CN112811785A - Preparation method of sludge drying agent - Google Patents

Preparation method of sludge drying agent Download PDF

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Publication number
CN112811785A
CN112811785A CN202011619982.4A CN202011619982A CN112811785A CN 112811785 A CN112811785 A CN 112811785A CN 202011619982 A CN202011619982 A CN 202011619982A CN 112811785 A CN112811785 A CN 112811785A
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sludge
drying agent
substance
temperature
drying
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陈玺
吴磊
郭沨
胡宝伽
谢雄
张宗仰
蔡维国
吴超
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China Gezhouba Group Ecological Environment Engineering Co ltd
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China Gezhouba Group Ecological Environment Engineering Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/12Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/14Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents
    • C02F11/143Treatment of sludge; Devices therefor by de-watering, drying or thickening with addition of chemical agents using inorganic substances
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00Treatment of sludge; Devices therefor
    • C02F11/10Treatment of sludge; Devices therefor by pyrolysis

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Treatment Of Sludge (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a preparation method of a sludge drying agent, which comprises the steps of firstly removing impurities from dredged sludge, standing for precipitation, then taking lower-layer settled sludge for extrusion dehydration, and drying to prepare sludge dry powder; then in CO2High-temperature pyrolysis in gas atmosphere, and finally acid washing, alkali washing and drying to obtain a finished product. The method obviously improves the dehydration effect of the sludge drier, increases the volume of sludge flocs, reduces the sedimentation volume of sludge and strengthens the dehydration performance of the sludge drier. The novel sludge drying agent which is equivalent to the dehydration performance of the existing sludge drying agent can be obtained by selecting waste sludge/dredged sludge which is easy to cause environmental pollution as a raw material and adopting a simple method for treatment, so that the production cost is obviously reduced, the waste utilization is realized, and the energy conservation and the environmental protection are realized.

Description

Preparation method of sludge drying agent
Technical Field
The invention belongs to the technical field of sludge treatment, and particularly relates to a preparation method of a sludge drying agent.
Background
Municipal sludge produced in main urban life of China has huge yield and is difficult to treat. The municipal sludge is treated mainly by sanitary landfill, incineration treatment, agricultural utilization, composting and the like. But the sanitary landfill treatment definitely requires that the water content of the sludge cake is not higher than 60 percent, and the incineration treatment is not higher than 50 percent. Therefore, the reduction of the residual moisture of the mud cake is an important step in the subsequent sludge treatment and disposal. Sludge drying is one of the common sludge treatment methods at present, and in addition to the modes of rapid stirring and the like, a sludge drying agent needs to be added in the drying process to further reduce the water content in the dried sludge finished product.
The dredged sludge serving as a byproduct for water environment restoration has the characteristics of high water content, loose structure and high organic matter content, and is prepared into a sludge drying agent by adopting a technical method, so that the quantity of the sludge can be effectively reduced, the aim of resource utilization is fulfilled, and the environmental pressure is reduced.
In the prior patent, for example, the granted Chinese patent CN102964054A provides a rapid drying process for dewatered sludge, which comprises pouring dewatered sludge into a stirrer, adding a drying agent ASG-1, adding a drying agent ASG-2 at a specific rotation speed, and stirring at the specific rotation speed to obtain a sludge dried finished product. The drying agent ASG-1 is powder prepared by mixing, calcining and grinding the drying auxiliary agent of the bauxite tailings, calcium oxide, calcium sulfate and ferrous sulfate according to a specific proportion. The drying agent ASG-2 is powder prepared by mixing the calcified red clay drying auxiliary agent with magnesium oxide and calcium sulfate according to a specific proportion, drying and grinding. However, although the moisture content of the sludge dried by the drying agent can be reduced from 80% to 40%, the treatment time is long, and the required equipment is complex and the cost is high.
For example, the chinese patent application CN109455900A provides a sludge drying agent, the raw materials of which include lime dry powder, gypsum dry powder, fly ash and probiotics, however, the drying agent is mainly used for preparing improved soil, although the moisture content of the sludge is reduced from 83% -87% to 45% -62%, the preparation time of the improved soil is as long as 6 days, which seriously affects the subsequent treatment period.
