CN87103312A - Process for gold extraction by acid leaching and polyurethane foam concentration and device - Google Patents
Process for gold extraction by acid leaching and polyurethane foam concentration and device Download PDFInfo
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- 238000002386 leaching Methods 0.000 title claims abstract description 101
- 239000010931 gold Substances 0.000 title claims abstract description 44
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 44
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229920005830 Polyurethane Foam Polymers 0.000 title claims abstract description 41
- 239000011496 polyurethane foam Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 40
- 238000000605 extraction Methods 0.000 title claims abstract description 6
- 239000002253 acid Substances 0.000 title claims description 63
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 11
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 90
- 239000007788 liquid Substances 0.000 claims description 41
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 35
- 229910017604 nitric acid Inorganic materials 0.000 claims description 35
- 238000005406 washing Methods 0.000 claims description 23
- 238000001179 sorption measurement Methods 0.000 claims description 18
- 238000010521 absorption reaction Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000003723 Smelting Methods 0.000 claims description 15
- 239000002699 waste material Substances 0.000 claims description 13
- 239000004568 cement Substances 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 7
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical class [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000003463 adsorbent Substances 0.000 claims description 3
- 239000000945 filler Substances 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 150000003672 ureas Chemical class 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims description 2
- 238000005325 percolation Methods 0.000 claims description 2
- 241001417490 Sillaginidae Species 0.000 claims 1
- 125000000687 hydroquinonyl group Chemical group C1(O)=C(C=C(O)C=C1)* 0.000 claims 1
- 239000005416 organic matter Substances 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 6
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005065 mining Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 43
- 239000004576 sand Substances 0.000 description 31
- 239000006260 foam Substances 0.000 description 19
- 238000003860 storage Methods 0.000 description 17
- 238000004519 manufacturing process Methods 0.000 description 13
- 239000000843 powder Substances 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 229920003023 plastic Polymers 0.000 description 9
- 239000004033 plastic Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 6
- 238000002791 soaking Methods 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 239000002912 waste gas Substances 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 210000003298 dental enamel Anatomy 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 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 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 241000863480 Vinca Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- GUWKQWHKSFBVAC-UHFFFAOYSA-N [C].[Au] Chemical compound [C].[Au] GUWKQWHKSFBVAC-UHFFFAOYSA-N 0.000 description 1
- 239000004063 acid-resistant material Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052586 apatite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
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- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- VSIIXMUUUJUKCM-UHFFFAOYSA-D pentacalcium;fluoride;triphosphate Chemical compound [F-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O VSIIXMUUUJUKCM-UHFFFAOYSA-D 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Images
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Manufacture And Refinement Of Metals (AREA)
Abstract
本发明为一种从矿石提取金的方法和装置。本法采用王水浸取、聚氨酯泡沫分离富集、对苯二酚还原。金回收率在90%~95%以上,具有回收率高、成本低、设备简单、投资少等特点。备有有效的环境保护措施。不仅适用于氧化矿,还适用于硫化矿等多种矿石的提取。甚宜于资源分散的中、小型矿区使用。The present invention is a method and device for extracting gold from ore. This method adopts aqua regia leaching, separation and enrichment of polyurethane foam, and reduction of hydroquinone. The gold recovery rate is above 90% to 95%, and has the characteristics of high recovery rate, low cost, simple equipment and less investment. Effective environmental protection measures are in place. It is not only suitable for oxidized ore, but also suitable for the extraction of various ores such as sulfide ore. It is very suitable for medium and small mining areas with scattered resources.
