CN112125320A - Method for desalting water from barren liquor or barren liquor generated in gold extraction process by cyanidation - Google Patents
Method for desalting water from barren liquor or barren liquor generated in gold extraction process by cyanidation Download PDFInfo
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- CN112125320A CN112125320A CN201910559515.8A CN201910559515A CN112125320A CN 112125320 A CN112125320 A CN 112125320A CN 201910559515 A CN201910559515 A CN 201910559515A CN 112125320 A CN112125320 A CN 112125320A
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- cyanide
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- 238000011033 desalting Methods 0.000 title claims abstract description 99
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 67
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 48
- 239000010931 gold Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000000605 extraction Methods 0.000 title claims abstract description 28
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 claims abstract description 178
- 238000010521 absorption reaction Methods 0.000 claims abstract description 82
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 claims abstract description 59
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 47
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 46
- 239000007788 liquid Substances 0.000 claims abstract description 41
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 40
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 29
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 28
- 238000010612 desalination reaction Methods 0.000 claims abstract description 21
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 14
- 230000001131 transforming effect Effects 0.000 claims abstract description 11
- 230000008929 regeneration Effects 0.000 claims abstract description 6
- 238000011069 regeneration method Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 145
- 238000006243 chemical reaction Methods 0.000 claims description 76
- 239000007789 gas Substances 0.000 claims description 60
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 52
- 239000000920 calcium hydroxide Substances 0.000 claims description 52
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 52
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 49
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 47
- 239000002893 slag Substances 0.000 claims description 39
- 239000012295 chemical reaction liquid Substances 0.000 claims description 36
- 238000007664 blowing Methods 0.000 claims description 34
- -1 alkaline earth metal cyanide Chemical class 0.000 claims description 30
- 239000000706 filtrate Substances 0.000 claims description 28
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 24
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 23
- 239000001569 carbon dioxide Substances 0.000 claims description 22
- 238000001914 filtration Methods 0.000 claims description 21
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 19
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims description 14
- CWVZGJORVTZXFW-UHFFFAOYSA-N [benzyl(dimethyl)silyl]methyl carbamate Chemical compound NC(=O)OC[Si](C)(C)CC1=CC=CC=C1 CWVZGJORVTZXFW-UHFFFAOYSA-N 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 13
- 230000002378 acidificating effect Effects 0.000 claims description 12
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 claims description 12
- 239000000839 emulsion Substances 0.000 claims description 12
- 229910001385 heavy metal Inorganic materials 0.000 claims description 11
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 230000020477 pH reduction Effects 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- 239000011491 glass wool Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 230000009466 transformation Effects 0.000 claims description 5
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
- UNLSXXHOHZUADN-UHFFFAOYSA-N barium cyanide Chemical compound [Ba+2].N#[C-].N#[C-] UNLSXXHOHZUADN-UHFFFAOYSA-N 0.000 claims description 3
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- UUCCCPNEFXQJEL-UHFFFAOYSA-L strontium dihydroxide Chemical compound [OH-].[OH-].[Sr+2] UUCCCPNEFXQJEL-UHFFFAOYSA-L 0.000 claims description 3
- 229910001866 strontium hydroxide Inorganic materials 0.000 claims description 3
- WTNNIXSCSYFNFP-UHFFFAOYSA-N strontium;dicyanide Chemical compound [Sr+2].N#[C-].N#[C-] WTNNIXSCSYFNFP-UHFFFAOYSA-N 0.000 claims description 3
- 150000001340 alkali metals Chemical group 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- 238000010828 elution Methods 0.000 claims description 2
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 claims description 2
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 58
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 29
- 230000035484 reaction time Effects 0.000 description 19
- 238000009423 ventilation Methods 0.000 description 9
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 8
- 235000011941 Tilia x europaea Nutrition 0.000 description 8
- 229920001973 fluoroelastomer Polymers 0.000 description 8
- 239000004571 lime Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000005070 sampling Methods 0.000 description 7
- 239000007832 Na2SO4 Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 238000009993 causticizing Methods 0.000 description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 238000002386 leaching Methods 0.000 description 5
- 239000012066 reaction slurry Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910052925 anhydrite Inorganic materials 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 3
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- MNWBNISUBARLIT-UHFFFAOYSA-N sodium cyanide Chemical compound [Na+].N#[C-] MNWBNISUBARLIT-UHFFFAOYSA-N 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000002535 acidifier Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 229910052923 celestite Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application 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
- 238000007255 decyanation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/08—Simple or complex cyanides of metals
- C01C3/10—Simple alkali metal cyanides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/08—Simple or complex cyanides of metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
Abstract
A method for desalting water from barren liquor or barren liquor generated in a cyaniding gold extraction process comprises the following steps: (1) preparing a desalting reagent solution; (2) acidifying and transforming; (3) hydrogen cyanide stripping and hydrogen cyanide stripping liquid treatment; (4) absorption desalination of hydrogen cyanide and regeneration of sodium cyanide. The method can remove sulfate radicals in the barren solution containing sodium sulfate, can convert the sodium sulfate into sodium hydroxide or sodium carbonate, is suitable for desalting the barren solution containing the sodium sulfate generated in the cyaniding gold extraction process, and has the advantages of low energy consumption, low cost and good effect.
Description
Technical Field
The invention relates to a method for desalting from a solution containing sodium sulfate, in particular to a method for desalting from barren liquor or water in barren liquor generated in a gold extraction process through cyanidation.
Background
During cyanidation gold extraction in gold smelters, a solution containing sodium sulphate, commonly referred to as barren liquor, is produced.
At present, for gold concentrate with high arsenic and high sulfur which is difficult to process, two-section roasting dearsenification and desulfurization treatment is generally adopted in China to obtain calcine, acid leaching decoppering and salt leaching deleading are firstly adopted to remove impurities, then a cyanidation method is used for processing to extract gold in the calcine,
in the process of extracting gold by cyanidation, gold-containing calcine is leached by alkaline solution containing cyanide while stirring and blowing, and gold in the impurity-removed calcine is leached and enters the solution.
And replacing gold in the solution with zinc powder to obtain primary coarse gold powder, and further refining to obtain commercial gold ingots. The gold contained in the solution after gold replacement is very micro and is called barren liquor, and the barren liquor returns to circularly leach gold. According to the process and the raw material condition, the gold leaching solution is required to contain 0.1-0.3% of Cyanogen (CN). During the continuous circulation of the gold leaching solution, impurities in the solution, such as Cu, Fe, Zn, sodium salt (Na)2SO4) Etc. are continuously enriched and increased. Cu and Fe in the solution are from calcine, sodium in sodium sulfate is from sodium hydroxide which is added as protective alkali, and sulfate ions are from residual sulfur in the calcine.
The sulfur content of the gold concentrate with high arsenic and high sulfur is up to 30 percent, after two-stage roasting and desulfurization, the sulfur content of the roasted product is about 1 percent, most of the roasted product is brought into a cyaniding gold leaching system, and the roasted product is oxidized by blown air under the alkaline condition to become sodium sulfate.
