CN117225595B - Reverse flotation process of hematite - Google Patents
Reverse flotation process of hematite Download PDFInfo
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- CN117225595B CN117225595B CN202311033011.5A CN202311033011A CN117225595B CN 117225595 B CN117225595 B CN 117225595B CN 202311033011 A CN202311033011 A CN 202311033011A CN 117225595 B CN117225595 B CN 117225595B
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- hematite
- reverse flotation
- ore pulp
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- 229910052595 hematite Inorganic materials 0.000 title claims abstract description 99
- 239000011019 hematite Substances 0.000 title claims abstract description 99
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 238000005188 flotation Methods 0.000 title claims abstract description 96
- 238000000034 method Methods 0.000 title claims abstract description 57
- 230000008569 process Effects 0.000 title claims abstract description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000003112 inhibitor Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 20
- 230000001105 regulatory effect Effects 0.000 claims abstract description 20
- 229920001444 polymaleic acid Polymers 0.000 claims abstract description 18
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 150000003931 anilides Chemical class 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 37
- 239000000047 product Substances 0.000 claims description 31
- 239000002131 composite material Substances 0.000 claims description 30
- 229920000141 poly(maleic anhydride) Polymers 0.000 claims description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 239000012141 concentrate Substances 0.000 claims description 15
- 239000004088 foaming agent Substances 0.000 claims description 14
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 241000779819 Syncarpia glomulifera Species 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000001739 pinus spp. Substances 0.000 claims description 9
- 229940036248 turpentine Drugs 0.000 claims description 9
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 8
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 8
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 7
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- BKRJTJJQPXVRRY-UHFFFAOYSA-M dodecyl-(2-hydroxyethyl)-dimethylazanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)CCO BKRJTJJQPXVRRY-UHFFFAOYSA-M 0.000 claims description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 6
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- WUBBRNOQWQTFEX-UHFFFAOYSA-N 4-aminosalicylic acid Chemical compound NC1=CC=C(C(O)=O)C(O)=C1 WUBBRNOQWQTFEX-UHFFFAOYSA-N 0.000 claims description 3
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 3
- 229960004909 aminosalicylic acid Drugs 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001308 synthesis method Methods 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 abstract description 19
- 235000019698 starch Nutrition 0.000 abstract description 19
- 239000008107 starch Substances 0.000 abstract description 19
- 239000000203 mixture Substances 0.000 abstract description 9
- 238000001914 filtration Methods 0.000 abstract description 4
- 230000005764 inhibitory process Effects 0.000 abstract description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 2
- 239000011707 mineral Substances 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 18
- 238000002360 preparation method Methods 0.000 description 12
- 229910052742 iron Inorganic materials 0.000 description 9
- 238000011084 recovery Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 229920002261 Corn starch Polymers 0.000 description 5
- 239000008120 corn starch Substances 0.000 description 5
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- JBSOOFITVPOOSY-KTKRTIGZSA-N 2-hydroxyoleic acid Chemical compound CCCCCCCC\C=C/CCCCCCC(O)C(O)=O JBSOOFITVPOOSY-KTKRTIGZSA-N 0.000 description 3
- 239000012190 activator Substances 0.000 description 3
- 125000000129 anionic group Chemical group 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 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
- 150000002888 oleic acid derivatives Chemical class 0.000 description 3
- 229940006295 sulfonated oleic acid Drugs 0.000 description 3
- 239000003784 tall oil Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of mineral separation, in particular to a reverse flotation process of hematite. The invention comprises the following steps: step one: crushing hematite ore according to the requirement, and grinding until the proportion of the granularity of-0.074 mm is more than or equal to 70%; step two: adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to be 30% -35%; step three: and (3) feeding the mixture into a flotation tank, regulating the pH value of the flotation pulp to 9-10 by using sodium carbonate or sodium hydroxide, and adding hydroxamated polymaleic acid and 4-hydroxy-3-carboxyl-maleic anilide as hematite inhibitors. The novel hematite inhibitor hydroximoylation polymaleic acid and 4-hydroxy-3-carboxyl-maleanilide adopted by the invention can be adsorbed on the surface of the hematite, the inhibition capacity and selectivity are stronger than those of starch, the water solubility is better than that of starch, the molecular weight is lower than that of starch, and the efficiency of the subsequent filtering process can be effectively improved; and the reverse flotation desilication process is simple in flow, convenient to operate, low in beneficiation cost, good in industrial feasibility and convenient for large-scale popularization.
