CN113955954A - Carbon dioxide high-pressure leaching decalcification process for fly ash - Google Patents
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- CN113955954A CN113955954A CN202111012141.1A CN202111012141A CN113955954A CN 113955954 A CN113955954 A CN 113955954A CN 202111012141 A CN202111012141 A CN 202111012141A CN 113955954 A CN113955954 A CN 113955954A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
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- C04B2/02—Lime
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0219—Fixed bed of solid material
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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
- C01F11/18—Carbonates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/00—Solvent extraction
- B01D2011/005—Co-current extraction
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P20/50—Improvements relating to the production of bulk chemicals
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
A fly ash carbon dioxide high pressure leaching decalcification process comprises the following steps: firstly, preparing slurry by washing fly ash with water, and performing suction filtration on the prepared slurry to obtain washing liquid and solid slag; secondly, washing the solid slag to prepare slurry, and converting calcium contained in the solid slag into calcium bicarbonate to be dissolved in water by adopting high-pressure carbon dioxide leaching; thirdly, carrying out suction filtration on the slurry subjected to high-pressure carbon dioxide leaching to obtain residual solid slag and water washing liquid, and decomposing calcium bicarbonate in the water washing liquid at normal temperature and normal pressure to generate calcium carbonate; and fourthly, calcining the calcium carbonate obtained in the third step to obtain quicklime and carbon dioxide gas, and reusing the carbon dioxide gas in the carbon dioxide high-pressure leaching stage in the second step. The method adopts a carbon dioxide high-pressure leaching mode to separate calcium carbonate from the solid slag after the washing of the fly ash, is more convenient than a cement kiln synergistic process, and can recycle the carbon dioxide for the washing of the fly ash and the carbon dioxide high-pressure leaching stage when the calcium carbonate is calcined.
Description
Technical Field
The invention belongs to the technical field of harmless treatment of fly ash generated by waste incineration, and particularly relates to a carbon dioxide high-pressure leaching decalcification process for fly ash.
Background
The fly ash is the residue collected in a flue gas purification system (APC) and a heat recovery system (such as an economizer, a boiler and the like), accounts for about 20 percent of the total quantity of the ash residue generated in the waste incineration, is the substance collected by a flue gas dust remover after the household waste incineration, and the waste incineration industry is explosively increased along with the increase of the clearing quantity of the household waste and the increase of the incineration treatment proportion. By the end of 2020, the total incineration amount of the garbage reaches 59.14 ten thousand tons/day, in the process of garbage incineration, a lot of harmful substances, such as dioxin, acid gases (such as hydrogen chloride and sulfur dioxide), nitrogen oxides, heavy metal dust and the like, can be generated, most of the pollutants can be intercepted by a dust removal system to form fly ash when flue gas purification is carried out, and the fly ash amount generated every year is about 1000 ten thousand tons. The large and medium-sized urban fly ash has large production amount and tense land resources, the disposal mode mainly based on landfill is under greater and greater pressure, and the reclamation, reduction and harmless treatment of the waste incineration fly ash are the final trends. Therefore, how to reasonably utilize the fly ash and realize the reutilization of the waste resources is urgent.
It is clear that the 'domestic waste incineration fly ash' belongs to dangerous waste when the 'national hazardous waste record' is revised in 2008, and the hazardous waste category is HW 18. The main components of the waste incineration fly ash can be roughly divided into three categories: water-soluble salts (sodium salt, potassium salt, etc. in a proportion of about 30%), calcium components (calcium oxide, calcium carbonate, etc. in a proportion of more than 56%), and others (heavy metals, silicon, phosphates, dioxins, etc. in a proportion of about 14%). Once the fly ash is discharged into the environment, the fly ash can cause serious pollution and damage to water, air and soil, meanwhile, heavy metals and dioxin can cause great harm to the environment and organisms, and although water-soluble sodium salt, potassium salt and calcium salt have no toxicity, the existence of the water-soluble salt can cause great harm to the harmless and resource treatment of the fly ash.
