CN109513946A - A kind of apparatus and method preparing big partial size palladium powder - Google Patents
A kind of apparatus and method preparing big partial size palladium powder Download PDFInfo
- Publication number
- CN109513946A CN109513946A CN201811281130.1A CN201811281130A CN109513946A CN 109513946 A CN109513946 A CN 109513946A CN 201811281130 A CN201811281130 A CN 201811281130A CN 109513946 A CN109513946 A CN 109513946A
- Authority
- CN
- China
- Prior art keywords
- palladium
- reaction kettle
- reducing agent
- catheter
- kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 104
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 60
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 48
- 230000007246 mechanism Effects 0.000 claims abstract description 27
- 238000011085 pressure filtration Methods 0.000 claims abstract description 14
- 238000003860 storage Methods 0.000 claims abstract description 14
- 230000003028 elevating effect Effects 0.000 claims abstract description 13
- 230000014759 maintenance of location Effects 0.000 claims abstract description 8
- 238000005086 pumping Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 6
- 239000002699 waste material Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000002912 waste gas Substances 0.000 claims description 4
- 229910001868 water Inorganic materials 0.000 claims description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 150000002940 palladium Chemical class 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- TVEXGJYMHHTVKP-UHFFFAOYSA-N 6-oxabicyclo[3.2.1]oct-3-en-7-one Chemical compound C1C2C(=O)OC1C=CC2 TVEXGJYMHHTVKP-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Classifications
-
- 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
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
It include palladium solution reservoir the invention discloses a kind of apparatus and method for preparing big partial size palladium powder, reducing agent storage tank, palladium solution catheter, negative-pressure liquid suction pipe, reaction kettle, reaction kettle elevating mechanism, fixed frame, reducing agent catheter, the reaction kettle is fitted on hanger bracket by reaction kettle elevating mechanism, the hanger bracket two sides are fitted on fixed frame by rotation axis, the reaction kettle top is connect by retention mechanism with kettle cover, the kettle cover is fixed at the fixed frame top, it is connect by palladium solution catheter with the liquid outlet of palladium solution reservoir bottom at the top of the kettle cover, valve is provided on the palladium solution catheter, it is connect by reducing agent catheter with the liquid outlet of reducing agent tank bottom at the top of the kettle cover, valve is provided on the reducing agent catheter, negative-pressure liquid suction pipe one end and pumping equipment connect It connects, the negative-pressure liquid suction pipe other end is coupled negative pressure filtration mouth, and the negative pressure filtration mouth is set to reaction kettle inner wall bottom.
Description
Technical field
The present invention relates to big partial size palladium powder preparation technique technical field, in particular to a kind of device for preparing big partial size palladium powder
With method.
Background technique
Palladium powder is main raw material(s) needed for various palladium class Related products, is usually used in electronics, chemical industry, automobile, military project, boat
The fields such as it.Palladium is a kind of efficient catalyst, is chiefly used in preparing the catalyst of petroleum, chemical industry and automobile industry.
The preparation method of palladium powder is various, is broadly divided into physical method and chemical method, and physical method includes high energy mechanical
Ball-milling method, atomization, evaporative condenser hair, chemical method mainly includes chemical reduction method, salt decomposition method.Chemical reduction method mainly wraps
Include solution phase chemical reduction, electrochemical reducing, photochemical reduction.According to the market demand, palladium powder prepares manufacturer, height at present
Main attention is invested ultra-fine and superfine alloy palladium powder preparation and research by school and scientific research institutions, and is ground to large-sized palladium powder
Study carefully less.The long electrocondution slurry for being used for electronics industry in ultrafine palladium powder end, and such height is then not necessarily in some other palladium application field
The material of cost.Since part is only to re-dissolve the palladium powder that buying comes to be used to produce it using palladium powder as the enterprise of raw material
Its palladium class product, therefore thinner palladium powder not only increases the production cost of upstream firm, and be easy to produce oxidation, water suction and
The problems such as dust collector.
Summary of the invention
In view of the above technical problems, the present invention provides a kind of apparatus and method for preparing big partial size palladium powder.
