CN110194903A - Chemical reaction kettle and the processing method for using the chemical reaction kettle - Google Patents
Chemical reaction kettle and the processing method for using the chemical reaction kettle Download PDFInfo
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- CN110194903A CN110194903A CN201910363503.8A CN201910363503A CN110194903A CN 110194903 A CN110194903 A CN 110194903A CN 201910363503 A CN201910363503 A CN 201910363503A CN 110194903 A CN110194903 A CN 110194903A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/62—Metallic pigments or fillers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/62—Metallic pigments or fillers
- C09C1/627—Copper
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/066—Treatment or coating resulting in a free metal containing surface-region
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/04—Aqueous dispersions
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Abstract
The invention discloses a kind of chemical reaction kettle and use the processing method of the chemical reaction kettle, it include: driving device, pass through driving device driving and the internal ball milling cylinder for having multiple abrasive material balls, the ball milling bracket of mounting ball grinding cylinder, the ball milling cylinder is equipped with multiple valves for connecting gas pipeline and mouth is added dropwise in reaction solution, the switch block of the inlet port and outlet port and corresponding inlet port and outlet port positioned at different height is additionally provided in the cambered surface of the ball milling cylinder, the both ends of the ball milling cylinder are equipped with electroheat pair panel.The present invention carries out the ball milling in sheet composite conductive powder production process, silver-plated and the multiple steps of polishing, concentration in the same apparatus, saves a large amount of manpower and material resources, save the cost, while reducing the consume that material is generated in equipment room transfer.
Description
Technical field
The present invention relates to chemical preparation fields, more particularly to a kind of chemical reaction kettle and adding using the chemical reaction kettle
Work method.
Background technique
As electronic component is intended to lighting, miniaturization, the demand of conductive powder is continuously increased.Conductive powder
In, the resistivity of silver powder is low, and electric conductivity is best, most widely used.But due to the at high price of silver powder and there is silver migration now
As limiting its use.Composite conductive powder be by metal material, ceramic material or high molecular material etc. two or more
Material prepared by combination process and the excellent heterogeneous material of electric conductivity, common composite conductive powder is in metal or non-
Metal powder surface coats one layer of silver layer, and the composite conducting material of this silver cladding can both reduce the cost of silver powder, but also with silver
The excellent conductive performance of powder.The common micromorphology of conductive powder be it is spherical and two kinds of sheet, in the applications such as circuit printing, piece
Contact area between sprills is bigger than globular powder, and flakelike powder arranges that the access to be formed is more continuous, and electric conductivity is more excellent
It is different.
The customary preparation methods of sheet composite conductive powder are that the ball-type metal sphere of powder is worn into sheet, then benefit using ball mill
It carries out the deposition of silver layer to sheet substrate in water phase with reaction kettle, the composite powder of silver cladding is finally put into ball mill and is carried out
The silver layer for interspersing shape is polished to continuous silver layer by the polishing of silver layer.Conventional sheet composite conductive powder preparation flow is complicated
It is cumbersome, it needs to spend more manpower and material resources, and material is that will cause certain loss in equipment room transfer.
Summary of the invention
The present invention in order to solve the problems, such as it is above-mentioned it is existing in the prior art using plurality of devices to carry out preparation inconvenient, mention
A kind of chemical reaction kettle and the processing method using the chemical reaction kettle out.
The technical solution adopted by the present invention is that:
The invention proposes a kind of chemical reaction kettles, comprising: driving device, by driving device driving and inside has multiple mills
The ball milling cylinder of pellet, the ball milling bracket of mounting ball grinding cylinder, the ball milling cylinder are equipped with multiple gas pipelines that connect
Mouth is added dropwise in valve and reaction solution, is additionally provided with the inlet port and outlet port positioned at different radial heights in the cambered surface of the ball milling cylinder
And the switch block of corresponding inlet port and outlet port, the both ends of the ball milling cylinder are equipped with electroheat pair panel.
