Method for increasing the rare earth grade of minerals containing cerium phosphate and xenotime

Abstract

The present invention discloses a method for improving the rare earth grade of minerals containing ceriumite and xenotime, comprising the following steps: 1) crushing and grinding the minerals containing ceriumite and xenotime to obtain a grinding product; 2) roughing the grinding product to obtain a rougher concentrate and a rougher tailing; 3) subjecting the rougher concentrate to tertiary concentrating to obtain a tertiary concentrating concentrate and a tertiary concentrating tailing; 4) subjecting the rougher tailing to two scavenging steps to obtain a secondary scavenging concentrate and a secondary scavenging tailing; 5) combining the obtained tertiary concentrating tailing and the secondary scavenging concentrate, grinding, and obtaining a regrinded middling product; subjecting the regrinded middling product to one roughing step and two scavenging steps to obtain a middling regrinding flotation concentrate and a secondary middling concentrating tailing; and 6) combining the obtained tertiary concentrating concentrate and the middling regrinding flotation concentrate to obtain a rare earth concentrate. The present invention can improve the rare earth grade of minerals containing ceriumite and xenotime.

Description

Technical Field

[0001] The present invention relates to a method for improving the rare earth grade of minerals containing cerium phosphate and xenotime. Background Art

[0002] Rare earth elements include the fifteen lanthanides, scandium, and yttrium. Rare earth elements are concentrated in specific accessory minerals associated with the ore. Some minerals that may contain rare earth elements are apatite, bastnaesite, monazite, and xenotime. Bastnaesite is a lanthanide carbonate. Monazite, apatite, and xenotime are phosphates. Xenotime and several lesser-known rare earth-containing minerals are hydrated aluminum phosphates. The methods used to separate rare earth element-containing minerals from ore deposits are specific to each mineral.

[0003] CN110813541A discloses a collector combination for flotation of monazite and xenotime from fine-grained seaside sand ore. The flotation process is the key to solving the flotation separation of monazite and xenotime from gangue in fine-grained seaside sand ore. This patent document provides a collector combination that can be used for flotation of monazite and xenotime from fine-grained seaside sand ore, with high selectivity, which can effectively improve the recovery rate of valuable minerals.

[0004] CN104874474A discloses a beneficiation method for xenotime ore, comprising the following steps: obtaining raw ore pulp; subjecting the raw ore pulp to weak magnetic separation to remove mechanical iron to obtain coarse ore pulp; subjecting the coarse ore pulp to strong magnetic separation to obtain primary xenotime ore concentrate and primary xenotime ore tailings; subjecting the primary xenotime ore tailings to scavenging to obtain secondary xenotime ore concentrate and secondary xenotime ore tailings; and subjecting the secondary xenotime ore tailings to secondary scavenging to obtain tertiary xenotime ore concentrate and tertiary xenotime ore tailings.

[0005] CN108034964A discloses a process for separating and extracting yttrium phosphate from rare earth ores. The process includes the following steps: ore dressing: grinding the raw ore, weak magnetic separation of tailings, strong magnetic separation of concentrate slurry, flotation of the concentrated slurry, and strong magnetic separation of the flotation concentrate to obtain a high-grade rare earth concentrate. The patent also requires extraction and electrolysis to extract high-purity yttrium phosphate.

[0006] So far, there has been no report on a method for increasing the rare earth grade of minerals containing cerium phosphate and xenotime. Summary of the Invention

[0007] In view of this, an object of the present invention is to provide a method for improving the rare earth grade of minerals containing cerium phosphate and xenotime, which can improve the rare earth grade of minerals containing cerium phosphate and xenotime.

[0008] The present invention adopts the following technical solutions to achieve the above-mentioned purpose.

[0009] The present invention provides a method for improving the rare earth grade of a mineral containing cerium phosphate and xenotime, comprising the following steps:

[0010] 1) crushing the mineral containing cerium phosphate and xenotime to obtain a crushed product; grinding the crushed product to obtain a grinding product;

[0011] 2) Adding 0.5-0.8 kg / t of basic carbonate, 0.8-1.2 kg / t of water glass, 2.0-3.0 kg / t of LF-P80, and 150-240 g / t of pine oil to the slurry of the grinding product in sequence, and performing aeration flotation to obtain a roughing concentrate and a roughing tailing; wherein the amount of each material is calculated based on 1 ton of the grinding product;

[0012] 3) adding 0.2-0.4 kg / t of water glass, 0.4-0.6 kg / t of LF-P80 and 30-60 g / t of pine oil to the pulp of the rougher concentrate, and performing aeration flotation to obtain a primary concentrated concentrate and a primary concentrated tailings; adding 40-70 g / t of water glass, 100-150 g / t of LF-P80 and 30-60 g / t of pine oil to the pulp of the primary concentrated concentrate, and performing aeration flotation to obtain a secondary concentrated concentrate and a secondary concentrated tailings; and adding 50-80 g / t of LF-P80 and 40-60 g / t of pine oil to the pulp of the secondary concentrated concentrate, and performing aeration flotation to obtain a tertiary concentrated concentrate and a tertiary concentrated tailings; wherein the amount of each material is calculated based on 1 ton of grinding product;

[0013] 4) adding 40-60 g / t of water glass, 100-300 g / t of LF-P80 and 40-60 g / t of pine oil to the pulp of the rougher tailings, and performing aeration flotation to obtain a primary scavenging concentrate and a primary scavenging tailings; adding 80-120 g / t of LF-P80 and 40-60 g / t of pine oil to the pulp of the primary scavenging concentrate, and performing aeration flotation to obtain a secondary scavenging concentrate and a secondary scavenging tailings; wherein the amount of each material is calculated based on 1 ton of grinding product;

