CN115254923B - Method for preparing high-purity calcium sulfate from waste incineration fly ash - Google Patents
Method for preparing high-purity calcium sulfate from waste incineration fly ash Download PDFInfo
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- CN115254923B CN115254923B CN202210930643.0A CN202210930643A CN115254923B CN 115254923 B CN115254923 B CN 115254923B CN 202210930643 A CN202210930643 A CN 202210930643A CN 115254923 B CN115254923 B CN 115254923B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/70—Chemical treatment, e.g. pH adjustment or oxidation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/30—Destroying solid waste or transforming solid waste into something useful or harmless involving mechanical treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/46—Sulfates
- C01F11/468—Purification of calcium sulfates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B2101/00—Type of solid waste
- B09B2101/30—Incineration ashes
Abstract
The utility model provides a method for preparing high-purity calcium sulfate from waste incineration fly ash, and belongs to the technical field of harmless and recycling treatment of waste incineration fly ash. The utility model prepares the high-purity anhydrous calcium sulfate with wide application through the waste incineration fly ash, and the waste incineration fly ash realizes the purpose of preparing the high-purity calcium sulfate through the procedures of dioxin detoxification, water washing, heavy metal removal, impurity removal, rinsing, pH adjustment and the like. The high-purity anhydrous calcium sulfate product prepared by the method has the calcium sulfate content reaching more than 95 percent and wide industrial application.
Description
Technical Field
The utility model relates to a method for preparing high-purity calcium sulfate from waste fly ash, belonging to the technical field of harmless and recycling treatment of household garbage incineration fly ash.
Background
As the main stream of the household garbage disposal is gradually transferred from sanitary landfill to garbage incineration, the household garbage incineration fly ash becomes an important pollutant. The fly ash from incineration of household garbage refers to the residue obtained by the collection of the household garbage incineration power plant in a flue gas purification system, and contains organic pollutants such as benzene series, dioxin and the like, trace heavy metals such as Pb, cr and the like. According to the domestic garbage incineration pollution control Standard (GB 18085-2014) provision is made: "fly ash from incineration of household garbage should be managed according to dangerous waste". Therefore, fly ash must be collected separately, and must not be mixed with household garbage, incineration residues, etc., nor with other hazardous wastes.
According to the technical specification (trial) of the pollution control of the fly ash of the incineration of the household garbage (HJ 1134-2020), the fly ash of the incineration of the household garbage is prevented from polluting the environment during the processes of collection, storage, transportation, treatment and disposal. The fly ash treatment method comprises water washing, solidification/stabilization, shaping, low-temperature pyrolysis, high-temperature sintering, high-temperature melting and the like, and the pollution control of the fly ash and the treatment product thereof in the utilization process meets the requirements of the solid waste recycling pollution control technical guidelines (HJ 1091-2020) and the comprehensive sewage discharge standard (GB 8978-2002).
The components with higher content in the fly ash comprise: the traditional water washing method is to wash out soluble chloride ions, then add sodium carbonate to remove calcium ions, and the decalcified solution enters an evaporator to be evaporated and crystallized to obtain industrial sodium chloride and potassium chloride, while sodium sulfate or calcium sulfate is always in evaporation mother liquor, and meanwhile, calcium sulfate crystallization has the characteristics of easy scaling, difficult cleaning and the like, and the calcium sulfate can be used as gypsum board or mixed material.
The fly ash with high calcium sulfate content enters a cement kiln for cooperative treatment, so that the setting strength of cement clinker is reduced, the grade of subsequent cement products is reduced, and the strength and stability of cement are greatly reduced.
Chinese patent 202110228506.8 describes a method for recovering lithium from lithium iron phosphate cathode material by using waste incineration fly ash. The patent utilizes the characteristic of high chlorine content of the waste incineration fly ash, utilizes the reaction of the electrolysis product of chlorine in the waste incineration fly ash and the lithium iron phosphate cathode material powder to promote the dissolution of lithium ions in the lithium iron phosphate cathode material powder, and realizes the high-efficiency separation of lithium, chlorine, phosphorus and iron through the second electrolytic tank. Patent describes that more than 96% of lithium in the lithium iron cathode material powder can be recovered. In practice, the electrolytic system is not operated stably because the sodium chloride/potassium chloride solution contains more than 50mg/kg of TOC.
