CN114477818B - Method for realizing efficient detoxification of heavy metal gypsum slag at normal temperature and normal pressure - Google Patents
Method for realizing efficient detoxification of heavy metal gypsum slag at normal temperature and normal pressure Download PDFInfo
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- CN114477818B CN114477818B CN202210005874.0A CN202210005874A CN114477818B CN 114477818 B CN114477818 B CN 114477818B CN 202210005874 A CN202210005874 A CN 202210005874A CN 114477818 B CN114477818 B CN 114477818B
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- heavy metal
- gypsum
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- detoxification
- gypsum slag
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- 229910052602 gypsum Inorganic materials 0.000 title claims abstract description 51
- 239000010440 gypsum Substances 0.000 title claims abstract description 51
- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 42
- 239000002893 slag Substances 0.000 title claims abstract description 30
- 238000001784 detoxification Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000012265 solid product Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical group [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000003929 acidic solution Substances 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 6
- 230000008859 change Effects 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000003723 Smelting Methods 0.000 claims description 2
- 125000000223 arsonoyl group Chemical group [H][As](*)(*)=O 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 3
- 235000019738 Limestone Nutrition 0.000 claims 1
- 229910019142 PO4 Inorganic materials 0.000 claims 1
- 239000006028 limestone Substances 0.000 claims 1
- 239000010452 phosphate Substances 0.000 claims 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 150000005837 radical ions Chemical class 0.000 claims 1
- -1 sulfate radical ions Chemical class 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 229910052785 arsenic Inorganic materials 0.000 description 18
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 17
- 238000005516 engineering process Methods 0.000 description 8
- 230000029087 digestion Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052925 anhydrite Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 150000004683 dihydrates Chemical class 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 150000005838 radical anions Chemical class 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000010891 toxic waste Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- 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
- C04B11/00—Calcium sulfate cements
- C04B11/26—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke
- C04B11/262—Calcium sulfate cements strating from chemical gypsum; starting from phosphogypsum or from waste, e.g. purification products of smoke waste gypsum other than phosphogypsum
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for realizing high-efficiency detoxification of heavy metal gypsum slag at normal temperature and normal pressure, belonging to the field of detoxification treatment of heavy metal gypsum slag. The method comprises the following specific steps: 1) Dripping acidic solution with a certain concentration on the surface of heavy metal gypsum slag to obtain insufficiently wetted solid; 2) Standing the solid obtained in the step 1); 3) After the acidic solution fully wets the solid particles, placing the solid particles at a certain temperature to promote the phase change of gypsum and realize detoxification; 4) Washing and centrifuging the product obtained in the step 3) to obtain a washing liquid and a solid product. The solid product is anhydrous gypsum, and the detoxification rate can reach 90% -100%. The method has the advantages of low energy consumption, less time consumption, high efficiency and higher social and economic benefits.
Description
Technical Field
The invention belongs to the technical field of detoxification treatment of heavy metal gypsum slag, and particularly relates to a method for realizing efficient detoxification of heavy metal gypsum slag at normal temperature and normal pressure.
Background
China is one of the major countries for nonferrous metal production and use. In nonferrous metal exploitation, mineral separation and smelting processes, chemical impurities, mineral packages and isomorphous displaced heavy metals in mineral lattices can be enriched in wastewater, waste residues, dust removal ash residues and tailings. The heavy metal gypsum slag is generated in the acid wastewater treatment process in the nonferrous metal industry, and is listed in the list of dangerous solid wastes due to the high toxicity, non-biodegradability and durability of heavy metals. The main phase of heavy metal gypsum slag is dihydrate gypsum, and heavy metal is usually adsorbed on the surface of gypsum, is entrapped between gypsum particles or is doped in gypsum lattices. Wherein heavy metal ions doped in the crystal lattice are difficult to remove efficiently by a common wet method or a fire method, mainly due to Cu 2+ 、Zn 2+ 、Cd 2+ Equivalent weight metal cations and Ca 2+ Having the same charge and similar thermochemical radius, HAsO 4 2- 、CrO 4 2- Iso-heavy metal acid radical anions and SO 4 2- With similar tetrahedral structure, thermochemical radius and same charge, the anions and cations respectively replace SO 4 2- /Ca 2+ The heavy metal gypsum waste residue is doped in gypsum lattices, so that the heavy metal gypsum waste residue detoxification efficiency is a key difficult problem.