Further, the ball milling cylinder is mounted on ball milling bracket by passing through the central axis in ball milling cylinder axle center, institute
State the both ends that the centrally disposed axis of mouth is added dropwise in reaction solution.
The invention also provides a kind of processing method of above-mentioned chemical reaction kettle, step includes:
Globular metallic powder is put into ball milling sprills in blocks in ball milling cylinder by step 1；
Step 2 obtains the substrate surface chemical silvering of flakelike powder in the silver-colored solution of reaction solution dropwise addition mouth dropwise addition and reducing solution
Sheet composite conductive powder；
Step 3 will polish sheet composite conductive powder surface in polishing fluid addition ball grinding cylinder body.
Wherein, step 1 specifically includes: by the mixture of ball-type metal powder and ball milling oil as in ball milling cylinder；It is passed through
Nitrogen makes ball milling barrel body rotation preset time t 1；Ball milling oil is filtered in discharge port after the completion of rotation.
Step 2 specifically includes: acidity alcohol solution is added, makes ball milling barrel body rotation preset time t 2；Going out after the completion of rotation
Material mouth filters acidity alcohol solution；Deionized water is added, is passed through nitrogen, ball milling cylinder is warming up to preset temperature；Ball milling
Barrel body rotation preset time t 3；Silver-colored solution and reducing agent solution, rotating ball grinding cylinder preset time t 4 is added dropwise；After the completion of rotation
The solvent that discharge port generates chemical silvering filters.
Step 3 specifically includes: polishing fluid is added from outlet material, is passed through nitrogen, ball milling barrel body rotation preset time t 5 turns
Sheet composite conductive powder is filtered out in discharge outlet after the completion of dynamic.
Preferably, the polishing fluid is made of solvent and dispersing agent, and the solvent is ethylene glycol or propylene glycol, the dispersion
Agent is anti-settling agent, rheology modified wax dispenser or aligns agent.
Further, the specific steps of the suction filtration are as follows: install strainer in discharge port, place Medium speed filter paper on strainer, filter
End connection bottle,suction and vacuum pump off the net are filtered.
Preferably, the acid alcoholic solvent is made of alcohols solvent and acidic materials, and the alcohols solvent is ethyl alcohol, isopropyl
Alcohol, n-butanol or isobutanol, acidic materials are hydrochloric acid, sulfuric acid, citric acid or stannous chloride.
Preferably, the reducing solution is tartaric acid, sodium potassium tartrate tetrahydrate or glucose.
Compared with the prior art, the present invention has the advantages that the present invention collects ball milling, deposition and polishing one, by mechanic
Industry is combined with chemical industry, is greatly reduced manpower and material resources needed for production process, is improved production efficiency, avoids
Material equipment transfer in caused by loss and waste.And have there are two the ball valve of supplied gas disengaging, in preparation reaction process
It is passed through nitrogen, discharge air, the environment of an isolating oxygen is provided for preparation reaction, avoids the generation of oxide layer, what is obtained answers
Conjunction conductive material electric conductivity is more preferable, quality is higher.Compared with conventional chemical reaction kettle, the present invention can make reactant contact area
It is bigger, it reacts more complete, improves deposition reaction efficiency and energy conversion efficiency, reduce the use of solvent and reagent, reduce
The discharge of waste liquid.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to embodiment or description of the prior art
Needed in attached drawing be briefly described, it should be apparent that, the accompanying drawings in the following description is only of the invention some
Embodiment for those of ordinary skill in the art without any creative labor, can also be according to these
Attached drawing obtains other attached drawings.
Fig. 1 is the structural diagram of the present invention；
Fig. 2 is the schematic diagram of internal structure of ball milling cylinder of the present invention；
Fig. 3 is the structural schematic diagram of ball milling body end surface of the present invention.
Specific embodiment
In order to which technical problems, technical solutions and advantages to be solved are more clearly understood, tie below
Accompanying drawings and embodiments are closed, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only
To explain the present invention, it is not intended to limit the present invention.
