CN112058503A - Silico-calcium collophanite double-reverse flotation process - Google Patents
Silico-calcium collophanite double-reverse flotation process Download PDFInfo
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- B03D1/02—Froth-flotation processes
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Abstract
The invention relates to a silico-calcium collophanite double reverse flotation process, which comprises the following specific steps: 1) reverse flotation magnesium removal; 2) dehydrating and mixing the reverse flotation demagging rough concentrate; 3) reverse flotation desilication: adding a regulator into the pulp after size mixing, regulating the pH value of the pulp to be 7-9, adding a cation collector to perform desiliconization reverse roughing operation, wherein the inside of a desiliconization reverse roughing tank is concentrate pulp, the concentrate pulp is concentrated and dehydrated to obtain final concentrate, desiliconization reverse roughing foam is scavenged, desiliconization middlings are arranged in a desiliconization scavenging tank, the desiliconization middlings are returned to the desiliconization reverse roughing operation, and the desiliconization scavenging foam is reverse flotation desiliconized tailings. The double reverse flotation process overcomes the problems of the existing flotation process, eliminates the interference of reverse flotation demagging on reverse flotation desilicification, obtains low-magnesium and low-silicon phosphate concentrate, reduces the foam amount and the viscosity of the foam, improves the fluidity of the flotation foam, is easy to convey the foam, improves the flotation efficiency, and ensures that the double reverse flotation of the silicon-calcium collophanite is easy to engineer.
Description
Technical Field
The invention belongs to the technical field of mineral processing, and particularly relates to a silico-calcic collophanite double-reverse flotation process.
Background
Phosphorite is an indispensable basic raw material for producing phosphate fertilizers and phosphorus chemical products, the resource reserves of phosphorite in China are rich, but the grade is low, the silicon-calcium medium-low grade collophanite is taken as the main material, and the phosphorite has the characteristics of complex mosaic relation, fine mosaic granularity and poor dissociation property of various minerals, and has high content of silicate minerals and carbonate minerals, so the development and the utilization of the phosphorite are difficult worldwide. At present, direct flotation is adopted for easily-selected phosphorite in phosphorite flotation, a single reverse flotation process is adopted in most ore dressing plants, a fatty acid soap anionic collector is used for floating dolomite gangue minerals in the phosphorite in a weakly acidic medium, the content of MgO is reduced, and the grade of phosphate concentrate is improved. The double reverse flotation process is reasonable in treatment of the type of phosphorite, the negative ion type collecting agent is used for reverse flotation and magnesium removal, the positive ion type collecting agent is used for reverse flotation and silicon removal, wherein an amine medicament is generally adopted as the collecting agent in the flotation and silicon removal process, and the collecting agent has the problems of large foaming amount, sticky foam, difficulty in defoaming, poor fluidity, difficulty in treatment of foam products, poor selectivity, sensitivity to slime and the like, so that the flotation and silicon removal effect is poor.
Therefore, the research and development of the flotation reagent with good flotation performance to develop and utilize the medium and low grade silicon calcium phosphate ore resources by combining the current phosphate ore dressing technical situation and the development of the flotation reagent have great significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a silico-calcareous collophanite double reverse flotation process with high demagging and desiliconization efficiency, which is simple to operate, does not need to treat mineral processing wastewater, can be directly recycled, simultaneously reduces the viscosity of foam, is easy to crush the foam, is convenient to convey and has more smooth flotation flow.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
the double reverse flotation process for silico-calcium collophanite is provided, and comprises the following steps:
1) reverse flotation demagging: crushing and grinding the silicon-calcium collophanite ore to separate mineral monomers, adding water to obtain ore pulp, enabling the obtained ore pulp to flow into a reverse flotation stirring tank, adding a demagging acid regulator into the tank to adjust the pH value of the ore pulp to be 5-6.5, enabling the adjusted material to enter a reverse flotation system, adding an anion collecting agent to perform demagging reverse roughing operation, enabling reverse flotation demagging rough concentrate to be in the flotation tank, adding the demagging acid regulator into reverse roughing foam again to enable the pH value of the ore pulp to be 4-4.8, performing reverse flotation demagging operation, enabling demagging middling to be in the scavenging tank, returning the demagging reverse roughing operation, and enabling scavenging foam to be reverse flotation demagging tailings;
2) dehydrating and mixing the reverse flotation demagging rough concentrate: transferring the reverse flotation demagging rough concentrate obtained in the step 1) into a settling concentration dehydration device to remove wastewater containing an anionic collector, directly adding the removed wastewater as supplemented water into the demagging reverse flotation and the reverse flotation demagging operation of the step 1) for flotation, allowing settling concentration underflow to enter a stirring tank, adding clear water or return water (wastewater obtained by concentration and dehydration in the reverse flotation desilication stage in the step 3) and mixing to obtain ore pulp with the mass concentration of 25-35%;
3) reverse flotation desilication: adding a regulator into the ore pulp subjected to size mixing in the step 2), regulating the pH value of the ore pulp to 7-9, adding a cationic collector to perform desiliconization and reverse roughing operation, wherein the desiliconization and reverse roughing tank is concentrate pulp, the concentrate pulp is concentrated and dehydrated to obtain final concentrate, the dehydrated wastewater is used as return water and is added into the step 2), desiliconization and reverse roughing foam is scavenged, desiliconization middlings are arranged in the desiliconization scavenging tank, the desiliconization middlings are returned to the desiliconization and reverse roughing operation, and the desiliconization scavenging foam is reverse flotation desiliconized tailings.
According to the scheme, the magnesium removal acidity regulator in the step 1) is sulfuric acid or phosphoric acid.
According to the scheme, the anionic collector in the step 1) is a fatty acid collector LAA-11, and the using amount of the anionic collector is 0.45-0.75Kg/t of raw ore.
According to the scheme, the regulator in the step 3) is a mixture of sodium hydroxide, sodium citrate and trisodium phosphate, and the mass ratio of the regulator to the sodium citrate is 1: 1: 3 to 5 percent, and the dosage is 2.5 to 3.5Kg/t of raw ore. The sodium hydroxide, the sodium citrate and the trisodium phosphate in the regulator are all alkaline regulators, the sodium hydroxide is mainly used for regulating the pH value of the ore pulp, and the sodium citrate and the trisodium phosphate can effectively inhibit phosphorus minerals from being floated and simultaneously synergistically reduce the viscosity of foams.
According to the scheme, the cationic collector in the step 3) is coconut oil diamine and derivatives thereof, and the using amount of the cationic collector is 0.3-0.75Kg/t of raw ore.
Preferably, the cationic collector is N-coco-1, 3-propylenediamine and its derivatives, such as N-coco-1, 3-propylenediguanidine.
The invention adopts a double reverse flotation process to carry out flotation on silico-calcium collophanite, in the double reverse flotation process of the silico-calcium collophanite, the reverse flotation demagging process structure is one-time roughing and one-time scavenging operation, scavenging middlings are returned, reverse flotation demagging rough concentrates are dehydrated and mixed, a regulator is added for carrying out reverse flotation desiliconization, and the reverse flotation silicate minerals process structure is one-time roughing and one-time scavenging operation scavenging middlings are returned.
The invention has the beneficial effects that: the double reverse flotation process overcomes the problems of the prior flotation process, eliminates the interference of reverse flotation and desilicication on reverse flotation by reverse flotation and demagging, and obtains the phosphate concentrate (P) with low magnesium and low silicon2O5More than 30%, MgO less than 0.8%, SiO2The content of the silicon-calcium collophanite is less than 8 percent), and simultaneously, the foam quantity is reduced, the viscosity of the foam is reduced, the fluidity of the flotation foam is improved, the foam is easy to convey, the flotation efficiency is improved, and the silicon-calcium collophanite double-reverse flotation is easy to engineer.
