CN114653479A - Multi-metal co-associated fluorite ore de-drug flotation method - Google Patents
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Abstract
The invention discloses a polymetallic co-associated fluorite ore reagent-removing flotation method. Concentrating and removing the chemical from tailings generated by flotation of tungsten ore by using a metal-organic complex, taking BK as a collecting agent, taking water glass, acidified water glass and ATM as an inhibitor, and performing a flotation process to obtain fluorite concentrate. The method is simple to operate, simplifies the production flow, realizes the recycling of mineral water and reagents, reduces the production cost, solves the problem of difficult fluorite flotation separation under the influence of tungsten ore flotation residual reagents, greatly improves the grade and recovery rate of fluorite concentrate, and has good economic benefit and application prospect.
Description
Technical Field
The invention relates to a fluorite beneficiation method, in particular to a method for recovering fluorite from tungsten tailings by adopting a demetallization flotation method after polymetallic associated fluorite ore adopts metal-organic complex flotation tungsten ore, and belongs to the technical field of mineral processing.
Background
Fluorite, also called fluorite, contains calcium fluoride (CaF) as main ingredient2) The rare earth is an important non-metal mineral resource, is a main source of chemical element fluorine in industry, is widely applied to the traditional industries and emerging fields of metallurgy, chemical industry, cement, medicine, national defense, fluorine chemical industry, new energy and the like, and is known as the second rare earth.
The fluorite resource reserves in China are rich and widely distributed, and the fluorite is one of the dominant mineral products in China. The fluorite deposit can be divided into a single type and a co-associated type according to the characteristics and conditions of ore formation. The single fluorite ore has less storage amount, high fluorite grade and simple selection; the associated fluorite ore has rich reserves, low fluorite grade, complex mineral intergrowth characteristics and difficult separation. At present, the development and utilization of fluorite resources in China are mainly single fluorite resources, along with the continuous development of industry, the demand of the fluorite resources is gradually increased, the single fluorite ore resources are gradually exhausted, and the problem of how to efficiently utilize the co-associated fluorite resources becomes a current urgent solution.
The associated fluorite ore can be divided into a lead-zinc sulfide ore type, a tungsten-tin polymetallic associated type and a rare earth-iron ore associated type according to different main metal and mineral combination characteristics, wherein the tungsten-tin-molybdenum polymetallic associated fluorite ore in the persimmon bamboo garden has abundant resource reserves and huge recycling value. In the traditional tungsten ore flotation process, a large amount of caustic soda and water glass are often added to obtain high-grade tungsten concentrate, so that fluorite minerals are strongly inhibited, the recovery rate and the grade of fluorite in tungsten flotation tailings are low, and the comprehensive recovery utilization rate is low. After the process transformation, the persimmon bamboo garden adopts a novel metal-organic complex flotation process, the addition of water glass and fatty acid in the tungsten selecting process is cancelled, the enrichment of fluorite in tungsten concentrate is avoided, the fluorite in tungsten flotation tailings is not inhibited by the water glass, and the fluorite has stronger surface activity, so that the efficient recycling of the fluorite is possible. However, a large amount of flotation reagents remain in the tungsten ore flotation operation, and a great influence is generated on the subsequent flotation separation of fluorite, wherein lead ions and complexes (Pb-BHA) formed by the lead ions and the benzohydroxamic acid are main influencing factors, the lead ions can activate the flotation of quartz and inhibit the flotation of fluorite, and the Pb-BHA complexes can activate the flotation of calcite, so that the fluorite sorting index is low.
Disclosure of Invention
Aiming at the technical problems of complicated subsequent fluorite flotation process, low recovery rate and the like caused by the influence of residual flotation reagents after the polymetallic co-associated fluorite ore is subjected to flotation and recovery of tungsten ore by using metal-organic complexes in the prior art, the invention aims to provide the polymetallic co-associated fluorite de-chemical flotation method.
