CN112551633B - Method for carrying out resource treatment on incineration fly ash to adsorb heavy metals in wastewater - Google Patents
Method for carrying out resource treatment on incineration fly ash to adsorb heavy metals in wastewater Download PDFInfo
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- CN112551633B CN112551633B CN202011530049.XA CN202011530049A CN112551633B CN 112551633 B CN112551633 B CN 112551633B CN 202011530049 A CN202011530049 A CN 202011530049A CN 112551633 B CN112551633 B CN 112551633B
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention provides a method for carrying out resource treatment on incineration fly ash to adsorb heavy metals in wastewater, which comprises the following steps: step 1, mixing 1-6 mol/L sodium sulfide solution and incineration fly ash in a liquid-solid ratio of (1-3) mL:1g of the mixture is uniformly mixed to obtain a mixed system; step 2, heating the mixed system at 100-200 ℃ to obtain a reaction solution containing zeolite, separating the zeolite in the reaction solution, and drying to obtain zeolite; and 3, soaking zeolite in wastewater which has a pH value of 4-8 and contains heavy metals, carrying out constant-temperature oscillation adsorption at room temperature until adsorption is balanced, separating the adsorbed zeolite from the adsorbed wastewater, and removing the heavy metals in the wastewater, wherein the wastewater treatment amount is large, and the wastewater can be purified to a discharge water standard while the heavy metal ions in the incineration fly ash are solidified, so that the purpose of treating the wastewater with waste is achieved.
Description
Technical Field
The invention relates to the field of solid waste treatment and heavy metal removal from wastewater, in particular to a method for carrying out resource treatment on incineration fly ash to adsorb heavy metal in wastewater.
Background
The output and accumulation of solid wastes such as municipal solid wastes and industrial wastes in China are increasing year by year, the incineration method becomes one of the main modes of the waste treatment, the wastes form three parts after being incinerated in a waste incinerator, namely slag, fly ash and waste gas, and the fly ash is the solid waste which is taken out by the waste gas and captured by a dust collector. The fly ash contains a large amount of Al2O3、SiO2、Na2O、Cl-In addition, a small amount of hazardous waste such as heavy metal ions of various types such as dioxin, mercury, lead, cadmium and the like is treated by a safe landfill method, a solidification stabilization method, a heavy metal extraction method and the like. In addition, the treatment of industrial wastewater and domestic wastewater is also in progressThe problem to be solved after the generation is intensified is urgently solved, and the water resource shortage and the water pollution degree deepening all put higher requirements on the wastewater treatment.
In the existing method, the dissolution of silicon and aluminum is accelerated by alkali eutectic heat treatment under nitrogen environment, and heavy metal is encapsulated to fix heavy metal ions in the process of sodalite assembly. However, the alkali eutectic heat treatment requires a higher heating temperature, which increases the energy consumption in the heat treatment process, and the heating in a nitrogen environment also increases the treatment cost.
The incineration fly ash can be used for preparing a novel heat-insulating material by adding fly ash and waste glass. The incineration fly ash contains a certain amount of silicon element, aluminum element and the like, and has great use value in the aspects of preparing adsorbing materials such as zeolite besides building materials. The zeolite has the advantages of large specific surface area and porosity, and can be used as an adsorbing material for purifying waste liquid containing heavy metal ions. Meanwhile, the adsorption of the zeolite has selectivity, and has the performances of acid resistance, high temperature resistance and radiation resistance, so that the zeolite can be well used for adsorbing heavy metal ions in industrial wastewater and can also be used for adsorbing ammonia ions in agricultural wastewater. Therefore, how to perform resource treatment on the incineration fly ash and further adsorb heavy metals in the wastewater is an urgent problem to be solved.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a method for carrying out resource treatment on incineration fly ash to adsorb heavy metals in wastewater, the wastewater treatment amount is large, the heavy metal ions in the incineration fly ash are solidified, and simultaneously, the wastewater can be purified to the discharge water standard, so that the purpose of treating waste by waste is achieved.
The invention is realized by the following technical scheme:
a method for carrying out resource treatment on incineration fly ash to adsorb heavy metals in wastewater comprises the following steps:
step 1, mixing 1-6 mol/L sodium sulfide solution and incineration fly ash in a liquid-solid ratio of (1-3) mL:1g of the mixture is uniformly mixed to obtain a mixed system;
step 2, heating the mixed system at 100-200 ℃ to obtain a reaction solution containing zeolite, separating the zeolite in the reaction solution, and drying to obtain zeolite;
and 3, soaking the zeolite in wastewater which has a pH value of 4-8 and contains heavy metals, carrying out constant-temperature oscillation adsorption at room temperature until adsorption is balanced, separating the adsorbed zeolite from the adsorbed wastewater, and removing the heavy metals from the wastewater.