Drawings
FIG. 1 is a flow chart of a double reverse flotation process in an embodiment of the invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Example 1
A silico-calcic collophanite double reverse flotation process is shown in a flow chart in figure 1 and comprises the following specific steps:
1) reverse flotation demagging: silico-calcareous low grade collophanite (P)2O525.56% of (A), 1.45% of MgO, SiO2The content of the mineral is 13.5 percent), mineral monomers are separated through crushing and grinding, water is added for size mixing until the mass concentration is 28 percent, then the mineral slurry flows into a stirring barrel, sulfuric acid (93 weight percent) with the dosage of 6.0Kg/t of raw ore and phosphoric acid with the dosage of 2.5Kg/t of raw ore are respectively added into the mineral slurry, the pH value of the mineral slurry is adjusted to be 6, anionic fatty acid (soap) collecting agent LAA-11 with the dosage of 0.45Kg/t is added, then the magnesium removal reverse roughing operation is carried out, and reverse flotation refined mineral slurry is arranged in a flotation tank; the carbonate mineral enters a reverse flotation foam product, sulfuric acid (93 wt%) with the amount of 3.0Kg/t of raw ore is added into the reverse flotation foam product again, scavenging is carried out after the pH value of ore pulp is 4, the scavenged flotation demagging is carried out to obtain a foam product reverse flotation demagging tailing, and the demagging middling in a scavenging tank returns to the reverse roughing operation;
2) standing and clarifying the reverse flotation concentrate pulp in the tank, removing wastewater containing an anionic collector by using a settling, concentrating and dehydrating device, wherein the wastewater can be used as return water to return to the reverse flotation and magnesium removal process in the step 1) without being treated, reducing the using amount of the clear water, adding the clear water or the return water of reverse flotation and desilicification into the dehydrated pulp, and mixing the pulp to obtain pulp with the mass concentration of 25%;
3) reverse flotation desilication: adding a mixture of sodium hydroxide, sodium citrate and trisodium phosphate into the ore pulp with the concentration of 25% in the step 2), wherein the mass ratio of the mixture to the trisodium phosphate is 1: 1: 3, mixing and stirring the raw ore with the amount of 2.5Kg/t for 2min, adjusting the pH value of the ore pulp to 7.0, adding N-cocoyl-1, 3-propylenediamine with the amount of 0.3Kg/t of the raw ore to perform desiliconization reverse roughing operation, wherein the desiliconization reverse roughing tank is concentrate pulp, the concentrate pulp is concentrated and dehydrated to obtain final concentrate, the dehydrated wastewater is used as return water and added into the step 2), the desiliconization reverse roughing foam product is used for scavenging the desiliconized silicate mineral tailings, the scavenging tank is used for desiliconization middlings, the desiliconization middlings are returned to the desiliconization reverse roughing operation, and the scavenged foam product is reverse flotation desiliconized tailings. Combining the reverse flotation demagging tailings in the step 1) and the reverse flotation desiliconization tailings in the step 3), discharging and stacking. Final concentrate grade P2O530.2 percent, the recovery rate is 86.52 percent, the magnesium removal rate is 75.12 percent, and the silicon removal rate is 65.56 percent.
Example 2
A silico-calcic collophanite double reverse flotation process comprises the following specific steps:
1) reverse flotation demagging: silico-calcareous low grade collophanite (P)2O525.56 percent of the total content of the magnesium oxide, 1.45 percent of the total content of the magnesium oxide and 13.5 percent of the total content of the SiO 2), crushing and grinding the ore to separate mineral monomers, adding water to adjust the pulp to have a mass concentration of 28 percent, then flowing into a stirring barrel, respectively adding 7.5Kg/t of sulfuric acid of the raw ore and 2.0Kg/t of phosphoric acid of the raw ore into the ore pulp, adjusting the pH value of the ore pulp to be 5.8, adding 0.75Kg/t of anionic fatty acid (soap) collecting agent LAA-11, and then carrying out demagging operation, wherein the flotation tank is reverse flotation concentrate; the carbonate mineral enters into the reverse flotation froth product, and the reverse flotation froth product is added with 3.0Kg/t of raw ore sulfuric acid (93 wt%) again to ensure thatScavenging after the pH value of the ore pulp is 4.5 to obtain foam product reverse flotation demagnetised tailings, and returning the demagnetised middlings in the scavenging tank to reverse roughing operation;
