CN108941597A - A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt - Google Patents
A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt Download PDFInfo
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- CN108941597A CN108941597A CN201810852465.8A CN201810852465A CN108941597A CN 108941597 A CN108941597 A CN 108941597A CN 201810852465 A CN201810852465 A CN 201810852465A CN 108941597 A CN108941597 A CN 108941597A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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Abstract
The invention discloses a kind of methods for preparing Ultrafine Platinum Powder by slightly solubility platinum salt, specifically: taking a certain amount of ammonium chloroplatinate solid to be added in deionized water, adjusting water phase pH with acid solution is 0.5~3, and heating, maintenance system temperature is 60~80 DEG C；The aqueous formic acid of 2~4 times of platinum theoretical amount of reduction is weighed, spare as reducing agent, formic acid content is greater than 85% in aqueous solution；The glycol water of 10~15wt% of compound concentration, it is spare as dispersing agent；Under agitation, be added dispersing agent into platiniferous water phase first, it is to be mixed uniformly after, reducing agent is slowly added dropwise into platiniferous water phase, during which with the pH value of acid solution adjustment system, maintains between 0.5~3；After adding reducing agent, it is stirred for 0.5~1h；Ultrafine Platinum Powder is obtained after filtration, washing and drying.The present invention uses solid phase reduction method, and ammonium chloroplatinate solid obtained in production process is directly restored as reducing agent, simplify production procedure by formic acid.
Description
Technical field
The invention belongs to technical field of resource recovery, are related to the recycling of noble metal platinum, and in particular to one kind is by indissoluble
The method that property platinum salt prepares Ultrafine Platinum Powder.
Background technique
Ultrafine Platinum Powder is widely used in the preparation of electronics industry thick film ink, such as platinum electrode slurry, platinum palladium electrode slurry, platinum
Gold electrode slurry etc. can produce the catalysis platinum electrode in automotive oxygen sensor and solar battery with these slurries, temperature passes
The platinum electrode of sensor and other electrodes or conducting wire for needing that there is high catalytic activity, high reliability.Ultrafine Platinum Powder is as platinum electricity
Main functionality phase in the slurry of pole, pattern, phase analyzed laser-light scattering, dispersibility etc. all generate great shadow to the property of slurry
It rings, finally the service performance of the electronic device of preparation is impacted.
Chinese patent application CN 102717090A discloses a kind of method for preparing Ultrafine Platinum Powder using liquid phase reduction,
Including preparing platinum salt solution, the pH value for adjusting platinum salt solution is 2~7, and under stirring, resulting platinum salt solution is added dropwise to
In the mixed solution of reducing solution and dispersing agent, continue to be stirred to react 10~30min after platinum salt solution drips, reaction is generated
Product be filtered, washed, dry after obtain Ultrafine Platinum Powder.The starting material of this method is soluble platinum salt, is needed soluble platinum
Salt is soluble in water, is then restored under conditions of dispersing agent is added with reducing agent, can not handle slightly solubility platinum salt.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing Ultrafine Platinum Powder by slightly solubility platinum salt, starting material is slightly solubility platinum
Salt.
To achieve the above object, The technical solution adopted by the invention is as follows:
A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt, specifically includes the following steps:
(1) preparation of platiniferous water phase: a certain amount of ammonium chloroplatinate solid is taken to be added in deionized water, the volume of deionized water
Ratio with ammonium chloroplatinate solid masses is 20~25:1 (ml/g)；
(2) adjustment of platiniferous aqueous pH values: adjusting water phase pH with acid solution is 0.5~3, and the acid solutions are 0.1
~0.5mol/L；
(3) adjustment of platiniferous water phase temperature: heating, maintenance system temperature are 60~80 DEG C；
(4) preparation of reducing solution: weighing the aqueous formic acid of 2~4 times of platinum theoretical amount of reduction, spare as reducing agent,
Formic acid content is greater than 85% in aqueous solution；
(5) preparation of dispersing agent: the glycol water of 10~15wt% of compound concentration, it is spare as dispersing agent；
(6) preparation of Ultrafine Platinum Powder: under agitation, being added dispersing agent into platiniferous water phase first, to be mixed uniform
Afterwards, reducing agent is slowly added dropwise into platiniferous water phase, during which with the pH value of acid solution adjustment system, maintains between 0.5~3；Add
After complete reducing agent, it is stirred for 0.5~1h；Ultrafine Platinum Powder is obtained after filtration, washing and drying.