For example, the sludge drying agent provided by CN110818212A, the raw materials include quicklime, waste activated carbon, aluminum salt, and dimethyldiallylammonium chloride, and the preparation method comprises heating dimethyldiallylammonium chloride, adding initiator, keeping warm, and stirring to form a polymeric dimethyldiallylammonium chloride solution; then adding waste activated carbon at normal temperature, stirring to form a semisolid mixture, adding aluminum salt, stirring for reaction, and finally adding quicklime to mix to form a powdery/granular efficient sludge drying agent. The principle of the drying agent is that the sludge to be treated is dehydrated, then the high-efficiency sludge drying agent is added, after being uniformly mixed, the dried sludge is obtained through multiple exothermic reactions, and the water content of the sludge is reduced from 65-85% to 15-45%. The premise that the method can achieve good drying effect is to meet special requirements on equipment, and the required time is relatively long.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a sludge drying agent, which is realized by the following technology.
A preparation method of a sludge drying agent comprises the following steps:
s1, removing impurities from the dredging sludge, standing and precipitating, removing supernatant, taking the lower layer settling sludge, extruding and dehydrating to prepare dehydrated mud cakes with the water content of 75-85%; drying at 90-110 ℃ to constant weight, cooling to room temperature, grinding and sieving with a 200-mesh sieve to obtain sludge dry powder; the particle size of the sludge dry powder is not more than 150 μm in general;
s2, adding the sludge dry powder obtained in the step S1 into CO2Regulating CO in gas atmosphere and room temperature environment2The gas flow rate is 100-350mL/min, and the reaction is carried out for 5-60 min;
s3, adjusting CO2The gas flow rate is 50-100mL/min, the temperature is raised to 400-600 ℃ according to the temperature rise rate of 10-30 ℃/min, and then the temperature is kept for 0.5-3h at constant temperature, and CO is added2Cooling to room temperature in a gas atmosphere, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3, sieving the ground substance A with a 200-mesh sieve, and pickling the substance A with weak acid solution to obtain a substance B; the molar ratio of weak acid molecules in the weak acid solution to the substance A is 2-4: 1:
and S5, leaching the substance B obtained in the step S4 with NaOH solution until the pH value is alkalescent, washing with deionized water until the pH value of washing water is 7, and drying to obtain the sludge drying agent.
The preparation method of the sludge drying agent is to utilize the waste of the dredged sludge (sludge), firstly carry out preliminary dehydration, impurity removal, drying and grinding to prepare sludge dry powder, and then carry out drying treatment on the sludge dry powder in pure CO2High-temperature pyrolysis in gas atmosphere, grinding after cooling, acid and alkali washing, water washing and drying.
As the pyrolysis temperature is increased to 200 ℃ from room temperature, moisture, adsorbed volatile organic compounds, carbon-oxygen micromolecule gas and hydrides of nitrogen and sulfur elements in the sludge are gasified and removed in the temperature section. When the temperature is continuously increased to 500 ℃, the alkyl side chain in the macromolecular organic matter in the sludge is subjected to a fracture decomposition reaction, and a hydrocarbon gas phase product with a small molecular weight is separated out. At this time, almost all organic matters in the sludge are decomposed. CO under closed conditions2Secondary reactions with carbon atoms in the biochar matrix open closed pores, resulting in the formation of more micropores and increased porosity. With the significant rise of the pyrolysis temperature, the organic aliphatic hydrocarbon in the sludge is decomposed into CO2、CH4And other biomass gases are gradually converted into an aromatized structure to form a porous support structure. The metal elements in the sludge can be combined with a carbon layer in the material to form coordinate bonds, so that the aromatic performance and the graphitization degree of the biochar material can be improved, and the stability of the biochar material in the environment is further improved. When silt is dehydrated by external force extrusion, the porous support structure provides a seepage channel, prevents silt from being compressed and deformed to cause blockage of pores, and then influences the dehydration effect of silt.