In order to achieve the technical purpose, the invention provides a multi-metal co-associated fluorite ore de-chemical flotation method, which is characterized in that tailings generated by flotation of tungsten ore by using a metal-organic complex are concentrated and de-chemically treated, BK is used as a collecting agent, water glass, acidified water glass and ATM are used as inhibitors, and fluorite concentrate is obtained through a flotation process.
The key point of the invention is that in the process of carrying out the reagent-removing flotation on the tailings generated by the flotation of the tungsten ore by the metal-organic complex is as follows: on the one hand, concentrate the medicine of taking off to the ore pulp, can reduce the influence of remaining flotation reagent to follow-up flotation by a wide margin, on the other hand, adopt special BK as the collector and regard water glass, acidizing water glass and ATM as gangue mineral inhibitor, through appropriate flow, improved the rate of recovery and the grade of fluorite concentrate greatly.
As a preferred scheme, the tailings comprise the following main minerals in the following content: CaF2 15wt％～25wt％，CaCO35 wt％～15wt％，SiO235-50 wt%, and the tungsten ore flotation residual agent is benzohydroxamic acid, lead ions and lead ion-benzohydroxamic acid complex. The residual flotation reagent affects the flotation efficiency of the subsequent fluorite mainly by activating quartz and calcite.
As a preferable scheme, the concentration and the removal of the pesticide are realized by a thickener, and the concentration is carried out until the concentration of the ore pulp is in the range of 50 to 70 weight percent. Before fluorite flotation, the ore pulp is concentrated and de-dosed by a thickener and concentrated to a proper concentration range so as to reduce the influence of residual medicament on the subsequent fluorite flotation separation.
As a preferable scheme, the pulp after concentration and reagent removal is added with water and is subjected to pulp mixing until the concentration is between 28 and 45 percent.
As a preferred solution, the flotation circuit comprises 1 rougher flotation +1 scavenger flotation +8 cleaner flotation.
As a preferred scheme, the roughly selected dosage system is as follows: BK 180-300 g/t, water glass 1600-2000 g/t.
As a preferred scheme, the selected dosage system is as follows: 1, fine selection: 100-140 g/t of acidified water glass and 10-12 g/t of ATM; and (3) selecting for 2 times: 80-100 g/t of acidified water glass and 8-10 g/t of ATM; and (3) fine selection: 60-80 g/t of acidified water glass and 4-6 g/t of ATM; and 4, fine selection: 40-60 g/t of acidified water glass and 4-6 g/t of ATM; and (3) 5 times of fine selection: 30-40 g/t of acidified water glass and 2-4 g/t of ATM; 6 times of fine selection: 20-30 g/t of acidified water glass and 2-4 g/t of ATM; 7 times of fine selection: 10-20 g/t of acidified water glass and 1-2 g/t of ATM; 8 times of fine selection: 10-20 g/t of acidified water glass and 1-2 g/t of ATM.
As a preferred scheme, the tailings after 1 time of concentration are returned to rough concentration, and the concentrate enters the next-stage concentration; returning tailings after 2-7 times of concentration back to the previous stage of concentration, and allowing concentrate to enter the next stage of concentration; and returning the tailings after 8 times of concentration to the previous-stage concentration.
As a preferable scheme, the acidified water glass is prepared by reacting water glass and sulfuric acid according to a mass ratio of 5: 1-5: 3. The acidified sodium silicate has higher inhibitory activity against calcium-containing gangue minerals.
As a preferred scheme, the scavenged tailings are directly discarded, and scavenged concentrate enters 1-time concentration.
