorption performance of the sludge carbon material becomes an important factor for popularization and use.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a modified sludge carbon material, compared with the traditional sludge carbon material, the modified sludge carbon material has better adsorption performance, improves the removal effect of soluble organic pollutants in sewage, realizes the purpose of sludge treatment and recycling, and provides a theoretical basis for future engineering practice and application.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of a modified sludge carbon material, which comprises the following steps:
s1, adding a flocculating agent into the obtained activated sludge of the sewage plant, dehydrating and conditioning the activated sludge, performing high-pressure dehydration treatment through centrifugation or plate-and-frame filter pressing, and then performing drying treatment through a blast drying box to obtain a sludge dry sludge cake;
s2, crushing and grinding the sludge dry mud cake obtained in the step S1 through a crusher, and sieving the sludge dry mud cake through a 100-mesh sieve to obtain powdery dry sludge;
s3, putting the powdery dry sludge obtained in the step S2 into a porcelain boat, filling the porcelain boat with the powdery dry sludge to prevent air from entering, and covering the porcelain boat with a porcelain cover plate; slowly placing the porcelain boat into a tube furnace, heating to 800 ℃ at a heating rate of 10 ℃/min under the nitrogen atmosphere, then staying for 30min for pyrolysis, cooling to room temperature after pyrolysis is finished, taking out a sample, washing surface ash by deionized water, and drying to obtain powdery peat;
s4, adding the powdered peat obtained in the step S3 into a modifier, wherein the modifier is one of hydrochloric acid, nitric acid or sodium hydroxide solution, soaking and shaking for 12-24h, removing supernatant, repeatedly washing with deionized water until washing liquor is neutral, and drying to obtain the sludge carbon material.
The preparation method of the invention firstly dehydrates the activated sludge of the sewage plant, pyrolyzes the activated sludge at high temperature under the anaerobic condition of 800 ℃, and then introduces different acid-base chemical reagents for immersion modification to prepare the modified sludge carbon material, which has good adsorption performance, can effectively remove the soluble organic pollutants in the sewage, and realizes the purposes of sludge disposal and resource utilization.
According to the invention, the sludge carbon material is modified by introducing an acid-base chemical reagent, so that ash content on the surface of the sludge carbon, which is difficult to clean by water, and mineral components, which are difficult to pyrolyze at high temperature in the pyrolysis process, can be cleaned, and the pore structure of the sludge carbon material is more completely exposed; in addition, functional groups are introduced into the sludge carbon material through modification, and the adsorption sites of the sludge carbon material are increased.
Further, in step S1, the flocculant is one or more of polyaluminium chloride (PAC), polyferric chloride (PFC), aluminium chloride, ferric chloride, aluminium sulfate, ferric sulfate, and Polyacrylamide (PAM).
Further, the concentration of the modifier of the hydrochloric acid, nitric acid or sodium hydroxide solution is 0.5-2 mol/L, and the mass ratio of the powdery sewage peat to the modifier is 1: 10.
the basic principle of the invention is as follows: the acid-base modifier has good corrosion action, so that ash and part of minerals covered on the surface in the sludge carbon can be dissolved, the surface of the sludge carbon is etched to be rougher, and the effects of increasing the specific surface area of the sludge carbon and enhancing the pore structure on the surface of the sludge carbon are achieved. In addition, the sludge carbon pyrolyzed at high temperature has the characteristic of high aromaticity, has good complexation and pi-electron adsorption with soluble organic matters in water, especially aromatic proteins, and introduces functional groups on the surface of the sludge carbon by an acid-base modifier, so that the surface adsorption sites of the sludge carbon are increased, and the adsorption performance of the sludge carbon is improved. The preparation method not only provides an idea for preparing the carbon from the sludge in the future, but also provides a good theoretical basis for utilizing the sludge resources.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) the invention provides a new idea for preparing the sludge carbon material, and the acid-base modifier is introduced to effectively remove ash and minerals on the surface of the sludge carbon and obviously increase the adsorption performance of the material;
(2) the preparation method has simple operation flow, easy control and adjustment, repeated use of the modified reagent and low cost;
(3) the invention synchronously realizes the recycling and harmless treatment of the sludge and provides a new direction for the future sludge treatment and recycling.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention.