The content of the ash is increased because organic matters in the sludge are continuously decomposed in the pyrolysis process, and inorganic components contained in the ash are not decomposed and released along with the increase of the pyrolysis temperature but are retained in the sludge. The product after high-temperature pyrolysis can remove part of ash after being washed by acid and alkali, and the porosity and permeability are improved. When weak acids such as phosphoric acid and the like are adopted for cleaning, the weak acid salt is adsorbed on the surface of the drying agent through electrostatic attraction, can be combined with metal cations in the sludge, forms an insoluble compound through complexation, and performs surface complexation with functional groups such as carboxyl, hydroxyl and the like, thereby improving the settling property of the sludge. More sodium salts can be used for etching the carbon skeleton by adopting alkaline washing, so that more micropores are generated, the specific surface area and the micropore volume are increased, the reaction contact area is increased, and the adsorption and sedimentation efficiency is improved.
Only the CO is mixed2Pretreatment of gas atmosphere-pyrolysis-acid washing-alkaline washing, especially with specific CO2The combination of the gas atmosphere, the acid washing and the sodium hydroxide leaching can maximize the specific surface area and the pore diameter of the sludge drying agent, improve the settling property, shorten the capillary water absorption time and improve the dehydration effect. Preferably, the drying temperature in step S1 is 105 ℃.
Preferably, in step S2, CO2The gas flow rate of (2) was 250mL/min, and the reaction time was 35 min.
Preferably, in step S3, CO2The flow rate of the gas is 80mL/min, the temperature is raised to 500 ℃ at the temperature raising rate of 25 ℃/min, and then the temperature is kept for 2 h.
Preferably, in step S3, the weak acid solution is at least one of phosphoric acid and citric acid.
More preferably, in step S3, the weak acid solution is a phosphoric acid solution. When the weak acid is phosphoric acid alone, the effect is best.
Further preferably, in step S3, the molar mass ratio of the weak acid molecules in the weak acid solution to the substance a is 3: 1.
Preferably, in step S5, weakly alkaline means a pH of 7.5-8.
Preferably, in step S5, the drying temperature is 40-50 ℃.
Compared with the prior art, the invention has the advantages that:
1. this patent uses CO2CO is controlled under the synergistic treatment action of gas atmosphere pretreatment, high-temperature pyrolysis, acid washing and alkali washing2Flow rate and pretreatment of gasThe time, the temperature and the reaction time of high-temperature pyrolysis are controlled, and the types and the dosage of acid and alkali used for acid washing and alkali washing are controlled, so that the dehydration effect of the sludge drying agent is obviously improved, the volume of sludge floc is increased, the sedimentation volume of sludge is reduced, and the dehydration performance of the sludge drying agent is enhanced.
2. The patent does not use expensive materials to prepare the drying agent, but selects waste sludge/dredged sludge which easily causes environmental pollution as raw materials, adopts a simple method to treat the raw materials, can obtain the novel sludge drying agent which is equivalent to the dehydration performance of the existing sludge drying agent, obviously reduces the production cost, realizes waste utilization, and is more energy-saving and environment-friendly.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following examples and comparative examples used dredging sludge from river channels in the lake region of the saltern pavilion.
Example 1
The sludge drying agent of the embodiment is prepared by the following method:
s1, removing impurities from the dredged sludge, standing and precipitating, removing supernatant, taking lower-layer settled sludge, and extruding and dehydrating to obtain dehydrated mud cakes with the water content of about 85%; putting the dehydrated mud cake into a drying oven, drying at 105 ℃ to constant weight, taking out, putting into a drying dish, cooling to room temperature, grinding and sieving to obtain dry sludge powder, collecting the dry sludge powder and storing by using a sealing bag;
s2, placing the dry sludge powder in a quartz boat, pushing the quartz boat to the middle position of the heating section of the horizontal tube furnace, firstly closing the tube furnace heating program, and introducing CO2Gas, conditioning CO2The gas flow rate is 250mL/min, and the reaction is carried out for 35min under the room temperature environment;
s3, adjusting CO2A gas flow rate of80mL/min, starting a tubular furnace heating program, heating to 500 ℃ according to a heating rate of 25 ℃/min, keeping the constant temperature for 2h, and continuing to perform CO treatment2Cooling to room temperature in a gas atmosphere, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3, and pickling with a phosphoric acid solution with the concentration of 20% to obtain a substance B; the molar ratio of weak acid molecules in the weak acid solution to the substance A is 3: 1;
s5, leaching the substance B obtained in the step S4 with 0.5mol/L NaOH solution to be alkalescent with the pH value of 8, washing with deionized water until the pH value of washing water is 7, finally putting into a drying oven, and drying at 40 ℃ to obtain the finished product of the sludge drying agent.
