A method for accurately detecting barium

By combining the melting-cooling-leaching-filtration method with modified stearic acid and pre-treated carbon nanotubes and other raw materials, the problems of limited detection range and high cost of barium in tungsten concentrate were solved, and barium detection with higher accuracy and efficiency was achieved.

CN115639099BActive Publication Date: 2025-09-09HUNAN SHIZHUYUAN NON FERROUS METAL
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Patent Information

Application Number
CN202211433949.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-11-16
Publication Date
2025-09-09
Estimated Expiration
2042-11-16

AI Technical Summary

Technical Problem

The existing technology for detecting the barium content in tungsten concentrate has problems such as limited detection range, high cost and inaccuracy, especially since the barium content has a significant impact during the flotation process.

Method used

The melting-cooling-leaching-filtration method is adopted, combined with the addition of modified stearic acid to anhydrous sodium carbonate. The modified stearic acid is modified by adding pretreated carbon nanotubes, nano-silica and other raw materials to the stearic acid to enhance the detection accuracy and efficiency.

Benefits of technology

The accuracy and efficiency of barium detection are improved, the detection cost is reduced, and the impact of the flotation process on the barium content is reduced.

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Abstract

The present invention discloses a method for accurately detecting barium, comprising the following steps: weighing 0.5g of a sample, adding 3g of sodium peroxide, covering the sample with 2g of anhydrous sodium carbonate, melting, cooling, leaching, and filtering, rinsing with hydrochloric acid, precipitating the sample in a beaker, filtering, and rinsing the filter paper with hot water. The method utilizes melting, cooling, leaching, and filtering techniques, combined with the addition of modified stearic acid to the anhydrous sodium carbonate. The modified stearic acid is modified by adding pretreated carbon nanotubes, nanosilica, and other raw materials to the stearic acid. Practical experiments have shown that the combination of these raw materials produces a synergistic enhancement effect, enhancing the accuracy and efficiency of barium detection.
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Description

Technical Field

[0001] The present invention relates to the technical field of barium detection, and in particular to a method for accurately detecting barium. Background Art

[0002] If the barium content in tungsten concentrate is too high, it will affect the production of downstream tungsten products and increase production costs. The current method for determining the barium content in tungsten concentrate is ICP determination. In existing ICP testing, a relatively accurate result can only be given within the range of the ICP instrument curve. This method can only predict the approximate content of barium in tungsten concentrate and is too expensive for instrument testing. Although the gravimetric method has a long analysis time, it has a wider detection range and high accuracy. It is not affected by the barium content of the ore during the flotation process. Summary of the Invention

[0003] In view of the defects of the prior art, the purpose of the present invention is to provide a method for accurately detecting barium to solve the problems raised in the above background technology.

[0004] The present invention solves the technical problem by adopting the following technical solutions:

[0005] The present invention provides a method for accurately detecting barium, comprising the following steps:

[0006] Weigh 0.5g of sample and add 3g of sodium peroxide, cover the surface with 2g of anhydrous sodium carbonate, melt-cool-leach-filter, rinse with hydrochloric acid, precipitate in the original beaker, filter, rinse the filter paper with hot water, repeatedly adjust the pH value of the filtrate appropriately during this filtration process, add ammonium sulfate and boil, precipitate for 8 hours and then filter, rinse the filter paper, remove it and place it in a corundum crucible for ashing, cooling and weighing.

[0007] Preferably, the surface covering 2g of anhydrous sodium carbonate is further added with modified stearic acid accounting for 5-10% of the total amount of anhydrous sodium carbonate.

[0008] Preferably, the modification method of the modified stearic acid is:

[0009] Stearic acid is added to 2-3 times of sodium alginate solution, and then 5-10% of pretreated carbon nanotubes and 1-5% of nano-silicon dioxide are added to the sodium alginate solution, stirred evenly, and finally hydrochloric acid is added to adjust the pH to 4.5-5.5, stirred evenly, and finally washed with water and dried to obtain modified stearic acid.

[0010] Preferably, the mass fraction of the sodium alginate solution is 10-20%.

[0011] Preferably, the preparation method of the pretreated carbon nanotubes is:

[0012] The carbon nanotubes are added into 2-3 times hydrochloric acid solution, followed by adding 2-5% silane coupling agent and 1-4% silica sol based on the total amount of the carbon nanotubes, stirring thoroughly, and finally washing with water and drying to obtain pretreated carbon nanotubes.

[0013] Preferably, the mass fraction of the hydrochloric acid solution is 5-10%.

