CN104925804B - Physics dissociation purifying plant and its method for purification of diamond synthesizing rod - Google Patents
Physics dissociation purifying plant and its method for purification of diamond synthesizing rod Download PDFInfo
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- CN104925804B CN104925804B CN201510426264.8A CN201510426264A CN104925804B CN 104925804 B CN104925804 B CN 104925804B CN 201510426264 A CN201510426264 A CN 201510426264A CN 104925804 B CN104925804 B CN 104925804B
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- 239000010432 diamond Substances 0.000 title claims abstract description 120
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 120
- 238000010494 dissociation reaction Methods 0.000 title claims abstract description 118
- 230000005593 dissociations Effects 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims abstract description 64
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 22
- 238000000746 purification Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 132
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 110
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 108
- 239000010439 graphite Substances 0.000 claims abstract description 108
- 229910052751 metal Inorganic materials 0.000 claims abstract description 80
- 239000002184 metal Substances 0.000 claims abstract description 80
- 238000000926 separation method Methods 0.000 claims abstract description 70
- 239000002904 solvent Substances 0.000 claims abstract description 69
- 230000002093 peripheral effect Effects 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 30
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 22
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 22
- 238000011049 filling Methods 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 97
- 239000012736 aqueous medium Substances 0.000 claims description 31
- 238000003860 storage Methods 0.000 claims description 29
- 239000003054 catalyst Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 16
- 238000007885 magnetic separation Methods 0.000 claims description 14
- 239000006148 magnetic separator Substances 0.000 claims description 10
- 238000012216 screening Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 230000003020 moisturizing effect Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000003638 chemical reducing agent Substances 0.000 claims description 3
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims 2
- 230000008569 process Effects 0.000 abstract description 36
- 239000002253 acid Substances 0.000 abstract description 18
- 238000005868 electrolysis reaction Methods 0.000 abstract description 12
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 9
- 229910052737 gold Inorganic materials 0.000 description 9
- 239000010931 gold Substances 0.000 description 9
- 239000011435 rock Substances 0.000 description 6
- 239000004575 stone Substances 0.000 description 6
- 238000003776 cleavage reaction Methods 0.000 description 5
- 230000007017 scission Effects 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
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- 239000003595 mist Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010306 acid treatment Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
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- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 2
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses physics dissociation purifying plant and its method for purification of a kind of diamond synthesizing rod, including dissociation tank, it is arranged on the agitator on dissociation tank, with the tank connected broken synthesis bar delivery device that dissociates, the top of described dissociation tank is provided with overflow blow tank, the peripheral separation equipment of overflow blow tank connection, peripheral separation equipment connects water system, water system connection dissociation tank and filling pipe.The present invention can make that synthetic rod realizes physics dissociating method graphite, metal solvent and diamond is separated from one another extracts, and prevent or at utmost reduce electrolysis and with acid amount；And it is with short production cycle, typically after a few minutes that dissociation tank is started working, just there is graphite to dissociate and come, it is possible to the row's of adding water graphite, and after ten minutes, it is possible to discharge diamond particles；Its preamble and postorder are added up typically can just produce diamond compound finished product in a shift, greatly reduce production cost and the pollution for environment, and the process cycle of shortening substantially increases the competitiveness of enterprise.
Description
Technical field
The present invention relates to the purification field of diamond synthesizing rod, the physics dissociation purification of specially a kind of diamond synthesizing rod
Device and its method of purification.
Background technology
Present diamond industry typically all uses powder synthetic rod technique, and the synthetic rod after synthesis is graphite and is touched by metal
Matchmaker is wrapped in the barred body of diamond particles, and postorder purification process seeks to a purification of diamond out, and realizes graphite and metal
The separation and recovery of catalyst.The purification of diamond is generally realized in purification workshop to synthetic rod using chemically treated method technique, its
Common process process is：Synthetic rod extracts metal solvent after being broken into little particle with the equipment and technique of chemical electrolysis, its
The recovery rate of electrolytic etching of metal is general more than 90%, and its acid electrolyte evaporates acid vapor, it is necessary to fan housing in electrolytic process
In exhausting to alkaline neutralizing tower and discharge, electrolysing period is generally four --- seven days or so, and the material after being electrolysed be graphite and
The mixture of diamond and residual metallic catalyst；Then being transferred to ball milling or roller refines particulate material, then through shaking table Buddha's warrior attendant
Stone and graphite are separated, and the diamond isolated also contains part catalyst and graphite, it is impossible to obtained pure diamond and produced
Product；Next it is transferred to again and carried out acid adding heating reaction with reactor, usually submerging material with the concentrated sulfuric acid and a small amount of nitric acid heats
Reaction, to aoxidize remaining graphite and react removal residual metal catalyst with diluted acid, the technical process produces substantial amounts of waste acid gas, needs
Cause alkaline rapids ball purifying column reaction absorbing acid gases, and reactor exclude material then need repeatedly to be rinsed with clear water to
Neutrality, could obtain more pure diamond；The acid water of rinsing carries out neutralization reaction with alkaline matter, uses filter press reality
Existing separation of solid and liquid, reacts the salt solids of generation as garbage emission, and its neutral water is used as discharge of wastewater.Next again to gold
Hard rock is cleaned and dried, to obtain pure diamond compound finished product.
