Method for processing and purifying medical stone

Abstract

The application relates to the technical field of mineral processing, and particularly discloses a method for processing and purifying medical stone. The method for processing and purifying medical stone provided by the application adopts hydraulic separation, flotation separation and magnetic separation to obtain medical stone primary products, removes most of the gangue minerals and impurities in raw materials, greatly reduces the amount of subsequent chemical treatment, and saves production cost; then hydrochloric acid is used for heating leaching to further remove Fe impurities, and high-quality medical stone powder is obtained. The application has the advantages of being economic and environment-friendly, easy to implement and operate, high in product yield and high in product quality, and realizes high-value recycling of low-grade medical stone.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of mineral processing, in particular to a method for processing and purifying medical stone. BACKGROUND

[0002] Medical stone is a kind of mineral with a long application history, which has four functions of releasing beneficial trace elements, adsorbing harmful substances, bidirectional adjustment of acid-base value and dissolution of oxygen. Medical stone contains dozens of constant elements, trace elements and rare earth elements, which are necessary for the growth and development of human beings and other organisms. In the field of food, medical stone powder can be used as a food additive to produce fortified food. At the same time, medical stone is an important mineral feed additive, which has the functions of promoting blood circulation and promoting growth and development. For example, medical stone powder as a feed additive can dissolve tens of times more effective components than ordinary water-soluble ones in a gastric acid environment.

[0003] For the utilization of medical stone, whether the elements needed by the human body can be dissolved is an important standard for identifying medical stone. At the same time, the lower the content of harmful elements dissolved, the higher the quality of medical stone. It is the consensus in the industry that the content of harmful elements should be lower than the average content of the earth's crust, i.e. the Clarke value. Therefore, for the utilization of medical stone, especially for the utilization of medical stone leaching liquor, as long as the content of harmful elements does not exceed the upper limit of the national drinking water standard, it is safe and reliable.

[0004] However, in actual production, there are not many medical stones with harmful elements lower than the Clarke value. The chemical composition and content of medical stone from different places are also different. The formation age characteristics, output mode of medical stone and the mixing of other minerals in the mining process will cause the enrichment of some harmful elements, resulting in high content of harmful elements in medical stone. In order to ensure the safety of medical stone in use, it is necessary to ensure that the content of harmful elements is within the normal range. Although medical stone has been applied in China for more than 2000 years, the analysis and testing, evaluation and research, purification and utilization of medical stone by modern technology and methods are still in the exploratory stage.

[0005] Therefore, it is necessary to study medical stone to propose a method for processing and purifying medical stone. SUMMARY

[0006] The technical problem solved by the present application is to provide a method for processing and purifying medical stone. Through the treatment process of fine grinding, physical beneficiation and chemical removal of impurities, high-quality medical stone products can be obtained, which can be used as food-grade medical stone.

[0007] To solve the above technical problems, the technical scheme adopted by the present application is as follows: a method for processing and purifying medical stone, comprising the steps of:

[0008] S1: break the mineral of medical stone to -10 mm, then prepare a mineral slurry with a mass percentage concentration of 60-65% by adding water, and then grind to a particle size of -0.075 mm accounting for more than 95% (i.e. the mass percentage content of the mineral with a particle size less than 0.075 mm is more than 95%), to obtain a grinding mineral slurry;

[0009] S2: adjust the grinding mineral slurry to a mass percentage concentration of 20-25% by adding water, remove fine mud of -10 μm by using hydraulic classification, and obtain -10 μm fine mud as fine mud tailings, and +10 μm particle size products enter the next step;

[0010] S3: adjust the +10 μm particle size products to a mass percentage concentration of 25-35% by adding water, then add an adjusting agent and a collecting agent, perform one-time gangue mineral roughing and one-time scavenging, and obtain a flotation froth and a flotation underflow, and the flotation froth is taken as a flotation tailings;

[0011] S4: adjust the flotation underflow to a mass percentage concentration of 25-30%, perform magnetic separation, and obtain magnetic material and non-magnetic material, and the magnetic material is taken as a magnetic tailings, and the non-magnetic material is concentrated to obtain a medical stone primary product;

[0012] S5: mix and react the medical stone primary product with dilute acid, control the liquid-solid ratio to be (1.5-3):1, remove impurities by leaching, then collect the solid, and obtain a leaching product, and the leaching product is washed to obtain a medical stone product.