The most widely applied fly ash recycling process is a cement kiln co-processing technology, but the co-processing cost is higher. The product operation of the cement enterprises is greatly influenced by the market, and the cooperative disposal of the household garbage can increase the land and investment of the cement enterprises, increase the product cost and influence the normal production of the cement products. Meanwhile, cement enterprises are far away from household garbage collection facilities, and the transportation cost is high.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a carbon dioxide high-pressure leaching decalcification process for fly ash, which mainly solves the technical problem that the prior cement kiln needs to utilize a third-party cement plant production line in cooperation, the additional cost is increased by the cooperation treatment of the fly ash, and the energy consumption and the operation cost cannot be further saved although hazardous waste is harmlessly treated.
In order to solve the technical problems, the invention provides a carbon dioxide high-pressure leaching decalcification process for fly ash, which comprises the following steps:
step one, preparing slurry by washing fly ash, and then carrying out suction filtration on the prepared slurry by using a suction filtration machine to obtain washing liquid and solid slag;
step two, washing the solid slag to prepare slurry, placing the prepared slurry in a high-pressure container, introducing excessive carbon dioxide gas into the slurry, and converting calcium contained in the solid slag into calcium bicarbonate to be dissolved in water by adopting high-pressure carbon dioxide leaching;
step three, continuously introducing carbon dioxide to separate out the liquid in the high-pressure reaction kettle, wherein the separated liquid is a calcium bicarbonate aqueous solution, calcium bicarbonate is decomposed under normal pressure to generate calcium carbonate, and the calcium bicarbonate aqueous solution can also be heated to accelerate the decomposition of calcium bicarbonate to generate calcium carbonate;
and step four, calcining the calcium carbonate obtained in the step three to obtain quicklime and carbon dioxide gas, and reusing the carbon dioxide gas in the carbon dioxide high-pressure leaching stage in the step two.
Preferably: firstly, preparing slurry by washing fly ash, and introducing carbon dioxide gas into the slurry to adjust the pH value to 6-8; and simultaneously recycling the carbon dioxide gas obtained in the fourth step for adjusting the pH value of the slurry.
Preferably: harmless recycling is carried out on the water washing liquid obtained in the step one, heavy metal elements in the water washing liquid are removed firstly, calcium ions and magnesium ions in the water washing liquid are removed to reduce the hardness of the water washing liquid, and finally, the residual water washing liquid is subjected to evaporative crystallization to obtain potassium salt and sodium salt.
Compared with the prior art, the invention has the following advantages:
1. in the washing process of the fly ash, carbon dioxide gas is adopted to adjust the pH value of the fly ash slurry, so that heavy metal and calcium ion precipitation are increased, the washing efficiency can be improved, and the cost is low;
2. calcium carbonate is separated by adopting a carbon dioxide high-pressure leaching mode, calcined calcium carbonate is generated, the process is more convenient than a cement kiln synergistic process, and carbon dioxide can be recycled in the calcining process and can be used in a fly ash water washing pulping stage and a carbon dioxide high-pressure leaching stage;
3. the calcined quicklime can be added with water to generate calcium hydroxide, and can be used in the flue gas purification stage of a waste incineration plant, so that a closed loop with maximized resource utilization is formed in the whole system of waste incineration power generation, flue gas purification and fly ash water washing.
Drawings
FIG. 1 is a flow chart of the overall process for fly ash decalcification.
Detailed Description
The present invention provides a fly ash carbon dioxide high pressure leaching decalcification process, which is further described with reference to the preferred embodiment and the attached figure 1.