At present, the treatment method of the heavy metal gypsum slag mainly comprises a curing technology, a stabilizing technology, a resource utilization technology and the like. The stabilizing technology has simple process, low cost and high efficiency, but the stability of the product is yet to be researched; the immobilization technology has various advantages due to different curing agents, such as cement curing is widely applied due to low cost, simple process and high curing strength, and plastic curing and melt curing can be used for high-toxic wastes due to strong corrosion resistance, impermeability and the like, but the curing tends to increase the volume of the wastes; the recycling technology mainly has the advantages of large treatment capacity, high arsenic removal rate and the like, but different recycling technologies have different limitations. Because the technologies mainly realize the macroscopic treatment of the gypsum slag, the failure to deeply study the microscopic mechanism of heavy metal separation, extraction and recovery leads to the failure to realize the separation of heavy metal and the complete detoxification of the heavy metal gypsum slag. In view of this, hydrothermal methods are widely used in detoxification treatment of gypsum slag because they destroy the gypsum lattice to release heavy metals and recrystallize into calcium sulfate. Gu Yongfeng and the like, an arsenic-containing gypsum and an acidic solution are mixed and subjected to recrystallization and solid-liquid separation in this order to obtain a low-arsenic gypsum and an arsenic-containing solution (publication No. CN 110395919A). Liuzhen and the like, placing the original electroplating sludge or pretreated electroplating sludge and alkali liquor into a hydrothermal kettle, introducing oxygen or air with a certain pressure, adding an oxidant, performing hydrothermal reaction at a fixed temperature, standing and cooling the obtained reaction system, performing suction filtration, wherein filtrate is high-concentration chromium liquid, and washing solids to obtain nontoxic minerals (publication No. CN 110527838B). However, the treatment processes by the hydrothermal method are all wet methods, and the reaction is required to be carried out in a large amount of solvents, and the heavy metals can be completely extracted after the reaction is carried out for several hours at the temperature of more than 100 ℃.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide a method for realizing high-efficiency detoxification of heavy metal gypsum slag, which is different from the wet method. The method provided by the invention is that gypsum slag is wetted by an acid solution at normal temperature and normal pressure, so that phase change from gypsum to anhydrous gypsum and separation and extraction of heavy metals are synchronously realized. The method is simple to operate, and the anhydrous gypsum almost free of heavy metals can be obtained by washing the solid product after phase change by using an alcohol solution.
The technical scheme for solving the technical problems is as follows:
a method for realizing high-efficiency detoxification of heavy metal gypsum slag at normal temperature and normal pressure comprises the steps of adding an acidic solution on the surface of gypsum slag at room temperature, standing to generate solid products (anhydrous gypsum and heavy metal-containing phases), and washing the solid products with alcohol to realize the separation of the heavy metal-containing phases, thereby achieving the purpose of heavy metal gypsum slag detoxification. The specific operation steps are as follows:
1. dripping acidic solution with a certain concentration on the surface of heavy metal gypsum slag to obtain insufficiently wetted solid;
2. standing the solid obtained in the step 1);
3. after the acidic solution fully wets the solid particles, placing the solid particles at a certain temperature to promote the phase change of gypsum and realize detoxification;
4. washing and centrifuging the product obtained in the step 3) to obtain a washing liquid and a solid product. And (3) digesting the solid product, wherein the arsenic content meets the requirement of safe stockpiling of the solid waste. And recovering heavy metals in the supernatant.
Drawings
FIG. 1 is a graph comparing XRD before treatment with standard card in example 1 of the present invention, PDF #00-033-0311 is the standard card of dihydrate gypsum, from which the main phase before treatment can be produced.
FIG. 2 is a graph comparing XRD after treatment with standard card in example 1 of the present invention, PDF #00-037-1496 is standard card of anhydrite, from which the treated main phase is anhydrite.
FIG. 3 is a graph showing arsenic concentration and arsenic detoxification rate in solid product digestion solutions before and after treatment according to the present invention as a function of detoxification temperature.
Detailed Description
The present invention will be further described with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A method for realizing high-efficiency detoxification of heavy metal gypsum slag at normal temperature and normal pressure comprises the following specific operation steps:
0.015. 0.015 g of arsenic-containing gypsum is taken, added with sulfuric acid solution with the concentration of 5.51 mol/kg to be wetted, and the solid-to-liquid ratio is 2.14:1 (w/w), and kept stand at 25 ℃ for 2 h. The solid product obtained after standing was washed and subjected to the relevant XRD test (fig. 1-2). The test result shows that the gypsum containing arsenic is converted into anhydrous gypsum phase under the action of sulfuric acid solution.
Example 2
A method for realizing high-efficiency detoxification of heavy metal gypsum slag at normal temperature and normal pressure comprises the following specific operation steps:
0.015. 0.015 g of arsenic-containing gypsum is taken, added with sulfuric acid solution with the concentration of 5.51 mol/kg to be wetted, and the solid-to-liquid ratio is 2.14:1 (w/w), and kept stand at 25 ℃ for 2 h. And (3) carrying out digestion on the obtained solid product after washing, measuring the arsenic content of the solid product and calculating the detoxification rate. Arsenic concentration in the digestion solution was 2.13. 2.13 mg/L, and the detoxification rate was 90.19% (FIG. 3).
Example 3
A method for realizing high-efficiency detoxification of heavy metal gypsum slag at normal temperature and normal pressure comprises the following specific operation steps:
0.015. 0.015 g of arsenic-containing gypsum is taken, added with sulfuric acid solution with the concentration of 5.51 mol/kg to be wetted, and the solid-to-liquid ratio is 2.14:1 (w/w), and kept stand at 35 ℃ for 2 h. And (3) carrying out digestion on the obtained solid product after washing, measuring the arsenic content of the solid product and calculating the detoxification rate. Arsenic concentration in the digestion solution was 0.18. 0.18 mg/L, and the detoxification rate was 99.27% (FIG. 3).