Description
The invention relates to a smelting method and a device for extracting gold by aqua regia leaching and polyurethane foam separation and enrichment
Currently, gold in ore is generally extracted by cyanidation, which is mainly 'carbon pulp cyanidation' through leaching with sodium cyanide, adsorption with activated carbon and electrolytic reduction. The method has high recovery rate (generally about 90 percent) and low cost, and is already used for production in 1973 by Homestake mining company in America, but the method is generally only suitable for oxidized ores, and the leaching rate of ores with high sulfur content is low by adopting a cyanidation method, for example, the leaching rate is 24-78 percent when the ore is used for extracting the pyrite in the newborn. Therefore, oxidation treatment is required before leaching, and the investment for building factories is large by adopting biological oxidation or roasting oxidation. In recent years, the vinca gold institute has conducted more systematic studies on the carbon pulp cyanide process and has been used for production. In order to reduce the production investment, a cyaniding heap leaching method (namely a method of leaching by a heap leaching pool, activated carbon adsorption and electrolytic reduction) is also adopted, but the recovery rate is inferior (60-90%), and the method is also only suitable for extracting the oxidized ore.
In recent years, gold ores are found in Guangdong province and some areas, but most of the gold ores are scattered, and in the development stage, a smelting method of sodium cyanide leaching, zinc wire reduction and sulfuric acid impurity removal is mostly adopted, although the method is low in investment, the recovery rate is very low (generally 40-60%), and the pollution is serious.
The polyurethane foam separation and enrichment gold is used as a separation means in chemical analysis, but a smelting method is not reported, and the smelting method and the separation method of analytical chemistry have great differences in the existence form, cost accounting, process flow, scale and the like of gold.
The invention aims to provide a smelting method and a device for separating, enriching and extracting gold by acid leaching polyurethane foam, which have the advantages of high recovery rate, simple equipment, low cost, less investment, less pollution and wide adaptability.
The acid leaching polyurethane foam gold extraction method comprises the working procedures of ore crushing, testing, leaching, separation and enrichment, washing and impurity removal, reduction, carrier removal, smelting, cleaning and the like.
1. Crushing: the ore is crushed into-22 meshes and +22 meshes by a hammer mill or other means.
2. And (3) testing: the appropriate amount of crushed ore was subjected to the following measurements:
(1) determining the gold content of the ore: the determination can be carried out by TMK carrier extraction colorimetry or other gold detection methods.
(2) Determining the dosage of hydrochloric acid and nitric acid: the amounts of the two acids normally consumed for leaching one ton of ore are 0.200.35 tons of industrial hydrochloric acid (specific gravity 1.15, content 30%) and 0.040.15 tons of industrial nitric acid (specific gravity 1.30, content 65%), respectively. The method has the advantages that different types of ores consume different amounts of aqua regia, and the ore components are different from each other in the amount of hydrochloric acid and nitric acid, so that the optimal amount of hydrochloric acid and nitric acid consumed by the ore is measured, the leaching rate is improved, economy is promoted, and the method has practical economic significance, and the dosage of the selected nitric acid is as small as possible because the nitric acid is higher than the hydrochloric acid in price.
The test method for determining the dosage of the hydrochloric acid and the nitric acid comprises the following steps: taking a certain amount of ore sand, leaching in a production process similar to the production process, wherein the leaching time is 4-6 days (the leaching time is properly prolonged when the temperature is lower than 10 ℃).
The method comprises the following specific steps: weighing 50 g of crushed ore sand in a plurality of beakers respectively, adding 30% industrial hydrochloric acid in different amounts into each beaker, adding water until the surface of the ore sand is soaked, stirring, covering surface glass, and soaking for 1 hour. Different amounts of 65% industrial nitric acid were added to each beaker and stirred. Soaking for 2.5-3 days (stirring twice a day). The first amount of 1/4% industrial hydrochloric acid and 1/4% industrial nitric acid were added to each cup (e.g., 12 ml of 30% industrial hydrochloric acid and 4 ml of 65% industrial nitric acid were added before a cup, 3 ml of 30% industrial hydrochloric acid and 1 ml of 65% industrial nitric acid were added). Stirring and soaking for 1.5-2 days (stirring twice every day). Filtering, and washing with hydrochloric acid solution of more than 5% (volume ratio) until the filtrate is colorless. And (3) measuring the gold content in the ore, calculating the leaching rate from the measurement result, calculating the cost from the leaching rate and the acid dosage, and selecting the optimal hydrochloric acid dosage and the optimal nitric acid dosage.