Example 2
The difference between the preparation method adopted by the sludge drying agent of the embodiment and the embodiment 1 is that: in step S2, CO2The gas flow rate of (2) was 350mL/min, and the reaction time was 5 min.
Example 3
The difference between the preparation method adopted by the sludge drying agent of the embodiment and the embodiment 1 is that: in step S2, CO2The gas flow rate of (2) was 100mL/min, and the reaction time was 60 min.
Example 4
The difference between the preparation method adopted by the sludge drying agent of the embodiment and the embodiment 1 is that: in step S3, CO2The gas flow rate of (2) is 100mL/min, the temperature is raised to 400 ℃ at a temperature raising rate of 25 ℃/min, and then the temperature is kept for 3 h.
Example 5
The difference between the preparation method adopted by the sludge drying agent of the embodiment and the embodiment 1 is that: in step S3, CO2The flow rate of the gas is 50mL/min, the temperature is raised to 600 ℃ at the temperature raising rate of 25 ℃/min, and then the temperature is kept for 0.5 h.
Example 6
The difference between the preparation method adopted by the sludge drying agent of the embodiment and the embodiment 1 is that: in step S3, a phosphoric acid solution is used in which the molar mass ratio of phosphoric acid molecules to the substance A is 4: 1.
Example 7
The difference between the preparation method adopted by the sludge drying agent of the embodiment and the embodiment 1 is that: in step S3, a phosphoric acid solution is used in which the molar mass ratio of phosphoric acid molecules to the substance A is 2: 1.
Example 8
The difference between the preparation method adopted by the sludge drying agent of the embodiment and the embodiment 1 is that: in step S3, citric acid with a concentration of 5% is used instead of phosphoric acid.
Comparative example 1
The method for producing the sludge drying agent of the present comparative example is different from that of example 1 in that CO is not present in step S2 and step S32The preparation method comprises the following steps:
s1, removing impurities from the dredged sludge, standing and precipitating, removing supernatant, taking lower-layer settled sludge, and extruding and dehydrating to obtain dehydrated mud cakes with the water content of about 85%; putting the dehydrated mud cake into a drying oven, drying at 105 ℃ to constant weight, taking out, putting into a drying dish, cooling to room temperature, grinding and sieving to obtain dry sludge powder, collecting the dry sludge powder and storing by using a sealing bag;
s2, placing the dry sludge powder in a quartz boat, pushing the quartz boat to the middle position of a heating section of the horizontal tube furnace, firstly closing a heating program of the tube furnace, and placing for 35min at room temperature;
s3, starting a tubular furnace heating program, heating to 500 ℃ at a heating rate of 25 ℃/min, keeping the temperature for 2h, cooling to room temperature, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3, and pickling with a phosphoric acid solution with the concentration of 20% to obtain a substance B; the molar mass ratio of weak acid molecules in the weak acid solution to the substance A is 3: 1;
s5, leaching the substance B obtained in the step S4 with 0.5mol/L NaOH solution to be alkalescent with the pH value of 8, washing with deionized water until the pH value of washing water is 7, finally putting into a drying oven, and drying at 40 ℃ to obtain the finished product of the sludge drying agent.