To achieve the goals above, technical solution of the present invention is specific as follows:
A kind of device preparing big partial size palladium powder, including palladium solution reservoir, reducing agent storage tank, palladium solution catheter, negative-pressure liquid suction
Pipe, reaction kettle, reaction kettle elevating mechanism, fixed frame, reducing agent catheter, the reaction kettle are cooperated by reaction kettle elevating mechanism
It is mounted on hanger bracket, the hanger bracket two sides are fitted on fixed frame by rotation axis, and the reaction kettle top passes through
Retention mechanism is connect with kettle cover, and the kettle cover is fixed at the fixed frame top, is led at the top of the kettle cover by palladium solution
Liquid pipe is connect with the liquid outlet of palladium solution reservoir bottom, and valve is provided on the palladium solution catheter, is led at the top of the kettle cover
It crosses reducing agent catheter to connect with the liquid outlet of reducing agent tank bottom, is provided with valve on the reducing agent catheter, it is described
Negative-pressure liquid suction pipe one end is connect with pumping equipment, and the negative-pressure liquid suction pipe other end is coupled negative pressure filtration mouth, the negative pressure
Filter tip is set to reaction kettle inner wall bottom, and the reaction kettle is internally provided with rabbling mechanism.
Waste gas exhaust pipe is provided at the top of the reaction kettle.
The palladium solution reservoir is internally provided with agitating paddle, and the shaft and electric machine main shaft of the agitating paddle are cooperatively connected, institute
Motor is stated to be set at the top of the palladium solution reservoir.
The reducing agent catheter is connect by flow controller with the liquid outlet of the reducing agent tank bottom.
The rabbling mechanism includes variable-frequency motor, belt type spiral blender, and the belt type spiral blender is set to described
Inside reaction kettle, the variable-frequency motor is set at the top of the reaction kettle, the shaft and the change of the belt type spiral blender
The main shaft of frequency motor is cooperatively connected.
Flexible heater set is provided with outside the reaction kettle.
The invention also discloses a kind of application methods of device for preparing big partial size palladium powder, include the following steps:
Step 1: in palladium solution reservoir, palladium complex Pd (NH is added3)4Cl2Solution, while deionized water be added make solution
Palladium concentration reach 50-100g/L；
Step 2: being packed into liquid reducer into reducing agent storage tank；
Step 3: opening the valve on palladium solution catheter flows into palladium solution in reaction kettle by palladium solution catheter, palladium solution
Liquid level closes valve when reaching 5L；
Step 4: opening the valve on reducing agent catheter, and the speed that reaction kettle is added in reducing agent is controlled by flow controller
Degree, it is 10-40ml/min that speed, which is added, in reducing agent；
Step 5: reaction starts to carry out, and starts variable-frequency motor, and the revolving speed of belt type spiral blender is 5-20r/min, works as reaction kettle
In when no longer generating bubble, and when solution ph reaches 10 in reaction kettle, close the valve on reducing agent catheter, stop being added
Reducing agent, and belt type spiral agitator speed improved and persistently stirs 2-5min to 20-40 r/min and turns off variable-frequency motor；
Step 6: the nozzle of negative-pressure liquid suction pipe being put into reaction kettle portion, is exported waste reaction solution in reaction kettle using negative pressure filtration mouth
The negative pressure filtration mouth of autoclave body, negative-pressure liquid suction pipe nozzle completely cuts off palladium powder in kettle, takes out negative-pressure liquid suction pipe after waste liquid is discharged；
Step 7: repeating operation 5-10 times of step 3-6；
Step 8: open reaction kettle top and kettle cover retention mechanism, by reaction kettle elevating mechanism by reaction kettle from hanger bracket
It falls, rotates hanger bracket, reaction kettle is made to vert, the big partial size palladium powder that reaction obtains is poured out, is cleaned repeatedly using deionized water
Palladium powder, until the pH value of washing lotion reaches 6-7, after drying, grading, the uniform palladium powder that granularity reaches 2mm will carry out palladium powder
Sale, for palladium powder of the granularity lower than 2mm when prepared by lower batch palladium powder, step 3-6 can directly be carried out by being fitted into reaction kettle in advance
Operation.