2FeS+4.5O2+4NaOH＝Fe2O3+2Na2SO4+2H2O
The sodium hydroxide in the above reaction formula may also be replaced by sodium bicarbonate or sodium carbonate:
2FeS+4.5O2+4NaHCO3＝Fe2O3+2Na2SO4+2H2O+4CO2
2FeS+4.5O2+2Na2CO3＝Fe2O3+2Na2SO4+2CO2
because carbon dioxide exists in the air and the reaction also generates carbon dioxide, sodium hydroxide added into the cyaniding gold extraction system reacts with the carbon dioxide to generate sodium carbonate.
And when the sodium sulfate is saturated, the sodium sulfate can be crystallized and separated out from the solution, so that a pipeline is blocked, and the production is influenced. The accumulated heavy metals Cu, Fe, Zn and the like can influence the gold replacement process by the zinc powder. Therefore, it is necessary to periodically extract a part of the treatment from the barren solution after gold substitution.
Because the barren solution contains cyanogen, the cyanogen content after the barren solution heavy metal removal treatment can hardly reach the discharge standard of 0.5mg/m specified by the state3Moreover, heavy metals are difficult to meet the national emission standards due to the cyanogen.
Along with the increasing environmental protection requirement, the up-to-standard discharge of the waste water can not meet the environmental protection requirement, and more manufacturers require the zero discharge of the waste water. In this case, the reclaimed water obtained after the treatment of removing heavy metals from the barren solution can only be returned to the cyaniding gold extraction system for recycling.
For the existing gold smelting plant, the treatment of barren solution for removing heavy metals is mature, and the adopted method is basically to add sulfuric acid for acidification, blast air decyanation and lime for neutralizing and removing heavy metals to obtain barren solution reclaimed water. However, the reclaimed water after heavy metal removal also contains sodium sulfate, and the solubility of the sodium sulfate in the water is very high, such as 19.5g/100g water at 20 ℃; however, when the temperature is lowered, particularly when the temperature is lowered to 0 ℃ or below, sodium sulfate is precipitated to block the pipeline, which affects the production.
Typical barren solution components of a gold smeltery in south are as follows: 70-80 g/l of sodium sulfate, 5-10 mg/l of arsenic, 1500-2500 mg/l of copper, 1-5 mg/l of lead, 200-300 mg/l of zinc, 500-700 mg/l of iron, 500-600 mg/l of calcium, 2-2 mg/l of magnesium, 300-600 mg/l of total cyanogen and pH 11.
At present, the methods for removing salts from the barren solution include an evaporation method and an open circuit method. The evaporation method is to evaporate and concentrate the reclaimed water after heavy metal removal from the barren solution, and the method has high energy consumption and high cost and is difficult to bear by factories. The open-circuit method of the reclaimed water in the barren solution is to discharge the reclaimed water after treating the reclaimed water to the national discharge standard, has high cost which is not qualified for the discharge standard, is limited by the environmental protection regulations of regions, countries and places, and many factories have no discharge indexes and can not use the reclaimed water.
In summary, the existing barren liquor desalination methods have the common disadvantages of high cost and difficult factory tolerance, or no wastewater discharge index and no discharge.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects in the prior art and provide a method for desalting barren liquor or barren liquor water generated in the cyaniding gold extraction process, which has low cost, low energy consumption, high efficiency and strong adaptability.
The technical scheme adopted for solving the technical problems is that the method for desalting the barren solution or the barren solution generated in the cyaniding gold extraction process comprises the following steps:
(1) preparing a desalting reagent solution, namely dissolving a desalting reagent and uniformly stirring to obtain the desalting reagent solution;
(2) acidifying and transforming: adding an acidic substance into the desalted reagent solution obtained in the step (1) to carry out acidification and transformation reaction, and adjusting the pH value to obtain a mixed solution of hydrogen cyanide and salt;
(3) stripping hydrogen cyanide and treating hydrogen cyanide stripping liquid: when the acidic substance added in the step (2) is sulfuric acid or hydrochloric acid, blowing air into the mixed solution of hydrogen cyanide and salt obtained in the step (2), and blowing off the generated hydrogen cyanide to obtain hydrogen cyanide gas and a blowing-off reaction liquid; collecting the blown hydrogen cyanide gas, removing the blow-off reaction liquid carried by the hydrogen cyanide gas, absorbing by using an emulsion prepared from alkaline earth metal hydroxide to generate a water-soluble alkaline earth metal cyanide solution, and filtering to obtain the alkaline earth metal cyanide solution and absorption reaction slag;
when the acidic substance added in the step (2) is carbon dioxide, obtaining a mixed solution of hydrogen cyanide and sodium bicarbonate in the step (2), blowing off the hydrogen cyanide, adding slaked lime into the blowing-off reaction solution, stirring, carrying out a causticization reaction, and filtering to obtain causticized slag calcium carbonate and a sodium hydroxide solution or a sodium carbonate solution;
(4) absorption desalination and sodium cyanide regeneration of hydrogen cyanide: and (3) mixing the alkaline earth metal cyanide solution obtained in the step (3) with barren liquor generated in the cyaniding gold extraction process or barren liquor water after heavy metal removal, reacting the alkaline earth metal cyanide with sodium sulfate in the barren liquor or barren liquor water to generate alkaline earth metal sulfate and sodium cyanide, and filtering to obtain alkaline earth metal sulfate filter residue and desalting filtrate containing sodium cyanide.
Further, in the step (1), the desalting reagent is alkali metal cyanide or alkaline earth metal cyanide; the alkali metal cyanide is sodium cyanide or potassium cyanide; the alkaline earth metal cyanide is calcium cyanide, barium cyanide, strontium cyanide (preferably sodium cyanide or calcium cyanide).
Further, in the step (3), the method for removing the stripping reaction liquid carried by the hydrogen cyanide gas is carried out by washing or mechanical interception by glass wool.
Further, in the step (4), the obtained desalting filtrate containing sodium cyanide is returned to the step (1) as a desalting reagent cyanide solution.
Further, in the step (1), when the desalting reagent cyanide is dissolved, the solvent is at least one of water, a barren solution containing sodium sulfate, water in the barren solution, sodium cyanide-containing solution and sodium sulfate-containing solution.
Further, when the acidic substance added in the step (2) is sulfuric acid, the pH is adjusted to 1-7 (preferably 1-3).
Further, when the acidic substance added in the step (2) is carbon dioxide, the pH is adjusted to 7-9 (preferably 8).
Further, in the step (3), the alkaline earth metal hydroxide is at least one of calcium hydroxide, barium hydroxide or strontium hydroxide (preferably calcium hydroxide); the liquid of the emulsion prepared by the alkaline earth metal hydroxide is at least one of water, barren solution, water in the barren solution or solution containing sodium sulfate; the mass concentration of the emulsion prepared by the alkaline earth metal hydroxide is 0.1-10% (preferably 1-5%).
Further, in the step (3), when the emulsion prepared from the alkaline earth metal hydroxide is a barren solution, water in the barren solution or a solution containing sodium sulfate, desalting reaction occurs in the step (3), water-soluble alkaline earth metal cyanide obtained after elution reaction reacts with sulfate ions in the sodium sulfate solution to generate a mixed solution of desalted residue precipitate and sodium cyanide, and filtering is performed to obtain desalted residue alkaline earth metal sulfate and a sodium cyanide solution.