Comparative example 2
Sludge drying agent of the present comparative exampleThe preparation method used differs from example 1 in that the original step S2 is not carried out, but rather the CO of step S3 is carried out directly after completion of step S12The preparation method comprises the following steps:
s1, removing impurities from the dredged sludge, standing and precipitating, removing supernatant, taking lower-layer settled sludge, and extruding and dehydrating to obtain dehydrated mud cakes with the water content of about 85%; putting the dehydrated mud cake into a drying oven, drying at 105 ℃ to constant weight, taking out, putting into a drying dish, cooling to room temperature, grinding and sieving to obtain dry sludge powder, collecting the dry sludge powder and storing by using a sealing bag;
s2, placing the dry sludge powder in a quartz boat, pushing the quartz boat to the middle position of a heating section of a horizontal tube furnace, starting a tube furnace heating program, heating to 500 ℃ at a heating rate of 25 ℃/min, keeping the constant temperature for 2h, cooling to room temperature, and taking out to obtain a substance A;
s3, grinding the substance A obtained in the step S2, and pickling with a phosphoric acid solution with the concentration of 20% to obtain a substance B; the molar mass ratio of weak acid molecules in the weak acid solution to the substance A is 3: 1;
s4, leaching the substance B obtained in the step S3 with 0.5mol/L NaOH solution to be alkalescent with the pH value of 8, washing with deionized water until the pH value of washing water is 7, finally putting into a drying oven, and drying at 40 ℃ to obtain the finished product of the sludge drying agent.
Comparative example 3
The method for producing the sludge drying agent of the present comparative example differs from example 1 in that the pretreatment and reaction are performed in the nitrogen atmosphere in step S2 and step S3, and CO is not used2The gas atmosphere of (2).
Comparative example 4
The difference between the preparation method of the sludge drying agent of this example and that of example 1 is that the weak acid used in step S2 and step S4 is a 20% acetic acid solution, not a phosphoric acid solution.
Comparative example 5
The difference between the preparation method adopted by the sludge drying agent in this embodiment and embodiment 1 is that no weak acid solution is used for pickling in step S4, and the specific preparation method is as follows:
s1, removing impurities from the dredged sludge, standing and precipitating, removing supernatant, taking lower-layer settled sludge, and extruding and dehydrating to obtain dehydrated mud cakes with the water content of about 85%; putting the dehydrated mud cake into a drying oven, drying at 105 ℃ to constant weight, taking out, putting into a drying dish, cooling to room temperature, grinding and sieving to obtain dry sludge powder, collecting the dry sludge powder and storing by using a sealing bag;
s2, placing the dry sludge powder in a quartz boat, pushing the quartz boat to the middle position of the heating section of the horizontal tube furnace, firstly closing the tube furnace heating program, and introducing CO2Gas, conditioning CO2The gas flow rate is 250mL/min, and the reaction is carried out for 35min under the room temperature environment;
s3, adjusting CO2The gas flow rate is 80mL/min, the heating program of the tube furnace is started, the temperature is raised to 500 ℃ according to the temperature rise rate of 25 ℃/min, the constant temperature is kept for 2h, and the reaction is continued in CO2Cooling to room temperature in a gas atmosphere, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3 to obtain a substance B;
s5, leaching the substance B obtained in the step S4 with 0.5mol/L NaOH solution to be alkalescent with the pH value of 8, washing with deionized water until the pH value of washing water is 7, finally putting into a drying oven, and drying at 40 ℃ to obtain the finished product of the sludge drying agent.
Comparative example 6
The difference between the preparation method adopted by the sludge drying agent of this embodiment and embodiment 1 is that no NaOH solution is used for alkaline washing in step S5, and the specific preparation method is as follows:
s1, removing impurities from the dredged sludge, standing and precipitating, removing supernatant, taking lower-layer settled sludge, and extruding and dehydrating to obtain dehydrated mud cakes with the water content of about 85%; putting the dehydrated mud cake into a drying oven, drying at 105 ℃ to constant weight, taking out, putting into a drying dish, cooling to room temperature, grinding and sieving to obtain dry sludge powder, collecting the dry sludge powder and storing by using a sealing bag;
s2, placing the dry sludge powder in a quartz boat, pushing the quartz boat to the middle position of the heating section of the horizontal tube furnace, and firstly closing the tube furnace and addingThermal procedure, introduction of CO2Gas, conditioning CO2The gas flow rate is 250mL/min, and the reaction is carried out for 35min under the room temperature environment;
s3, adjusting CO2The gas flow rate is 80mL/min, the heating program of the tube furnace is started, the temperature is raised to 500 ℃ according to the temperature rise rate of 25 ℃/min, the constant temperature is kept for 2h, and the reaction is continued in CO2Cooling to room temperature in a gas atmosphere, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3, and pickling with a phosphoric acid solution with the concentration of 20% to obtain a substance B; the molar mass ratio of weak acid molecules in the weak acid solution to the substance A is 3: 1;
and S5, washing the substance B obtained in the step S4 with deionized water until the pH value of washing water is 7, finally putting the substance B into a drying oven, and drying at 40 ℃ to obtain a finished product of the sludge drying agent.
