CN113814255A - Antimony tailing harmless treatment technology based on inorganic flocculant - Google Patents
Antimony tailing harmless treatment technology based on inorganic flocculant Download PDFInfo
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- CN113814255A CN113814255A CN202110685242.9A CN202110685242A CN113814255A CN 113814255 A CN113814255 A CN 113814255A CN 202110685242 A CN202110685242 A CN 202110685242A CN 113814255 A CN113814255 A CN 113814255A
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- tailings
- inorganic flocculant
- leaching
- antimony
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- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 43
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000005516 engineering process Methods 0.000 title claims abstract description 22
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000002386 leaching Methods 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000243 solution Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 229960000583 acetic acid Drugs 0.000 claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 28
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 20
- 150000002500 ions Chemical class 0.000 claims abstract description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 10
- 230000006641 stabilisation Effects 0.000 claims abstract description 10
- 238000011105 stabilization Methods 0.000 claims abstract description 10
- 230000007306 turnover Effects 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims description 18
- 238000007711 solidification Methods 0.000 claims description 11
- 230000008023 solidification Effects 0.000 claims description 11
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 238000009616 inductively coupled plasma Methods 0.000 claims description 8
- 238000001819 mass spectrum Methods 0.000 claims description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims 1
- 229910052785 arsenic Inorganic materials 0.000 abstract description 20
- 230000000694 effects Effects 0.000 abstract description 5
- 230000005012 migration Effects 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 239000008394 flocculating agent Substances 0.000 abstract description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 abstract 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 14
- YHGPYBQVSJBGHH-UHFFFAOYSA-H iron(3+);trisulfate;pentahydrate Chemical compound O.O.O.O.O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O YHGPYBQVSJBGHH-UHFFFAOYSA-H 0.000 description 8
- 229910001385 heavy metal Inorganic materials 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- -1 hydroxyl ferric oxide Chemical compound 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 238000005065 mining Methods 0.000 description 3
- 238000005456 ore beneficiation Methods 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 231100000419 toxicity Toxicity 0.000 description 3
- 230000001988 toxicity Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- WQHONKDTTOGZPR-UHFFFAOYSA-N [O-2].[O-2].[Mn+2].[Fe+2] Chemical compound [O-2].[O-2].[Mn+2].[Fe+2] WQHONKDTTOGZPR-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000011066 ex-situ storage Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000001617 migratory effect Effects 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 1
- 229910001439 antimony ion Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/33—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by chemical fixing the harmful substance, e.g. by chelation or complexation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/40—Inorganic substances
- A62D2101/43—Inorganic substances containing heavy metals, in the bonded or free state
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention provides an antimony tailing harmless treatment technology based on an inorganic flocculant, which specifically comprises the following steps: mixing the tailings, water and an inorganic flocculant in a mass ratio of 1:5: 0.1-10%; curing for 24 hours on a water shaking bed; placing the mixed solution in an oven for drying; mixing a leaching solution prepared by glacial acetic acid and solidified tailings in a zero-headspace extractor according to a solid-to-liquid ratio of 1: 20; fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min; then filtering the obtained mixed solution by adopting a 0.25 mu m needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrometry. According to the invention, through the adsorption effect of hydroxyl hydrate generated by the hydrolysis of the flocculating agent, Sb and As elements in the fine tailings are adsorbed to form a stable complex, so that the migration of the Sb and As elements is reduced, and the harmless treatment of the tailings is realized.
Description
Technical Field
The invention belongs to the technical field of industrial tailing disposal, and particularly relates to a antimony tailing harmless treatment technology based on an inorganic flocculant.
Background
China is one of the countries in the world where antimony ore is mined earlier, and is also the country in the world where the antimony yield is the largest currently. Antimony mining areas are mainly mined in a hole mining mode, a large amount of mine solid wastes are stockpiled disorderly for a long time, and a large amount of land resources are occupied. More seriously, because the soil process is adopted for private beneficiation in the early stage, a large amount of low-grade antimony ore beneficiation tailings are mixed into solid mine waste, wherein the content of heavy metals such as antimony, arsenic and the like and harmful substances is high, the antimony ore beneficiation tailings are released when being subjected to leaching erosion action such as surface water, rainfall and the like, and enter surrounding soil and rivers along with runoff and infiltration action of water, so that the antimony ore beneficiation tailings not only cause great pollution to the safety of the ecological environment near a mining area, but also threaten the living environment and the water safety of surrounding residents.
The currently common tailings disposal methods include: underground filling, in-situ or ex-situ landfill and resource utilization. If the surrounding mine has been shut down, the mine tailing downhole filling scheme is not feasible. The scheme of in-situ or ex-situ landfill of the tailings after the anti-seepage treatment by using the anti-seepage film and the like is temporary and permanent, although the method plays a role in preventing the transmission of pollutants such as heavy metal ions and the like to a certain extent, the pollution source still exists, and the problem of the pollution of the tailings cannot be fundamentally solved. The pollution problem is thoroughly solved, and the resource utilization of the tailings is one of the main ways. If the resource utilization of the tailings is to be realized, the heavy metals and toxic substances in the tailings need to be cured.
