Method for determining silicon dioxide content in copper smelting tailings by alkali fusion combined with ICP-OES

Abstract

The invention relates to a method for determining the content of silicon dioxide in copper smelting tailings by combining alkali melting with ICP-OES method, and belongs to the technical field of determining the content of silicon dioxide in copper smelting tailings. The method comprises the following specific steps: S1, alkali melting treatment: selecting 1-3g of a sample with a particle size not greater than 100mm, drying the sample at 100-105°C for 1h, placing the sample in a dryer and cooling it to room temperature, then placing the sample in a 30mL nickel crucible pre-added with 2g of potassium hydroxide, adding 2g-3g of sodium peroxide, placing the nickel crucible containing the sample in a muffle furnace at 700°C for 15-20min, and taking it out for cooling; S2, mixing: moving the nickel crucible into a 400ml plastic beaker, adding 10mL of 80°C hot water, covering it with a watch glass, and after the melt is reacted, pouring the reactant in the crucible into the plastic beaker, and dripping 6-8g of digestion solution drop by drop along the wall of the crucible. By combining alkali melting treatment with ICP-OES detection, rapid detection is achieved, energy consumption and chemical reagent consumption are reduced, operation is simple, and the recovery rate of copper smelting tailings is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of determination of silicon dioxide content in copper smelting tailings, and specifically relates to a method for determining the silicon dioxide content in copper smelting tailings by alkali fusion combined with ICP-OES method. Background Art

[0002] Copper smelting tailings are by-products of copper smelting. They contain a variety of metal and non-metal elements, among which silicon is an important component. Accurate detection of silicon content is of great significance for resource utilization of copper smelting tailings, environmental protection and optimization of smelting processes. The physical and chemical properties of copper smelting tailings are complex, and comprehensive treatment is usually required to achieve resource utilization. In the process of resource utilization, accurate detection of silicon content is one of the key links, which directly affects the selection of subsequent treatment processes and resource recovery efficiency.

[0003] At present, according to the different silicon contents in copper smelting tailings, the main detection method is chemical titration. Although it can detect the silicon content more accurately, the operation is cumbersome, time-consuming, and requires a large amount of chemical reagents, which is not conducive to environmental protection and cost control. In addition, with the continuous development of smelting technology, the composition of copper smelting tailings is becoming more and more complex, and the traditional detection methods are gradually exposed in terms of accuracy and sensitivity. In addition, the existing technology lacks a fast, simple and efficient method for detecting the silicon content in copper smelting tailings, and cannot meet the requirements of industrial production for detection speed and accuracy;

[0004] The determination of silicon dioxide content in conventional copper smelting slag is potassium fluorosilicate titration method. The sample (the sample particle size should not be greater than 100 μm, and the sample should be dried at 100℃~105℃ for 1 hour and then placed in a dryer to cool to room temperature.) is placed in a 30mL nickel crucible with 2g potassium hydroxide added in advance, and 2g~3g sodium peroxide is added. It is heated on a low-temperature electric furnace to evaporate the water until it is fluid and shaken well, and then transferred to a 700℃ muffle furnace to melt for 15 minutes, and then taken out and cooled. The crucible is transferred to a 400ml plastic beaker, 10mL hot water is added, and a watch glass is covered. After the melt is reacted, the reactants in the crucible are poured into the plastic beaker, and a few drops of hydrochloric acid are dripped along the wall of the crucible. The crucible is washed with hot water (the total volume does not exceed 25mL), and 16m~17mL nitric acid is added, mixed, and cooled to room temperature. Add 6 ml potassium fluoride solution and 5 g to 6 g potassium chloride to saturation, shake for 3 min to 5 min, let stand for 10 min to 20 min, use a plastic funnel, filter with medium-speed filter paper, wash the plastic beaker 2 to 3 times with washing liquid (weigh 250 g potassium chloride and dissolve it in 3000 ml of water, add 1000 mL ethanol, dilute to 5000 mL with water, mix well, add 1 ml phenolphthalein ethanol solution, and neutralize with sodium hydroxide solution (2 g / l) until the solution is slightly red.) Wash the precipitate 3 times, put the filter paper and precipitate together in the original plastic beaker, add 10 mL potassium chloride-ethanol solution, add 1 mL phenolphthalein ethanol solution dropwise, neutralize most of the free acid with sodium hydroxide solution, crush the paper, and then neutralize with sodium hydroxide standard titration solution until the solution is light pink. At this time, ignore the consumed volume of sodium hydroxide standard titration solution, add 150 mL boiling potassium sodium tartrate solution, and titrate with sodium hydroxide standard titration solution while hot until the pink color just appears as the end point. The disadvantages are as follows:

[0005] ① The operation is cumbersome and time-consuming: Traditional titration and gravimetric methods involve multiple steps, including sample preparation, melting, dissolution, precipitation, filtration, and titration. The operation is cumbersome because each step requires precise control of temperature, time, and the amount of chemical reagents to ensure the accuracy of the analysis results. In addition, each step requires waiting for the reaction to complete or the solution to cool, which also increases the total processing time. The entire process takes up to 8 hours, and the detection is time-consuming and complicated.

[0006] ② High consumption of chemical reagents: Traditional methods often require a large amount of chemical reagents for sample digestion and determination, which not only increases the detection cost, but may also lead to environmental pollution and waste of resources. For example, although the X-fluorescence method is simple and fast, its instrumentation, standard filter membrane purchase costs, and operating costs are high, making it difficult to popularize.

[0007] ③ Unable to meet the needs of industrial production: Traditional methods usually cannot meet the requirements of industrial production for detection speed and accuracy. Especially in large-scale production, a fast, simple and efficient detection method is needed.

[0008] In contrast, the method of alkali fusion combined with ICP for detecting silicon content proposed in this patent can overcome the defects of the above-mentioned traditional methods. Summary of the invention

[0009] The purpose of the present invention is to provide a method for determining the silicon dioxide content in copper smelting tailings by alkali fusion combined with ICP-OES in order to solve the above problems.

[0010] The present invention achieves the above-mentioned purpose through the following technical solutions:

[0011] The present invention provides a method for determining the content of silicon dioxide in copper smelting tailings by alkali fusion combined with ICP-OES method, and the specific steps are as follows:

[0012] S1. Alkali melting treatment: select 1-3g of sample with a particle size not greater than 100mm, then dry the sample at 100℃~105℃ for 1h, place it in a dryer and cool it to room temperature, then place it in a 30mL nickel crucible pre-added with 2g potassium hydroxide, add 2g~3g sodium peroxide, place the nickel crucible containing the sample in a 700℃ muffle furnace for 15-20min, and take it out to cool;

[0013] S2, mixing: move the nickel crucible into a 400ml plastic beaker, add 10mL of 80℃ hot water, cover with a watch glass, and after the melt has finished reacting, pour the reactants in the crucible into the plastic beaker, and drip 6-8g of digestion solution along the crucible wall drop by drop;

[0014] S3. Detection: The cooled sample was placed in a 250 mL volumetric flask and the silicon content was detected by ICP-OES.

[0015] As a further optimization scheme of the present invention, the digestion solution is nitric acid or hydrochloric acid.

[0016] As a further optimization solution of the present invention, the sample is specifically tailings.

[0017] As a further optimization scheme of the present invention, the ICP-OES is specifically an inductively coupled plasma optical emission spectrometer.

[0018] As a further optimization scheme of the present invention, the working conditions of the ICP-OES are as follows: the ICP-OES RF power is 1200W, the nebulizer pressure is 300Pa, the cooling gas flow rate is 2L·min-1, the auxiliary gas flow rate is 3L·min-1, the peristaltic pump flow rate is 30mL·min-1, the plasma observation mode is vertical, the vertical integration time is 25s, and the number of integrations is 3.

