CN108821354A - A method of preparing nitric acid iridium solution - Google Patents
A method of preparing nitric acid iridium solution Download PDFInfo
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- CN108821354A CN108821354A CN201811111110.XA CN201811111110A CN108821354A CN 108821354 A CN108821354 A CN 108821354A CN 201811111110 A CN201811111110 A CN 201811111110A CN 108821354 A CN108821354 A CN 108821354A
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- nitric acid
- iridium
- hydroxide
- potassium
- preparing
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/46—Ruthenium, rhodium, osmium or iridium
- B01J23/468—Iridium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of methods for preparing nitric acid iridium solution, it is desirable to provide a method of it prepares and easily prepares nitric acid iridium solution.It includes the following steps：（1）Potassium hexachloroiridate is prepared using ammonium chloroiridate；（2）The potassium hexachloroiridate being prepared is reacted with potassium hydroxide and generates hydroxide iridium：（3）The hydroxide iridium being prepared is dissolved in nitric acid, nitric acid iridium solution is made.Nitric acid iridium Chlorine in Solution ion residues of the invention are low, with better heat-resisting quantity and service life.
Description
Technical field
The present invention relates to noble metal catalyst preparation technical fields, more particularly, to a kind of side for preparing nitric acid iridium solution
Method.
Background technique
Noble metal catalyst is widely used in the fields such as vent gas treatment, organic synthesis, noble metal catalyst it is expensive and
It is not easy to prepare, how reducing usage amount, increasing catalytic activity and improve reuse rate is the emphasis studied at present.Study table
Bright, compared with the noble metal catalyst containing chlorine, the noble metal catalyst without chlorine has significant catalysis advantage.When both are urged
After agent aging, the catalytic activity of the catalyst containing chlorine be will be greatly reduced, while chlorine can reduce the heat-resisting quantity of catalyst and make
Use the service life.
The catalyst of iridium, which is widely used in, prepares hydrazine decomposing catalyst, cleaning catalyst for tail gases of automobiles and unsaturated carbon hydrocarbonylation
Close object hydrogenation catalyst.Preparing iridium catalyst master raw material to be used is chloro-iridic acid, and chloride ion therein is to catalyst obtained
Influence is very big, researches and develops the new iridic compound without chlorine of one kind and chloro-iridic acid is replaced just to be particularly important.The nitrate of noble metal
Compound is due to not chloride ion-containing, and the advantages that being easy dissolution, dosage increased year by year in recent years, and synthetic method is there is not yet report.
Summary of the invention
The shortcomings that present invention is directed in the prior art, provide a kind of method for preparing nitric acid iridium solution.This method can be effective
Control the Chloride residue in product.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions：
A method of preparing nitric acid iridium solution comprising following steps：
（1）Potassium hexachloroiridate is prepared using ammonium chloroiridate；
（2）The potassium hexachloroiridate being prepared is reacted with potassium hydroxide and generates hydroxide iridium：
（3）The hydroxide iridium being prepared is dissolved in nitric acid, nitric acid iridium solution is made.
Preferably, the step（1）In, the preparation method of potassium hexachloroiridate is as follows：By ammonium chloroiridate（g）:Chloroazotic acid（ml）=
1:4 ratio mixes, and a small amount of insoluble matter is filtered to remove after ammonium chloroiridate all dissolution, by ammonium chloroiridate（g）:Potassium chloride (g)=
1:Potassium chloride is added in the ratio of 0.4-0.5, and reaction temperature is 50-60 DEG C, reaction time 3-4h.
Preferably, the step（2）In, the preparation process of hydroxide iridium is, by potassium hexachloroiridate（g）：Potassium hydroxide
(g)：Water (ml)=1:0.5-0.55:The ratio of 10-11 mixes, and reaction temperature is 70-80 DEG C.
Preferably, the step（3）In, hydroxide iridium (mol):Nitric acid (mol)=1:3-3.1, reaction temperature are room
Temperature.
Compared with prior art, the invention has the advantages that：
The present invention uses ammonium chloroiridate for starting material, and ammonium chloroiridate is made after potassium hexachloroiridate and reacts generation with sodium hydroxide again
Hydroxide iridium is finally dissolved in nitric acid and nitric acid iridium solution, Chloride residue is made<3ppm.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, and those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.It is not specified in embodiment specific
Technology or conditions person described technology or conditions or carries out according to the literature in the art according to product description.It is used
Production firm person is not specified in reagent or instrument, is the conventional products that can be obtained by purchase.Obviously, described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained under that premise of not paying creative labor belongs to the model that the present invention protects
It encloses.
Embodiment 1
10 grams of ammonium chloroiridates are weighed, 40ml chloroazotic acid is added, 4.5 grams of chlorinations are added after being all filtered to remove a small amount of insoluble matter after dissolution
Potassium reacts 3 hours at 55 DEG C, and obtained solid is filtered, and is dried to obtain 9.86 grams of potassium hexachloroiridate solids after washing 3 times.By chlorine
After iridium acid potassium stirs into suspension in the purified water of 100ml, 5 grams of potassium hydroxide are added, it is a large amount of dark blue to having in 75 DEG C of reactions
Until color solid occurs.After blue solid filtering 3 drying of washing, by hydroxide iridium (mol):Nitric acid (mol)=1:3
Nitric acid iridium solution, Chloride residue is made after being dissolved with 10% nitric acid solution in ratio<3ppm.
