CN111992336B - Selective desorption and recycling method for mineral surface medicament - Google Patents
Selective desorption and recycling method for mineral surface medicament Download PDFInfo
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- CN111992336B CN111992336B CN202010833845.4A CN202010833845A CN111992336B CN 111992336 B CN111992336 B CN 111992336B CN 202010833845 A CN202010833845 A CN 202010833845A CN 111992336 B CN111992336 B CN 111992336B
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- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 63
- 239000011707 mineral Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000003795 desorption Methods 0.000 title claims abstract description 47
- 239000003814 drug Substances 0.000 title claims abstract description 36
- 238000004064 recycling Methods 0.000 title claims abstract description 20
- 238000005188 flotation Methods 0.000 claims abstract description 55
- 230000008569 process Effects 0.000 claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 238000009775 high-speed stirring Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 55
- 239000000126 substance Substances 0.000 claims description 18
- 239000002738 chelating agent Substances 0.000 claims description 16
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 12
- 229910052718 tin Inorganic materials 0.000 claims description 12
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052721 tungsten Inorganic materials 0.000 claims description 10
- 239000010937 tungsten Substances 0.000 claims description 10
- VDEUYMSGMPQMIK-UHFFFAOYSA-N benzhydroxamic acid Chemical compound ONC(=O)C1=CC=CC=C1 VDEUYMSGMPQMIK-UHFFFAOYSA-N 0.000 claims description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 7
- 150000002910 rare earth metals Chemical class 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- HBROZNQEVUILML-UHFFFAOYSA-N salicylhydroxamic acid Chemical compound ONC(=O)C1=CC=CC=C1O HBROZNQEVUILML-UHFFFAOYSA-N 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- PGKQTZHDCHKDQK-UHFFFAOYSA-N 2-phenylethenylphosphonic acid Chemical compound OP(O)(=O)C=CC1=CC=CC=C1 PGKQTZHDCHKDQK-UHFFFAOYSA-N 0.000 claims description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 2
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052783 alkali metal Inorganic materials 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims description 2
- GXCSNALCLRPEAS-CFYXSCKTSA-N azane (Z)-hydroxyimino-oxido-phenylazanium Chemical compound N.O\N=[N+](/[O-])c1ccccc1 GXCSNALCLRPEAS-CFYXSCKTSA-N 0.000 claims description 2
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 claims description 2
- JLXAQYGJCVUJLE-UHFFFAOYSA-N n-hydroxynonanamide Chemical compound CCCCCCCCC(=O)NO JLXAQYGJCVUJLE-UHFFFAOYSA-N 0.000 claims description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 239000012141 concentrate Substances 0.000 abstract description 40
- 238000003723 Smelting Methods 0.000 abstract description 11
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 7
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 239000008396 flotation agent Substances 0.000 abstract description 3
- 230000002349 favourable effect Effects 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000011084 recovery Methods 0.000 description 17
- 230000009286 beneficial effect Effects 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 230000000694 effects Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 7
- 238000011160 research Methods 0.000 description 5
- 239000003112 inhibitor Substances 0.000 description 4
- 235000019353 potassium silicate Nutrition 0.000 description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 4
- SRIJLARXVRHZKD-UHFFFAOYSA-N OP(O)=O.C=CC1=CC=CC=C1 Chemical compound OP(O)=O.C=CC1=CC=CC=C1 SRIJLARXVRHZKD-UHFFFAOYSA-N 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 239000010433 feldspar Substances 0.000 description 3
- 230000002779 inactivation Effects 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- BXONZOXNGWRXND-UHFFFAOYSA-N [Ce].[C].[F] Chemical compound [Ce].[C].[F] BXONZOXNGWRXND-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002223 garnet Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 1
- 239000010428 baryte Substances 0.000 description 1
- 229910052601 baryte Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- -1 celadon Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 229910001919 chlorite Inorganic materials 0.000 description 1
- 229910052619 chlorite group Inorganic materials 0.000 description 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 229910052892 hornblende Inorganic materials 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002547 new drug Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/12—Agent recovery
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; Specified applications
- B03D2203/02—Ores
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of mineral flotation and reagent recycling, and particularly discloses a selective desorption method of a mineral surface reagent, which comprises the steps of adding a desorbent into ore pulp of minerals with chelating reagents on the surfaces, desorbing the minerals and the reagents under the assistance of high-speed stirring, and then carrying out solid-liquid separation to obtain the minerals and the recycled reagents; the medicament comprises a chelating collector; the desorbent is acid or alkali; and the dosage of the desorbent is 30-100 g/t. The invention also provides a method for recycling the recovered medicament. According to the technical scheme, the selective desorption separation of minerals and medicaments can be improved and realized by utilizing the chemical-physical synergistic effect of the desorbent and the high-speed stirring, so that the desorbent is favorable for avoiding the damage of the medicaments and the loss of the minerals, the medicaments on the surfaces of the minerals can be effectively recovered, the subsequent mineral concentrate smelting process is improved, and the corresponding water treatment cost is reduced.