2) standing and clarifying the reverse flotation concentrate pulp in the tank, removing wastewater containing an anionic collector by using a settling, concentrating and dehydrating device, wherein the wastewater can be used as return water to return to the reverse flotation and magnesium removal process in the step 1) without being treated, reducing the using amount of the clear water, adding the clear water or the return water of reverse flotation and desilicification into the dehydrated pulp, and mixing the pulp to obtain pulp with the mass concentration of 25%;
3) reverse flotation desilication: reverse flotation desilication: adding a mixture of sodium hydroxide, sodium citrate and trisodium phosphate into the ore pulp with the concentration of 25% in the step 2), wherein the mass ratio of the mixture to the trisodium phosphate is 1: 1: 4, mixing and stirring the raw ore with the amount of 3.0Kg/t for 2min, adjusting the pH value of the ore pulp to 8.0, adding N-cocoyl-1, 3-propylenediamine with the amount of 0.6Kg/t of the raw ore to perform desiliconization reverse roughing operation, wherein the desiliconization reverse roughing tank is concentrate pulp, the concentrate pulp is concentrated and dehydrated to obtain final concentrate, the dehydrated wastewater is used as return water and added into the step 2), the desiliconization reverse roughing foam product is used for scavenging the desiliconized silicate mineral tailings, the scavenging tank is used for desiliconization middlings, the desiliconization middlings are returned to the desiliconization reverse roughing operation, and the scavenged foam product is reverse flotation desiliconized tailings. Combining the reverse flotation demagging tailings in the step 1) and the reverse flotation desiliconization tailings in the step 3), discharging and stacking. Final concentrate grade P2O530.1 percent, the recovery rate is 86.6 percent, the magnesium removal rate is 75.56 percent, and the silicon removal rate is 66.56 percent.
Example 3
A silico-calcic collophanite double reverse flotation process comprises the following specific steps:
1) reverse flotation demagging: silico-calcareous low grade collophanite (P)2O525.56% of (A), 1.45% of MgO, SiO2Content of 13.5%), breaking and grinding to separate mineral monomers, mixing to 28% mass concentration, stirring in stirring tank, adding 9.0Kg/t sulfuric acid (93 wt%) and 1.5Kg/t phosphoric acid, regulating pH to 5.5, and adding 0.75Kg/t collecting agent of anionic fatty acid (soap)Performing magnesium removal and reverse roughing operation after LAA-11, wherein reverse flotation concentrate pulp is in the flotation tank; the carbonate mineral enters a reverse flotation foam product, sulfuric acid (93 wt%) with the amount of 3.0Kg/t of raw ore is added into the reverse flotation foam product again, scavenging is carried out after the pH value of ore pulp is 4.8, the scavenged flotation demagging is carried out to obtain a foam product reverse flotation demagging tailing, and the demagging middling in a scavenging tank returns to the reverse roughing operation;
2) standing and clarifying the reverse flotation concentrate pulp in the tank, removing wastewater containing an anionic collector by using a settling, concentrating and dehydrating device, wherein the wastewater can be used as return water to return to the reverse flotation and magnesium removal process in the step 1) without being treated, reducing the using amount of the clear water, adding the clear water or the return water of reverse flotation and desilicification into the dehydrated pulp, and mixing the pulp to obtain pulp with the mass concentration of 25%;
3) reverse flotation desilication: adding a mixture of sodium hydroxide, sodium citrate and trisodium phosphate into the ore pulp with the concentration of 25% in the step 2), wherein the mass ratio of the mixture to the trisodium phosphate is 1: 1: 5, mixing and stirring the raw ore with the amount of 3.5Kg/t for 2min, adjusting the pH value of the ore pulp to 9.0, adding N-cocoyl-1, 3-propylenediamine with the amount of 0.75Kg/t of the raw ore to perform desiliconization reverse roughing operation, wherein the desiliconization reverse roughing tank is concentrate pulp, the concentrate pulp is concentrated and dehydrated to obtain final concentrate, the dehydrated wastewater is used as return water and added into the step 2), the desiliconization reverse roughing foam product is used for scavenging the desiliconized silicate mineral tailings, the scavenging tank is used for desiliconization middlings, the desiliconization middlings are returned to the desiliconization reverse roughing operation, and the scavenged foam product is reverse flotation desiliconized tailings. Combining the reverse flotation demagging tailings in the step 1) and the reverse flotation desiliconization tailings in the step 3), discharging and stacking. Final concentrate grade P2O530.3 percent, the recovery rate is 86.1 percent, the magnesium removal rate is 73.56 percent, and the silicon removal rate is 62.56 percent.