Preferably, in step (6), the volume of the dispersing agent is the 0.5~1% of platiniferous water phase volume.
Preferably, in step (6), the rate of addition of the reducing agent is 1~5mL/ (minL).
Preferably, in step (3), heating method is heating water bath.
Preferably, in step (2) and step (6), the acid solution is hydrochloric acid solution.
Preferably, in step (6), the mixing speed is 200~400r/min.
Compared with prior art, the invention has the following beneficial effects:
1, the present invention is directly gone back ammonium chloroplatinate solid obtained in production process using solid phase reduction method
Original, it is not necessary that platinum powder is first made in ammonium chloroplatinate solid, platinum powder redissolution prepares chloroplatinic acid, simplifies production procedure, has saved energy
Consumption.
2, the present invention is using formic acid as reducing agent, and compared to hydrazine hydrate, formaldehyde etc., formic acid cost is lower.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Fig. 2 is the transmission electron microscope picture of Ultrafine Platinum Powder made from the embodiment of the present invention 1.
Fig. 3 is the transmission electron microscope picture of Ultrafine Platinum Powder made from the embodiment of the present invention 2.
Fig. 4 is the transmission electron microscope picture of Ultrafine Platinum Powder made from the embodiment of the present invention 3.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments.
Reagent used in following embodiment is unless otherwise specified commercial goods reagent, and purity is that analysis is pure.
Embodiment 1
A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt, process flow referring to Fig. 1, specifically includes the following steps:
(1) preparation of platiniferous water phase: weighing 30g ammonium chloroplatinate solid in 1L beaker, and 600ml deionized water is added, goes
The volume of ionized water and the ratio of ammonium chloroplatinate solid masses are 20:1 (ml/g), are stirred evenly；
(2) adjustment of platiniferous aqueous pH values: being added dropwise the hydrochloric acid solution of 0.1mol/L under stirring, and adjustment water phase pH is
0.5；
(3) adjustment of platiniferous water phase temperature: beaker being put into water-bath and is heated, and maintenance system temperature is 60 DEG C；
(4) preparation of reducing solution: 29.2g aqueous formic acid is weighed in 100ml beaker, formic acid content is greater than in aqueous solution
85%, aqueous formic acid dosage is 4 times for restoring platinum theoretical amount；
(5) preparation of dispersing agent: the aqueous solution of the ethylene glycol containing 10wt% is prepared, takes 3ml spare；
(6) preparation of Ultrafine Platinum Powder: under conditions of low whipping speed is 200r/min, being firstly added dispersing agent, to be mixed
After uniformly, reducing agent is slowly added dropwise into solution, rate of addition is 1mL/ (minL), during which with the hydrochloric acid solution of 0.1mol/L
The pH value of adjustment system, maintains 0.5；After adding reducing agent, it is stirred for 0.5h, the product for then generating reaction filters, and washes
It washs, obtains Ultrafine Platinum Powder after dry.
Ultrafine Platinum Powder particle manufactured in the present embodiment is uniform spherical shape, and average grain diameter is 200nm or so, soilless sticking,
Transmission electron microscope photo is as shown in Figure 2.