It should be noted that it can be directly another when element is referred to as " being fixed on " or " being set to " another element
On one element or indirectly on another element.When an element is known as " being connected to " another element, it can
To be directly to another element or be indirectly connected on another element.
In the description of the present invention, it is to be understood that, term " center ", " length ", " width ", " thickness ", "upper",
The orientation or position of the instructions such as "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outside"
Relationship is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of description of the present invention and simplification of the description, without referring to
Show or imply that signified device or element must have a particular orientation, be constructed and operated in a specific orientation, therefore cannot manage
Solution is limitation of the present invention.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
The interaction relationship of connection or two elements inside two elements.It for the ordinary skill in the art, can be with
The concrete meaning of above-mentioned term in the present invention is understood as the case may be.
With reference to the accompanying drawing and the principle of the present invention and structure is described in detail in embodiment.
As shown in Figures 1 to 3, the invention proposes a kind of anaerobic mechanochemistry for being used to prepare sheets of conductive composite powder is anti-
Answer kettle, comprising: driving device, ball milling cylinder 1 and ball milling bracket 2, ball milling cylinder 1 are equipped with the central axis 5 across its axle center, in
It is cased with bearing 7 in mandrel 5, is mounted on ball milling bracket 2 by the support of bearing 7, supports ball milling cylinder 1 by ball milling bracket 2
And can be rotated along central axis 5, one end of ball milling cylinder 1 is arranged in driving device, and ball milling cylinder 1 can be driven to rotate, make ball milling
Abrasive material ball 16 in cylinder 1 moves the effect for playing ball milling, and ball milling cylinder 1 is equipped with multiple valves for connecting gas pipeline
11, it is closed after gas can be filled with when ball milling cylinder 1 is static, the condition of chemical reaction is provided, on the central axis 5 of ball milling cylinder 1
Equipped with reaction solution be added dropwise mouth 12, can dropwise reaction liquid when ball milling cylinder 1 is static or when rotate, for chemically react chemical drugs are provided
Agent is additionally provided with inlet port and outlet port in the cambered surface of ball milling cylinder 1, when the rotation of ball milling cylinder 1 to designated state, discharge port position
It is located at top in bottom feed inlet, and is designed with switch block on discharge port and feed inlet, for seals.Present invention collection ball milling,
Deposition and polishing one, mechanical industry is combined with chemical industry, greatly reduces manpower object needed for production process
Power improves production efficiency, loss and waste caused by avoiding material in equipment transfer.The generation for avoiding oxide layer, obtains
The composite conducting material electric conductivity arrived is more preferable, quality is higher.Compared with conventional chemical reaction kettle, the present invention can be such that reactant connects
Contacting surface product is bigger, reacts more complete, improves deposition reaction efficiency and energy conversion efficiency, reduces making for solvent and reagent
With reducing the discharge of waste liquid.
In the present invention, driving device includes driving motor 3 and electric machine support 4, is arranged in the shaft of driving motor 3 actively
Gear 31 is also arranged with multiple bearings 7, and bearing 7, which is mounted on electric machine support 4, guarantees that the shaft of driving motor can normally turn
Dynamic, one end of ball milling cylinder 1 is equipped with a circle and cooperates from end face driven gear 13 outstanding with driving gear 31, drives so as to pass through
Dynamic motor 3 drives ball milling cylinder 1 to rotate, wherein driving motor uses fire-proof motor, guarantees the safety of chemical reaction.
In the present invention, switch block includes: lid 6, fastening gantry 14 and bolt assembly, and lid 6 covers respectively there are two being total to
At inlet port and outlet port, inlet port and outlet port are closed, fastening gantry 14 is fixed on ball milling cylinder 1, and is extended to
The top of inlet port and outlet port, fastening gantry 14 are equipped with threaded hole, and bolt assembly is screwed at threaded hole, tightens rear one end
It may pass through threaded hole, withstand on lid 6 and compress lid 6, so that inlet port and outlet port be completely enclosed, bolt assembly includes
Stud and the locking nut positioned at rotation stud one end are rotated, convenient for the operation tightened and unscrewed.Wherein, discharge outlet is equipped with
Screening Network 15, Screening Network 15 can completely cut off abrasive material ball 16, filter out ball milling powder, and in specific implement, the mesh of Screening Network can be with
For 200-400 mesh.