Chinese patent 202122805952.9 describes a recycling method of waste incineration fly ash, which finally realizes the efficient energy-saving treatment of the waste incineration fly ash through a granulator, a mixer and a smelting furnace, and realizes the reduction, harmless and recycling of the waste incineration fly ash by preparing heat-insulating cotton through melting and solidifying the fly ash. The technology does not consider the technical specifications of the ecological environmental protection department, and the fly ash can be recycled and harmless only by achieving the aim of pretreatment.
The Chinese patent 202210076178.9 describes a water washing desalting device and method for the meeting of household garbage incineration, which mainly adopts a filtering tank to carry out solid-liquid separation. It is not described for high chlorine ash.
Chinese patent 202010222818.3 discloses a high-efficiency dechlorination agent and a dechlorination method for waste incineration fly ash, wherein the dechlorination agent adopts a mixed material of nitrate, phosphoric acid and organic acid to dechlorinate, and the quality of crystalline salt and the organic content of condensate are affected by the organic matter and the nitrate. The electrochemical dechlorination is adopted, the electrode types and dechlorination effects are not effectively described, and the effective description of fly ash recycling is lacked.
The Chinese literature discusses a liquid to ash ratio of 6: under the condition of 1, the secondary countercurrent rinsing is adopted to clean the waste incineration fly ash of the fire grate, the final chlorine ion content can only be cleaned to 1.7%, and meanwhile, the recycling of effective resources except sodium chloride and potassium chloride in the waste incineration fly ash is lacked, so that the method is a conventional treatment method. Meanwhile, the liquid-ash ratio reaches 6:1, the water consumption is higher, and the energy consumption [ Wang Yuting, shang Minghui, zong Da and the like of the subsequent solid-liquid separation are increased; secondary countercurrent washing characteristic of fly ash from incineration of fire grate refuse [ J ]. University of Zhejiang, industrial edition, 2019,53 (5): 981-987.
Therefore, the prior art lacks a method for recycling high-purity calcium sulfate by utilizing the fly ash of the household garbage, which is simple and effective in operation and low in cost.
Disclosure of Invention
Aiming at the problems in the prior art, the utility model provides a method for preparing high-purity calcium sulfate by using waste incineration fly ash, which creatively recycles impurity calcium sulfate in the process of countercurrent rinsing and dechlorination of the fly ash by knowing the chemical substance characteristics in the water washing process of the waste incineration fly ash and combining the sulfur content requirement of the cement clinker prepared by a subsequent cement kiln according to the characteristics of the household waste incineration fly ash. The solubility of the calcium sulfate is more than 0.72% under the condition of high-concentration chlorine content, so that the preparation of high-purity calcium sulfate by recycling the calcium sulfate in the solution and utilizing the calcium hydroxide in the ash has technical feasibility and innovation. The utility model utilizes the waste incineration fly ash to recycle the product which is widely applied, namely calcium sulfate, and the solid waste recycling technology has wide application prospect.
In order to achieve the technical purpose, the technical scheme of the utility model is as follows.
In one aspect, the utility model provides a method for preparing high-purity calcium sulfate from waste incineration fly ash, which is characterized by comprising the following steps:
(1) The waste incineration fly ash enters a three-stage countercurrent rinsing device after passing through a dioxin cracking device, so that sulfate radical in the fly ash is dissolved into primary pressure filtrate to the maximum extent;
(2) Adding ferrous sulfate and sodium sulfide into the primary pressure filtrate obtained in the step (1) to remove heavy metal ions in the solution; press-filtering by a plate frame to obtain filtrate; adding anhydrous sodium sulfate into the filtrate after plate-frame filter pressing, fully stirring, adopting plate-frame filter pressing to perform solid-liquid separation, and returning supernatant to fly ash water washing;
(3) And (3) adding deionized water into the coarse-grade calcium sulfate crystals to mix, regulating the pH value to 4-4.5 by using sulfuric acid, carrying out solid-liquid separation by adopting plate-frame filter pressing, washing the solid subjected to the plate-frame filter pressing by using deionized water, regulating the pH value of supernatant to 7-7.5 by using sodium hydroxide, carrying out solid-liquid separation by using a plate-frame filter press, and drying to obtain the high-purity anhydrous calcium sulfate.