Description
Technical Field
The invention relates to the technical field of mineral separation, in particular to a reverse flotation process of hematite.
Background
SiO 2 is the most common impurity in hematite. For the 'iron extraction and silicon reduction', the most common methods in the current production mainly comprise two methods, namely cationic reverse flotation and anionic reverse flotation. In both reverse flotation processes, inhibitors are used to inhibit hematite, which is retained as an iron concentrate in the tailings, while quartz impurities are removed by flotation with a cationic or anionic collector. Thus, the flotation reagent plays a key role in the reverse flotation desilication of hematite.
Currently, the prior art for reverse flotation of hematite is mainly:
The Chinese patent with publication number CN105233992A discloses a normal-temperature short-flow reverse flotation method of hematite, which comprises the following steps: (1) adding water into ore feed to prepare ore pulp; (2) Carrying out reverse flotation roughing on ore pulp at 22-25 ℃, and (3) carrying out reverse flotation concentration on roughing concentrate at 22-25 ℃ to obtain concentrate and concentration tailings; the collector comprises the following chemical components in percentage by mass: sodium lignin sulfonate 0-60%; 35-90% of acidized oil; 5-20% of polyoxyethylene polyoxypropylene block polyether.
The invention discloses a 'method for desilication of hematite by reverse flotation' of Chinese patent publication No. CN109622233A, which comprises the steps of mixing hematite samples to be selected with water, stirring uniformly to obtain ore pulp, and adding the collector under the natural pH value of the ore pulp; optionally, adding an inhibitor, and performing reverse flotation desilication to obtain a hematite concentrate product. The method selects quaternary ammonium salt collecting agents.
The Chinese patent document with the publication number of CN212403982U discloses a 'system for preparing hematite inhibitor corn starch for reverse flotation', which specifically comprises a feeding device and a preparation device, wherein the preparation device comprises: the device comprises a first preparation unit, a cold water supply device, a second preparation unit and a hot water supply device, wherein the cold water supply device supplies cold water to the first preparation unit, the first preparation unit is also connected with a feeding device, and corn starch and the cold water form a corn starch colloid in the first preparation unit; the hot water supply device supplies hot water to the second preparation unit, the second preparation unit is also connected with the first preparation unit, and the corn starch colloid and the hot water form a corn starch solution in the second preparation unit to serve as a hematite inhibitor for reverse flotation.
The currently practiced process, whether cationic or anionic, hematite depressants are essential, largely determine the "iron and silicon" effect. Starch and its derivatives are the most common and most widely used inhibitors of hematite. Studies have shown that the ability of starch to inhibit hematite is due to hydrogen bonding formed between the hydroxyl groups of starch and the hematite mineral. However, starch is generally high in molecular weight, resulting in poor solubility properties and also tends to cause difficulties in concentrate and tailings filtration. Based on this, a reverse flotation process of hematite is proposed, which provides a solution to the above problems.
Disclosure of Invention
The invention aims to provide a reverse flotation process of hematite, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the method comprises the following steps:
step one: crushing hematite ore according to the requirement, and grinding until the proportion of the granularity of-0.074 mm is more than or equal to 70%;
Step two: adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to be 30% -35%;
Step three: feeding the mixture into a flotation tank, regulating the pH value of flotation pulp to 9-10 by using sodium carbonate or sodium hydroxide, adding hydroxamated polymaleic acid (HAPMA) and 4-hydroxy-3-carboxyl-maleanilide (ASPMA) as hematite inhibitors, and stirring for 5 minutes;
step four: and adding a composite collector M and a foaming agent into the ore pulp for primary reverse flotation roughing and primary reverse flotation concentration to obtain hematite concentrate and concentration tailings.