[0013] As an embodiment of the present application, in step S2, the separation equipment used in the hydraulic classification process is a hydraulic classification tank or a hydrocyclone.

[0014] As an embodiment of the present application, in step S3, the adjusting agent is sodium carbonate, and the amount used is 200-800 g per ton of medical stone mineral; and the collecting agent is oleic acid or sodium oleate, and the amount used is 100-300 g per ton of medical stone mineral.

[0015] As an embodiment of the present application, in step S4, the magnetic separation uses a high gradient magnetic separator, and the background field strength of the magnetic separation is 0.6-1.0 T, and the pulse is 60-90 r / min.

[0016] As an embodiment of the present application, in step S5, the dilute acid is dilute hydrochloric acid, and the mass percentage concentration is 1-3%.

[0017] As an embodiment of the present application, in step S5, the heating temperature of the reaction is 40-50°C; and the reaction time is 1-3 h.

[0018] The method for processing and purifying the medical stone provided by the application obtains the medical stone primary product, the mass percentage content of Fe in the medical stone primary product is 0.05-0.15%, As is less than 10 mg / Kg, Pb is less than 15 mg / Kg, Cd is less than 2 mg / Kg, Hg is less than 0.1 mg / Kg, and F is less than 400 mg / Kg.

[0019] The method for processing and purifying the medical stone provided by the application obtains the medical stone product, the mass percentage content of Fe in the medical stone product is 0.02-0.04%, the content of As is 5-8 mg / Kg, the content of Pb is 8-12 mg / Kg, the content of Cd is 1.2-1.8 mg / Kg, the content of Hg is 0.05-0.08 mg / Kg, and the content of F is 100-310 mg / Kg.

[0020] The method for processing and purifying the medical stone provided by the application first grinds the medical stone mineral to the required fineness of the product by crushing and grinding. Then, the fine light mineral is removed cleanly and economically by using the hydraulic desliming separation, and the-10-micron fine particle level is collected as the fine mud tailings; the main component of the fine mud tailings is the impurities containing Fe and Pb, which removes the harmful impurities and avoids the interference of the fine mud on the subsequent flotation. The +10-micron coarse particle level concentrate obtained by separation is subjected to froth flotation separation, and the flotation froth is collected as the flotation tailings and removed; the flotation mainly removes the fluorine-containing mineral and the heavy metal-containing sulfide mineral, and the flotation froth mainly contains F, Hg, As, Pb and Cd. The underflow is subjected to high-gradient magnetic separation, and the magnetic product is collected as the magnetic tailings and removed together with the-10-micron fine particle gangue and the flotation tailings; the magnetic tailings mainly contain Fe impurities, and the non-magnetic product obtained by high-gradient magnetic separation is the medical stone primary product. Through the above physical separation steps, most of the gangue minerals and impurities in the medical stone raw material are removed, the amount of acid chemical purification treatment is greatly reduced, and the production cost is saved. Then, the obtained medical stone primary product is stirred and subjected to dilute acid leaching at a temperature of 40-50 DEG C, and the solid after leaching is cleaned and filtered to obtain the high-quality medical stone product. The Fe content in the mineral can be further reduced by stirring and heating acid leaching, and the high-quality medical stone product can be obtained, which can be used as food-grade medical stone.