Antimony Sb, arsenic As and compounds thereof have toxicity, and the harm of arsenic and antimony in tailings to the environment is not only related to the total content of the antimony Sb and arsenic As but also determined by the existence morphological distribution of the antimony Sb and arsenic As. The existing forms of arsenic and antimony in tailings mainly comprise: exchangeable state, carbonate bound state, iron-manganese oxide bound state, organic bound state, and sludge state. The exchangeable arsenic has the greatest biological effectiveness and the strongest mobility, and easily enters plants and human bodies through food chains to cause toxic action; the arsenic in residue state has the lowest toxicity and the lowest migration ability. Therefore, it is necessary to reduce or suppress the bioavailability of arsenic and promote the conversion of arsenic from a highly toxic and highly migratory form to a less active, less migratory form, and less toxic form, and to perform effective stable solidification. Arsenic and antimony are adjacent elements of the same family, and have similar physicochemical properties.
Because the tailings have fine granularity and high specific surface area, the transfer and diffusion of heavy metal ions are more easily caused, and the tailings have greater environmental hazard compared with coarse tailing sand, and in order to reduce the content of heavy metals and toxic substances in the tailings, the establishment of a harmless treatment technology suitable for antimony tailings is urgently needed.
Disclosure of Invention
Aiming at the problems, the invention provides a antimony tailing harmless treatment technology based on an inorganic flocculant, which adsorbs Sb and As elements in fine tailings to form a stable complex through the adsorption effect of hydroxyl hydrate generated by hydrolyzing the flocculant, so that the migration of the Sb and As elements is reduced, and the harmlessness of the tailings is promoted.
In order to achieve the purpose, the technical scheme adopted by the invention is an antimony tailing harmless treatment technology based on an inorganic flocculant, and the antimony tailing harmless treatment technology specifically comprises the following steps:
(1) mixing the tailings, water and an inorganic flocculant in a mass ratio of 1:5: 0.1-10%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by using a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by using an inductively coupled plasma mass spectrometry.
Further, the inorganic flocculant adopted in the step (1) is one of polymeric ferric sulfate, polymeric aluminum ferric chloride and basic aluminum chloride.
Further, the concentration of the leaching solution prepared by glacial acetic acid in the step (4) is 17.25mL of glacial acetic acid/L, and the pH value is 2.64; wherein the water used for the preparation is deionized water.
The harmless treatment technology principle of the invention is as follows:
the flocculant can be hydrolyzed to generate hydroxyl ferric oxide or hydroxyl aluminum oxide, and the hydroxyl hydrate can adsorb Sb and As elements in the fine tailings in an obligatory adsorption and non-obligatory adsorption mode, form a stable complex and reduce the migration of the Sb and As elements.
Ferric ion Fe in polymeric ferric sulfate3+The iron ions can also directly react with Sb (III) and As (III) in soil to convert the Sb (V) and As (V) with low toxicity into stable complexes, and meanwhile, the hydrates of the iron ions can convert harmful elements such As arsenic, antimony and the like from exchangeable states into iron-manganese oxide combined states.
Compared with the prior art, the antimony tailing harmless treatment technology based on the inorganic flocculant has the following beneficial effects:
by adopting the inorganic flocculant, the arsenic and antimony elements in the tailings can be effectively solidified. And 0.1% of polymeric ferric sulfate is adopted to cure heavy metals and harmful components in the tailings, so that the curing effect is remarkable, and the economic cost can be greatly saved.
Detailed Description
In order to more clearly and completely describe the present invention, the following will further describe a technique for harmless treatment of antimony tailings based on inorganic flocculant in accordance with the present invention.
Example 1
An antimony tailing harmless treatment technology based on an inorganic flocculant comprises the following specific steps:
(1) mixing tailings, water and polymeric ferric sulfate in a mass ratio of 1:5: 0.1%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by adopting a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrum.
For the leaching solution prepared by glacial acetic acid in the step (4), the concentration is 17.25mL of glacial acetic acid/liter, and the pH value is 2.64; wherein the water used for the preparation is deionized water.
Example 2
An antimony tailing harmless treatment technology based on an inorganic flocculant comprises the following specific steps:
(1) mixing tailings, water and polymeric ferric sulfate in a mass ratio of 1:5: 1%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by adopting a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrum.
For the leaching solution prepared by glacial acetic acid in the step (4), the concentration is 17.25mL of glacial acetic acid/liter, and the pH value is 2.64; wherein the water used for the preparation is deionized water.
Example 3
An antimony tailing harmless treatment technology based on an inorganic flocculant comprises the following specific steps:
(1) mixing tailings, water and polymeric ferric sulfate in a mass ratio of 1:5: 10%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by adopting a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrum.
For the leaching solution prepared by glacial acetic acid in the step (4), the concentration is 17.25mL of glacial acetic acid/liter, and the pH value is 2.64; wherein the water used for the preparation is deionized water.