[0014] 5) The obtained tertiary concentrator tailings and secondary scavenging concentrate are combined and ground to obtain a reground middling product; 0.3-0.6 kg / t of basic carbonate, 0.5-0.7 kg / t of water glass, 1.0-1.5 kg / t of LF-P80 and 130-180 g / t of pine oil are sequentially added to the slurry of the reground middling product, and aeration flotation is performed to obtain a middling rougher concentrate and a middling rougher tailing; 0.2-0.4 kg / t of water glass are sequentially added to the slurry of the middling rougher concentrate; water glass, 0.4-0.7 kg / t LF-P80 and 30-60 g / t pine oil, and aeration flotation to obtain a primary middling concentrate and a primary middling tailings; 20-40 g / t water glass, 0.1-0.3 kg / t LF-P80 and 30-60 g / t pine oil are sequentially added to the slurry of the primary middling concentrate, and aeration flotation is performed to obtain a middling regrinding flotation concentrate and a secondary middling tailings; wherein the amount of each material is calculated based on 1 ton of grinding product;

[0015] 6) The obtained tertiary concentrated ore and the middling regrinding flotation concentrate are combined to obtain the rare earth concentrate.

[0016] According to the method of the present invention, preferably, in step 1), the REO grade of the mineral containing ceriumite and xenotime is 2-13 wt%, and the mass ratio of ceriumite to xenotime is 1:3.1-7.5.

[0017] According to the method of the present invention, preferably, in step 1), the mineral raw material containing cerium phosphate and xenotime also contains gangue minerals, and the gangue minerals are mainly quartz and illite.

[0018] According to the method of the present invention, preferably, in step 1), the particle size of the crushed product is below 2.0 mm; the grinding concentration is 50-65 wt %, and the grinding fineness is -240 mesh, accounting for 85-90%.

[0019] According to the method of the present invention, preferably, in step 2), after adding basic carbonate to the ore pulp of the grinding product, stirring is carried out for 1 to 5 minutes, after adding water glass, stirring is carried out for 2 to 5 minutes, after adding LF-P80, stirring is carried out for 2 to 7 minutes, and after adding pine oil, stirring is carried out for 1 to 5 minutes; the operating temperature of the aeration flotation is 35 to 40°C.

[0020] According to the method of the present invention, preferably, in step 3), after adding water glass to the pulp of the roughing concentrate, stirring is carried out for 2 to 5 minutes; after adding LF-P80, stirring is carried out for 2 to 5 minutes; after adding pine oil, stirring is carried out for 1 to 2 minutes; after adding water glass to the pulp of the primary concentrated concentrate, stirring is carried out for 2 to 4 minutes, after adding LF-P80, stirring is carried out for 2 to 5 minutes, and after adding pine oil, stirring is carried out for 1 to 2 minutes; after adding LF-P80 to the pulp of the secondary concentrated concentrate, stirring is carried out for 2 to 4 minutes, and after adding pine oil, stirring is carried out for 1 to 2 minutes; the operating temperature of the aeration flotation is 35 to 40°C.

[0021] According to the method of the present invention, preferably, in step 4), after adding water glass to the pulp of the rougher tailings, stirring is carried out for 2 to 4 minutes; after adding LF-P80, stirring is carried out for 2 to 5 minutes; after adding pine oil, stirring is carried out for 1 to 2 minutes; after adding LF-P80 to the pulp of the primary scavenging concentrate, stirring is carried out for 2 to 4 minutes, and after adding pine oil, stirring is carried out for 1 to 2 minutes; the operating temperature of the aeration flotation is 35 to 40°C.

[0022] According to the method of the present invention, preferably, in step 5), the grinding concentration is 55-70 wt%, and the grinding fineness is -0.045 mm, accounting for 85-90%.

[0023] According to the method of the present invention, preferably, in step 5), after adding basic carbonate to the reground middlings, stirring is performed for 2 to 4 minutes, after adding water glass, stirring is performed for 2 to 3 minutes, after adding LF-P80, stirring is performed for 2 to 4 minutes, and after adding pine oil, stirring is performed for 1 to 2 minutes; after adding water glass to the pulp of the middling rougher concentrate, stirring is performed for 2 to 3 minutes, after adding LF-P80, stirring is performed for 2 to 4 minutes, and after adding pine oil, stirring is performed for 1 to 2 minutes; after adding water glass to the pulp of the primary middling concentrate, stirring is performed for 2 to 4 minutes, after adding LF-P80, stirring is performed for 2 to 4 minutes, and after adding pine oil, stirring is performed for 1 to 2 minutes; the operating temperature of the aeration flotation is 35 to 45°C; wherein, the basic carbonate is sodium carbonate or potassium carbonate.

[0024] According to the method of the present invention, preferably, in the rare earth concentrate, the REO grade is greater than 45wt%, the REO recovery rate is greater than 85%, the content of xenotime is 60-70wt%, and the content of cerium aluminum phosphate is 10-15.5wt%.

[0025] The method of the present invention utilizes a specific process flow to increase the rare earth grade of ore containing both ceriumite and xenotime. Preferably, the method of the present invention, through a process flow of crushing and grinding, preferential flotation, and regrinding and reselection of the middlings, increases the rare earth grade of the resulting rare earth concentrate by more than six times, preferably more than seven times, and more preferably more than eight times. DETAILED DESCRIPTION

[0026] The present invention will be further described below in conjunction with specific embodiments, but the protection scope of the present invention is not limited thereto.

