CN106006629A - Method for recovering diamonds from sapphire grinding waste slurry and product of method - Google Patents
Method for recovering diamonds from sapphire grinding waste slurry and product of method Download PDFInfo
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- CN106006629A CN106006629A CN201610620711.8A CN201610620711A CN106006629A CN 106006629 A CN106006629 A CN 106006629A CN 201610620711 A CN201610620711 A CN 201610620711A CN 106006629 A CN106006629 A CN 106006629A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a method for recovering diamonds from sapphire grinding waste slurry and a product of the method. The specific technique is adopted to recover diamonds from sapphire grinding waste slurry without damaging the properties of the diamonds, thereby reutilizing the diamonds and reducing the discharge amount of harmful waste. The combination of centrifugal deoiling and saponifying deoiling can implement thorough solid-liquid separation, so the organic matter removal rate of the liquid is up to 80% or above. The sulfuric acid and perchloric acid react with impurities, so the solid organic matter (solid resins and copper powder) impurity removal rate is up to 95% or above. The centrifugal separation and settling separation are combined to implement separation and refinement, so that the aluminum oxide and bentonite impurity removal rate is up to 95% or above; and thus, the obtained diamond powder particles have high purity, can be used repeatedly, and can effectively lower the cost of the sapphire grinding processing technique.
Description
Technical field
The present invention relates to technical field of mineral processing, useless with grinding in particular to a kind of sapphire
Slip reclaims method and the product of diamond.
Background technology
Sapphire (Sapphire), mineral name corundum, trigonal system crystalline solid.Indigo plant in industry
Gem is a kind of monocrystalline (α-Al of aluminium oxide2O3), its Mohs' hardness reaches 9.0, is only second to diamond.
And the special lattice structure of sapphire also determines it and has excellent physical property and chemical stability,
Such as, fabulous thermal conductance, splendid electric insulating quality and light transmission, high temperature resistant, high intensity, height
Hardness etc..Therefore, sapphire is widely used in infrared military installation, guided missile, submarine, Gao Gong
The window material of rate light laser etc..Again due to sapphire C face and GaN single crystal film lattice constant mismatch
Rate is little, meets resistant to elevated temperatures requirement in GaN single crystal film growth course simultaneously, so, sapphire again by
As GaN/Al2O3The backing material that light emitting diode (LED) is ideal, is widely used in LED
In industry.In recent years, universal along with smart mobile phone, sapphire is again by the intensity, resistance to of its superelevation
Mill property and resistance to marring, be the most gradually applied to mobile phone screen, Touch control key, bonnet cover glass and take the photograph
As head diaphragm etc..The most all applications, the newest application, will stimulate blue precious
The demand of stone has a raising by a relatively large margin.
But, no matter which field is Sapphire Substrate be applied to, it is necessary first to do is exactly by sapphire
It is the thin slice about 800 μm that monocrystal crystal bar uses the methods such as diamond wire saw to cut into thickness, so
After to be processed into thickness by grinding step and polishing process again be the thin slice about 600 μm.And grind
Mill thinning process is one of link the most key in the sapphire course of processing, and it is related to sapphire lining
The product parameters such as the fineness of egative film, flatness, roughness.Sapphire Substrate slice lapping thinning process
Mainly with diamond as abrasive material, then by itself and aqueous solvent (predominantly ethylene glycol) or oil-based solvent
(predominantly white oil) mixes by a certain percentage, and adds suitable dispersant and be configured to certain density
Suspension, reaches to grind thinning effect by the mechanical grinding effect of diamond.At present, sapphire adds
The PCD micropowder used during work mainly has 5-9 (D50=6.5 ± 0.3 μm), 4-8 (D50=5.6
± 0.2 μm), several size specification such as 3-6 (D50=4.2 ± 0.2 μm).In process of lapping, gold
The granule of hard rock can be tapered, and granularity also can taper into, these diamond particles and process of lapping
The copper powder of middle generation, aluminium oxide etc. grind the liquid substances such as chip and abrasive solvents, auxiliary agent, abluent
Form grinding waste slurry material.And for this partial mill waste slurry, the main process of sapphire processing enterprise
Method walks hazardous waste disposal program according to laws and regulations exactly.The most descending in current economy, ring
Under the background that packing pressure continues to increase, danger useless processing cost spending is undoubtedly one for enterprise
No small burden；It addition, environment be also result in by the discharge of danger wastes digests pressure greatly.