The invention provides a multi-metal associated fluorite ore drug-removal flotation method, which comprises the following specific steps:
step 1: fluorite removal flotation is carried out on the tailings after the tungsten ore flotation is carried out by using the metal-organic complex, and CaF in the tungsten ore flotation tailings215 to 25 weight percent of CaCO35 to 15 weight percent of SiO2The content is 35-50 wt%, the ore belongs to high calcium carbonate low-grade fluorite ore, and meanwhile, the tailings contain a certain amount of tungsten ore flotation residual agents of benzohydroxamic acid and lead ions and lead ion-benzohydroxamic acid complexes;
step 2: tungsten ore flotation tailings are used as fluorite reagent removal flotation feeding and enter concentration reagent removal operation, a thickener is used for concentrating ore pulp until the ore pulp concentration is 50% -70%, the influence of most residual reagents such as lead nitrate and benzohydroxamic acid on fluorite flotation separation is eliminated, concentrated water returns to tungsten ore sorting operation, the ore after concentration and reagent removal is added with water until the ore pulp concentration is 28% -45%, and flotation reagents (BK 180-300 g/t, water glass 1600-2000 g/t) are added and enter roughing operation;
and step 3: the tailings of the roughing operation enter a scavenging operation, the tailings of the scavenging operation are directly discarded, and the concentrate of the scavenging operation is combined with the concentrate of the roughing operation to enter a concentration operation;
and 4, step 4: adding 100-140 g/t of acidified water glass (the mass ratio of the water glass to concentrated sulfuric acid is 5: 1-5: 3) and 10-12 g/t of calcium carbonate inhibitor ATM in one concentration operation, returning tailings in the one concentration operation to a rough concentration operation, feeding concentrate in the one concentration operation to a secondary concentration operation, adding 80-100 g/t of acidified water glass and 8-10 g/t of calcium carbonate inhibitor ATM in the secondary concentration operation, returning tailings in the secondary concentration operation to a first concentration operation, feeding concentrate in the secondary concentration operation to a third concentration operation, adding 60-80 g/t of acidified water glass and 4-6 g/t of calcium carbonate inhibitor ATM in the third concentration operation; returning tailings of the third concentration operation to the second concentration operation, and adding concentrate of the third concentration operation to the fourth concentration operation, wherein the fourth concentration operation is added with acidified water glass with the dosage of 40-60 g/t and calcium carbonate inhibitor ATM with the dosage of 4-6 g/t; returning tailings of the four-time concentration operation to the three-time concentration operation, allowing concentrate of the four-time concentration operation to enter the five-time concentration operation, and adding 30-40 g/t of acidified water glass and 2-4 g/t of calcium carbonate inhibitor ATM into the five-time concentration operation; returning tailings of the five-time concentration operation to four-time concentration operation, and feeding concentrate of the five-time concentration operation to six-time concentration operation, wherein the acidified water glass with the dosage of 20-30 g/t and the calcium carbonate inhibitor ATM with the dosage of 2-4 g/t are added in the six-time concentration operation; returning tailings of the six-time concentration operation to five-time concentration operation, and feeding concentrate of the six-time concentration operation to seven-time concentration operation, wherein the seven-time concentration operation is added with 10-20 g/t of acidified water glass and 1-2 g/t of calcium carbonate inhibitor ATM; returning tailings of the seven-time concentration operation to six-time concentration operation, and feeding concentrate of the seven-time concentration operation to eight-time concentration operation, wherein 10-20 g/t of acidified water glass and 1-2 g/t of calcium carbonate inhibitor ATM are added in the eight-time concentration operation; and returning the tailings after the eight-time concentration operation to the seven-time concentration operation, wherein the concentrate obtained after the eight-time concentration operation is the final fluorite concentrate.
Compared with the prior art, the technical scheme of the invention has the beneficial technical effects that:
(1) according to the invention, through carrying out reagent removal flotation on fluorite, the influence of residual reagents on the subsequent fluorite flotation separation in the tungsten ore flotation process is effectively reduced, the recovery rate of fluorite is greatly improved, and higher-grade fluorite concentrate is obtained.