Although the test method is accurate and reliable, the test method is tedious and time-consuming, so that a simple and feasible method can be selected according to the local resource condition. The following methods can generally be used: taking 50 g of ore sand, wetting the ore sand with a little water, and gradually and intermittently adding 30% industrial hydrochloric acid at 40-50 ℃ until no obvious reaction occurs. And adding hydrochloric acid according to the weight ratio of the ore sand to the hydrochloric acid of 1: 0.07-0.10, wherein the total amount is the amount of the hydrochloric acid required by leaching (if 5.0 g of hydrochloric acid is used until no obvious reaction exists, the amount of the hydrochloric acid is 5.0+50 x (0.07-0.10) ═ 8.5-10 g). The addition of 65% industrial nitric acid at this temperature was continued intermittently until no significant reaction was observed. The amount used in this case is the amount of nitric acid required for leaching.
The test method is simple, but not precise enough, and may use insufficient amount of nitric acid during production, but can sample and test during production, supplement nitric acid properly when necessary and prolong leaching time.
The test results of the dosage of hydrochloric acid and nitric acid of several ore samples are as follows:
(1) sulfide ore (high silicon), ore powder color: grey black, ore source: in the Guangdong Qingyuan Xinzhou region, the ore grade is as follows: 50 g/ton, test temperature: 20 ℃, ore dosage: 50 g, water usage: 10 ml, hydrochloric acid concentration: specific gravity 1.19, content 38%, nitric acid concentration: specific gravity 1.40, content 68% (the temperature, ore dosage, water dosage, hydrochloric acid concentration and nitric acid concentration of the following tests are the same).
Hydrochloric acid amount (ml): 5.06.37.58.8
Amount of nitric acid used (ml): 1.81.51.51.8
Leaching rate (%): 86.594.495.297.2
(2) Oxidized ore (containing small amount of copper sulfide, etc.)
Color of the mineral powder: yellow-brown, ore source: guangdong Gaoyuan river platform area, the ore grade: 137 g/ton.
Hydrochloric acid amount (ml): 9.511.418.828.837.556.2
Amount of nitric acid used (ml): 3.03.86.39.412.518.8
Leaching rate (%): 93.296.897.797.998.399.4
(3) Sulfide ore, color of ore powder: black gray, ore source: in the Guangdong engde Jiulong district, the ore grade: 42 g/ton.
Hydrochloric acid amount (ml): 10.025.030.030.0
Amount of nitric acid used (ml): 2.08.020.035.0
Leaching rate (%): 35547491.0
3. Leaching: the crushed ore is placed in a sealed acid-resistant pool with a percolation device consisting of a trough, a cover plate, cobblestone sand and the like, and measured amounts of hydrochloric acid and nitric acid are added, preferably, the acid is added to leach the metal splashes, and then the nitric acid is added, so that the amount of the nitric acid is reduced, the cost is reduced, and excessive sulfur precipitation is avoided.
The hydrochloric acid and the nitric acid can be added in a leaching process in a divided manner, so that a large amount of fresh aqua regia is always available, and gold dissolution is facilitated.
In the leaching process, the ore sand is required to be in full contact with the dissolved acid, the finer the ore crushing is, the more beneficial the gold leaching is, but the more easy the ore powder hardening is, and the leaching difficulty is caused. For this purpose, the ore should not be crushed too finely, the sand layer should not be too thick (generally below 40 cm), coarse sand or coarse low-grade sand may be infiltrated into the ore powder, and a suitable amount of inert filler, such as hard foam or other inert filler, may be infiltrated into the sand. Meanwhile, the acid can be directly added into the bottom of the pool, so that the acid permeates from the bottom to the top. In order to facilitate the formation of aqua regia by hydrochloric acid and nitric acid, leaching solution flows out from the upper layer and the lower layer of the ore simultaneously, and acid solution on the upper layer of the ore flows downwards by virtue of a liquid separator. The liquid separator can be made into a float bowl with a hole by an acid-proof plastic bottle, and can be tied into a piece of rigid foam plastic in order to enable the bottle to float. One end of the float bowl is tied with a rope and is laid down when needed and lifted when not used, the other end of the float bowl is connected with a liquid outlet pipe by an acid-resistant hose, and a liquid outlet pipe orifice is inserted into a sand layer on the cobblestones. The leaching solution can be pumped into a leaching pool by an acid-proof pump for recycling. The leaching time is properly prolonged when the temperature is lower than 10 ℃ and the leaching time is generally 4-6 days at normal temperature. The waste gas generated by the reaction is absorbed by an absorption tank which is connected in series with three cement tanks (the first cement tank is made of acid-resistant cement) containing water, saturated limewater and saturated urea. In order to facilitate the absorption of waste gas, an acid-resistant air pump can be arranged.