As shown in figure 1, the invention provides a fly ash carbon dioxide high-pressure leaching decalcification process, which is to wash fly ash with water to prepare slurry, introduce carbon dioxide gas into the fly ash water washing slurry to adjust the pH value to 6-8, which is favorable for heavy metal and calcium ion precipitation, then carry out suction filtration to obtain water washing liquid and solid slag, wherein the water washing liquid is subjected to resource treatment of sequentially removing heavy metal, calcium and magnesium, and evaporating, crystallizing and extracting potassium salt and sodium salt; preparing slurry from filter cakes, namely solid residues generated after washing fly ash water according to a solid-to-liquid ratio of 1: 1-50, introducing excessive carbon dioxide, improving the solubility of the carbon dioxide under high pressure, converting calcium in the solid residues into calcium bicarbonate by adopting a high-pressure leaching mode, dissolving the calcium bicarbonate into water washing liquid, so as to realize decalcification, calcium bicarbonate in the water washing liquid can be decomposed into calcium carbonate at normal temperature and normal pressure, the obtained calcium carbonate is calcined to generate quicklime, and meanwhile, carbon dioxide gas generated in the calcium carbonate calcining process is collected, the carbon dioxide can be reused in the fly ash washing step to adjust the pH value, and can also be reused in the carbon dioxide high-pressure leaching stage, so that the material consumption in the fly ash recycling process is saved, and finally calcium hydroxide obtained by adding water into quick lime is reused in the flue gas purification stage of a waste incineration plant, so that the whole system of waste incineration power generation, flue gas purification and fly ash washing forms a closed loop.
As mentioned above, the invention can realize rapid and thorough decalcification treatment of fly ash, and recovery of calcium in fly ash, compared with conventional cement kiln collaborative process, the cement kiln needs to utilize a third party cement plant production line in collaboration, the process can be completed independently, leaching is carried out by high pressure carbon dioxide to obtain calcium carbonate, calcium carbonate is calcined to obtain lime, carbon dioxide in the calcining process is collected and can be reused in the stages of fly ash water washing and high pressure leaching, and finally calcium hydroxide is obtained by adding water into quick lime, so that the process can be used in the flue gas purification stage of a waste incineration plant, and a closed loop on the process is formed.
Example 1, as shown in fig. 1, it comprises the following steps:
step one, preparing slurry by washing fly ash, introducing carbon dioxide gas into the slurry to adjust the pH value to 6-8, and then carrying out suction filtration on the prepared slurry by using a suction filtration machine to obtain washing liquid and solid slag; the water washing liquid is subjected to harmless and recycling treatment, heavy metal elements in the water washing liquid are removed firstly, calcium ions and magnesium ions in the water washing liquid are removed to reduce the hardness of the water washing liquid, and finally the remaining water washing liquid is subjected to evaporative crystallization to obtain potassium salt and sodium salt, wherein the method specifically comprises the following steps: adding a chelating agent into the water washing solution to remove heavy metals contained in the water washing solution to obtain heavy metal residues and primary detergentDissolving the liquid; adding NaOH into the obtained primary purified liquid to adjust the pH value to 12, and then introducing CO2Obtaining mixed slag of calcium carbonate and magnesium hydroxide, mixing the mixed slag of calcium carbonate and magnesium hydroxide and secondary purifying liquid; evaporating and crystallizing the secondary purifying liquid through an MVR evaporator, cooling and crystallizing to obtain potassium salt, and obtaining potassium salt and mixed salt waste liquid through centrifugal separation, wherein the secondary purifying liquid is mainly potassium salt and sodium salt, the solubility of sodium chloride is small along with the change of temperature, and the solubility of sodium chloride is smaller than that of potassium chloride when the temperature is high, so that the secondary purifying liquid is evaporated and crystallized through the MVR evaporator, the potassium salt can be recovered through cooling and crystallizing, and the sodium chloride is mainly contained in the remaining mixed waste liquid; electrolyzing the mixed salt waste liquid to obtain NaOH and chlorine;
step two, preparing slurry from the solid residues according to a solid-liquid ratio of 1: 1-10, placing the prepared slurry in a high-pressure container, setting the pressure of a high-pressure reaction kettle to be 0.6-1MPa, stirring at a speed of 400r/min, introducing excessive carbon dioxide gas into the slurry for reaction for 1-2 hours, converting calcium contained in the solid residues into calcium bicarbonate by adopting high-pressure carbon dioxide leaching, dissolving the calcium bicarbonate in water, and leaching for multiple times according to a decalcification effect;
and step three, continuously introducing carbon dioxide to separate out the liquid in the high-pressure reaction kettle, wherein the separated liquid is a calcium bicarbonate aqueous solution, calcium bicarbonate is decomposed under normal pressure to generate calcium carbonate, and the calcium bicarbonate aqueous solution can also be heated to accelerate the decomposition of calcium bicarbonate to generate calcium carbonate.
