Method for detecting content of tantalum in tantalum pentachloride n-butyl alcohol solution

Abstract

The invention provides a method for detecting the content of tantalum in a tantalum pentachloride n-butyl alcohol solution, which comprises the following steps: S1, taking a proper amount of tantalum pentachloride n-butyl alcohol solution, and putting into a crucible; s2, adding excessive deionized water, stirring, and dropwise adding analytically pure ammonia water until the pH value is 7.0 + / -0.2 to generate tantalum hydroxide precipitate; s3, first-stage high-temperature sintering: carrying out constant-temperature sintering on the tantalum hydroxide precipitate at 280-320 DEG C for 28-32 minutes, and removing volatile organic compounds and moisture; s4, second-stage high-temperature sintering is conducted, specifically, the temperature is increased to 580-620 DEG C, constant-temperature sintering is conducted for 58-63 min, and tantalum hydroxide is completely converted into tantalum pentoxide; and S5, after cooling, weighing the total weight of the crucible, calculating to obtain the net weight of tantalum pentoxide, and calculating to obtain the tantalum content according to the mass fraction of tantalum in tantalum pentoxide. The method for detecting the content of tantalum in the tantalum pentachloride n-butyl alcohol solution has the characteristics of high detection speed, high precision and the like.

Description

Technical Field

[0001] The invention relates to the technical field of chemical analysis, and in particular to a method for detecting the tantalum content in a tantalum pentachloride n-butanol solution. Background Art

[0002] Tantalum compounds are key raw materials in electronic components, corrosion-resistant materials, and other fields, and the accuracy of their content detection directly affects product performance. Traditional methods such as spectrophotometry and inductively coupled plasma ion emission escalation (ICP-OES) are highly equipment-dependent and require complex pre-treatment processes. When detecting high-concentration tantalum solutions, impurity ions interfere significantly, resulting in poor repeatability and increased errors. Existing detection methods based on precipitation conversion suffer from problems such as interference from residual organic matter and unstable conversion rates due to imperfect sintering processes.

[0003] Therefore, it is necessary to develop an efficient, low-cost, and high-precision tantalum content detection method to solve the above technical problems. Summary of the Invention

[0004] The technical problem to be solved by the present invention is to provide a method for detecting the tantalum content in a tantalum pentachloride n-butanol solution, which has the characteristics of fast detection speed, high precision and the like.

[0005] The technical solution of the present invention is:

[0006] A method for detecting the tantalum content in a tantalum pentachloride n-butanol solution comprises the following steps:

[0007] Step S1, taking an appropriate amount of tantalum pentachloride n-butanol solution and placing it in a crucible;

[0008] Step S2, adding excess deionized water, stirring, and then adding analytical grade ammonia dropwise until the pH reaches 7.0±0.2 to generate tantalum hydroxide precipitate;

[0009] Step S3, first stage high temperature sintering: sintering the tantalum hydroxide precipitate at a constant temperature of 280-320°C for 28-32 minutes to remove volatile organic compounds and moisture;

[0010] Step S4, second stage high temperature sintering: heating to 580-620°C and sintering at a constant temperature for 58-63 minutes to completely convert tantalum hydroxide into tantalum pentoxide;

[0011] Step S5: After cooling, weigh the total weight of the crucible to calculate the net weight of tantalum pentoxide, and calculate the tantalum content based on the mass fraction of tantalum in tantalum pentoxide.

[0012] Furthermore, in step S3, the constant temperature sintering temperature is 300° C., and the sintering time is 30 minutes.

[0013] Furthermore, in step S4, the constant temperature sintering temperature is 600° C. and the sintering time is 60 minutes.

[0014] Compared with the prior art, the method for detecting the tantalum content in tantalum pentachloride n-butanol solution provided by the present invention has the following beneficial effects:

[0015] First, the present invention provides a method for detecting the tantalum content in a tantalum pentachloride n-butanol solution. By adjusting the pH during the reaction, the tantalum is completely precipitated as tantalum hydroxide, avoiding co-precipitation of impurities. A two-stage high-temperature sintering process then completely converts the tantalum hydroxide into the highly stable tantalum pentoxide. The tantalum content is then calculated based on a fixed mass fraction of the tantalum pentoxide. This method offers the advantages of simple operation and minimal error, making it suitable for rapid quality control analysis of tantalum solutions in industrial production.