4. Separation and enrichment: gold in the leached solution is adsorbed by taking polyurethane foam as an adsorbent, namely, the leaching solution completely passes through a device filled with polyurethane foam, the device can be made by filling the polyurethane foam in an acid-resistant pipe, the polyurethane foam in the pipe is not pressed too tightly and is not easy to loose too, the using amount of the polyurethane foam is determined according to the gold content of ore, and the weight ratio of the gold content of the ore to the using amount of the polyurethane foam is 1: 15-25. In order to prevent the oxidation of foams, an antioxidant is added into the leaching solution before adsorption, wherein the antioxidant can be urea, and the dosage of the urea is as follows: the weight ratio of the ore to the urea is 1: 0.004-0.006, and in order to avoid mortar flowing into the adsorption pipe during adsorption and filtering the leaching solution before adsorption, a filtering device similar to a leaching pool structure, namely a filtering device provided with grooves, a cover plate, cobblestones, sand and the like, can be arranged for filtering.
5. Washing to remove impurities: industrial hydrochloric acid with the concentration of more than 3% is used as a detergent, mainly used for washing polyurethane foam to remove other metals except gold, and washed until the effluent washing liquid is yellow.
6. Reduction: gold adsorbed by polyurethane foam after impurity removal is reduced by using organic matters with reducibility as reducing agents, preferably hydroquinone is selected as the reducing agents, and the dosage of the hydroquinone is 1-2 times, generally 1.2 times, of the weight of the gold contained in the ore. The reducing agent should be allowed to react with the gold in the polyurethane foam sufficiently, and the time is generally 20-30 minutes. The reduced polyurethane foam can be squeezed out of the solution in the foam by a squeezing machine. The solution was filtered through ordinary filter paper, the filtrate was discarded, and the polyurethane foam was placed in a clean room and dried.
7. Removing the carrier: namely, the polyurethane foam and the filter paper are burned off. The polyurethane foam, the filter residue and the filter paper are firstly carbonized at about 250 ℃ until no reddish brown gas escapes. The waste gas generated in the carbonization process can be serially connected with absorption devices respectively containing dilute acid, lime water and solid alkali-lime for absorption, and an air pump can be arranged for facilitating the absorption. The carbide is dried and burned at a high temperature of about 700 ℃ until no black color exists.
8. Smelting: and smelting the gold ash into blocks at high temperature. For further purification, borax, preferably anhydrous borax, is added to the gold ash before smelting, and the weight ratio of gold to borax is more than 1: 0.5, generally 1: 0.5-1. Smelting the mixture into blocks at a high temperature of not less than 1200 ℃, wherein the temperature is generally 1200-1250 ℃. The smelting time is 25-30 minutes.
9. Cleaning: after the production is finished, the hard foamed plastics in the ore sand are recovered, water can be added into the leaching pool, and the hard foamed plastics are stirred to float and fished out. The waste acid can be used for replacing water and washing ore during secondary production, and the redundant waste acid can be used for treating apatite or producing phosphate fertilizer or used for other purposes, and can also be placed in loess, limestone and the like for natural absorption.