[0014] Preferably, modified lanthanum oxide is added in an amount of 5-10% of the total amount of ammonium sulfate during the boiling of ammonium sulfate.

[0015] Preferably, the preparation method of the modified lanthanum oxide is:

[0016] Place lanthanum oxide in 3-5 times the volume of hydrogen peroxide and allow to stand for 1-3 hours at a temperature of 60-70°C, then wash and dry.

[0017] Then add it into 3-5 times of deionized water and stir evenly, add hydrochloric acid to adjust the pH to 5.0, stir and mix thoroughly, and finally wash with water and dry to obtain modified lanthanum oxide.

[0018] Preferably, the particle size of the lanthanum oxide is 10-20 mesh.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] The method for accurately detecting barium of the present invention adopts the technical methods of melting-cooling-leaching-filtration, etc., in combination with adding modified stearic acid to anhydrous sodium carbonate, and the modified stearic acid is modified by adding pretreated carbon nanotubes, nano-silica and other raw materials to the stearic acid. After actual operation, it is found that the combination of the raw materials has a synergistic enhancement effect, thereby enhancing the accuracy and efficiency of detecting barium. DETAILED DESCRIPTION

[0021] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0022] A method for accurately detecting barium in this embodiment includes the following steps:

[0023] Weigh 0.5g of sample and add 3g of sodium peroxide, cover the surface with 2g of anhydrous sodium carbonate, melt-cool-leach-filter, rinse with hydrochloric acid, precipitate in the original beaker, filter, rinse the filter paper with hot water, repeatedly adjust the pH value of the filtrate appropriately during this filtration process, add ammonium sulfate and boil, precipitate for 8 hours and then filter, rinse the filter paper, remove it and place it in a corundum crucible for ashing, cooling and weighing.

[0024] In this embodiment, the surface is covered with 2g of anhydrous sodium carbonate and modified stearic acid is added to the anhydrous sodium carbonate content of 5-10%.

[0025] The modification method of the modified stearic acid of the present embodiment is:

[0026] Stearic acid is added to 2-3 times of sodium alginate solution, and then 5-10% of pretreated carbon nanotubes and 1-5% of nano-silicon dioxide are added to the sodium alginate solution, stirred evenly, and finally hydrochloric acid is added to adjust the pH to 4.5-5.5, stirred evenly, and finally washed with water and dried to obtain modified stearic acid.

[0027] The mass fraction of the sodium alginate solution in this embodiment is 10-20%.

[0028] The preparation method of the pretreated carbon nanotubes in this embodiment is as follows:

[0029] The carbon nanotubes are added into 2-3 times hydrochloric acid solution, followed by adding 2-5% silane coupling agent and 1-4% silica sol based on the total amount of the carbon nanotubes, stirring thoroughly, and finally washing with water and drying to obtain pretreated carbon nanotubes.

[0030] The mass fraction of the hydrochloric acid solution in this embodiment is 5-10%.

[0031] In the present embodiment, modified lanthanum oxide is added during the boiling of ammonium sulfate, which accounts for 5-10% of the total amount of ammonium sulfate.

[0032] The preparation method of the modified lanthanum oxide of this embodiment is:

[0033] Place lanthanum oxide in 3-5 times the volume of hydrogen peroxide and allow to stand for 1-3 hours at a temperature of 60-70°C, then wash and dry.

[0034] Then add it into 3-5 times of deionized water and stir evenly, add hydrochloric acid to adjust the pH to 5.0, stir and mix thoroughly, and finally wash with water and dry to obtain modified lanthanum oxide.

[0035] The particle size of the lanthanum oxide in this embodiment is 10-20 mesh.

[0036] Example 1.

[0037] A method for accurately detecting barium in this embodiment includes the following steps:

[0038] Weigh 0.5g of sample and add 3g of sodium peroxide, cover the surface with 2g of anhydrous sodium carbonate, melt-cool-leach-filter, rinse with hydrochloric acid, precipitate in the original beaker, filter, rinse the filter paper with hot water, repeatedly adjust the pH value of the filtrate appropriately during this filtration process, add ammonium sulfate and boil, precipitate for 8 hours and then filter, rinse the filter paper, remove it and place it in a corundum crucible for ashing, cooling and weighing.

[0039] In this embodiment, the surface is covered with 2g of anhydrous sodium carbonate and modified stearic acid is added to the anhydrous sodium carbonate content of 5-10%.