Wherein, the palladium complex Pd (NH in the step 13)4Cl2Solution, be Pd (NH3)2Cl2With NH3·H2O reaction
What production obtained.
Wherein, in step 1, reactant is carried out by flexible heater set in operating process to be heated to 80 degrees Celsius, to add
Fast response process.
The beneficial effects of the present invention are:
1, according to the market demand, varigrained big partial size can be prepared by the cycle-index and speed of agitator for changing liquid feeding reaction
Palladium powder, powder obtained is pollution-free, not oxidizable, water suction, does not fly upward phenomenon, and powder tap density is high.
2, the device structure is simple to operation, and when production can observe palladium powder growing state, high production efficiency in kettle at any time.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the device that the present invention prepares big partial size palladium powder.
Fig. 2 is the process flow chart for the device application method that the present invention prepares big partial size palladium powder.
Wherein, 1-palladium solution reservoir, 2-reducing agent storage tank, 3-motor, 4-variable-frequency motor, 5-palladium solution catheter,
6-waste gas exhaust pipe, 7-negative-pressure liquid suction pipe, 8-flow controller, 9-reaction kettle, 10-reaction kettle elevating mechanism, 11-band
Formula spiral agitator, 12-hanger bracket, 13-fixed frame, 14-reducing agent catheter.
Specific embodiment
Embodiment 1
As shown in Figure 1, a kind of device for preparing big partial size palladium powder, including palladium solution reservoir 1, reducing agent storage tank 2, palladium solution drain
Pipe 5, negative-pressure liquid suction pipe 7, reaction kettle 9, reaction kettle elevating mechanism 10, fixed frame 13, reducing agent catheter 14, reaction kettle 9 pass through
Reaction kettle elevating mechanism 10 is fitted on hanger bracket 12, and 12 two sides of hanger bracket are fitted to fixed frame 13 by rotation axis
On, 9 top of reaction kettle is connect by retention mechanism with kettle cover, and kettle cover is fixed at 13 top of fixed frame, is passed through at the top of kettle cover
Palladium solution catheter 5 is connect with the liquid outlet of 1 bottom of palladium solution reservoir, and valve, kettle cover top are provided on palladium solution catheter 5
It is connect by reducing agent catheter 14 with the liquid outlet of 2 bottom of reducing agent storage tank, is provided with valve on reducing agent catheter 14, born
Pressure 7 one end of pipette is connect with pumping equipment, and 7 other end of negative-pressure liquid suction pipe is coupled negative pressure filtration mouth, and negative pressure filtration mouth is set
It is placed in 9 inner wall bottom of reaction kettle, reaction kettle 9 is internally provided with rabbling mechanism, waste gas exhaust pipe 6, palladium are provided at the top of reaction kettle 9
Solution reservoir 1 is internally provided with agitating paddle, and the shaft and 3 main shaft of motor of agitating paddle are cooperatively connected, and motor 3 is set to the storage of palladium solution
1 top of tank, reducing agent catheter 14 are connect by flow controller 8 with the liquid outlet of 2 bottom of reducing agent storage tank, rabbling mechanism packet
Variable-frequency motor 4, belt type spiral blender 11 are included, belt type spiral blender 11 is set to inside reaction kettle 9, and variable-frequency motor 4 is arranged
In 9 top of reaction kettle, the shaft of belt type spiral blender 11 and the main shaft of variable-frequency motor 4 are cooperatively connected, and are arranged outside reaction kettle 9
Flexible heating mantle.