Example 4
An antimony tailing harmless treatment technology based on an inorganic flocculant comprises the following specific steps:
(1) mixing the tailings, water and polyaluminium sulfate in a mass ratio of 1:5: 0.1%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by adopting a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrum.
For the leaching solution prepared by glacial acetic acid in the step (4), the concentration is 17.25mL of glacial acetic acid/liter, and the pH value is 2.64; wherein the water used for the preparation is deionized water.
Example 5
An antimony tailing harmless treatment technology based on an inorganic flocculant comprises the following specific steps:
(1) mixing the tailings, water and polyaluminum ferric chloride in a mass ratio of 1:5: 0.1%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by adopting a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrum.
For the leaching solution prepared by glacial acetic acid in the step (4), the concentration is 17.25mL of glacial acetic acid/liter, and the pH value is 2.64; wherein the water used for the preparation is deionized water.
Example 6
An antimony tailing harmless treatment technology based on an inorganic flocculant comprises the following specific steps:
(1) mixing the tailings, water and polyaluminium chloride in a mass ratio of 1:5: 0.1%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by adopting a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrum.
For the leaching solution prepared by glacial acetic acid in the step (4), the concentration is 17.25mL of glacial acetic acid/liter, and the pH value is 2.64; wherein the water used for the preparation is deionized water.
Example 7
An antimony tailing harmless treatment technology based on an inorganic flocculant comprises the following specific steps:
(1) mixing the tailings, water and basic aluminum chloride in a mass ratio of 1:5: 0.1%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by adopting a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrum.
For the leaching solution prepared by glacial acetic acid in the step (4), the concentration is 17.25mL of glacial acetic acid/liter, and the pH value is 2.64; wherein the water used for the preparation is deionized water.
Ion concentration tests are carried out on the tailings leachate treated by the technology described in each example, and the experimental data are shown in table 1.
Table 1 detection of curing effect of inorganic flocculant based on acid leaching experiment
| Treatment method | Adding a flocculating agent | As(mg/L) | Sb(mg/L) |
| As received | Is free of | 0.961 | 1.401 |
| Example 1 | 0.1% polymeric ferric sulfate | 0.464 | 0.216 |
| Example 2 | 1% polymeric ferric sulfate | 0.494 | 0.026 |
| Example 3 | 10% polymeric ferric sulfate | 0.592 | 0.148 |
| Example 4 | 0.1% polyaluminium sulfate | 0.665 | 0.378 |
| Example 5 | 0.1% polyaluminum ferric chloride | 0.589 | 0.784 |
| Example 6 | 0.1% polyaluminium chloride | 0.485 | 0.836 |
| Example 7 | 0.1% basic aluminum chloride | 0.639 | 0.938 |
From table 1, the concentrations of arsenic and antimony ions in the tailings leachate treated by the innocent treatment technology are both obviously reduced, and the requirements of 'hazardous waste identification standard leaching toxicity identification' (GB5085.3-2007) and 'emission standard of industrial pollutants of tin, antimony and mercury' (GB30770-2014) are met, namely, the invention can realize effective solidification on heavy metal ions in the tailings and can be used for innocent treatment of antimony tailings. The combined effect of using the 0.1% polymeric ferric sulphate treatment technique provided in example 1 is best considering the leaching effect and economic cost.
The above examples are only for illustrating the preferred embodiments of the present invention, not for all examples, and do not limit the scope of the present invention. In practice, any modification, equivalent replacement, improvement and the like within the spirit and principle of the present invention are included in the protection scope of the present invention.
Claims (3)
1. An antimony tailing harmless treatment technology based on an inorganic flocculant is characterized by comprising the following steps:
(1) mixing the tailings, water and an inorganic flocculant in a mass ratio of 1:5: 0.1-10%;
(2) after mixing, curing treatment is carried out for 24 hours on a water shaking bed;
(3) after solidification, placing the mixed solution of the tailings and the inorganic flocculant in an oven for drying treatment, wherein the drying temperature and the drying time are respectively 105 ℃ and 24 hours;
(4) preparing a leaching solution by using glacial acetic acid, and mixing the leaching solution and the solidified tailings obtained in the step (3) in a zero-headspace extractor according to a solid-liquid ratio of 1:20 after the preparation is finished;
(5) fixing a zero headspace extractor on a turnover type oscillating device, and leaching for 18 hours at the rotating speed of 30 r/min;
(6) and filtering the mixed solution obtained after the leaching test by adopting a 0.25-micrometer needle filter, collecting 10mL of filtered clear solution, adding high-purity nitric acid for stabilization, and testing the ion concentration by adopting an inductively coupled plasma mass spectrum.
2. The antimony tailings harmless treatment technology based on the inorganic flocculant of claim 1, wherein the inorganic flocculant adopted in the step (1) is one of polymeric ferric sulfate, polymeric aluminum ferric chloride and basic aluminum chloride.
3. The antimony tailings harmless treatment technology based on the inorganic flocculant of claim 1, wherein the leaching solution prepared by glacial acetic acid in the step (4) has a concentration of 17.25mL glacial acetic acid/L and a pH value of 2.64; wherein the water used for the preparation is deionized water.
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