Preferably, the incineration fly ash in the step 1 is the incineration fly ash after drying treatment, the drying temperature is 100-110 ℃, and the drying time is 1-6 h.
Preferably, the incineration fly ash in the step 1 is one or two of incineration fly ash of domestic garbage and incineration fly ash of medical waste.
Preferably, in the step 1, the sodium sulfide solution and the incineration fly ash are stirred for 2-10 min at a rotating speed of 30-60 r/min.
Preferably, in the step 2, the mixed system is heated by microwaves, the microwave power is 800-1200W, and the heating time is 10-20 min.
Preferably, in the step 3, the pH value of the wastewater containing the heavy metals is adjusted to 4-8 by using a sodium hydroxide solution or dilute nitric acid.
Preferably, the liquid-solid ratio of the wastewater to the zeolite in the step 3 is 3-12 ml/g.
Preferably, the oscillation in step 3 is horizontal reciprocating oscillation or rotary oscillation.
Preferably, the oscillation rate of the zeolite in the step 3 in the wastewater is 100-220 r/min, and the adsorption time is 50-200 min.
Preferably, in the step 3, the adsorbed zeolite is washed by a sodium chloride solution with the concentration of 0.5-3 mol/L, then the zeolite treated by the sodium chloride is filtered, and then the zeolite obtained by filtering is dried at the temperature of 55-65 ℃ and then is continuously recycled according to the step 3.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention relates to a method for absorbing heavy metals in wastewater by carrying out resource treatment on incineration fly ash, which uses low-cost sodium sulfideMixing the fly ash with sodium sulfide solution to obtain zeolite with porous structure, and adding S in the sodium sulfide solution2-And a part of heavy metal ions (such as Cd) in incineration fly ash3+、Pd2+、Cr3+、Hg2+And the like) to react, a part of heavy metal ions in the incineration fly ash are solidified in a sulfide precipitation mode, the cost is lower compared with that of the traditional additive, such as sodium hydroxide, the synthesized zeolite is used for further solidifying the heavy metal in the incineration fly ash, the porous structure of the zeolite selectively adsorbs the heavy metal and impurities in the wastewater under the condition that the pH value is 4-8, and the heavy metal ions in the wastewater, such as Cu, are mainly adsorbed through the adsorption-ion exchange action of the zeolite2+、Pb2+、Zn2+、Cd2+、Hg2+The method takes the environment-friendly idea of treating waste with waste as guidance, recycles the incineration fly ash as a resource, realizes the purification treatment of the heavy metal wastewater, and has the advantages of high treatment speed, wide application range and good application prospect; meanwhile, the incineration fly ash does not need to be washed, so that water resources are saved, and the resource utilization rate is improved.
Furthermore, under the action of microwave-assisted heating, the heating speed is high, the heating is uniform, the synthesis speed of the zeolite is high, and S is promoted2-The reaction with heavy metal ions in the incineration fly ash improves the crystallization speed and porosity of the zeolite, and the obtained zeolite has stronger adsorption capacity.
Furthermore, the adsorption capacity of the zeolite subjected to adsorption saturation is still in a higher range after slow release treatment, the zeolite can be recycled, the treatment cost is reduced, the resource utilization rate is improved, and the wastewater is directly discharged after reaching the discharge water standard.