During above-mentioned handling process, electrowinning process acidic electrolysis bath, the acid vapor that electrolytic process is produced will be by taking out
Wind apparatus are discharged to acid mist purifying tower treatment；The strong acid such as reactor sulfuric acid, nitric acid heating reaction removal graphite and residual metal,
The substantial amounts of concentrated sulfuric acid, concentrated nitric acid are consumed, its process produces substantial amounts of acid mist to be also required to acid mist purifying tower treatment；Above-mentioned treatment
Process, the acid mist that technical process is produced is processed with purifying column absorption, and its equipment investment is big, and operating cost is high.And eluriate reactor
Also produce substantial amounts of waste acid water during with the material after acid treatment, it is necessary to plus basic matterial such as caustic soda etc. be allowed to reach come neutralization reaction
Realize that solids is discharged through filtering (press filtration) after to neutrality, the waste water after neutralization reaction can also contain harmful material, after discharge
Still suffer from environmental pollution.Enterprise often produces 5000 myriagram lashing wire hard rocks, and it reaches more than 20 tons with acid amount, causes environmental protection facility to throw
Enter huge, tend not to qualified discharge, and the process time is long, is typically dosed into the process needs that finished product purifies output from preamble
7 days or so.
Therefore, improve the deduction technique of existing diamond synthesizing rod, realize that process cycle is short, and dropped during deduction
Low production cost and the pollution to environment, have been a good problems to study.
The content of the invention
In order to overcome above-mentioned deficiency of the prior art, existing diamond synthesizing rod can be shortened the invention provides one kind
Process cycle, and the physics dissociation purification of the diamond synthesizing rod of production cost and environmental pollution is reduced in purification process
Device and its method of purification.
The object of the present invention is achieved like this：
A kind of physics dissociation purifying plant of diamond synthesizing rod, including dissociation tank 1, are arranged on the stirring on dissociation tank 1
Device 2, the broken synthesis bar delivery device 7 being connected with dissociation tank 1, the top of described dissociation tank 1 is provided with overflow blow tank,
The peripheral separation equipment 3 of overflow blow tank connection, peripheral separation equipment connects water system 4, water system 4 connection dissociation tank 1 and moisturizing
Pipe；
Described peripheral separation equipment 3 includes filter, screen(ing) machine, magnetic separator, agitator and shaking table or its any combination；
Described water system 4 includes separation of material material stock water tank 4-1, the water storage being connected with separation of material material stock water tank 4-1
Case 4-2, the dissociation tank 1 being connected by pipeline with storage tank 4-2；Described storage tank 4-2 connects moisturizing pipeline a simultaneously, while
Water pump 4-3 and feed-water valve 4-4 is provided with storage tank 4-2 and the pipeline of the centre of dissociation tank 1；
The described top of dissociation tank 1 is provided with the motor being connected with agitator 2, the reductor with motor connection, reductor
Agitating shaft with mixing component is connected by shaft coupling；Mechanical lifting gear 5 is provided with described agitator 2；
Described dissociation tank 1 is vertical upper uncovered structure, and its ratio of height to diameter is 0.6-1.2: 1, and tank mouth is provided with overflow discharging
Groove；It is arranged on the agitator 2 inside dissociation tank 1 and includes paddle, vane type or bar type structure, wherein mixing part is high in tank
Spend in 3/4 altitude range；
The tank body periphery middle part of described dissociation tank 1 is symmetrically arranged with rotating shaft 6, and rotating shaft 6 is fixed by axle bed with frame；
The method purified using the physics dissociation purifying plant of above-mentioned diamond synthesizing rod, is comprised the following steps：
Synthesis bar after broken in broken synthesis bar delivery device 7 is put into dissociation tank 1, dissociation tank 1 is built-in
There are abrading-ball and aqueous medium；Agitator 2, the drive of the drive device that agitator 2 is constituted in motor and speed reducer are provided with dissociation tank 1
Under dynamic, the linear velocity for making the abrading-ball and material in aqueous medium to give is moved in tank, abrading-ball and conjunction during stirring movement
Into the comprehensive function that recirculation gas stripper effect, shearing-crushing power and attrition crushing power between abrading-ball etc. are produced between rod material particles
Under so that graphite is stripped first, is suspended in aqueous medium；Further, the metal solvent film that it is wrapped in diamond
Also shearing-crushing power and attrition crushing power between abrading-ball is stripped under acting on, and its metal solvent is carefully cut and the metal that dissociates
The diamond of catalyst film is existed in aqueous medium in the lump；So it is achieved that the solution of graphite, metal solvent and diamond three
From separation；
Realize graphite, metal solvent and the diamond of dissociation by being arranged on the overflow dissociated on tank 1 in dissociation tank 1
Blow tank, using outside drain tank by the way of upper discharge；The mode of described upper discharge is in given different speed of agitator；Low
Graphite fine powder is in and suspends completely during rotating speed, to being added water in dissociation tank 1, makes the mixture of material from the tank mouth of dissociation tank 1
Overflow blow tank overflows, to discharge based on graphite slurry；When improving rotating speed and reaching metal solvent and also suspend completely, graphite and metal
Catalyst is carefully cut and is overflowed by the overflow blow tank from the tank mouth of dissociation tank 1；And then improve rotating speed, the Buddha's warrior attendant for being dissociated out
Stone is also reached when suspending completely, and diamond particles and graphite, metal solvent are carefully cut with aqueous medium in the lump from the tank mouth of dissociation tank 1
Overflow blow tank discharge；
It is different according to the rotating speed that its agitator is stirred, discharge respectively graphite slurry, graphite+metal solvent carefully cut, graphite+gold
Category catalyst carefully cuts+diamond；The separation that peripheral separation equipment 3 realizes screening graphite, metal solvent and diamond is sequentially entered, point