As shown in Fig. 2, a kind of application method for the device for preparing big partial size palladium powder, includes the following steps:
Step 1: in palladium solution reservoir 1, being added by Pd (NH3)2Cl2With NH3·H2The palladium complex Pd that O reaction production obtains
(NH3)4Cl2Solution, while deionized water, which is added, makes the palladium concentration of solution reach 50g/L, passes through flexible heater in operating process
Set carries out reactant to be heated to 80 degrees Celsius, to accelerate reaction process；
Step 2: being packed into liquid reducer into reducing agent storage tank 2；
Step 3: opening the valve on palladium solution catheter 5 flows into palladium solution in reaction kettle 9 by palladium solution catheter 5, palladium
Solution level closes valve when reaching 5L；
Step 4: opening the valve on reducing agent catheter 14, and reducing agent is controlled by flow controller 8, reaction kettle 9 is added
Speed, it is 10ml/min that speed, which is added, in reducing agent；
Step 5: reaction starts to carry out, and starts variable-frequency motor 4, the revolving speed of belt type spiral blender 11 is 5r/min, when reaction kettle 9
In when no longer generating bubble, and when solution ph reaches 10 in reaction kettle 9, close the valve on reducing agent catheter 14, stop
Reducing agent is added, and 11 revolving speed of belt type spiral blender improved and persistently stirs 2min to 20 r/min and turns off variable-frequency motor 4；
Step 6: the nozzle of negative-pressure liquid suction pipe 7 being put into 9 bottom of reaction kettle, will react useless in reaction kettle 9 using negative pressure filtration mouth
Liquid exports autoclave body, and the negative pressure filtration mouth of 7 nozzle of negative-pressure liquid suction pipe completely cuts off palladium powder in kettle, takes out negative pressure after waste liquid is discharged
Pipette 7；
Step 7: repeating operation 5 times of step 3-6；
Step 8: the retention mechanism on reaction kettle 9 top and kettle cover is opened, by reaction kettle elevating mechanism 10 by reaction kettle 9 from suspension
It is fallen on frame 12, rotates hanger bracket 12, reaction kettle 9 is made to vert, the big partial size palladium powder that reaction obtains is poured out, uses deionized water
Palladium powder is cleaned repeatedly, until the pH value of washing lotion reaches 6, for palladium powder after drying, grading, granularity reaches the uniform palladium powder of 2mm
It will sell, when prepared by lower batch palladium powder, be fitted into reaction kettle 9 in advance directly to carry out palladium powder of the granularity lower than 2mm
The operation of step 3-6.
Embodiment 2
As shown in Fig. 2, a kind of application method for the device for preparing big partial size palladium powder, includes the following steps:
Step 1: in palladium solution reservoir 1, being added by Pd (NH3)2Cl2With NH3·H2The palladium complex Pd that O reaction production obtains
(NH3)4Cl2Solution, while deionized water, which is added, makes the palladium concentration of solution reach 100g/L, in operating process by flexible plus
Hot jacket carries out reactant to be heated to 80 degrees Celsius, to accelerate reaction process；
Step 2: being packed into liquid reducer into reducing agent storage tank 2；
Step 3: opening the valve on palladium solution catheter 5 flows into palladium solution in reaction kettle 9 by palladium solution catheter 5, palladium
Solution level closes valve when reaching 5L；
Step 4: opening the valve on reducing agent catheter 14, and reducing agent is controlled by flow controller 8, reaction kettle 9 is added
Speed, it is 40ml/min that speed, which is added, in reducing agent；
Step 5: reaction starts to carry out, and starts variable-frequency motor 4, and the revolving speed of belt type spiral blender 11 is 20r/min, works as reaction kettle
When no longer generating bubble in 9, and when solution ph reaches 10 in reaction kettle 9, the valve on reducing agent catheter 14 is closed, is stopped
Reducing agent is added, and 11 revolving speed of belt type spiral blender improved and persistently stirs 5min to 40 r/min and turns off variable-frequency motor 4；
Step 6: the nozzle of negative-pressure liquid suction pipe 7 being put into 9 bottom of reaction kettle, will react useless in reaction kettle 9 using negative pressure filtration mouth
Liquid exports autoclave body, and the negative pressure filtration mouth of 7 nozzle of negative-pressure liquid suction pipe completely cuts off palladium powder in kettle, takes out negative pressure after waste liquid is discharged
Pipette 7；
Step 7: repeating operation 10 times of step 3-6；
Step 8: the retention mechanism on reaction kettle 9 top and kettle cover is opened, by reaction kettle elevating mechanism 10 by reaction kettle 9 from suspension
It is fallen on frame 12, rotates hanger bracket 12, reaction kettle 9 is made to vert, the big partial size palladium powder that reaction obtains is poured out, uses deionized water
Palladium powder is cleaned repeatedly, until the pH value of washing lotion reaches 7, for palladium powder after drying, grading, granularity reaches the uniform palladium powder of 2mm
It will sell, when prepared by lower batch palladium powder, be fitted into reaction kettle 9 in advance directly to carry out palladium powder of the granularity lower than 2mm
The operation of step 3-6.