Description
Technical Field
The invention belongs to the technical field of mineral flotation and hydrometallurgy, and particularly relates to a method capable of selectively desorbing beneficial agents on the surface of a mineral, which comprises a desorption method and a recycling method.
Background
In the field of flotation, the types of mineral collectors are mainly divided into a fatty acid system and a chelating agent system. Fatty acid systems have low agent cost but poor selectivity, and chelant systems have high agent cost but good selectivity. However, the fatty acid system is usually accompanied by the use of a large amount of inhibitors, such as water glass, etc., to improve the grade of the target mineral concentrate, which leads to tailing settlement and tail water recycling difficulties. Along with the improvement of the requirement of environmental protection and the higher requirement of the grade of some mineral concentrate products, such as tungsten, tin, rare earth, rutile ore and the like, the chelating agent system medicament is more and more valued and widely used. However, the medicament cost of the chelating agent system is generally higher, which leads to the increase of the production cost, and the popularization and the application of the chelating agent system are also influenced. Therefore, finding a technique to reduce the cost of using chelating agents is of great importance for further applications of chelating agents.
A large amount of beneficial agents, particularly collecting agents, remain on the surface of the mineral concentrate obtained after flotation. However, most mineral concentrates are smelted directly and no further treatment is currently available. Not only does this waste a large amount of valuable beneficial agent, but also because the residual agent on the surface of mineral concentrate leads to the difficulty of smelting, has also increased the waste water treatment cost after smelting simultaneously.
Disclosure of Invention
The invention aims to provide a method for selectively desorbing a mineral surface agent, which aims to solve the problems of high use cost, low efficiency and high wastewater treatment cost of smelting enterprises of chelating agents.
A second object of the present invention is to provide a method for recycling chemicals on the surface of minerals, which is capable of separating chemicals from the minerals to be floated and recycling the chemicals.
The desorption of minerals and agents in flotation concentrates still belongs to the blank of the industry. The invention aims to realize desorption and separation of minerals and agents in flotation concentrate for the first time, however, researches find that the selectivity of agent desorption needs to be properly solved for successfully realizing agent desorption, and the technical problems of agent inactivation, leaching loss of minerals and the like are avoided. In order to solve the technical problem, the inventor of the invention provides the following technical scheme through intensive research:
a selective desorption method of mineral surface agents is characterized in that a desorbent is added into ore pulp of minerals (namely concentrate obtained by agent flotation, the invention is also called flotation concentrate for short) with chelating agents on the surface, the minerals and the agents are desorbed under the assistance of high-speed stirring, and then the minerals and the recovered agents are obtained through solid-liquid separation;
the chelating agent (also called agent for short in the invention) comprises a chelating collector;
the desorbent is acid or alkali; and the dosage of the desorbent is 30-100 g/t.
According to the technical scheme of the invention, the selective desorption and separation of minerals and medicaments can be improved and realized by utilizing the chemical-physical synergistic effect of the desorbent and the high-speed collision (high-speed stirring), and the desorbent is also favorable for avoiding the damage of the medicaments and the loss of the minerals and can effectively recover the medicaments on the surfaces of the minerals. Based on the technical scheme of the invention, the selective desorption of the mineral surface medicament can be realized for the first time, and the technical blank of the industry is filled.
The mineral with the chelating agent on the surface is concentrate obtained by flotation of a chelating collecting agent.
In the invention, the chelating agent is at least one of hydroximic acid collecting agent, organic phosphonic acid collecting agent and hydroxylamine collecting agent.
