CN104789807B - A kind of method for improving the water base compound slip discharging of hard alloy - Google Patents
A kind of method for improving the water base compound slip discharging of hard alloy Download PDFInfo
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- CN104789807B CN104789807B CN201510116257.8A CN201510116257A CN104789807B CN 104789807 B CN104789807 B CN 104789807B CN 201510116257 A CN201510116257 A CN 201510116257A CN 104789807 B CN104789807 B CN 104789807B
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Abstract
The invention discloses a kind of method for improving the water base compound slip discharging of hard alloy, comprises the steps：Add 80～92wt.%WC powder, 8～20wt.%Co powder and 120ml～300ml/kg deionized waters, and add the 0.1～2.0wt.% dispersants and 0.005～0.050wt.% defoamer calculated by powder solid content, and it is not added with forming agent, ball milling in roller ball mill together, Ball-milling Time is 32 72h, 30～40r/min of rotational speed of ball-mill；After ball milling terminates, phosphoric acid is measured, adjust ball mill rotational speed of ball-mill；Calculate slip discharging rate.The present invention reduces phosphoric acid by reducing ball mill milling intensity, improves water and powder wettability by adding auxiliary agent, and is not added with the processing modes such as forming agent in mechanical milling process, so as to solve hard alloy aqueous slurries discharging problem.
Description
Technical field
The present invention relates to powder metallurgical technology, more particularly to one kind improve the water base compound slip of hard alloy unloading
The method of material.
Background technology
The preparation of compound is one step of key of CEMENTED CARBIDE PRODUCTION, and traditional method is mainly with ethanol, acetone and hexamethylene
Deng organic solvent as wet grinding media, slurry ball-milling needs to filter through 325 eye mesh screens (aperture 43um) after terminating, it is to avoid thick paraffin
The iron filings produced in granule and ball milling are impacted to alloy property；Carbide alloy mixture is prepared as ball-milling medium using water,
Can solve pollution of the organic solvent to environment, but ball milling terminates rear slip and cross 325 eye mesh screens to draw off, main cause has：
(1) as the surface tension of water is more larger than ethanol, slip easily brings air in ball milling so as to form bubble, and vacuolar membrane can be attached to
So as to hindering slip to draw off on screen cloth mesh；(2) forming agent of the water base compound of hard alloy adopts emulsifing wax, contains in emulsifing wax
There is hydrophilic surfactant active, adsorb and the elastica with some strength is formed in bubble surface, cause liquid-sheet disintegration difficulty to add
Greatly；(3) therefore ethanol can be difficult to reunite after powder ball milling, and water is deposited with powder with complete wetting with carbide alloy mixture
In certain angle of wetting, interface energy is larger, and for a long time, fine powder is easily reunited as surface energy is larger after high intensity ball milling,
Cause powder size distribution more to be concentrated, during particle packing between gap larger, need the filling of more liquid, be just avoided that
There is internal friction in granule, phosphoric acid can otherwise increased, affects slip discharging.
The water base compound slip of hard alloy cross screen cloth discharging problem directly affect productivity effect and postorder production can connect
Continuousization carry out.
Content of the invention
It is an object of the invention to overcoming the deficiency of prior art, there is provided one kind improves the water base compound slip of hard alloy
The method of discharging, reduces phosphoric acid by reducing ball mill milling intensity, improves water and powder moistening by adding auxiliary agent
Property, and the processing modes such as forming agent are not added with mechanical milling process, so as to solve hard alloy aqueous slurries discharging problem.
The technical solution adopted for the present invention to solve the technical problems is：One kind improves the water base compound slip of hard alloy
The method of discharging, comprises the steps：
80～92wt.%WC powder, 8～20wt.%Co powder and 120ml～300ml/kg deionized waters is added, and is added
Press 0.1～2.0wt.% dispersants and 0.005～0.050wt.% defoamer of the calculating of powder solid content, and not add-on type
Agent, ball milling in roller ball mill together, Ball-milling Time is 32-72h, 30～40r/min of rotational speed of ball-mill；
After ball milling terminates, discharging is carried out using 400 eye mesh screens, using rotary viscosity measuring phosphoric acid, according to viscosity
Change adjustment ball mill rotational speed of ball-mill, the more little then phosphoric acid of rotational speed of ball-mill is also less；
Press slip solid-to-liquid ratio 2.8～3.2:1 water yield that can be added when calculating discharging, cleaning stick to mill ball and ball
Slip on grinding machine wall, the gross weight for drawing off slip are designated as m1, the material and deionized water gross weight that put in ball milling are designated as m, grind
Ball wear weight is designated as m2；Then
Slip discharging rate %=(m1-m2)/m*100%.
The dispersant is polycarboxylic acid.
The defoamer is polyhydric alcohol.
Compared with prior art, the invention has the beneficial effects as follows：
The present invention passes through to add dispersant and defoamer in slip, with advantages below：(1) can sieve in guarantee slip
Under the early stage that net draws off, the filtration mesh that improve water-based rigid alloy compound slip (brings up to 400 from 180-230 mesh
Mesh)；(2) slip crosses 400 eye mesh screens, in solid content up under 70%-80%, still can exit more than 99% slip.