In the present invention, the material of abrasive material ball 16 is steel ball, zirconium ball, polystyrene spheres or Teflon ball.
In the particular embodiment, switch valve 11 is ball valve, totally two, is separately positioned on the two sides of feed inlet, is used for nitrogen
The discharge of gas being passed through with air provides the environment of an isolating oxygen for preparation reaction, avoids the generation of oxide layer, obtain
Composite conducting material electric conductivity is more preferable, quality is higher.
The both ends of ball milling cylinder 1 are equipped with electroheat pair panel 18, for heating in synthetic composite material, heating temperature 20-
100 DEG C, suitable temperature is provided for chemical reaction.
It is additionally provided with more semicircle ribs 17 in ball milling cylinder 1, the shape of semicircle rib 17 is the steel pipe being cut in half, two
End is connected on the inner wall at 1 both ends of ball milling cylinder, and from the end face of ball milling cylinder 1, semicircle rib 17 is arranged in a ring, can be stirred
Abrasive material ball 16 is driven to eminence and provides gravitional force progress abrasive material by the abrasive material ball 16 in dynamic ball milling cylinder 1.
The invention also provides a kind of processing methods using above-mentioned chemical reaction kettle, specifically include: step 1, will be spherical
Metal powder puts into ball milling sprills in blocks in ball milling cylinder；The silver-colored solution of mouth dropwise addition and reducing solution is added dropwise in reaction solution in step 2
The substrate surface chemical silvering of flakelike powder is obtained into sheet composite conductive powder；Polishing fluid is added in ball grinding cylinder body step 3
Sheet composite conductive powder surface is polished.The present invention is by the ball milling, silver-plated in sheet composite conductive powder production process
With the multiple steps of polishing, concentration carries out in the same apparatus, saves a large amount of manpower and material resources, save the cost is reduced simultaneously
The consume that material is generated in equipment room transfer.
In the present invention, step 1 is specifically included: abrasive material ball being placed in ball grinding cylinder body, abrasive material ball can be zirconium ball, polyphenyl second
Alkene ball, Teflon ball etc., having a size of 0.5-3mm, the quantity of abrasive material ball at most accounts for the 1/4 of ball milling cylinder volume.By spherical metal
Powder substrate is mixed with ball milling oil according to weight ratio 1:1.5-2.5.Wherein globular metallic powder can be spherical nickel powder and spherical copper
Powder etc., ingredient includes mineral oil, fatty acid and organic solvent in ball milling oil, wherein mineral oil: fatty acid: organic solvent is
100:0.1-1:0.1-1, mineral oil can be able to be lauric acid/dodecanoic acid, tetradecylic acid, ten for mineral oil, fatty acid such as D40, D60, D70, D80
Six acid, stearic acid and oleic acid etc., organic solvent can be dimethylbenzene, trimethylbenzene etc..Abrasive material ball and metal powder and ball milling oil it is mixed
Closing the ratio between object is 12-8:1.By the mixture of globular metallic powder and ball milling oil as in ball milling cylinder.In air pipe interface one end
Nitrogen is connected, other end connects hose, and the hose other end is placed in water.It opens nitrogen ball valve and is passed through nitrogen；Open air
Ball valve is discharged the intracorporal air of ball grinding cylinder, the one end of hose in water can be observed and continuously generate bubble.The logical nitrogen time is 5-
15min can shut two ball valves, start ball milling.By ball milling barrel body rotation preset time t 1, t1 be can be set to 5-12 hours,
As Ball-milling Time increases, rotational speed of ball-mill gradient is reduced.Strainer is loaded onto discharge port, puts Medium speed filter paper on strainer, under strainer
Bottle,suction and vacuum pump in termination, filter ball milling oil.