The device for extracting gold by acid leaching polyurethane foam comprises a leaching system (shown in figure 1) consisting of a plurality of acid-resistant pools, an acid-resistant pump absorption device, a feeding pool and an absorption device, wherein the acid-resistant pool for leaching is a leaching pool, the acid-resistant pool for storing leaching liquid is a liquid storage pool, the acid-resistant pool for washing is a washing pool, and the acid-resistant pool for storing waste acid is a waste acid pool. The pools have a certain level difference (see figure 2), and the pools are connected with each other by acid-proof pipes, and each acid-proof pipe is provided with a faucet capable of adjusting the flow rate. In order to facilitate the recycling of leaching acid, each pool is provided with an acid-resistant pipe which is communicated with an acid-resistant pump, and a plurality of taps are arranged on the acid-resistant pipe so as to facilitate the circulation of solution and the washing of the acid-resistant pump. The absorption device is formed by connecting three cement ponds respectively containing water, saturated limewater and saturated urea in series, wherein the cement ponds containing water are made of acid-resistant cement, and are respectively communicated with the leaching pond and the liquid storage pond by an acid-resistant pipe with a tap. In order to facilitate the absorption of waste gas, an acid-resistant air pump can be arranged. The feeding tank is used for feeding, and an acid-proof pipe with a tap is communicated with the liquid storage tank. Both the leaching tank and the liquid storage tank are provided with liquid level meters made of transparent acid-resistant materials, such as acid-resistant plastic tubes, so that the liquid and the reaction conditions in the tank can be observed during production. The leaching tank and the liquid storage tank are provided with sealing facilities, and screws and acid-resistant rubber gaskets can be arranged on the tank wall to enable the plate cover to be tightly sealed. The adsorption device is characterized in that polyurethane foam plastic is filled in an acid-resistant pipe, an adsorption pipe is arranged at the bottom of a washing pool, leaching solution passes through the washing pool and completely passes through the adsorption pipe, and waste acid flows into a waste acid pool. A groove with the depth of about 10 cm and the width of about 10 cm is arranged at one side of the bottoms of the leaching pond and the liquid storage pond close to the solution outlet, in order to prevent the groove from being blocked by the mortar, a 7-shaped cover plate is used for covering the groove at a position which is 10 cm away from the bottom of the pond, one side of the cover plate is provided with a hole, and the other side of the cover plate, which is vertical to the bottom of the pond, can be supported by a support column made of an acid. In order to accelerate infiltration and make circular flow, the bottom of the two pools is padded with cobbles about 10 cm high, and a layer of coarse sand about 5 cm high is laid on the cobbles. The bottom of the groove is provided with 1 to a plurality of guide pipes with holes, one end of each guide pipe is sealed and inserted into the cobble layer, and the other end of each guide pipe passes through the 7-shaped cover plate and is communicated with the groove. A plurality of taps capable of adjusting the flow rate of the solution are arranged at the bottom of the two tanks close to the groove, wherein one tap is arranged at the bottom of the groove, and the other taps are arranged at the upper part of the tank. In order to facilitate the leaching of the leaching tank, a liquid separator buoy is arranged in the leaching tank, the liquid separator buoy can be made of an acid-resistant plastic bottle, one end of the liquid separator buoy is connected with an acid-resistant hose through an acid-resistant hose, the acid-resistant hose is inserted into a sand layer of cobble soil, the other end of the liquid separator buoy is tied with a rope, and the liquid separator buoy is put down when in use and lifted when not in use. (see leaching pool side section view 3)
The present invention has been completed in this way
(1) Crushing: crushing the sulfur-containing ore with the grade of 81 g/ton to ore powder (A) with the mesh of minus 22 by a hammer type dry powder machine, and crushing the sulfide ore with the grade of 8.8 g/ton to ore sand (B) with the shape of fine sand (most of the sulfide ore is plus 22 meshes) by a hammer type wet powder machine.