[0016] 2. The method for detecting the tantalum content in the tantalum pentachloride n-butanol solution provided by the present invention does not require the use of expensive equipment such as a spectrometer, and the detection cost is low.

[0017] 3. The method for detecting the tantalum content in tantalum pentachloride n-butanol solution provided by the present invention shortens the sintering temperature to about 90 minutes, thereby improving the detection efficiency.

[0018] 4. In view of the high viscosity of tantalum pentachloride n-butanol solution, this application avoids the problem of uneven precipitation caused by local oversaturation through a specific neutralization rate (such as slow addition of ammonia water). DETAILED DESCRIPTION

[0019] In order to enable those skilled in the art to better understand the technical solutions in the embodiments of the present invention and to make the above-mentioned objects, features and advantages of the present invention more obvious and understandable, the specific implementation methods of the present invention are further described below.

[0020] The endpoints of the ranges and any values disclosed herein are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoints of each range, the endpoints of each range and individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed herein.

[0021] A method for detecting the tantalum content in a tantalum pentachloride n-butanol solution comprises the following steps:

[0022] Step S1: 10 ml of tantalum pentachloride n-butanol solution (concentration of 200 g / L, theoretical tantalum pentachloride content of 2 g) is placed in a crucible with a crucible weight of X g;

[0023] Step S2, adding excess deionized water (>20 ml), stirring, and then adding analytical grade ammonia dropwise until the pH reaches 7.0±0.2 to form tantalum hydroxide precipitate;

[0024] Step S3, first stage high temperature sintering: sintering the tantalum hydroxide precipitate at a constant temperature of 300°C for 30 minutes to remove volatile organic compounds and moisture;

[0025] Step S4, second stage high temperature sintering: heating to 600°C and sintering at a constant temperature for 60 minutes to completely convert tantalum hydroxide into tantalum pentoxide;

[0026] Step S5: After cooling, weigh the total weight of the crucible Yg, and calculate the net weight of tantalum pentoxide = Yg-Xg (the theoretical amount of tantalum pentoxide is 1.23g). In this embodiment, the measured weight of tantalum pentoxide is 1.222g.

[0027] From this, we can see that the measured tantalum pentoxide content deviates from the theoretical value by only 0.008g, indicating high measurement accuracy. The actual tantalum content can then be calculated based on the mass fraction of tantalum in tantalum pentoxide.

[0028] Example 1

[0029] A method for rapidly detecting the tantalum content in a tantalum pentachloride n-butanol solution comprises the following steps:

[0030] Step S1: 10 ml of tantalum pentachloride n-butanol solution (concentration of 200 g / L, theoretical tantalum pentachloride content of 2 g) is placed in a crucible weighing 70.905 g.

[0031] Step S2, adding 25 ml of deionized water, stirring, and then adding analytical grade ammonia dropwise until the pH reaches 7.0±0.2 to generate tantalum hydroxide precipitate;

[0032] Step S3, first stage high temperature sintering: sintering the tantalum hydroxide precipitate at a constant temperature of 300°C for 30 minutes to remove volatile organic compounds and moisture;

[0033] Step S4, second stage high temperature sintering: heating to 600°C and sintering at a constant temperature for 60 minutes to completely convert tantalum hydroxide into tantalum pentoxide;

[0034] Step S5: After cooling, the total weight of the crucible is weighed to 72.127 g, and the net weight of tantalum pentoxide is calculated to be 1.222 g (the theoretical amount of tantalum pentoxide is 1.23 g). In this embodiment, the actual measured mass of tantalum pentoxide is 1.222 g.

[0035] Example 2

[0036] A method for rapidly detecting the tantalum content in a tantalum pentachloride n-butanol solution comprises the following steps:

[0037] Step S1: 10 ml of tantalum pentachloride n-butanol solution (concentration of 200 g / L, theoretical tantalum pentachloride content of 2 g) is placed in a crucible weighing 37.624 g.