Furthermore, TFe in the hematite ore is more than or equal to 45 wt% and SiO 2 in the hematite ore is more than or equal to 15 wt%.
Further, the adding amount of the hematite inhibitor in the third step is 100-150 g/t, and the using amount ratio of the hydroxamated polymaleic acid to the 4-hydroxy-3-carboxyl-maleimide is 1:1-1:2 (molar ratio) based on the total amount of the ore pulp.
Further, the method for synthesizing the hydroxamated polymaleic acid in the step three comprises the following steps:
at 85-90 ℃, the maleic anhydride is polymerized in toluene solution by Benzoyl Peroxide (BPO) to prepare polymaleic anhydride (PMA), and the molecular weight of the polymaleic anhydride is about 1000;
At 20-30 ℃, hydroxylamine hydrochloride with the anhydride bond mole ratio of 30% in the polymaleic anhydride is dissolved in a methanol solution, and sodium hydroxide with the same mole amount is added to release hydroxylamine, then filtrate is dripped into the methanol solution of polymaleic anhydride to react for 3 hours at room temperature, and after the reaction is completed, the product is dried, so that the hydroxamated polymaleic acid is obtained.
Further, the synthesis method of the 4-hydroxy-3-carboxyl-maleanilide in the step three comprises the following steps:
at 85-90 ℃, the maleic anhydride is polymerized in toluene solution by benzoyl peroxide to prepare polymaleic anhydride, and the molecular weight of the polymaleic anhydride is about 1200;
at 20-30 ℃, p-aminosalicylic acid and polymaleic anhydride with the anhydride bond mole ratio of 10% in polymaleic anhydride are dissolved in Tetrahydrofuran (THF), the reaction is carried out for 3 hours at room temperature, and after the reaction is finished, the product is dried, so that 4-hydroxy-3-carboxyl-maleanilide is obtained.
Further, in the fourth step, the composite collector M is mixed with sodium lignin sulfonate, sodium dodecyl sulfate, dodecyl dimethyl hydroxyethyl ammonium chloride and ethylene glycol according to a mass ratio of 1:2:2:2.
Further, in the fourth step, a composite collector M and a foaming agent are added into ore pulp for primary reverse flotation roughing and primary reverse flotation refining, and the method comprises the following steps:
adding a composite collector M into the ore pulp and stirring for 4min;
adding 50g/t of turpentine as a foaming agent, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher separation;
and adding hematite inhibitor hydroxamated polymaleic acid and 4-hydroxy-3-carboxyl-maleic anilide into the roughing product for reverse flotation and concentration with a composite collector M, and collecting the concentration product.
Further, in the reverse flotation roughing process, the adding amount of the composite collector M is 300-400 g/t based on the total amount of ore pulp;
And the addition amount of the hematite inhibitor is 150-180 g/t and the addition amount of the composite collector M is 350-350 g/t based on the total amount of the primary selected products.
Compared with the prior art, the invention has the beneficial effects that:
The novel hematite inhibitor hydroximoylation polymaleic acid and 4-hydroxy-3-carboxyl-maleanilide adopted by the invention can be adsorbed on the surface of the hematite, the inhibition capacity and selectivity are stronger than those of starch, the water solubility is better than that of starch, the molecular weight is lower than that of starch, and the efficiency of the subsequent filtering process can be effectively improved;
The composite collector has the characteristics of good solubility, convenient preparation and no corrosion to equipment; the material is low-temperature resistant and has good sorting effect at 5-10 ℃; the method has the advantages of strong collecting capacity, small dosage and high selectivity;
The reverse flotation process can obtain hematite concentrate TFe which is more than or equal to wt 62 percent, the recovery rate is more than or equal to 87 percent, and the reverse flotation desilication process is simple in flow, convenient to operate, low in beneficiation cost, good in industrial feasibility and convenient for large-scale popularization.
Drawings
FIG. 1 is a schematic illustration of the process flow of the present invention.
Description of the embodiments
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
An inverse flotation process of hematite, the beneficiation process flow adopted in the embodiment is shown in figure 1;
some hematite sample was from Liaoning some iron ore, where TFe wt 46.75%, siO 2 wt 17.34%.