(2) Test (determination of acid amount): taking 50 g of ore, wetting the ore with a little water, adding a small amount of 30% industrial hydrochloric acid of about 2 g at the temperature of 40-50 ℃, stirring, adding a small amount of acid when bubbles stop generating, and continuing to add until no obvious bubbles are generated. 10.0 g of hydrochloric acid was removed at this time, and 5.0 g of hydrochloric acid was added. Similarly, 65% industrial nitric acid was added, and 10.0 g was used until no significant bubbles were formed. Accordingly, the weight ratio of 30% hydrochloric acid to 65% nitric acid was determined as: ore, 30% hydrochloric acid, 65% nitric acid 1: 0.30: 0.20.
(3) Leaching: and (3) uniformly mixing 180 kg of mineral powder (A) and 320 kg of mineral powder (B), taking about 0.08 cubic hard foam plastic (hereinafter referred to as hard foam), and tearing into irregular blocks with the diameter of 1-3 cm. And (3) placing the mixed ore sand and hard foam in a leaching pool, and uniformly distributing the hard foam in the ore sand (the surface layer is 4-5 cm and does not contain the hard foam). The cover plate is covered and sealed, the absorption device is connected, the faucet is closed, and the float bowl of the liquid separator is hoisted. The reservoir was also sealed. From the feed tank, 120 kg of 30% industrial hydrochloric acid (amount determined in the test 4/5) was added to the reservoir, 30 kg of water were added (the solution was allowed to soak through the sand), the feed tank panel was covered and pressed with a weight. Pumping the hydrochloric acid solution into a leaching tank by an acid-proof pump, and soaking for 1-2 hours until the violent reaction is basically stopped. The leaching tank tap is opened (the low-level tap is not opened), and the leaching solution is put into the liquid storage tank. 80 kg of 65% industrial nitric acid (4/5% in test) is added to the liquid storage tank, the tap of the leaching tank is closed, and the mixed solution is pumped into the leaching tank by an acid-proof pump (the reaction is violent and can be added twice). In order to prevent the aqua regia from corroding the acid-proof pump, the water is used for washing immediately after the acid is pumped and the interior of the pump body is soaked by the water. The ore sand is leached for 2.5 days (the air temperature is about 10 ℃), and the leaching operation is as follows: after the violent reaction is finished, opening a tap of the leaching pool, allowing the leaching solution to flow downwards slowly, and opening the tap when the acid solution flows to the surface of the ore sand until the acid solution is drained. The leach pond tap was closed. Pumping the leaching solution back to the leaching pool, soaking for 2-3 hours, putting down a float bowl of the liquid separator when the mortar sinking solution is clear, allowing the clear solution to flow downwards through the liquid separator (allowing the mortar to flow out) and allowing the solution on the surface of the ore sand to flow out about 1/2, lifting up the liquid separator, and opening a tap to allow the solution to flow downwards slowly through the ore sand layer (slightly increasing the flow rate when the solution flows to the surface of the ore sand). After the solution was drained, it was treated as above. The operation is circulated twice a day. After 2.5 days of this leaching, the solution was placed in a reservoir. 30 kg of 30% industrial hydrochloric acid and 20 kg of 65% industrial nitric acid are added, the tap of the leaching pool is closed, and acid liquor is pumped into the leaching pool. Leaching for three days according to the above operation. And taking the leaching solution and the ore sand for assay, wherein the assay result shows that the leaching rate is about 90 percent, adding 20 kilograms of nitric acid, and leaching for one day. And if necessary, starting an acid-resistant air pump to enable an absorption device to absorb toxic waste gas in the leaching process.