[0040] The modification method of the modified stearic acid of the present embodiment is:

[0041] Stearic acid is added to 2 times sodium alginate solution, and then 5% pretreated carbon nanotubes and 1% nano-silica are added to the sodium alginate solution, stirred evenly, and finally hydrochloric acid is added to adjust the pH to 4.5, stirred evenly, and finally washed with water and dried to obtain modified stearic acid.

[0042] The mass fraction of the sodium alginate solution in this embodiment is 10%.

[0043] The preparation method of the pretreated carbon nanotubes in this embodiment is as follows:

[0044] The carbon nanotubes were added into a 2-fold hydrochloric acid solution, followed by adding 2% of the total amount of the carbon nanotubes and 1% of silica sol, stirring thoroughly, and finally washing with water and drying to obtain pretreated carbon nanotubes.

[0045] The mass fraction of the hydrochloric acid solution in this embodiment is 5%.

[0046] In the present embodiment, modified lanthanum oxide was added during the boiling of ammonium sulfate, which was 5% of the total amount of ammonium sulfate.

[0047] The preparation method of the modified lanthanum oxide of this embodiment is:

[0048] Place lanthanum oxide in 3 times hydrogen peroxide solution and let it stand for 1 hour at a temperature of 60°C, then wash and dry;

[0049] Then add it into 3 times the amount of deionized water and stir evenly, add hydrochloric acid to adjust the pH to 5.0, stir and mix thoroughly, and finally wash with water and dry to obtain modified lanthanum oxide.

[0050] The particle size of the lanthanum oxide in this embodiment is 10 mesh.

[0051] Example 2.

[0052] A method for accurately detecting barium in this embodiment includes the following steps:

[0053] Weigh 0.5g of sample and add 3g of sodium peroxide, cover the surface with 2g of anhydrous sodium carbonate, melt-cool-leach-filter, rinse with hydrochloric acid, precipitate in the original beaker, filter, rinse the filter paper with hot water, repeatedly adjust the pH value of the filtrate appropriately during this filtration process, add ammonium sulfate and boil, precipitate for 8 hours and then filter, rinse the filter paper, remove it and place it in a corundum crucible for ashing, cooling and weighing.

[0054] In this embodiment, the surface is covered with 2 g of anhydrous sodium carbonate to which modified stearic acid is added, which accounts for 10% of the total amount of anhydrous sodium carbonate.

[0055] The modification method of the modified stearic acid of the present embodiment is:

[0056] Stearic acid is added to 3 times sodium alginate solution, and then 10% pretreated carbon nanotubes and 5% nano-silica are added to the sodium alginate solution, stirred evenly, and finally hydrochloric acid is added to adjust the pH to 5.5, stirred evenly, and finally washed with water and dried to obtain modified stearic acid.

[0057] The mass fraction of the sodium alginate solution in this embodiment is 20%.

[0058] The preparation method of the pretreated carbon nanotubes in this embodiment is as follows:

[0059] The carbon nanotubes were added into a 3-fold hydrochloric acid solution, followed by adding 5% of the total amount of the carbon nanotubes and 4% of silica sol, stirring thoroughly, and finally washing with water and drying to obtain pretreated carbon nanotubes.

[0060] The mass fraction of the hydrochloric acid solution in this embodiment is 10%.

[0061] In the present embodiment, modified lanthanum oxide accounting for 10% of the total amount of ammonium sulfate was added during the boiling of ammonium sulfate.

[0062] The preparation method of the modified lanthanum oxide of this embodiment is:

[0063] Place lanthanum oxide in 5 times hydrogen peroxide solution and let it stand for 3 hours at a temperature of 70°C, then wash and dry;

[0064] Then add it into 5 times the amount of deionized water and stir evenly, add hydrochloric acid to adjust the pH to 5.0, stir and mix thoroughly, and finally wash with water and dry to obtain modified lanthanum oxide.

[0065] The particle size of the lanthanum oxide in this embodiment is 20 mesh.

[0066] Example 3.

[0067] A method for accurately detecting barium in this embodiment includes the following steps:

[0068] Weigh 0.5g of sample and add 3g of sodium peroxide, cover the surface with 2g of anhydrous sodium carbonate, melt-cool-leach-filter, rinse with hydrochloric acid, precipitate in the original beaker, filter, rinse the filter paper with hot water, repeatedly adjust the pH value of the filtrate appropriately during this filtration process, add ammonium sulfate and boil, precipitate for 8 hours and then filter, rinse the filter paper, remove it and place it in a corundum crucible for ashing, cooling and weighing.

[0069] In this embodiment, the surface is covered with 2g of anhydrous sodium carbonate and modified stearic acid is added to the anhydrous sodium carbonate content of 5-10%.

