Collecting agent for removing iron and aluminum through phosphorite activation flotation and application method of collecting agent

Abstract

The invention relates to the technical field of collophanite beneficiation, and discloses a collecting agent for phosphorite activation flotation to remove iron and aluminum and an application method of the collecting agent. The collecting agent is good in solubility, high in selectivity and small in dosage, the collecting agent contains a phosphate group and a long hydrophobic carbon chain, the phosphate group can be combined with free calcium and magnesium ions in ore pulp under the neutral condition to exist in the form of magnesium hydroxide, interacts with limonite and bauxite and is adsorbed on the surface of minerals, and therefore the collecting agent can be recycled. Therefore, the floatable collecting agent for increasing the minerals has high collecting capacity on activated fine-fraction gangue minerals containing iron and aluminum and can be applied to the phosphorite flotation process, and separation of phosphate concentrate, bauxite and limonite is achieved.

Description

Technical Field

[0001] The invention relates to the technical field of collophanite beneficiation, and in particular to a collector for de-ironization and de-aluminization of phosphate ore by activation flotation and an application method thereof. Background Art

[0002] As a non-renewable resource, phosphate rock is an important component of agricultural fertilizers and phosphorus-based chemicals. The siliceous gangue minerals in phosphate rock are mainly quartz and aluminate minerals, limonite, etc. The iron oxide and aluminum oxide in phosphate rock are usually called sesquioxides, often expressed as R 2 O 3 express.

[0003] When the solution contains high levels of iron and aluminum, sludge will be formed during the wet phosphoric acid process, which will increase the density and viscosity of the acid, making it difficult to concentrate phosphoric acid and reducing the effective utilization rate of phosphoric acid and product quality. With the depletion of high-quality phosphate ore resources, a large amount of medium- and low-grade phosphate ore is needed, and the content of magnesium, silicon, sesquioxides and other impurities in medium- and low-grade phosphate ore is significantly higher than that in rich ore.

[0004] Simply removing magnesium gangue minerals is no longer enough to meet the needs of phosphorus chemical production, especially the production of high-quality calcium phosphates has stricter requirements on the content of iron and aluminum minerals in the raw materials. Therefore, it is necessary to develop agents with strong selectivity and capture ability for iron and aluminum minerals in phosphate ore and corresponding application methods to reduce the content of iron and aluminum minerals in phosphate concentrate, which is of great significance to the application of phosphate ore. Summary of the invention

[0005] The object of the present invention is to provide a collector for removing iron and aluminum from phosphate ore by activated flotation and an application method thereof.

[0006] The scheme of the present invention is:

[0007] A collector for activated flotation of phosphate ore to remove iron and aluminum, the collector being a phosphate collector; the phosphate collector being one or more of isomeric tridecanol polyoxyethylene ether phosphatidic acid, isooctyl alcohol polyoxyethylene ether sodium phosphate, fatty alcohol polyoxyethylene ether phosphate, octyl alcohol polyoxyethylene ether potassium phosphate, dodecyl polyoxyethylene ether potassium phosphate and lauryl alcohol potassium phosphate.

[0008] The invention also discloses a collector for activated flotation and de-ironization of phosphate ore, which is used for flotation separation of phosphate ore, bauxite and limonite.

[0009] The present invention also discloses a collector application method for activated flotation of phosphate ore to remove iron and aluminum, comprising the following steps:

[0010] S1. After crushing and grinding the ore, a slurry with a concentration of 20-25% is obtained;

[0011] S2. Add Na to the slurry2 CO 3 Adjust the pH value of the slurry to 6-8, then add alkali metal ion solution to activate the iron and aluminum minerals, and then add phosphate collectors and synergists in sequence and stir them separately;

[0012] S3. Turn on the flotation machine to inflate and start flotation to obtain foam products and de-ironized aluminum-phosphate concentrate.

[0013] As a preferred technical solution, the pH value in S2 is 7.