Further, in the step (4), the pH value for carrying out the causticization reaction is more than or equal to 13.
The principle of the invention is as follows:
when NaCN is used as the initial step in the desalination cycle, the desalination cycle is: preparing a desalting reagent solution (newly prepared or recycled by a subsequent process) in the step (1); acidifying and transforming; step (3) stripping hydrogen cyanide and treating hydrogen cyanide stripping liquid; (4) absorption desalination of hydrogen cyanide and regeneration of sodium cyanide. The sodium cyanide produced can be recycled in steps (1), (2), (3) of the invention.
When calcium cyanide is used as an initial step of cyclic desalination, the calcium cyanide cannot be recycled and can only be used as an initial step of the cyclic desalination of sodium cyanide; the desalination cycle is: preparing calcium cyanide (prepared by absorbing hydrogen cyanide gas generated after acidification and transformation of sodium cyanide by slaked lime or other alkaline earth metal hydroxides), desalting in step (4) (obtaining sodium cyanide solution and calcium sulfate), filtering to obtain sodium cyanide solution, step (1), step (2), step (3) and returning to step (1).
Calcium cyanide (or barium cyanide, strontium cyanide) solution is reacted with sodium sulfate to produce insoluble sulfate, and the sodium sulfate is converted into sodium cyanide while the sulfate precipitate is produced.
Carrying out desalting reaction by using an alkaline earth metal cyanide desalting agent:
Ca(CN)2+Na2SO4＝2NaCN+CaSO4↓
Ba(CN)2+Na2SO4＝2NaCN+BaSO4↓
Sr(CN)2+Na2SO4＝2NaCN+SrSO4↓
acidifying the sodium cyanide solution generated in the desalting process by adding acid to obtain aqueous solution hydrocyanic acid containing hydrogen cyanide; pure hydrocyanic acid has a boiling point of 25.7 ℃, is mutually soluble with water, and can be removed from water by blowing, and the acid used can be sulfuric acid, hydrochloric acid, carbonic acid or other acids.
Acidification transformation of 2NaCN + H2SO4＝Na2SO4+2HCN
NaCN+HCl＝NaCl+HCN
NaCN+CO2+H2O＝NaHCO3+HCN
Absorbing the hydrogen cyanide blown out by air blast with slaked lime or other alkaline earth metal hydroxides to generate alkaline earth metal cyanide; the alkaline earth metal cyanide reacts with the sodium sulfate solution to remove the sodium sulfate in the solution.
Alkaline earth metal cyanide formation reaction:
2HCN+Ca(OH)2＝Ca(CN)2+H2O
2HCN+Ba(OH)2＝Ba(CN)2+H2O
2HCN+Sr(OH)2＝Sr(CN)2+H2O
in the process of generating hydrogen cyanide by acidification and transformation, when sulfuric acid or hydrochloric acid is used as an acidifying agent, sodium sulfate or sodium chloride is generated and is not well utilized; when carbonic acid is used as an acidifying agent, sodium bicarbonate is generated, and sodium hydroxide (or sodium carbonate) and causticized slag calcium carbonate can be generated by a classical causticization reaction with lime.
NaHCO3+Ca(OH)2＝CaCO3↓+NaOH+H2O
NaHCO3+NaOH＝Na2CO3+H2O
Total reaction 2NaHCO3+Ca(OH)2＝CaCO3↓+Na2CO3+2H2O
The generated sodium hydroxide and sodium carbonate can be used as protective alkali in the cyaniding gold extraction process, so that the sodium bicarbonate does not need to be completely converted into sodium hydroxide and sodium carbonate.
The total reaction of desalting and causticizing to generate sodium hydroxide is as follows:
2CO2+Na2SO4+3Ca(OH)2=CaSO4↓+2CaCO3↓+2NaOH+2H2O
the desalting and causticizing total reaction for generating the sodium carbonate comprises the following steps:
2CO2+Na2SO4+2Ca(OH)2=CaSO4↓+CaCO3↓+Na2CO3+2H2O
in the causticizing reaction in the step (3) of the embodiment of the invention, the sodium cyanide is only partially causticized by the solution containing the sodium bicarbonate after the sodium cyanide is decarbonized, and the pH value of the solution is adjusted to be more than 11, so that the solution is conveniently returned to a cyaniding gold extraction system for use. Or directly sending the carbonation stripping liquid with the pH value of 9 to a cyanidation gold extraction system for use without causticization reaction.
The causticization of sodium bicarbonate or sodium carbonate to produce alkali is a mature process.
The invention has the beneficial effects that: (1) the desalting reagent is a reagent required by cyaniding gold extraction, is regenerated in the desalting process, can be recycled, and can also be sent to a cyaniding gold extraction system for use once or several times, so that the difficulty in evaporation and concentration is overcome, a large amount of water does not need to be evaporated, and the energy consumption is low; (2) sodium in the sodium sulfate contained in the barren solution is converted into sodium hydroxide or sodium carbonate which is a reagent required for cyaniding and gold extraction; (3) the reagents consumed by the desalination of the invention are acidic substances (carbon dioxide is consumed in the preferred scheme) and lime, and the sources are wide, and the cost is low and the raw materials are easy to obtain; (4) the produced calcium sulfate of the desalting slag (preferably causticized slag calcium carbonate produced in the scheme) can be made into building material gypsum and light calcium carbonate with higher utilization value.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus used in step (3) of the embodiment of the present invention;
FIG. 2 is a schematic structural diagram of the apparatus used in step (2) of the embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
The carbonation equipment for introducing carbon dioxide used in the step 2 of the embodiment of the invention is shown in figure 2 and comprises a carbon dioxide gas cylinder 11, a pressure reducing valve 12, a pressure gauge 13, a reactor 14, a bottle shaking machine 15 and a reactor fixing frame 10, wherein the carbon dioxide gas cylinder 11 is connected with the pressure reducing valve 12, the pressure reducing valve 12 is connected with the reactor 14 through a rubber pipe, the pressure gauge 13 is connected on the rubber pipe, the pressure in the reactor is detected, and the reactor is made of transparent plastic and resists the pressure of 0.2 MPa. When the device works, a solution needing carbonation is added into a reactor, air above the liquid level is blown out through carbon dioxide, then the carbon dioxide is introduced to reach a specified pressure, the pressure reducing valve 12 is closed, the reactor is placed on a bottle shaking machine to shake, and the pressure change is observed through the pressure gauge 13; when the pressure is reduced, the pressure reducing valve 13 is opened to charge air to a specified pressure; the operation is repeated until the pressure in the reactor does not drop any more, and the reaction end point is obtained.
The device used in step 1 of the embodiment of the invention is a beaker and an electric stirrer which are commonly used in a chemical or metallurgical laboratory, the used desalting reagent is commercial sodium cyanide, the used solvent for preparing the sodium cyanide solution is water, barren solution or barren solution reclaimed water, and the desalting filtrate produced in step (3) or step (4) can be directly used and contains regenerated sodium cyanide.
