Method for preparing yellow phosphorus through flotation and smelting of flotation tailings
Through the joint preparation method of flotation tailings flotation smelting, the problem of yellow phosphorus production restriction caused by the reduction of high-quality phosphorus ores is solved, and the efficient utilization of phosphorus ores and the efficient production of yellow phosphorus is achieved.
Patent Information
- Application Number
- CN202510000425.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-02
- Publication Date
- 2025-04-18
AI Technical Summary
Due to the reduction of high-quality phosphorus ores, yellow phosphorus production is restricted, and the problem of the source of ore production of yellow phosphorus needs to be solved.
The flotation tailings flotation smelting joint preparation method includes rough selection, selection, ball making and roasting reduction steps, flotation and ball making are flotation and ball making using chemical agents such as sulfuric acid, phosphoric acid, fatty acid collectors and binders, and finally reducing in a roasting furnace to obtain yellow phosphorus.
It realizes efficient utilization of phosphate ore, reduces grinding energy consumption, improves the production efficiency and resource utilization of yellow phosphorus, and avoids resource waste.
Smart Images
Figure CN119841288A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of mineral processing, and in particular to a method for preparing yellow phosphorus by combining flotation and smelting of flotation tailings. Background Art
[0002] Among the allotropes of phosphorus, yellow phosphorus and red phosphorus are the most widely used. The safety matches in our daily life and the organic pesticides used in agriculture all come from red phosphorus. The hot acids and phosphates needed in fertilizers, pesticides, medicines, food and electronics industries all come from yellow phosphorus.
[0003] Yellow phosphorus adopts the electric furnace process, in which phosphate ore, silica and coke are reduced at high temperature in the electric furnace, and the phosphide in the phosphate ore is reduced to elemental phosphorus, which escapes in the electric furnace in the form of phosphorus vapor, and solid yellow phosphorus is obtained after multi-stage condensation. The above process requires that the P2O5 content in the phosphate ore entering the furnace is greater than 25%. With the increasing consumption of high-quality phosphate ore, the phosphorus block ore that can be used to produce yellow phosphorus is becoming less and less, and it is urgent to solve the problem of the source of ore for yellow phosphorus production. Summary of the invention
[0004] The object of the present invention is to provide a method for preparing yellow phosphorus by combining flotation tailings flotation and smelting, so as to solve the problem in the prior art that yellow phosphorus production is limited due to the reduction of high-quality phosphate ore.
[0005] The scheme of the present invention is: a method for preparing yellow phosphorus by flotation tailings flotation smelting, characterized in that it comprises the following steps:
[0006] S1. Add the flotation tailings with a P2O5 content of 5.0% to 10.0% into the flotation machine for roughing. Sulfuric acid is added during the flotation process. The flotation foam is used as the roughing tailings. The pulp in the flotation tank enters the fine selection.
[0007] S2, after adding phosphoric acid, sulfuric acid and fatty acid collectors in the flotation tank in turn, reverse flotation is carried out; the flotation foam is combined with the S1 roughing tailings as the final tailings, and the flotation pulp in the flotation tank is used as the flotation concentrate, which is filtered to a water content of 10.0-20.0%;
[0008] S3, adding binder and water to the filtered flotation concentrate in turn, mixing, kneading, pressing, and then adding the flotation concentrate to the ball making machine to make balls, and drying after the ball making is completed;
[0009] S4. Add carbon powder to the dried ore balls and mix well. Then add the balls into a roasting furnace, introduce N2 protection, roast and reduce the balls at a temperature of 1200-1300° C. for 30-60 minutes, and condense to obtain yellow phosphorus.
[0010] As a preferred technical solution, in the step S1, 1.0-3.0 kg / t of sulfuric acid is added and stirred for 0.5-1.0 min. The mass concentration of the sulfuric acid is 40.0%.
[0011] As a preferred technical solution, in step S1, 1.8-2.0 kg / t of sulfuric acid is added and stirred for 0.5-1.0 min. The mass concentration of the sulfuric acid is 40.0%.