[0014] As a preferred technical solution, the amount of collector in S2 is 30-60 g / t.

[0015] As a preferred technical solution, the synergist is tributyl phosphate, and its amount is 100-200 g / t.

[0016] As a preferred technical solution, the alkali metal ion solution in S2 is MgCl with a concentration of 5%. 2 Aqueous solution or 5% lime milk aqueous solution.

[0017] As a preferred technical solution, the method further includes step S4, adding an alkali metal ion solution to the de-iron aluminum phosphate concentrate to perform secondary activation on the mineral, and then sequentially adding a phosphate collector and a synergist, stirring them separately, and then performing secondary aeration flotation. Repeating the activation and flotation steps can enhance the effect of activation separation.

[0018] Advantages of the present invention:

[0019] The collector of the present invention has good solubility, strong selectivity and small dosage. The collector contains a phosphate group and a long hydrophobic carbon chain. The phosphate group can be combined with free calcium and magnesium ions in the ore pulp under neutral conditions to exist in the form of hydroxy magnesium, and interact with limonite and bauxite, and adsorb on the mineral surface, thereby increasing the floatability of the mineral. The collector has a strong collection ability for activated fine-grained iron-aluminum gangue minerals, and can be applied to the phosphate ore flotation process to achieve the separation of phosphate concentrate from bauxite and limonite. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 This is a process flow chart of Example 1 of the present invention;

[0021] Figure 2 This is a process flow chart of Example 3 of the present invention. DETAILED DESCRIPTION

[0022] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further described below in conjunction with specific embodiments.

[0023] Example 1

[0024] (1) For P 2 O 5 Content 28.74%, MgO content 0.59%, sesquioxide (Fe 2 O 3 +Al 2 O 3 ) Collophanite with a content of 2.45%, the ore is crushed and ground to obtain a pulp with a fineness of -0.074mm, a content of 87%, and a concentration of 20%;

[0025] (2) Pour the slurry into a 0.5L single-tank flotation machine, adjust the stirring speed to 1900r / min, and add Na 2 CO 3 Adjust the pH of the slurry to 7, and then add 2kg / t of 5% MgCl 2 The alkali metal ion solution is used to activate the iron and aluminum minerals, and then 50 g / t of phosphate collector isotridecyl alcohol polyoxyethylene ether phosphatidic acid and 150 g / t of synergist tributyl phosphate are added in sequence, and stirred for 1 min respectively to fully disperse the slurry and fully combine the reagent with the slurry;

[0026] (3) Turn on the flotation machine to inflate and start flotation to obtain foam products and iron-free aluminum-phosphate concentrate. Filter, dry and weigh the foam products and tailings respectively, and test the phosphorus, magnesium, iron and aluminum content in the concentrate and tailings to calculate the product yield, recovery rate and MER value. MER value = w(Fe 2 O 3 +Al 2 O 3 +MgO) / w(P 2 O 5 ).

[0027] When the dosage of alkali metal ions is 2kg / t, P can be obtained after flotation using alkali metal ions as activating agents. 2 O 5 Phosphate concentrate with a content of 28.63%, a MgO content of 0.64%, and a MER value of 0.087. In addition, there is a difference in the distribution of iron and aluminum minerals in the concentrate and tailings, and the content of iron and aluminum in the concentrate is lower than that in the tailings.