Embodiment 2
100 grams of ammonium chloroiridates are weighed, 400ml chloroazotic acid is added, 50 grams of chlorine are added after being all filtered to remove a small amount of insoluble matter after dissolution
Change potassium at 55 DEG C, react 3.5 hours, obtained solid is filtered, is dried to obtain 99 grams of potassium hexachloroiridate solids after washing 3 times.It will
After potassium hexachloroiridate stirs into suspension in the purified water of 1000ml, 50 grams of potassium hydroxide are added, it is a large amount of to having in 70 DEG C of reactions
Until blue solid occurs.After blue solid filtering 3 drying of washing, by hydroxide iridium (mol):Nitric acid (mol)=
1:Nitric acid iridium solution, Chloride residue is made after being dissolved with 10% nitric acid solution in 3.1 ratio<3ppm.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (4)
1. a kind of method for preparing nitric acid iridium solution, it is characterised in that include the following steps：
（1）Potassium hexachloroiridate is prepared using ammonium chloroiridate；
（2）The potassium hexachloroiridate being prepared is reacted with potassium hydroxide and generates hydroxide iridium：
（3）The hydroxide iridium being prepared is dissolved in nitric acid, nitric acid iridium solution is made.
2. preparing the method for nitric acid iridium solution according to claim 1, it is characterised in that：The step（1）In, potassium hexachloroiridate
Preparation method it is as follows：By ammonium chloroiridate（g）:Chloroazotic acid（ml）=1:4 ratio mixes, and filters after ammonium chloroiridate all dissolution
A small amount of insoluble matter is removed, by ammonium chloroiridate（g）:Potassium chloride (g)=1:Potassium chloride is added in the ratio of 0.4-0.5, and reaction temperature is
50-60 DEG C, reaction time 3-4h.
3. preparing the method for nitric acid iridium solution according to claim 1, it is characterised in that：The step（2）In, hydroxide iridium
Preparation process be, by potassium hexachloroiridate（g）：Potassium hydroxide (g)：Water (ml)=1:0.5-0.55:The ratio of 10-11 mixes, reaction
Temperature is 70-80 DEG C.
4. preparing the method for nitric acid iridium solution according to claim 1, it is characterised in that：The step（3）In, hydroxide iridium
(mol):Nitric acid (mol)=1:3-3.1, reaction temperature are room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811111110.XA CN108821354B (en) | 2018-09-22 | 2018-09-22 | Method for preparing iridium nitrate solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811111110.XA CN108821354B (en) | 2018-09-22 | 2018-09-22 | Method for preparing iridium nitrate solution |
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| Publication Number | Publication Date |
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| CN108821354A true CN108821354A (en) | 2018-11-16 |
| CN108821354B CN108821354B (en) | 2020-10-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811111110.XA Active CN108821354B (en) | 2018-09-22 | 2018-09-22 | Method for preparing iridium nitrate solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114074959A (en) * | 2020-08-21 | 2022-02-22 | 中国石油化工股份有限公司 | Iridium-containing solution, preparation method of iridium hydroxide and application of iridium hydroxide |
| CN116177626A (en) * | 2023-02-17 | 2023-05-30 | 派瑞科技有限公司 | Method for preparing iridium nitrate solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116243A (en) * | 1995-04-17 | 1996-02-07 | 中国有色金属工业总公司昆明贵金属研究所 | Method for making pure iridium |
| CN101985696A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting iridium from iridium containing materials |
| 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 |
-
2018
- 2018-09-22 CN CN201811111110.XA patent/CN108821354B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1116243A (en) * | 1995-04-17 | 1996-02-07 | 中国有色金属工业总公司昆明贵金属研究所 | Method for making pure iridium |
| CN101985696A (en) * | 2010-12-01 | 2011-03-16 | 金川集团有限公司 | Method for extracting iridium from iridium containing materials |
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 王希通等: "《简明化学方程式辞典》", 30 September 1989 * |
| 马世昌: "《基础化学反应》", 31 January 2003 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114074959A (en) * | 2020-08-21 | 2022-02-22 | 中国石油化工股份有限公司 | Iridium-containing solution, preparation method of iridium hydroxide and application of iridium hydroxide |
| CN114074959B (en) * | 2020-08-21 | 2024-02-13 | 中国石油化工股份有限公司 | Iridium-containing solution, preparation method of iridium hydroxide and application of iridium hydroxide |
| CN116177626A (en) * | 2023-02-17 | 2023-05-30 | 派瑞科技有限公司 | Method for preparing iridium nitrate solution |
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| CN108821354B (en) | 2020-10-16 |
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