[0019] The beneficial effects of the present invention are as follows: the combination of alkali melting treatment and ICP-OES detection greatly shortens the detection time, making the detection process more concise and efficient, and can quickly complete the silicon content detection of a large number of samples, meeting the rapid detection requirements of industrial production; in addition, the detection method of the present invention reduces energy consumption and chemical reagent consumption, and at the same time, due to the high sensitivity and high accuracy of ICP-OES detection, the number of repeated detections and verifications can be reduced, further reducing the detection cost; and the detection method of the present invention is easy to operate, does not require complex sample pretreatment steps, reduces the difficulty of operation and labor intensity, and more accurately detects the silicon content in copper smelting tailings, which is helpful to optimize the smelting process and tailings utilization plan, improve the recovery rate of copper smelting tailings, and can avoid low utilization rate due to excessively high or low silicon content by accurately controlling the silicon content. DETAILED DESCRIPTION

[0020] The present application is described in further detail below. It is necessary to point out that the following specific implementation methods are only used to further illustrate the present application and cannot be understood as limiting the scope of protection of the present application. Technicians in this field can make some non-essential improvements and adjustments to the present application based on the above application content.

[0021] 1. Materials

[0022] Unless otherwise specified, the methods used in the present invention are conventional methods known to those skilled in the art, and the reagents and other materials used are commercially available products unless otherwise specified.

[0023] (1) The ICP-OES in the present invention specifically adopts the iCAP 7200Duo inductively coupled plasma emission spectrometer produced by Thermo Fisher Scientific. It should be noted that the instrument is used to detect silicon content;

[0024] (2) The main components of the tailings in the present invention include: 41% iron, 28%-35% silicon dioxide, 2.0% zinc, and 0.17% copper. The iron and silicon are mainly in the form of fayalite.

[0025] 2. Methods

[0026] 2.1. The method for determining the content of silicon dioxide in copper smelting tailings by alkali fusion combined with ICP-OES method, the specific steps are as follows:

[0027] S1, alkali melting treatment: select 2g of sample with a particle size of 90mm, then dry the sample at 103℃ for 1h, place it in a desiccator and cool it to room temperature, then place it in a 30mL nickel crucible pre-added with 2g of potassium hydroxide, add 2.5g of sodium peroxide, place the nickel crucible containing the sample in a muffle furnace at 700℃ for 17min, and take it out to cool;

[0028] Among them, the sample is specifically tailings;

[0029] S2, mixing: move the nickel crucible into a 400ml plastic beaker, add 10mL of 80℃ hot water, cover with a watch glass, and after the melt has finished reacting, pour the reactants in the crucible into the plastic beaker, and drip 7g of digestion solution along the crucible wall drop by drop;

[0030] Wherein, the digestion solution is nitric acid;

[0031] S3. Detection: The cooled sample was placed in a 250 mL volumetric flask and the silicon content was detected by ICP-OES.

[0032] Among them, ICP-OES is specifically an inductively coupled plasma optical emission spectrometer, and the working conditions of ICP-OES are as follows:

[0033] The ICP-OES RF power was 1200W, the nebulizer pressure was 300Pa, the cooling gas flow rate was 2L·min-1, the auxiliary gas flow rate was 3L·min-1, the peristaltic pump flow rate was 30mL·min-1, the plasma observation mode was vertical, the vertical integration time was 25s, and the number of integrations was 3.

[0034] Example 1

[0035] The present invention uses ICP-OES as the core detection method, and its high sensitivity and high resolution significantly improve the detection precision and accuracy of silicon content. By precisely controlling the detection conditions, the accuracy and reliability of the test results can be ensured to meet the needs of high-precision detection. Through a large number of experiments on the present invention, it can be found that the silicon dioxide content of the tailings is 28%-35%. By sending 5 groups of samples to the test, and then using potassium fluorosilicate titration and the patented method for comparison, the results are as follows:

[0036] Table 1 Method comparison test results

[0037]

[0038] It can be seen from Table 1 that the results of this method are basically consistent with the results of the external inspection standard and the potassium fluorosilicate titration method, with no significant difference.