For example, the chelating collector is one or more of benzohydroxamic acid, salicylhydroxamic acid, octylhydroxamic acid, styrenephosphonic acid, and ammonium N-nitrosophenylhydroxylamine.
The mineral species of the invention include one or more of tungsten ore, tin ore, rare earth ore, rutile and ilmenite.
Preferably, the acid is one which ionizes H in water+The substance of (1); preferably at least one of hydrochloric acid and sulfuric acid;
preferably, the base is one which ionizes OH in water-The substance of (1); preferably at least one of hydroxides and carbonates of alkali metals.
The research of the invention also finds that the physical and chemical synergy of the desorbent and the high-speed collision is beneficial to improving the separation selectivity of minerals and medicaments. Research also finds that the further control of conditions such as ore pulp concentration, desorbent dosage, high-speed collision stirring speed and the like in the treatment process is beneficial to further improving the separation selectivity of minerals and medicaments, improving the medicament recovery rate, avoiding medicament inactivation and avoiding mineral loss.
In the invention, the dosage of the desorbent is based on the mineral flotation raw ore. The flotation raw ore refers to raw ore before reaction with the chelating agent. Preferably, the dosage of the desorbent is 60-80 g/t.
Preferably, the concentration of the ore pulp is 10-70%, preferably 15-60%; further preferably 20-40%; more preferably 25 to 35%.
In the invention, the high-speed stirring speed is 2000-3000 r/min; further preferably 2500 to 2800 r/min.
In the invention, the temperature in the desorption process is room temperature, and preferably 5-40 ℃.
The desorption time is preferably 10-30 min; more preferably 15 to 25 min.
Preferably, after the analysis, solid-liquid separation is performed, and the analyzed minerals and the recovered chemical are recovered.
Preferably, the solid-liquid separation means is centrifugation, and the rotation speed of the centrifugation is 800-1400 r/min; further preferably 1000 to 1200 r/min.
The invention also provides a method for recycling the mineral surface medicament, which adopts the desorption method to obtain the recycled medicament; and recycling the recovered chemicals to the flotation of the next batch of minerals.
The recycling method can effectively recycle beneficial agents on the surface of the floated minerals, and reduces the difficulty of subsequent smelting of the minerals and the environmental protection pressure. Moreover, the research also unexpectedly finds that the recycling of the recovered medicament can further improve the flotation effect, such as the recovery rate and/or the grade of the flotation, on the premise of reducing new medicaments and the use amount.
In the invention, the recycling method mixes the recovered chemical with the reduced new chemical and is used for the flotation of the minerals of the next batch; the decrement proportion of the new medicament is 15-50%. The decrement proportion is 15-50% decrement based on the original planned dosage. In the present invention, the originally planned amount refers to the amount of the flotation reagent used to obtain the mineral to be recovered. More preferably, the recycling of the recovered drug is such that the amount of the new drug is reduced by 20 to 40%.
According to the technical scheme, the recycling treatment can reduce the dosage of the medicament, and can also improve the performances such as flotation recovery rate and/or grade unexpectedly, so that the performances are improved on the premise of really saving resources.
Advantageous effects
(1) The selective desorption and the recycling of the mineral surface medicament are realized for the first time.
In the invention, the potential of the surface of the mineral and the structure of the adsorbed medicament are modified by the desorbent and are further cooperated with high-speed stirring, so that the high-selectivity separation of the mineral and the medicament chelated on the surface can be realized based on the physical and chemical synergistic action, and moreover, the inactivation of the medicament and the loss of the mineral are also avoided. The recycled medicament is further recycled, so that the flotation performance can be improved unexpectedly by matching with the recycled medicament under the condition of reducing new medicament.
(2) The desorption method is simple and efficient; the recycling of the desorption agent is beneficial to reducing the cost of the flotation agent and the treatment cost of the smelting water, and simultaneously improving the smelting process.