In the present invention, step 2 is specifically included:
Acid alcoholic solvent is added after the completion of filtering and carries out ball grinding stirring, wash the ball milling oil of sheet metal powder surface and removes it
Oxide.Acid alcoholic solvent is that alcohols solvent and acidic materials form, alcohols solvent can be ethyl alcohol, isopropanol, n-butanol or
Isobutanol etc., acidic materials can be hydrochloric acid, sulfuric acid, citric acid or stannous chloride etc..Make ball milling barrel body rotation preset time t 2
It is stirred, t2 can be set to 10-50 min, filter after the completion in discharge port to acidity alcohol solution.Deionization is added
Water.Feed inlet is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen 3-15 minutes, fastens ball valve.Open ball milling cylinder
Heating panel temperature is adjusted to 40-70 DEG C by the thermocouple panel at both ends, and ball milling barrel body rotation preset time t 3 carries out ball milling and stirs
It mixes, t3 is 10-50 min.The preparation method of silver-colored solution is silver nitrate to be added in deionized water, then suitable ammonium hydroxide is added dropwise makes
Obtaining solution becomes clear.The preparation of reducing solution is that reducing agent is added in deionized water, and wherein reducing agent can be winestone
Acid, sodium potassium tartrate tetrahydrate, glucose etc..Drop is reacted at the silver-colored solution prepared and reducing solution hose and ball milling cylinder both ends
Add mouth to be connected, carries out rate controlling control amount using peristaltic pump and add, control drips in 1 to 4h.Silver-colored solution and reducing solution drop
After the completion of adding, control ball milling barrel body rotation preset time t 4 carries out ball grinding stirring, and t4 can be set between 10-60min.Turn off
Thermocouple panel.Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, right
The solvent that chemical silvering generates is filtered.Substituted in the way of ball milling stirring paddle stirring in the way of carry out silver-plated, can make
Deposition reaction stirring it is more abundant, contact of the reactant with substrate is more abundant, at the same reduce react needed for solution amount, subtract
The discharge of few waste liquid.
In the present invention, step 3 is specifically included:
Polishing fluid is made of solvent and dispersing agent two parts, and solvent can make ethylene glycol, propylene glycol etc., and dispersing agent can be anti-settling
Agent, rheology modified wax dispenser align agent etc..Feed inlet is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen
3-15 minutes, fasten ball valve.Polishing fluid is added in sheet composite conductive powder, polishing is lubricated to powder.Control ball
Grinding cylinder rotates preset time t 5 and carries out ball milling, and t5 can be set to 1-3 hours.Screening Network is loaded onto discharge port, Screening Network
Mesh number can be 200-400 mesh, filter out sheet composite conductive powder and filtrate, be cleaned one time with ethyl alcohol.Obtained experiment is produced
Object carries out suction filtration drying, and sheet composite conductive powder can be obtained.Sheet prepared by the silver-plated method of conventional aqueous reaction
The silver layer on composite conductive powder surface is to intersperse shape Argent grain, and as the oxidation of substrate will lead to electric conductivity decline, the present invention will
The Argent grain for interspersing shape is polished to the silver layer of continuous and derivable with the mode of low speed ball milling, substantially increases leading for sheet composite powder
Electrical property and shelf stability.
The following are three specific embodiments in the present invention, wherein embodiment one are as follows:
The Teflon ball that 80kg sphere diameter is 0.6mm is placed in ball milling cylinder.
The D60 mineral oil, 0.05kg lauric acid/dodecanoic acid and 0.01kg dimethylbenzene of 6.54kg are uniformly mixed and are configured to ball milling oil.
6.6kg ball milling oil and 3kg spherical copper powder are mixed, ball milling cylinder is added to.
Feed inlet is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen 15 minutes, fastens ball valve.
Ball milling drum speed is adjusted to 26rpm, ball milling 5 hours；Revolving speed is dropped into 22rpm, ball milling 3 hours；Revolving speed is dropped
To 18rpm, ball milling 1 hour.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to ball milling
Oil is filtered.