[0039] Example 2

[0040] This method was used to determine the silicon dioxide content in different copper smelting slag samples, and precision tests were carried out. The results are shown in Table 2;

[0041] Table 2 Precision test results

[0042]

[0043]

[0044] It can be seen from Table 2 that the results of the determination of the silicon dioxide content in different copper smelting slag samples by this method are stable and highly precise.

[0045] 2.2 Effect of digestion solution on the accuracy of silica content detection

[0046] (1) The method for determining the content of silicon dioxide in copper smelting tailings by alkali fusion combined with ICP-OES is referred to 2.1, wherein the phosphoric acid described in Table 3 is used to replace the nitric acid in Example 1;

[0047] The method of alkaline melting combined with ICP-OES method for determining the silicon dioxide content in copper smelting tailings in Example 3 was used to compare the silicon dioxide content in 5 groups of samples (tailings) with the external inspection standard results and potassium fluorosilicate titration method. The results are shown in Table 4.

[0048] The raw material composition of the digestion solution is shown in the following table (Table 3):

[0049] project Digestion solution Example 1 Nitric acid Example 3 Phosphoric acid

[0050] The following table is: (Table 4) Method comparison test results

[0051]

[0052] It can be seen from Table 4 that, compared with Example 1, the method of determining the silicon dioxide content in copper smelting tailings by alkali fusion combined with ICP-OES method adopted in Example 1 is the best, and the use of phosphoric acid as a digestion solution will affect the accuracy of the detection of the silicon dioxide content in the tailings.

[0053] The above-mentioned embodiments only express several implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the present invention. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention.

Claims

1. A method for determining the content of silicon dioxide in copper smelting tailings by alkali melting combined with ICP-OES, characterized in that: The specific steps are as follows: S1. Alkali melting treatment: select 1-3g of sample with a particle size not greater than 100mm, then dry the sample at 100℃~105℃ for 1h, place it in a dryer and cool it to room temperature, then place it in a 30mL nickel crucible pre-added with 2g potassium hydroxide, add 2g~3g sodium peroxide, place the nickel crucible containing the sample in a 700℃ muffle furnace for 15-20min, and take it out to cool; S2, mixing: move the nickel crucible into a 400ml plastic beaker, add 10mL of 80℃ hot water, cover with a watch glass, and after the melt has finished reacting, pour the reactants in the crucible into the plastic beaker, and drip 6-8g of digestion solution along the crucible wall drop by drop; S3. Detection: The cooled sample was placed in a 250 mL volumetric flask and the silicon content was detected by ICP-OES.

2. The method for determining the content of silicon dioxide in copper smelting tailings by alkali fusion combined with ICP-OES according to claim 1, characterized in that: The digestion solution is nitric acid or hydrochloric acid.

3. The method for determining the content of silicon dioxide in copper smelting tailings by alkali fusion combined with ICP-OES according to claim 1, characterized in that: The sample is specifically tailings.

4. The method for determining the content of silicon dioxide in copper smelting tailings by alkali fusion combined with ICP-OES according to claim 4, characterized in that: The ICP-OES is specifically an inductively coupled plasma optical emission spectrometer.

5. The method for determining the content of silicon dioxide in copper smelting tailings by alkali fusion combined with ICP-OES according to claim 4, characterized in that: The working conditions of the ICP-OES are as follows: The ICP-OES radio frequency power was 1200 W, the atomizer pressure was 300 Pa, and the cooling gas flow rate was 2 L min -1、 The auxiliary gas flow rate is 3 L min -1 , peristaltic pump flow rate is 30mL·min -1 , the plasma observation mode is vertical, the vertical integration time is 25s, and the number of integrations is 3.

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