The water for separating out enters water system 4, and overflow discharge is used for during water is then returned to cleavage tank 1 by pump and valve again；Through above-mentioned outer
The material for being wrapped in diamond particles not being dissociated completely of separation equipment magnetic separation separation is enclosed, material material stock water tank is sequentially passed through
After in 4-1 and storage tank 4-2, continuation is dissociated in can returning to dissociation tank 1；Water system 4 can include material stock water tank 4-1, water storage
Case 4-2, water pump 4-3 and the valve 4-4 that adds water；
It is different according to the rotating speed that its agitator is stirred, discharge respectively graphite slurry, graphite+metal solvent carefully cut, graphite+gold
Category catalyst carefully cuts+diamond；Sequentially entering peripheral separation equipment 3 carries out screening separation, and the material for by screening separate enters and divides
Precipitated from material material stock water tank 4-1, when the water level in separation of material material stock water tank 4-1 reaches upper water level, water is overflowed to
The storage tank 4-2 being connected with material material stock water tank 4-1, the water in storage tank 4-2 is by being provided with water pump 4-3 with the valve 4- that adds water
4 pipeline is admitted to dissociation tank 1；Diamond is wrapped in through separate be not dissociated completely of above-mentioned peripheral separation equipment magnetic separation
After the material of grain is sequentially passed through in material material stock water tank 4-1 and storage tank 4-2, continuation is dissociated in returning to dissociation tank 1；
The abrading-ball and synthesis bar added in dissociation tank is the 30-60% of tank volume, and synthetic rod material and mill
The volume ratio of ball is 5%-50%；Described abrading-ball includes Ceramic Balls and steel ball, and described Ceramic Balls include aluminum oxide and oxygen
Change zirconium ball；The granularity of abrading-ball is φ 3-12mm；The linear velocity of agitating shaft stirring material is in 1m/s--6m/s；
Described peripheral separation equipment includes filter, and the fine graphite and metal solvent for dissociateing carefully are cut to carry out filtering de-
Water, graphite and catalyst after dehydration can enter magnetic separation or the shaking table separation circuit of bottom；
Described peripheral separation equipment includes magnetic separator, and the metal solvent dissociateed in next material is carefully cut magnetic separation to be separated
Out；
Described peripheral separation equipment includes agitator, and the fine graphite and metal solvent that dissociate carefully are cut with pumping mode
And diamond is realized separating with shaking table.
Positive beneficial effect：The present invention can make synthetic rod realize physics dissociating method graphite, metal solvent and Buddha's warrior attendant
Stone is separated from one another to be extracted, and is prevented or is at utmost reduced electrolysis and measured with acid；And it is with short production cycle, typically in dissociation tank
After a few minutes of start-up operation, just there is graphite to dissociate and come, it is possible to the row's of adding water graphite, and after ten minutes, it is possible to discharge
Diamond particles；Its preamble and postorder are added up typically can just produce diamond compound finished product in a shift.Dissociation
Tank dissociates synthetic rod efficiency based on 80%, and its tailing can return again to the tank that dissociates, it is also possible to use electrolysis PROCESS FOR TREATMENT, its electrolysis
Inventory then have dropped 80%；As tailing is processed using electrolysis, more than 90% metal solvent can be processed again, so, its electricity
The tailing of solution is exactly to use reactor acid treatment, its reactor treatment inventory only be left 2%, greatly reduce production cost and
For the pollution of environment, the process cycle of shortening substantially increases the competitiveness of enterprise.
Brief description of the drawings
Fig. 1 is purifying technique system block diagram of the invention；
Fig. 2 is purifying plant structural representation of the invention；
It is in figure：Dissociation tank 1, agitator 2, peripheral separation equipment 3, drum sieve 3-1, water system 4, separation of material material stock water
Case 4-1, storage tank 4-2, water pump 4-3, feed-water valve 4-4, mechanical lifting gear 5, rotating shaft 6, broken synthesis bar delivery device
7th, moisturizing pipeline a.
Specific embodiment
Below in conjunction with the accompanying drawings, the present invention is described further：
As shown in Figure 1 and Figure 2, a kind of physics dissociation purifying plant of diamond synthesizing rod, including dissociation tank 1, is arranged on solution
Agitator 2 on tank 1, the broken synthesis bar delivery device 7 being connected with dissociation tank 1, the top of described dissociation tank 1 is set
There is overflow blow tank, the peripheral separation equipment 3 of overflow blow tank connection, peripheral separation equipment connects water system 4, and water system 4 is connected
Dissociation tank 1 and filling pipe；
Described peripheral separation equipment 3 includes filter, screen(ing) machine, magnetic separator and agitator or its any combination；
Described water system 4 includes separation of material material stock water tank 4-1, the water storage being connected with separation of material material stock water tank 4-1
Case 4-2, the dissociation tank 1 being connected by pipeline with storage tank 4-2；Described storage tank 4-2 connects moisturizing pipeline a simultaneously, while
Water pump 4-3 and feed-water valve 4-4 is provided with storage tank 4-2 and the pipeline of the centre of dissociation tank 1；
The described top of dissociation tank 1 is provided with the motor being connected with agitator 2, the reductor with motor connection, reductor
Agitating shaft with mixing component is connected by shaft coupling；Mechanical lifting gear 5 is provided with described agitator 2；
Described dissociation tank 1 is vertical upper uncovered structure, and its ratio of height to diameter is 0.6-1.2: 1, and tank mouth is provided with overflow discharging
Groove；It is arranged on the agitator 2 inside dissociation tank 1 and includes paddle, vane type and bar type structure, wherein mixing part is high in tank
Spend in 3/4 altitude range；
The tank body periphery middle part of described dissociation tank 1 is symmetrically arranged with rotating shaft 6, and rotating shaft 6 is fixed by axle bed with frame；Turn
Tank body is fixed during axle tightening, and tank body can around the shaft turn round rollover to more than horizontal level when unclamping rotating shaft tightening.