[0027] The present invention provides a method for improving the rare earth grade of a mineral containing cerium phosphate and xenotime, comprising: (1) a crushing and grinding step; (2) a roughing step; (3) a cleaning step of the roughing concentrate; (4) a scavenging step of the roughing tailings; (5) a middling treatment step; and (6) a merging step. Each step is described below.

[0028] Crushing and Grinding Steps

[0029] The minerals containing cerium phosphate and xenotime are crushed to obtain crushed products; and the crushed products are ground to obtain grinding products.

[0030] The minerals containing ceriumite and xenotime also contain gangue minerals in addition to ceriumite and xenotime, and the gangue minerals are mainly quartz and illite.

[0031] The rare earth grade (i.e., REO grade) of the mineral containing acerite and xenotime can be 2-13 wt%, preferably 3-10 wt%, more preferably 4-8.5 wt%, for example, 4.35 wt%, 5.34 wt%, 6.02 wt%, and 7.5 wt%. The mass ratio of acerite to xenotime can be 1:3.1-7.5, preferably 1:3.3-7.5, and more preferably 1:3.5-6.5.

[0032] In certain embodiments, the mineral containing cerium phosphate and xenotime is crushed to -10 mm using a jaw crusher, and is secondary crushed using a double-roll crusher and sieved using a sieving machine to obtain a crushed product with a particle size of less than 2.0 mm.

[0033] In certain embodiments, the crushed product is ground, the grinding concentration is 50-65%, and the grinding fineness is -240 mesh, accounting for 85-90%.

[0034] <Rough Selection Step>

[0035] Basic carbonate, water glass, LF-P80, and pine oil are sequentially added to the grinding product slurry, followed by aeration flotation to produce a rougher concentrate and rougher tailings. The amount of each material is calculated based on 1 ton of grinding product. This helps improve the rare earth grade of the resulting rare earth concentrate.

[0036] The basic carbonate can be sodium carbonate or potassium carbonate, preferably sodium carbonate. The amount of basic carbonate used can be 0.5-0.8 kg / t, preferably 0.55-0.75 kg / t, and more preferably 0.6-0.7 kg / t. The amount of water glass used can be 0.8-1.2 kg / t, preferably 0.9-1.1 kg / t, and more preferably 0.95-1.0 kg / t. The amount of LF-P80 used can be 2.0-3.0 kg / t, preferably 2.2-2.8 kg / t, and more preferably 2.5-2.8 kg / t. In the present invention, LF-P80 is a hydroxamic acid collector and can be purchased from Baotou Linfeng Technology Co., Ltd. The amount of pine oil used can be 150-240 g / t, preferably 160-220 g / t, and more preferably 180-210 g / t. The operating temperature of the aeration flotation can be 35-40°C.

[0037] In the present invention, after adding basic carbonate to the slurry of the grinding product, stirring is carried out for 1 to 5 minutes, preferably 1 to 3 minutes, more preferably 1 to 2 minutes; after adding water glass, stirring is carried out for 2 to 5 minutes, preferably 2 to 4 minutes, more preferably 2 to 3 minutes; after adding LF-P80, stirring is carried out for 2 to 7 minutes, preferably 2 to 5 minutes, more preferably 2 to 4 minutes; after adding pine oil, stirring is carried out for 1 to 5 minutes, preferably 1 to 3 minutes, more preferably 1 to 2 minutes.

[0038] <Benefiting Steps for Rougher Concentrate>

[0039] The rougher concentrate is further subjected to flotation, which is beneficial to improving the rare earth grade of the obtained rare earth concentrate.

[0040] In the present invention, the selection steps include the first selection, the second selection and the third selection, which are specifically described as follows:

[0041] First selection

[0042] Sodium silicate, LF-P80 and pine oil are sequentially added to the pulp of the rougher concentrate, and aeration flotation is performed to obtain primary concentrated concentrate and primary concentrated tailings.

[0043] After adding water glass to the rougher concentrate slurry, stir for 2-5 minutes, preferably 2-4 minutes, more preferably 2.5-3 minutes; after adding LF-P80, stir for 2-5 minutes, preferably 2.5-4 minutes, more preferably 2.5-3 minutes; after adding pine oil, stir for 1-2 minutes, preferably 1-1.5 minutes. The operating temperature of aeration flotation is 35-40°C, for example, 38°C.

[0044] Based on 1 ton of ground ore, the amount of water glass used can be 0.2-0.4 kg / t, preferably 0.25-0.35 kg / t, more preferably 0.28-0.35 kg / t, for example 0.3 kg / t. The amount of LF-P80 used can be 0.4-0.6 kg / t, preferably 0.45-0.55 kg / t, more preferably 0.5-0.55 kg / t. The amount of pine oil used can be 30-60 g / t, preferably 35-55 g / t, more preferably 40-50 g / t.

[0045] Second Selection

[0046] Water glass, LF-P80 and pine oil are sequentially added to the pulp of the primary concentrated ore, and aeration flotation is performed to obtain secondary concentrated ore and secondary concentrated tailings.

[0047] After adding water glass to the primary concentrate slurry, stir for 2-4 minutes, preferably 2.5-4 minutes, more preferably 2.5-3.5 minutes; after adding LF-P80, stir for 2-5 minutes, preferably 2.5-4.5 minutes, more preferably 2.5-4 minutes; after adding pine oil, stir for 1-2 minutes, preferably 1-1.5 minutes. The operating temperature of aeration flotation is 35-40°C.