The method is realized by the following steps:
(1) Crushing hematite ore, grinding until the particle size is-0.074 mm, wherein the proportion is more than or equal to 70%;
(2) Adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to be 32%;
(3) Sending the mixture into a flotation tank, regulating the pH value of flotation pulp to be 10 by using sodium carbonate, adding HAPMA and ASPMA as hematite inhibitors, wherein the addition amount is 120g/t, the dosage ratio of HAPMA to ASPMA is 1:1, and stirring for 5 minutes;
(4) Adding 300g/t of a composite collector M (mixing sodium lignin sulfonate, sodium dodecyl sulfonate, dodecyl dimethyl hydroxyethyl ammonium chloride and ethylene glycol according to the mass ratio of 1:2:2:2), and stirring for 4 min; adding 50g/t of turpentine as a foaming agent, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher separation; adding hematite inhibitor (HAPMA: ASPMA molar ratio is 1:1.2) into the roughed product, performing reverse flotation and concentration by using a composite collector M (the dosage is 350 g/t), and collecting the concentrated product.
The example gives a hematite concentrate TFe wt 63.26%, recovery 89.27%, siO 2 wt 2.12%.
Comparative example 1
Hematite samples were from Liaoning iron ore, with TFe wt 46.75%, siO 2 wt 17.34%.
The method comprises the following steps:
(1) Crushing hematite ore, grinding until the particle size is-0.074 mm, wherein the proportion is more than or equal to 70%;
(2) Adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to be 32%;
(3) Feeding the mixture into a flotation tank, regulating the pH value of flotation pulp to be 10 by using sodium carbonate, adding starch as a hematite inhibitor, adding 600g/t, and stirring for 5 minutes;
(4) Weighing 20 parts of hydroxy oleic acid, 40 parts of sulfonated oleic acid and 20 parts of tall oil, mixing the three fatty acids at room temperature, stirring for 15-30min, adding 10 parts of foaming agent turpentine, and continuously stirring for 15min to obtain a uniform solution. Dissolving 16 parts of sodium hydroxide into 100 parts of water, slowly adding the solution into the solution, uniformly stirring the solution at 35 ℃ to fully saponify the solution to obtain a hematite reverse flotation desilication collector M2, adding the M2 into ore pulp according to 600g/t, and stirring the solution for 4min; adding quartz activator calcium oxide with the dosage of 500g/t, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher; and adding starch (the dosage is 650 g/t) into the roughing product, carrying out reverse flotation and concentration on the roughing product by using a composite collector M2 (the dosage is 750 g/t), and collecting the concentration product.
The example obtained hematite concentrate TFe wt 57.72%, recovery 81.35%, siO 2 wt 3.75%.
Examples
An inverse flotation process of hematite, the beneficiation process flow adopted in the embodiment is shown in figure 1;
some hematite sample was from Hebei's certain iron ore, where TFe wt 48.23%, siO 2 wt 15.52%.
The method is realized by the following steps:
(1) Crushing hematite ore, grinding until the particle size is-0.074 mm, wherein the proportion is more than or equal to 70%;
(2) Adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to 35%;
(3) Sending the mixture into a flotation tank, regulating the pH value of flotation pulp to be 10 by using sodium carbonate, adding HAPMA and ASPMA as hematite inhibitors, wherein the addition amount is 115g/t, the dosage ratio of HAPMA to ASPMA is 1:1, and stirring for 5 minutes;
(4) Adding 300g/t of a composite collector M (mixing sodium lignin sulfonate, sodium dodecyl sulfonate, dodecyl dimethyl hydroxyethyl ammonium chloride and ethylene glycol according to the mass ratio of 1:2:2:2), and stirring for 4 min; adding 50g/t of turpentine as a foaming agent, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher separation; adding hematite inhibitor (HAPMA: ASPMA molar ratio is 1:1.2) into the roughed product, performing reverse flotation and concentration by using a composite collector M (the dosage is 350 g/t), and collecting the concentrated product.