[0028] Example 2

[0029] (1) For P 2 O 5 Content 28.96%, MgO content 0.9%, sesquioxide (Fe 2 O 3 +Al 2 O 3) Collophanite with a content of 2.65%, the ore is crushed and ground to obtain a slurry with a fineness of -0.074mm, a content of 87%, and a concentration of 20%;

[0030] (2) Pour the slurry into a 0.5L single-tank flotation machine, adjust the stirring speed to 1900r / min, and add Na 2 CO 3 Adjust the slurry pH to 7, then add 2kg / t of 5% MgCl 2 The aqueous solution is used to activate the iron and aluminum minerals, and then different types of phosphate collectors 50g / t and synergist tributyl phosphate 150g / t are added respectively, and stirred for 1min respectively to fully disperse the slurry and fully combine the reagents with the slurry;

[0031] Phosphate collectors include E1310P (isomeric tridecanol polyoxyethylene ether phosphatidic acid), OEP-70 (sodium isooctyl polyoxyethylene ether phosphate), AEO-3p (fatty alcohol polyoxyethylene ether phosphate), ODEP-K (potassium octyl polyoxyethylene ether phosphate), MAEP-K (potassium dodecyl polyoxyethylene ether phosphate), and MAP-k (potassium lauryl phosphate).

[0032] (3) Turn on the flotation machine to inflate and start flotation to obtain foam products and iron-free aluminum-phosphate concentrate. Filter, dry and weigh the foam products and tailings respectively, and test the phosphorus, magnesium, iron and aluminum content in the concentrate and tailings to calculate the product yield, recovery rate and MER value. MER value = w(Fe 2 O 3 +Al 2 O 3 +MgO) / w(P 2 O 5 ).

[0033] Experimental studies have shown that, using activated flotation, under the condition of the same reagent dosage, the concentrate recovery rate of E1310P is 69.47%, the grade is 31.48%, and the MER value is 0.071; the concentrate recovery rate of AEO-3p is 50.13%, the grade is 31.78%, and the MER value is 0.104; the concentrate recovery rate of ODEP-k is 51.19%, the grade is 31.48%, and the MER value is 0.071; the concentrate recovery rate of MAEP-K is 47.23%, the grade is 30.75%, and the MER value is 0.112; the concentrate recovery rate of MAP-k is 48.15%, the grade is 30.65%, and the MER value is 0.117; the concentrate recovery rate of OEP-70 is 45.15%, the grade is 29.85%, and the MER value is 0.121. Under the same reagent dosage conditions, the flotation effect of E1310P is better than other reagents. It has a stronger collection ability for iron and aluminum minerals, and is better in removing iron and aluminum and reducing MER values.

[0034] Example 3

[0035] (1) For P 2 O 5 The content is 27.55%, MgO content is 1.03%, sesquioxide (Fe 2 O 3 +Al 2 O 3 ) Collophanite with a content of 2.65%, after crushing and grinding, the ore is obtained into a pulp with a fineness of -0.074mm, a content of 88%, and a concentration of 20%;

[0036] (2) Pour the slurry into a 0.5L single-tank flotation machine and adjust the stirring speed to 1900r / min. 2 CO 3 Adjust the pH of the slurry to 7 and add 1.4 kg / t of 5% MgCl for the first time. 2 After the alkali metal ion solution is activated, 50 g / t of isomeric tridecanol polyoxyethylene ether phosphatidic acid and 150 g / t of synergist tributyl phosphate are added, and after sufficient mixing and slurry preparation, the fine-grained iron-aluminum gangue minerals in the phosphate concentrate are removed by flotation to obtain P 2 O 5 De-iron aluminum phosphate concentrate 1 and P with a content of 28.04% 2 O 5 Activated reverse flotation tailings 1 with a content of 25.27%.

[0037] 1.4 kg / t of 5% MgCl was added to the slurry of the de-ironized aluminum phosphate concentrate 1. 2 After alkali metal ion solution is activated, 30 g / t of collector isomeric tridecanol polyoxyethylene ether phosphatidic acid and 150 g / t of synergist tributyl phosphate are fully mixed and slurried, and P is obtained by flotation. 2 O 5 De-iron aluminum phosphate concentrate 2 and P with a content of 29.73% 2 O 5 Activated reverse flotation tailings 2 with a content of 28.72%.

[0038] De-iron aluminum phosphate concentrate 2P 2 O 5 The content is 29.73%, the MgO content is 1.61%, and the sesquioxide content is 1.49%.