[0048] Based on 1 ton of ground ore, the amount of water glass used can be 40-70 g / t, preferably 45-65 g / t, and more preferably 50-60 g / t. The amount of LF-P80 used can be 100-150 g / t, preferably 120-150 g / t, and more preferably 130-140 g / t. The amount of pine oil used can be 30-60 g / t, preferably 40-55 g / t, and more preferably 45-50 g / t.

[0049] The third selection

[0050] LF-P80 and pine oil are added to the pulp of the secondary concentrated ore in sequence, and aeration flotation is performed to obtain tertiary concentrated ore and tertiary concentrated tailings.

[0051] After adding LF-P80 to the secondary concentrate slurry, stir for 2 to 4 minutes, preferably 2.5 to 4 minutes, more preferably 2.5 to 3 minutes; after adding pine oil, stir for 1 to 2 minutes, preferably 1 to 1.5 minutes. The operating temperature of aeration flotation is 35 to 40°C.

[0052] Based on 1 ton of ground product, the amount of LF-P80 used can be 50-80 g / t, preferably 55-75 g / t, more preferably 60-70 g / t. The amount of pine oil used can be 40-60 g / t, preferably 45-60 g / t, more preferably 50-55 g / t.

[0053] <Scavenging steps for rougher tailings>

[0054] The sweeping step of the present invention includes a first sweeping step and a second sweeping step, which is beneficial to improving the recovery rate.

[0055] First scan

[0056] Sodium silicate, LF-P80 and pine oil are sequentially added to the pulp of the roughing tailings, and aeration flotation is performed to obtain primary scavenging concentrate and primary scavenging tailings.

[0057] After adding water glass to the rougher tailings slurry, stir for 2-4 minutes, preferably 2-3.5 minutes, more preferably 2.5-3 minutes; after adding LF-P80, stir for 2-5 minutes, preferably 2-4 minutes, more preferably 2.5-3.5 minutes; after adding pine oil, stir for 1-2 minutes, preferably 1-1.5 minutes. The operating temperature of the aeration flotation is 35-40°C, for example, 38°C.

[0058] Based on 1 ton of ground ore, the amount of water glass used can be 40-60 g / t, preferably 45-55 g / t, and more preferably 47-50 g / t; the amount of LF-P80 used can be 100-300 g / t, preferably 120-280 g / t, and more preferably 150-220 g / t; and the amount of pine oil used can be 40-60 g / t, preferably 45-55 g / t, and more preferably 50-55 g / t.

[0059] Second sweep

[0060] LF-P80 and pine oil are added to the pulp of the primary scavenging concentrate in sequence, and aeration flotation is performed to obtain the secondary scavenging concentrate and secondary scavenging tailings.

[0061] After adding LF-P80 to the slurry of the primary scavenged concentrate, stir for 2 to 4 minutes, preferably 2 to 3 minutes; after adding pine oil, stir for 1 to 2 minutes, preferably 1 to 1.5 minutes. The operating temperature of the aeration flotation is 35 to 40°C, for example, 38°C.

[0062] Based on 1 ton of ground product, the amount of LF-P80 used can be 80-120 g / t, preferably 90-110 g / t, and more preferably 100-110 g / t. The amount of pine oil used can be 40-60 g / t, preferably 45-55 g / t, and more preferably 50-55 g / t.

[0063] <Mid-stage ore processing steps>

[0064] The middlings product is the product obtained by combining the tertiary beneficiation tailings and the secondary scavenging concentrate. In the present invention, the tertiary beneficiation tailings and the secondary scavenging concentrate are combined and ground to obtain the reground middlings product. This helps to improve the recovery rate.

[0065] The concentration of the ground ore is 55-70 wt%, preferably 60-70 wt%, more preferably 60-65 wt%. The fineness of the ground ore is -0.045 mm, accounting for 85-90%.

[0066] The regrinded middlings are processed as described below.

[0067] Rough separation of regrinding middlings

[0068] Basic carbonate, water glass, LF-P80 and pine oil are added to the pulp of the reground middlings in sequence, and aeration flotation is performed to obtain middling rougher concentrate and middling rougher tailings.

[0069] The basic carbonate may be sodium carbonate or potassium carbonate, preferably sodium carbonate.

[0070] After adding basic carbonate to the regrinded ore product, stir for 2-4 minutes, preferably 2.5-3.5 minutes, for example, 3 minutes; after adding water glass, stir for 2-3 minutes, preferably 2-2.5 minutes; after adding LF-P80, stir for 2-4 minutes, preferably 2-3 minutes; after adding pine oil, stir for 1-2 minutes, preferably 1-1.5 minutes. The operating temperature of the aeration flotation is 35-45°C, for example, 38°C or 40°C.

[0071] Based on 1 ton of ground ore, the amount of basic carbonate used can be 0.3-0.6 kg / t, preferably 0.35-0.55 kg / t, and more preferably 0.4-0.5 kg / t. The amount of water glass used can be 0.5-0.7 kg / t, preferably 0.55-0.65 kg / t, and more preferably 0.6-0.65 kg / t. The amount of LF-P80 used can be 1.0-1.5 kg / t, preferably 1.1-1.4 kg / t, and more preferably 1.2-1.3 kg / t. The amount of pine oil used can be 130-180 g / t, preferably 140-170 g / t, and more preferably 150-160 g / t.

[0072] Further flotation of middling rougher concentrate

[0073] Sodium silicate, LF-P80 and pine oil are sequentially added to the pulp of the middling rougher concentrate, and aeration flotation is performed to obtain the primary middling concentrate and the primary middling tailings.