FIG. 1 is a flow chart of a method for preparing a modified sludge carbon material according to an embodiment of the present invention;
FIG. 2a is an SEM image of unmodified powdered sludge according to example 1 of the present invention;
FIG. 2b is an SEM image of a modified sludge carbon material in example 1 of the present invention;
FIG. 3a is a graph showing the adsorption/desorption curves and pore sizes and pore volumes of unmodified powdered peat according to example 1 of the present invention;
FIG. 3b is a graph showing the adsorption/desorption curve and pore volume of the modified sludge carbon material in example 1 of the present invention;
FIG. 4a is an SEM image of unmodified powdered peat according to example 2 of the present invention;
FIG. 4b is an SEM image of a modified sludge carbon material in example 2 of the present invention;
FIG. 5a is a graph showing the adsorption/desorption curves and pore sizes and pore volumes of unmodified powdered peat according to example 2 of the present invention;
FIG. 5b is a graph showing the adsorption/desorption curve and pore volume of the modified sludge carbon material in example 2 of the present invention;
FIG. 6 is a three-dimensional fluorescence comparison graph of an original effluent water sample of a secondary sedimentation tank, an effluent water sample of a sludge carbon material modified by adding hydrochloric acid, and an effluent water sample of a sludge carbon material modified by adding sodium hydroxide in the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
Example 1: preparation of modified sludge carbon material
Referring to fig. 1, embodiment 1 of the present invention provides a method for preparing a modified sludge carbon material, including the following steps:
(1) adding a cationic Polyacrylamide (PAM) flocculant into the residual activated sludge of a certain municipal sewage treatment plant according to the mass ratio of 5 per mill of Total Suspended Solids (TSS) contained in the activated sludge, reacting for 30min to carry out dehydration conditioning, carrying out plate-and-frame filter pressing, carrying out high-pressure dehydration treatment, and then carrying out drying treatment through a 105 ℃ blast drying box to obtain a sludge dry sludge cake.
(2) Crushing, grinding and sieving the obtained sludge dry mud cake with a 100-mesh sieve to obtain powdery dry sludge, and storing the powdery dry sludge in a dryer; putting the powdery dry sludge into a porcelain boat, wherein the porcelain boat is filled with the powdery dry sludge to prevent air from entering, and the porcelain boat is covered by a porcelain cover plate; slowly placing the porcelain boat into a tube furnace, raising the temperature to 800 ℃ at a heating rate of 10 ℃/min in a nitrogen atmosphere, then staying for 30min for pyrolysis, cooling to room temperature after pyrolysis is finished (nitrogen circulation needs to be kept in the process), taking out a sample, washing off surface ash by deionized water, and drying for storage to obtain powdery peat;
(3) preparing 500ml of 1mol/L hydrochloric acid solution, adding 20g of powdered peat, oscillating at the constant temperature of 180r/min at the temperature of 20 ℃ for 12h, repeatedly washing with deionized water until the washing liquor is neutral, and drying to obtain the modified sludge carbon material.
The micro-morphologies of the powdery sludge carbon before modification and the modified sludge carbon material are represented by Scanning Electron Microscopy (SEM), which is shown in fig. 2a and 2 b; the powdery sludge carbon before modification and the modified sludge carbon material adopt N2The adsorption and desorption curves (BET) characterize the specific surface area, as shown in fig. 3a and 3b, respectively.
The micro-morphology and the pore structure distribution of the peat before and after modification are obviously changed: comparing fig. 2a and fig. 2b, it can be seen that the surface of the sludge carbon material modified by hydrochloric acid is rougher than that before modification, the etching trace is obvious, and the opening degree of the pores is higher. As can be seen from comparison between FIG. 3a and FIG. 3b, the adsorption performance of the sludge carbon material modified by hydrochloric acid is improved to a higher level than that before modification, and the pore structure is changed from a single 2nm micropore and a single 10nm mesopore into a micro-mesoporous structure with wide pore distribution, which indicates that the pores of the material are opened after the material is eluted and etched by hydrochloric acid, and the specific surface area is 117.11m2Lifting/g to 148.96m2This is also confirmed laterally.