[0039] Example 4

[0040] (1) For P 2 O 5 The content is 28.25%, MgO content is 0.93%, sesquioxide (Fe 2 O3 +Al 2 O 3 ) Collophanite with a content of 2.45%, after crushing and grinding, the ore is obtained into a pulp with a fineness of -0.074mm, a content of 87%, and a concentration of 21%;

[0041] (2) Pour the slurry into a 0.5L single-tank flotation machine and adjust the stirring speed to 1900r / min. 2 CO 3 Adjust the pH of the slurry to 7, add 1.4kg / t of 5% lime milk aqueous solution for activation, add 50g / t of E1310P:AEO-3P compounded at a mass ratio of 1:1 and 150g / t of tributyl phosphate synergist, mix well and adjust the slurry, and then flotate to remove the fine-grained iron-aluminum gangue minerals in the phosphate concentrate to obtain P 2 O 5 De-iron aluminum phosphate concentrate 1 and P with a content of 29.14% 2 O 5 Activated reverse flotation tailings 1 with a content of 25.77%.

[0042] 1.4 kg / t of 5% lime milk aqueous solution (CaO) was added to the pulp of the de-iron aluminum phosphate concentrate 1 for activation, and 30 g / t of collector and 150 g / t of synergist LSD-Z, which were compounded in a mass ratio of 1:1, were added. After fully mixing and slurrying, P was obtained by flotation. 2 O 5 De-iron aluminum phosphate concentrate 2 and P with a content of 30.23% 2 O 5 Activated reverse flotation tailings 2 with a content of 28.53%.

[0043] De-iron aluminum phosphate concentrate 2P 2 O 5 The content is 30.23%, the MgO content is 1.01%, and the sesquioxide content is 1.59%.

[0044] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.

Claims

1. A collector for de-ironization and de-aluminization of phosphate ore, characterized in that: The collector is a phosphate collector, and the phosphate collector is one or more of isomeric tridecyl alcohol polyoxyethylene ether phosphatidic acid, isooctyl alcohol polyoxyethylene ether sodium phosphate, fatty alcohol polyoxyethylene ether phosphate, octyl alcohol polyoxyethylene ether potassium phosphate, dodecyl polyoxyethylene ether potassium phosphate and lauryl alcohol potassium phosphate.

2. The collector for de-ironization and de-aluminization of phosphate ore according to claim 1, characterized in that: The collector is used for flotation separation of bauxite and limonite in phosphate ore.

3. A method for using a collector for de-ironization and de-aluminization of phosphate ore as claimed in claim 1, characterized in that: The following steps are involved: S1. After crushing and grinding the ore, a slurry with a concentration of 20-25% is obtained; S2. Add Na2CO3 to the slurry to adjust the pH value of the slurry to 6-8, then add alkali metal ion solution to activate the mineral, and then add phosphate collector and synergist in sequence, and stir them separately; S3. Turn on the flotation machine to inflate and start flotation to obtain foam products and de-ironized aluminum-phosphate concentrate.

4. The method for using a collector for de-ironization and aluminum removal from phosphate ore according to claim 3, characterized in that: The pH value of S2 is 7.

5. The method for using a collector for de-ironization and aluminum removal in activated flotation of phosphate ore as claimed in claim 3, characterized in that: The amount of collector in S2 is 30-60 g / t.

6. The method for using a collector for de-ironization and aluminum removal from phosphate ore according to claim 3, characterized in that: The synergist is tributyl phosphate, and the amount thereof is 100-200 g / t.

7. The method for using a collector for de-ironization and aluminum removal from phosphate ore according to claim 3, characterized in that: The method further comprises step S4, wherein an alkali metal ion solution is added to the de-iron aluminum phosphate concentrate to perform secondary activation on the mineral, and then a phosphate collector and a synergist are added in sequence, and after stirring, secondary aeration flotation is performed.

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