The equipment used in step 3 of the embodiment of the invention is shown in figure 1 and comprises a three-mouth flask 1, a gas washing bottle 2, an absorption bottle 3, an absorption bottle 4, a water circulation vacuum pump 5, a three-mouth bottle support 8 and a blower 9, wherein the three-mouth flask 1, the gas washing bottle 2, the absorption bottle 3, the absorption bottle 4, the water circulation vacuum pump 5 and the blower 9 are connected by a fluororubber pipe resistant to hydrogen cyanide corrosion; one port of the three-mouth flask 1 is a gas leading-out port for leading out gas, the middle port is a feeding port for feeding, the other port is used for inserting a thermometer 6 and an air blowing pipe 7, one end of the air blowing pipe 7 with a gas dispersion head is inserted into the solution contained in the three-mouth flask 1 so as to disperse and blow blown air into the solution, and the other end of the air blowing pipe 7 is connected with a blower 9.
During working, adding the measured acidizing fluid produced in the step (2) into the three-neck flask 1 through a feeding port of the three-neck flask 1, adding a certain amount of aqueous solution or glass wool into the gas washing bottle 2, putting a certain amount of slaked lime and water or solution into the absorption bottle 3, adding a certain amount of sodium hydroxide solution into the absorption bottle 4, connecting a pipeline, starting a water circulation vacuum pump 5 to pump air, blowing gas such as air into the three-neck flask 1 through a blowing pipe 7, and timing; hydrogen cyanide gas produced in the three-neck flask 1 enters the gas washing bottle 2 through the fluororubber pipe for impurity removal, acidification liquid drops carried in the gas are removed, and then the gas enters the absorption bottle 3 to react with slaked lime in the absorption bottle 3 to generate calcium cyanide; the hydrogen cyanide gas which is not completely reacted enters the absorption bottle 4 through the fluororubber pipe and reacts with sodium hydroxide to generate sodium cyanide, and the tail gas is pumped away through the water circulating vacuum pump 5.
When the solution charged in the absorption flask 3 in the step (3) is a sodium sulfate-containing solution such as a lean solution or water in a lean solution, the absorption flask 4, the water circulating vacuum pump 5 is eliminated and the slaked lime is added to the absorption flask 3 in a small amount and a plurality of times, the desalting reaction to produce calcium sulfate which occurs in the step (4) occurs in the step (3), and the step (4) can be omitted.
After the stripping absorption desalination reaction is finished, pouring the acidic stripping reaction liquid out of the three-neck flask 1, carrying out causticization reaction in the step (4), filtering, sampling and testing; and (4) taking out the slurry in the absorption bottle 3, filtering, drying the slag, and analyzing the content of calcium sulfate and the content of cyanogen in the absorption liquid in the slag.
Barren liquor used in the examples of the present invention was sourced from gold smelter No. 1 (No. 2) in south. Sodium cyanide, technical grade, content 98.0%, carbon dioxide, technical grade, content 98%, slaked lime (slaked lime), technical grade, calcium hydroxide content 72.22%, concentrated sulfuric acid, concentration 98%, chemical purity; the reagents used are all available from conventional commercial sources.
The barren liquor composition used in this example is as follows (in mg/l):
| serial number | Cu | Sb | As | Zn | Pb | Ca | Mg | Total cyanogen | Sodium sulfate, g/l |
| 1 | 1502 | 13.5 | 6.13 | 509.87 | 4.15 | 500.8 | 2.8 | 309.34 | 70.85 |
| 2 | 1840 | 12.7 | 5.64 | 280.65 | 1.79 | 636.8 | 2.76 | 250.43 | 72.99 |
And (3) respectively taking a part of the No. 1 barren solution and the No. 2 barren solution to carry out heavy metal removal treatment to produce barren solution reclaimed water. Ingredients are shown in the following table (in mg/l):
| serial number | Cu | Sb | As | Zn | Pb | Cg | Mg | Total cyanogen | Sodium sulfate, g/ |
| 3 | 19.23 | 2.41 | 1.6 | 12.21 | 2.57 | 500.8 | 2.2 | 30.83 | 70.57 |
| 4 | 17.27 | 2.51 | 1.91 | 11.07 | 1.91 | 636.8 | 1.76 | 32.15 | 72.99 |
Example 1
(1) Preparing a desalting reagent solution, namely adding 5g of sodium cyanide into 150ml of water, stirring and dissolving to obtain a sodium cyanide solution with the concentration of 33.3g/l and the pH value of 13;
(2) acidifying and transforming; : adding 10ml of concentrated sulfuric acid into 20ml of water, stirring, cooling to room temperature, adding into a three-necked flask 1, wherein the temperature is 8 ℃, adding 150ml of the sodium cyanide solution prepared in the step 1 into the three-necked flask 1, detecting the pH value of the solution to be 1, and capping the feeding port of the three-necked flask;
(3) hydrogen cyanide stripping and hydrogen cyanide stripping liquid treatment; adding 100ml of sulfuric acid solution with the pH value of 2 into a gas washing bottle 2, filling 10g of hydrated lime into an absorption bottle 3, adding 150ml of water, adding 300ml of sodium hydroxide solution with the mass concentration of 10% into the absorption bottle 4, connecting a pipeline, starting an air blower 9, starting a water circulating vacuum pump 5 to pump air, blowing air into a three-neck flask 1 through an air blowing pipe 7 when the temperature of the solution displayed by a thermometer 6 is 12 ℃, blowing the air into the three-neck flask 1 through an air blowing pipe 7, allowing hydrogen cyanide gas generated in the three-neck flask 1 to enter the gas washing bottle 2, washing the hydrogen cyanide gas by water in the gas washing bottle 2, washing liquid drops carried in the gas, allowing the liquid drops to enter the absorption bottle 3, absorbing most of the hydrogen cyanide by slaked lime emulsion in the absorption bottle 3, reacting with calcium hydroxide to generate calcium cyanide solution, allowing the rest of the hydrogen cyanide to enter the absorption bottle 4, and reacting with the sodium; the tail gas is pumped away by a vacuum pump 5; after reacting for 120 minutes, stopping blowing, pouring out the slurry in the absorption bottle 3, filtering to obtain unreacted slag and 140ml of filtrate, sampling and testing, wherein the filtrate contains 13.8g/l of Cyanogen (CN);
(4) absorption desalination and sodium cyanide regeneration of hydrogen cyanide: and (3) mixing 100ml of filtrate prepared in the step (3) with 100ml of barren liquor water No. 3, slowly generating white precipitate, standing for 2 hours until no new precipitate is generated, filtering, drying filter residues for 2 hours at 120 ℃, weighing 3.1g, testing 95.5% of calcium sulfate, filtering 200ml of filtrate, sampling and testing 9.2g/l of sodium cyanide.