[0021] The present application is directed to the problem that low-grade medical stone minerals with high harmful element content and easy to be dissolved or mixed with other impurities are difficult to utilize, and provides a medical stone processing and purification method. The present application utilizes economic, efficient hydrodynamic separation, flotation separation and magnetic separation to obtain medical stone primary products, and then uses hydrochloric acid warming leaching to obtain high-quality medical stone powder. The medical stone product has a yield of greater than 75%, a mass percentage content of -200 mesh particle size products of 95%, a mass percentage content of Fe of less than 0.05%, As of less than 10 mg / Kg, Pb of less than 15 mg / Kg, Cd of less than 2 mg / Kg, Hg of less than 0.1 mg / Kg, and F of less than 400 mg / Kg. The present application has the advantages of being economic and environmentally friendly, easy to implement and operate, high product yield and product quality, and realizes high-value utilization of low-grade medical stone. BRIEF DESCRIPTION OF DRAWINGS

[0022] Figure 1 is a process flow chart of the medical stone processing and purification method provided by the present application. DETAILED DESCRIPTION

[0023] The technical solutions of the present application will be described in detail below through specific examples.

[0024] In the following examples, the reagents used, sodium carbonate, oleic acid, sodium oleate and hydrochloric acid, are all commercially available. When preparing the beneficiation reagents, except for the addition of the oleic acid stock solution, the rest are prepared with water. The concentrations in each example are all mass percentage concentrations.

[0025] Example 1

[0026] The present example provides a method for processing and purifying medical stone, which is carried out with reference to the process flow chart shown in Figure 1 The elemental analysis of the medical stone mineral processed is as follows:

[0027] Element Fe (wt%) As Pb Cd Hg F Content 0.96 20 mg / Kg 21 mg / Kg 1.8 mg / Kg 0.18 mg / Kg 600 mg / Kg

[0028] The processing steps are as follows:

[0029] (1) The medical stone mineral is crushed in a crusher, and the particle size is crushed to -10 mm by controlling the sieve size. Then, water is added to adjust the grinding concentration to 60%, and the medical stone mineral is ground to a particle size of -0.075 mm accounting for 98.46%, to obtain a grinding slurry;

[0030] (2) The mass percentage concentration of the grinding slurry is diluted to 20% with water, and then a hydrocyclone is used to remove -10 μm fine mud, to obtain -10 μm fine mud and +10 μm particle size products, and the -10 μm fine mud is fine mud tailings;

[0031] (3) adding clean water to adjust the concentration of the +10 μm particle size product obtained in step (2) to 30%, and then adding sodium carbonate and oleic acid in turn, the dosages of the two reagents being 600 g and 120 g per ton of the mineral, respectively, to perform one rough separation and one scavenging separation of the gangue mineral, to obtain a flotation froth and a flotation underflow, the flotation froth being a flotation tailing;

[0032] (4) adjusting the concentration of the flotation underflow obtained in step (3) to 25% to perform magnetic separation by using a high gradient magnetic separator, the background field strength of the high gradient magnetic separator being 0.8 T, and the pulse being 60 r / min, to obtain magnetic material and non-magnetic material, the magnetic material being a magnetic tailing; and the non-magnetic material being concentrated and filtered to obtain a preliminary product of the mineral, and the fine mud tailing, the flotation tailing and the magnetic tailing being combined to be discarded as a tailing;

[0033] (5) placing the preliminary product of the mineral obtained in step (4) in a water bath heating stirrer, adding 1.5% dilute hydrochloric acid, and controlling the water bath heating temperature to be 50°C under the condition of a liquid-to-solid ratio of 2:1, and heating and stirring for 2 h, and then cleaning and filtering the solid product after leaching to obtain a mineral powder product.

[0034] The yield of the mineral powder product relative to the dry sample of the mineral is 78.21%, and the content of the -200 mesh particle size is 97.41%.

[0035] The elemental analysis of the preliminary product of the mineral and the final mineral powder product obtained in this example is shown in the following table.

[0036]

[0037] Example 2

[0038] This example provides a method for processing and purifying the mineral, which is performed with reference to the process flow diagram shown in Figure 1 The elemental analysis of the mineral to be processed is as follows:

[0039] Element Fe (wt%) As Pb Cd Hg F Content 1.82 42 mg / Kg 65 mg / Kg 2.4 mg / Kg 2 mg / Kg 800 mg / Kg

[0040] The processing steps are as follows:

[0041] (1) crushing the mineral in a crusher, and controlling the screening to break the particle size to -10 mm, and then adding water to adjust the grinding concentration to 65%, and grinding the mineral to a particle size of -0.075 mm accounting for 96.42% to obtain a grinding slurry;