[0012] As a preferred technical solution, in the step S2, first add 1.0-5.0 kg / t of phosphoric acid, stir for 0.50-1.0 min, then add 10.0-30.0 kg / t of sulfuric acid, stir for 0.5-1.0 min, then add 1.0-4.0 kg / t of fatty acid collector, stir for 2.0-3.0 min.
[0013] As a preferred technical solution, in the step S2, 1.0-1.2 kg / t of phosphoric acid is first added, stirred for 0.50-1.0 min, then 20.0-20.5 kg / t of sulfuric acid is added, stirred for 0.5-1.0 min, and then 2.5-3.0 kg / t of fatty acid collector is added, stirred for 2.0-3.0 min.
[0014] As a preferred technical solution, the fatty acid collector in step S2 is YP6-6.
[0015] As a preferred technical solution, in the step S3, the amount of binder used is 0.4-2.0% of the mass of the flotation concentrate, the amount of water added is 5.0-10.0% of the flotation concentrate, and the particle size of the pellets is 10mm-25mm.
[0016] As a preferred technical solution, in the step S3, the amount of binder used is 0.4-0.5% of the mass of the flotation concentrate, the amount of water added is 5.0-6.0% of the flotation concentrate, and the particle size of the pellets is 10mm-25mm.
[0017] As a preferred technical solution, the binder in S3 is slag acid.
[0018] As a preferred technical solution, the slag acid includes 1wt% to 6wt% of phosphoric acid and 10wt% to 25wt% of gypsum.
[0019] As a preferred technical solution, the flow rate of N2 introduced in the S4 step is 0.5 to 1.0 L / min.
[0020] As a preferred technical solution, the flow rate of N2 introduced in the S4 step is 0.5 to 0.6 L / min.
[0021] As a preferred technical solution, the amount of carbon powder used is 15-30% of the mass of the flotation concentrate.
[0022] As a preferred technical solution, the amount of carbon powder used is 20-25% of the mass of the flotation concentrate.
[0023] Advantages of the present invention:
[0024] The present invention further develops and utilizes flotation tailings, and pelletizes the phosphate concentrate obtained by enriching the flotation tailings to replace yellow phosphate ore for yellow phosphorus production, thereby realizing efficient utilization of phosphate ore.
[0025] The invention is simple to operate, saves energy consumption, reduces production costs, improves utilization rate, avoids waste of resources to a great extent, and increases overall income.
[0026] The invention effectively reduces the energy consumption of grinding, realizes the graded use of phosphate ore, and makes effective use of phosphate ore resources. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 It is a process framework diagram of the present invention. DETAILED DESCRIPTION
[0028] 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.
[0029] The following examples are only used to further illustrate the present invention in detail, but do not constitute any limitation to the present invention; the materials used in the following examples, unless otherwise specified, were purchased from conventional chemical reagent companies and raw material suppliers.
[0030] Example 1
[0031] The P2O5 content of flotation tailings in a flotation plant in Yunnan is 6.12%. After one roughing and one concentrating, flotation concentrate is obtained. Specifically, the flotation tailings are added to the flotation machine for roughing, and sulfuric acid with a mass concentration of 40% is added at 2.0kg / t for roughing. After stirring for 1min, flotation is performed. The flotation foam is used as roughing tailings, and the pulp in the flotation tank enters the concentrating. Phosphoric acid 1.0kg / t is added for concentrating, stirring for 1.0 minute, sulfuric acid 20.0kg / t is added, stirring for 1.0 minute, and then fatty acid collector YP6-6 2.5kg / t is added. After stirring for 3.0 minutes, reverse flotation is performed. The flotation pulp in the flotation tank is used as flotation concentrate and filtered through a vacuum filter to a water content of 10.0%. Then 0.4% slag acid is added as a binder, and 5.0% water is added in turn to mix well, knead into a ball, put into a ball making machine for ball making, and then dried. The particle size of the ball is 10mm. Add 20% of the mass of flotation concentrate to the carbon powder and mix with the ore balls, then put into the roasting furnace, pass 0.5L / min of N2 protection, roast and reduce at 1300℃, condense the escaped phosphorus vapor, and obtain yellow phosphorus. The specific indicators are shown in Table 1.