[0074] After adding water glass to the slurry of the middling rougher concentrate, stir for 2-3 minutes, preferably 2.5-3 minutes; after adding LF-P80, stir for 2-4 minutes, preferably 2.5-3.5 minutes; after adding pine oil, stir for 1-2 minutes, preferably 1-1.5 minutes. The operating temperature of the aeration flotation is 35-45°C, for example, 38°C or 40°C.

[0075] Based on 1 t of grinding product, the amount of water glass used can be 0.2-0.4 kg / t, preferably 0.25-0.35 kg / t, and more preferably 0.28-0.32 kg / t; the amount of LF-P80 used can be 0.4-0.7 kg / t, preferably 0.45-0.65 kg / t, and more preferably 0.5-0.6 kg / t; the amount of pine oil used can be 30-60 g / t, preferably 35-55 g / t, and more preferably 40-50 g / t.

[0076] The tailings from the primary middling beneficiation can be returned to the rougher feed of the regrinding middling product.

[0077] Further flotation of primary middling concentrate

[0078] Sodium silicate, LF-P80 and pine oil are sequentially added to the pulp of the primary middling concentrate, and aeration flotation is performed to obtain the middling regrinding flotation concentrate and the secondary middling tailings.

[0079] After adding water glass to the slurry of the primary middling concentrate, stir for 2-4 minutes, preferably 2.5-3.5 minutes, more preferably 2.5-3 minutes; after adding LF-P80, stir for 2-4 minutes, preferably 2.5-3.5 minutes, more preferably 2.5-3 minutes; after adding pine oil, stir for 1-2 minutes, preferably 1-1.5 minutes. The operating temperature of the aeration flotation is 35-45°C, for example, 38°C or 40°C.

[0080] Based on 1 t of grinding product, the amount of water glass used can be 20-40 g / t, preferably 25-35 g / t, and more preferably 30-35 g / t; the amount of LF-P80 used can be 0.1-0.3 kg / t, preferably 0.15-0.25 kg / t, and more preferably 0.2-0.25 kg / t; the amount of pine oil used can be 30-60 g / t, preferably 35-55 g / t, and more preferably 40-50 g / t.

[0081] The secondary middling beneficiation tailings can be returned to the middling rougher concentrate for further flotation feed.

[0082] <Merge Steps>

[0083] The obtained tertiary concentrate and middling regrinding flotation concentrate are combined to form rare earth concentrate.

[0084] The rare earth concentrate has a REO grade greater than 45 wt%, preferably greater than 46 wt%, more preferably greater than 48 wt%, for example, greater than 48 wt% and less than 50 wt%. The REO recovery rate is greater than 85%, preferably greater than 87%, more preferably greater than 88%. The xenotime content is 60-70 wt%, preferably 61-69 wt%, more preferably 61.5-68.5 wt%. The cerium content is 10-15.5 wt%, preferably 11-15 wt%, more preferably 11.5-14.7 wt%.

[0085] <Measurement Method>

[0086] Determination of REO grade: The automatic quantitative analysis system for mineral characterization (AMICS) was used for determination.

[0087] Xenotime content: determined by automatic quantitative analysis system for mineral characterization (AMICS).

[0088] The content of cerium phosphate was determined by automatic quantitative analysis system for mineral characterization (AMICS).

[0089] The raw materials used in the following examples and comparative examples are described as follows:

[0090] LF-P80: purchased from Baotou Linfeng Technology Co., Ltd., a hydroxamic acid collector.

[0091] Water glass: purchased from Shandong Gucheng Chemical Technology Co., Ltd., modulus 2.5.

[0092] Example 1

[0093] The rare earth grade of the mineral containing cerium phosphate and xenotime is 5.34wt%, wherein the mass ratio of cerium phosphate to xenotime is 1:4.31.

[0094] The above-mentioned mineral was crushed to -10 mm using a jaw crusher, and then secondary crushed using a roller crusher and screened using a screen to obtain a crushed product with a particle size of less than 2.0 mm. The crushed product was ground at a grinding concentration of 60 wt % and a grinding fineness of -240 mesh accounting for 87.5%, thereby obtaining a ground product.

[0095] To the grinding product slurry, add 0.6 kg / t of sodium carbonate and stir for 3 minutes; add 1.0 kg / t of water glass and stir for 3 minutes; add 2.5 kg / t of LF-P80 and stir for 2 minutes; add 200 g / t of pine oil and stir for 1 minute. Then, perform aeration flotation at 40°C to obtain a rougher concentrate and rougher tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0096] To the pulp of the rougher concentrate, add 0.3 kg / t of water glass and stir for 2 minutes; then add 500 kg / t of LF-P80 and stir for 3 minutes; then add 50 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a primary concentrate and primary tailings. To the pulp of the primary concentrate, add 50 g / t of water glass and stir for 2 minutes; then add 100 g / t of LF-P80 and stir for 3 minutes; then add 50 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a secondary concentrate and secondary tailings. To the pulp of the secondary concentrate, add 50 g / t of collector and stir for 3 minutes; then add 50 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a tertiary concentrate and tertiary tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0097] To the rougher tailings slurry, add 50g / t of water glass and stir for 2 minutes; then add 200g / t of LF-P80 and stir for 3 minutes; then add 50g / t of pine oil and stir for 1 minute; then perform aeration flotation at 40°C to produce a primary scavenging concentrate and primary scavenging tailings. To the primary scavenging concentrate slurry, add 100g / t of LF-P80 and stir for 3 minutes; then add 50g / t of pine oil and stir for 1 minute; then perform aeration flotation at 40°C to produce a secondary scavenging concentrate and secondary scavenging tailings. The material amounts are calculated based on 1 ton of grinding product.