[0070] The modification method of the modified stearic acid of the present embodiment is:

[0071] Stearic acid is added to 3 times sodium alginate solution, and then 7.5% pretreated carbon nanotubes and 3% nano-silica are added to the sodium alginate solution, stirred evenly, and finally hydrochloric acid is added to adjust the pH to 5.0, stirred evenly, and finally washed with water and dried to obtain modified stearic acid.

[0072] The mass fraction of the sodium alginate solution in this embodiment is 15%.

[0073] The preparation method of the pretreated carbon nanotubes in this embodiment is as follows:

[0074] The carbon nanotubes were added into a 3-fold hydrochloric acid solution, followed by the addition of 3% silane coupling agent and 2% silica sol based on the total amount of the carbon nanotubes, and the mixture was stirred thoroughly. Finally, the mixture was washed with water and dried to obtain pretreated carbon nanotubes.

[0075] The mass fraction of the hydrochloric acid solution in this embodiment is 6%.

[0076] In the present embodiment, modified lanthanum oxide was added during the boiling of ammonium sulfate, accounting for 7.5% of the total amount of ammonium sulfate.

[0077] The preparation method of the modified lanthanum oxide of this embodiment is:

[0078] Place lanthanum oxide in 4 times hydrogen peroxide solution and let it stand for 2 hours at a temperature of 65°C, then wash and dry;

[0079] Then add it into 4 times the amount of deionized water and stir evenly, add hydrochloric acid to adjust the pH to 5.0, stir and mix thoroughly, and finally wash with water and dry to obtain modified lanthanum oxide.

[0080] The particle size of the lanthanum oxide in this embodiment is 15 mesh.

[0081] Example 4.

[0082] A method for accurately detecting barium in this embodiment includes the following steps:

[0083] Weigh 0.5g of sample and add 3g of sodium peroxide, cover the surface with 2g of anhydrous sodium carbonate, melt-cool-leach-filter, rinse with hydrochloric acid, precipitate in the original beaker, filter, rinse the filter paper with hot water, repeatedly adjust the pH value of the filtrate appropriately during this filtration process, add ammonium sulfate and boil, precipitate for 8 hours and then filter, rinse the filter paper, remove it and place it in a corundum crucible for ashing, cooling and weighing.

[0084] In this embodiment, the surface is covered with 2g of anhydrous sodium carbonate and modified stearic acid is added to the anhydrous sodium carbonate content of 5-10%.

[0085] The modification method of the modified stearic acid of the present embodiment is:

[0086] Stearic acid is added to 2 times sodium alginate solution, and then 6% pretreated carbon nanotubes and 2% nano-silica are added to the sodium alginate solution, stirred evenly, and finally hydrochloric acid is added to adjust the pH to 4.5, stirred evenly, and finally washed with water and dried to obtain modified stearic acid.

[0087] The mass fraction of the sodium alginate solution in this embodiment is 15%.

[0088] The preparation method of the pretreated carbon nanotubes in this embodiment is as follows:

[0089] The carbon nanotubes were added into a 3-fold hydrochloric acid solution, followed by the addition of 3% silane coupling agent and 2% silica sol based on the total amount of the carbon nanotubes, and the mixture was stirred thoroughly. Finally, the mixture was washed with water and dried to obtain pretreated carbon nanotubes.

[0090] The mass fraction of the hydrochloric acid solution in this embodiment is 6%.

[0091] In the present embodiment, modified lanthanum oxide accounting for 6% of the total amount of ammonium sulfate was added during the boiling of ammonium sulfate.

[0092] The preparation method of the modified lanthanum oxide of this embodiment is:

[0093] Place lanthanum oxide in 4 times hydrogen peroxide solution and let it stand for 2 hours at a temperature of 65°C, then wash and dry;

[0094] Then add it into 4 times the amount of deionized water and stir evenly, add hydrochloric acid to adjust the pH to 5.0, stir and mix thoroughly, and finally wash with water and dry to obtain modified lanthanum oxide.

[0095] The particle size of the lanthanum oxide in this embodiment is 15 mesh.

[0096] Example 5.

[0097] A method for accurately detecting barium in this embodiment includes the following steps:

[0098] Weigh 0.5g of sample and add 3g of sodium peroxide, cover the surface with 2g of anhydrous sodium carbonate, melt-cool-leach-filter, rinse with hydrochloric acid, precipitate in the original beaker, filter, rinse the filter paper with hot water, repeatedly adjust the pH value of the filtrate appropriately during this filtration process, add ammonium sulfate and boil, precipitate for 8 hours and then filter, rinse the filter paper, remove it and place it in a corundum crucible for ashing, cooling and weighing.