0.024kg hydrochloric acid is added in 6kg isopropanol, acidity alcohol solution is configured to.
Discharge port is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen 6 minutes, fastens ball valve.
Acidity alcohol solution is added in ball milling cylinder, revolving speed is adjusted to 12rpm, ball grinding stirring 20min.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to acidity
Alcoholic solution is filtered.
2kg deionized water is added, locks feed inlet, opens ball valve, is passed through nitrogen, air is discharged, leads to nitrogen 6 minutes, closes
Tight ball valve.
The electroheat pair heating plate for opening ball milling cylinder both ends, adjusts the temperature to 45 DEG C.
Ball milling drum speed is adjusted to 12rpm, starts ball grinding stirring.
1.26kg silver nitrate is uniformly mixed with 2kg deionized water, is charged with ammonium hydroxide to solution from brown bleach,
Preparation obtains silver-colored solution.1kg sodium potassium tartrate tetrahydrate is mixed with 2kg deionized water, preparation obtains reducing agent solution.
Prepared silver-colored solution and reducing agent solution are added drop-wise to simultaneously in ball grinding cylinder body, control is added dropwise in 2h.
After silver-colored solution and reducing agent solution are added dropwise, continue ball milling 30min, turn off thermocouple.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to chemistry
The solvent of silver-plated generation is filtered.
0.06kg anti-settling agent is uniformly mixed with 2.95kg ethylene glycol, ball milling cylinder is added.Feed inlet is locked, ball is opened
Valve is passed through nitrogen, and air is discharged, and leads to nitrogen 6 minutes, fastens ball valve.
Ball milling drum speed is adjusted to 12rpm, ball grinding stirring 1.5h.
200 mesh subnettings are loaded onto discharge port, sheet composite conductive powder and filtrate is filtered out, is cleaned one time with ethyl alcohol.
Suction filtration drying is carried out to obtained experimental product, sheet composite conductive powder can be obtained.
Embodiment two are as follows:
The zirconium pearl that 80kg sphere diameter is 1mm is placed in ball milling cylinder.
The D80 mineral oil, 0.03kg oleic acid and 0.01kg trimethylbenzene of 5.56kg are uniformly mixed and are configured to ball milling oil.
5.6kg ball milling oil and 2.8kg spherical copper powder are mixed, ball milling cylinder is added to.
Feed inlet is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen 12 minutes, fastens ball valve.
Ball milling drum speed is adjusted to 28rpm, ball milling 4 hours；Revolving speed is dropped into 20rpm, ball milling 4 hours；Revolving speed is dropped
To 15rpm, ball milling 2 hours.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to ball milling
Oil is filtered.
The 0.017kg concentrated sulfuric acid is added in 5.6kg ethyl alcohol, acidity alcohol solution is configured to.
Discharge port is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen 5 minutes, fastens ball valve.
Acidity alcohol solution is added in ball milling cylinder, revolving speed is adjusted to 10rpm, ball grinding stirring 30min.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to acidity
Alcoholic solution is filtered.
2kg deionized water is added, locks feed inlet, opens ball valve, is passed through nitrogen, air is discharged, leads to nitrogen 5 minutes, closes
Tight ball valve.
The electroheat pair heating plate for opening ball milling cylinder both ends, adjusts the temperature to 40 DEG C.
Ball milling drum speed is adjusted to 10rpm, starts ball grinding stirring.
2.2kg silver nitrate is uniformly mixed with 3kg deionized water, is charged with ammonium hydroxide to solution from brown bleach,
Preparation obtains silver-colored solution.1.7kg glucose is mixed with 4kg deionized water, preparation obtains reducing agent solution.
Prepared silver-colored solution and reducing agent solution are added drop-wise to simultaneously in ball grinding cylinder body, control is added dropwise in 2.5h.
After silver-colored solution and reducing agent solution are added dropwise, continue ball milling 50min, turn off thermocouple.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to chemistry
The solvent of silver-plated generation is filtered.