[0038] Step S2, adding 25 ml of deionized water, stirring, and then adding analytical grade ammonia dropwise until the pH reaches 7.0±0.2 to generate tantalum hydroxide precipitate;

[0039] Step S3, first stage high temperature sintering: sintering the tantalum hydroxide precipitate at 300°C for 30 minutes to remove volatile organic compounds and moisture;

[0040] Step S4, second stage high temperature sintering: heating to 600°C and sintering at a constant temperature for 60 minutes to completely convert tantalum hydroxide into tantalum pentoxide;

[0041] Step S5: After cooling, the total weight of the crucible is weighed to 38.845 g, and the net weight of tantalum pentoxide is calculated to be 1.221 g (the theoretical amount of tantalum pentoxide is 1.23 g). In this embodiment, the actual measured mass of tantalum pentoxide is 1.221 g.

[0042] Example 3

[0043] A method for rapidly detecting the tantalum content in a tantalum pentachloride n-butanol solution comprises the following steps:

[0044] Step S1: 10 ml of tantalum pentachloride n-butanol solution (concentration of 200 g / L, theoretical tantalum pentachloride content of 2 g) is placed in a crucible. The crucible weighs 42.066 g.

[0045] Step S2, adding 25 ml of deionized water, stirring, and then adding analytical grade ammonia dropwise until the pH reaches 7.0±0.2 to generate tantalum hydroxide precipitate;

[0046] Step S3, first stage high temperature sintering: sintering the tantalum hydroxide precipitate at 300°C for 30 minutes to remove volatile organic compounds and moisture;

[0047] Step S4, second stage high temperature sintering: heating to 600°C and sintering at a constant temperature for 60 minutes to completely convert tantalum hydroxide into tantalum pentoxide;

[0048] Step S5: After cooling, the total weight of the crucible is weighed to 43.287 g, and the net weight of tantalum pentoxide is calculated to be 1.221 g (the theoretical amount of tantalum pentoxide is 1.23 g). In this embodiment, the actual measured mass of tantalum pentoxide is 1.221 g.

[0049] Example 4

[0050] A method for rapidly detecting the tantalum content in a tantalum pentachloride n-butanol solution comprises the following steps:

[0051] Step S1: 10 ml of tantalum pentachloride n-butanol solution (concentration of 200 g / L, theoretical tantalum pentachloride content of 2 g) is placed in a crucible weighing 45.412 g.

[0052] Step S2, adding 25 ml of deionized water, stirring, and then adding analytical grade ammonia dropwise until the pH reaches 7.0±0.2 to generate tantalum hydroxide precipitate;

[0053] Step S3, first stage high temperature sintering: sintering the tantalum hydroxide precipitate at 300°C for 30 minutes to remove volatile organic compounds and moisture;

[0054] Step S4, second stage high temperature sintering: heating to 600°C and sintering at a constant temperature for 60 minutes to completely convert tantalum hydroxide into tantalum pentoxide;

[0055] Step S5: After cooling, the total weight of the crucible is weighed to 46.634 g, and the net weight of tantalum pentoxide is calculated to be 1.222 g (the theoretical amount of tantalum pentoxide is 1.23 g). In this embodiment, the actual measured mass of tantalum pentoxide is 1.222 g.

[0056] Example 5

[0057] A method for rapidly detecting the tantalum content in a tantalum pentachloride n-butanol solution comprises the following steps:

[0058] Step S1: 10 ml of tantalum pentachloride n-butanol solution (concentration of 200 g / L, theoretical tantalum pentachloride content of 2 g) is placed in a crucible. The crucible weighs 42.719 g.

[0059] Step S2, adding 25 ml of deionized water, stirring, and then adding analytical grade ammonia dropwise until the pH reaches 7.0±0.2 to generate tantalum hydroxide precipitate;

[0060] Step S3, first stage high temperature sintering: sintering the tantalum hydroxide precipitate at 300°C for 30 minutes to remove volatile organic compounds and moisture;

[0061] Step S4, second stage high temperature sintering: heating to 600°C and sintering at a constant temperature for 60 minutes to completely convert tantalum hydroxide into tantalum pentoxide;

[0062] Step S5: After cooling, the total weight of the crucible is weighed to 43.944 g, and the net weight of tantalum pentoxide is calculated to be 1.225 g (the theoretical amount of tantalum pentoxide is 1.23 g). In this embodiment, the actual measured mass of tantalum pentoxide is 1.225 g.

