CN111982890A - Mixed acid for dissolving molybdenum-titanium-nickel alloy and preparation method and application thereof - Google Patents
Mixed acid for dissolving molybdenum-titanium-nickel alloy and preparation method and application thereof Download PDFInfo
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- CN111982890A CN111982890A CN202010808450.9A CN202010808450A CN111982890A CN 111982890 A CN111982890 A CN 111982890A CN 202010808450 A CN202010808450 A CN 202010808450A CN 111982890 A CN111982890 A CN 111982890A
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Abstract
The invention relates to a mixed acid for dissolving molybdenum-titanium-nickel alloy, a preparation method and application thereof, wherein the volume ratio of hydrofluoric acid to nitric acid in the mixed acid is (1.5-2.5): 1; the mass concentration of the hydrofluoric acid is 35-38%; the mass concentration of the nitric acid is 65-68%. The invention realizes the high-efficiency dissolution of the molybdenum-titanium-nickel alloy by reasonably configuring the components and the proportion in the mixed acid, the dissolution time is 20-40min, and the detection standard of the ICP-OES machine is reached.
Description
Technical Field
The invention relates to the field of alloy dissolution, in particular to a mixed acid for dissolving molybdenum-titanium-nickel alloy and a preparation method and application thereof.
Background
The mo-ti-ni alloy is an important alloying metal commonly used in connection with tft-type lcd, and the content of the individual metal is decisive for the relevant properties, so it is necessary to know the content.
An inductively coupled plasma emission spectrometer (ICP-OES) is a common device for testing components of the chromium-tantalum-titanium alloy, interference is little when the inductively coupled plasma emission spectroscopy is applied to test the chromium-tantalum-titanium alloy, a test signal is stable, operation is simple, and the molybdenum-titanium-nickel alloy needs to be dissolved before testing.
CN102944496A discloses a method for detecting the content of molybdenum in ferromolybdenum, which comprises the following steps: A. weighing a ferromolybdenum sample with the mass of m in a beaker, adding nitric acid, heating to dissolve, and adding water; B. filtering the solution, and adjusting the volume of the filtrate to a fixed scale; C. adding EDTA solution into the solution, and adjusting the solution to turn from bright yellow to reddish with ammonium hydroxide; D. adding a buffer solution into the solution, heating the solution to boiling, taking the solution down, dropwise adding 8-hydroxyquinoline solution under full stirring, and standing; E. cooling to room temperature, and then using a constant m2Filtering the glass sand core crucible, washing the beaker with hot water, washing and precipitating for one time, drying the beaker after filtering, standing the beaker, taking the dried beaker out, placing the beaker in a drying cylinder, cooling the beaker to room temperature, and weighing the beaker to a constant volume mL; F. the method has the advantages of simple steps, convenient operation, accuracy, rapidness, high efficiency and low cost, and brings great benefits to enterprises.
CN105548164A discloses a method for measuring titanium in a metallurgical product, which belongs to the technical field of alloy detection, and particularly relates to a method for measuring titanium in a titanium-silicon alloy. The method adopts an acid dissolution method to dissolve a sample, and adopts an ammonium ferric sulfate titration method to determine the content of titanium, so that the method can well meet the determination requirement of the main component titanium content (mass fraction is 30-80%) in the titanium-silicon alloy. The method has the advantages of less interference, high precision, good selectivity, simple and easy operation and high accuracy.
CN102269669A discloses a method for dissolving a nickel-based alloy sample with high Mo content, which comprises the steps of adding aqua regia into a container filled with a weighed nickel-based alloy sample with high Mo content, heating to boil and keeping, wherein reddish brown gas is generated in the container; when the reddish brown gas disappears, the solution is kept boiling, and HNO is added into the solution3Continuously heating to generate red brown gas; when the reddish brown gas disappeared, HCl was added to the solution and heating was continued and the sample was completely dissolved. The method can realize complete dissolution of the sample without using HF acid or other cosolvent for dissolution, and has no toxicity of the HF acid; avoids the corrosion of HF acid to glass,the volumetric parameters of the glass container used for measurement are influenced to different degrees by the corrosion of HF, thereby influencing the accuracy of the detection result.
However, the prior art lacks a molybdenum-titanium-nickel alloy dissolving solution to realize ICP-OES test.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a mixed acid for dissolving molybdenum-titanium-nickel alloy, a preparation method and application thereof, which realize the efficient dissolution of the molybdenum-titanium-nickel alloy, the dissolution time is 20-40min, and the detection standard of ICP-OES on-machine is reached.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a mixed acid for dissolving molybdenum-titanium-nickel alloy, wherein the volume ratio of hydrofluoric acid to nitric acid in the mixed acid is (1.5-2.5): 1;
the mass concentration of the hydrofluoric acid is 35-38%;
the mass concentration of the nitric acid is 65-68%.