The invention provides a simple and efficient selective desorption technology for mineral surface agents, and the desorbed agents are recycled for the flotation process, so that the sustainable use technology of agent adsorption-desorption-reuse-adsorption is realized. The technology not only realizes the sustainable recycling of expensive chelating agents, reduces the cost of flotation agents, but also reduces the wastewater treatment cost and the smelting process in the smelting process (the less the agent residue on the surface of the concentrate affects the smelting process), protects the ecological environment, realizes the win-win situation of mineral processing enterprises and smelting enterprises, and ensures the economic benefit and sustainable development of the enterprises.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, it is obvious that the drawings described below are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a graph showing the effect of desorption of benzohydroxamic acid; from left to right, comparative example 1, comparative example 2, example 5, example 6 and example 1 were followed.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
In the following cases, the temperature of the flotation process was room temperature (15-35 ℃) unless otherwise stated.
Example 1
Performing tungsten flotation on sulfur-selecting tailings (tungsten raw ore) taken from Chenzhou of Hunan province, wherein WO3The grade is 0.40%, the gangue mainly comprises garnet and calcite, the dosage of the roughing collector is 600g/t lead nitrate, 500g/t benzohydroxamic acid, the flotation pH of the ore pulp is 9.0, the flotation time is 6min, the stirring speed of the flotation machine is 2000r/min, and the flotation result (without concentrated solution) is shown in table 1. Then, the tungsten concentrate ore pulp is put into a stirrer, the concentration of the ore pulp is adjusted to be 25%, the stirring speed is 2700r/min, then, 60g/t of sodium hydroxide serving as a desorption agent (aiming at tungsten raw ore) is added, after stirring is carried out for 15min, the ore pulp immediately enters a centrifugal machine for concentration, and centrifugal concentrated solution containing a large amount of beneficial collecting agents returns to the original flotation flow for use. Color concentrateThe color is shown in FIG. 1. After the concentrated solution is added, the dosage of the lead nitrate and the dosage of the benzohydroxamic acid are respectively reduced to 450g/t and 350g/t (30 percent of reduction compared with the original planned medicament), other flotation conditions are consistent, and the flotation results (concentrated solution, namely recycled medicament groups) are shown in Table 1. The results in table 1 show that, after the concentrated solution of the tungsten concentrate surface desorption agent is added, the grade of the tungsten rough concentrate is slightly increased, but the recovery rate is greatly increased, and meanwhile, the use amounts of the collecting agents of lead nitrate and benzohydroxamic acid are respectively reduced by 25.00% and 30.00%, so that the concentrated solution has a better effect on the grade and/or recovery rate, and the indication is obvious in the treatment technical effect on the concentrate.
TABLE 1
Example 2
Tin ore (raw tin ore) taken from a certain old dressing plant in Yunnan is subjected to flotation, wherein the grade of Sn is 0.55 percent, gangue mainly comprises quartz and feldspar, the dosage of a roughing collector is 500g/t of lead nitrate, 700g/t of benzohydroxamic acid, the dosage of inhibitor water glass is 300g/t, the pH value of ore pulp flotation is 8.0, 40g/t of No. 2 oil, the speed is 2000r/min, and the flotation result (without concentrated solution) is shown in Table 2. Then, the tin concentrate ore pulp is put into a stirrer, the concentration of the ore pulp is adjusted to be 30%, the stirring speed is 2800r/min, then, 80g/t (aiming at tin raw ore) of desorbent hydrochloric acid is added, after stirring is carried out for 20min, the ore pulp immediately enters a centrifugal machine for concentration, and centrifugal concentrated solution containing a large amount of beneficial collecting agents returns to the original flotation process for use. After the concentrated solution is added, the use amounts of lead nitrate and benzohydroxamic acid are respectively reduced to 400g/t and 550g/t, other flotation conditions are consistent, and flotation results (with the concentrated solution) are shown in Table 2. The results in table 2 show that after the concentrated solution of the tin concentrate surface desorption agent is added, the grade and the recovery rate of the tin concentrate are greatly increased, and meanwhile, the use amounts of the collecting agents of lead nitrate and benzohydroxamic acid are respectively reduced by 20.00% and 21.43%, and the effect is remarkable.