Further, the dioxin cracker may be a known conventional dioxin cracker, for example, the ash-degrading dioxin unit in CN 202010426670.5.
Further, the three-stage countercurrent rinse device may be a known conventional three-stage countercurrent rinse device, for example, a three-stage countercurrent cleaning system in CN 201810388415.9. Further, clear liquid obtained after the third-stage rinsing fly ash is subjected to filter pressing by a filter press enters a second-stage rinsing tank, and filter pressing liquid obtained after the second-stage rinsing fly ash is subjected to filter pressing by the filter press enters a first-stage rinsing tank; and (5) primary rinsing to obtain primary pressure filtrate.
Further, the concentration of dioxin in the fly ash after the cracking of the dioxin in the step (1) is less than 50ng-TEQ/kg, and the chlorine content is less than 1%.
Further, the adding concentration of the sodium sulfide is 20-100 mg/L, and the sodium sulfide is used for removing amphoteric lead, zinc, nickel, chromium ions and/or organic mercury in the solution. Further, the adding concentration of the sodium sulfide is 50-60 mg/L.
Further, the ferrous sulfate heptahydrate with the adding concentration of 100-350 mg/L is used for removing redundant sulfur ions. Further, the adding concentration of the sodium sulfide is 230-270 mg/L.
Further, the concentration of the residual calcium ions in the press filtrate is more than 2000mg/L, so that the calcium ions can be efficiently removed, and stable calcium sulfate crystals can be generated.
Further, the coarse-grade calcium sulfate crystals in the step (3) are dissolved by deionized water, and the dilution ratio is 1:1, the pH value is regulated to 4 to 4.5 by 3 to 5mol/L of high-purity sulfuric acid, so that partial metal oxide without calcium sulfate can be dissolved into supernatant fluid, and the purity of the calcium sulfate is increased.
Further, the mixed solution formed after the pH is adjusted is subjected to solid-liquid separation to obtain relatively high-purity calcium sulfate crystals.
Still further, the relatively high purity calcium sulfate crystals are produced by passing deionized water 1:1, adding 3-5 mol/L sodium hydroxide to adjust the pH value to 7-7.5, fully stirring and reacting, and carrying out solid-liquid separation by adopting plate-frame filter pressing again to obtain the high-purity calcium sulfate containing water.
Further, the high-purity anhydrous calcium sulfate with the content higher than 95% is obtained after the high-purity calcium sulfate is dried at high temperature; if the purity is less than 95%, repeating the step of the step (3) until the purity is higher than 95%.
From the above description, it can be seen that the present utility model has the following advantages:
1. the method of the utility model utilizes the household garbage incineration fly ash with wide sources and stable yield to prepare the high-purity calcium sulfate, and has the obvious purpose of treating waste with waste and changing waste into valuable.
2. The method reduces the sulfate content in the fly ash and improves the quality of clinker in the cement kiln.
3. The method adopted by the utility model not only can obtain high-purity calcium sulfate, but also can reduce the adding amount of sodium carbonate in the waste incineration fly ash water washing process, and has remarkable economy.
4. The utility model can meet the related requirements of the technical specification (trial) of the pollution control of the fly ash of the incineration of the household garbage (HJ 1134-2020), the concentration of the dioxin after treatment is less than 50ng-TEQ/kg, and the chlorine content is less than 1%;
5. the utility model ensures the stable operation of the whole flow system by whole-course continuous feeding and continuous discharging.
6. The method has simple operation and strong adaptability, and can meet the fly ash treatment requirements of different scales and different sulfate contents.
7. The utility model reduces the sulfate content in the waste incineration fly ash for problem identification, and systematically provides a method for solving the problems.
8. The utility model adopts a simple treatment method, combines the dissolution promoting effect and the ion coprecipitation principle under the condition of high salt content, saves the operation cost to the maximum extent, and simultaneously provides a new solution idea.
Drawings
FIG. 1 is a schematic process diagram of a method for preparing high purity calcium sulfate from waste incineration fly ash according to the present utility model;
Detailed Description
The following examples further illustrate the features of the present utility model, but are not intended to limit the scope of the utility model in any way.