Embodiment 2
A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt, process flow referring to Fig. 1, specifically includes the following steps:
(1) preparation of platiniferous water phase: weighing 30g ammonium chloroplatinate solid in 1L beaker, and 690ml deionized water is added, goes
The volume of ionized water and the ratio of ammonium chloroplatinate solid masses are 23:1 (ml/g), are stirred evenly；
(2) adjustment of platiniferous aqueous pH values: being added dropwise the hydrochloric acid solution of 0.3mol/L under stirring, and adjustment water phase pH is
1；
(3) adjustment of platiniferous water phase temperature: beaker being put into water-bath and is heated, and maintaining temperature is 70 DEG C；
(4) preparation of reducing solution: 21.9g aqueous formic acid is weighed in 100ml beaker, formic acid content is greater than in aqueous solution
85%, aqueous formic acid dosage is 3 times for restoring platinum theoretical amount；
(5) preparation of dispersing agent: the aqueous solution of the ethylene glycol containing 10wt% is prepared, takes 5ml spare；
(6) preparation of Ultrafine Platinum Powder: under conditions of low whipping speed is 300r/min, being firstly added dispersing agent, to be mixed
After uniformly, reducing agent is slowly added dropwise into solution, rate of addition is 3mL/ (minL), during which with the hydrochloric acid solution of 0.3mol/L
The pH value of adjustment system, maintains 1；After adding reducing agent, it is stirred for 1h；The product that then reaction is generated filters, and washs, and does
Ultrafine Platinum Powder is obtained after dry.
Ultrafine Platinum Powder particle manufactured in the present embodiment is uniform spherical shape, and average grain diameter is 300nm or so, soilless sticking,
Transmission electron microscope photo is as shown in Figure 3.
Embodiment 3
A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt, process flow referring to Fig. 1, specifically includes the following steps:
(1) preparation of platiniferous water phase: weighing 30g ammonium chloroplatinate solid in 1L beaker, and 750ml deionized water is added, goes
The volume of ionized water and the ratio of ammonium chloroplatinate solid masses are 25:1 (ml/g), are stirred evenly；
(2) adjustment of platiniferous aqueous pH values: being added dropwise the hydrochloric acid solution of 0.5mol/L under stirring, and adjustment water phase pH is
3；
(3) adjustment of platiniferous water phase temperature: beaker being put into water-bath and is heated, and maintaining temperature is 80 DEG C；
(4) preparation of reducing solution: weighing 14.6g formic acid in 100ml beaker, and formic acid content is greater than 85% in aqueous solution,
Formic acid dosage is 2 times for restoring platinum theoretical amount；
(5) preparation of dispersing agent: the aqueous solution of the ethylene glycol containing 10wt% is prepared, takes 6ml spare；
(6) preparation of Ultrafine Platinum Powder: under conditions of low whipping speed is 400r/min, being firstly added dispersing agent, to be mixed
After uniformly, reducing agent is slowly added dropwise into solution, rate of addition is 5mL/ (minL), during which with the hydrochloric acid solution of 0.5mol/L
The pH value of adjustment system, maintains 3；After adding reducing agent, it is stirred for 1h；The product that then reaction is generated filters, and washs, and does
Ultrafine Platinum Powder is obtained after dry.
Ultrafine Platinum Powder particle manufactured in the present embodiment is uniform spherical shape, and average grain diameter is 250nm or so, slight to reunite,
Its transmission electron microscope photo is as shown in Figure 4.
Claims (6)
1. a kind of method for preparing Ultrafine Platinum Powder by slightly solubility platinum salt, which comprises the following steps:
(1) preparation of platiniferous water phase: a certain amount of ammonium chloroplatinate solid is taken to be added in deionized water, the volume and chlorine of deionized water
The ratio of platinic acid ammonium solid masses is 20~25:1 (ml/g)；
(2) adjustment of platiniferous aqueous pH values: with acid solution adjust water phase pH be 0.5~3, the acid solutions be 0.1~
0.5mol/L；
(3) adjustment of platiniferous water phase temperature: heating, maintenance system temperature are 60~80 DEG C；
(4) preparation of reducing solution: weighing the aqueous formic acid of 2~4 times of platinum theoretical amount of reduction, spare as reducing agent, water-soluble
Formic acid content is greater than 85% in liquid；
(5) preparation of dispersing agent: the glycol water of 10~15wt% of compound concentration, it is spare as dispersing agent；
(6) preparation of Ultrafine Platinum Powder: under agitation, being added dispersing agent into platiniferous water phase first, it is to be mixed uniformly after, delay
Slowly reducing agent is added dropwise into platiniferous water phase, during which with the pH value of acid solution adjustment system, maintains between 0.5~3；Add reduction
After agent, it is stirred for 0.5~1h；Ultrafine Platinum Powder is obtained after filtration, washing and drying.