[0042] (2) diluting the grinding slurry to a mass percentage concentration of 20% by using clean water, and then removing -10 μm fine mud by using a hydrocyclone to obtain -10 μm fine mud and +10 μm particle size product, the -10 μm fine mud being a fine mud tailing;

[0043] (3) adding clean water to adjust the concentration of the +10 μm particle size product obtained in step (2) to 25%, and then adding sodium carbonate and sodium oleate in turn, the dosages of the agents being 800 g and 250 g per ton of the mineral, respectively, to perform one rough separation of the gangue mineral and one scavenging, to obtain a flotation froth and a flotation underflow, the flotation froth being a flotation tailing;

[0044] (4) adjusting the concentration of the flotation underflow obtained in step (3) to 30% to perform magnetic separation by using a high gradient magnetic separator, the background field strength of the high gradient magnetic separator being 0.6 T, and the pulse being 80 r / min, to obtain magnetic material and non-magnetic material, the magnetic material being a magnetic tailing; and the non-magnetic material being concentrated and filtered to obtain a preliminary product of the mineral, and the fine mud tailing, the flotation tailing and the magnetic tailing being combined to be discarded as a tailing;

[0045] (5) placing the preliminary product of the mineral obtained in step (4) in a water bath heating stirrer, adding 1.0% dilute hydrochloric acid, and controlling the water bath heating temperature to be 45℃ under the condition of a liquid-to-solid ratio of 1.5:1, and heating and stirring for 2.5 h, to clean and filter the solid product after leaching, to obtain a mineral powder product.

[0046] The yield of the mineral powder product relative to the dry sample of the mineral is 82.14%, and the content of the -200 mesh particle size is 95.79%.

[0047] The elemental analysis of the preliminary product of the mineral and the final mineral powder product obtained in this example is shown in the following table.

[0048]

[0049] Example 3

[0050] This example provides a method for processing and purifying the mineral, which is performed with reference to the process flow diagram shown in Figure 1 The elemental analysis of the mineral to be processed is as follows:

[0051] Element Fe (wt%) As Pb Cd Hg F Content 1.64 64 mg / Kg 150 mg / Kg 1.5 mg / Kg 1 mg / Kg 1000 mg / Kg

[0052] The processing steps are as follows:

[0053] (1) crushing the mineral in a crusher, and controlling the screening to crush the particle size to -10 mm, and then adding water to adjust the grinding concentration to 62%, and grinding the mineral to a particle size of -0.075 mm accounting for 97.82%, to obtain a grinding slurry;

[0054] (2) diluting the grinding slurry to a mass percentage concentration of 20% by using clean water, and then removing -10 μm fine mud by using a hydrocyclone, to obtain -10 μm fine mud and +10 μm particle size product, the -10 μm fine mud being a fine mud tailing;

[0055] (3) Add clean water to adjust the concentration of the +10 μm particle size product obtained in step (2) to 28%, and then add sodium carbonate and oleic acid in an amount of 200 g and 220 g per ton of the mineral, respectively, to perform one rough separation and one scavenging separation, to obtain a flotation froth and a flotation underflow, wherein the flotation froth is a flotation tailing;

[0056] (4) Adjust the concentration of the flotation underflow obtained in step (3) to 28%, and then perform magnetic separation using a high gradient magnetic separator, wherein the background field strength of the high gradient magnetic separator is 0.7 T, and the pulse is 90 / min, to obtain magnetic material and non-magnetic material, wherein the magnetic material is a magnetic tailing, and the non-magnetic material is concentrated and filtered to obtain a preliminary product of the mineral, and the fine mud tailing, the flotation tailing and the magnetic tailing are combined to be discarded as a tailing;

[0057] (5) Place the preliminary product of the mineral obtained in step (4) in a water bath heating stirrer, add 2.5% dilute hydrochloric acid, control the liquid-solid ratio to be 2.5:1, and control the water bath heating temperature to be 40°C, and heat and stir for 3.0 h, then clean and filter the solid product after leaching to obtain a mineral powder product.