Comparative experiment of adsorption effect
Under the same conditions, feeding unmodified sewage peat, modified sludge carbon materials and commercial coconut shell activated carbon into a secondary sedimentation tank of a sewage plant in an adding amount of 0.1g/L for carrying out an adsorption experiment, wherein the chemical demand (COD) of sewage in the initial secondary sedimentation tank is 43.67 mg/L; the COD of the effluent after 12 hours of the three is respectively measured, and the comparative experiment results are shown in the following table 1:
TABLE 1 comparison of adsorption effects of different carbon materials
| Product classification | COD(mg/L) | Adsorption capacity (mg/g) |
| Sewage peat | 26.68 | 169.9 |
| Commercial coconut shell activated carbon | 17.44 | 262.3 |
| Hydrochloric acid modified peat | 21.39 | 222.8 |
As can be seen from Table 1, after the sewage peat is modified by the hydrochloric acid in the secondary sedimentation tank for 12 hours, the chemical demand (COD) of the effluent is reduced from 43.67mg/L to 21.39mg/L, typical organic matters in the effluent sample are greatly reduced, and the adsorption effect of the effluent sample can be comparable to that of commercial coconut shell activated carbon. More specifically, the COD removal rate of the sludge carbon modified by hydrochloric acid is 51.12%, which is 12.11% higher than that of the unmodified sludge carbon (the COD removal rate is 39.01%), and the sludge carbon is slightly inferior to that of coconut shell activated carbon (the COD removal rate is 60.07%), but can also achieve higher removal rate.
Example 2: preparation of modified sludge carbon material
Referring to fig. 1, embodiment 2 of the present invention provides a method for preparing a modified sludge carbon material, including the following steps:
(1) adding a polyaluminium chloride (PAC) flocculant into the residual activated sludge of a certain municipal sewage treatment plant according to the mass ratio of 5 per mill of Total Suspended Solids (TSS) contained in the activated sludge, reacting for 30min to carry out dehydration conditioning, carrying out plate-and-frame filter pressing, carrying out high-pressure dehydration treatment, and then carrying out drying treatment through a 105 ℃ blast drying box to obtain a sludge dry sludge cake.
(2) Crushing, grinding and sieving the obtained sludge dry mud cake with a 100-mesh sieve to obtain powdery dry sludge, and storing the powdery dry sludge in a dryer; putting the powdery dry sludge into a porcelain boat, wherein the porcelain boat is filled with the powdery dry sludge to prevent air from entering, and the porcelain boat is covered by a porcelain cover plate; slowly placing the porcelain boat into a tube furnace, raising the temperature to 800 ℃ at a heating rate of 10 ℃/min in a nitrogen atmosphere, then staying for 30min for pyrolysis, cooling to room temperature after pyrolysis is finished (nitrogen circulation needs to be kept in the process), taking out a sample, washing off surface ash by deionized water, and drying for storage to obtain powdery peat;
(3) preparing 500ml of 2mol/L sodium hydroxide solution, adding 20g of powdered peat, oscillating at the constant temperature of 180r/min at the temperature of 20 ℃ for 12h, repeatedly washing with deionized water until the washing liquor is neutral, and drying to obtain the modified sludge carbon material.
Adopting SEM to represent the micro-morphologies of the powdery sludge carbon before modification and the modified sludge carbon material, which are respectively shown in FIG. 4a and FIG. 4 b; the powdery sludge carbon before modification and the modified sludge carbon material are characterized by BET specific surface areas, as shown in FIG. 5a and FIG. 5 b.
Comparing fig. 4a and fig. 4b, it can be seen that the surface of the modified sludge carbon material becomes rougher, and obviously fine pores are exposed on the surface, which indicates that the modified sludge carbon material also has good elution effect on the sludge carbon mineral by using NaOH solution as a modifier.
Comparing fig. 5a and fig. 5b, it can be known that the adsorption and desorption values of the modified sludge carbon material are higher, and the adsorption performance is obviously improved; the pore of the material is changed into a mesopore with larger pore from the original 2nm micropore and 10nm mesopore, and the mesopore is changed into an adsorbing material taking the mesopore as the main; the specific surface area is 130.11m2The/g is increased to 179.81m2The improvement is obvious, and the side surface reflects the enhancement of the adsorption performance of the material.
