A preparation method of ammonium hexaiodide iridate

Abstract

This invention belongs to the field of precious metal metallurgy technology and relates to a method for preparing ammonium hexaiodoiridate. By activating the raw materials in an ethanol system, this method significantly reduces the preparation time required in the conventional preparation process and increases the direct yield of ammonium hexaiodoiridate. Repeated centrifugation increases the raw material contact area, further shortening the preparation time. This method achieves a preparation time of ≤8 days, a direct yield of ≥70%, and a product purity of ≥99.5%.

Description

Technical Field

[0001] The invention belongs to the technical field of precious metal metallurgy and relates to a method for preparing ammonium hexaiodideiridate. Background Art

[0002] Ammonium hexaiodoiridate is used in reagent synthesis and catalytic reactions. However, the current method for preparing ammonium hexaiodoiridate involves dissolving powdered ammonium hexachloroiridate in a cold, concentrated aqueous potassium iodide solution and allowing it to stand for several weeks, yielding dark blue crystals of ammonium hexaiodoiridate. This existing method suffers from long preparation times and low direct yields of the product, ammonium hexaiodoiridate.

[0003] In view of the problems existing in the prior art, there is an urgent need for a preparation method with greatly shortened preparation time and high direct product yield. Summary of the Invention

[0004] The present invention aims to solve the problems existing in the prior art and provides a method for preparing ammonium hexaiodideiridate. The method has a preparation time of ≤8 days, a direct yield of ≥70%, and a product purity of ≥99.5%.

[0005] The technical solution provided by the present invention is.

[0006] A method for preparing ammonium hexaiodideiridate comprises the following specific steps:

[0007] Step 1: Prepare mixed solution A:

[0008] Ammonium hexachloroiridate was placed in a beaker, soaked in ethanol and heated to obtain an ammonium hexachloroiridate active solution. A saturated potassium iodide aqueous solution was added to the system, and an ultrasonic oscillation device was turned on to disperse the active solution to obtain a turbid mixed solution A.

[0009] Step 2: Preparation of ammonium hexaiodide iridate:

[0010] The mixed solution A is repeatedly centrifuged in a refrigerated centrifuge to obtain the precipitated product, ammonium hexaiodide.

[0011] Furthermore, in step 1, the amount of ethanol used is 3-5 ml per gram of ammonium hexachloroiridate.

[0012] Furthermore, in step 1, the volume ratio of the ammonium hexachloroiridate active solution to the saturated potassium iodide aqueous solution is 1:5~8.

[0013] Furthermore, in step 1, the temperature is 50-70°C.

[0014] Furthermore, in step 1, the ultrasonic oscillation power is 150-200 W, and the dispersion time is 30-50 min.

[0015] Furthermore, in step 2, the cold water temperature is 10-20°C.

[0016] Furthermore, in step 2, the centrifugation time is 5 to 8 days.

[0017] Compared with the prior art, the present invention has the following beneficial effects.

[0018] The invention activates the raw materials in an ethanol system, thereby greatly reducing the preparation time required in the original preparation process and increasing the direct yield of ammonium hexaiodide iridate; repeated centrifugation increases the contact area of ​​the raw materials and further shortens the preparation time.

[0019] The preparation time of ammonium hexaiodide iridate by the method is ≤8 days, while the prior art takes several weeks; the direct yield of ammonium hexaiodide iridate is ≥70%, while the prior art takes about 55%; the purity of the ammonium hexaiodide product is ≥99.5%, while the prior art takes ≥97%. DETAILED DESCRIPTION

[0020] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0021] A method for preparing ammonium hexaiodideiridate comprises the following specific steps:

[0022] Step 1: Prepare mixed solution A:

[0023] Ammonium hexachloroiridate was placed in a beaker, soaked in ethanol and heated to obtain an ammonium hexachloroiridate active solution. A saturated potassium iodide aqueous solution was added to the system, and an ultrasonic oscillation device was turned on to disperse the active solution to obtain a turbid mixed solution A.

[0024] Step 2: Preparation of ammonium hexaiodide iridate:

[0025] The mixed solution A is repeatedly centrifuged in a refrigerated centrifuge to obtain the precipitated product, ammonium hexaiodide.

[0026] Furthermore, in step 1, the amount of ethanol used is 3-5 ml per gram of ammonium hexachloroiridate.

[0027] Furthermore, in step 1, the volume ratio of the ammonium hexachloroiridate active solution to the saturated potassium iodide aqueous solution is 1:5~8.

[0028] Furthermore, in step 1, the temperature is 50-70°C.

[0029] Furthermore, in step 1, the ultrasonic oscillation power is 150-200 W, and the dispersion time is 30-50 min.

[0030] Furthermore, in step 2, the cold water temperature is 10-20°C.

[0031] Furthermore, in step 2, the centrifugation time is 5 to 8 days.

[0032] Example 1.

[0033] Place 10g of ammonium hexachloroiridate in a beaker and soak it in 30ml of ethanol. Raise the temperature to 50°C and add 200ml of saturated potassium iodide solution. Maintain the reaction temperature at 50°C and disperse it under 150W ultrasonic vibration for 30 minutes. Place the mixture in a centrifuge tube and centrifuge at 20°C and 200 rpm for 5 days. Filter to obtain the product, ammonium hexaiodoiridate, test it, and store it.

[0034] result:

[0035] Direct yield of ammonium hexaiodideiridate: 71%;

[0036] Preparation time of ammonium hexaiodide iridate: 5 days;

[0037] Ammonium hexaiodideiridate purity: 99.6%.

[0038] Example 2.