The example gives a hematite concentrate TFe wt 65.13%, recovery 90.68% and SiO 2 wt 1.97%.
Comparative example 2
Hematite samples were from Hebei certain iron ore, where TFe wt 48.23%, siO 2 wt 15.52%. The method comprises the following steps:
(1) Crushing hematite ore, grinding until the particle size is-0.074 mm, wherein the proportion is more than or equal to 70%;
(2) Adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to 35%;
(3) Feeding the mixture into a flotation tank, regulating the pH value of flotation pulp to be 10 by using sodium carbonate, adding starch as a hematite inhibitor, adding 600g/t, and stirring for 5 minutes;
(4) Weighing 20 parts of hydroxy oleic acid, 40 parts of sulfonated oleic acid and 20 parts of tall oil, mixing the three fatty acids at room temperature, stirring for 15-30min, adding 10 parts of foaming agent turpentine, and continuously stirring for 15min to obtain a uniform solution. Dissolving 16 parts of sodium hydroxide into 100 parts of water, slowly adding the solution into the solution, uniformly stirring the solution at 35 ℃ to fully saponify the solution to obtain a hematite reverse flotation desilication collector M2, adding the M2 into ore pulp according to 650g/t, and stirring the solution for 4min; adding quartz activator calcium oxide with the dosage of 500g/t, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher; and adding starch (the dosage is 650 g/t) into the roughing product, carrying out reverse flotation and concentration on the roughing product by using a composite collector M2 (the dosage is 800 g/t), and collecting the concentration product.
The example gives a hematite concentrate TFe wt 58.83%, recovery 82.73%, siO 2 wt 3.28%.
Examples
An inverse flotation process of hematite, the beneficiation process flow adopted in the embodiment is shown in figure 1;
Some hematite sample comes from some foreign iron ore, of which TFe wt 50.18%, siO 2 wt 15.31%.
The method is realized by the following steps:
(1) Crushing hematite ore, grinding until the particle size is-0.074 mm, wherein the proportion is more than or equal to 70%;
(2) Adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to be 32%;
(3) Sending the mixture into a flotation tank, regulating the pH value of flotation pulp to be 10 by using sodium carbonate, adding HAPMA and ASPMA as hematite inhibitors, wherein the addition amount is 110g/t, the dosage ratio of HAPMA to ASPMA is 1:1, and stirring for 5 minutes;
(4) Adding 300g/t of a composite collector M (mixing sodium lignin sulfonate, sodium dodecyl sulfonate, dodecyl dimethyl hydroxyethyl ammonium chloride and ethylene glycol according to the mass ratio of 1:2:2:2), and stirring for 4 min; adding 50g/t of turpentine as a foaming agent, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher separation; adding hematite inhibitor (HAPMA: ASPMA molar ratio is 1:1.2) into the roughed product, performing reverse flotation and concentration by using a composite collector M (320 g/t), and collecting the concentrated product.
The example gives a hematite concentrate TFe wt 65.85%, recovery 90.86% and SiO 2 wt 1.87%.
Comparative example 3
Hematite samples were from foreign iron ores, of which TFe wt 50.18%, siO 2 wt 15.31%. The method comprises the following steps:
(1) Crushing hematite ore, grinding until the particle size is-0.074 mm, wherein the proportion is more than or equal to 70%;
(2) Adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to be 32%;
(3) Feeding the mixture into a flotation tank, regulating the pH value of flotation pulp to be 10 by using sodium carbonate, adding starch as a hematite inhibitor, adding 600g/t, and stirring for 5 minutes;
(4) Weighing 20 parts of hydroxy oleic acid, 40 parts of sulfonated oleic acid and 20 parts of tall oil, mixing the three fatty acids at room temperature, stirring for 15-30min, adding 10 parts of foaming agent turpentine, and continuously stirring for 15min to obtain a uniform solution. Dissolving 16 parts of sodium hydroxide into 100 parts of water, slowly adding the solution into the solution, uniformly stirring the solution at 35 ℃ to fully saponify the solution to obtain a hematite reverse flotation desilication collector M2, adding the M2 into ore pulp according to 660g/t, and stirring the solution for 4min; adding quartz activator calcium oxide with the dosage of 500g/t, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher; and adding starch (the dosage is 650 g/t) into the roughing product, carrying out reverse flotation and concentration on the roughing product by using a composite collector M2 (the dosage is 800 g/t), and collecting the concentration product.