Example 2
(1) Preparing a desalting reagent solution, namely adding 13g of sodium cyanide into 200ml of water in No. 4 barren solution, stirring and dissolving to prepare a sodium cyanide solution with the concentration of 65g/l, and keeping the temperature at 16 ℃ and the pH value at 13;
(2) acidifying and transforming; adding 200ml sodium cyanide solution into a reactor 14, connecting a carbon dioxide gas bottle 11 with a pressure reducing valve 12 according to the figure 2, connecting a pressure gauge 13 and the reactor 14 by using a fluororubber pipe, opening a valve of the pressure reducing valve 12 for ventilation, then closing the valve, loosening the pipeline connected with the reactor 14, discharging air in the pipeline and the liquid level of the reactor 14, reconnecting the pipeline, opening the valve for ventilation, closing the valve of the pressure reducing valve 12 when the pressure indicated value of the pressure gauge is increased to 0.07MPa, putting the reactor 14 on a flask shaking machine 15 for fixation, starting the flask shaking machine, observing the pressure value change of the pressure gauge 13, opening the valve for ventilation when the pressure is reduced to 0.5MPa, increasing the indicated value of the pressure gauge to 0.07MPa, closing the valve of the pressure reducing valve 12, repeating the operation, after 60 minutes, keeping the indicated value of the pressure gauge to be no longer reduced to 0.045MPa, and reaching the end point of the reaction, closing a valve of the pressure reducing valve 12, closing the bottle shaking machine, taking the reactor 14 from the bottle shaking machine, releasing the pipeline, and enabling the pH of the carbonation reaction liquid in the reactor to be 7, the liquid temperature to be 16 ℃ and the room temperature to be 16 ℃;
(3) hydrogen cyanide stripping absorption and hydrogen cyanide stripping liquid treatment; putting glass wool into a gas washing bottle 2, putting 30g of hydrated lime into an absorption bottle 3, adding 500ml of water, adding 300ml of sodium hydroxide solution with the mass concentration of 10% into the absorption bottle 4, connecting a pipeline, starting an air blower 9, starting a water circulating vacuum pump 5 to pump air, wherein the temperature of the solution displayed by a thermometer 6 is 16 ℃, blowing air into a three-neck flask 1 through an air blowing pipe 7, introducing hydrogen cyanide gas generated in the three-neck flask 1 into the gas washing bottle 2, removing liquid drops carried in the gas, introducing the gas into the absorption bottle 3, absorbing most of hydrogen cyanide by slaked lime emulsion in the absorption bottle 3, reacting with calcium hydroxide to generate calcium cyanide solution, and introducing the rest of hydrogen cyanide into the absorption bottle 4 to react with the sodium hydroxide solution in the absorption bottle 4 to generate sodium cyanide; the tail gas is pumped away by a vacuum pump 5; after the reaction is carried out for 104 minutes, stopping blowing, pouring out the slurry in the absorption bottle 3, filtering to obtain unreacted slag and filtrate 430ml, drying the slag for 2 hours at 120 ℃, weighing 20.55g, sampling and testing the filtrate to obtain the product containing 11.6g/l of Cyanogen (CN);
(4) desalting and sodium cyanide regeneration: mixing 250ml of filtrate prepared in the step (3) with 100ml of No. 1 barren solution to slowly generate white precipitate, standing for 2 hours until no new precipitate is generated, filtering, drying filter residue at 120 ℃ for 2 hours, weighing 3.75g, testing 97.5% of calcium sulfate, testing 350ml of filtrate, and sampling to test 8.1g/l of sodium cyanide.
Example 3
(1) Preparing a desalting reagent solution, namely adding 6g of sodium cyanide into 164ml of water, stirring and dissolving to prepare a sodium cyanide solution with the concentration of 36.6g/l, wherein the pH value is 13 and the temperature is 15 ℃;
(2) acidifying and transforming; adding 164ml sodium cyanide solution into a reactor 14, connecting a carbon dioxide gas bottle 11 with a pressure reducing valve 12 according to the figure 2, connecting a pressure gauge 13 and the reactor 14 by using a fluororubber pipe, opening a valve of the pressure reducing valve 12 for ventilation, then closing the valve, loosening a pipeline connected with the reactor 14, discharging air in the pipeline and the liquid level of the reactor 14, reconnecting the pipeline, opening the valve for ventilation, closing the valve of the pressure reducing valve 12 when the pressure indicated value of the pressure gauge is increased to 0.07MPa, putting the reactor 14 on a flask shaking machine 15 for fixing, starting the flask shaking machine, observing the pressure value change of the pressure gauge 13, opening the valve for ventilation when the pressure is reduced to 0.5MPa, increasing the indicated value of the pressure gauge to 0.07MPa, closing the valve of the pressure reducing valve 12, repeating the operation, keeping the pressure indicated value of the pressure gauge to 0.047MPa after 60 minutes, and stopping the reaction, closing a valve of the pressure reducing valve 12, closing the bottle shaking machine, taking the reactor 14 from the bottle shaking machine, loosening the pipeline, and ensuring that the pH of the carbonation reaction liquid in the reactor 14 is 7.5, the liquid temperature is 16 ℃ and the room temperature is 16 ℃;
(3) desalination by stripping absorption of hydrogen cyanide and causticization treatment of hydrogen cyanide stripping liquid
(3.1) stripping, absorbing and desalting hydrogen cyanide; adding 160ml of the carbonation reaction liquid prepared in the step (2) into a three-neck flask 1, putting glass wool into a gas washing bottle 2, adding 530ml of water in No. 3 lean solution into an absorption bottle 3, connecting the three-neck flask (1), the gas washing bottle (2) and the absorption bottle (3) by using a fluororubber pipe, canceling an absorption bottle 4 and a water circulation vacuum pump 5, starting an air blower 9, blowing air into the three-neck flask 1 through an air blowing pipe 7, controlling the solution temperature displayed by a thermometer 6 to be 21 ℃, enabling hydrogen cyanide generated in the three-neck flask 1 to enter the gas washing bottle 2, removing a part of liquid drops carried in the gas, enabling the liquid drops to enter the absorption bottle 3, absorbing the hydrogen cyanide by slaked lime emulsion in the absorption bottle 3, reacting the hydrogen cyanide with calcium hydroxide to generate calcium cyanide, reacting the calcium cyanide with sodium sulfate to generate calcium sulfate and sodium cyanide, and pumping off tail gas through an air draft cabinet; in the absorption reaction process, a small amount of slaked lime is added into the absorption bottle 3 in several times, the pH value of the slurry is kept to be not less than 13, after the reaction is carried out for 60 minutes, a hydrogen cyanide detector is used for detecting that the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 is 0, the blast is stopped, and the adding amount of the slaked lime is 6.01 g;
further, pouring out the stripping reaction liquid in the three-necked bottle 1 in the step (3), detecting the pH value to be 9, adding the reaction liquid into a reactor 14, and carrying out secondary carbonation reaction according to the step (2), wherein the reaction time is 10 minutes, the carbon dioxide pressure is 0.06-0.053 MPa, and the end point pH is 7;
further, according to the step of the step (3), the second carbonation reaction liquid (pH 9) was subjected to a second blowing, absorbing and desalting reaction for 50 minutes, and the amount of slaked lime was 2.21 g;
further, carrying out third carbonation on the secondary stripping reaction liquid (with the pH value of 9) according to the step (2), wherein the reaction time is 10 minutes, the end point pH value is 7, and the temperature of the carbonated liquid is 21 ℃;
further, carrying out a stripping absorption reaction on the third carbonated solution according to the step (3), wherein the reaction time is 62 minutes, the reaction temperature is 16 ℃, detecting the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 to be 0 by using a hydrogen cyanide detector, stopping blowing, and adding 1.3g of slaked lime;
further, filtering the third absorption reaction slurry to obtain desalting slag and desalting filtrate, wherein the desalting slag is not washed and is directly dried at 120 ℃, and 11.01g of the desalting slag is weighed, the calcium sulfate content of the desalting slag is 45.63 percent, the desalting filtrate is 520ml, and the desalting filtrate contains 55.36g/l of sodium sulfate and 6.1g/l of Cyanide (CN);
the consumption of lime in the desalting reaction is 9.52g in total, and the output desalting slag is 11.01g in total;
(3.2) causticizing the hydrogen cyanide stripping liquid: taking 160ml of the third stripping reaction liquid obtained in the step (3) out of the three-necked bottle 1, pouring the third stripping reaction liquid into a beaker, measuring the pH value to be 9, and sampling and detecting the Cyanogen (CN) content to be 0.07 g/l; adding slaked lime into the rest 146ml of blow-off reaction liquid while stirring for carrying out causticization reaction, simultaneously detecting the pH value of the solution, keeping the reaction temperature at 17 ℃, stopping adding slaked lime when the pH value reaches 11, continuing stirring for 5 minutes, carrying out vacuum filtration to obtain 134ml of causticized slag and causticized filtrate, wherein the causticization reaction time is 60 minutes, and 36.12g of lime is consumed; the causticized slag is dried and weighed 34.14g, and the causticized filtrate contains 8.3g/l of sodium hydroxide.