Existing water-based rigid alloy slip is crossed 325 eye mesh screens and cannot be drawn off, using following methods (as reduced sieve number extremely
180-230 mesh, ultrasonic activation are sieved through filter, add a large amount of water dilution slips etc.) the discharging rate of slip is also only capable of reaching 90%, no
Only discharging inefficiency, and introducing impurity easily in slip, causes alloy hole.
With reference to embodiments the present invention is described in further detail；But it is water base that one kind of the present invention improves hard alloy
The method of compound slip discharging is not limited to embodiment.
Specific embodiment
Embodiment
A kind of method of the water base compound slip discharging of improvement hard alloy of the invention, is by reducing ball mill ball milling
Intensity improves water and powder wettability by adding auxiliary agent, and is not added with forming agent etc. in mechanical milling process reducing phosphoric acid
Processing mode, so that solve hard alloy aqueous slurries discharging problem.
A kind of method of the water base compound slip discharging of improvement hard alloy of the invention, is water base mixed according to hard alloy
The characteristics of material slip easy to foaming, reunion is closed, adds suitable defoamer and dispersant to be obviously improved the state of slip, which includes
Following steps：
80～92wt.%WC powder, 8～20wt.%Co powder and 120ml～300ml/kg deionized waters is added, and is added
0.1～2.0wt.% dispersants and 0.005～0.050wt.% defoamer of the calculating of powder solid content is pressed, together in roller ball
Ball milling in grinding machine, Ball-milling Time are 32-72h, and wherein, above-mentioned dispersant is polycarboxylic acid, and defoamer is polyhydric alcohol；
After ball milling terminates, discharging is carried out using 400 eye mesh screens (aperture 38um)；Using U.S.'s Brookfield DV-I+ types
Rotary viscosity measuring phosphoric acid, viscosity measurement procedure is：First, the slip after ball milling is taken in container, filling height should
It is higher than rotor groove part；Second, different rotors are coordinated with rotating speed, can there are different viscosity measurement scopes, such as table 1
Shown, suitable rotor and rotating speed should be selected as far as possible during measurement viscosity, make phosphoric acid value between range 40%～60%, can
To obtain accurate measurement result；3rd, before measurement, reply slip is stirred mixing 15min, it is to avoid slip is placed and sent out
Layer estranged, starts instrument power source measurement, reads after display screen numerical stability, and repeated measurement 3 times is averaged, while needing to record
Ambient temperature during detection；
1 rotating cylinder viscometer rotor of table and rotating speed and corresponding viscosity measurement scope
| Viscosity measurement scope/cp | 64# | 63# | 62# | 61# |
| 100r/min | 0～3600 | 0～1200 | 0～300 | 0～60 |
| 50r/min | 0～7200 | 0～2400 | 0～600 | 0～120 |
| 20r/min | 0～18000 | 0～6000 | 0～1500 | 0～300 |
| 10r/min | 0～36000 | 0～12000 | 0～3000 | 0～600 |
There is certain angle of wetting in water and WC powder, both interface energies are larger, for a long time, fine particle after high intensity ball milling
Easily reunite as surface energy is larger, cause powder size distribution more concentrate, during particle packing between gap increase,
And added water yield during ball milling cannot blind when, during slip flowing there is the increase of internal friction probability in powder particle, from
And increase phosphoric acid.Generally phosphoric acid is little, and slip easily draws off, discharging rate high；Phosphoric acid is big, and slip is difficult
To draw off, discharging rate relatively low；Rotational speed of ball-mill reduce can significantly reduce milling intensity, therefore the rotational speed of ball-mill of ball mill from
Original 50r/min (critical speed 71%) is reduced to 30～40r/min (critical speed 43～57%), so that phosphoric acid
Decline, finally obtain suitable phosphoric acid；
Press slip solid-to-liquid ratio 2.8～3.2:1 water yield that can be added when calculating discharging, cleaning stick to mill ball and ball
Slip on grinding machine wall, the gross weight for drawing off slip are designated as m1, in ball milling put into material and deionized water gross weight be m, mill ball
Abrasion weight is designated as m2,Wherein m2Weight be ball milling before with ball milling after grinding in ball grinder ball gross weight difference；
Slip discharging rate %=(m1-m2)/m*100%
Slip discharging rate is mainly used to the compound casting yield after characterizing through ball milling, as the preparation of compound is that hard is closed
One step of key of gold production, if water base compound can realize the discharging rate similar to ethanol compound, greatly can push away
Enter the industrialization production of water base compound.
One kind that a specific example is below lifted to further describe the present invention improves the water base compound of hard alloy
The method of slip discharging.