The method purified using the physics dissociation purifying plant of above-mentioned diamond synthesizing rod, is comprised the following steps：
Synthesis bar after broken in broken synthesis bar delivery device 7 is put into dissociation tank 1, dissociation tank 1 is built-in
There are abrading-ball and aqueous medium；Agitator 2, the drive of the drive device that agitator 2 is constituted in motor and speed reducer are provided with dissociation tank 1
Under dynamic, the linear velocity for making the abrading-ball and material in aqueous medium to give is moved in tank, abrading-ball and conjunction during stirring movement
Into the comprehensive function that recirculation gas stripper effect, shearing-crushing power and attrition crushing power between abrading-ball etc. are produced between rod material particles
Under so that graphite is stripped first, is suspended in aqueous medium；Further, the metal solvent film that it is wrapped in diamond
Also shearing-crushing power and attrition crushing power between abrading-ball is stripped under acting on, and its metal solvent is carefully cut and the metal that dissociates
The diamond of catalyst film is existed in aqueous medium in the lump；So it is achieved that the solution of graphite, metal solvent and diamond three
From separation；
Realize graphite, metal solvent and the diamond of dissociation by being arranged on the overflow dissociated on tank 1 in dissociation tank 1
Blow tank, using outside drain tank by the way of upper discharge；The mode of described upper discharge is in given different speed of agitator；
Graphite fine powder is in and suspends completely during the slow-speed of revolution, to being added water in dissociation tank 1, makes the mixture of material from the tank mouth of dissociation tank 1
Overflow blow tank overflow, to discharge based on graphite slurry；When improving rotating speed and reaching metal solvent and also suspend completely, graphite and gold
Thin the cutting of category catalyst is overflowed by the overflow blow tank from the tank mouth of dissociation tank 1；And then improve rotating speed, the gold for being dissociated out
Hard rock is also reached when suspending completely, and diamond particles and graphite, metal solvent are carefully cut with aqueous medium in the lump from the tank mouth of dissociation tank 1
On overflow blow tank discharge；
It is different according to the rotating speed that its agitator is stirred, discharge respectively graphite slurry, graphite+metal solvent carefully cut, graphite+gold
Category catalyst carefully cuts+diamond；Sequentially entering peripheral separation equipment 3 carries out screening separation, and the material for by screening separate enters and divides
Precipitated from material material stock water tank 4-1, when the water level in separation of material material stock water tank 4-1 reaches upper water level, water is overflowed to
The storage tank 4-2 being connected with material material stock water tank 4-1, the water in storage tank 4-2 is by being provided with water pump 4-3 with the valve 4- that adds water
4 pipeline is admitted to dissociation tank 1；Diamond is wrapped in through separate be not dissociated completely of above-mentioned peripheral separation equipment magnetic separation
After the material of grain is sequentially passed through in material material stock water tank 4-1 and storage tank 4-2, continuation is dissociated in returning to dissociation tank 1；
The abrading-ball and synthesis bar added in dissociation tank is the 30-60% of tank volume, and synthetic rod material and mill
The volume ratio of ball is 5%-50%；Described abrading-ball includes Ceramic Balls and steel ball, and described Ceramic Balls include aluminum oxide and oxygen
Change zirconium ball；The granularity of abrading-ball is φ 3-12mm；The linear velocity of agitating shaft stirring material is in 1m/s--6m/s；
The speed of described upper discharge is equal to the addition flow for adding water；
Described peripheral separation equipment includes filter, and the fine graphite and metal solvent for dissociateing carefully are cut to carry out filtering de-
Water；
Including peripheral separation equipment include magnetic separator, dissociate come material in metal solvent carefully cut magnetic separation separate
Out.
Described peripheral separation equipment includes agitator, and the fine graphite and metal solvent that dissociate carefully are cut with pumping mode
And diamond is realized separating with shaking table.
The first section time that dissociation work starts, there is diamond to be dissociated out, in the stirring dissociation process in later stage,
Diamond particles may be frayed, and particularly low intensive diamond particles can be grated, and cause the excessively broken of diamond；Institute
With avoid and solve the diamond in dissociation process excessively crush it is critical that.Its method for solving to crush is
It is dissociated go out diamond particles carry out discharge in time.So in the course of work that dissociates, using time segment intermittent discharge side
Formula, i.e., after dissociation starts, arrange based on graphite when presented black lead wash water in having dissociateed graphite and water when adding water
Slurry；Wait having there is a certain amount of metal solvent to improve speed of agitator when being dissociated into thin cutting, graphite and metal are arranged when adding water
Catalyst carefully cuts slurry；After there are a certain amount of diamond particles to be dissociated out, speed of agitator high is just brought up to, discharge in time is
The diamond mass for dissociateing.