Example 4
(1) Preparing a desalting reagent solution, namely adding 26g of sodium cyanide into 200ml of barren solution No. 1, stirring and dissolving to prepare a 130g/l sodium cyanide solution, wherein the pH value is 13 and the temperature is 17 ℃;
(2) acidifying and transforming; adding 200ml sodium cyanide solution into a reactor 14, connecting a carbon dioxide gas bottle 11 with a pressure reducing valve 12 according to the figure 2, connecting a pressure gauge 13 and the reactor 14 by using a fluororubber pipe, opening a valve of the pressure reducing valve 12 for ventilation, then closing the valve, loosening a pipeline connected with the reactor 14, discharging air in the pipeline and the liquid level of the reactor 14, reconnecting the pipeline, opening the valve for ventilation, closing the valve of the pressure reducing valve 12 when the pressure indicated value of the pressure gauge is increased to 0.07MPa, putting the reactor 14 on a flask shaking machine 15 for fixation, starting the flask shaking machine, observing the pressure value change of the pressure gauge 13, opening the valve for ventilation when the pressure is reduced to 0.3MPa, increasing the indicated value of the pressure gauge to 0.07MPa, closing the valve of the pressure reducing valve 12, repeating the operation, keeping the indicated value of the pressure gauge to be 0.032MPa after 120 minutes, and stopping the reaction, closing a valve of the pressure reducing valve 12, closing the bottle shaking machine, taking the reactor 14 from the bottle shaking machine, loosening the pipeline, and enabling the pH of the carbonation reaction liquid in the reactor to be 9, the liquid temperature to be 17 ℃ and the room temperature to be 16 ℃;
(3) hydrogen cyanide stripping absorption and hydrogen cyanide stripping liquid treatment;
(3.1) stripping and absorbing desalting of hydrogen cyanide; adding 200ml of the carbonation reaction liquid prepared in the step (2) into a three-mouth bottle 1, adding glass wool into a gas washing bottle 2, adding 520ml of the absorption desalting liquid produced in the example 3 into an absorption bottle 3, mixing the three-mouth bottle 1 and the gas washing bottle 2, the absorption bottle (3) is connected by a fluororubber pipe, the absorption bottle 4 and the water circulation vacuum pump 5 are cancelled, the blower 9 is started, air is blown into the three-mouth flask 1 through the blowing pipe 7, the temperature of the solution displayed by the thermometer 6 is 21 ℃, hydrogen cyanide generated in the three-mouth flask 1 enters the gas washing bottle 2, most of liquid drops carried in the gas are removed, the hydrogen cyanide enters the absorption bottle 3, the hydrogen cyanide is absorbed by slaked lime emulsion in the absorption bottle 3, the hydrogen cyanide reacts with calcium hydroxide to generate calcium cyanide, the calcium cyanide reacts with sodium sulfate to generate calcium sulfate and sodium cyanide, and tail gas is pumped away through the exhaust cabinet; in the absorption reaction process, adding a small amount of slaked lime into an absorption bottle in batches, keeping the pH value of slurry to be not less than 13, detecting the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 by using a hydrogen cyanide detector after reacting for 44 minutes, stopping blowing, and adding 15.5g of slaked lime;
further, pouring out the reaction stripping liquid in the three-mouth bottle 1 in the step (3), detecting the pH value to be 9, adding the reaction stripping liquid into the reactor 14, and carrying out secondary carbonation reaction according to the step (2), wherein the reaction time is 20 minutes, the carbon dioxide pressure is 0.07-0.035 MPa, and the end point pH is 7.5;
further, according to the step of the step (3), carrying out secondary carbonation reaction liquid for the second time, carrying out air stripping absorption desalting reaction for 60 minutes, wherein the adding amount of slaked lime is 10.78 g;
further, carrying out third carbonation on the secondary stripping reaction liquid according to the step (2), wherein the reaction time is 39 minutes, the end point pH is 7, and the temperature of the carbonated liquid is 12 ℃;
further, carrying out air stripping absorption reaction on the third carbonated solution according to the step (3), wherein the reaction time is 47 minutes, the reaction temperature is 12 ℃, detecting the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 to be 0 by using a hydrogen cyanide detector, stopping blowing, and adding 9.22g of calcium hydroxide;
further, filtering the third absorption reaction slurry, washing with a small amount of water to obtain desalting slag and desalting filtrate, drying and weighing 52.79g of the desalting slag, wherein the content of calcium sulfate in the desalting slag is 33.39%, the content of the desalting filtrate is 575ml, the content of sodium sulfate is 37.11g/l, and the content of Cyanide (CN) is 23.6 g/l;
the consumption of slaked lime in the desalting reaction accounts for 35.5g, and the output desalting slag accounts for 33.39 g;
and (3.2) causticizing the hydrogen cyanide blow-off liquid: taking 200ml of the third stripping reaction liquid obtained in the step (3) out of the three-necked bottle 1, pouring the third stripping reaction liquid into a beaker, measuring the pH value to be 9, and sampling and detecting the Cyanogen (CN) content to be 0.03 g/l; adding slaked lime into the rest 190ml of blow-off reaction liquid while stirring for carrying out causticization reaction, simultaneously detecting the pH value of the solution, controlling the reaction temperature to be 18 ℃, stopping adding lime when the pH value reaches 13, continuing stirring for 5 minutes, carrying out vacuum filtration to obtain 120ml of causticized slag and causticized filtrate, controlling the causticization reaction time to be 58 minutes, and consuming 70g of lime; the causticized slag is dried and weighed 72.65g, and the causticized filtrate contains 29.06g/l of sodium hydroxide.