[0098] The middlings obtained by combining the tertiary concentrator tailings and the secondary scavenging concentrate were ground in a rod mill with a grinding concentration of 65wt% and a grinding fineness of -0.045mm accounting for 88%, thereby obtaining a reground middling product.

[0099] To the slurry of the reground middlings, add 0.5 kg / t of sodium carbonate and stir for 3 minutes; add 0.55 kg / t of water glass and stir for 2 minutes; add 1.2 kg / t of LF-P80 and stir for 3 minutes; add 140 g / t of pine oil and stir for 1 minute. Then, perform aeration flotation at 40°C to obtain a middling rougher concentrate and middling rougher tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0100] To the slurry of the middling rougher concentrate, add 0.3 kg / t of water glass and stir for 2 minutes; then add 0.5 kg / t of LF-P80 and stir for 3 minutes; then add 45 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a primary middling concentrate and a primary middling concentrate tailings. To the slurry of the primary middling concentrate, add 30 g / t of water glass and stir for 1 minute; then add 0.2 kg / t of LF-P80 and stir for 3 minutes; then add 45 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a middling regrinding flotation concentrate and a secondary middling concentrate tailings. The middling concentrate tailings are recycled step by step; the material amounts are calculated based on 1 ton of grinding product.

[0101] The obtained tertiary concentrate and middling regrinding flotation concentrate are combined to form rare earth concentrate.

[0102] Example 2

[0103] The rare earth grade of the mineral containing cerium phosphate and xenotime is 4.35wt%, wherein the mass ratio of cerium phosphate to xenotime is 1:3.62.

[0104] The above-mentioned mineral was crushed to -10 mm using a jaw crusher, and then secondary crushed using a roller crusher and screened using a screen to obtain a crushed product with a particle size of less than 2.0 mm. The crushed product was ground at a grinding concentration of 60 wt % and a grinding fineness of -240 mesh accounting for 87.5%, thereby obtaining a ground product.

[0105] To the grinding product slurry, add 0.55 kg / t of sodium carbonate and stir for 1 minute; add 0.9 kg / t of water glass and stir for 2 minutes; add 2.0 kg / t of LF-P80 and stir for 3 minutes; add 180 g / t of pine oil and stir for 1 minute. Then, perform aeration flotation at 40°C to obtain a rougher concentrate and rougher tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0106] To the pulp of the rougher concentrate, add 0.28 kg / t of water glass and stir for 2 minutes; then add 0.45 kg / t of LF-P80 and stir for 3 minutes; then add 40 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a primary concentrate and primary tailings. To the pulp of the primary concentrate, add 55 g / t of water glass and stir for 2 minutes; then add 120 g / t of LF-P80 and stir for 2 minutes; then add 40 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a secondary concentrate and secondary tailings. To the pulp of the secondary concentrate, add 60 g / t of LF-P80 and stir for 3 minutes; then add 50 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a tertiary concentrate and tertiary tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0107] To the pulp of the rougher tailings, add 50g / t of water glass and stir for 2 minutes; then add 150g / t of LF-P80 and stir for 3 minutes; then add 40g / t of pine oil and stir for 1 minute; then perform aeration flotation at 40°C to produce a primary scavenging concentrate and primary scavenging tailings. To the pulp of the primary scavenging concentrate, add 90g / t of LF-P80 and stir for 3 minutes; then add 45g / t of pine oil and stir for 1 minute; then perform aeration flotation at 40°C to produce a secondary scavenging concentrate and secondary scavenging tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0108] The intermediate ore product obtained by combining the tertiary concentrating tailings and the secondary scavenging concentrate is ground in a rod mill with a grinding concentration of 65wt% and a grinding fineness of -0.045mm accounting for 88.5%, thereby obtaining a reground intermediate ore product.

[0109] To the slurry of the reground middlings, add 0.4 kg / t of sodium carbonate and stir for 2 minutes; add 0.5 kg / t of water glass and stir for 2 minutes; add 1.2 kg / t of LF-P80 and stir for 3 minutes; add 140 g / t of pine oil and stir for 1 minute. Then, perform aeration flotation at 40°C to obtain a middling rougher concentrate and middling rougher tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0110] To the slurry of the middling rougher concentrate, add 0.3 kg / t of water glass and stir for 2 minutes; then add 0.4 kg / t of LF-P80 and stir for 2 minutes; then add 40 g / t of pine oil and stir for 1 minute; then aerate and flotate at 38°C to obtain a primary middling concentrate and a primary middling concentrate tailings. To the slurry of the primary middling concentrate, add 25 g / t of water glass and stir for 2 minutes; then add 0.18 kg / t of LF-P80 and stir for 2 minutes; then add 40 g / t of pine oil and stir for 1 minute; then aerate and flotate at 38°C to obtain a middling regrinding flotation concentrate and a secondary middling concentrate tailings. The middling concentrate tailings are recycled step by step; the material amounts are calculated based on 1 ton of grinding product.

[0111] The obtained tertiary concentrate and middling regrinding flotation concentrate are combined to form rare earth concentrate.

[0112] Example 3

[0113] The rare earth grade of the mineral containing cerium phosphate and xenotime is 6.02 wt %, wherein the mass ratio of cerium phosphate to xenotime is 1:5.83.