[0032] Table 1
[0033] <![CDATA[P205% of flotation tailings]]> <![CDATA[Composite tailings P205%]]> <![CDATA[P205% of flotation concentrate]]> <![CDATA[P205% Reduction Rate%]]> 6.12％ 5.03％ 23.08 93.12％
[0034] Example 2
[0035] The P2O5 content of flotation tailings in a flotation plant in Yunnan is 8.06%. After one roughing and one concentrating, flotation concentrate is obtained. Specifically, the flotation tailings are added to the flotation machine for roughing, and sulfuric acid with a mass concentration of 40% is added at 2.0kg / t for roughing. After stirring for 1min, flotation is performed. The flotation foam is used as roughing tailings, and the pulp in the flotation tank enters the concentrating. Phosphoric acid 1.0kg / t is added for concentrating, stirring for 1.0 minute, sulfuric acid 20.0kg / t is added, stirring for 1.0 minute, and then fatty acid collector YP6-6 2.5kg / t is added. After stirring for 3.0 minutes, reverse flotation is performed. The flotation pulp in the flotation tank is used as flotation concentrate, and filtered through a vacuum filter to a water content of 10.0%. Then 0.4% slag acid is added as a binder, and 5.0% water is added in turn to mix well, knead into a ball, put into a ball making machine to make balls, and then dried. The particle size of the balls is 10mm. Add 20% of the mass of flotation concentrate carbon powder and mix with the ore balls, then put into the roasting furnace, pass 0.5L / min of N2 protection, roast and reduce at 1300℃, condense the escaped phosphorus vapor, and obtain yellow phosphorus. The specific indicators are shown in Table 2.
[0036] Table 2
[0037] <![CDATA[P205% of flotation tailings]]> <![CDATA[Composite tailings P205%]]> <![CDATA[P205% of flotation concentrate]]> <![CDATA[P205% Reduction Rate%]]> 8.06％ 5.56％ 24.22 95.08％
[0038] Example 3
[0039] The P2O5 content of flotation tailings in a flotation plant in Yunnan is 9.80%. After one roughing and one concentrating, flotation concentrate is obtained. Specifically, the flotation tailings are added to the flotation machine for roughing, and sulfuric acid with a mass concentration of 40% is added at 3.0kg / t for roughing. After stirring for 1min, flotation is performed. The flotation foam is used as roughing tailings, and the pulp in the flotation tank enters the concentrating. Phosphoric acid 5.0kg / t is added for concentrating, stirred for 1.0 minute, sulfuric acid 30.0kg / t is added, stirred for 1.0 minute, and fatty acid collector YP6-61kg / t is added. After stirring for 3.0 minutes, reverse flotation is performed. The flotation pulp in the flotation tank is used as flotation concentrate and filtered through a vacuum filter to a water content of 10.0%. Then 0.4% slag acid is added as a binder, and 5.0% water is added in turn to mix well, knead into a ball, put into a ball making machine for ball making, and then dried. The particle size of the ball is 10mm. Add 30% of the mass of flotation concentrate carbon powder and mix with the ore balls, then put into the roasting furnace, pass 1L / min of N2 protection, roast and reduce at 1200℃, and condense the escaped phosphorus vapor to obtain yellow phosphorus.
[0040] <![CDATA[P205% of flotation tailings]]> <![CDATA[Composite tailings P205%]]> <![CDATA[P205% of flotation concentrate]]> <![CDATA[P205% reduction rate%]]> 9.8％ 5.78％ 24.80 96.32％
[0041] S1. Add the flotation tailings with a P2O5 content of 7.0% into the flotation machine for roughing. Sulfuric acid is added during the flotation process. The flotation foam is used as the roughing tailings. The pulp in the flotation tank enters the fine selection.
[0042] S2, after adding phosphoric acid, sulfuric acid and fatty acid collectors in the flotation tank in turn, reverse flotation is carried out; the flotation foam is combined with the roughing tailings of S1 as the final tailings, and the flotation pulp in the flotation tank is used as the flotation concentrate, which is poured into a vacuum filter and filtered to a water content of 12%;
[0043] S3, adding binder and water to the filtered flotation concentrate in turn, mixing, kneading, pressing, and then adding the flotation concentrate to the ball making machine to make balls, and drying after the ball making is completed;
[0044] S4. Add 20% of the mass of the flotation concentrate to the dried ore balls, mix well, add to the roasting furnace, introduce N2 protection, and then roast and reduce at a temperature of 1300° C. for 60.0 min, and condense to obtain yellow phosphorus.