[0058] The yield of the mineral powder product relative to the dry sample of the mineral is 88.54%, and the content of the -200 mesh particle size is 96.84%.

[0059] The elemental analysis of the preliminary product of the mineral and the final mineral powder product obtained in this example is shown in the following table.

[0060]

[0061] Example 4

[0062] This example provides a method for processing and purifying the mineral, which is performed with reference to the process flow diagram shown in Figure 1 The elemental analysis of the mineral is as follows:

[0063] Element Fe (wt%) As Pb Cd Hg F Content 2.41 15 mg / Kg 20 mg / Kg 2.3 mg / Kg 1.5 mg / Kg 1200 mg / Kg

[0064] The processing steps are as follows:

[0065] (1) Crush the mineral in a crusher, and control the screening to break the particle size to -10 mm, then add water to adjust the grinding concentration to 60%, and grind the mineral to a particle size of -0.075 mm accounting for 96.71% to obtain a grinding slurry;

[0066] (2) Dilute the grinding slurry to a mass percentage concentration of 24% using clean water, and then use a hydrocyclone to remove -10 μm fine mud to obtain -10 μm fine mud and +10 μm particle size product, wherein the -10 μm fine mud is a fine mud tailing;

[0067] (3) adding clean water to adjust the concentration of the +10 μm particle size product obtained in step (2) to 35%, then adding sodium carbonate and sodium oleate in turn, the dosages of the agents being 800 g and 300 g per ton of the mineral, respectively, to perform one rough separation of the gangue mineral and one scavenging, to obtain a flotation froth and a flotation underflow, the flotation froth being a flotation tailing;

[0068] (4) adjusting the concentration of the flotation underflow obtained in step (3) to 30% to perform magnetic separation by using a high gradient magnetic separator, the background field strength of the high gradient magnetic separator being 0.6 T, the pulse being 60 r / min, to obtain magnetic material and non-magnetic material, the magnetic material being a magnetic tailing; the non-magnetic material is concentrated and filtered to obtain a preliminary product of the mineral, and the fine mud tailing, the flotation tailing and the magnetic tailing are combined to be discarded as a tailing;

[0069] (5) placing the preliminary product of the mineral obtained in step (4) in a water bath heating stirrer, adding 3.0% dilute hydrochloric acid, controlling the liquid-solid ratio to be 3:1, and controlling the water bath heating temperature to be 45℃, and heating and stirring for 2.5 h, and then cleaning and filtering the solid product after leaching to obtain a mineral powder product.

[0070] The yield of the mineral powder product relative to the dry sample of the mineral is 86.45%, and the content of the -200 mesh particle size is 95.92%.

[0071] The elemental analysis of the preliminary product of the mineral and the final mineral powder product obtained in this example is shown in the following table.

[0072]

[0073]

[0074] Example 5

[0075] This example provides a method for processing and purifying the mineral, which is performed with reference to the process flow diagram shown in Figure 1 The elemental analysis of the mineral to be processed is as follows:

[0076] Element Fe (wt%) As Pb Cd Hg F Content 0.86 8 mg / Kg 180 mg / Kg 1.8 mg / Kg 0.08 mg / Kg 500 mg / Kg

[0077] The processing steps are as follows:

[0078] (1) crushing the mineral in a crusher, and controlling the screening to crush the particle size to -10 mm, then adding water to adjust the grinding concentration to 63%, and grinding the mineral to a particle size of -0.075 mm accounting for 97.54% to obtain a grinding slurry;

[0079] (2) the mass percentage concentration of the ground ore slurry is diluted with clean water to 20%, and then the -10 μm fine mud is removed by using a hydrocyclone, to obtain -10 μm fine mud and +10 μm particle size product, and the -10 μm fine mud is fine mud tailings;

[0080] (3) the +10 μm particle size product obtained in step (2) is adjusted to a concentration of 30% by adding clean water, and then sodium carbonate and oleic acid are added in sequence, and the dosages of the reagents are 400 g and 100 g per ton of the zeolite mineral, respectively, to perform one-time gangue mineral roughing and one-time scavenging, to obtain flotation froth and flotation underflow, and the flotation froth is flotation tailings;