Drawings
FIG. 1 is a schematic process flow diagram of the process of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention discloses a method for carrying out resource treatment on incineration fly ash to adsorb heavy metals in wastewater, which comprises the following steps as shown in figure 1:
step (1), drying incineration fly ash;
the drying temperature is 105 +/-5 ℃, and the drying time is 1-6 h. The incineration fly ash comprises one or more of solid waste incineration fly ash such as domestic waste incineration fly ash, medical waste incineration fly ash and the like;
and (2) mixing a sodium sulfide solution with the dried incineration fly ash in a liquid-solid ratio of (1-3) mL:1g of the mixture is mixed and stirred evenly;
the concentration of the sodium sulfide solution can be adjusted according to the Si/Al molar ratio in the dried incineration fly ash, and the adjustment range is 1-6 mol/L, so that the synthesis of zeolite is facilitated;
the types of the prepared zeolite are different according to different silicon-aluminum ratios, but the zeolite can be used for treating heavy metal wastewater and is stirred for 2-10 min in a stirrer with the rotating speed of 30-60 r/min;
step (3), adding the uniformly stirred mixture obtained in the step (2) into a reaction container for microwave heating, and then filtering and drying to obtain zeolite with a porous structure, so that the crystallization speed of a target product is improved; wherein sodium sulfide reacts with heavy metal in fly ash to solidify a part of heavy metal in fly ash in the form of sulfide precipitate, and microwave-assisted treatment can promote S2-The zeolite generated by the reaction with the heavy metal ions in the fly ash can better fix the residual heavy metal ions in the fly ash;
the microwave power is 800-1200W, the heating temperature is 100-200 ℃, and the heating time is 10-20 min;
step (4), adjusting the pH value of the wastewater, detecting the pH value of the wastewater according to different taken wastewater, and adjusting the pH value to be 4-8 by using sodium hydroxide or dilute nitric acid to enable zeolite to achieve the optimal adsorption effect; then mixing the zeolite prepared in the step (3) with a certain proportion, oscillating and adsorbing at constant temperature until the adsorption is balanced, and separating the adsorbed zeolite from the wastewater to finish the removal of heavy metals in the wastewater;
the liquid-solid ratio of the zeolite mixed with the wastewater is adjusted according to the heavy metal content in different wastewater, and the adjustment range is 3-12 ml/g. The oscillation mode adopts horizontal reciprocating oscillation or rotary oscillation. The oscillating adsorption time is 50-200 min, the oscillating speed is 100-220 r/min, and the adsorption is carried out under the room temperature condition;
step (5), the zeolite with saturated adsorption can be recycled after being treated, or the zeolite with saturated adsorption can be directly used as a building material;
and (3) carrying out solid-liquid separation on the adsorbed zeolite and the wastewater, repeatedly washing and filtering the separated zeolite saturated in adsorption by using a sodium chloride solution with the concentration of 0.5-3 mol/L, and drying the filtered zeolite at 60 +/-5 ℃ until the weight of the zeolite is kept unchanged so as to be repeatedly recycled.
In the case of example 1, the following examples,
drying the household garbage incineration fly ash at 105 ℃ for 4h, then adjusting the concentration of a sodium sulfide solution to be 6mol/L, and mixing the solution and the dried household garbage incineration fly ash according to a liquid-solid ratio of 2 mL:1g of the mixture is stirred for 5min in a stirrer with the rotating speed of 50 r/min. Then regulating the microwave power to 1000W, and carrying out microwave heating on the uniformly stirred mixture for 10min at the temperature of 125 ℃ to prepare the zeolite. Ni is added to the mixture with the concentration of 100mol/L2+Adjusting the pH value of the wastewater in the laboratory to 7, adding 4ml/g of zeolite, oscillating horizontally and reciprocally at a constant temperature of 150r/min for 120min at room temperature until the adsorption is balanced, filtering and separating the adsorbed zeolite and the wastewater to remove heavy metals in the wastewater, and adsorbing Ni in the wastewater2+The removal rate is 97.67%, and the zeolite saturated in adsorption is repeatedly washed by 1mol/L sodium chloride solution and then dried to constant weight at 60 ℃ for recycling, and can be used for 6 times.
In the case of example 2, the following examples,
drying the medical waste incineration fly ash at 110 ℃ for 6h, then adjusting the concentration of a sodium sulfide solution to be 5mol/L, and stirring the sodium sulfide solution and the dried medical waste incineration fly ash in a stirrer with the rotating speed of 40r/min for 10min according to the liquid-solid ratio of 3mL to 1 g. Regulating microwave power to 1200W, and heating the uniformly stirred mixture at 150 deg.C for 20min to obtain zeolite. Cr is added with the concentration of 25mol/L6+Electroplating wastewater ofAdjusting the pH value of the wastewater to be 7, adding 3ml/g of zeolite into the wastewater, oscillating horizontally for 60min at a constant temperature of 180r/min at room temperature until the adsorption is balanced, then settling and separating the adsorbed zeolite from the wastewater to remove heavy metals in the wastewater, and adsorbing Cr in the wastewater6+The removal rate is 95.37%, and the zeolite saturated in adsorption can be used as a building material.
In the case of example 3, the following example was carried out,
drying the household garbage incineration fly ash at the temperature of 110 ℃ for 1h, then adjusting the concentration of a sodium sulfide solution to be 3mol/L, and stirring the sodium sulfide solution and the dried household garbage incineration fly ash in a stirrer with the rotating speed of 50r/min for 8min according to the liquid-solid ratio of 3mL to 1 g. Regulating microwave power to 1000W, and microwave heating the uniformly stirred mixture at 125 deg.C for 20min to obtain zeolite. Hg is contained in the solution with the concentration of 1mol/L2+Adjusting the pH value of the electroplating wastewater to 7, adding 12ml/g of zeolite into the wastewater, oscillating horizontally and reciprocally at a constant temperature of 200r/min for 60min at room temperature until the adsorption is balanced, settling and separating the adsorbed zeolite from the wastewater to remove heavy metals in the wastewater, and adsorbing Hg in the wastewater2+The removal rate is 94.53%, and the zeolite with saturated adsorption can be used as a building material.
