CN114427036A - Method for dissolving rhodium powder and rhodium dissolving solution obtained by same - Google Patents
Method for dissolving rhodium powder and rhodium dissolving solution obtained by same Download PDFInfo
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Abstract
The invention discloses a method for dissolving rhodium powder and rhodium dissolving solution obtained by the same, wherein the method comprises the following steps: firstly, pretreating the rhodium powder by using concentrated sulfuric acid and concentrated nitric acid to obtain a pretreatment solution, then adding a strong oxidant into the pretreatment solution for heating treatment, and finally carrying out aftertreatment to obtain a rhodium dissolving solution. The volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 1 (1.5-6), based on 1g of rhodium powder, the dosage of the concentrated sulfuric acid is 15-40 mL, based on 1g of rhodium powder, and the dosage of the strong oxidant is 25-60 mL. The invention adopts strong acid and strong oxidant to directly dissolve rhodium powder, compared with the alloy activation dissolving method, the method does not need to add other chemical elements because the rhodium powder is directly dissolved, thereby avoiding the interference of other elements.
Description
Technical Field
The invention belongs to the technical field of precious metals, and particularly relates to a method for dissolving rhodium powder.
Background
Rhodium is used as a noble metal and plays a significant role in the petrochemical industry and the metallurgical industry, and rhodium-phosphine complex catalysts are applied to the field of hydroformylation.
The noble metal rhodium powder is compact, chemically inert, low in activity and very insoluble, so that the preparation and yield of the rhodium-phosphine catalyst are directly influenced, serious waste is caused, and economic loss is caused. The dissolution of rhodium is an important leading technology and a difficult problem in metallurgical technology, and the current dissolution technologies of rhodium mainly comprise an electrochemical dissolution method, a microwave digestion method, a sodium bisulfate-dilute acid dissolution method, an alloy activation dissolution method and the like. The method is characterized in that other metal elements are introduced, the steps are more, the period is longer, and the preparation of the rhodium-phosphine catalyst is influenced finally.
The prior document relates to the dissolution of rhodium in insoluble rhodium powder by chloroauric acid solution, the chloroauric acid solution and the rhodium powder can generate oxidation-reduction reaction under specific conditions, and the rhodium powder is oxidized and dissolved to generate H3RhCl6And (4) the chloroauric acid in the solution is reduced to generate sponge gold powder. However, the adopted raw material chloroauric acid is high in price and is not suitable for large-scale application.
The prior document also relates to electrochemical dissolution of rhodium, 0.6g of rhodium powder is weighed into an electrolytic cell, then a proper amount of 8mol/L hydrochloric acid is added into the electrolytic cell, and the electrolytic cell is put into an oil bath and adjusted to the required temperature. And (3) assembling a circuit, selecting graphite rods with different diameters as electrodes, connecting the electrodes with an ammeter, setting the voltage to be 3-5V, carrying out an electrolysis reaction, and stopping sampling after electrolyzing for a period of time to measure the rhodium solubility. However, this method requires the use of special electrolytic equipment.
In the prior literature, rhodium powder is dissolved in a hydrochloric acid-sodium chlorate system by adopting an aqueous solution chlorination method, and the influence of factors such as reaction temperature, acidity, oxidant dosage, time, liquid-solid ratio and the like on the rhodium dissolution rate is examined. The result shows that after the concentrated hydrochloric acid is heated to 85 ℃, sodium chlorate begins to be added, the acidity is 8-9 mol/L, the using amount of a saturated sodium chlorate solution is 250mL, the liquid-solid ratio is 45mL/g, the reaction time is 2 hours, and the one-time dissolution rate of rhodium powder reaches more than 95%. However, the dissolution effect of this method is yet to be further improved.
Chinese patent CN106011495A discloses a rhodium powder dissolving method, which comprises the following steps: (1) mixing: mixing rhodium powder and base metal powder according to a certain mass ratio; (2) mechanical activation; (3) acid soluble base metals: dissolving out base metals from the mixed material obtained in the step (2) by adopting hydrochloric acid, and carrying out solid-liquid separation to obtain a rhodium material; (4) dissolution of rhodium: and (4) putting the rhodium material obtained in the step (3) into an ultrasonic dissolution reactor, and dissolving the rhodium material by using aqua regia, wherein the dissolution rate of rhodium powder is more than 95%. The invention adopts the synergistic effect of mechanical activation and ultrasonic wave to improve the dissolution efficiency of rhodium, rhodium powder and base metal powder are mixed and subjected to mechanical activation, so that rhodium and base metal are alloyed, rhodium lattices generate defects, the interatomic binding energy is reduced, the lattice internal energy is increased, and the reaction activity is enhanced; and the aqua regia is dissolved under the assistance of ultrasonic waves, so that the dissolution of rhodium is accelerated, and the dissolution time is shortened. The method has more steps and is not easy to be applied in later period of industrialization.