TABLE 2
Example 3
The method comprises the steps of carrying out flotation on rare earth ore (fluorine-carbon cerium raw ore) taken from a certain Sichuan crown Ning selection plant, wherein the REO grade is 3.06%, gangue mainly comprises feldspar, quartz, barite and fluorite, the dosage of roughing inhibitor water glass is 3000g/t, the dosage of collecting agent salicylhydroxamic acid is 4000g/t, No. 2 oil is 40g/t, the speed is 2000r/min, and the flotation result (without concentrated solution) is shown in Table 3. Then, the rare earth concentrate ore pulp is put into a stirrer, the concentration of the ore pulp is adjusted to be 35%, the stirring speed is 2600r/min, then 80g/t of sodium hydroxide (aiming at fluorine-carbon cerium raw ore) as a desorption agent is added, the ore pulp is stirred for 25min, then the ore pulp immediately enters a centrifugal machine for concentration, and centrifugal concentrated solution containing a large amount of beneficial collecting agents is returned to the original flotation process for use. After the concentrated solution is added, the dosage of the salicylhydroxamic acid is reduced to 3000g/t, other flotation conditions are consistent, and the flotation results (with the concentrated solution) are shown in table 3. From the results in table 3, it can be seen that, after the concentrated solution of the rare earth concentrate surface desorption agent is added, the grade and the recovery rate of the rare earth concentrate are greatly increased, particularly the recovery rate is increased, and meanwhile, the use amount of the collecting agent salicylhydroxamic acid is reduced by 25.00%, and the effect is remarkable.
TABLE 3
Example 4
Subjecting rutile ore (rutile crude ore) from certain selection factory of Ziyang of Hubei to flotation, wherein TiO is2The grade is 3.19%, the gangue is mainly hornblende, garnet, chlorite, celadon, feldspar and the like, the dosage of roughing inhibitors sodium hexametaphosphate and water glass is 1000 g/t and 300g/t respectively, the dosage of collecting agents styrene phosphonic acid is 800g/t, the dosage of lead nitrate is 200g/t, No. 2 oil is 10g/t, the speed is 2000r/min, and the flotation result (without concentrated solution) is shown in a table 4. Then, willThe rutile concentrate ore pulp is put into a stirrer, the concentration of the ore pulp is adjusted to be 30%, the stirring speed is 2700r/min, then desorption agent sulfuric acid is added for 60g/t (aiming at rutile raw ore), after stirring for 20min, the ore pulp immediately enters a centrifugal machine for concentration, and centrifugal concentrated solution containing a large amount of beneficial collecting agents is returned to the original flotation process for use. After the concentrated solution was added, the amount of styrene phosphonic acid was reduced to 500g/t, and other flotation conditions were consistent, and the flotation results (with concentrated solution) are shown in Table 4. The results in table 4 show that after the concentrated solution of the rutile concentrate surface desorption agent is added, the grade of the rutile concentrate is slightly increased, but the recovery rate is greatly increased, and meanwhile, the dosage of the collecting agent styrene phosphonic acid is reduced by 37.50%, and the effect is remarkable.
TABLE 4
Comparative example 1
The amount of sodium hydroxide as a desorbent was 0g/t, the rest was the same as in example 1, and the color of the concentrate after desorption was shown in FIG. 1, and the flotation results are shown in Table 5.
Comparative example 2
The amount of sodium hydroxide as a desorbent was 15g/t, the rest was the same as in example 1, and the color of the concentrate after desorption was shown in FIG. 1, and the flotation results are shown in Table 5.
Example 5
The amount of sodium hydroxide as a desorbent was 30g/t, the rest was the same as in example 1, and the color of the concentrate after desorption was shown in FIG. 1, and the flotation results are shown in Table 5.
Example 6
The amount of sodium hydroxide as a desorbent was 90g/t, the rest was the same as in example 1, and the color of the concentrate after desorption was shown in FIG. 1, and the flotation results are shown in Table 5.
The desorption pictures of comparative examples 1-2, examples 5 and 6 and example 1 are shown in fig. 1, and it can be seen from the figure that the color of the concentrate after the surface desorption of the concentrate is gradually deepened with the increase of the dosage of the desorbent, the color tends to be stable after a certain dosage is reached (60g/t, example 1), the COD value also tends to be stable, the grade and the recovery rate of the tungsten concentrate also gradually increase and then stabilize, which indicates that the increase of the dosage of the desorbent is helpful for improving the desorption amount of the beneficial agent on the surface of the mineral, namely the dosage of the desorbent is an important influence factor of the invention.