[0114] The above-mentioned mineral was crushed to -10 mm using a jaw crusher, and then secondary crushed using a roller crusher and screened using a screen to obtain a crushed product with a particle size of less than 2.0 mm. The crushed product was ground at a grinding concentration of 65 wt % and a grinding fineness of -240 mesh accounting for 89%, thereby obtaining a ground product.

[0115] To the grinding product slurry, add 0.7 kg / t of sodium carbonate and stir for 1 minute; add 1.2 kg / t of water glass and stir for 2 minutes; add 2.8 kg / t of LF-P80 and stir for 3 minutes; add 220 g / t of pine oil and stir for 1 minute. Then, perform aeration flotation at 42°C to obtain a rougher concentrate and rougher tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0116] To the pulp of the rougher concentrate, add 0.35 kg / t of water glass and stir for 2 minutes; then add 0.6 kg / t of LF-P80 and stir for 3 minutes; then add 60 g / t of pine oil and stir for 1 minute; then flotate at 38°C with aeration to produce a primary concentrate and primary concentrate tailings. To the pulp of the primary concentrate, add 65 g / t of water glass and stir for 2 minutes; then add 150 g / t of LF-P80 and stir for 3 minutes; then add 50 g / t of pine oil and stir for 1 minute; then flotate at 38°C with aeration to produce a secondary concentrate and secondary concentrate tailings. To the pulp of the secondary concentrate, add 80 g / t of LF-P80 and stir for 3 minutes; then add 60 g / t of pine oil and stir for 1 minute; then flotate at 38°C with aeration to produce a tertiary concentrate and tertiary concentrate tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0117] To the rougher tailings slurry, add 60g / t of water glass and stir for 2 minutes; then add 250g / t of LF-P80 and stir for 3 minutes; then add 60g / t of pine oil and stir for 1 minute; then perform aeration flotation at 40°C to produce a primary scavenging concentrate and primary scavenging tailings. To the primary scavenging concentrate slurry, add 110g / t of LF-P80 and stir for 3 minutes; then add 60g / t of pine oil and stir for 1 minute; then perform aeration flotation at 40°C to produce a secondary scavenging concentrate and secondary scavenging tailings. The material amounts are calculated based on 1 ton of grinding product.

[0118] The intermediate ore product obtained by combining the tertiary concentrating tailings and the secondary scavenging concentrate was ground in a rod mill with a grinding concentration of 68wt% and a grinding fineness of -0.045mm accounting for 87.6%, thereby obtaining a reground intermediate ore product.

[0119] To the slurry of the reground middlings, add 0.5 kg / t of sodium carbonate and stir for 2 minutes; add 0.6 kg / t of water glass and stir for 2 minutes; add 1.5 kg / t of LF-P80 and stir for 3 minutes; add 180 g / t of pine oil and stir for 1 minute. Then, perform aeration flotation at 40°C to obtain a middling rougher concentrate and middling rougher tailings. The amounts of each material are calculated based on 1 ton of grinding product.

[0120] To the slurry of the middling rougher concentrate, add 0.4 kg / t of water glass and stir for 2 minutes; then add 0.7 kg / t of LF-P80 and stir for 2 minutes; then add 50 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a primary middling concentrate and a primary middling concentrate tailings. To the slurry of the primary middling concentrate, add 40 g / t of water glass and stir for 2 minutes; then add 0.3 kg / t of LF-P80 and stir for 3 minutes; then add 60 g / t of pine oil and stir for 1 minute; then aerate and flotate at 40°C to obtain a middling regrinding flotation concentrate and a secondary middling concentrate tailings. The middling concentrate tailings are recycled step by step; the material amounts are calculated based on 1 ton of grinding product.

[0121] The obtained tertiary concentrate and middling regrinding flotation concentrate are combined to form rare earth concentrate.

[0122] Comparative Example 1

[0123] The only difference from Example 1 is that the tertiary concentrating tailings and the secondary scavenging concentrate are combined to obtain a middling product, which is not further ground and is directly processed to the next step.

[0124] Table 1

[0125]

[0126] The present invention is not limited to the above-mentioned embodiments. Any modification, improvement, or substitution that can be conceived by those skilled in the art without departing from the essential content of the present invention shall fall within the scope of the present invention.