Therefore, it is very important to develop a technology for dissolving rhodium powder rapidly and efficiently.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a method for dissolving rhodium powder, which comprises the steps of digesting the rhodium powder by concentrated sulfuric acid and concentrated nitric acid, and adding a strong oxidant to strengthen the dissolution reaction.
(1) A method of dissolving rhodium powder comprising: firstly, pretreating the rhodium powder by using concentrated sulfuric acid and concentrated nitric acid to obtain a pretreatment solution, then adding a strong oxidant into the pretreatment solution for heating treatment, and finally carrying out aftertreatment to obtain a rhodium dissolving solution.
(2) The method according to the above (1), wherein the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 1 (1.5-6), preferably 1 (2-5).
(3) The method according to the above (1), wherein the amount of the concentrated sulfuric acid is 15 to 40mL, preferably 20 to 35mL, based on 1g of the rhodium powder.
(4) The method according to the above (1), wherein the pretreatment is carried out at 80 to 150 ℃ for 4 to 12 hours.
(5) The method according to the above (4), wherein the pretreatment is carried out at 100 to 120 ℃ for 6 to 10 hours.
(6) The method according to the above (1), wherein the strong oxidant is at least one selected from perchloric acid and sodium perchlorate.
(7) The method according to the above (6), wherein the amount of the strong oxidant is 25 to 60mL, preferably 30 to 50mL, based on 1g of the rhodium powder.
(8) The method according to the above (1), wherein the heat treatment is carried out at 80 to 150 ℃ for 4 to 12 hours;
preferably, the temperature is 100-120 ℃ and the time is 6-10 hours.
(9) The method according to any one of (1) to (8) above, wherein the post-treatment comprises filtration and washing in this order, preferably washing with water.
(10) A rhodium dissolved solution obtained by the method according to any one of the above (1) to (9).
Detailed Description
The features and advantages of the present invention will become more apparent and appreciated from the following detailed description of the invention.
One of the objects of the present invention is to provide a method for dissolving rhodium powder, comprising: firstly, pretreating the rhodium powder by using concentrated sulfuric acid and concentrated nitric acid to obtain a pretreatment solution, then adding a strong oxidant into the pretreatment solution for heating treatment, and finally carrying out aftertreatment to obtain a rhodium dissolving solution.
In a preferred embodiment, the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 1 (1.5-6).
In a further preferred embodiment, the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 1 (2-5).
In a preferred embodiment, the amount of concentrated sulfuric acid is 15 to 40mL based on 1g of rhodium powder.
In a further preferred embodiment, the amount of concentrated sulfuric acid is 20 to 35mL based on 1g of rhodium powder.
In a preferred embodiment, the pretreatment is carried out at 80 to 150 ℃ for 4 to 12 hours.
In a further preferred embodiment, the pretreatment is carried out at 100 to 120 ℃ for 6 to 10 hours.
In a preferred embodiment, the strong oxidant is selected from at least one of perchloric acid, sodium perchlorate.
In a further preferred embodiment, the strong oxidizer is used in an amount of 25 to 60mL based on 1g of rhodium powder.
In a further preferred embodiment, the strong oxidizer is used in an amount of 30 to 50mL based on 1g of rhodium powder.
In a preferred embodiment, the heating treatment is carried out at 80-150 ℃ for 4-12 hours.
In a further preferred embodiment, the heat treatment is performed at 100 to 120 ℃ for 6 to 10 hours.
In a preferred embodiment, the post-treatment comprises filtration and washing in sequence.
In a further preferred embodiment, the washing is carried out with water.
Preferably, the water is preferably selected from deionized water and/or ultrapure water.
The second object of the present invention is to provide a rhodium-dissolved solution obtained by the method described in the first object of the present invention.
In the prior art, an alloy activation dissolution method is common, and the method comprises the steps of melting metals such as iron, zinc and the like and rhodium at high temperature to form an alloy, removing base metals by using dilute acid, dissolving by using strong oxidizing acid to obtain a rhodium solution, and analyzing or purifying.
Therefore, in the invention, the combination of the pretreatment by adopting the combination of concentrated sulfuric acid and concentrated nitric acid and the retreatment of perchloric acid greatly improves the dissolution degree of rhodium powder, and simultaneously, the method does not need to add other chemical elements and avoids the interference of other elements.