[0081] (4) the flotation underflow obtained in step (3) is adjusted to a slurry concentration of 28%, and then is subjected to magnetic separation by using a high gradient magnetic separator, the background field strength of the high gradient magnetic separator is 1.0 T, and the pulse is 75 r / min, to obtain magnetic material and non-magnetic material, and the magnetic material is magnetic tailings; the non-magnetic material is concentrated and filtered to obtain the zeolite primary product, and the fine mud tailings, the flotation tailings and the magnetic tailings are combined and discarded as tailings;

[0082] (5) the zeolite primary product obtained in step (4) is placed in a water bath heating stirrer, 2.0% dilute hydrochloric acid is added, the liquid-solid ratio is 1.5:1, the water bath heating temperature is controlled to be 45℃, and the heating and stirring is performed for 1.0 h, the leached solid product is cleaned and filtered, and the zeolite powder product is obtained.

[0083] The yield of the zeolite powder product relative to the dry zeolite mineral sample is 90.24%, and the -200 mesh particle size content is 97.19%.

[0084] The elemental analysis of the zeolite primary product obtained in the example and the final zeolite powder product is shown in the following table.

[0085]

[0086] It is shown by the above examples that the method for processing and purifying high-quality zeolite powder provided by the application obtains high-quality zeolite products, and realizes high-value recycling of low-grade zeolite minerals.

Claims

1. A method for processing and purifying maifanite, characterized in that, Including the following steps: S1: Crush the maifanite mineral to -10mm, then add water to prepare a mineral slurry with a mass percentage concentration of 60-65%, and then grind it to a particle size of -0.075mm with a proportion greater than 95% to obtain the grinding slurry; S2: Add water to adjust the grinding slurry to a mass percentage concentration of 20-25%, and use hydraulic classification to remove the -10μm fine mud. The -10μm fine mud obtained is used as fine mud tailings, and the +10μm particle size product enters the next step of processing. S3: The +10μm particle size product is adjusted to a mass percentage concentration of 25-35% by adding water, and then a modifier and a collector are added. A roughing and scavenging process is performed on the gangue minerals to obtain flotation froth and flotation underflow. The flotation froth is used as flotation tailings. The modifier is sodium carbonate, added at a rate of 200-800g per ton of maifanite minerals; the collector is oleic acid or sodium oleate, added at a rate of 100-300g per ton of maifanite minerals. S4: The flotation underflow is adjusted to a mass percentage concentration of 25-30% and then subjected to magnetic separation to obtain magnetic and non-magnetic materials. The magnetic materials are used as magnetic tailings, and the non-magnetic materials are concentrated to obtain maifanite primary product. The magnetic separation is performed using a high-gradient magnetic separator with a background field strength of 0.6-1.0T and a pulse rate of 60-90r / min. S5: The primary product of maifanite is mixed with dilute acid and reacted, with the liquid-solid ratio controlled at (1.5~3):1, to remove impurities. The solid is then collected to obtain the leached product. The leached product is then washed to obtain the maifanite product.

2. The method according to claim 1, characterized in that, In step S2, the sorting equipment used in the hydraulic classification process is a hydraulic classification box or a hydrocyclone.

3. The method according to claim 1, characterized in that, In step S5, the dilute acid is dilute hydrochloric acid with a mass percentage concentration of 1-3%.

4. The method according to claim 3, characterized in that, In step S5, the heating temperature of the reaction is 40~50℃.

5. The method according to any one of claims 1-4, characterized in that, The primary product of maifanite contains 0.05-0.15% Fe by mass, As < 10 mg / Kg, Pb < 15 mg / Kg, Cd < 2 mg / Kg, Hg < 0.1 mg / Kg, and F < 400 mg / Kg; and / or, the maifanite product contains 0.02-0.04% Fe by mass, As 5-8 mg / Kg, Pb 8-12 mg / Kg, Cd 1.2-1.8 mg / Kg, Hg 0.05-0.08 mg / Kg, and F 100-310 mg / Kg.

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