Example 4
Yichang certain silicon-calcium collophanite double reverse floating process test
The chemical composition of Yichang certain phosphate ore is shown in Table 1.
TABLE 1 chemical composition of raw ore
Crushing raw ore to-2 mm by a crusher, grinding by an ore grinder to the fineness of-0.074 mm and 81.0 percent by weight, adding water to adjust the pulp to the mass concentration of 33.5 percent, adding 9.0Kg/t of raw ore sulfuric acid (93 percent by weight) and 1.5Kg/t of raw ore phosphoric acid into the pulp, adjusting the pH value of the pulp to 5.2, adding 0.6Kg/t of raw ore collecting agent LAA-11, performing reverse-flotation and reverse-roughing operation, performing reverse-flotation on the pulp, feeding carbonate mineral into a reverse-flotation foam product, adding 3.0Kg/t of raw ore sulfuric acid (93 percent by weight) into the reverse-flotation foam product, performing scavenging after the pH value of the pulp is 4.5, performing scavenging to obtain a foam product reverse-flotation and magnesium-removed tailings, returning the magnesium-removed pulp in the scavenging tank to the reverse-roughing operation, standing the reverse-flotation operation in the scavenging tank, and (2) removing the wastewater containing the anionic collecting agent by using a settling, concentrating and dehydrating device, wherein the wastewater can be used as return water to return to the reverse flotation demagging process without being treated, reducing the using amount of clear water, adding clear water or return water of reverse flotation desilicification into the dehydrated ore pulp, and mixing the pulp to obtain the ore pulp with the mass concentration of 28%. Adding a mixture of sodium hydroxide, sodium citrate and trisodium phosphate into the ore pulp, wherein the mass ratio of the sodium hydroxide to the sodium citrate to the trisodium phosphate is 1: 1: 4, mixing and stirring the raw ore with the amount of 3.0Kg/t for 2min, adjusting the pH value of the ore pulp to 8.0, adding N-cocoyl-1, 3-propylenediamine with the amount of 0.75Kg/t of the raw ore to perform desiliconization reverse roughing operation, wherein the desiliconization reverse roughing tank is concentrate pulp, the concentrate pulp is concentrated and dehydrated to obtain final concentrate, the dehydrated wastewater is used as return water and added into the previous step, a desiliconization reverse roughing foam product is used for scavenging the desiliconized mineral tailings, a product in the scavenging tank is desiliconized middlings, the desiliconized middlings are returned to the desiliconization reverse roughing operation, and the scavenged foam product is reverse flotation desiliconized tailings. The reverse flotation demagging tailings and the reverse flotation desilicication tailings are merged, discharged and stacked. Final concentrate grade P2O530.5%, MgO content 0.72%, SiO2Content of 7.5%, yield 73.52%, concentrate P2O5The recovery was 86.23%.
Example 5
In the silico-calcium collophanite double reverse flotation process described in example 2, the reverse flotation desilication regulator is a mixture of sodium hydroxide, sodium citrate and trisodium phosphate, and the mass ratio of the reverse flotation desilication regulator to the trisodium phosphate is 1: 1: 4, the amount is 3.0Kg/t raw ore, after the regulator is added, the foam amount of the reverse flotation is reduced and is brittle, and the foam is easy to be defoamed, and the foam height without the regulator and with the regulator is shown in a table 2.
TABLE 2 foam height (cm) without addition of conditioner
Table 2 shows that the regulator of the invention is not added and added in the roughing of the reverse flotation desiliconization, the stacking height of reverse flotation foam in a container is 16.5cm and 13.5cm in sequence, the height of the foam is reduced by 3 and 0cm, after standing for 30min, the regulator of the invention is not added, the height of the foam is only reduced by 4.5cm, and the foam height is reduced by 5.5cm by adding the regulator of the invention, which indicates that the regulator of the invention reduces the foam generation amount in the process of the reverse flotation desiliconization, accelerates the defoaming speed, and improves the defoaming speed by 0.17 mm/min.