The invention realizes the high-efficiency dissolution of the molybdenum-titanium-nickel alloy by reasonably configuring the components and the proportion in the mixed acid, the dissolution time is 20-40min, and the detection standard of the ICP-OES machine is reached.
In the present invention, the volume ratio of hydrofluoric acid to nitric acid in the mixed acid is (1.5-2.5):1, and may be, for example, 1.5:1, 1.7:1, 2:1, 2.2:1 or 2.5:1, but is not limited to the above-mentioned values, and other values not mentioned in the above range are also applicable.
In the present invention, the hydrofluoric acid may be contained in a concentration of 35 to 38% by mass, for example, 35%, 36%, 37%, 38%, etc., but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
In the present invention, the nitric acid may have a mass concentration of 65 to 68%, for example, 65%, 66%, 67%, or 68%, but the nitric acid is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
In a preferable technical scheme of the invention, the volume ratio of hydrofluoric acid to nitric acid in the mixed acid is (1.8-2): 1.
In a preferred embodiment of the present invention, the hydrofluoric acid has a concentration of 36 to 37% by mass.
In a preferred embodiment of the present invention, the mass concentration of the nitric acid is 66 to 67%.
In a second aspect, the present invention provides a method for producing the mixed acid according to the first aspect, the method comprising: mixing hydrofluoric acid and nitric acid according to the volume ratio of (1.5-2.5) to 1 to obtain the mixed acid.
In a third aspect, the present invention provides the use of a mixed acid as described in the first aspect, said use comprising the steps of: mixing and heating the molybdenum-titanium-nickel alloy and the mixed acid to obtain a solution in which molybdenum, titanium and nickel are dissolved;
the molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 14.97 to 15.3 percent of Ni, 8.93 to 9.15 percent of Ti and the balance of molybdenum.
In the present invention, the content of Ni in the molybdenum-titanium-nickel alloy is 14.97 to 15.3% by mass, and may be, for example, 14.97%, 15%, 15.1%, 15.2%, or 15.3%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
In the present invention, the content of Ti in the molybdenum titanium nickel alloy is 8.93 to 9.15% by mass, and may be, for example, 8.93%, 8.95%, 8.97%, 8.99%, 9%, 9.1%, or 9.15% by mass, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
In a preferred embodiment of the present invention, the solid-to-liquid ratio of the molybdenum-titanium-nickel alloy to the mixed acid in the mixing is (0.1 to 0.2):6, and may be, for example, 0.1:6, 0.12:6, 0.14:6, 0.16:6, 0.18:6, or 0.2:6, but is not limited to the above-mentioned values, and other values not shown in the above range are also applicable, and the unit of the liquid-to-solid ratio is g/mL.
In a preferred embodiment of the present invention, the heating temperature is 90 to 110 ℃, and may be, for example, 90 ℃, 95 ℃, 100 ℃, 105 ℃ or 110 ℃, but is not limited to the values listed, and other values not listed in the range are also applicable.
In a preferred embodiment of the present invention, the heating time is 20 to 40min, for example, 20min, 25min, 30min, 35min or 40min, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
As a preferred technical scheme of the invention, the application comprises the following steps: mixing and heating the molybdenum-titanium-nickel alloy and the mixed acid to obtain a solution in which molybdenum, titanium and nickel are dissolved;
the molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 14.97 to 15.3 percent of Ni, 8.93 to 9.15 percent of Ti and the balance of molybdenum;
the solid-to-liquid ratio of the molybdenum-titanium-nickel alloy and the mixed acid in the mixing is (0.1-0.2) to 6, and the unit of the liquid-to-solid ratio is g/mL; the heating temperature is 90-110 ℃; the heating time is 20-40 min;
the volume ratio of hydrofluoric acid to nitric acid in the mixed acid is (1.5-2.5) to 1; the mass concentration of the hydrofluoric acid is 35-38%; the mass concentration of the nitric acid is 65-68%.
Compared with the prior art, the invention at least has the following beneficial effects:
the invention realizes that the molybdenum-titanium-nickel alloy can be dissolved within 20-40min by reasonably configuring the components and the proportion in the mixed acid, and reaches the detection standard of ICP-OES on-machine.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a preparation method of a mixed acid for dissolving a molybdenum-titanium-nickel alloy, which comprises the following steps: mixing hydrofluoric acid and nitric acid according to the volume ratio of 2:1 to obtain the mixed acid; the mass concentration of the hydrofluoric acid is 36%; the mass concentration of the nitric acid is 66%.