(2) According to the invention, concentration and reagent removal operation is added before fluorite flotation, so that the flotation separation of fluorite is facilitated, the mineral separation backwater utilization rate is improved, the reagent usage amount is reduced, and the environmental protection is facilitated.
(3) The method has the advantages of simple process flow, convenient operation, great reduction of production cost, and good economic benefit and application prospect.
Drawings
FIG. 1 is a flow diagram of the fluorite reagent-removing flotation process of example 1.
Detailed Description
The following examples are intended to further illustrate the present invention and are not intended to limit the scope of the invention as claimed.
Example 1
The tungsten flotation tailings of a certain polymetallic ore in Hunan are taken as research objects, the tailings contain associated fluorite, and the fluorite is a main useful mineral recovered from the tailings. CaF in the tailings220.67% of CaCO3The content is 5.33%, the gangue minerals mainly comprise quartz, mica, garnet and the like, belong to high-calcium-carbonate low-grade fluorite ores, the total concentration of the benzohydroxamic acid in the residual flotation reagent is about 10mg/L, and the total concentration of the lead nitrate is about 15 mg/L.
Aiming at polymetallic ore tungsten flotation tailings, the existing process adopts a process of firstly carrying out alkali and then carrying out acid, high-grade fluorite concentrate is obtained through a coarse primary cleaning process and an eight-fine secondary cleaning process, and low-grade fluorite concentrate is obtained through the tailings obtained through the fine cleaning process and a coarse primary cleaning process and a three-fine secondary cleaning process.
The method comprises the following specific steps:
the method comprises the following steps: adding 300g/t of sodium carbonate, 2000g/t of water glass and 300g/t of BK300g/t into roughing operation, carrying out primary scavenging on tailings in the roughing operation, combining concentrate in the primary scavenging operation and concentrate in the roughing operation, carrying out a first concentration operation, and directly discarding tailings in the primary scavenging operation.
Step two: the first fine concentration is blank fine concentration, the concentrate in the first fine concentration operation enters a second fine concentration operation, and the tailings in the first fine concentration operation enter a low-degree fluorite rough concentration operation; selecting II, selecting III, selecting IV, selecting V, selecting VI, selecting VII, selecting VIII, and adding acidified water glass in the amount of 240g/t, 200g/t, 160g/t, 120g/t, 100g/t, 80g/t, and 50 g/t; returning tailings of 2-7 times of concentration operation to the previous stage operation in sequence, and enabling concentrate to enter the next stage concentration in sequence; and returning the tailings subjected to the eight-operation fine concentration to the seven-operation fine concentration, wherein the concentrate subjected to the eight-operation fine concentration is the final high-grade fluorite concentrate.
Step three: adding BK 50g/t into low-degree fluorite roughing, leading tailings of the low-degree fluorite roughing operation to enter low-degree fluorite scavenging operation, merging concentrate of the low-degree fluorite scavenging operation and concentrate of the low-degree fluorite roughing operation, leading the concentrate of the low-degree fluorite scavenging operation to enter a low-degree fluorite concentration operation, and directly discarding tailings of the low-degree fluorite scavenging operation.
Step four: the acidification sodium silicate with the dosage of 40g/t, 30g/t and 20g/t is respectively added in the first low-degree fluorite concentration operation, the tailings of the first low-degree fluorite concentration operation and the second low-degree fluorite concentration operation return to the previous-level operation in sequence, the concentrates of the first low-degree fluorite concentration operation and the second low-degree fluorite concentration operation enter the next-level concentration in sequence, the tailings of the third low-degree fluorite concentration operation return to the second low-degree fluorite concentration operation, and the concentrates of the third low-degree fluorite concentration operation are final low-grade fluorite concentrates.
Finally obtaining CaF2High-grade fluorite concentrate and CaF with content of 93%2The low-grade fluorite concentrate with the content of 85 percent is influenced by residual medicaments of benzohydroxamic acid, lead nitrate and the like in tailings, and the total recovery rate of fluorite is lower and is only about 40 percent.