If a kind of method can be invented, and the diadust in grinding waste slurry material is reclaimed, and will be recovered to
Diadust repeat recycling, will be possible not only to save the production cost of enterprise, it is also possible to greatly
The recycling and environmental conservation of promotion resource.
In the prior art subsequent treatment to grinding waste slurry material, can only be by complicated technique recovery section
The processing of sapphire front road is worth relatively low boron carbide particles, and is worth higher during rear road is processed
Diamond particles then cannot reclaim, and can only be wasted in follow-up offal treatment operation.
In view of this, the special proposition present invention.
Summary of the invention
The first object of the present invention is that providing a kind of sapphire to grind in slug reclaims diamond
Method, the method technique reclaiming diamond in described sapphire grinding slug is simple, it is possible to have
Imitating to grind waste material from sapphire and reclaim highly purified diamond dust granule, described powder particle is permissible
Repeatedly utilize, it is possible to effectively reduce the cost of sapphire grinding process technique.
The second object of the present invention is to provide a kind of employing in above-mentioned sapphire grinding slug to return
The method receiving diamond reclaims the diamond dust granule obtained, described diamond dust particle purity
Height, can repeatedly utilize, it is possible to effectively reduce the cost of sapphire grinding process technique.
In order to realize the above-mentioned purpose of the present invention, spy by the following technical solutions:
A kind of sapphire grinds the method reclaiming diamond in slug, comprises the steps:
(1) described sapphire is ground slug centrifugation de-oiling；
(2) gained is centrifuged bed material and carries out saponification oil removing；
(3) gained saponification slurry is saltoutd；
(4) gained is saltoutd material dissolution, dispersion in a solvent, be centrifuged clean；
(5) gained is centrifuged bed material and sulphuric acid and perchloric acid impurity removal reaction；
(6) being cleaned by gained material gravitational settling to pH is 6-7, and the dispersed with stirring that adds water is uniform, by institute
Obtain suspension to be centrifuged；
(7) gained is centrifuged bed material to react with sodium silicate solution, natural subsidence, gained solution again from
The heart collects centrifugal bed material, and gained is centrifuged bed material and cleans, dries, and obtains diamond dust granule.
The inventive method, uses special process, it is possible to grinds from sapphire and reclaims diamond slug,
Do not damage the performance of diamond self, make diamond reuse, reduce the discharge capacity of harmful waste；
Centrifugation de-oiling and saponification oil removing is used to coordinate, it is possible to make solid-liquid separation thorough, fluid organic material clearance
Reach more than 80%；Sulphuric acid and perchloric acid is used to react with impurity, solid organic matters (hard resin, copper powder)
Removal of impurity reaches more than 95%；Centrifugation and settlement separate combination, it is achieved separation and purification, aluminium oxide
Reaching more than 95% with bentonite removal of impurity, gained diamond dust particle purity is high, can repeat many
Secondary utilization, it is possible to effectively reduce the cost of sapphire grinding process technique.
Preferably, described sapphire is ground slug centrifugation de-oiling, use tripod pendulum type batch centrifugal or great Rong
The grinding waste material centrifugation de-oiling that amount tube centrifuge etc. will be collected, obtains centrifugal bed material；Gained is centrifuged the end
Containing diamond, copper powder, phenolic resin, aluminium oxide, Organic substance solvent etc. in material.
Described sapphire can be ground waste material and carry out preliminary removing oil by centrifugation de-oiling, it is simple to subsequent technique enters
One step removes other impurity.
Preferably, gained is centrifuged bed material and carries out in saponification oil removal process, to step (1) gained
Centrifugal bed material in add water, centrifugal bed material is 1:5-10, preferably 1:7-8 with the mass ratio of water,
More preferably 1:7.5；Adding alkali, bed material is 1:0.5-2 with the mass ratio of alkali, is preferably
1:1-1.5, more preferably 1:1.2, carry out saponification oil removing reaction.
Preferably, one or more during described alkali includes the highly basic such as sodium hydroxide, potassium hydroxide.
Preferably, reaction temperature is 90-100 DEG C, and the response time is 4-8h；Preferably, reaction temperature
For 92-98 DEG C, the response time is 5-7h；It is further preferred that reaction temperature is 94-96 DEG C, reaction
Time is 6h.
Use certain concentration and the aqueous slkali of consumption, react at a certain temperature, in conjunction with follow-up saltouing,
The operations such as dissolving, it is possible to effectively remove the oils and fats impurity remained in centrifugal bed material, it is simple to subsequent technique enters
OK, the purity of gained diamond dust granule is improved.