(4) Separation and enrichment: the leaching solution of the leaching pool is put into the liquid storage pool at a higher speed, and the tap is closed after the solution is completely discharged. 0.5-0.6 ton of 3% (volume ratio) hydrochloric acid washing liquor is prepared in a waste acid pool, and 80-100 kg of washing liquor is pumped into a leaching pool by an acid-resistant pump after the solution in the leaching pool is drained. The tap was opened and the solution was allowed to drain through the sand bed. Then the same amount of washing liquid is added for washing, the process is repeated for a plurality of times, and the solution is put into the liquid storage tank each time. The test shows that the solution has no gold, when the solution is washed to the last previous time, a polyurethane foam adsorption tube (containing about 0.5 kg of polyurethane foam in the tube) of a washing pool is arranged, meanwhile, 4 kg of urea is added to a liquid storage pool in two times through a feeding pool, the solution flows through the polyurethane foam adsorption tube through the washing pool after the solution is subjected to violent reaction and is static (0.5-1 hour), so that gold is adsorbed on the polyurethane foam, and finally waste acid flows into a waste acid pool. When the solution flows through the polyurethane foam adsorption tube, the flow speed is controlled within 15-20 cm/min of the linear speed. At this time, the washing and leaching of the ore sand in the pond and the adsorption are carried out simultaneously. After the adsorption is finished, closing the tap of the liquid storage pool, opening the leaching pool and the low-level tap of the liquid storage pool, receiving the effluent liquid by a storage tank, allowing the clear liquid to remain in the next secondary production and adsorbing the clear liquid by polyurethane foam, and pouring the slurry liquid into the leaching pool for recycling. The waste acid liquor is reserved for recycling and processing.
(5) Washing: 3% by volume of industrial hydrochloric acid (about 40 kg) was added to the washing tank and the solution was passed through an adsorption tube to wash the polyurethane foam, and the wash was repeated until the effluent was yellow-free. The tube was allowed to drain.
(6) Reduction: the polyurethane foam adsorption tube is detached, the foam is taken out and put into a smooth and clean plastic barrel (if the foam on the surface layer in the tube is permeated with mortar, 5 percent (volume ratio) of hydrochloric acid is needed to be separated and cleaned and then put into the barrel), a solution containing 30 g of hydroquinone is added, as little water as possible is added to immerse the foam, the foam is extruded to ensure that the solution is uniform and fully contacted with the foam, and the soaking time is 20 to 30 minutes. Squeezing out the solution in the foam with a squeezing machine, filtering with common filter paper, and discarding the filtrate. And combining the filter paper, the filter residue and the polyurethane foam, and placing the mixture in a clean room for air drying.
(7) Removing the carrier: putting the dried polyurethane foam into an enamel cup, covering the enamel cup with a half cup, putting the enamel cup into a carbonization furnace, and carbonizing at about 250 ℃ until no reddish brown gas escapes. The carbonized gold carbon is transferred into a porcelain evaporating dish and is burnt in a high-temperature furnace at about 700 ℃ until no black color exists.
(8) Smelting: taking out brown gold ash, putting 20 g of anhydrous borax, uniformly stirring, putting into a crucible (or a porcelain evaporation dish), burning at about 700 ℃, when the powder sinks and starts to bond from loose foam, extruding the content by a glass rod, adding the borax-gold ash, and burning again. In this way, as much borax-gold dust as possible was put into the crucible. Burning at 1200-1250 deg.c for 25 min while taking out the crucible and shaking twice at high temperature to eliminate impurity from gold as far as possible.
(9) Cleaning: after production, the air extractor is opened to allow the exhaust gas in the leaching tank and the liquid storage tank to be absorbed. Uncovering the cover plate of the leaching tank, adding water and stirring to enable the hard foam to float, and fishing out the hard foam for next production. Cleaning the leaching pool and the liquid storage pool, and replacing the absorption liquid.
Drawings
1. Leaching pool 2, liquid storage pool 3, washing pool 4, waste acid pool 5, acid-proof pump 6, acid-proof air pump 7, guide pipe 8, adsorption pipe 9, absorption pool 10, feeding pool 11, groove 12, 7-shaped cover plate 13, support column 14, separator float 15, hose 16, hard foam 17, ore 18, coarse sand 19, cobblestone 20, liquid level meter
Claims (18)
1. The acid leaching polyurethane foam gold extraction method comprises aqua regia leaching, polyurethane foam separation and enrichment and smelting, and is characterized in that the dosage of hydrochloric acid and nitric acid is determined before leaching, the dosage of polyurethane foam adsorbent for separation and enrichment is determined according to the gold content of ore, the adsorbed polyurethane foam takes hydrochloric acid as a detergent to remove impurities, reduces gold by taking organic matter with reducibility as a reducing agent, removes a polyurethane foam carrier by burning, and smelts gold into blocks by anhydrous borax at high temperature.