Have been drained off the graphite outside tank, metal solvent, diamond carries out individually separated and reclaims through the follow-up equipment of periphery,
It can not return again to tank internal disintegration by the diamond particles that the metal solvent of complete cleavage is wrapped up after magnetic separator is selected
Or processed by the electrolysis of postorder electrowinning process.
Water system, water tank and pump, valve and the pipeline composition with least more than one, the storage of the also simultaneous discharging of its water tank
Case；The water of its peripheral separation equipment discharge can also be discharged to the water system, by workshop water supply line when the water system needs moisturizing
Connection supply.
The course of work of the water system of its self-loopa is：Water tank has the original work of the water circulation that can meet Cleaving Process
Make water level；Water system adds the initial water for reaching working water level to cleavage tank during cleavage tank initialization；In material cleavage mistake
It is different according to the rotating speed that its agitator is stirred to being added water in tank in journey, can discharge respectively graphite, graphite+metal solvent carefully cut,
Graphite+metal solvent carefully cuts+diamond.
Peripheral separation equipment can configure screen(ing) machine, the fine graphite and metal solvent for dissociateing carefully to be cut realized with diamond and is sieved
Separate.
Peripheral separation equipment can be with configurating filtered machine, and the fine graphite and metal solvent for dissociateing carefully are cut to carry out filtering de-
Water.
Peripheral separation equipment can configure magnetic separator, the metal solvent dissociateed in next material is carefully cut magnetic separation and is isolated
Come.
Peripheral separation equipment can configure agitator, with pumping mode the fine graphite and metal solvent for dissociateing carefully cut with
And diamond is realized separating with shaking table.
Peripheral separation equipment can configure magnetic separator, and what what magnetic separation was separate be not dissociated completely is wrapped in diamond particles
Material can return again to continue to dissociate in dissociation tank.
Enter as recyclable economic materials after the graphite and metal solvent dewatered drying that through above-mentioned peripheral separation equipment separate
Capable other purposes.
The diamond for through above-mentioned peripheral separation equipment separate obtains pure Buddha's warrior attendant after carrying out cleaning treatment through finishing operations
Stone compound finished product.
Embodiment 1
As shown in figure 1,：By the synthesis bar less than 10mm for crushing, the dissociation with abrading-ball and aqueous medium is put into
In tank, its dissociation tank in have agitating shaft, on its agitating shaft have stirring rod or stirring vane, by mechanical force drive agitating shaft and
Stirring rod or stirring vane, make to stir it.General abrading-ball is inorganic porcelain ball, such as aluminum oxide, zirconium oxide, and its sphere diameter exists
φ3- 12mm；The volume ratio of abrading-ball and the synthesis bar for adding is not more than 1: 0.5；The linear velocity one that material is stirred in tank
As in 2m/s--8m/s.Abrading-ball and synthetic rod material are added from tank body top, add the amount of abrading-ball and synthesis bar general in tank
The 30-60% in body height is controlled, amount of water is that its water level peak is lower slightly not spill over tank mouth when normal stirring is exchanged views
It is advisable；In whipping process, under abrading-ball and synthetic rod material and aqueous medium effect, to the shearing-crushing of synthesis bar between abrading-ball
Under the comprehensive function of power and attrition crushing power etc., low intensive graphite is separated by the mechanical force between abrading-ball first, as thin
The graphite of grain, separates as the educt in aqueous medium first.
Continue to extend mixing time, be stripped graphite and be wrapped in metal solvent film the consulting in abrading-ball of diamond
It is stripped during mill and is come off, as tiny catalyst powder also into aqueous medium, this process is until most of catalyst film quilt
Stripping, the graphite being achieved in synthetic rod, metal solvent, diamond realize physical separation.
Graphite, metal solvent particulate and diamond are had been separated into, is discharged from tank body top by aqueous medium, its discharge
Mode is to improve agitator shaft speed, diamond, catalyst fine grained and graphite is fully suspended, while to being added water in tank, making in water
Diamond, catalyst fine grained and graphite in medium overflow from tank mouth simultaneously, outside material drain tank.
In above-mentioned technical process, graphite is separated at first, starts to realize that graphite is separated after general several minutes, this
Shi Buxu improves speed of agitator, only to being added water in tank the water containing graphite need to be made to be overflowed outside drain tank from tank mouth.This process can be with
Interval is carried out, it is possible to achieve at utmost discharge graphite in advance.During graphite is discharged, its metal solvent fine particles also can
Discharge therewith.
Under the effect of exchanging views of abrading-ball, the metal solvent film of diamond particles appearance parcel is successively progressively to be stripped
, if the diamond for being stripped catalyst film continues to be exchanged views in tank, it is likely to result in diamond particle surfaces
Fray, the diamond particles that will also result in low-intensity particle are crushed.In order to avoid transition is exchanged views to separated diamond
Grain causes to damage and excessively broken, in time the diamond discharge for having been carried out separate, and its method is to improve agitator shaft speed
To diamond in aqueous medium be in suspension, while add water to making from outside tank mouth drain tank.Certainly, the discharge purpose is discharge gold
Hard rock, but graphite and metal solvent the fine grained also companion discharge with aqueous medium.The process can be with row's graphite step knot
Close, such as first arrange graphite, then arrange diamond.
Above method process has been realized in synthetic rod physical method and realizes graphite, metal solvent, diamond three
Dissociation tank in separation, and in mixed state drain tank outside.