The example obtained hematite concentrate TFe wt 60.46%, recovery 83.29%, siO 2 wt 2.98%.
Examples
An inverse flotation process of hematite, the beneficiation process flow adopted in the embodiment is shown in figure 1;
The method specifically comprises the following steps:
step one: crushing hematite ore according to the requirement, and grinding until the proportion of the granularity of-0.074 mm is more than or equal to 70%;
In the hematite ore, TFe is more than or equal to 45 wt percent, and SiO 2 is more than or equal to 15 wt percent;
Step two: adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to be 30% -35%;
Step three: feeding the mixture into a flotation tank, regulating the pH value of flotation pulp to 9-10 by using sodium carbonate or sodium hydroxide, adding hydroxamated polymaleic acid (HAPMA) and 4-hydroxy-3-carboxyl-maleanilide (ASPMA) as hematite inhibitors, and stirring for 5 minutes;
the method for synthesizing the hydroxamated polymaleic acid comprises the following steps:
at 85-90 ℃, the maleic anhydride is polymerized in toluene solution by Benzoyl Peroxide (BPO) to prepare polymaleic anhydride (PMA), and the molecular weight of the polymaleic anhydride is about 1000;
Dissolving hydroxylamine hydrochloride with the anhydride bond molar ratio of 30% in the polymaleic anhydride in a methanol solution at 20-30 ℃, adding sodium hydroxide with the same molar amount to release hydroxylamine, then dripping filtrate into the methanol solution of the polymaleic anhydride, reacting for 3 hours at room temperature, and drying the product after the reaction is completed to obtain the hydroxamated polymaleic acid;
The synthesis method of the 4-hydroxy-3-carboxyl-maleanilide comprises the following steps:
at 85-90 ℃, the maleic anhydride is polymerized in toluene solution by benzoyl peroxide to prepare polymaleic anhydride, and the molecular weight of the polymaleic anhydride is about 1200;
Dissolving para-aminosalicylic acid and polymaleic anhydride with the anhydride bond molar ratio of 10% in polymaleic anhydride in Tetrahydrofuran (THF) at 20-30 ℃ for 3h at room temperature, and drying the product after the reaction is finished to obtain 4-hydroxy-3-carboxyl-maleanilide;
Step four: adding a composite collector M and a foaming agent into ore pulp for primary reverse flotation roughing and primary reverse flotation concentration to obtain hematite concentrate and concentration tailings;
the adding amount of the hematite inhibitor in the third step is 100-150 g/t, and the dosage ratio of the hydroxamated polymaleic acid to the 4-hydroxy-3-carboxyl-maleanilide is 1:1-1:2 (molar ratio) based on the total amount of the ore pulp;
the composite collector M is prepared by mixing sodium lignin sulfonate, sodium dodecyl sulfonate, dodecyl dimethyl hydroxyethyl ammonium chloride and ethylene glycol according to a mass ratio of 1:2:2:2;
The reverse flotation comprises the following specific operation steps:
adding a composite collector M into the ore pulp and stirring for 4min;
adding 50g/t of turpentine as a foaming agent, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher separation;
Adding hematite inhibitor hydroxamated polymaleic acid and 4-hydroxy-3-carboxyl-maleic anilide into the roughing product for reverse flotation and selection with a composite collector M, and collecting the selected product;
In the reverse flotation roughing process, the adding amount of the composite collector M is 300-400 g/t based on the total amount of ore pulp;
the adding amount of the hematite inhibitor is 150-180 g/t and the adding amount of the composite collector M is 350-350 g/t based on the total amount of the primary selected products, and the method is not particularly limited.