Comparative example 7
The difference between the preparation method of the sludge drying agent of this example and that of example 1 is that CO is not present in step S2 and step S32The reaction is performed in the gas atmosphere of (3), and the acid washing is not performed with the weak acid solution in the step S4. Namely, the specific preparation method of the alkali washing only in the step S5 comprises the following steps:
s1, removing impurities from the dredged sludge, standing and precipitating, removing supernatant, taking lower-layer settled sludge, and extruding and dehydrating to obtain dehydrated mud cakes with the water content of about 85%; putting the dehydrated mud cake into a drying oven, drying at 105 ℃ to constant weight, taking out, putting into a drying dish, cooling to room temperature, grinding and sieving to obtain dry sludge powder, collecting the dry sludge powder and storing by using a sealing bag;
s2, placing the dry sludge powder in a quartz boat, pushing the quartz boat to the middle position of a heating section of the horizontal tube furnace, firstly closing a heating program of the tube furnace, and placing for 35min at room temperature;
s3, starting a tubular furnace heating program, heating to 500 ℃ at a heating rate of 25 ℃/min, keeping the temperature for 2h, cooling to room temperature, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3 to obtain a substance B;
s5, leaching the substance B obtained in the step S4 with 0.5mol/L NaOH solution to be alkalescent with the pH value of 8, washing with deionized water until the pH value of washing water is 7, finally putting into a drying oven, and drying at 40 ℃ to obtain the finished product of the sludge drying agent.
Comparative example 8
The difference between the preparation method of the sludge drying agent of this example and that of example 1 is that CO is not present in step S2 and step S32The reaction was carried out in an atmosphere of (3), and in step S5, alkali washing with NaOH solution was not carried out, that is, only acid washing in step S4 was carried out. The preparation method comprises the following steps:
s1, removing impurities from the dredged sludge, standing and precipitating, removing supernatant, taking lower-layer settled sludge, and extruding and dehydrating to obtain dehydrated mud cakes with the water content of about 85%; putting the dehydrated mud cake into a drying oven, drying at 105 ℃ to constant weight, taking out, putting into a drying dish, cooling to room temperature, grinding and sieving to obtain dry sludge powder, collecting the dry sludge powder and storing by using a sealing bag;
s2, placing the dry sludge powder in a quartz boat, pushing the quartz boat to the middle position of a heating section of the horizontal tube furnace, firstly closing a heating program of the tube furnace, and placing for 35min at room temperature;
s3, starting a tubular furnace heating program, heating to 500 ℃ at a heating rate of 25 ℃/min, keeping the temperature for 2h, cooling to room temperature, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3, and pickling with a phosphoric acid solution with the concentration of 20% to obtain a substance B; the molar mass ratio of weak acid molecules in the weak acid solution to the substance A is 3: 1;
and S5, washing the substance B obtained in the step S4 with deionized water until the pH value of washing water is 7, finally putting the substance B into a drying oven, and drying at 40 ℃ to obtain a finished product of the sludge drying agent.