Example 1
A method for preparing high-purity calcium sulfate from waste incineration fly ash comprises the following steps:
(1) The waste incineration fly ash passes through a dioxin cracking device until the concentration of dioxin is less than 50ng-TEQ/kg and the chlorine content is less than 1%, and then enters a three-stage countercurrent rinsing device, so that sulfate radical in the fly ash is dissolved into primary pressure filtrate to the greatest extent;
(2) Adding 20-100 mg/L ferrous sulfate and 100-350 mg/L sodium sulfide into the primary pressure filtrate obtained in the step (1) to remove heavy metal ions in the solution; press-filtering by a plate frame to obtain filtrate; adding anhydrous sodium sulfate into the filtrate after plate-frame filter pressing, fully stirring, adopting plate-frame filter pressing to perform solid-liquid separation, and returning supernatant to fly ash water washing;
(3) And (3) adding deionized water into the coarse-grade calcium sulfate crystals to mix, regulating the pH value to 4-4.5 by using sulfuric acid, carrying out solid-liquid separation by adopting plate-frame filter pressing, washing the solid subjected to the plate-frame filter pressing by using deionized water, regulating the pH value of supernatant to 7-7.5 by using sodium hydroxide, carrying out solid-liquid separation by using a plate-frame filter press, and drying to obtain the high-purity anhydrous calcium sulfate.
The process schematic diagram of the preparation of high-purity calcium sulfate by utilizing the waste incineration fly ash is shown in figure 1.
Example 2
For the fly ash of a self-provided incineration plant of a certain market company of Jiangsu Nantong, the sulfate content in the fly ash is 0.8 percent, the fly ash is treated by the method of the embodiment 1, wherein 50mg/L of sodium sulfide and 250mg/L of ferrous sulfate (one-stage solid-liquid separation) are added, the addition amount of anhydrous sulfuric acid is 7.1g/L, the sulfuric acid is configured to be 3.5mol/L, the pH value is regulated to 4.35, the concentration of sodium hydroxide is configured to be 3.5mol/L, the pH value is regulated to be=7 (two-stage solid-liquid separation), and the purity of calcium sulfate crystals obtained by the two-stage solid-liquid separation reaches 98.2 percent.
Example 3
For the fly ash of the self-provided incineration plant of Jiaxing Zhejiang, the sulfate content in the fly ash is 0.72 percent, the fly ash is treated by the method of the embodiment 1, wherein 60mg/L of sodium sulfide, 250mg/L of ferrous sulfate and 8.5g/L of anhydrous sulfuric acid are added, the sulfuric acid is configured to be 3.5mol/L, the pH value is adjusted to be 4.35, the concentration of sodium hydroxide is configured to be 3.5mol/L, the pH value is adjusted to be 7, and the purity of the obtained calcium sulfate crystal reaches 98.5 percent. At the same time, the sulfate ion entering the evaporator was reduced from 5600mg/L to 3400mg/L.
Example 4
For a fly ash treatment line in Zhejiang, the influence of scaling of calcium sulfate on the evaporator is reduced by reducing the concentration of sulfate ions entering the evaporator after treatment by the method of the embodiment 1. The discharge amount of the evaporation mother liquor is reduced from 1% to 0.75%.
Example 5
According to the method provided by the utility model, 150kg of sodium carbonate is needed to be added per ton of fly ash, the carbonate amount for removing calcium is reduced to 100 kg/ton of fly ash through the sulfate coprecipitation, the cost of 50kg of calcium carbonate per ton of fly ash is saved, the unit price of the calcium carbonate is 4000 yuan/ton, the cost of 200 yuan/ton of ash is saved, and the cost is 40000 yuan/ton of ash is converted into the cost of 40000 yuan per day. According to 330 days of the year, the cost is saved by 1320 ten thousand yuan, and the obvious economic benefit is embodied. And high-purity anhydrous calcium sulfate with wide application is also recovered.
It is to be understood that the foregoing detailed description of the utility model is merely illustrative of the utility model and is not limited to the embodiments of the utility model. It will be understood by those of ordinary skill in the art that the present utility model may be modified or substituted for elements thereof to achieve the same technical effects; as long as the use requirement is met, the utility model is within the protection scope of the utility model.