Claims (6)
1. A silico-calcic collophanite double reverse flotation process is characterized by comprising the following specific steps:
1) reverse flotation demagging: crushing and grinding the silicon-calcium collophanite ore to separate mineral monomers, adding water to obtain ore pulp, enabling the obtained ore pulp to flow into a reverse flotation stirring tank, adding a demagging acid regulator into the tank to adjust the pH value of the ore pulp to be 5-6.5, enabling the adjusted material to enter a reverse flotation system, adding an anion collecting agent to perform demagging reverse roughing operation, enabling reverse flotation demagging rough concentrate to be in the flotation tank, adding the demagging acid regulator into reverse roughing foam again to enable the pH value of the ore pulp to be 4-4.8, performing reverse flotation demagging operation, enabling demagging middling to be in the scavenging tank, returning the demagging reverse roughing operation, and enabling scavenging foam to be reverse flotation demagging tailings;
2) dehydrating and mixing the reverse flotation demagging rough concentrate: transferring the reverse flotation demagging rough concentrate obtained in the step 1) into a settling concentration dehydration device to remove wastewater containing an anionic collector, directly adding the removed wastewater as supplemented water into the demagging reverse flotation and reverse flotation demagging operation of the step 1) for flotation, allowing settling concentration underflow to enter a stirring tank, and adding clear water or return water for size mixing to obtain ore pulp with the mass concentration of 25-35%;
3) reverse flotation desilication: adding a regulator into the ore pulp subjected to size mixing in the step 2), regulating the pH value of the ore pulp to 7-9, adding a cationic collector to perform desiliconization and reverse roughing operation, wherein the desiliconization and reverse roughing tank is concentrate pulp, the concentrate pulp is concentrated and dehydrated to obtain final concentrate, the dehydrated wastewater is used as return water and is added into the step 2), desiliconization and reverse roughing foam is scavenged, desiliconization middlings are arranged in the desiliconization scavenging tank, the desiliconization middlings are returned to the desiliconization and reverse roughing operation, and the desiliconization scavenging foam is reverse flotation desiliconized tailings.
2. The silico-calcic collophanite double reverse flotation process of claim 1, wherein the demagging acidity regulator of step 1) is sulfuric acid or phosphoric acid.
3. The silico-calcic collophanite double reverse flotation process according to claim 1, wherein the anionic collector in step 1) is fatty acid collector LAA-11, and the amount of the anionic collector is 0.45-0.75Kg/t raw ore.
4. The silico-calcium collophanite double reverse flotation process according to claim 1, wherein the modifier of step 3) is a mixture of sodium hydroxide, sodium citrate and trisodium phosphate, and the mass ratio of the modifier is 1: 1: 3 to 5 percent, and the dosage is 2.5 to 3.5Kg/t of raw ore.
5. The silico-calcic collophanite double reverse flotation process according to claim 1, wherein the cationic collector in step 3) is cocodiamine and derivatives thereof, and the dosage is 0.3-0.75Kg/t raw ore.
6. The silico-calcic collophanite double reverse flotation process according to claim 5, wherein the cationic collector is N-coco-1, 3-propylenediamine and its derivatives.
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CN113182077A (en) * | 2021-04-08 | 2021-07-30 | 宜都兴发化工有限公司 | Reverse flotation process for synchronously removing magnesium and aluminum in phosphorite |
CN113182078A (en) * | 2021-04-08 | 2021-07-30 | 宜都兴发化工有限公司 | Phosphorite mixing reverse flotation process |
CN114011580A (en) * | 2021-10-29 | 2022-02-08 | 宜都兴发化工有限公司 | Impurity removal method for low-grade micro-fine particle phosphate ore |
CN114011585A (en) * | 2021-10-29 | 2022-02-08 | 宜都兴发化工有限公司 | Flotation method for fine-grained collophanite in gravity concentration tailings |
CN114308398A (en) * | 2021-12-24 | 2022-04-12 | 武汉工程大学 | Flotation washing, decoloring and purifying method for phosphogypsum |
CN114682387A (en) * | 2020-12-30 | 2022-07-01 | 中蓝连海设计研究院有限公司 | Phosphorite double-reverse flotation method |
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