Example 2
The embodiment provides a preparation method of a mixed acid for dissolving a molybdenum-titanium-nickel alloy, which comprises the following steps: mixing hydrofluoric acid and nitric acid according to the volume ratio of 2.5:1 to obtain the mixed acid; the mass concentration of the hydrofluoric acid is 35%; the mass concentration of the nitric acid is 68%.
Example 3
The embodiment provides a preparation method of a mixed acid for dissolving a molybdenum-titanium-nickel alloy, which comprises the following steps: mixing hydrofluoric acid and nitric acid according to the volume ratio of 1.5:1 to obtain the mixed acid; the mass concentration of the hydrofluoric acid is 38%; the mass concentration of the nitric acid is 65%.
Example 4
The embodiment provides a preparation method of a mixed acid for dissolving a molybdenum-titanium-nickel alloy, which comprises the following steps: mixing hydrofluoric acid and nitric acid according to the volume ratio of 1.7:1 to obtain the mixed acid; the mass concentration of the hydrofluoric acid is 37%; the mass concentration of the nitric acid is 67%.
Example 5
The embodiment provides a preparation method of a mixed acid for dissolving a molybdenum-titanium-nickel alloy, which comprises the following steps: mixing hydrofluoric acid and nitric acid according to the volume ratio of 2.2:1 to obtain the mixed acid; the mass concentration of the hydrofluoric acid is 35%; the mass concentration of the nitric acid is 65%.
Application example 1
Heating and dissolving the molybdenum-titanium-nickel alloy by using the mixed acid obtained in the embodiment 1, wherein the solid-to-liquid ratio (g/mL) of the molybdenum-titanium-nickel alloy and the mixed acid in the dissolving process is 0.1: 6; the heating temperature is 100 ℃; and heating for 30min to completely dissolve the molybdenum-titanium-nickel alloy.
The molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 15% of Ni, 9% of Ti and the balance of molybdenum.
Application example 2
Heating and dissolving the molybdenum-titanium-nickel alloy by using the mixed acid obtained in the embodiment 2, wherein the solid-to-liquid ratio (g/mL) of the molybdenum-titanium-nickel alloy and the mixed acid in the dissolving process is 0.2: 6; the heating temperature is 90 ℃; heating for 22min, and completely dissolving the molybdenum-titanium-nickel alloy.
The molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 14.98% of Ni, 9.15% of Ti and the balance of molybdenum.
Application example 3
Heating and dissolving the molybdenum-titanium-nickel alloy by using the mixed acid obtained in the embodiment 3, wherein the solid-to-liquid ratio (g/mL) of the molybdenum-titanium-nickel alloy and the mixed acid in the dissolving process is 0.15: 6; the heating temperature is 105 ℃; and heating for 40min to completely dissolve the molybdenum-titanium-nickel alloy.
The molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 15.3% of Ni, 8.93% of Ti and the balance of molybdenum.
Application example 4
Heating and dissolving the molybdenum-titanium-nickel alloy by using the mixed acid obtained in the embodiment 4, wherein the solid-to-liquid ratio (g/mL) of the molybdenum-titanium-nickel alloy and the mixed acid in the dissolving process is 0.13: 6; the heating temperature is 108 ℃; heating for 36min to completely dissolve the molybdenum-titanium-nickel alloy.
The molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 15.2% of Ni, 8.97% of Ti and the balance of molybdenum.
Application example 5
Heating and dissolving the molybdenum-titanium-nickel alloy by using the mixed acid obtained in the example 5, wherein the solid-to-liquid ratio (g/mL) of the molybdenum-titanium-nickel alloy to the mixed acid in the dissolving process is 0.17: 6; the heating temperature is 95 ℃; and heating for 27min to completely dissolve the molybdenum-titanium-nickel alloy.
The molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 15.1% of Ni, 8.99% of Ti and the balance of molybdenum.
Comparative example 1
The difference from application example 1 is that the titanium-molybdenum-nickel alloy cannot be dissolved without adding nitric acid to the mixed acid used for dissolution.
Comparative example 2
The difference from application example 1 is that the titanium-molybdenum-nickel alloy cannot be dissolved without adding hydrofluoric acid to the mixed acid used for dissolution.