Claims (9)
1. a kind of device for preparing big partial size palladium powder, it is characterised in that: including palladium solution reservoir (1), reducing agent storage tank (2), palladium
Solution catheter (5), negative-pressure liquid suction pipe (7), reaction kettle (9), reaction kettle elevating mechanism (10), fixed frame (13), reducing agent are led
Liquid pipe (14), the reaction kettle (9) are fitted on hanger bracket (12) by reaction kettle elevating mechanism (10), the hanger bracket
(12) two sides are fitted on fixed frame (13) by rotation axis, and reaction kettle (9) top passes through retention mechanism and kettle cover
Connection, the kettle cover are fixed at the fixed frame (13) top, pass through palladium solution catheter (5) and palladium at the top of the kettle cover
The liquid outlet of solution reservoir (1) bottom connects, and valve is provided on the palladium solution catheter (5), is passed through at the top of the kettle cover
Reducing agent catheter (14) is connect with the liquid outlet of reducing agent storage tank (2) bottom, is provided on the reducing agent catheter (14)
Valve, described negative-pressure liquid suction pipe (7) one end are connect with pumping equipment, and negative-pressure liquid suction pipe (7) other end is coupled negative pressure
Filter tip, the negative pressure filtration mouth are set to the reaction kettle (9) inner wall bottom, and the reaction kettle (9) is internally provided with stirring
Mechanism.
2. a kind of device for preparing big partial size palladium powder according to claim 1, it is characterised in that: reaction kettle (9) top
Portion is provided with waste gas exhaust pipe (6).
3. a kind of device for preparing big partial size palladium powder according to claim 1, it is characterised in that: the palladium solution reservoir
(1) it is internally provided with agitating paddle, the shaft and motor (3) main shaft of the agitating paddle are cooperatively connected, and the motor (3) is set to institute
It states at the top of palladium solution reservoir (1).
4. a kind of device for preparing big partial size palladium powder according to claim 1, it is characterised in that: the reducing agent catheter
(14) it is connect by flow controller (8) with the liquid outlet of reducing agent storage tank (2) bottom.
5. a kind of device for preparing big partial size palladium powder according to claim 1, it is characterised in that: the rabbling mechanism includes
Variable-frequency motor (4), belt type spiral blender (11), the belt type spiral blender (11) are set to the reaction kettle (9) inside,
The variable-frequency motor (4) is set at the top of the reaction kettle (9), the shaft and the frequency conversion of the belt type spiral blender (11)
The main shaft of motor (4) is cooperatively connected.
6. a kind of device for preparing big partial size palladium powder according to any one of claims 1 to 5, it is characterised in that: the reaction
Flexible heater set is provided with outside kettle (9).