Comparative example 9
The difference between the preparation method used for the sludge drying agent of this example and that of example 1 is that no acid washing with a weak acid solution is performed in step S4, and no alkali washing with a NaOH solution is performed in step S5, i.e., only CO is performed in steps S2 and S32The reaction in a gaseous atmosphere of (3). The preparation method comprises the following steps:
s1, removing impurities from the dredged sludge, standing and precipitating, removing supernatant, taking lower-layer settled sludge, and extruding and dehydrating to obtain dehydrated mud cakes with the water content of about 85%; putting the dehydrated mud cake into a drying oven, drying at 105 ℃ to constant weight, taking out, putting into a drying dish, cooling to room temperature, grinding and sieving to obtain dry sludge powder, collecting the dry sludge powder and storing by using a sealing bag;
s2, placing the dry sludge powder in a quartz boat, pushing the quartz boat to the middle position of the heating section of the horizontal tube furnace, firstly closing the tube furnace heating program, and introducing CO2Gas, conditioning CO2The gas flow rate is 250mL/min, and the reaction is carried out for 35min under the room temperature environment;
s3, adjusting CO2The gas flow rate is 80mL/min, the heating program of the tube furnace is started, the temperature is raised to 500 ℃ according to the temperature rise rate of 25 ℃/min, the constant temperature is kept for 2h, and the reaction is continued in CO2Cooling to room temperature in a gas atmosphere, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3 to obtain a substance B;
and S5, washing the substance B obtained in the step S4 with deionized water until the pH value of washing water is 7, finally putting the substance B into a drying oven, and drying at 40 ℃ to obtain a finished product of the sludge drying agent.
Application example 1: parameter detection of sludge drying Agents prepared in examples 1-8 and comparative examples 1-9
The sludge drying agents prepared in examples 1 to 8 and comparative examples 1 to 9 were used to measure the specific surface area, total pore volume and average particle diameter. The EVO 18 type scanning electron microscope of Carl Zeiss company is selected for observing the surface appearance of the sludge and the sludge activated carbon.
The specific surface area and the pore size distribution were determined by a model JW-BK100A specific surface area and pore size analyzer from Chi Gaobo. The method is characterized by adopting a liquid nitrogen low-temperature adsorption-desorption method for determination, namely, liquid nitrogen is used as an adsorption medium, and nitrogen adsorption and desorption tests are carried out under the condition that the temperature is 77K. The sample should be first vacuum dried for 6h by degassing and 2h at 200 ℃ before testing in order to effectively remove moisture and other impurity gases from the sample tube. And obtaining a curve through testing, namely the adsorption and desorption isotherm. And analyzing the adsorption and desorption isothermal curves, calculating the specific surface area of the product according to a Brunauer-Emmett-Teller (BET) model, and obtaining the mesopore distribution condition by using a Barrett-Joyner-Halenda (BJH) model. The total pore volume was calculated from the nitrogen adsorption volume at the relative saturation pressure point P/P0 of 0.99; the micropore volume can be calculated by a t-plot method; the mesopore pore volume of the material is obtained by subtracting the micropore volume from the total pore volume of the material. The results of the measurements are shown in Table 1 below.
TABLE 1 sludge drying agent parameter test results
Figure BDA0002873879820000091
Figure BDA0002873879820000101
As can be seen from Table 1 above, when CO of step S2 is adjusted2Flow rate and reaction time of the gas atmosphere of (1), CO of step S32The flow rate, the heating rate, the highest temperature and the reaction time of the heating atmosphere have certain influence on the specific surface area, the total pore volume and the average pore diameter of the sludge drying agent. When CO is not adopted in steps S2 and S32The gas atmosphere (2) of (4) directly from step S1 to step S3 without performing step S2, and the specific surface area, total pore volume and average pore diameter of the sludge drying agent are seriously affected by other gas atmospheres without performing acid washing or alkali washing. CO was carried out simultaneously only in the manner of examples 1 to 82The sludge drying agent with larger specific surface area, total pore volume and average pore diameter can be obtained only by the reaction in the gas atmosphere and the acid washing and the alkali washing in sequence.