Preferably, after cooling, gained saponification slurry is added water and salt is saltoutd, after end of saltouing,
Material can float over liquid phase surface, and material bottom is clear water solution, and the clear water solution extracting bottom out can be by
Material skims collection.
Preferably, described salt includes the customary salt apoplexy due to endogenous wind such as sodium chloride, potassium chloride, sodium sulfate, sodium carbonate
One or more.
Preferably, material dissolution of being saltoutd by gained, dispersion in a solvent, are centrifuged cleaning；Described
Solvent includes the conventional organic solvents such as dehydrated alcohol, ethyl acetate, acetone or isopropanol；Saltout material
It is 1:2-6, preferably 1:3-5, more preferably 1:4 with the volume ratio of dehydrated alcohol；Then stir
Mix and be uniformly dispersed, be then centrifuged cleaning.
Use the solvent of specific consumption, it is possible to fully dissolve gained and saltout material, it is simple to remove oil residues
Fat impurity.
Preferably, gained is centrifuged bed material dry pulverize after again with sulphuric acid and perchloric acid impurity removal reaction.
Preferably, during gained is centrifuged bed material and sulphuric acid and perchloric acid impurity removal reaction, by gained from
Heart bed material adds in reactor, is subsequently adding concentrated sulphuric acid, and centrifugal bed material with the mass ratio of concentrated sulphuric acid is
0.8-2:30, preferably 1.2-1.6:30, more preferably 1.4:30；Course of reaction drips
Perchloric acid, centrifugal bed material is 1-1.6:3, preferably 1.2-1.4:3 with the mass ratio of perchloric acid, enters one
Step is preferably 1.3:3.
Preferably, the mass fraction of described concentrated sulphuric acid is 95%-98%；The mass fraction of described perchloric acid is
70%-75%.
Preferably, reaction temperature is 180-240 DEG C, and the response time is 2-8h；Preferably, reaction temperature
Degree is for 200-220 DEG C, and the response time is 4-6h；It is further preferred that reaction temperature is 208-212 DEG C,
Response time is 5h.
By centrifugal bed material at a certain temperature, sulphuric acid and perchloric acid with specific consumption react, it is possible to have
Effect removes the impurity such as copper powder, phenolic resin, organic solvent, it is simple to subsequent technique is carried out, and improves gained
The purity of diamond dust granule.
Preferably, in the reacted material of step (5) gained, add water carry out gravitational settling cleaning,
Until clean to the pH value of slurry be 6-7.
It is further preferred that the drying materials after being cleaned by gained is except water, obtain dried material, wherein
Mainly contain diamond, aluminium oxide and large granular impurity.
Preferably, adding water in the material after cleaning, material is 1:5-20 with the mass ratio of water, excellent
Elect 1:5-15 as, more preferably 1:10；Dispersed with stirring is uniform, obtains diamond and aluminium oxide
Suspension.
Preferably, described material carries out mass ratio calculating with its dry powder weight.
Preferably, collect finely dispersed suspension, centrifugal in centrifuge, isolate in material
Fine grained diamond and aluminium oxide.
Preferably, gained being centrifuged bed material and reacts with sodium silicate aqueous solution, natural subsidence separates, and separates
Go out the non-diamond granule foreign in centrifugal bed material.
Sodium silicate can react with remaining alumina impurities, and product can pass through natural subsidence,
Remove with precipitation form.
Preferably, the mass fraction of described sodium silicate aqueous solution is 0.01%-0.1%, is preferably
0.03%-0.07%, more preferably 0.05%.
Preferably, described in each step of the present invention, centrifugal bed material all carries out mass ratio calculating with its dry powder weight.
The above-mentioned above-mentioned sapphire that uses is used to grind the method recovery reclaiming diamond in slug
The diamond dust granule obtained.
Gained diamond dust particle purity is high, can repeatedly utilize, it is possible to effectively reduce blue precious
The cost of stone grinding process technique.
Compared with prior art, the invention have the benefit that
The inventive method, uses special process, it is possible to grinds from sapphire and reclaims diamond slug,
Do not damage the performance of diamond self, make diamond reuse, reduce the discharge capacity of harmful waste；
Centrifugation de-oiling and saponification oil removing is used to coordinate, it is possible to make solid-liquid separation thorough, fluid organic material clearance
Reach more than 80%；Sulphuric acid and perchloric acid is used to react with impurity, solid organic matters (hard resin, copper powder)
Removal of impurity reaches more than 95%；Centrifugation and settlement separate combination, it is achieved separation and purification, aluminium oxide
Reaching more than 95% with bentonite removal of impurity, gained diamond dust particle purity is high, can repeat many
Secondary utilization, it is possible to effectively reduce the cost of sapphire grinding process technique.