7. a kind of application method of device for preparing big partial size palladium powder according to claim 6, it is characterised in that: including such as
Lower step:
Step 1: in palladium solution reservoir (1), palladium complex Pd (NH is added3)4Cl2Solution, while be added deionized water make it is molten
The palladium concentration of liquid reaches 50-100g/L；
Step 2: to loading liquid reducer in reducing agent storage tank (2)；
Step 3: opening the valve on palladium solution catheter (5) makes palladium solution flow into reaction kettle (9) by palladium solution catheter (5)
In, palladium solution level closes valve when reaching 5L；
Step 4: opening the valve on reducing agent catheter (14), and control reducing agent by flow controller (8) and reaction is added
The speed of kettle (9), it is 10-40ml/min that speed, which is added, in reducing agent；
Step 5: reaction starts to carry out, and starts variable-frequency motor (4), and the revolving speed of belt type spiral blender (11) is 5-20r/min, when
When no longer generating bubble in reaction kettle (9), and when reaction kettle (9) interior solution ph reaches 10, close reducing agent catheter (14)
On valve, stop that reducing agent is added, and belt type spiral blender (11) revolving speed improved to 20-40 r/min and persistently stirs 2-
5min turns off variable-frequency motor (4)；
Step 6: the nozzle of negative-pressure liquid suction pipe (7) is put into reaction kettle (9) bottom, it will be in reaction kettle (9) using negative pressure filtration mouth
Waste reaction solution exports autoclave body, and the negative pressure filtration mouth of negative-pressure liquid suction pipe (7) nozzle completely cuts off palladium powder in kettle, after waste liquid is discharged
It takes out negative-pressure liquid suction pipe (7)；
Step 7: repeating operation 5-10 times of step 3-6；
Step 8: the retention mechanism on reaction kettle (9) top and kettle cover is opened, by reaction kettle elevating mechanism (10) by reaction kettle (9)
It is fallen from hanger bracket (12), rotates hanger bracket (12), reaction kettle (9) is made to vert, the big partial size palladium powder that reaction obtains is poured out,
Clean palladium powder repeatedly using deionized water, until the pH value of washing lotion reaches 6-7, after drying, grading, granularity reaches palladium powder
The uniform palladium powder of 2mm will be sold, and palladium powder of the granularity lower than 2mm is packed into reaction kettle (9) in advance when prepared by lower batch palladium powder
In can directly carry out the operation of step 3-6.
8. a kind of application method of device for preparing big partial size palladium powder according to claim 7, it is characterised in that: the step
Palladium complex Pd (NH in rapid 13)4Cl2Solution, be Pd (NH3)2Cl2With NH3·H2O reaction production obtains.
9. a kind of application method of device for preparing big partial size palladium powder according to claim 7 or 8, it is characterised in that: institute
It states in step 1, reactant is carried out by flexible heater set in operating process to be heated to 80 degrees Celsius, to accelerate reaction process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811281130.1A CN109513946B (en) | 2018-10-30 | 2018-10-30 | Device and method for preparing large-particle-size palladium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811281130.1A CN109513946B (en) | 2018-10-30 | 2018-10-30 | Device and method for preparing large-particle-size palladium powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109513946A true CN109513946A (en) | 2019-03-26 |
| CN109513946B CN109513946B (en) | 2020-05-15 |
Family
ID=65772738
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811281130.1A Active CN109513946B (en) | 2018-10-30 | 2018-10-30 | Device and method for preparing large-particle-size palladium powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109513946B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112657426A (en) * | 2020-12-18 | 2021-04-16 | 烟台昱晟化工新材料有限公司 | Reaction device for quickly taking out chemical raw materials and using method |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06299212A (en) * | 1993-04-14 | 1994-10-25 | Mitsubishi Materials Corp | Production of oxidation resistant palladium powder |
| JPH10330811A (en) * | 1997-06-05 | 1998-12-15 | Tanaka Kikinzoku Kogyo Kk | Production of highly crystalline palladium powder |
| CN103526233A (en) * | 2013-10-11 | 2014-01-22 | 金川集团股份有限公司 | Method for high-efficiency separation of palladium from silver electrolyte |