And the respective extraction of three is further realized, can be realized using periphery separation equipment using following：
Diamond is extracted in sieving：The graphite of the mixed state discharged from tank by aqueous medium, metal solvent fine grained, Buddha's warrior attendant
Stone, such as diamond are abrasive material level coarsenesses, can realize that the extraction of graphite+catalyst and diamond is separated with the method for sieving, and
Graphite+the catalyst of screenings can realize that the two is extracted and separate with shaking table or magnetic selection method.
Metal solvent is extracted in magnetic separation：The graphite of the mixed state discharged from tank by aqueous medium, metal solvent fine grained, gold
Hard rock, extracts metal solvent with magnetic selection method.Magnetic separation can also be the catalyst and diamond particles that not will be completely dissociated
Select, return again into dissociation tank continue to realize dissociation.
Shaking table extracts diamond：The material of discharge is delivered to shaking table, graphite and the thin separation cut of catalyst is realized or is realized gold
The separation of hard rock particle.
The material of the liquefied mixture of discharge, agitator is emitted into, the agitator makes solid material using agitating mode
Water-containing materials, are then delivered to shaking table by complete suspended state with pump, and the separation of target solids thing is realized with shaking table, graphite,
Metal solvent is carefully cut, diamond is extracted.
Embodiment 2
As shown in Fig. 2 a vertical upper end is open and top has a dissociation tank of overflow discharge, also one agitator,
The mixing part of agitator is located at the middle and lower part in dissociation tank；Agitator also has screw rod synchronous lifting device, can make to stir portion
Divide and rise to tank body upper oral part top completely, it is repaired inside agitator and cleaning dissociation tank；In order to realize that tank body is tieed up
Repair with thorough cleaning tank, the approximate center location on the outside of tank body has two symmetrical rotating shafts, by seat supports and fixation, branch
Seat is fitted and fixed in frame；Tank body is fixed during rotating shaft tightening, and tank body can around the shaft turn round rollover when unclamping rotating shaft tightening
To more than horizontal level.
A drum sieve 3-1 is configured in the outlet of dissociation tank body discharge, the material for sieving dissociation tank discharge, this implementation
The sieve bucket of example is divided into two-stage, and the first order is fine screen mesh, is mainly used in screening graphite powder and metal solvent is carefully cut, and the second level is to meet
The sieve bucket of diamond grit is sieved, mainly screening separates diamond；The sieve bucket lower section correspondence placement of drum sieve 3-1 can be filled with water
Hopper, the upper overflow lip position of hopper and storage tank realize that current are connected；The storage tank and the connection of water pump, its water pump go out
Waterpipe causes the position added water in the tank of direction on dissociation tank, also has valve on the outlet pipe, can adjust in dissociation tank
Amount of water.By the synthesis bar less than 10mm for crushing, put into the dissociation tank with abrading-ball and aqueous medium, its is general
Abrading-ball is inorganic porcelain ball, such as aluminum oxide, zirconium oxide, and its sphere diameter is in φ 3-12mm；Abrading-ball and the synthesis bar for adding
Volume ratio is general below 1: 0.5；The linear velocity that material is stirred in tank is in 2m/s--6m/s.Abrading-ball and synthetic rod thing
Material is added from tank body top, and the interior amount general control for adding abrading-ball and synthesis bar of tank is initial to add in the 30-60% of body height
Water be when normal stirring is exchanged views its water level peak not spill over, tank mouth is lower slightly to be advisable.
Its course of work is：In whipping process, under abrading-ball and synthetic rod material and aqueous medium effect, the pairing between abrading-ball
Under the comprehensive function of shearing-crushing power and attrition crushing power into bar etc., low intensive graphite is first by the machinery between abrading-ball
Power is separated, and as fine grain graphite, is separated first as the educt in aqueous medium.
Continue to extend mixing time, be stripped graphite and be wrapped in metal solvent film the consulting in abrading-ball of diamond
It is stripped during mill and is come off, as tiny catalyst powder also into aqueous medium, this process is until most of catalyst film quilt
Stripping, the graphite being achieved in synthetic rod, metal solvent, diamond realize physical separation.
Graphite, metal solvent particulate and diamond are had been separated into, is discharged from tank body top by aqueous medium, its discharge
Mode is to improve agitator shaft speed, diamond, catalyst fine grained and graphite is fully suspended, while to being added water in tank, making in water
Diamond, catalyst fine grained and graphite in medium overflow from tank mouth simultaneously, outside material drain tank.
In above-mentioned technical process, graphite is separated at first, starts to realize that graphite is separated after general several minutes, this
Shi Buxu improves speed of agitator, only the water containing graphite need to be made to be overflowed outside drain tank from tank mouth, the material of discharge to being added water in tank
Fluid is directly entered rotary screen, and the material graphite and water based on first order rotary screen its graphite are entered into following by screen cloth
The hopper being filled with water, it is possible to achieve a certain amount of aquadag, water overflows to storage tank after the water tank reaches water level.This process can
Carried out with interval, it is possible to achieve at utmost discharge graphite in advance.During graphite is discharged, its metal solvent fine particles
Can discharge therewith.