[0063] Temperature and time will affect the rate of the hydrolysis reaction and the purity of the product. Higher temperatures may speed up the reaction rate, but too high a temperature may cause the precipitate to decompose or cause side reactions. Too short a time may result in incomplete reaction, and too long a time may cause the precipitate to dissolve or adsorb impurities. After experimental analysis, it was found that when the temperature was 60-80°C and the time was 30-60 minutes, the conversion rate reached the highest and the purity of the precipitate was good. When the temperature exceeded 80°C, the precipitate began to decompose, resulting in a decrease in yield; below 60°C, the reaction rate was slow, and it took longer to achieve the same conversion rate. Similarly, a time of more than 60 minutes may not significantly increase the yield, but may instead cause a decrease in yield due to the dissolution of the precipitate.

[0064] This method improves anti-interference capabilities in complex systems with high chloride ion concentrations and residual organic solvents by using ammonia to control pH and a masking agent (ammonia) to suppress Cl- interference, followed by high-temperature drying to remove organic matter. Reliable results are achieved with recoveries >96% and RSDs <1.2%. This method provides technical support for the quality control of high-purity tantalum compounds.

[0065] The core principle of gravimetric determination of tantalum content in n-butanol solutions of tantalum pentachloride (TaCl₅) is hydrolysis precipitation followed by weighing and quantification. This universality can be extended to other tantalum compounds (such as ethanolic solutions of tantalum pentachloride) through the following strategy, ensuring accuracy. Tantalum chlorides (such as TaCl₅) hydrolyze in aqueous solution to form a hydroxide precipitate. Regardless of whether the solvent is n-butanol, ethanol, or another organic solvent, the nature of the hydrolysis reaction is determined by the H⁺ concentration and temperature, and is independent of the solvent's polarity.

[0066] The purity of tantalum hydroxide (Ta(OH)5) precipitation depends on: Cl-residual control: inhibiting Cl- coordination through pH adjustment and masking agents (such as ammonia). Organic matter removal: removing solvent residues through hot washing and heating volatilization.

[0067] This protocol is universal and applicable to tantalum systems containing various organic solvents. It is cost-effective, requiring no complex equipment and suitable for batch testing. Its high reliability meets the needs of industrial quality control. This method provides a standardized analytical solution for tantalum compound production, waste treatment, and resource recovery.

[0068] The embodiments of the present invention are described in detail above, but the present invention is not limited to the described embodiments. It is apparent to those skilled in the art that various changes, modifications, substitutions, and variations made to these embodiments without departing from the principles and spirit of the present invention are still within the scope of protection of the present invention.

Claims

1. A method for detecting the tantalum content in tantalum pentachloride n-butanol solution, characterized in that: The steps include: Step S1, taking an appropriate amount of tantalum pentachloride n-butanol solution and placing it in a crucible; Step S2, adding excess deionized water, stirring, and then adding analytical grade ammonia dropwise until the pH reaches 7.0±0.2 to generate tantalum hydroxide precipitate, with the ammonia dropwise acceleration rate ≤10 ml / min; Step S3, first stage high temperature sintering: sintering the tantalum hydroxide precipitate at a constant temperature of 280-320°C for 28-32 minutes to remove volatile organic compounds and moisture; Step S4, second stage high temperature sintering: heating to 580-620°C and sintering at a constant temperature for 58-63 minutes to completely convert tantalum hydroxide into tantalum pentoxide; Step S5: After cooling, weigh the total weight of the crucible to calculate the net weight of tantalum pentoxide, and calculate the tantalum content based on the mass fraction of tantalum in tantalum pentoxide.

2. The method for detecting tantalum content in tantalum pentachloride n-butanol solution according to claim 1, characterized in that: In step S3, the constant temperature sintering temperature is 300° C. and the sintering time is 30 minutes.

3. The method for detecting tantalum content in tantalum pentachloride n-butanol solution according to claim 1, characterized in that: In step S4, the constant temperature sintering temperature is 600° C. and the sintering time is 60 minutes.