| CN103934470A (en) * | 2014-04-04 | 2014-07-23 | 中南大学 | Preparation method for Marks decanedron Pd nano particles |
| CN104028774A (en) * | 2014-06-11 | 2014-09-10 | 励福实业（江门）贵金属有限公司 | Activated palladium powder and preparation method and application thereof |
| CN105312589A (en) * | 2014-07-23 | 2016-02-10 | 南京理工大学 | Synthesis method of superfine palladium powder |
| CN206276381U (en) * | 2016-11-29 | 2017-06-27 | 石家庄瑞凯化工有限公司 | A kind of reactor of quick blend feedstock |
| JP2018076574A (en) * | 2016-11-11 | 2018-05-17 | 株式会社日高ファインテクノロジーズ | Method for producing palladium powder |
-
2018
- 2018-10-30 CN CN201811281130.1A patent/CN109513946B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06299212A (en) * | 1993-04-14 | 1994-10-25 | Mitsubishi Materials Corp | Production of oxidation resistant palladium powder |
| JPH10330811A (en) * | 1997-06-05 | 1998-12-15 | Tanaka Kikinzoku Kogyo Kk | Production of highly crystalline palladium powder |
| CN103526233A (en) * | 2013-10-11 | 2014-01-22 | 金川集团股份有限公司 | Method for high-efficiency separation of palladium from silver electrolyte |
| CN103934470A (en) * | 2014-04-04 | 2014-07-23 | 中南大学 | Preparation method for Marks decanedron Pd nano particles |
| CN104028774A (en) * | 2014-06-11 | 2014-09-10 | 励福实业（江门）贵金属有限公司 | Activated palladium powder and preparation method and application thereof |
| CN105312589A (en) * | 2014-07-23 | 2016-02-10 | 南京理工大学 | Synthesis method of superfine palladium powder |
| JP2018076574A (en) * | 2016-11-11 | 2018-05-17 | 株式会社日高ファインテクノロジーズ | Method for producing palladium powder |
| CN206276381U (en) * | 2016-11-29 | 2017-06-27 | 石家庄瑞凯化工有限公司 | A kind of reactor of quick blend feedstock |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112657426A (en) * | 2020-12-18 | 2021-04-16 | 烟台昱晟化工新材料有限公司 | Reaction device for quickly taking out chemical raw materials and using method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109513946B (en) | 2020-05-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109513946A (en) | A kind of apparatus and method preparing big partial size palladium powder | |
| CN104805289B (en) | The high efficiente callback automation equipment of cadmium ion and recovery method in a kind of high cadmium solution | |
| CN205925710U (en) | From reation kettle who takes circulation water purification device | |
| CN205435740U (en) | A heatable reation kettle for chemical industry industry | |
| CN115427138A (en) | Multiphase interface reactor | |
| CN108097189A (en) | A kind of chemical industry energy conservation and environmental protection reaction kettle | |
| CN205570297U (en) | Can regulate and control stirring reation kettle of temperature automatically | |
| CN206325413U (en) | A kind of dissolution kettle | |
| CN211436048U (en) | Device for mixing alkaline vanadium-containing material and vanadium-containing clinker | |
| CN208512543U (en) | A kind of reaction kettle with cleaning function | |
| CN206762870U (en) | A kind of intensified by ultrasonic wave leaching device | |
| CN205586978U (en) | Multifunctional reactor | |
| CN205379866U (en) | Intelligence chemical industry reation kettle | |
| CN207591849U (en) | A kind of reaction kettle with double temperature control | |
| CN209352924U (en) | A kind of pyridine carboxylic acid biological enzyme reactor | |
| CN206642707U (en) | A kind of high-order dropping tank | |
| CN207391292U (en) | Amino acid Water soluble fertilizer process units | |
| CN208018607U (en) | A kind of vacuum feed reaction kettle | |
| CN208497368U (en) | Vertical blender for plastics | |
| CN207576392U (en) | A kind of chemical industry energy conservation and environmental protection reaction kettle | |
| CN107350481A (en) | The preparation method and system of a kind of super-fine cobalt powder | |
| CN211539478U (en) | Silver nanoparticle manufacturing installation based on mao bamboo hemicellulose | |
| CN215689937U (en) | Fluidized bed coating machine | |
| CN220737489U (en) | High-efficient reation kettle | |
| CN214514514U (en) | Reaction device for preparing nano magnesium hydroxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20240321 Address after: 737199 No. 2 Jianshe Road, Jinchuan District, Jinchang City, Gansu Province (east of Beijing Road, west of Heya Road, south of Guiyang Road) Patentee after: Jinchuan Group Copper Gui Co.,Ltd. Country or region after: Zhong Guo Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: Zhong Guo |
|
| TR01 | Transfer of patent right |