Detailed description of the invention
Below in conjunction with detailed description of the invention, technical scheme is clearly and completely described,
Implement it will be appreciated by those skilled in the art that following described embodiment is a part of the present invention
Example rather than whole embodiments, be merely to illustrate the present invention, and be not construed as limiting the present invention's
Scope.Based on the embodiment in the present invention, those of ordinary skill in the art are not making creative labor
The every other embodiment obtained under dynamic premise, broadly falls into the scope of protection of the invention.In embodiment
Unreceipted actual conditions person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or
Instrument unreceipted production firm person, being can be by the commercially available conventional products bought and obtain.
Embodiment 1
A kind of sapphire grinds the method reclaiming diamond in slug, comprises the steps:
(1) the grinding waste material centrifugation de-oiling using tripod pendulum type batch centrifugal to collect, obtains centrifugal bed material；From
Containing diamond, copper powder, phenolic resin, aluminium oxide, Organic substance solvent etc. in heart bed material；
(2) in the centrifugal bed material of step (1) gained, pure water is added, centrifugal bed material and pure water
Mass ratio be 1:5, add sodium hydrate solid, centrifugal bed material with the mass ratio of sodium hydroxide is
1:0.5；Then mixed slurry is put in water-bath, while stirring heating in water bath, carry out saponification oil removing
Reaction, reaction temperature is 90-92 DEG C, and the response time is 8h；
(3), after saponification terminates, reacted slurry is poured in the Plastic Drum equipped with cold pure water,
Add enough sodium chloride, carry out operation of saltouing；Saltouing after end, material can float over water liquid surface, thing
Material bottom is clear water solution, and material can be skimmed collection by the clear water solution extracting bottom out；
(4) in step (3) gained material, add the volume of ethanol solution, material and ethanol solution
Ratio is 1:2-6, and then dispersed with stirring is uniform, then is centrifuged cleaning with pure water；
(5) the centrifugal bed material after step (4) eccentric cleaning is dried, then pulverize；
(6) the centrifugal bed material that step (5) crushes is put in quartz reaction still, add dense sulfur
Acid, centrifugal bed material is 2:30 with the mass ratio of concentrated sulphuric acid, and reaction temperature is 180-184 DEG C, during reaction
Between be 8h；Dripping perchloric acid in course of reaction, centrifugal bed material is 1.6:3 with the mass ratio of perchloric acid；
This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(7) in step (6) reacted material, add pure water and carry out gravitational settling cleaning, directly
It is 6-7 to the pH value cleaned to slurry；
(8) material cleaned for step (7) is dried again except water, obtain dried material；Wherein
Mainly contain diamond, aluminium oxide and large granular impurity；
(9) in the dried material that step (8) obtains, add the matter of pure water, material and pure water
Amount ratio is 1:5, and then dispersed with stirring is uniform, obtains the suspension of diamond and aluminium oxide；
(10) finely dispersed suspension is taken centrifugal, to isolate thin in material in centrifuge
Particle diamond and aluminium oxide；Gained is centrifuged bed material and imports in glass beaker again, adds enough quality and divides
Number is the sodium silicate solution of 0.01%, carries out natural subsidence separation, to be separated off out in centrifugal bed material
Non-diamond granule foreign；
(11) gained solution recentrifuge collects centrifugal bed material, and adds pure water and be carried out, so
Post-drying removes moisture removal, the i.e. available diamond dust granule that can reuse.