2. the method according to claim 1 for preparing Ultrafine Platinum Powder by slightly solubility platinum salt, which is characterized in that in step (6),
The volume of the dispersing agent is the 0.5~1% of platiniferous water phase volume.
3. the method according to claim 1 or 2 for preparing Ultrafine Platinum Powder by slightly solubility platinum salt, which is characterized in that step (6)
In, the rate of addition of the reducing agent is 1~5mL/ (minL).
4. the method according to claim 1 or 2 for preparing Ultrafine Platinum Powder by slightly solubility platinum salt, which is characterized in that step (3)
In, heating method is heating water bath.
5. the method according to claim 1 or 2 for preparing Ultrafine Platinum Powder by slightly solubility platinum salt, which is characterized in that step (2)
In step (6), the acid solution is hydrochloric acid.
6. the method according to claim 1 or 2 for preparing Ultrafine Platinum Powder by slightly solubility platinum salt, which is characterized in that step (6)
In, the mixing speed is 200~400r/min.
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| CN201810852465.8A CN108941597A (en) | 2018-07-27 | 2018-07-27 | A method of Ultrafine Platinum Powder is prepared by slightly solubility platinum salt |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115948659A (en) * | 2022-12-06 | 2023-04-11 | 昆明贵研催化剂有限责任公司 | Method for recovering superfine platinum powder from preparation tail liquid of platinum compound |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294416A (en) * | 1989-05-09 | 1990-12-05 | Ishifuku Kinzoku Kogyo Kk | Production of platinum powder |
| CN102717090A (en) * | 2011-03-31 | 2012-10-10 | 北京有色金属研究总院 | Method for preparing ultrafine platinum powder by adopting liquid-phase reduction |
| CN103341636A (en) * | 2013-07-08 | 2013-10-09 | 重庆材料研究院有限公司 | Method for preparing fine platinum powder used for negative electrode fine platinum wire in intensified thermocouple wires |
| CA2843532A1 (en) * | 2013-03-05 | 2014-09-05 | Heraeus Precious Metals Gmbh & Co. Kg | Method for producing highly pure platinum powder, as well as platinum powder that can be obtained according to said method, and use thereof |
| JP2014169484A (en) * | 2013-03-04 | 2014-09-18 | Sumitomo Metal Mining Co Ltd | Method for producing platinum powder |
| CN107838434A (en) * | 2017-10-30 | 2018-03-27 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity platinum powder |
-
2018
- 2018-07-27 CN CN201810852465.8A patent/CN108941597A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02294416A (en) * | 1989-05-09 | 1990-12-05 | Ishifuku Kinzoku Kogyo Kk | Production of platinum powder |
| CN102717090A (en) * | 2011-03-31 | 2012-10-10 | 北京有色金属研究总院 | Method for preparing ultrafine platinum powder by adopting liquid-phase reduction |
| JP2014169484A (en) * | 2013-03-04 | 2014-09-18 | Sumitomo Metal Mining Co Ltd | Method for producing platinum powder |
| CA2843532A1 (en) * | 2013-03-05 | 2014-09-05 | Heraeus Precious Metals Gmbh & Co. Kg | Method for producing highly pure platinum powder, as well as platinum powder that can be obtained according to said method, and use thereof |
| CN103341636A (en) * | 2013-07-08 | 2013-10-09 | 重庆材料研究院有限公司 | Method for preparing fine platinum powder used for negative electrode fine platinum wire in intensified thermocouple wires |
| CN107838434A (en) * | 2017-10-30 | 2018-03-27 | 贵研铂业股份有限公司 | A kind of preparation method of high-purity platinum powder |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115948659A (en) * | 2022-12-06 | 2023-04-11 | 昆明贵研催化剂有限责任公司 | Method for recovering superfine platinum powder from preparation tail liquid of platinum compound |
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