Example 5
(1) Preparing a desalting reagent solution, namely adding 13g of sodium cyanide into 200ml of barren solution No. 2, stirring and dissolving to obtain a sodium cyanide-containing solution with the pH value of 13; the temperature is 16 ℃;
(2) acidifying and transforming: after the carbonation reaction time is 152 minutes, the pressure indicated value of the pressure gauge is maintained to be 0.02MPa and not to be reduced, the reaction reaches the end point, the valve of the pressure reducing valve 12 is closed, the bottle shaking machine is closed, the reactor 14 is taken down from the bottle shaking machine, the pipeline is loosened, the pH of the carbonation reaction liquid in the reactor is 7, the liquid temperature is 21 ℃, and the room temperature is 21 ℃;
(3) hydrogen cyanide is stripped, absorbed and desalted and sodium cyanide is regenerated; adding 520ml of the absorption desalting solution produced in the example 3 into an absorption bottle 3, reacting for 33 minutes, detecting the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 by using a hydrogen cyanide detector to be 0ppm, stopping blowing, adding calcium hydroxide at one time, wherein the adding amount is 20g, and the reaction temperature is 17 ℃;
further, pouring out the reaction stripping liquid in the three-necked bottle 1 in the step (3), detecting the pH value to be 9, adding the reaction stripping liquid into a reactor 14, and carrying out secondary carbonation reaction according to the step (2), wherein the reaction time is 24 minutes, the carbon dioxide pressure is 0.07-0.055 MPa, the end-point pH is 7.0, and the reaction temperature is 17 ℃; detecting that the carbonization liquid contains 0.52g/l of Cyanogen (CN);
further, according to the step of the step (3), carrying out secondary carbonation reaction liquid, carrying out secondary blowing-off absorption desalting reaction for 68 minutes, wherein the addition amount of slaked lime is 10g at one time, and the reaction temperature is 17 ℃; (ii) a
Further, carrying out a third carbonation reaction on the secondary stripping reaction liquid according to the step (2), wherein the reaction time is 20 minutes, the end point pH is 7, and the temperature of the carbonation liquid is 12 ℃;
further, carrying out a stripping absorption reaction on the third carbonated solution according to the step (3), wherein the reaction time is 103 minutes, the reaction temperature is 12 ℃, a hydrogen cyanide detector is used for detecting that the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 is 27.8ppm, blowing is stopped, and the addition amount of calcium hydroxide is 0 g;
further, filtering the third absorption (desalination) reaction slurry to obtain desalination slag and desalination filtrate, directly drying the desalination slag for 2 hours at 120 ℃ without washing, weighing 30.80g, wherein the calcium sulfate content of the desalination slag is 40.44%, and the total desalination filtrate washing liquid is 450ml, 15.82g/l of sodium sulfate and 22.6g/l of Cyanide (CN);
the consumption of slaked lime in the desalting reaction accounts for 30g, and the output desalting slag accounts for 30.80 g;
172ml of stripping reaction solution containing 0.054g/l of cyanide
Example 6
(1) Preparing desalting reagent solution by adding 6g sodium cyanide into 200ml barren solution with water No. 3, stirring to dissolve to obtain 36.6g/l sodium cyanide solution with pH value of 13; the temperature is 16 ℃;
(2) acidifying and transforming; after the carbonation reaction time is 120 minutes, the indicated value of the pressure gauge is maintained at 0.03MPa and does not drop any more, the reaction reaches the end point, a valve of the pressure reducing valve 12 is closed, the bottle shaking machine is closed, the reactor 14 is taken down from the bottle shaking machine, the pipeline is loosened, the pH of the carbonation reaction liquid in the reactor is 7, the liquid temperature is 15 ℃, and the room temperature is 15 ℃;
(3) hydrogen cyanide is stripped, absorbed and desalted and sodium cyanide is regenerated; adding 500ml No. 2 barren solution into an absorption bottle 3, slowly adding slaked lime in batches, after reacting for 120 minutes, detecting the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 by using a hydrogen cyanide detector to be 0ppm, stopping blowing, wherein the adding amount of the slaked lime is 15g, and the reaction temperature is 10 ℃;
further, pouring out the stripping reaction liquid in the three-necked bottle 1 in the step (3), detecting the pH value to be 9, adding the reaction liquid into a reactor 14, and carrying out secondary carbonation reaction according to the step (2), wherein the reaction time is 60 minutes, the carbon dioxide pressure is 0.07-0.03 MPa, the end point pH is 7.0, and the reaction temperature is 14 ℃;
further, according to the step of the step (3), carrying out secondary carbonation reaction liquid, carrying out secondary blowing-off absorption desalting reaction for 70 minutes, slowly adding slaked lime in a sub-step manner, wherein the adding amount is 15g, and the reaction temperature is 14 ℃;
further, carrying out a third carbonation reaction on the secondary stripping reaction liquid according to the step (2), wherein the reaction time is 54 minutes, the end point pH value is 7, and the carbonation reaction temperature is 14 ℃;
further, carrying out a stripping absorption reaction on the third carbonated solution according to the step (3), slowly adding slaked lime in several times, reacting for 60 minutes at the reaction temperature of 12 ℃, detecting the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 to be 0ppm by using a hydrogen cyanide detector, stopping blowing, and adding 10g of slaked lime;
further, filtering the third absorption desalting reaction slurry to obtain desalting slag and desalting filtrate, wherein the desalting slag is not washed and is directly dried for 2 hours at 120 ℃, 43.69g of desalting slag is weighed, the calcium sulfate content of the desalting slag is 33.26 percent, the desalting filtrate is 380ml, the sodium sulfate content is 56.27g/l, and the Cyanogen (CN) content is 6.2 g/l;
the total consumption of lime in the desalting reaction is 40g, and the total output of desalting slag is 43.69 g;
the stripping reaction solution (200 ml) contained Cyanide (CN)0.07 g/l.