Embodiment 2
A kind of sapphire grinds the method reclaiming diamond in slug, comprises the steps:
(1) the grinding waste material centrifugation de-oiling using tripod pendulum type batch centrifugal to collect, obtains centrifugal bed material；From
Containing diamond, copper powder, phenolic resin, aluminium oxide, Organic substance solvent etc. in heart bed material；
(2) in the centrifugal bed material of step (1) gained, pure water is added, centrifugal bed material and pure water
Mass ratio be 1:10, add potassium hydroxide solid, centrifugal bed material with the mass ratio of potassium hydroxide is
1:2；Then mixed slurry is put in water-bath, while stirring heating in water bath, carry out saponification oil removing anti-
Should, reaction temperature is 98-100 DEG C, and the response time is 4h；
(3), after saponification terminates, reacted slurry is poured in the Plastic Drum equipped with cold pure water,
Add enough potassium chloride, carry out operation of saltouing；Saltouing after end, material can float over water liquid surface, thing
Material bottom is clear water solution, and material can be skimmed collection by the clear water solution extracting bottom out；
(4) in step (3) gained material, add the volume of ethanol solution, material and ethanol solution
Ratio is 1:6, and then dispersed with stirring is uniform, then is centrifuged cleaning with pure water；
(5) the centrifugal bed material after step (4) eccentric cleaning is dried, then pulverize；
(6) the centrifugal bed material that step (5) crushes is put in quartz reaction still, add dense sulfur
Acid, centrifugal bed material is 0.8:30 with the mass ratio of concentrated sulphuric acid；Reaction temperature is 236-240 DEG C, reaction
Time is 2h；Dripping perchloric acid in course of reaction, centrifugal bed material is 1:3 with the mass ratio of perchloric acid；
This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(7) in step (6) reacted material, add pure water and carry out gravitational settling cleaning, directly
It is 6-7 to the pH value cleaned to slurry；
(8) material cleaned for step (7) is dried again except water, obtain dried material；Wherein
Mainly contain diamond, aluminium oxide and large granular impurity；
(9) in the dried material that step (8) obtains, add the matter of pure water, material and pure water
Amount ratio is 1:20, and then dispersed with stirring is uniform, obtains the suspension of diamond and aluminium oxide；
(10) finely dispersed suspension is taken centrifugal, to isolate thin in material in centrifuge
Particle diamond and aluminium oxide；Gained is centrifuged bed material and imports in glass beaker again, adds enough quality and divides
Number is the sodium silicate solution of 0.1%, carries out natural subsidence separation, to be separated off out in centrifugal bed material
Non-diamond granule foreign；
(11) gained solution recentrifuge collects centrifugal bed material, and adds pure water and be carried out, so
Post-drying removes moisture removal, the i.e. available diamond dust granule that can reuse.
Embodiment 3
A kind of sapphire grinds the method reclaiming diamond in slug, comprises the steps:
(1) the grinding waste material centrifugation de-oiling using tripod pendulum type batch centrifugal to collect, obtains centrifugal bed material；From
Containing diamond, copper powder, phenolic resin, aluminium oxide, Organic substance solvent etc. in heart bed material；
(2) in the centrifugal bed material of step (1) gained, pure water is added, centrifugal bed material and pure water
Mass ratio be 1:7, add sodium hydrate solid, centrifugal bed material with the mass ratio of sodium hydroxide is
1:1；Then mixed slurry is put in water-bath, while stirring heating in water bath, carry out saponification oil removing anti-
Should, reaction temperature is 92-94 DEG C, and the response time is 7h；
(3), after saponification terminates, reacted slurry is poured in the Plastic Drum equipped with cold pure water,
Add sufficient amount of sulfuric acid sodium, carry out operation of saltouing；Saltouing after end, material can float over water liquid surface, thing
Material bottom is clear water solution, and material can be skimmed collection by the clear water solution extracting bottom out；
(4) in step (3) gained material, add the volume of ethanol solution, material and ethanol solution
Ratio is 1:3, and then dispersed with stirring is uniform, then is centrifuged cleaning with pure water；
(5) the centrifugal bed material after step (4) eccentric cleaning is dried, then pulverize；
(6) the centrifugal bed material that step (5) crushes is put in quartz reaction still, add dense sulfur
Acid, centrifugal bed material is 1.6:30 with the mass ratio of concentrated sulphuric acid；Reaction temperature is 198-202 DEG C, reaction
Time is 6h；Dripping perchloric acid in course of reaction, centrifugal bed material is 1.4:3 with the mass ratio of perchloric acid；
This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(7) in step (6) reacted material, add pure water and carry out gravitational settling cleaning, directly
It is 6-7 to the pH value cleaned to slurry；
(8) material cleaned for step (7) is dried again except water, obtain dried material；Wherein
Mainly contain diamond, aluminium oxide and large granular impurity；
(9) in the dried material that step (8) obtains, add the matter of pure water, material and pure water
Amount ratio is 1:5, and then dispersed with stirring is uniform, obtains the suspension of diamond and aluminium oxide；
(10) finely dispersed suspension is taken centrifugal, to isolate thin in material in centrifuge
Particle diamond and aluminium oxide；Gained is centrifuged bed material and imports in glass beaker again, adds enough quality and divides
Number is the sodium silicate solution of 0.03%, carries out natural subsidence separation, to be separated off out in centrifugal bed material
Non-diamond granule foreign；
(11) gained solution recentrifuge collects centrifugal bed material, and adds pure water and be carried out, so
Post-drying removes moisture removal, the i.e. available diamond dust granule that can reuse.