Under the effect of exchanging views of abrading-ball, the metal solvent film of diamond particles appearance parcel is successively progressively to be stripped
, if the diamond for being stripped catalyst film continues to be exchanged views in tank, it is likely to result in diamond particle surfaces
Fray, the diamond particles that will also result in low-intensity particle are crushed.In order to avoid transition is exchanged views to separated diamond
Grain causes to damage and excessively broken, in time the diamond discharge for having been carried out separate, and its method is to improve agitator shaft speed
To diamond in aqueous medium be in suspension, while add water to making from outside tank mouth drain tank.Relatively coarse grained Buddha's warrior attendant during discharge
Stone is reached by first order fine screen mesh and fall into the following hopper that is filled with water, diamond particles precipitation by screen cloth after bucket net is sieved in the second level
To bottom, and the water for getting off therewith is reached in arrange after overflow height storage tank.Certainly, the discharge purpose is discharge diamond,
But the graphite and metal solvent fine grained with aqueous medium are also in company with discharge.The process can be combined with row's graphite step, than
As first arranged graphite, then arrange diamond.
In discharging process, discharge the granularity of material if greater than second level sieve number, then can be from the low side of drum sieve 3-1
End is discharged, and is directly entered the following hopper that is filled with water.
Above method process has been realized in synthetic rod physical method and realizes graphite, metal solvent, diamond three
Separation in dissociation tank, and solid-liquor separation and material point in mixed state drain tank after outer through drum sieve 3-1 realizations substantially
From.
Discharge material can be used cooperatively directly with wet separator, be separated first, then again through screen(ing) machine or shaking table
Etc. realizing respective feed separation.
The material (containing after upper bar magnetic separation) of discharge can be carried out in being pumped to shaking table when suspending completely down to agitator in material
Feed separation.
Water-containing materials can be drained into centrifugal dehydration by the material of discharge by magnetic separation or the treated materials of drum sieve 3-1
Machine, discharges moisture, then carries out respective feed separation with shaking table or magnetic separator again.
The present invention can make synthetic rod realize physics dissociating method graphite, metal solvent and diamond extraction separated from one another
Out, prevent or at utmost reduce electrolysis and measured with acid；And with short production cycle, a few minutes typically started working in dissociation tank
Zhong Hou, just has graphite to dissociate and comes, it is possible to the row's of adding water graphite, and after ten minutes, it is possible to discharge diamond particles；Its
Preamble and postorder are added up typically can just produce diamond compound finished product in a shift.Dissociation tank dissociation synthetic rod effect
Based on 80%, its tailing can return again to the tank that dissociates to rate, it is also possible to which, with PROCESS FOR TREATMENT is electrolysed, inventory of its electrolysis then have dropped
80%；As tailing is processed using electrolysis, more than 90% metal solvent can be processed again, so, the tailing of its electrolysis is exactly to use
Reactor acid treatment, the inventory of its reactor treatment is only left 2%, greatly reduces production cost and the dirt for environment
Dye, the process cycle of shortening substantially increases the competitiveness of enterprise.
Embodiment described above has only related to the minority in many implementation methods of the invention, although description is more specific and detailed
Carefully, but can not therefore and be interpreted as the limitation to the scope of the claims of the present invention.It should be pointed out that for the common skill of this area
For art personnel, without departing from the inventive concept of the premise, some deformations and improvement are can be made into, these belong to this hair
Bright protection domain.
Claims (10)
1. diamond synthesizing rod physics dissociation purifying plant, it is characterised in that including dissociation tank (1), be arranged on dissociation tank (1)
On agitator (2), and dissociation tank (1) the broken synthesis bar delivery device (7) that is connected, the top of described dissociation tank (1)
Overflow blow tank is provided with, the peripheral separation equipment (3) of overflow blow tank connection, peripheral separation equipment connects water system (4), water system
System (4) connection dissociation tank (1) and filling pipe.
2. diamond synthesizing rod according to claim 1 physics dissociation purifying plant, it is characterised in that：Described periphery
Separation equipment (3) includes filter, magnetic separator, agitator and shaking table or its any combination.
3. diamond synthesizing rod according to claim 1 physics dissociation purifying plant, it is characterised in that：Described water system
System (4) includes separation of material material stock water tank (4-1), the storage tank (4-2) being connected with separation of material material stock water tank (4-1), with storage
The dissociation tank (1) that water tank (4-2) is connected by pipeline；Described storage tank (4-2) while connect moisturizing pipeline (a), while storage
Water pump (4-3) and feed-water valve (4-4) are provided with water tank (4-2) pipeline middle with dissociation tank (1).
4. diamond synthesizing rod according to claim 1 physics dissociation purifying plant, it is characterised in that：Described dissociation
Tank (1) top is provided with the motor being connected with agitator (2), and the reductor with motor connection, reductor is connected by shaft coupling
Agitating shaft with mixing component；Mechanical lifting gear (5) is provided with described agitator (2).
5. the diamond synthesizing rod according to claim 1-4 Arbitrary Terms physics dissociation purifying plant, it is characterised in that：Institute
The dissociation tank (1) stated is vertical upper uncovered structure, and its ratio of height to diameter is 0.6-1.2: 1, and tank mouth is provided with overflow blow tank；It is arranged on
To have paddle, vane type or bar type structure, wherein mixing part is 3/4 in tank inner height to the internal agitator (2) of dissociation tank (1)
In altitude range；The tank body periphery middle part of described dissociation tank (1) is symmetrically arranged with rotating shaft (6), and rotating shaft (6) is by axle bed and machine
Frame is fixed.