The invention provides a multi-metal associated fluorite ore de-medicated flotation method, which comprises the following specific steps:
step (1), concentrating and removing the raw ore: concentrating the tungsten ore flotation tailings in a thickener until the concentration of ore pulp is about 65%, returning concentrated water to tungsten ore sorting operation, and supplementing water to the ore subjected to concentration and reagent removal until the concentration of the ore pulp is about 30% to obtain ore pulp to be floated;
step (2) rough concentration: the ore pulp to be floated enters a roughing operation, collecting agent BK 250g/t and inhibitor water glass 1800g/t are added, roughing foam enters a concentrating operation, roughed tailings enter a scavenging operation, concentrate subjected to scavenging operation enters a concentrating operation, and tailings subjected to scavenging operation are directly discarded.
Step (3) fine selection: the rough concentrate obtained by rough concentration and scavenging concentrate are merged and enter concentration operation, the concentration operation is carried out for eight times totally, the concentration of ore pulp in the concentration operation is controlled to be about 24 percent, acidified water glass and ATM are selected as gangue mineral inhibitors, the dosage of the acidified water glass added in the concentration operation is respectively 120g/t, 80g/t, 60g/t, 50g/t, 30g/t, 20g/t and 10g/t, the dosage of the acidified water glass added in the concentration operation is respectively 10g/t, 8g/t, 4g/t, 2g/t, 1g/t and 1g/t, and returning tailings obtained in the concentration operation to the previous-stage flotation operation, and obtaining the final fluorite concentrate after eight times of concentration.
The acidified water glass used in the fine selection in the step (3) is prepared by reacting water glass and concentrated sulfuric acid according to the mass ratio of 5: 1.
Detecting to obtain CaF2The recovery rate of the fluorite concentrate with the grade of 92.05% and the recovery rate of 60.04% is improved by 20% compared with the prior process of firstly carrying out alkali and then carrying out acid on the fluorite concentrate with little change of the grade of the concentrate.
Example 2
CaF in flotation tailings of certain wolframite2The content of CaCO is 24.76 percent3The content of SiO is 8.79 percent2The content is 46.54%, the total concentration of the benzohydroxamic acid in the residual flotation reagent is about 12mg/L, and the total concentration of the lead nitrate is about 16 mg/L. The flotation process adopts concentration and reagent removal, namely a coarse sweeping and seven-time sweeping flow, wherein swept ore concentrate enters primary concentration, and tailings obtained by secondary, third, fourth, fifth, sixth and seventh times of concentration return to the previous flotation operation in sequence.
The method comprises the following specific steps:
step (1), concentrating and removing the raw ore: and concentrating the tungsten ore flotation tailings by using a thickener until the concentration of ore pulp is about 68 percent, and removing most of tungsten ore flotation residual agents. Adding water to the ore after concentration and reagent removal until the concentration of the ore pulp is about 28 percent to obtain ore pulp to be floated;
step (2) rough concentration: the ore pulp to be floated is subjected to roughing operation, collecting agent BK 200g/t and inhibitor water glass 2000g/t are added, roughing foam is subjected to fine selection operation, roughed tailings are subjected to scavenging operation, concentrate in the scavenging operation is subjected to fine selection operation, and scavenged tailings are directly discarded.
Step (3) fine selection: the rough concentrate obtained by rough concentration and scavenging concentrate are merged and enter concentration operation, the concentration operation is carried out for seven times totally, the concentration of ore pulp in the concentration operation is controlled to be about 24 percent, acidified water glass and ATM are selected as gangue mineral inhibitors, the dosage of the acidified water glass added in the concentration operation is respectively 120g/t, 100g/t, 80g/t, 60g/t, 40g/t, 20g/t and 10g/t, the dosage of the acidified water glass added in the concentration operation is respectively 12g/t, 10g/t, 6g/t, 4g/t, 2g/t and 1g/t, the tailings obtained by the concentration operation are returned to the upper-level flotation operation, and obtaining the final fluorite concentrate after seven times of fine concentration.