Example 7
(1) Preparing a desalting reagent solution, namely taking 410ml of desalting filter washing solution produced in example 5, 15.82g/l of sodium sulfate, 22.6g/l of Cyanide (CN) and pH value of 13; the temperature is 12 ℃;
(2) acidifying and transforming; after the carbonation reaction time is 120 minutes, the indicated value of the pressure gauge is maintained at 0.038MPa, when the indicated value does not fall any more, the reaction reaches the end point, a valve of a pressure reducing valve 12 is closed, a bottle shaking machine is closed, a reactor 14 is taken off from the bottle shaking machine, a pipeline is loosened, the pH of the carbonation reaction liquid in the reactor is 7, the liquid temperature is 12 ℃, and the room temperature is 11 ℃;
(3) hydrogen cyanide is stripped, absorbed and desalted and sodium cyanide is regenerated; 370ml of the absorption desalting solution produced in the example 6 is added into an absorption bottle 3, after the reaction is carried out for 157 minutes, a hydrogen cyanide detector is used for detecting the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 to be 0ppm, the blowing is stopped, calcium hydroxide is slowly added in a plurality of times, the adding amount is 33g, and the reaction temperature is 10 ℃;
further, pouring out the stripping reaction liquid in the three-mouth bottle 1 in the step (3), detecting the pH value to be 9, adding the reaction liquid into a reactor 14, and carrying out secondary carbonation reaction according to the step (2), wherein the reaction time is 60 minutes, the carbon dioxide pressure is 0.07-0.041 MPa, the end point pH is 7.0, and the reaction temperature is 9 ℃;
further, according to the step of the step (3), performing blowing-off absorption desalination reaction for the second time, wherein the reaction time is 70 minutes, calcium hydroxide is slowly added in a divided manner, the adding amount is 20g, and the reaction temperature is 9 ℃;
further, carrying out third carbonation on the secondary stripping reaction liquid according to the step (2), wherein the reaction time is 54 minutes, the end point pH is 7, and the carbonation reaction temperature is 8-11 ℃;
further, carrying out a stripping absorption reaction on the third carbonated solution according to the step (3), slowly adding slaked lime in several times, reacting for 139 minutes at the reaction temperature of 12 ℃, detecting the content of hydrogen cyanide gas at the outlet of the absorption bottle 3 to be 0ppm by using a hydrogen cyanide detector, stopping blowing, and adding 20g of slaked lime;
further, filtering the third stripping absorption reaction slurry to obtain desalted slag and desalted filtrate, wherein the desalted slag is not washed and is directly dried for 2 hours at 120 ℃, 78.18g of desalted slag is weighed, the calcium sulfate content of the desalted slag is 27.7 percent, 200ml of desalted filtrate contains 25.55g/l of sodium sulfate and 26g/l of Cyanogen (CN);
the consumption of slaked lime in the desalting reaction is 73g in total, and the produced desalting slag is 78.18g in total;
410ml of stripping reaction solution containing 0.01g/l of cyanide
The percentages in the above examples are mass percentages.
Those not described in detail in the specification are prior art known to those skilled in the art.
Claims (10)
1. A method for desalting water from barren liquor or barren liquor generated in a cyaniding gold extraction process is characterized by comprising the following steps of:
(1) preparing a desalting reagent solution, namely dissolving a desalting reagent and uniformly stirring to obtain the desalting reagent solution;
(2) acidifying and transforming: adding an acidic substance into the desalted reagent solution obtained in the step (1) to perform acidification and transformation reaction, and adjusting the pH value to obtain a mixed solution of hydrogen cyanide and salt;
(3) hydrogen cyanide stripping absorption and hydrogen cyanide stripping liquid treatment: when the acidic substance added in the step (2) is sulfuric acid or hydrochloric acid, blowing air into the mixed solution of hydrogen cyanide and salt obtained in the step (2), and blowing off the generated hydrogen cyanide to obtain hydrogen cyanide gas and a blowing-off reaction liquid; collecting the blown hydrogen cyanide gas, removing the blow-off reaction liquid carried by the hydrogen cyanide gas, absorbing by using an emulsion prepared from alkaline earth metal hydroxide to generate a water-soluble alkaline earth metal cyanide solution, and filtering to obtain the alkaline earth metal cyanide solution and absorption reaction slag;
when the acidic substance added in the step (2) is carbon dioxide, obtaining a mixed solution of hydrogen cyanide and sodium bicarbonate in the step (2), blowing off the hydrogen cyanide, adding slaked lime into the blowing-off reaction solution, stirring, carrying out a causticization reaction, and filtering to obtain causticized slag calcium carbonate and a sodium hydroxide solution or a sodium carbonate solution;
(4) desalting and sodium cyanide regeneration: and (3) mixing the alkaline earth metal cyanide solution obtained in the step (3) with barren liquor generated in the cyaniding gold extraction process or barren liquor water after heavy metal removal, reacting the alkaline earth metal cyanide with sodium sulfate in the barren liquor or barren liquor water to generate alkaline earth metal sulfate and sodium cyanide, and filtering to obtain alkaline earth metal sulfate filter residue and desalting filtrate containing the sodium cyanide.
2. The method for desalting water from barren liquor or barren liquor generated in a cyanidation gold extraction process according to claim 1, characterized in that: in the step (1), the desalting reagent is alkali metal cyanide or alkaline earth metal cyanide; the alkali metal cyanide is sodium cyanide or potassium cyanide; the alkaline earth metal cyanide is at least one of calcium cyanide, barium cyanide and strontium cyanide.
3. The process of claim 1 or 2 for the desalination of water from barren liquor or barren liquor produced during cyanidation for gold extraction, characterized in that: in the step (3), the method for removing the stripping reaction liquid carried by the hydrogen cyanide gas is carried out by washing or mechanical interception by glass wool.
4. The method for desalting the barren liquor or the barren liquor water generated in the cyanidation gold extraction process according to any one of claims 1 to 3, characterized by comprising the following steps: in the step (4), the obtained desalting filtrate containing sodium cyanide is returned to the step (1) as a desalting reagent cyanide solution.
5. The method for desalting the barren liquor or the barren liquor water generated in the cyanidation gold extraction process according to any one of claims 1 to 4, characterized by comprising the following steps: in the step (1), when the desalting reagent cyanide is dissolved, the solvent is at least one of water, a barren solution containing sodium sulfate, water in the barren solution, sodium cyanide and a solution containing sodium sulfate.
6. The method for desalting the barren liquor or the barren liquor water generated in the cyanidation gold extraction process according to any one of claims 1 to 5, characterized by comprising the following steps: and (3) when the acidic substance added in the step (2) is sulfuric acid, adjusting the pH value to 1-7.
7. The method for desalting the barren solution or the barren solution water generated in the cyanidation gold extraction process according to any one of claims 1 to 6, characterized by comprising the following steps: and (3) when the acidic substance added in the step (2) is carbon dioxide, adjusting the pH value to 7-9.
8. The method for desalting the barren solution or the barren solution water generated in the cyanidation gold extraction process according to any one of claims 1 to 7, characterized by comprising the following steps: in the step (3), the alkaline earth metal hydroxide is at least one of calcium hydroxide, barium hydroxide or strontium hydroxide; the liquid of the emulsion prepared by the alkaline earth metal hydroxide is at least one of water, barren solution, water in the barren solution or solution containing sodium sulfate; the mass concentration of the emulsion prepared from the alkaline earth metal hydroxide is 0.1-10%.
9. The method for desalting water from barren liquor or barren liquor generated in a cyanidation gold extraction process according to claim 8, characterized in that: in the step (3), when the emulsion prepared by the alkaline earth metal hydroxide is barren solution, barren solution water or a solution containing sodium sulfate, desalting reaction is carried out in the step (3), water-soluble alkaline earth metal cyanide obtained after elution reaction is reacted with sulfate ions in the sodium sulfate solution to generate a mixed solution of desalting residue precipitate and sodium cyanide, and filtering is carried out to obtain the desalting residue alkaline earth metal sulfate and the sodium cyanide solution.
10. The method for desalting the barren solution or the barren solution water generated in the cyanidation gold extraction process according to any one of claims 1 to 9, characterized by comprising the following steps: in the step (4), the pH value of the causticization reaction is more than or equal to 13.
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