[0099] In this embodiment, the surface is covered with 2g of anhydrous sodium carbonate and modified stearic acid is added to the anhydrous sodium carbonate content of 5-10%.

[0100] The modification method of the modified stearic acid of the present embodiment is:

[0101] Stearic acid is added to 4 times the sodium alginate solution, and then 8% pretreated carbon nanotubes and 4% nano-silica are added to the sodium alginate solution, stirred evenly, and finally hydrochloric acid is added to adjust the pH to 5.4, stirred evenly, and finally washed with water and dried to obtain modified stearic acid.

[0102] The mass fraction of the sodium alginate solution in this embodiment is 17%.

[0103] The preparation method of the pretreated carbon nanotubes in this embodiment is as follows:

[0104] The carbon nanotubes were added into a 3-fold hydrochloric acid solution, followed by adding 5% of the total amount of the carbon nanotubes and 4% of silica sol, stirring thoroughly, and finally washing with water and drying to obtain pretreated carbon nanotubes.

[0105] The mass fraction of the hydrochloric acid solution in this embodiment is 8%.

[0106] In the present embodiment, modified lanthanum oxide accounting for 9% of the total amount of ammonium sulfate was also added during the boiling of ammonium sulfate.

[0107] The preparation method of the modified lanthanum oxide of this embodiment is:

[0108] Place lanthanum oxide in 4 times hydrogen peroxide solution and let it stand for 2 hours at a temperature of 68°C, then wash and dry;

[0109] Then add it into 4 times the amount of deionized water and stir evenly, add hydrochloric acid to adjust the pH to 5.0, stir and mix thoroughly, and finally wash with water and dry to obtain modified lanthanum oxide.

[0110] The particle size of the lanthanum oxide in this embodiment is 18 mesh.

[0111] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0112] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A method for accurately detecting barium, characterized in that: The following steps are involved: Weigh 0.5g of sample and add 3g of sodium peroxide, cover the surface with 2g of anhydrous sodium carbonate, melt-cool-leach-filter, rinse with hydrochloric acid, precipitate in the original beaker, filter, rinse the filter paper with hot water, and repeatedly adjust the pH value of the filtrate appropriately during filtration; add ammonium sulfate and boil, precipitate for 8 hours and then filter, rinse the filter paper, remove it and place it in a corundum crucible for ashing, cooling and weighing; the anhydrous sodium carbonate is also added with modified stearic acid of 5-10% of the total amount of anhydrous sodium carbonate; the modification method of the modified stearic acid is as follows: Stearic acid is added to 2-3 times of sodium alginate solution, and then 5-10% of pretreated carbon nanotubes and 1-5% of nano-silica are added to the sodium alginate solution, and stirred evenly. Finally, hydrochloric acid is added to adjust the pH to 4.5-5.5, and stirred evenly. Finally, the solution is washed with water and dried to obtain modified stearic acid.

2. A method for accurately detecting barium according to claim 1, characterized in that: The mass fraction of the sodium alginate solution is 10-20%.

3. The method for accurately detecting barium according to claim 1, characterized in that: The preparation method of the pretreated carbon nanotubes is as follows: Add carbon nanotubes to 2-3 times hydrochloric acid solution, then add 2-5% silane coupling agent and 1-4% silica sol based on the total amount of carbon nanotubes, stir thoroughly, wash with water and dry to obtain pretreated carbon nanotubes.

4. A method for accurately detecting barium according to claim 3, characterized in that: The mass fraction of the hydrochloric acid solution is 5-10%.

5. The method for accurately detecting barium according to claim 1, characterized in that: During the boiling of ammonium sulfate, modified lanthanum oxide is added in an amount of 5-10% of the total amount of ammonium sulfate.

6. A method for accurately detecting barium according to claim 5, characterized in that: The preparation method of the modified lanthanum oxide is: Place lanthanum oxide in 3-5 times the volume of hydrogen peroxide and allow to stand for 1-3 hours at a temperature of 60-70°C, then wash and dry. Then add it into 3-5 times of deionized water and stir evenly, add hydrochloric acid to adjust the pH to 5.0, stir and mix thoroughly, and finally wash with water and dry to obtain modified lanthanum oxide.

7. A method for accurately detecting barium according to claim 6, characterized in that: The particle size of the lanthanum oxide is 10-20 meshes.

Citation Information

Patent Citations

  • Method and system for determining content of barium element in tungsten ore

    CN103308412A