The acidified water glass used in the fine selection in the step (3) is prepared by reacting water glass and concentrated sulfuric acid according to the mass ratio of 5: 2.
Detecting and analyzing to obtain CaF292.85% grade, and 59.37% recovery rate.
Claims (9)
1. A multi-metal associated fluorite ore de-drug flotation method is characterized by comprising the following steps: concentrating and removing the chemical from tailings generated by flotation of tungsten ore by using a metal-organic complex, taking BK as a collecting agent, taking water glass, acidified water glass and ATM as an inhibitor, and performing a flotation process to obtain fluorite concentrate.
2. The method for removing the chemicals and floating the polymetallic co-associated fluorite ore according to claim 1, which is characterized in that: the tailings comprise the following main minerals in percentage by weight: CaF2 15wt％～25wt％，CaCO35 wt％～15wt％，SiO235-50 wt%, and the tungsten ore flotation residual agent is benzohydroxamic acid, lead ions and lead ion-benzohydroxamic acid complex.
3. The method for removing the chemicals and floating the polymetallic co-associated fluorite ore according to claim 1, which is characterized in that: the concentration and the removal of the chemicals are realized by a thickener, and the concentration is carried out until the concentration of the ore pulp is within the range of 50 wt% -70 wt%.
4. The method for flotation by removing the chemicals from the polymetallic co-associated fluorite ore according to any one of claims 1 to 3, which is characterized in that: the flotation process comprises 1 roughing, 1 scavenging and 8 concentrating.
5. The method for removing the chemicals and floating the polymetallic co-associated fluorite ore according to claim 4, which is characterized in that: the medicament system in the rough selection is as follows: BK 180-300 g/t, water glass 1600-2000 g/t.
6. The method for flotation by removing the chemicals from the polymetallic co-associated fluorite ore according to claim 4, wherein: the medicament system selected in the fine selection is as follows:
1, fine selection: 100-140 g/t of acidified water glass and 10-12 g/t of ATM;
and (3) selecting for 2 times: 80-100 g/t of acidified water glass and 8-10 g/t of ATM;
and (3) fine selection: 60-80 g/t of acidified water glass and 4-6 g/t of ATM;
and 4, fine selection: 40-60 g/t of acidified water glass and 4-6 g/t of ATM;
and (3) 5 times of fine selection: 30-40 g/t of acidified water glass and 2-4 g/t of ATM;
6 times of fine selection: 20-30 g/t of acidified water glass and 2-4 g/t of ATM;
7 times of fine selection: 10-20 g/t of acidified water glass and 1-2 g/t of ATM;
8 times of fine selection: 10-20 g/t of acidified water glass and 1-2 g/t of ATM.
7. The method for removing the chemicals and floating the polymetallic co-associated fluorite ore according to claim 6, which is characterized in that: returning the tailings subjected to the 1-time concentration to rough concentration, and feeding the concentrate to the next-stage concentration; returning tailings after 2-7 times of concentration back to the previous stage of concentration, and allowing concentrate to enter the next stage of concentration; and returning the tailings subjected to 8 times of concentration to the previous-stage concentration.
8. The method for removing the chemicals and floating the polymetallic co-associated fluorite ore according to claim 6, which is characterized in that: the acidified water glass is prepared by reacting water glass and concentrated sulfuric acid according to the mass ratio of 5: 1-5: 3.
9. The method for removing the chemicals and floating the polymetallic co-associated fluorite ore according to claim 1, which is characterized in that: the scavenged tailings are directly discarded, and concentrate enters 1-time concentration.
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| 孔朝鹏 等: "河南某白钨矿伴生高钙萤石综合回收新工艺研究", 《矿冶工程》 * |
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