The endpoints of the ranges and any values disclosed in the present application are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein. In the following, various technical solutions can in principle be combined with each other to obtain new technical solutions, which should also be regarded as specifically disclosed herein.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention adopts strong acid and strong oxidant to directly dissolve rhodium powder, compared with the alloy activation dissolving method, the method does not need to add other chemical elements because the rhodium powder is directly dissolved, thereby avoiding the interference of other elements.
(2) The rhodium powder is dissolved more directly and efficiently by adopting the method, the interference is less, and the economical efficiency is good.
Examples
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
It is to be further understood that the various features described in the following detailed description may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention can be made, as long as the technical solution formed by the combination does not depart from the idea of the present invention, and the technical solution formed by the combination is part of the original disclosure of the present specification, and also falls into the protection scope of the present invention.
The raw materials used in the examples and comparative examples are disclosed in the prior art if not particularly limited, and may be, for example, obtained commercially directly or prepared according to the methods disclosed in the prior art.
In the following examples and comparative examples, the concentration of perchloric acid is 72%; 98% of concentrated sulfuric acid; 37% of hydrochloric acid; the nitric acid concentration was 68%.
In the examples and comparative examples, the rhodium concentration in the rhodium-containing waste liquid was measured and analyzed by an inductively coupled plasma emission spectrometer, and the dissolution rate of rhodium was calculated.
Wherein, the rhodium dissolution rate adopts the following calculation formula:
the rhodium dissolution rate is (volume of rhodium-containing solution constant volume V × rhodium concentration C)/(mass of rhodium powder M × purity of rhodium powder) × 100%.
[ example 1 ]
Adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 4mL of concentrated sulfuric acid and 8mL of concentrated nitric acid into the iodometric flask respectively, heating to react at 100 ℃ for 6 hours, and cooling to room temperature to obtain rhodium-containing liquid;
adding 6mL of perchloric acid, heating and reacting for 6 hours at 100 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 99.6% by detection.
[ example 2 ]
Adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 6mL of concentrated sulfuric acid and 24mL of concentrated nitric acid into the iodometric flask respectively, heating to react for 8 hours at the temperature of 120 ℃, and cooling to room temperature to obtain rhodium-containing liquid;
adding 8mL of perchloric acid, heating to react for 7 hours at 120 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 99.7% through detection.
[ example 3 ]
Adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 7mL of concentrated sulfuric acid and 35mL of concentrated nitric acid into the iodometric flask respectively, heating to react for 10 hours at the temperature of 120 ℃, and cooling to room temperature to obtain rhodium-containing liquid;
adding 10mL of perchloric acid, heating to react for 10 hours at 120 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 99.8% through detection.
[ example 4 ]
Adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 5mL of concentrated sulfuric acid and 17.5mL of concentrated nitric acid into the iodometric flask respectively, heating to react at 120 ℃ for 7 hours, and cooling to room temperature to obtain rhodium-containing liquid;
adding 7mL of perchloric acid, heating to react for 7 hours at 120 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 99.7% through detection.
[ example 5 ]
Adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 7mL of concentrated sulfuric acid and 31.5mL of concentrated nitric acid into the iodometric flask respectively, heating to react at 120 ℃ for 6 hours, and cooling to room temperature to obtain rhodium-containing liquid;
adding 9mL of perchloric acid, heating to react for 10 hours at 110 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 99.8% through detection.
[ example 6 ]
Adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 5mL of concentrated sulfuric acid and 15mL of concentrated nitric acid into the iodometric flask respectively, heating to react for 10 hours at the temperature of 100 ℃, and cooling to room temperature to obtain rhodium-containing liquid;
adding 6mL of perchloric acid, heating to react for 10 hours at 120 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 99.7% through detection.
Comparative example
Comparative example 1
The procedure of example 1 was repeated except that: replacing perchloric acid with an equal amount of hydrogen peroxide:
adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 4mL of concentrated sulfuric acid and 8mL of concentrated nitric acid into the iodometric flask respectively, heating to react at 100 ℃ for 6 hours, and cooling to room temperature to obtain rhodium-containing liquid;
then adding 6mL of hydrogen peroxide, heating and reacting for 6 hours at 100 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting the filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 98.7% by detection.
Comparative example 2
The procedure of example 1 was repeated except that: the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 1: 1.
Adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 4mL of concentrated sulfuric acid and 4mL of concentrated nitric acid into the iodometric flask respectively, heating to react at 100 ℃ for 6 hours, and cooling to room temperature to obtain rhodium-containing liquid;
adding 6mL of perchloric acid, heating and reacting for 6 hours at 100 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 99.1% through detection.
Comparative example 3
Adding 0.2g (with the purity of 99.95%) of the rhodium powder into an iodometric flask, slowly adding 9.6mL of concentrated hydrochloric acid and 2.4mL of concentrated nitric acid into the iodometric flask respectively, heating to react at 100 ℃ for 6 hours, and cooling to room temperature to obtain rhodium-containing liquid;
adding 6mL of perchloric acid, heating and reacting for 6 hours at 100 ℃, cooling to room temperature, filtering and washing the rhodium-containing solution, and collecting filtrate;
the volume is determined by deionized water, and the dissolution rate of rhodium is 97.2 percent through detection.
The invention has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to be construed in a limiting sense. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (10)
1. A method of dissolving rhodium powder comprising: firstly, pretreating the rhodium powder by using concentrated sulfuric acid and concentrated nitric acid to obtain a pretreatment solution, then adding a strong oxidant into the pretreatment solution for heating treatment, and finally carrying out aftertreatment to obtain a rhodium dissolving solution.
2. The method according to claim 1, wherein the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 1 (1.5-6), preferably 1 (2-5).
3. The method according to claim 1, wherein the concentrated sulfuric acid is used in an amount of 15 to 40mL, preferably 20 to 35mL, based on 1g of rhodium powder.
4. The method of claim 1, wherein the pre-treatment is performed at 80-150 ℃ for 4-12 hours.
5. The method according to claim 4, wherein the pretreatment is performed at 100 to 120 ℃ for 6 to 10 hours.
6. The method of claim 1, wherein the strong oxidant is selected from at least one of perchloric acid and sodium perchlorate.
7. The method according to claim 6, wherein the amount of the strong oxidant is 25 to 60mL, preferably 30 to 50mL, based on 1g of rhodium powder.
8. The method according to claim 1, wherein the heat treatment is carried out at 80 to 150 ℃ for 4 to 12 hours; preferably, the temperature is 100-120 ℃ and the time is 6-10 hours.
9. The method according to any one of claims 1 to 8, wherein the post-treatment comprises filtration and washing in that order, preferably with water.
10. A rhodium dissolved solution obtained by the method according to any one of claims 1 to 9.
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| CN101177306A (en) * | 2007-11-12 | 2008-05-14 | 中国海洋石油总公司 | Method for recovering rhodium chloride from waste rhodium catalyst |
| CN101503220A (en) * | 2008-12-30 | 2009-08-12 | 西安凯立化工有限公司 | Preparation of rhodium chloride |
| CN101576497A (en) * | 2009-03-06 | 2009-11-11 | 刘征涛 | Plasma emission spectrum detection method of content of platinum, palladium and rhodium in ceramic materials |
| CN103341639A (en) * | 2013-07-24 | 2013-10-09 | 贵研资源（易门）有限公司 | Method for dissolving rhodium powder difficult to dissolve |
| CN106011495A (en) * | 2016-06-27 | 2016-10-12 | 昆明贵金属研究所 | Dissolution method for rhodium powder |
| CN108264100A (en) * | 2018-03-18 | 2018-07-10 | 中船重工黄冈贵金属有限公司 | A kind of high-efficiency synthesis method of rhodium nitrate solution |
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2020
- 2020-09-25 CN CN202011020308.4A patent/CN114427036A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177306A (en) * | 2007-11-12 | 2008-05-14 | 中国海洋石油总公司 | Method for recovering rhodium chloride from waste rhodium catalyst |
| CN101503220A (en) * | 2008-12-30 | 2009-08-12 | 西安凯立化工有限公司 | Preparation of rhodium chloride |
| CN101576497A (en) * | 2009-03-06 | 2009-11-11 | 刘征涛 | Plasma emission spectrum detection method of content of platinum, palladium and rhodium in ceramic materials |
| CN103341639A (en) * | 2013-07-24 | 2013-10-09 | 贵研资源（易门）有限公司 | Method for dissolving rhodium powder difficult to dissolve |
| CN106011495A (en) * | 2016-06-27 | 2016-10-12 | 昆明贵金属研究所 | Dissolution method for rhodium powder |
| CN108264100A (en) * | 2018-03-18 | 2018-07-10 | 中船重工黄冈贵金属有限公司 | A kind of high-efficiency synthesis method of rhodium nitrate solution |
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