Comparative example 3
The difference from the application example 1 is that hydrochloric acid (30 wt%) is added to the mixed acid used in the dissolution, the volume ratio of hydrofluoric acid to nitric acid to hydrochloric acid is 2:1:0.5, and the titanium-molybdenum-nickel alloy is completely dissolved after being dissolved for 60 min.
Comparative example 4
The difference from the application example 1 is that sulfuric acid (30 wt%) is further added to the mixed acid used in the dissolution, the volume ratio of hydrofluoric acid to nitric acid to sulfuric acid is 2:1:0.5, and the titanium-molybdenum-nickel alloy is completely dissolved after being dissolved for 70 min.
Comparative example 5
The difference from the application example 1 is that the titanium-molybdenum-nickel alloy is completely dissolved only when the volume ratio of hydrofluoric acid to nitric acid in the mixed acid used in the dissolution is 1:1 and the titanium-molybdenum-nickel alloy is dissolved for 80 min.
Comparative example 6
The difference from the application example 1 is that the titanium-molybdenum-nickel alloy is completely dissolved only when the volume ratio of hydrofluoric acid to nitric acid in the mixed acid used in the dissolution is 1:2 and the titanium-molybdenum-nickel alloy is dissolved for 75 min.
Comparative example 7
The difference from the application example 1 is that the titanium-molybdenum-nickel alloy is completely dissolved after the mixed acid used in the dissolution is dissolved for 95min, wherein the volume ratio of hydrofluoric acid to nitric acid is 3: 1.
According to the results of the above examples and comparative examples, the molybdenum-titanium-nickel alloy can be dissolved within 20-40min by reasonably configuring the components and the proportion in the mixed acid, so that the detection standard of ICP-OES machine is reached.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. The mixed acid for dissolving the molybdenum-titanium-nickel alloy is characterized in that the volume ratio of hydrofluoric acid to nitric acid in the mixed acid is (1.5-2.5): 1;
the mass concentration of the hydrofluoric acid is 35-38%;
the mass concentration of the nitric acid is 65-68%.
2. The mixed acid of claim 1, wherein the volume ratio of hydrofluoric acid to nitric acid in the mixed acid is (1.8-2): 1.
3. The mixed acid according to claim 1 or 2, wherein the hydrofluoric acid has a mass concentration of 36 to 37%.
4. The mixed acid according to any one of claims 1 to 3, wherein the mass concentration of the nitric acid is 66 to 67%.
5. A method for preparing the mixed acid according to any one of claims 1 to 4, wherein the method comprises: mixing hydrofluoric acid and nitric acid according to the volume ratio of (1.5-2.5) to 1 to obtain the mixed acid.
6. Use of the mixed acid molybdenum titanium nickel alloy in solution according to any one of claims 1 to 4, characterized in that it comprises the following steps: mixing and heating the molybdenum-titanium-nickel alloy and the mixed acid to obtain a solution in which molybdenum, titanium and nickel are dissolved;
the molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 14.97 to 15.3 percent of Ni, 8.93 to 9.15 percent of Ti and the balance of molybdenum.
7. The use of the dissolved molybdenum titanium nickel alloy of claim 6, wherein the solid-to-liquid ratio of molybdenum titanium nickel alloy to mixed acid in the mixture is (0.1-0.2):6, and the unit of the liquid-to-solid ratio is g/mL.
8. Use of the dissolved molybdenum titanium nickel alloy according to claim 6 or 7, characterized in that the heating temperature is 90-110 ℃.
9. Use of the dissolved molybdenum titanium nickel alloy according to any one of claims 6 to 8, characterized in that the heating time is 20 to 40 min.
10. Use of the dissolved molybdenum titanium nickel alloy according to any one of claims 6 to 9, characterized in that it comprises the following steps: mixing and heating the molybdenum-titanium-nickel alloy and the mixed acid to obtain a solution in which molybdenum, titanium and nickel are dissolved;
the molybdenum-titanium-nickel alloy comprises the following components in percentage by mass: 14.97 to 15.3 percent of Ni, 8.93 to 9.15 percent of Ti and the balance of molybdenum;
the solid-to-liquid ratio of the molybdenum-titanium-nickel alloy and the mixed acid in the mixing is (0.1-0.2) to 6, and the unit of the liquid-to-solid ratio is g/mL; the heating temperature is 90-110 ℃; the heating time is 20-40 min;
the volume ratio of hydrofluoric acid to nitric acid in the mixed acid is (1.5-2.5) to 1; the mass concentration of the hydrofluoric acid is 35-38%; the mass concentration of the nitric acid is 65-68%.
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