0.06kg dispersing agent and 2.95kg mixed with propylene glycol is uniform, ball milling cylinder is added.Feed inlet is locked, ball is opened
Valve is passed through nitrogen, and air is discharged, and leads to nitrogen 5 minutes, fastens ball valve.
Ball milling drum speed is adjusted to 10rpm, ball grinding stirring 2.5h.
Screening Network is loaded onto discharge port, filters out sheet composite conductive powder and filtrate, is cleaned one time with ethyl alcohol.
Suction filtration drying is carried out to obtained experimental product, sheet composite conductive powder can be obtained.
Embodiment three are as follows:
The polystyrene spheres that 80kg sphere diameter is 1mm are placed in ball milling cylinder.
The D70 mineral oil, 0.03kg stearic acid and 0.01kg trimethylbenzene of 5.96kg are uniformly mixed and are configured to ball milling oil.
6kg ball milling oil and 3kg globular powdered nickel are mixed, ball milling cylinder is added to.
Feed inlet is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen 10 minutes, fastens ball valve.
Ball milling drum speed is adjusted to 30rpm, ball milling 4 hours；Revolving speed is dropped into 25rpm, ball milling 3 hours；Revolving speed is dropped
To 20rpm, ball milling 3 hours.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to ball milling
Oil is filtered.
0.03kg stannous chloride is added in 6kg ethyl alcohol, acidity alcohol solution is configured to.
Discharge port is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen 4 minutes, fastens ball valve.
Acidity alcohol solution is added in ball milling cylinder, revolving speed is adjusted to 13rpm, ball grinding stirring 30min.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to acidity
Alcoholic solution is filtered.
3kg deionized water is added, locks feed inlet, opens ball valve, is passed through nitrogen, air is discharged, leads to nitrogen 5 minutes, closes
Tight ball valve.
The electroheat pair heating plate for opening ball milling cylinder both ends, adjusts the temperature to 50 DEG C.
Ball milling drum speed is adjusted to 13rpm, starts ball grinding stirring.
2kg silver nitrate is uniformly mixed with 4kg deionized water, ammonium hydroxide is charged with to solution from brown bleach, matches
Silver-colored solution is made.1.6kg tartaric acid is mixed with 4kg deionized water, preparation obtains reducing agent solution.
Prepared silver-colored solution and reducing agent solution are added drop-wise to simultaneously in ball grinding cylinder body, control is added dropwise in 3h.
After silver-colored solution and reducing agent solution are added dropwise, continue ball milling 40min, turn off thermocouple.
Strainer is loaded onto discharge port, Medium speed filter paper is put on strainer, strainer lower end connects bottle,suction and vacuum pump, to chemistry
The solvent of silver-plated generation is filtered.
0.03kg is aligned into agent and 2.97kg mixed with propylene glycol is uniform, ball milling cylinder is added.
Feed inlet is locked, ball valve is opened, is passed through nitrogen, air is discharged, leads to nitrogen 5 minutes, fastens ball valve.
Ball milling drum speed is adjusted to 13rpm, ball grinding stirring 2.5h.
Screening Network is loaded onto discharge port, filters out sheet composite conductive powder and filtrate, is cleaned one time with ethyl alcohol.
Suction filtration drying is carried out to obtained experimental product, sheet composite conductive powder can be obtained.