Embodiment 4
A kind of sapphire grinds the method reclaiming diamond in slug, comprises the steps:
(1) the grinding waste material centrifugation de-oiling using tripod pendulum type batch centrifugal to collect, obtains centrifugal bed material；From
Containing diamond, copper powder, phenolic resin, aluminium oxide, Organic substance solvent etc. in heart bed material；
(2) in the centrifugal bed material of step (1) gained, pure water is added, centrifugal bed material and pure water
Mass ratio be 1:8, add potassium hydroxide solid, centrifugal bed material with the mass ratio of potassium hydroxide is
1:1.5, then puts in water-bath by mixed slurry, while stirring heating in water bath, carries out saponification oil removing
Reaction, reaction temperature is 96-98 DEG C, and the response time is 5h；
(3), after saponification terminates, reacted slurry is poured in the Plastic Drum equipped with cold pure water,
Add enough sodium carbonate, carry out operation of saltouing；Saltouing after end, material can float over water liquid surface, thing
Material bottom is clear water solution, and material can be skimmed collection by the clear water solution extracting bottom out；
(4) in step (3) gained material, add the volume of ethanol solution, material and ethanol solution
Ratio is 1:5, and then dispersed with stirring is uniform, then is centrifuged cleaning with pure water；
(5) the centrifugal bed material after step (4) eccentric cleaning is dried, then pulverize；
(6) the centrifugal bed material that step (5) crushes is put in quartz reaction still, add dense sulfur
Acid, centrifugal bed material is 1.2:30, more preferably 1.4:30 with the mass ratio of concentrated sulphuric acid；Reaction temperature
Degree is for 218-222 DEG C, and the response time is 4h；In course of reaction, drip perchloric acid, centrifugal bed material with
The mass ratio of perchloric acid is 1.2:3；This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(7) in step (6) reacted material, add pure water and carry out gravitational settling cleaning, directly
It is 6-7 to the pH value cleaned to slurry；
(8) material cleaned for step (7) is dried again except water, obtain dried material；Wherein
Mainly contain diamond, aluminium oxide and large granular impurity；
(9) in the dried material that step (8) obtains, add the matter of pure water, material and pure water
Amount ratio is 1:15, and then dispersed with stirring is uniform, obtains the suspension of diamond and aluminium oxide；
(10) finely dispersed suspension is taken centrifugal, to isolate thin in material in centrifuge
Particle diamond and aluminium oxide；Gained is centrifuged bed material and imports in glass beaker again, adds enough quality and divides
Number is the sodium silicate solution of 0.07%, carries out natural subsidence separation, to be separated off out in centrifugal bed material
Non-diamond granule foreign；
(11) gained solution recentrifuge collects centrifugal bed material, and adds pure water and be carried out, so
Post-drying removes moisture removal, the i.e. available diamond dust granule that can reuse.
Embodiment 5
A kind of sapphire grinds the method reclaiming diamond in slug, comprises the steps:
(1) the grinding waste material centrifugation de-oiling using tripod pendulum type batch centrifugal to collect, obtains centrifugal bed material；From
Containing diamond, copper powder, phenolic resin, aluminium oxide, Organic substance solvent etc. in heart bed material；
(2) in the centrifugal bed material of step (1) gained, pure water is added, centrifugal bed material and pure water
Mass ratio be 1:7.5, add sodium hydrate solid, centrifugal bed material with the mass ratio of sodium hydroxide is
1:1.2；Then mixed slurry is put in water-bath, while stirring heating in water bath, carry out saponification oil removing
Reaction, reaction temperature is 94-96 DEG C, and the response time is 6h；
(3), after saponification terminates, reacted slurry is poured in the Plastic Drum equipped with cold pure water,
Add enough sodium chloride, carry out operation of saltouing；Saltouing after end, material can float over water liquid surface, thing
Material bottom is clear water solution, and material can be skimmed collection by the clear water solution extracting bottom out；
(4) in step (3) gained material, add the volume of ethanol solution, material and ethanol solution
Ratio is 1:4, and then dispersed with stirring is uniform, then is centrifuged cleaning with pure water；
(5) the centrifugal bed material after step (4) eccentric cleaning is dried, then pulverize；
(6) the centrifugal bed material that step (5) crushes is put in quartz reaction still, add dense sulfur
Acid, centrifugal bed material is 1.4:30 with the mass ratio of concentrated sulphuric acid；Reaction temperature is 208-212 DEG C, reaction
Time is 5h；Dripping perchloric acid in course of reaction, centrifugal bed material is 1.3:3 with the mass ratio of perchloric acid；
This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(7) in step (6) reacted material, add pure water and carry out gravitational settling cleaning, directly
It is 6-7 to the pH value cleaned to slurry；
(8) material cleaned for step (7) is dried again except water, obtain dried material；Wherein
Mainly contain diamond, aluminium oxide and large granular impurity；
(9) in the dried material that step (8) obtains, add the matter of pure water, material and pure water
Amount ratio is 1:10, and then dispersed with stirring is uniform, obtains the suspension of diamond and aluminium oxide；
(10) finely dispersed suspension is taken centrifugal, to isolate thin in material in centrifuge
Particle diamond and aluminium oxide；Gained is centrifuged bed material and imports in glass beaker again, adds enough quality and divides
Number is the sodium silicate solution of 0.05%, carries out natural subsidence separation, to be separated off out in centrifugal bed material
Non-diamond granule foreign；
(11) gained solution recentrifuge collects centrifugal bed material, and adds pure water and be carried out, so
Post-drying removes moisture removal, the i.e. available diamond dust granule that can reuse.