By 36kg tungsten-carbide powders (Fsss=0.8um), 4kg cobalt dusts (Fsss=0.8um), 10.6kg deionized waters and
Compounding ball-milling additive puts into ball milling in 50L ball grinding cylinders (D=0.38m), and wherein above-mentioned compounding ball-milling additive includes 200g
Dispersant, 80g antioxidants and 8g defoamer.In Ball-milling Time 48h, rotational speed of ball-mill 30r/min (equivalent to critical speed
43%) He 4:Under the conditions of the ball-milling technology of 1 ratio of grinding media to material, it is possible to obtain suitable phosphoric acid；After ball milling terminates, do not add water straight
400 eye mesh screens (aperture 38um) discharging is taken over, finally adding remaining 1.9L deionized waters carries out cleaning ball mill and grinding
Slip on ball, according to discharging rate formula：
Slip discharging rate %=(m1-m2)/m*100%
Through weighing, slip weight m is drawn off1=52.765kg, weight difference m before and after mill ball ball milling2=0.2kg, in ball milling
Input pressed powder and deionized water gross weight are m=52.788kg；
Slip discharging rate %=(52.765-0.2)/52.788*100%=99.6%；
The slip for drawing off is measured slip under 62# rotors and 100r/min rotating speeds and is glued using rotary viscosity measuring viscosity
Spend for 80cp, according to added material powder and deionized water weight ratio, the solid-to-liquid ratio for being calculated slip is 3.2:1
The ultra-fine emulsifing wax of 1.6kg is mixed in slip (accounts for the 4wt.% of powder solid content, emulsifing wax mean particle size D 50 is
0.8um), 60min is stirred with mechanical agitator low whipping speed 500r/min, after waiting slip to be sufficiently mixed with emulsifing wax, adopt
Use open spray drying, acquisition particle morphology is subglobose spraying material, the water base compound oxygen content for preparing is
0.59%, oxygen content is substantially suitable with alcohol-based compound, and the microstructure of the alloy porosity for preparing is A02B00.
The present invention passes through to add dispersant and defoamer in slip, on the one hand, can cross what screen cloth drew off in guarantee slip
Under early stage, the filtration mesh (bringing up to 400 mesh from 180-230 mesh) of water-based rigid alloy compound slip is improve；The opposing party
400 eye mesh screens are crossed in face, slip, in solid content up under 70%-80%, still can exit more than 99% slip.
Above-mentioned simply presently preferred embodiments of the present invention, not makees any pro forma restriction to the present invention.Although it is of the invention
Disclosed above with preferred embodiment, but it is not limited to the present invention.Any those of ordinary skill in the art, are not taking off
In the case of technical solution of the present invention scope, all technical solution of the present invention is made perhaps using the technology contents of the disclosure above
How possible variation and modification, or it is revised as equivalents Equivalent embodiments.Therefore, every without departing from technical solution of the present invention
Content, according to the technology of the present invention essence to any simple modification made for any of the above embodiments, equivalent variations and modification, all should fall
In the range of technical solution of the present invention protection.
Claims (3)
1. a kind of method for improving the water base compound slip discharging of hard alloy, it is characterised in that：Comprise the steps：
80～92wt.%WC powder, 8～20wt.%Co powder and 120ml～300ml/kg deionized waters is added, and is added by powder
0.1～2.0wt.% dispersants and 0.005～0.050wt.% defoamer that last solid content is calculated, and forming agent is not added with, one
Ball milling in roller ball mill is played, Ball-milling Time is 32-72h, 30～40r/min of rotational speed of ball-mill；
After ball milling terminates, discharging is carried out using 400 eye mesh screens, using rotary viscosity measuring phosphoric acid, according to the change of viscosity
Change adjustment ball mill rotational speed of ball-mill, the more little then phosphoric acid of rotational speed of ball-mill is also less；
Press slip solid-to-liquid ratio 2.8～3.2:1 water yield that can be added when calculating discharging, cleaning stick to mill ball and ball mill
Slip on wall, the gross weight for drawing off slip are designated as m1, the material and deionized water gross weight that put in ball milling are designated as m, grind ball milling
Damage weight and be designated as m2；Then
Slip discharging rate %=(m1-m2)/m*100%.
2. the method for improving the water base compound slip discharging of hard alloy according to claim 1, it is characterised in that：Described
Dispersant is polycarboxylic acid.
3. the method for improving the water base compound slip discharging of hard alloy according to claim 1, it is characterised in that：Described
Defoamer is polyhydric alcohol.
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| US5028362A (en) * | 1988-06-17 | 1991-07-02 | Martin Marietta Energy Systems, Inc. | Method for molding ceramic powders using a water-based gel casting |
| SE529370C2 (en) * | 2006-01-09 | 2007-07-17 | Sandvik Intellectual Property | Water-based cemented carbide slurry, gelled cemented carbide and ways of producing a gelled body and a sintered cemented carbide body |
| CN101884892B (en) * | 2010-06-25 | 2012-09-05 | 北京工业大学 | Method for agglomerating and granulizing superfine nano WC-Co composite powder |
| CN102719689A (en) * | 2011-03-29 | 2012-10-10 | 厦门钨业股份有限公司 | PEG-based complex forming agent for water-based cemented carbide mixture |
| CN102717061A (en) * | 2011-03-29 | 2012-10-10 | 厦门钨业股份有限公司 | A paraffin base compound forming agent for a water base cemented carbide mixture |
| CN102732741A (en) * | 2011-04-01 | 2012-10-17 | 厦门钨业股份有限公司 | Method for preparing cemented carbide mixture by using water as wet grinding medium |
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