[0039] Place 10g of ammonium hexachloroiridate in a beaker, soak it in 40ml of ethanol, heat it to 50°C, add 300ml of saturated potassium iodide solution, heat it to 60°C, and disperse it under 180W ultrasonic field for 40 minutes. Then, add it to a centrifuge tube and centrifuge it at 15°C and 250 rpm for 6 days. Filter to obtain the ammonium hexaiodoiridate product, analyze it, and store it.

[0040] result:

[0041] Direct yield of ammonium hexaiodide iridate: 73%;

[0042] Preparation time of ammonium hexaiodideiridate: 6 days;

[0043] Purity of ammonium hexaiodideiridate: 99.6%.

[0044] Example 3.

[0045] Place 10g of ammonium hexachloroiridate in a beaker, soak it in 50ml of ethanol, and heat it to 60°C. Add 400ml of saturated potassium iodide aqueous solution to the system. Heat it to 70°C and disperse it under a 200W ultrasonic field for 50 minutes. Then, add the solution to a centrifuge tube and centrifuge it at 10°C and 300 rpm for 8 days. Filter to obtain the product, analyze it, and store it.

[0046] result:

[0047] Direct yield of ammonium hexaiodide iridate: 76%;

[0048] Preparation time of ammonium hexaiodide iridate: 8 days;

[0049] Ammonium hexaiodideiridate purity: 99.7%.

[0050] Comparative Example 1.

[0051] Place 10 grams of ammonium hexachloroiridate in a beaker and heat to 50°C. Add 200 ml of saturated potassium iodide solution. Maintain the reaction temperature at 50°C and disperse under 150W ultrasonic vibration for 30 minutes. Place in cold water and allow to precipitate at low temperature for 5 days. Filter to obtain the product, ammonium hexaiodoiridate, test it, and store it.

[0052] Direct yield of ammonium hexaiodideiridate: 58%;

[0053] Preparation time of ammonium hexaiodide iridate: 5 days;

[0054] Ammonium hexaiodideiridate purity: 99.1%.

[0055] Comparative Example 2.

[0056] Place 10g of ammonium hexachloroiridate in a beaker, soak it in 30ml of ethanol, heat it to 50°C, and disperse it under 150W ultrasonic vibration for 30 minutes. Then, mix it with 200ml of saturated potassium iodide aqueous solution, add it to a centrifuge tube, and centrifuge it at 20°C and 200 rpm for 5 days. Filter it to obtain the product ammonium hexaiodoiridate, test it, and put it into storage.

[0057] Direct yield of ammonium hexaiodideiridate: 66%;

[0058] Preparation time of ammonium hexaiodide iridate: 5 days;

[0059] Purity of ammonium hexaiodideiridate: 99.4%.

[0060] Comparative Example 3.

[0061] Place 200ml of saturated potassium iodide aqueous solution in a beaker and add 30ml of ethanol. Heat to 50°C and disperse under 150W ultrasonic vibration for 30 minutes. Add 10g of ammonium hexachloroiridate to the system, mix thoroughly, and then add to a centrifuge tube. Centrifuge at 20°C and 200 rpm for 5 days. Filter to obtain the product ammonium hexaiodoiridate, analyze it, and store it.

[0062] Direct yield of ammonium hexaiodide iridate: 60%;

[0063] Preparation time of ammonium hexaiodide iridate: 5 days;

[0064] Ammonium hexaiodideiridate purity: 99.2%.

[0065] Comparative Example 4.

[0066] Place 10g of ammonium hexachloroiridate in a beaker and soak it in 30ml of ethanol. Raise the temperature to 50°C and add 200ml of saturated potassium iodide aqueous solution. Maintain the reaction temperature at 50°C and disperse under 150W ultrasonic vibration for 30 minutes. Place the mixture in cold water and allow it to precipitate at low temperature for 5 days. Filter the mixture to obtain the ammonium hexaiodoiridate product, analyze it, and store it.

[0067] Direct yield of ammonium hexaiodideiridate: 62%;

[0068] Preparation time of ammonium hexaiodide iridate: 5 days;

[0069] Ammonium hexaiodideiridate purity: 99.2%.

[0070] Comparative Example 5.

[0071] The prior art is to place 10 grams of powdered ammonium hexachloroiridate in a beaker, add 200 ml of concentrated potassium iodide solution, mix well, and put into a centrifuge tube. Centrifuge at a temperature of 20°C and a speed of 200 rpm for 5 days, filter, and obtain the product ammonium hexaiodoiridate, test it, and put it into storage.

[0072] Direct yield of ammonium hexaiodideiridate: 51%;

[0073] Preparation time of ammonium hexaiodide iridate: 5 days;

[0074] Ammonium hexaiodideiridate purity: 89%.

Claims

1. A method for preparing ammonium hexaiodide iridate, characterized in that: The specific steps include: Step 1: Prepare mixed solution A: Place ammonium hexachloroiridate in a beaker, soak it in ethanol, and heat it to 50-70°C to obtain an ammonium hexachloroiridate active solution. Add a saturated potassium iodide aqueous solution to the system and use an ultrasonic oscillator to disperse the active solution at a power of 150-200 W for 30-50 minutes to obtain a turbid mixed solution A. Use 3-5 ml of ethanol per gram of ammonium hexachloroiridate. Step 2: Preparation of ammonium hexaiodide iridate: The mixed solution A is repeatedly centrifuged in a refrigerated centrifuge for 5 to 8 days to obtain the precipitated product, ammonium hexaiodideiridate.

2. The method for preparing ammonium hexaiodide iridate according to claim 1, wherein In the step 1, the volume ratio of the ammonium hexachloroiridate active solution to the saturated potassium iodide aqueous solution is 1:5-8.

3. The preparation method of ammonium hexaiodide iridate according to claim 1, wherein In step 2, the temperature of the cold water is 10-20°C.