Claims

1. A method for increasing the rare earth grade of a mineral containing cerium phosphate and xenotime, characterized in that: The following steps are involved: 1) Crushing the minerals containing cerium phosphate and xenotime to obtain crushed products; grinding the crushed products to obtain grinding products; 2) Add 0.5-0.8 kg / t of basic carbonate, 0.8-1.2 kg / t of water glass, 2.0-3.0 kg / t of LF-P80, and 150-240 g / t of pine oil to the slurry of the grinding product in sequence, and perform aeration flotation to obtain rougher concentrate and rougher tailings. The amount of each material is calculated based on 1 ton of grinding product. 3) 0.2-0.4 kg / t of water glass, 0.4-0.6 kg / t of LF-P80 and 30-60 g / t of pine oil are sequentially added to the pulp of the rougher concentrate, and aeration flotation is performed to obtain a primary concentrate and a primary concentrate tailings; 40-70 g / t of water glass, 100-150 g / t of LF-P80 and 30-60 g / t of pine oil are sequentially added to the pulp of the primary concentrate, and aeration flotation is performed to obtain a secondary concentrate and a secondary concentrate tailings; 50-80 g / t of LF-P80 and 40-60 g / t of pine oil are sequentially added to the pulp of the secondary concentrate, and aeration flotation is performed to obtain a tertiary concentrate and a tertiary concentrate tailings; wherein the amount of each material used is calculated based on 1 ton of grinding product; 4) 40-60 g / t of water glass, 100-300 g / t of LF-P80, and 40-60 g / t of pine oil are sequentially added to the pulp of the rougher tailings, and aeration flotation is performed to obtain a primary scavenging concentrate and a primary scavenging tailings; 80-120 g / t of LF-P80 and 40-60 g / t of pine oil are sequentially added to the pulp of the primary scavenging concentrate, and aeration flotation is performed to obtain a secondary scavenging concentrate and a secondary scavenging tailings; the amount of each material used is calculated based on 1 ton of grinding product; 5) The obtained tertiary concentrator tailings and secondary scavenging concentrate are combined and ground to obtain a reground middling product; 0.3-0.6 kg / t of basic carbonate, 0.5-0.7 kg / t of water glass, 1.0-1.5 kg / t of LF-P80 and 130-180 g / t of pine oil are sequentially added to the pulp of the reground middling product, and aeration flotation is performed to obtain a middling rougher concentrate and a middling rougher tailing; 0.2-0.4 kg / t of water glass, 0.4-0.7 kg / t of LF-P80 and 30-60 g / t of pine oil are sequentially added to the pulp of the middling rougher concentrate, and aeration flotation is performed to obtain a primary middling concentrate and a primary middling concentrate tailing; 20-40 g / t of water glass, 0.1-0.3 kg / t of pine oil and 130-180 g / t of pine oil are sequentially added to the pulp of the primary middling concentrate. LF-P80 and 30-60g / t pine oil are used for aeration flotation to obtain middling regrinding flotation concentrate and secondary middling beneficiation tailings. The amount of each material is calculated based on 1t of grinding product. 6) The obtained tertiary concentrate and the middling regrinding flotation concentrate are combined to obtain the rare earth concentrate; Among them, LF-P80 is a hydroxamic acid collector purchased from Baotou Linfeng Technology Co., Ltd.

2. The method according to claim 1, characterized in that In step 1), the REO grade of the mineral containing acerite and xenotime is 2-13 wt %, and the mass ratio of acerite to xenotime is 1:3.1-7.

5.

3. The method according to claim 2, characterized in that In step 1), the mineral raw materials containing cerium phosphate and xenotime also contain gangue minerals, and the gangue minerals are mainly quartz and illite.

4. The method according to claim 2, characterized in that In step 1), the particle size of the crushed product is below 2.0 mm; the grinding concentration is 50-65 wt%, and the grinding fineness is -240 mesh, accounting for 85-90%.

5. The method according to claim 2, characterized in that In step 2), after adding basic carbonate to the ore pulp of the grinding product, stir for 1 to 5 minutes, after adding water glass, stir for 2 to 5 minutes, after adding LF-P80, stir for 2 to 7 minutes, and after adding pine oil, stir for 1 to 5 minutes. The operating temperature of the aeration flotation is 35 to 40°C.

6. The method according to claim 2, characterized in that In step 3), after adding water glass to the pulp of the rougher concentrate, stir for 2 to 5 minutes; after adding LF-P80, stir for 2 to 5 minutes; after adding pine oil, stir for 1 to 2 minutes; after adding water glass to the pulp of the primary concentrate, stir for 2 to 4 minutes, after adding LF-P80, stir for 2 to 5 minutes, and after adding pine oil, stir for 1 to 2 minutes; after adding LF-P80 to the pulp of the secondary concentrate, stir for 2 to 4 minutes, and after adding pine oil, stir for 1 to 2 minutes; the operating temperature of the aeration flotation is 35 to 40°C.

7. The method according to claim 2, characterized in that In step 4), after adding water glass to the pulp of the rougher tailings, stir for 2 to 4 minutes; after adding LF-P80, stir for 2 to 5 minutes; after adding pine oil, stir for 1 to 2 minutes; after adding LF-P80 to the pulp of the primary scavenging concentrate, stir for 2 to 4 minutes, and after adding pine oil, stir for 1 to 2 minutes; the operating temperature of the aeration flotation is 35 to 40°C.

8. The method according to claim 2, characterized in that In step 5), the grinding concentration is 55-70 wt%, and the grinding fineness is -0.045 mm, accounting for 85-90%.

9. The method according to claim 2, characterized in that In step 5), after adding basic carbonate to the regrinded middlings, the mixture is stirred for 2 to 4 minutes, after adding water glass, the mixture is stirred for 2 to 3 minutes, after adding LF-P80, the mixture is stirred for 2 to 4 minutes, and after adding pine oil, the mixture is stirred for 1 to 2 minutes; after adding water glass to the pulp of the middling rougher concentrate, the mixture is stirred for 2 to 3 minutes, after adding LF-P80, the mixture is stirred for 2 to 4 minutes, and after adding pine oil, the mixture is stirred for 1 to 2 minutes; after adding water glass to the pulp of the primary middling concentrate, the mixture is stirred for 2 to 4 minutes, after adding LF-P80, the mixture is stirred for 2 to 4 minutes, and after adding pine oil, the mixture is stirred for 1 to 2 minutes; the operating temperature of the aeration flotation is 35 to 45°C; wherein, the basic carbonate is sodium carbonate or potassium carbonate.

10. The method according to any one of claims 2 to 9, characterized in that: In the rare earth concentrate, the REO grade is greater than 45wt%, the REO recovery rate is greater than 85%, the content of xenotime is 60-70wt%, and the content of cerium aluminum phosphate is 10-15.5wt%.

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