TABLE 5 COD values of concentrates and flotation results at different desorbent dosages
Example 7
The concentration of the slurry in the concentrate desorption process was 10%, the other steps were the same as in example 2, the grade Sn of the obtained tin concentrate was 4.02%, and the recovery rate was 65.35%.
Example 8
The concentration of the ore pulp in the desorption process of the concentrate is 70 percent, the rest is the same as that of the example 2, the grade Sn of the obtained tin concentrate is 3.68 percent, and the recovery rate is 68.72 percent.
Comparative example 3
The stirring speed in the concentrate desorption process is 1000r/min, the rest is the same as that in the example 2, the grade Sn of the obtained tin concentrate is 3.15 percent, and the recovery rate is 61.10 percent.
Compared with the embodiment 2, the embodiments 7-8 and the comparative example 3 show that both too low and too high concentration of the ore pulp during desorption have influence on agent desorption, and further the flotation result is poor; meanwhile, the stirring speed of ore pulp in the desorption process can directly influence the desorption effect of the medicament, and the stirring speed is too low, so that the desorption effect is influenced, and the subsequent flotation index is deteriorated.
In conclusion, by adopting the method provided by the invention, based on the physical and chemical double synergistic effects of the desorbent and the high-speed stirring, the recovery of the chelating agent on the surface of the concentrate can be effectively realized, in addition, the rotating speed of the desorbent and the high-speed stirring and the concentration of the ore pulp in the desorption process are further controlled, the COD recovery of the agent is further improved, the recovery rate is improved, and in addition, the recovered agent is recycled, so that not only can the new agent for the flotation of a new batch of minerals be reduced, but also the flotation recovery rate or/and grade can be improved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and various modifications and changes may be made by those skilled in the art. Any improvement or equivalent replacement directly or indirectly applied to other related technical fields within the spirit and principle of the invention and the contents of the specification and the drawings of the invention shall be included in the protection scope of the invention.
Claims (19)
1. A selective desorption method of mineral surface agents is characterized in that a desorbent is added into ore pulp of minerals with chelating agents on the surface, the minerals and the agents are desorbed under the assistance of high-speed stirring, and then the minerals and the recovered agents are obtained through solid-liquid separation;
the medicament comprises a chelating collector;
the desorbent is acid or alkali; and the dosage of the desorbent is 30-100 g/t.
2. The method according to claim 1, wherein the chelating agent is at least one of a hydroximic acid collector, an organic phosphonic acid collector and a hydroxylamine collector.
3. The method of claim 1 wherein the chelating collector is one or more of benzohydroxamic acid, salicylhydroxamic acid, octylhydroxamic acid, styrenephosphonic acid, and ammonium N-nitrosophenylhydroxylamine.
4. The method of claim 1, wherein the mineral species comprises one or more of tungsten ore, tin ore, rare earth ore, rutile and ilmenite.
5. The method of claim 1, wherein the pulp concentration is 10-70%.
6. The method of claim 1, wherein the pulp concentration is 15-60%.
7. The method of claim 1, wherein the acid ionizes H in water+The substance of (1).
8. The method of claim 7, wherein the acid is at least one of hydrochloric acid and sulfuric acid.
9. The method of claim 1, wherein the base ionizes OH in water-The substance of (1).
10. The method of claim 9, wherein the base is at least one of a hydroxide and a carbonate of an alkali metal.
11. The method of claim 1, wherein the high speed stirring speed is 2000 to 3000 r/min.
12. The method according to claim 1, wherein the temperature of the desorption process is room temperature.
13. The method according to claim 1, wherein the temperature during desorption is 5 to 40 ℃.
14. The method according to claim 1, wherein the desorption time is 10 to 30 min.
15. The method according to claim 1, wherein the mineral after the analysis and the recovered chemical are recovered by performing solid-liquid separation after the analysis.
16. The method according to claim 15, wherein the solid-liquid separation means is centrifugation.
17. The method of claim 16, wherein the rotation speed of the centrifuge is 800 to 1400 r/min.
18. A method for recycling a mineral surface agent, which is characterized in that the recovered agent is obtained by the method of any one of claims 1 to 17; and recycling the recovered chemicals to the flotation of the next batch of minerals.
19. The method of claim 18 wherein the recycled chemical is mixed with a reduced amount of new chemical for flotation of the next batch of minerals; the decrement proportion of the new medicament is 15-50%.
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