In the case of the example 4, the following example,
drying the medical waste incineration fly ash at 110 ℃ for 6h, then adjusting the concentration of a sodium sulfide solution to be 1mol/L, and stirring the sodium sulfide solution and the dried medical waste incineration fly ash for 2min in a stirrer with the rotating speed of 60r/min according to the liquid-solid ratio of 1mL to 1 g. Regulating microwave power to 800W, and heating the uniformly stirred mixture at 100 deg.C for 18min to obtain zeolite. Cr is added with the concentration of 25mol/L6+The pH value of the electroplating wastewater is adjusted to 4, then 3ml/g zeolite is added into the wastewater, the wastewater is subjected to constant-temperature rotary oscillation for 50min at the oscillation rate of 220r/min at the room temperature until the adsorption is balanced, then the adsorbed zeolite is separated from the wastewater through sedimentation to remove heavy metals in the wastewater, the adsorbed saturated zeolite is repeatedly cleaned by 0.5mol/L sodium chloride solution and dried at 55 ℃ until the heavy metals are removedConstant weight for recycling.
In the case of example 5, the following examples were carried out,
drying the household garbage incineration fly ash at 105 ℃ for 4h, then adjusting the concentration of a sodium sulfide solution to be 6mol/L, and mixing the solution and the dried household garbage incineration fly ash according to a liquid-solid ratio of 2 mL:1g of the mixture is stirred for 5min in a stirrer with the rotating speed of 30 r/min. Then regulating the microwave power to 1000W, and carrying out microwave heating on the uniformly stirred mixture for 10min at the temperature of 200 ℃ to prepare the zeolite. Ni is added to the mixture with the concentration of 100mol/L2+Adjusting the pH value of the wastewater in the laboratory to 8, adding 4ml/g of zeolite, oscillating horizontally and reciprocally at a constant temperature of 100r/min for 200min at room temperature until the adsorption is balanced, filtering and separating the adsorbed zeolite from the wastewater to remove heavy metals in the wastewater, repeatedly cleaning the adsorbed saturated zeolite with 3mol/L sodium chloride solution, and drying the zeolite at 65 ℃ to a constant weight for recycling.
Claims (2)
1. A method for carrying out resource treatment on incineration fly ash to adsorb heavy metals in wastewater is characterized by comprising the following steps:
step 1, mixing 1-6 mol/L sodium sulfide solution and dried incineration fly ash in a liquid-solid ratio of (1-3) mL:1g of the fly ash is uniformly mixed to obtain a mixed system, the drying temperature of the drying treatment is 100-110 ℃, the drying time is 1-6 h, and the incineration fly ash is one or two of domestic garbage incineration fly ash and medical waste incineration fly ash;
step 2, performing microwave heating treatment on the mixed system at 100-200 ℃, wherein the microwave power is 800-1200W, the heating time is 10-20 min, so as to obtain a reaction liquid containing zeolite, and separating and drying the zeolite in the reaction liquid to obtain zeolite;
step 3, adjusting the pH value of the wastewater containing heavy metals to 4-8 by using a sodium hydroxide solution or dilute nitric acid, soaking zeolite in the wastewater containing heavy metals and having a pH value of 4-8, wherein the liquid-solid ratio of the wastewater to the zeolite is 3-12 ml/g, performing constant-temperature horizontal reciprocating type oscillation adsorption or constant-temperature rotary oscillation adsorption at room temperature, wherein the oscillation rate is 100-220 r/min, the adsorption time is 50-200 min, and separating the adsorbed zeolite from the adsorbed wastewater;
and 4, cleaning the adsorbed zeolite by using a sodium chloride solution with the concentration of 0.5-3 mol/L, filtering the zeolite after the sodium chloride treatment, drying the zeolite obtained by filtering at 55-65 ℃, and continuously recycling according to the step 3 to complete the removal of heavy metals in the wastewater.
2. The method for carrying out resource treatment on incineration fly ash to adsorb heavy metals in wastewater according to claim 1, characterized in that in step 1, the sodium sulfide solution and the incineration fly ash after drying treatment are stirred for 2-10 min at a rotation speed of 30-60 r/min to obtain a mixed system.
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