Present device concentrates the ball milling in sheet composite conductive powder production process, the silver-plated and multiple steps of polishing
It carries out in the same apparatus, saves a large amount of manpower and material resources, save the cost, while reducing material and shifting production in equipment room
Raw consume.Substituted in the way of ball milling stirring paddle stirring in the way of carry out it is silver-plated, can make deposition reaction stirring more
Sufficiently, contact of the reactant with substrate is more abundant, while reducing the amount for reacting required solution, reduces the discharge of waste liquid.It is conventional
The silver-plated method of aqueous reaction prepared by the silver layer on sheet composite conductive powder surface be to intersperse shape Argent grain, with substrate
Oxidation will lead to electric conductivity decline, the Argent grain for interspersing shape is polished to continuous and derivable with the mode of low speed ball milling by the present invention
Silver layer substantially increases the electric conductivity and shelf stability of sheet composite powder.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of chemical reaction kettle characterized by comprising driving device, by driving device driving and inside is with multiple
The ball milling cylinder (1) of abrasive material ball (16), the ball milling bracket (2) of mounting ball grinding cylinder (1), the ball milling cylinder (1) are equipped with more
Mouth (12) are added dropwise in a valve (11) for connecting gas pipeline and reaction solution, are additionally provided with position in the cambered surface of the ball milling cylinder (1)
In the inlet port and outlet port of different radial heights and the switch block of corresponding inlet port and outlet port, the ball milling cylinder
(1) both ends are equipped with electroheat pair panel (18).
2. mechanico-chemical reaction kettle as described in claim 1, which is characterized in that the ball milling cylinder (1) is by passing through ball milling
The central axis (5) in cylinder axle center is mounted on ball milling bracket (2), and mouth (12) centrally disposed axis (5) are added dropwise in the reaction solution
Both ends.
3. a kind of processing method of the described in any item chemical reaction kettles of claim 1 to 2, which is characterized in that step includes:
Globular metallic powder is put into ball milling sprills in blocks in ball milling cylinder by step 1；
Step 2 obtains the substrate surface chemical silvering of flakelike powder in the silver-colored solution of reaction solution dropwise addition mouth dropwise addition and reducing solution
Sheet composite conductive powder；
Step 3 will polish sheet composite conductive powder surface in polishing fluid addition ball grinding cylinder body.
4. processing method as claimed in claim 3, which is characterized in that the step 1 specifically includes: by globular metallic powder with
The mixture of ball milling oil is as in ball milling cylinder；It is passed through nitrogen, makes ball milling barrel body rotation preset time t 1；Going out after the completion of rotation
Material mouth filters ball milling oil.
5. abrasive material process as claimed in claim 3, which is characterized in that the step 2 specifically includes: it is molten that acid alcohol is added
Liquid makes ball milling barrel body rotation preset time t 2；Acidity alcohol solution is filtered in discharge port after the completion of rotation；Deionization is added
Water is passed through nitrogen, and ball milling cylinder is warming up to preset temperature；Ball milling barrel body rotation preset time t 3；Silver-colored solution and reduction is added dropwise
Agent solution, rotating ball grinding cylinder preset time t 4；It is filtered after the completion of rotation in the solvent that discharge port generates chemical silvering.
6. abrasive material process as claimed in claim 3, which is characterized in that the step 3 specifically includes: adding from outlet material
Enter polishing fluid, be passed through nitrogen, ball milling barrel body rotation preset time t 5 filters out sheet composite guide in discharge outlet after the completion of rotation
Electro-powder.
7. abrasive material process as claimed in claim 3, which is characterized in that the polishing fluid is made of solvent and dispersing agent,
The solvent is ethylene glycol or propylene glycol, and the dispersing agent is anti-settling agent, rheology modified wax dispenser or aligns agent.
8. abrasive material process as described in claim 4 or 5, which is characterized in that the specific steps of the suction filtration are as follows: discharging
Mouth installs strainer, and Medium speed filter paper is placed on strainer, and strainer lower end connection bottle,suction and vacuum pump are filtered.
9. abrasive material process as claimed in claim 5, which is characterized in that the acidity alcoholic solvent is by alcohols solvent and acidity
Material composition, the alcohols solvent are ethyl alcohol, isopropanol, n-butanol or isobutanol, and acidic materials are hydrochloric acid, sulfuric acid, citric acid
Or stannous chloride.
10. abrasive material process as claimed in claim 5, which is characterized in that the reducing solution is tartaric acid, potassium tartrate
Sodium or glucose.
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| CN201910363503.8A CN110194903A (en) | 2019-04-30 | 2019-04-30 | Chemical reaction kettle and the processing method for using the chemical reaction kettle |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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