Claims (7)
1. The method for preparing high-purity calcium sulfate by using the waste incineration fly ash is characterized by comprising the following steps of:
(1) After the waste incineration fly ash passes through a dioxin cracking device, the waste incineration fly ash enters a three-stage countercurrent rinsing device, sulfate radical in the fly ash is dissolved into primary pressure filtrate, the concentration of dioxin in the fly ash after the dioxin cracking in the step (1) is less than 50ng-TEQ/kg, and the chlorine content is less than 1%;
(2) Adding ferrous sulfate and sodium sulfide into the primary pressure filtrate obtained in the step (1) to remove heavy metal ions in the solution; press-filtering by a plate frame to obtain filtrate; adding anhydrous sodium sulfate into the filtrate after plate-frame filter pressing, fully stirring, adopting plate-frame filter pressing to perform solid-liquid separation, and returning supernatant to fly ash water washing; the adding concentration of the sodium sulfide is 20-100 mg/L, and the adding concentration of the ferrous sulfate is 100-350 mg/L of ferrous sulfate heptahydrate;
(3) And (3) adding deionized water into the coarse-grade calcium sulfate crystals obtained in the step (2), mixing, adjusting the pH value to 4-4.5, performing solid-liquid separation by adopting plate-frame filter pressing, washing the solid subjected to the plate-frame filter pressing by using deionized water, adjusting the pH value of the supernatant to 7-7.5, performing solid-liquid separation by adopting a plate-frame filter press, and drying to obtain the high-purity anhydrous calcium sulfate.
2. The method of claim 1, wherein the concentration of residual calcium ions in the press filtrate is greater than 2000mg/L.
3. The method of claim 1, wherein the coarse-scale calcium sulfate crystals in step (3) are dissolved in deionized water at a dilution ratio of 1:1, the pH value is regulated to 4 to 4.5 by 3 to 5mol/L of high-purity sulfuric acid.
4. A method according to claim 3, wherein the mixed liquor formed after pH adjustment is subjected to solid-liquid separation to obtain relatively high purity calcium sulfate crystals.
5. The method of claim 4, wherein the relatively high purity calcium sulfate crystals are produced by passing deionized water 1:1, adding 3-5 mol/L sodium hydroxide to adjust the pH value to 7-7.5, fully stirring and reacting, and carrying out solid-liquid separation by adopting plate-frame filter pressing again to obtain the high-purity calcium sulfate containing water.
6. The method according to claim 5, wherein the high purity calcium sulfate is dried at high temperature to obtain high purity anhydrous calcium sulfate with a content of more than 95%; if the purity is less than 95%, repeating the step of the step (3) until the purity is higher than 95%.
7. The method of any one of claims 1-6, wherein the fly ash is derived from household waste incineration fly ash.
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| CN204122439U (en) * | 2014-07-30 | 2015-01-28 | 富阳鹿山双龙化工有限公司 | For the city garbage burning flying ash resource pretreatment system of cement producting material |
| CN109575880B (en) * | 2018-11-01 | 2021-07-02 | 杭州秀澈环保科技有限公司 | Method for preparing I-type snow melting agent by utilizing garbage fly ash |
| CN109264898A (en) * | 2018-11-27 | 2019-01-25 | 上海电气集团股份有限公司 | A kind of flying dust multistage dechlorination and water lotion decalcification softening process and its system |
| CN110238157A (en) * | 2019-05-21 | 2019-09-17 | 浙江大学 | A kind of method and system of the dechlorination of flying dust depth and recycling modification |
| CN111533156A (en) * | 2020-05-09 | 2020-08-14 | 广东飞南资源利用股份有限公司 | Treatment process of incineration fly ash and treatment process of incineration ash |
| CN112090018A (en) * | 2020-08-27 | 2020-12-18 | 北京金隅琉水环保科技有限公司 | Process for treating fly ash by using purified waste acid |
| CN112775145A (en) * | 2020-12-22 | 2021-05-11 | 江山市虎鼎环保科技有限公司 | Efficient secondary washing process for household garbage incineration fly ash |
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