In summary, the novel hematite inhibitors HAPMA and ASPMA adopted by the invention can be adsorbed on the surface of the hematite, have stronger inhibition capacity and selectivity than starch, have better water solubility than starch and lower molecular weight than starch, and can effectively improve the efficiency of the subsequent filtering process; and moreover, the reverse flotation desilication process is simple in flow, convenient to operate, low in beneficiation cost, good in industrial feasibility and convenient for large-scale popularization.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A process for reverse flotation of hematite, comprising the steps of:
step one: crushing hematite ore according to the requirement, and grinding until the proportion of the granularity of-0.074 mm is more than or equal to 70%;
Step two: adding water into hematite powder to prepare ore pulp, and regulating the concentration of the ore pulp to be 30% -35%;
Step three: feeding the ore pulp into a flotation tank, regulating the pH value of the ore pulp to 9-10 by using sodium carbonate or sodium hydroxide, adding hydroxamated polymaleic acid and 4-hydroxy-3-carboxyl-maleic anilide as hematite inhibitors, stirring for 5 minutes, wherein the adding amount of the hematite inhibitors is 100-150 g/t based on the total amount of the ore pulp, and the using amount ratio of the hydroxamated polymaleic acid to the 4-hydroxy-3-carboxyl-maleic anilide is 1:1-1:2;
step four: adding a composite collector M and a foaming agent into ore pulp for primary reverse flotation roughing and primary reverse flotation concentration to obtain hematite concentrate and concentration tailings; the composite collector M is prepared by mixing sodium lignin sulfonate, sodium dodecyl sulfonate, dodecyl dimethyl hydroxyethyl ammonium chloride and ethylene glycol according to a mass ratio of 1:2:2:2.
2. The reverse flotation process of hematite according to claim 1, wherein TFe is not less than 45% by weight and SiO 2 is not less than 15% by weight of the hematite ore.
3. The reverse flotation process of hematite according to claim 1, wherein the method for synthesizing the hydroxamated polymaleic acid in the step three is as follows:
at 85-90 ℃, the maleic anhydride is polymerized in toluene solution by benzoyl peroxide to prepare polymaleic anhydride with the molecular weight of about 1000;
at 20-30 ℃, hydroxylamine hydrochloride with the anhydride bond mole ratio of 30% in the polymaleic anhydride is dissolved in methanol solution, and sodium hydroxide with the same mole amount is added to release hydroxylamine, then filtrate is dripped into the methanol solution of polymaleic anhydride to react for 3 hours at room temperature, and after the reaction is completed, the product is dried, so that the hydroxamated polymaleic acid is obtained.
4. The reverse flotation process of hematite according to claim 1, wherein the synthesis method of 4-hydroxy-3-carboxyl-maleanilide in the third step comprises the following steps:
At 85-90 ℃, the maleic anhydride is polymerized in toluene solution by benzoyl peroxide to prepare polymaleic anhydride with the molecular weight of about 1200;
Dissolving para-aminosalicylic acid and polymaleic anhydride with the anhydride bond mole ratio of 10% in polymaleic anhydride in tetrahydrofuran at 20-30 ℃ for reaction for 3 hours at room temperature, and drying the product after the reaction is finished to obtain 4-hydroxy-3-carboxyl-maleanilide.
5. The process according to claim 1, wherein in the fourth step, the composite collector M and the foaming agent are added into the ore pulp to perform primary reverse flotation roughing and primary reverse flotation concentration, and the process comprises the following steps:
adding a composite collector M into the ore pulp and stirring for 4min;
adding 50g/t of turpentine as a foaming agent, stirring for 2min, aerating for flotation for 4min, and performing reverse flotation rougher separation;
and adding hematite inhibitor hydroxamated polymaleic acid and 4-hydroxy-3-carboxyl-maleic anilide into the roughing product for reverse flotation and concentration with a composite collector M, and collecting the concentration product.
6. The reverse flotation process of hematite according to claim 5, wherein the adding amount of the composite collector M is 300-400 g/t based on the total amount of ore pulp in the reverse flotation roughing process;
The addition amount of the hematite inhibitor is 150-180 g/t and the addition amount of the composite collector M is 350-350 g/t based on the total amount of the primary selected products.
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