[0045] In the step S1, 2.0 kg / t of sulfuric acid is added and stirred for 1.0 min. The mass concentration of the sulfuric acid is 40.0%.
[0046] In the step S2, 1.0 kg / t of phosphoric acid is first added, stirred for 1.0 min, then 20.00 kg / t of sulfuric acid is added, stirred for 1.0 min, and then 2.5 kg / t of fatty acid collector is added, stirred for 3.0 min.
[0047] In the step S2, the fatty acid collector is YP6-6, and the YP6-6 contains fatty acids with 6 to 12 carbon chains.
[0048] In the step S3, the amount of binder added in the first ball making is 0.4% of the mass of the flotation concentrate, the amount of water added is 5.0% of the flotation concentrate, and the particle size of the ball making is 20 mm.
[0049] The binder in S3 is slag acid.
[0050] The flow rate of N2 introduced in step S4 is 0.5 L / min.
[0051] 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 method for preparing yellow phosphorus by flotation tailings flotation smelting, characterized in that: The following steps are involved: S1. Add the flotation tailings with a P2O5 content of 5.0% to 10.0% into the flotation machine for roughing. Sulfuric acid is added during the flotation process. The flotation foam is used as the roughing tailings. The pulp in the flotation tank enters the fine separation. S2, after adding phosphoric acid, sulfuric acid and fatty acid collectors in the flotation tank in turn, reverse flotation is carried out; the flotation foam is combined with the S1 roughing tailings as the final tailings, and the flotation pulp in the flotation tank is used as the flotation concentrate, which is filtered to a water content of 10.0-20.0%; S3, adding binder and water to the filtered flotation concentrate in turn, mixing, kneading, pressing, and then adding the flotation concentrate to the ball making machine to make balls, and drying after the ball making is completed; S4. Add carbon powder to the dried ore balls and mix well. Then add the balls into a roasting furnace, introduce N2 protection, roast and reduce the balls at a temperature of 1200-1300° C. for 30-60 minutes, and condense to obtain yellow phosphorus.
2. The method for preparing yellow phosphorus by flotation and smelting of flotation tailings as claimed in claim 1, characterized in that: In the step S1, 1.0-3.0 kg / t of sulfuric acid is added and stirred for 0.5-1.0 min. The mass concentration of the sulfuric acid is 40.0%.
3. The method for preparing yellow phosphorus by flotation and smelting of flotation tailings as claimed in claim 1, characterized in that: In the step S2, 1.0-5.0 kg / t of phosphoric acid is first added, stirred for 0.50-1.0 min, then 10.0-30.0 kg / t of sulfuric acid is added, stirred for 0.5-1.0 min, and then 1.0-4.0 kg / t of fatty acid collector is added, stirred for 2.0-3.0 min.
4. A method for preparing yellow phosphorus by flotation and smelting of flotation tailings as claimed in claim 1 or 3, characterized in that: In the step S2, the fatty acid collector is YP6-6.
5. The method for preparing yellow phosphorus by flotation and smelting of flotation tailings as claimed in claim 1, characterized in that: In the step S3, the amount of binder used is 0.4-2.0% of the mass of the flotation concentrate, the amount of water added is 5.0-10.0% of the flotation concentrate, and the particle size of the pellets is 10mm-25mm.
6. The method for preparing yellow phosphorus by flotation and smelting of flotation tailings as claimed in claim 1 or 5, characterized in that: The binder in S3 is slag acid.
7. The method for preparing yellow phosphorus by flotation and smelting of flotation tailings as claimed in claim 1, characterized in that: The flow rate of N2 introduced in the step S4 is 0.5-1.0 L / min.
8. The method for preparing yellow phosphorus by flotation and smelting of flotation tailings as claimed in claim 1, characterized in that: The amount of carbon powder used is 15-30% of the mass of the flotation concentrate.