6. the method for being purified using the physics dissociation purifying plant of above-mentioned diamond synthesizing rod, is comprised the following steps：
Synthesis bar after broken in broken synthesis bar delivery device (7) is put into dissociation tank (1), in dissociation tank (1)
Equipped with abrading-ball and aqueous medium；Agitator (2), the driving that agitator (2) is constituted in motor and speed reducer are provided with dissociation tank (1)
Under the driving of device, the linear velocity for making the abrading-ball and material in aqueous medium to give is moved in tank, during stirring movement
The comprehensive of recirculation gas stripper effect, shearing-crushing power and attrition crushing power between abrading-ball etc. is produced between abrading-ball and synthetic rod material particles
Under cooperation is used so that graphite is stripped first, is suspended in aqueous medium；Further, the metal that it is wrapped in diamond
It is stripped under catalyst film shearing-crushing power also between abrading-ball and the effect of attrition crushing power, its metal solvent is carefully cut and dissociated
The diamond for falling metal solvent film exists in aqueous medium in the lump；So it is achieved that graphite, metal solvent and diamond three
The dissociation of person is separated；Realize graphite, metal solvent and the diamond of dissociation by being arranged on dissociation tank in dissociation tank (1)
(1) the overflow blow tank on, using outside drain tank by the way of upper discharge；The mode of described upper discharge is given different
Speed of agitator；In the slow-speed of revolution, graphite fine powder is in and suspends completely, to being added water in dissociation tank (1), makes the mixture of material from solution
Overflow blow tank in the tank mouth of tank (1) overflows, to discharge based on graphite slurry；It is also complete that raising rotating speed reaches metal solvent
During suspension, graphite and thin the cutting of metal solvent are overflowed by the overflow blow tank from the tank mouth of dissociation tank (1)；And then raising rotating speed,
The diamond for being dissociated out is also reached when suspending completely, and diamond particles and graphite, metal solvent are carefully cut with aqueous medium
Overflow blow tank discharge from the tank mouth of dissociation tank (1) in the lump；
Different according to the rotating speed that its agitator is stirred, discharge graphite slurry, graphite+metal solvent are carefully cut respectively, graphite+metal is touched
Matchmaker carefully cuts+diamond；Sequentially entering peripheral separation equipment (3) carries out screening separation, and the material for by screening separate enters separation
Material material stock water tank (4-1) is precipitated, when the water level in separation of material material stock water tank (4-1) reaches upper water level, water overflow
To the storage tank (4-2) being connected with material material stock water tank (4-1), water in storage tank (4-2) by be provided with water pump (4-3) and
Add water valve (4-4) pipeline be admitted to dissociation tank (1)；Through separate be not dissociated completely of above-mentioned peripheral separation equipment magnetic separation
It is wrapped in after the material of diamond particles sequentially passed through in material material stock water tank (4-1) and storage tank (4-2), returns to dissociation tank
(1) continue to dissociate in.
7. diamond synthesizing rod according to claim 6 physics dissociation method of purification, it is characterised in that：It is described to add solution
Abrading-ball and synthesis bar in tank are the 30-60% of tank volume, and the volume ratio of synthetic rod material and abrading-ball is 5%-
50%；Described abrading-ball includes Ceramic Balls and steel ball, and described Ceramic Balls include aluminum oxide and zirconia ball；The granularity of abrading-ball is
φ3-12mm；The linear velocity of agitating shaft stirring material is in 1m/s--6m/s.
8. diamond synthesizing rod according to claim 7 physics dissociation method of purification, it is characterised in that：Described periphery
Separation equipment includes filter, and the fine graphite and metal solvent for dissociateing carefully are cut carries out filtering means dehydration.
9. diamond synthesizing rod according to claim 7 physics dissociation method of purification, it is characterised in that：Described periphery
Separation equipment includes magnetic separator, the metal solvent dissociateed in next material is carefully cut magnetic separation and is separated.
10. diamond synthesizing rod according to claim 7 physics dissociation method of purification, it is characterised in that：Described is outer
Enclosing separation equipment includes agitator, and the fine graphite and metal solvent for dissociateing carefully are cut and diamond shaking table with pumping mode
Realize separating.
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| CN108277500A (en) * | 2018-04-14 | 2018-07-13 | 新郑市新材料专业孵化器服务中心 | A kind of diamond electrorefining device |
| CN109384222B (en) * | 2018-09-29 | 2020-08-07 | 河南省力量钻石股份有限公司 | Method for extracting diamond |
| CN110201939B (en) * | 2019-07-02 | 2024-05-31 | 华北水利水电大学 | Method and apparatus for fluidization separation of artificial diamond |
| CN114471929A (en) * | 2020-11-13 | 2022-05-13 | 石门县顺超科技发展有限公司 | Diamond purification device |
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| CN1003773B (en) * | 1987-05-19 | 1989-04-05 | 吉林省冶金研究所 | 3R type and 2H type graphite separation equipment |
| JP2624285B2 (en) * | 1988-03-15 | 1997-06-25 | 和子 山本 | Synthetic diamond separation equipment |
| CN1151893C (en) * | 2002-11-07 | 2004-06-02 | 华北工学院 | Pollution-free gas-phase oxidation separation purification method for artificial diamond |
| CN202864970U (en) * | 2012-09-05 | 2013-04-10 | 江苏海澜正和环境科技有限公司 | High-efficiency purifier |
| CN103922332B (en) * | 2014-04-01 | 2016-01-27 | 安庆市凯立金刚石科技有限公司 | A kind of artificial diamond purifying method |
| CN103896264A (en) * | 2014-04-01 | 2014-07-02 | 安庆市凯立金刚石科技有限公司 | Diamond synthesis rod purification process |
| CN204752216U (en) * | 2015-07-20 | 2015-11-11 | 三门峡天钻晶体材料有限公司 | Physics of synthetic stick of diamond purification device that dissociates |
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