Application example 2: dehydration Performance of activated sludge Using sludge-drying Agents prepared in examples 1-8 and comparative examples 1-9
Taking 119 parts of activated sludge with initial water content of 90% of a certain sewage treatment plant, and respectively putting the activated sludge into beakers, wherein the amount of each part is 100 mL; respectively measuring 2g of the sludge drying agents prepared in examples 1-8 and comparative examples 1-9, adding the sludge drying agents into the corresponding activated sludge, and taking the activated sludge in the rest beaker as a blank control; the beaker is placed on a magnetic stirrer and stirred for 3min at 200r/min, and then stirred for 5min at 100 r/min. And after conditioning is finished, respectively testing the dehydration performance of the activated sludge conditioned by the sludge drying agent. The sedimentation performance evaluation adopts SV30, the height of a sludge solid sedimentation interface is recorded once every 2min, the observation is continued for 30min, and finally a curve of the sedimentation interface height along with time is obtained; the filtration performance evaluation uses capillary water absorption time, the inner diameter of a funnel for testing is 16mm, and each sample is tested for three times; the dehydration performance evaluation method is to use a vacuum filtration device to dehydrate the conditioned activated sludge under 0.06MPa until no water drops, and then the dehydration is finished. And drying the mud cake sample in a 105 ℃ oven to constant weight, taking out, placing in a drying vessel for cooling, weighing, and calculating according to the mass change of the mud cake before and after drying treatment to obtain the water content of the dewatered sludge mud cake. The test results are shown in table 2.
TABLE 2 dewatering Performance test of activated sludge
Figure BDA0002873879820000102
Figure BDA0002873879820000111
As is clear from Table 2 above, when the drying agent is used, the sedimentation volume ratio of the activated sludge and the water content after the dehydration by the same dehydration method become significantly large, and the sedimentation time and the fine water absorption time become significantly long. When CO is not used2When the gas atmosphere pretreatment-high temperature pyrolysis-acid washing-alkali washing synergistic treatment method is used, although a certain dehydration effect can be achieved on the activated sludge, the effect is not ideal.

Claims (9)

1. The preparation method of the sludge drying agent is characterized by comprising the following steps:
s1, removing impurities from the dredging sludge, standing and precipitating, removing supernatant, taking the lower layer settling sludge, extruding and dehydrating to prepare dehydrated mud cakes with the water content of 75-85%; drying at 90-110 ℃ to constant weight, cooling to room temperature, grinding and sieving with a 200-mesh sieve to obtain sludge dry powder;
s2, adding the sludge dry powder obtained in the step S1 into CO2Regulating CO in gas atmosphere and room temperature environment2The gas flow rate is 100-350mL/min, and the reaction is carried out for 5-60 min;
s3, adjusting CO2The gas flow rate is 50-100mL/min, the temperature is raised to 400-600 ℃ according to the temperature rise rate of 10-30 ℃/min, and then the temperature is kept for 0.5-3h at constant temperature, and CO is added2Cooling to room temperature in a gas atmosphere, and taking out to obtain a substance A;
s4, grinding the substance A obtained in the step S3, sieving the ground substance A with a 200-mesh sieve, and pickling the substance A with weak acid solution to obtain a substance B; the molar ratio of weak acid molecules in the weak acid solution to the substance A is 2-4: 1;
and S5, leaching the substance B obtained in the step S4 with NaOH solution until the pH value is alkalescent, washing with deionized water until the pH value of washing water is 7, and drying to obtain the sludge drying agent.
2. The method for producing a sludge drying agent as claimed in claim 1, wherein the drying temperature in step S1 is 105 ℃.
3. The method according to claim 1, wherein in step S2, CO is used as a drying agent2The gas flow rate of (2) was 250mL/min, and the reaction time was 35 min.
4. The method according to claim 1, wherein in step S4, CO is used as a drying agent2The flow rate of the gas is 80mL/min, the temperature is raised to 500 ℃ at the temperature raising rate of 25 ℃/min, and then the temperature is kept for 2 h.
5. The method of claim 1, wherein in step S4, the weak acid solution is at least one of phosphoric acid and citric acid.
6. The method for preparing a sludge drying agent as claimed in claim 5, wherein in step S3, the weak acid solution is phosphoric acid solution.
7. The method for preparing a sludge drying agent as claimed in claim 5 or 6, wherein in step S3, the molar mass ratio of weak acid molecules in the weak acid solution to the substance A is 3: 1.
8. The method for preparing a sludge drying agent as claimed in claim 1, wherein the weak alkaline means that the pH value is 7.5-8 in step S5.
9. The method for preparing a sludge drying agent as claimed in claim 1, wherein in the step S5, the drying temperature is 40-50 ℃.
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