Embodiment of the present invention 1-5 method gained diamond dust particulate component (mass fraction) is carried out
Detection, result is as follows:
Table 1 present invention grinds, from sapphire, the diamond components testing result reclaimed slug
By table 1 it can be seen that sapphire of the present invention grinds the method reclaiming diamond in slug,
Can effectively remove sapphire grind the copper powder in slug, phenolic resin, aluminium oxide, bentonite,
The impurity such as Organic substance solvent, gained diamond dust particle purity is high, can repeatedly utilize, energy
Enough costs effectively reducing sapphire grinding process technique.
Although illustrate and describing the present invention with specific embodiment, however it will be appreciated that above respectively
Embodiment only in order to technical scheme to be described, is not intended to limit；The ordinary skill of this area
Personnel it is understood that without departing from the spirit and scope of the present invention, can be to aforementioned each reality
Execute the technical scheme described in example to modify, or the most some or all of technical characteristic is carried out
Equivalent；And these amendments or replacement, do not make the essence of appropriate technical solution depart from the present invention
The scope of each embodiment technical scheme；It is, therefore, intended that include belonging to this in the following claims
All these substitutions and modifications in invention scope.
Claims (10)
1. a sapphire grinds the method reclaiming diamond in slug, it is characterised in that bag
Include following steps:
(1) described sapphire is ground slug centrifugation de-oiling；
(2) gained is centrifuged bed material and carries out saponification oil removing；
(3) gained saponification slurry is saltoutd；
(4) gained is saltoutd material dissolution, dispersion in a solvent, be centrifuged clean；
(5) gained is centrifuged bed material and sulphuric acid and perchloric acid impurity removal reaction；
(6) being cleaned by gained material gravitational settling to pH is 6-7, and the dispersed with stirring that adds water is uniform, will
Gained suspension is centrifuged；
(7) gained being centrifuged bed material to react with sodium silicate solution, natural subsidence, gained solution is again
Centrifugal collection is centrifuged bed material, and gained is centrifuged bed material and cleans, dries, and obtains diamond dust granule.
A kind of sapphire the most according to claim 1 grinds the side reclaiming diamond in slug
Method, it is characterised in that gained is centrifuged bed material and carries out in saponification oil removal process, to step (1)
Adding water in the centrifugal bed material of gained, centrifugal bed material is 1:5-10, preferably 1:7-8 with the mass ratio of water,
More preferably 1:7.5；Adding alkali, bed material is 1:0.5-2 with the mass ratio of alkali, is preferably
1:1-1.5, more preferably 1:1.2, heating carries out saponification.
A kind of sapphire the most according to claim 1 grinds the side reclaiming diamond in slug
Method, it is characterised in that described saponification temperature is 90-100 DEG C, the response time is 4-8h；Preferably
Ground, reaction temperature is 92-98 DEG C, and the response time is 5-7h；It is further preferred that reaction temperature is
94-96 DEG C, the response time is 6h.
A kind of sapphire the most according to claim 1 grinds and reclaims diamond in slug
Method, it is characterised in that described solvent includes dehydrated alcohol, ethyl acetate, acetone or isopropanol.
A kind of sapphire the most according to claim 4 grinds and reclaims diamond in slug
Method, it is characterised in that the volume ratio of saltout material and dehydrated alcohol is 1:2-6, preferably 1:3-5,
More preferably 1:4.