Adsorption experiments
Similar to example 1, the sludge carbon material modified by sodium hydroxide is put into a secondary sedimentation tank of a sewage plant in an adding amount of 0.1g/L, and sampling analysis is carried out after 12h, so that COD is reduced from 43.67mg/L of original effluent to 19.92mg/L, the removal rate reaches 54.4%, the adsorption capacity reaches 237.5mg/L, and the adsorption performance is slightly improved compared with that of the sludge carbon material modified by hydrochloric acid in example 1.
Three-dimensional fluorescence contrast analysis
The embodiment of the invention also performs three-dimensional fluorescence comparative analysis on the original effluent of the secondary sedimentation tank and the effluent water sample of the sludge carbon material modified by adding hydrochloric acid or sodium hydroxide into the secondary sedimentation tank, and analyzes typical organic matters in water, wherein the analysis result is shown in figure 6.
As shown in fig. 6, the soluble organic substances in the sewage of the water plant mainly include Tryptophan Proteins (TPN), Aromatic Proteins (APN), Fulvic Acid (FA), and Humic Acid (HA). After the hydrochloric acid or the sodium hydroxide modified sewage peat is respectively put into the water outlets of the secondary sedimentation tanks for 12 hours, the fluorescent substance peak intensity of the water sample of the outlet water is obviously reduced, which indicates that the sludge carbon material modified by the acid and the alkali has obvious effect of removing soluble organic matters in the sewage, and the direct reason of reducing the COD of the sewage is also the reason.
Meanwhile, compared with the removal effect of the acid-base modified sludge carbon, the difference between the two is not obvious, which shows that the enhancement mechanism of the acid-base modification on the original sludge carbon performance is mainly based on the elution effect and the improvement of the adsorption performance by exposing functional groups.
In conclusion, the modified sludge carbon material is prepared from the solid waste excess sludge which is difficult to be recycled as the adsorbent, so that the resource utilization of the sludge is realized; compared with the adsorption effect of commercial grade activated carbon, the adsorption experiment shows that under the same conditions, the adsorption performance of the modified sludge carbon material is better than that before modification, is slightly inferior to that of the commercial grade activated carbon adsorbent, but still has unusual adsorption capacity, can be applied to treatment of large-scale municipal sludge, and has innovativeness and environmental friendliness. And secondly, the modified sludge carbon material has simple preparation process and lower cost, and the acid-base solution used for modifying the sludge carbon material can be recycled, so that the preparation cost of the material is reduced, and the method is an effective way of treating wastes with processes of wastes against one another and changing wastes into valuables. In addition, the preparation process of the modified sludge carbon material is simple, stable and safe, solves the problem of difficult sludge treatment, realizes sludge recycling, and is an environment-friendly novel adsorption material.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. The preparation method of the modified sludge carbon material is characterized by comprising the following steps:
s1, taking a certain amount of activated sludge, adding a flocculating agent, and then physically dehydrating and drying to obtain a sludge dry mud cake;
s2, crushing and grinding the sludge dry mud cake prepared in the step S1, and sieving the crushed and ground sludge dry mud cake with a 100-mesh sieve to obtain powdery dry sludge;
s3, putting the powdery dry sludge obtained in the step S2 into a tube furnace, pyrolyzing at 800 ℃ for 30min under the anaerobic condition, cooling, taking out a sample, washing away surface ash by deionized water, and drying to obtain powdery sludge carbon;
s4, adding the powdered peat obtained in the step S3 into an acid or alkali modifier, soaking for 12-24h, repeatedly washing with deionized water until the washing liquor is neutral, and drying to obtain the modified sludge carbon material.
2. The method according to claim 1, wherein in step S1, the flocculant is one or more selected from polyaluminium chloride, polyferric chloride, aluminium chloride, ferric chloride, aluminium sulfate, ferric sulfate and polyacrylamide.
3. The method as claimed in claim 1, wherein in step S4, the acid or alkali modifier is one of hydrochloric acid, nitric acid or sodium hydroxide solution.