And step four, calcining the calcium carbonate obtained in the step three to obtain quicklime and carbon dioxide gas, wherein the carbon dioxide gas can be simultaneously recycled for adjusting the pH value of the slurry in the step one and for the carbon dioxide high-pressure leaching stage in the step two.
Example 2, which comprises the steps of:
step one, adopting a multi-stage reverse pulping fly ash washing mode,
1) mixing fly ash and water according to the proportion of 1: 3-5, preparing slurry, and introducing carbon dioxide gas into the slurry to adjust the pH value to 6-8;
2) carrying out suction filtration on the slurry prepared in the step 1) by using a suction filter to obtain high-concentration water washing liquid and solid residues;
3) mixing the solid slag obtained in the step 2) with water according to the ratio of 1: 3-5 of solid-to-liquid ratio to prepare slurry;
4) carrying out suction filtration on the slurry prepared in the step 3) by using a suction filtration machine to obtain high-concentration water washing liquid and solid residues;
5) mixing the solid slag obtained in the step 4) with water according to the ratio of 1: 3-5 of solid-to-liquid ratio to prepare slurry;
6) carrying out suction filtration on the slurry prepared in the step 5) by using a suction filtration machine to obtain high-concentration water washing liquid and solid residues;
7) mixing the solid slag obtained in the step 6) with water according to the ratio of 1: 5-8 of solid-to-liquid ratio to prepare slurry;
8) carrying out suction filtration on the slurry prepared in the step 7) by using a suction filtration machine to obtain low-concentration water washing liquid and solid slag, concentrating the low-concentration water washing liquid by using a DTRO membrane to obtain concentrated water and fresh water, recycling the concentrated water in the step 1) for mixing with fly ash to prepare the slurry, increasing the pulping concentration by recycling the reverse concentrated water, maximally increasing the salt content in the water washing liquid, further recovering soluble salt resources in the concentrated water, and recycling the fresh water in the step 7) for mixing with the solid slag to prepare the slurry, so that water resources can be recycled; mixing the high-concentration water washing liquid obtained in the steps 2), 4) and 6), then carrying out harmless treatment and recycling, firstly removing heavy metal elements in the mixed high-concentration water washing liquid, then removing calcium and magnesium ions in the high-concentration water washing liquid to reduce the hardness of the high-concentration water washing liquid, finally carrying out evaporative crystallization on the residual high-concentration water washing liquid to obtain potassium salt and sodium salt, and carrying out water washing for three times and increasing the desalination rate of the solid-to-liquid ratio water washing for one time to reach about 95%;
step two, preparing slurry from the solid residues obtained in the step 8) according to a solid-to-liquid ratio of 1: 10-50, placing the prepared slurry into a high-pressure reaction kettle, setting the pressure of the high-pressure reaction kettle to be 0.6-1MPa, stirring at a speed of 400r/min, introducing excessive carbon dioxide gas into the slurry for reaction for 1-2 hours, further increasing the solubility of carbon dioxide, and converting calcium contained in the solid residues into calcium bicarbonate to be dissolved in water by adopting high-pressure carbon dioxide leaching. Leaching for multiple times according to decalcification effect;
step three, continuously introducing carbon dioxide to separate out the liquid in the high-pressure reaction kettle, wherein the separated liquid is a calcium bicarbonate aqueous solution, calcium bicarbonate is decomposed under normal pressure to generate calcium carbonate, and the calcium bicarbonate aqueous solution can also be heated to accelerate the decomposition of calcium bicarbonate to generate calcium carbonate;
and step four, calcining the calcium carbonate obtained in the step three to obtain quicklime and carbon dioxide gas, wherein the carbon dioxide gas can be simultaneously recycled for adjusting the pH value of the slurry in the step one and for the carbon dioxide high-pressure leaching stage in the step two.