2. The method of claim 1, wherein said leaching is performed by adding hydrochloric acid to leach the metal, then adding nitric acid and hydrochloric acid in portions, and repeating the steps a plurality of times.
3. The method of claim 1, wherein the leaching is performed by feeding the leaching solution in a counter-current manner and infiltrating an inert filler into the ore.
4. A method according to claim 1, wherein the leach solution is recycled.
5. The method of claim 1, wherein said polyurethane foam adsorbent is present in an amount of: the weight ratio of the gold content of the ore to the polyurethane foam is 1: 15-25.
6. A method according to claim 1, characterized in that urea is added to the leach solution prior to separation and enrichment.
7. The method of claim 6, wherein said urea is added in an amount of: the weight ratio of the ore to the urea is 1: 0.004-0.006, generally 1: 0.004.
8. The method of claim 1, wherein the hydrochloric acid is used as a hydrochloric acid solution having a concentration of not less than 3% by volume.
9. The method of claim 1, wherein said reducing agent is hydroquinone solution.
10. The reducing agent according to claim 9, wherein the hydroquinone solution is used in an amount of: the weight ratio of the gold content of the ore to the hydroquinone is 1-2 times, and is generally 1.2 times.
11. The method of claim 1, wherein the polyurethane foam carrier and the filter paper are carbonized at about 250 ℃ until no reddish brown gas escapes, and are ashed at about 700 ℃ to be colorless.
12. The method of claim 1, wherein said smelting is carried out by adding anhydrous borax to gold ash and smelting at a temperature of not less than 1200 ℃.
13. The process of claim 12, wherein said anhydrous borax is present in an amount of: the weight ratio of the gold to the anhydrous borax is more than 1: 0.5, and the weight ratio of the gold to the anhydrous borax is 1: 0.5-1 generally.
14. The device for acid-leaching polyurethane foam gold-extracting method is characterized by that it is formed from several acid-resisting pools, acid-resisting pump, absorption device, feeding pool and adsorption device, and its leaching system is formed from acid-resisting pool for leaching, acid-resisting pool for storing leaching liquor, liquid-storing pool, acid-resisting pool for washing, waste acid pool and acid-resisting pool for holding waste acid, and all the pools have a certain grade difference, and are connected by means of acid-resisting pipe, and all the acid-resisting pools are communicated with acid-resisting pump, and all the acid-resisting pipes are equipped with taps capable of regulating flow rate.
15. The apparatus of claim 14 wherein said leaching solution and liquid reservoir are percolation devices formed by cobblestones, grit, gutters, and "7" shaped covers.
16. The apparatus of claim 14 wherein said leach pond includes diverter pontoons.
17. The apparatus according to claim 14, characterized in that 1 to several conduits with sealed holes at one end are placed at the bottom of the leaching tank.
18. The apparatus of claim 14 wherein said absorption means comprises three cement tanks in series containing water, saturated lime water, and saturated urea respectively (wherein the first tank is made of acid-resistant cement).
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CN87103312A CN1008117B (en) | 1987-05-07 | 1987-05-07 | Gold extraction method and device by acid leaching polyurethane foam |
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CN87103312A CN1008117B (en) | 1987-05-07 | 1987-05-07 | Gold extraction method and device by acid leaching polyurethane foam |
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CN87103312A true CN87103312A (en) | 1988-11-16 |
CN1008117B CN1008117B (en) | 1990-05-23 |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111413189A (en) * | 2020-05-18 | 2020-07-14 | 中国科学院地质与地球物理研究所 | Method for detecting trace elements in pyrite |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111413189A (en) * | 2020-05-18 | 2020-07-14 | 中国科学院地质与地球物理研究所 | Method for detecting trace elements in pyrite |
CN111413189B (en) * | 2020-05-18 | 2020-10-20 | 中国科学院地质与地球物理研究所 | Method for detecting trace elements in pyrite |
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