Example 4
A method for realizing high-efficiency detoxification of heavy metal gypsum slag at normal temperature and normal pressure comprises the following specific operation steps:
0.015. 0.015 g of arsenic-containing gypsum is taken, added with sulfuric acid solution with the concentration of 5.51 mol/kg to be wetted, and the solid-to-liquid ratio is 2.14:1 (w/w), and is kept stand at 45 ℃ for 2 h. And (3) carrying out digestion on the obtained solid product after washing, measuring the arsenic content of the solid product and calculating the detoxification rate. Arsenic concentration in the digestion solution is lower than the detection limit of 0.04 mg/L, and the detoxification rate is close to 100% (figure 3).
Claims (5)
1. The method for realizing high-efficiency detoxification of heavy metal gypsum slag at normal temperature and normal pressure is characterized by comprising the following steps:
1) Dropwise adding a sulfuric acid solution with the concentration of 0.1-8mol/kg on the surface of heavy metal gypsum slag to obtain insufficiently wetted solids, wherein the solid-liquid mass ratio of the gypsum slag to the sulfuric acid solution is 1:1-20:1;
2) Standing the solid obtained in the step 1) for 0-36 hours at the temperature of 15-60 ℃ until the acidic solution fully wets the solid particles to promote the phase change of the gypsum and realize detoxification;
3) Washing and centrifuging the product obtained in the step 2) to obtain a washing liquid and a solid product.
2. The method according to claim 1, characterized in that: the heavy metal gypsum slag comprises gypsum slag formed by limestone precipitation of acid heavy metal wastewater generated by nonferrous metal ore dressing and smelting enterprises, and gypsum slag produced by phosphate industry.
3. The method according to claim 1, characterized in that: the heavy metal acid radical ions in the heavy metal gypsum slag, which replace sulfate radical ions to enter gypsum lattices, comprise HAsO 4 2- 、CrO 4 2- 。
4. The method according to claim 1, wherein the washing liquid of step 3) is water or an organic solvent.
5. The method according to claim 1, wherein in step 3), the product obtained in step 2) is washed with water or an organic solvent for 2 times, and the solid product and the supernatant are obtained by centrifugal separation, wherein the supernatant is a heavy metal phase soluble in water or an organic solvent, and the solid product is anhydrous gypsum.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210005874.0A CN114477818B (en) | 2022-01-05 | 2022-01-05 | Method for realizing efficient detoxification of heavy metal gypsum slag at normal temperature and normal pressure |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210005874.0A CN114477818B (en) | 2022-01-05 | 2022-01-05 | Method for realizing efficient detoxification of heavy metal gypsum slag at normal temperature and normal pressure |
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| Publication Number | Publication Date |
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| CN114477818A CN114477818A (en) | 2022-05-13 |
| CN114477818B true CN114477818B (en) | 2024-01-19 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0112317A1 (en) * | 1982-12-22 | 1984-06-27 | Boliden Aktiebolag | A method for re-crystallizing gypsum |
| CN101885600A (en) * | 2010-07-21 | 2010-11-17 | 中南大学 | Heavy metal waste slag treatment method and sulfur building material prepared thereby |
| CN103495271A (en) * | 2013-10-09 | 2014-01-08 | 北京科技大学 | Complex innocent treatment method for heavy metal gypsum |
| CN109052331A (en) * | 2018-08-22 | 2018-12-21 | 湖南锐异资环科技有限公司 | Recycling method of arsenic-containing gypsum slag |
| CN110395919A (en) * | 2019-08-09 | 2019-11-01 | 中国科学院沈阳应用生态研究所 | A kind of method that the gypsum resourceization containing arsenic is handled and the application for handling the low arsenic gypsum of gained |
| CN112279538A (en) * | 2020-11-02 | 2021-01-29 | 中南大学 | Method for extracting pollutants in gypsum slag by combined roasting-acid leaching |
-
2022
- 2022-01-05 CN CN202210005874.0A patent/CN114477818B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0112317A1 (en) * | 1982-12-22 | 1984-06-27 | Boliden Aktiebolag | A method for re-crystallizing gypsum |
| CN101885600A (en) * | 2010-07-21 | 2010-11-17 | 中南大学 | Heavy metal waste slag treatment method and sulfur building material prepared thereby |
| CN103495271A (en) * | 2013-10-09 | 2014-01-08 | 北京科技大学 | Complex innocent treatment method for heavy metal gypsum |
| CN109052331A (en) * | 2018-08-22 | 2018-12-21 | 湖南锐异资环科技有限公司 | Recycling method of arsenic-containing gypsum slag |
| CN110395919A (en) * | 2019-08-09 | 2019-11-01 | 中国科学院沈阳应用生态研究所 | A kind of method that the gypsum resourceization containing arsenic is handled and the application for handling the low arsenic gypsum of gained |
| CN112279538A (en) * | 2020-11-02 | 2021-01-29 | 中南大学 | Method for extracting pollutants in gypsum slag by combined roasting-acid leaching |
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