A kind of sapphire the most according to claim 1 grinds the side reclaiming diamond in slug
Method, it is characterised in that during gained is centrifuged bed material and sulphuric acid and perchloric acid impurity removal reaction, by institute
Bed material must be centrifuged add in reactor, be subsequently adding concentrated sulphuric acid, centrifugal bed material and the mass ratio of concentrated sulphuric acid
For 0.8-2:30, preferably 1.2-1.6:30, more preferably 1.4:30；Course of reaction is dripped
Adding perchloric acid, centrifugal bed material is 1-1.6:3, preferably 1.2-1.4:3 with the mass ratio of perchloric acid, enters
One step is preferably 1.3:3.
A kind of sapphire the most according to claim 1 grinds the side reclaiming diamond in slug
Method, it is characterised in that the reaction temperature that gained is centrifuged bed material and sulphuric acid and perchloric acid impurity removal reaction is
180-240 DEG C, the response time is 2-8h；Preferably, reaction temperature is 200-220 DEG C, the response time
For 4-6h；It is further preferred that reaction temperature is 208-212 DEG C, the response time is 5h.
A kind of sapphire the most according to claim 1 grinds and reclaims diamond in slug
Method, it is characterised in that cleaning gained material gravitational settling to pH is 6-7, add water stirring point
Dissipating uniformly, material is 1:5-20, preferably 1:5-15, more preferably 1:10 with the mass ratio of water；
Dispersed with stirring is uniform, obtains the suspension of diamond and aluminium oxide.
A kind of sapphire the most according to claim 1 grinds and reclaims diamond in slug
Method, it is characterised in that the mass fraction of described sodium silicate aqueous solution is 0.01%-0.1%, preferably
For 0.03%-0.07%, more preferably 0.05%.
10. use the arbitrary described above-mentioned sapphire that uses of claim 1-9 to grind in slug
The method reclaiming diamond reclaims the diamond dust granule obtained.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829953A (en) * | 2017-02-14 | 2017-06-13 | 北京国瑞升科技股份有限公司 | A kind of diamond recovery and the method for recycling and product |
| CN108002388A (en) * | 2017-11-09 | 2018-05-08 | 重庆大学 | Boron carbide efficient circulation recycles new method in a kind of Sapphire Substrate grinding waste liquid |
| CN110540199A (en) * | 2018-07-10 | 2019-12-06 | 蓝思科技（长沙）有限公司 | Method for extracting diamond powder from aqueous diamond liquid |
| CN113415817A (en) * | 2021-07-22 | 2021-09-21 | 东莞晶驰光电科技有限公司 | Method for regenerating sapphire raw material and regenerated sapphire |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229113A (en) * | 2011-06-07 | 2011-11-02 | 王楚雯 | Method for recovering sapphire powder |
| CN103350996A (en) * | 2013-06-29 | 2013-10-16 | 开封恒锐新金刚石制品有限公司 | Method of recycling diamond from liquid resin |
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2016
- 2016-08-01 CN CN201610620711.8A patent/CN106006629B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229113A (en) * | 2011-06-07 | 2011-11-02 | 王楚雯 | Method for recovering sapphire powder |
| CN103350996A (en) * | 2013-06-29 | 2013-10-16 | 开封恒锐新金刚石制品有限公司 | Method of recycling diamond from liquid resin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829953A (en) * | 2017-02-14 | 2017-06-13 | 北京国瑞升科技股份有限公司 | A kind of diamond recovery and the method for recycling and product |
| CN108002388A (en) * | 2017-11-09 | 2018-05-08 | 重庆大学 | Boron carbide efficient circulation recycles new method in a kind of Sapphire Substrate grinding waste liquid |
| CN110540199A (en) * | 2018-07-10 | 2019-12-06 | 蓝思科技（长沙）有限公司 | Method for extracting diamond powder from aqueous diamond liquid |
| CN113415817A (en) * | 2021-07-22 | 2021-09-21 | 东莞晶驰光电科技有限公司 | Method for regenerating sapphire raw material and regenerated sapphire |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106006629B (en) | 2017-11-14 |
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Effective date of registration: 20180108 Address after: 124000 Shuangtaizi District Fine Chemical Industry Park hatching base, Panjin City, Liaoning Province, A22 Patentee after: Panjin guoruisheng Technology Co., Ltd. Address before: 102500 Beijing City, Fangshan District Yanshan Gang Nan Lu Dong Yi Xiang C No. 6 room 218 Patentee before: Beijing Polystar Hitech Ltd. |