4. The method of claim 1, wherein the concentration of the acid or alkali modifier is 0.5mol/L-2mol/L in step S4.
5. The method of claim 4, wherein in step S4, the mass ratio of the powdered peat to the modifier is 1: 10.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111298821A (en) * | 2020-02-07 | 2020-06-19 | 天津大学 | Method for preparing novel iron-nitrogen-carbon catalyst by utilizing printing and dyeing wastewater flocculated sludge |
| CN111389368A (en) * | 2020-04-22 | 2020-07-10 | 徐州工程学院 | Preparation method of excess sludge biochar and application of excess sludge biochar in removing tetracycline in water |
| CN111592903A (en) * | 2020-04-29 | 2020-08-28 | 中国科学院广州能源研究所 | Method for removing tar by using municipal sludge |
| CN112108114A (en) * | 2020-09-09 | 2020-12-22 | 中国科学院武汉岩土力学研究所 | Preparation method of permeable reactive barrier material |
| CN112811785A (en) * | 2020-12-30 | 2021-05-18 | 中国葛洲坝集团生态环境工程有限公司 | Preparation method of sludge drying agent |
| CN113092336A (en) * | 2021-04-06 | 2021-07-09 | 西南石油大学 | Device and method for researching influence of coke deposition on reservoir physical properties |
| CN113786806A (en) * | 2021-09-30 | 2021-12-14 | 南通大学 | Ternary modified sewage peat defluorinating agent and preparation method thereof |
| CN114409078A (en) * | 2022-01-10 | 2022-04-29 | 南京工业大学 | Preparation and application method of sludge carbon-based functional material for improving A/O biochemical treatment efficiency of coal chemical wastewater |
| CN115108705A (en) * | 2022-06-30 | 2022-09-27 | 浙江科技学院 | Preparation method, product and application of modified magnetic sewage peat |
| CN115920964A (en) * | 2022-12-19 | 2023-04-07 | 中国科学技术大学 | Preparation method and application for realizing upgrading and conversion of municipal sludge into high-performance monatomic catalyst |
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| CN111298821A (en) * | 2020-02-07 | 2020-06-19 | 天津大学 | Method for preparing novel iron-nitrogen-carbon catalyst by utilizing printing and dyeing wastewater flocculated sludge |
| CN111389368A (en) * | 2020-04-22 | 2020-07-10 | 徐州工程学院 | Preparation method of excess sludge biochar and application of excess sludge biochar in removing tetracycline in water |
| CN111592903A (en) * | 2020-04-29 | 2020-08-28 | 中国科学院广州能源研究所 | Method for removing tar by using municipal sludge |
| CN111592903B (en) * | 2020-04-29 | 2021-10-19 | 中国科学院广州能源研究所 | Method for removing tar by using municipal sludge |
| CN112108114B (en) * | 2020-09-09 | 2021-08-24 | 中国科学院武汉岩土力学研究所 | Preparation method of permeable reactive barrier material |
| CN112108114A (en) * | 2020-09-09 | 2020-12-22 | 中国科学院武汉岩土力学研究所 | Preparation method of permeable reactive barrier material |
| CN112811785A (en) * | 2020-12-30 | 2021-05-18 | 中国葛洲坝集团生态环境工程有限公司 | Preparation method of sludge drying agent |
| CN113092336A (en) * | 2021-04-06 | 2021-07-09 | 西南石油大学 | Device and method for researching influence of coke deposition on reservoir physical properties |
| CN113786806A (en) * | 2021-09-30 | 2021-12-14 | 南通大学 | Ternary modified sewage peat defluorinating agent and preparation method thereof |
| CN114409078A (en) * | 2022-01-10 | 2022-04-29 | 南京工业大学 | Preparation and application method of sludge carbon-based functional material for improving A/O biochemical treatment efficiency of coal chemical wastewater |
| CN114409078B (en) * | 2022-01-10 | 2024-05-28 | 南京工业大学 | Preparation and application methods of sludge carbon-based functional material for improving A/O biochemical treatment efficiency of coal chemical wastewater |
| CN115108705A (en) * | 2022-06-30 | 2022-09-27 | 浙江科技学院 | Preparation method, product and application of modified magnetic sewage peat |
| CN115108705B (en) * | 2022-06-30 | 2023-08-11 | 浙江科技学院 | Preparation method, product and application of modified magnetic sludge peat |
| CN115920964A (en) * | 2022-12-19 | 2023-04-07 | 中国科学技术大学 | Preparation method and application for realizing upgrading and conversion of municipal sludge into high-performance monatomic catalyst |
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