Counting: table 1a shows the XRF analysis data of fly ash.
| Element(s) | Cl | Ca | O | Na | K | S | Si | Mg | Zn | Fe | Al |
| Mass fraction | 26.13 | 25.88 | 19 | 11.01 | 6.327 | 3.095 | 1.06 | 0.619 | 0.4664 | 0.354 | 0.348 |
Table 1b shows the detected data of XRF analysis of fly ash.
| Element(s) | P | Ti | Pb | Br | Cu | Ba | Mn | Cr | Sr | Rb | Cd |
| Mass fraction | 0.103 | 0.078 | 0.074 | 0.051 | 0.051 | 0.03 | 0.013 | 0.012 | 0.0097 | 0.0064 | 0.0015 |
Table 2 shows the calcium content before and after washing with water.
| Content of calcium% | |
| Before washing fly ash with water | 27.57 |
| After washing with fly ash water | 26.87 |
Table 3 shows statistical examples 1-2 and comparative examples.
| The decalcification rate% | |
| Example 1 | 84.99 |
| Example 2 | 91.47 |
As can be seen from Table 3, compared with the conventional fly ash treatment process, the carbon dioxide high-pressure leaching decalcification process for fly ash provided by the invention can effectively recover calcium resources under mild conditions, thereby realizing the harmlessness and reclamation of fly ash.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, changes and equivalent process changes made to the above embodiment according to the technical spirit of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (3)
1. A fly ash carbon dioxide high pressure leaching decalcification process is characterized by comprising the following steps:
step one, preparing slurry by washing fly ash, and then carrying out suction filtration on the prepared slurry by using a suction filtration machine to obtain washing liquid and solid slag;
step two, washing the solid slag to prepare slurry, placing the prepared slurry in a high-pressure container, introducing excessive carbon dioxide gas into the slurry, and converting calcium contained in the solid slag into calcium bicarbonate to be dissolved in water by adopting high-pressure carbon dioxide leaching;
step three, continuously introducing carbon dioxide to separate out the liquid in the high-pressure reaction kettle, wherein the separated liquid is a calcium bicarbonate aqueous solution, calcium bicarbonate is decomposed under normal pressure to generate calcium carbonate, and the calcium bicarbonate aqueous solution can also be heated to accelerate the decomposition of calcium bicarbonate to generate calcium carbonate;
and step four, calcining the calcium carbonate obtained in the step three to obtain quicklime and carbon dioxide gas, and reusing the carbon dioxide gas in the carbon dioxide high-pressure leaching stage in the step two.
2. The carbon dioxide high pressure leaching decalcification process of fly ash according to claim 1, wherein: firstly, preparing slurry by washing fly ash, and introducing carbon dioxide gas into the slurry to adjust the pH value to 6-8; and simultaneously recycling the carbon dioxide gas obtained in the fourth step for adjusting the pH value of the slurry.
3. The carbon dioxide high pressure leaching decalcification process of fly ash according to claim 2, wherein: harmless recycling is carried out on the water washing liquid obtained in the step one, heavy metal elements in the water washing liquid are removed firstly, calcium ions and magnesium ions in the water washing liquid are removed to reduce the hardness of the water washing liquid, and finally, the residual water washing liquid is subjected to evaporative crystallization to obtain potassium salt and sodium salt.
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| CN114888056A (en) * | 2022-04-12 | 2022-08-12 | 中南大学 | Method for synchronously solidifying carbon dioxide and deeply dechlorinating waste incineration fly ash |
| CN115448349A (en) * | 2022-08-31 | 2022-12-09 | 江西盖亚环保科技有限公司 | Method for recovering calcium salt from waste incineration fly ash |
| CN115522059A (en) * | 2022-08-31 | 2022-12-27 | 江西盖亚环保科技有限公司 | Method for separating rare earth from fly ash |
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