CN106241794B - It is a kind of that the method and product that diamond is reclaimed in slug are ground from sapphire - Google Patents
It is a kind of that the method and product that diamond is reclaimed in slug are ground from sapphire Download PDFInfo
- Publication number
- CN106241794B CN106241794B CN201610621402.2A CN201610621402A CN106241794B CN 106241794 B CN106241794 B CN 106241794B CN 201610621402 A CN201610621402 A CN 201610621402A CN 106241794 B CN106241794 B CN 106241794B
- Authority
- CN
- China
- Prior art keywords
- diamond
- slug
- bed material
- ground
- centrifugation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
Abstract
The invention provides a kind of method and product that recovery diamond in slug is ground from sapphire.The inventive method, using special process, it can be ground from sapphire in slug and reclaim diamond, do not damaged the performance of diamond itself, reuse diamond, reduce the discharge capacity of harmful waste；Centrifugally operated successively is used, separation of solid and liquid can be made thorough, fluid organic material clearance is up to more than 80%；Reacted using sulfuric acid and perchloric acid and impurity, solid organic matters (hard resin, copper powder) removal of impurity is up to more than 95%；Centrifuge and sedimentation separation combines, realize separation and purification, aluminum oxide and bentonite removal of impurity up to more than 95%, gained diamond dust particle purity is high, can repeatedly utilize, can effectively reduce the cost of sapphire grinding process technique.
Description
Technical field
The present invention relates to technical field of mineral processing, grinds in slug and reclaims from sapphire in particular to one kind
The method and product of diamond.
Background technology
Sapphire (Sapphire), mineral name corundum, trigonal system crystalline solid.Sapphire in industry is aluminum oxide
A kind of monocrystalline (α-Al2O3), its Mohs' hardness reaches 9.0, is only second to diamond.And the special lattice structure of sapphire is also determined
Having determined it has excellent physical property and chemical stability, such as, fabulous thermal conductance, splendid electric insulating quality and printing opacity
Property, high temperature resistant, high intensity, high rigidity etc..Therefore, sapphire is widely used in infrared military installation, guided missile, submarine, height
The window material of power light laser etc..Again because sapphire C faces and GaN single crystal film lattice constant mismatch rate are small, meet simultaneously
Resistant to elevated temperatures requirement in GaN single crystal film growth course, so, sapphire is again by as GaN/Al2O3Light emitting diode (LED) is most
For preferable backing material, it is widely used in LED industry.In recent years, as the popularization of smart mobile phone, sapphire rely on again
Intensity, wearability and the resistance to marring of its superelevation, mobile phone screen, Touch control key, bonnet cover glass gradually it have been applied to and have taken the photograph
As head diaphragm etc..A variety of application fields above, especially new application field, will stimulate sapphire demand to have one
Raising by a relatively large margin.
But no matter which field is Sapphire Substrate be applied to, it is necessary first to which what is done is exactly by sapphire monocrystal crystal bar
The methods of using diamond wire saw cuts into thickness as 800 μm or so of thin slice, then passes through grinding step and buffer again
Sequence is processed into the thin slice that thickness is 600 μm or so.And it is the most key in sapphire process to grind thinning process
One of link, it is related to the product parameters such as the finish, flatness, roughness of sapphire substrate sheet.Sapphire substrate sheet is ground
Thinning process is ground mainly using diamond as abrasive material, then it is (main with aqueous solvent (predominantly ethylene glycol) or oil-based solvent
For white oil) mix by a certain percentage, and add appropriate dispersant and be configured to certain density suspension, pass through the machine of diamond
Tool ablation reaches grinding and effect is thinned.At present, the PCD micro mists used in sapphire process mainly have 5-9 (D50=
6.5 ± 0.3 μm), 4-8 (D50=5.6 ± 0.2 μm), several size specifications such as 3-6 (D50=4.2 ± 0.2 μm).Ground
Cheng Zhong, the particle of diamond can be tapered, and granularity can also taper into, caused by these diamond particles and process of lapping
Grinding chip and abrasive solvents, auxiliary agent, cleaning agent etc. the liquid substance such as copper powder, aluminum oxide form grinding waste slurry material.And for this
Partial mill waste slurry, the main methods of sapphire processing enterprise are exactly to walk hazardous waste disposal journey according to laws and regulations
Sequence.Constantly descending in current economy, under the background that environmental protection pressure continues to increase, dangerous waste processing cost is paid wages for enterprise
A undoubtedly no small burden；In addition, the discharge of danger wastes also result in greatly digestion pressure to environment.If energy
Invent a kind of method to reclaim the diadust in grinding waste slurry material, and the diadust being recovered to is repeated into profit again
With, will can not only save the production cost of enterprise, can also greatly facilitate resource recycle and environmental protection.
Prior art is to that in the subsequent treatment of grinding waste slurry material, can only pass through the preceding road of technique recovery section sapphire of complexity
Relatively low boron carbide particles are worth in processing, and being worth higher diamond particles in being processed for rear road can not then reclaim, only
It can be wasted in follow-up offal treatment process.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention in provide it is a kind of from sapphire grind slug in reclaim diamond method, it is described
From sapphire grind slug in reclaim diamond method technique it is simple, can effectively from sapphire grind waste material in reclaim
The diamond dust particle of high-purity, the powder particle can be utilized repeatedly, can effectively be reduced sapphire grinding and be added
The cost of work technique.
The second object of the present invention is reclaiming diamond in offer is a kind of using the above-mentioned grinding slug from sapphire
Method reclaim obtained diamond dust particle, described diamond dust particle purity is high, can repeatedly utilize, energy
Enough costs for effectively reducing sapphire grinding process technique.
In order to realize the above-mentioned purpose of the present invention, spy uses following technical scheme：
It is a kind of that the method that diamond is reclaimed in slug is ground from sapphire, comprise the following steps：
(1) sapphire is ground into slug centrifugation de-oiling；
(2) gained centrifugation bed material is disperseed with solvent, eccentric cleaning；
(3) gained is centrifuged into bed material and sulfuric acid and perchloric acid impurity removal reaction；
(4) it is 6-7 to clean resulting material gravitational settling to pH, adds water to be dispersed with stirring uniformly, gained suspension is centrifuged；
(5) gained is centrifuged into bed material to react with sodium silicate solution, centrifugation bottom is collected by centrifugation in natural subsidence, resulting solution again
Material, the cleaning of gained centrifugation bed material, drying, obtains diamond dust particle.
The inventive method, using special process, it can be ground from sapphire in slug and reclaim diamond, not damage Buddha's warrior attendant
The performance of stone itself, reuses diamond, reduces the discharge capacity of harmful waste；Centrifugally operated successively is used, can be made solid
Liquid separation is thorough, and fluid organic material clearance is up to more than 80%；Reacted using sulfuric acid and perchloric acid with impurity, solid organic matters
(hard resin, copper powder) removal of impurity is up to more than 95%；Centrifuge and sedimentation separation combines, realize separation and purification, aoxidize
Up to more than 95%, gained diamond dust particle purity is high, can repeatedly utilize, can for aluminium and bentonite removal of impurity
Effectively reduce the cost of sapphire grinding process technique.
Preferably, the sapphire is ground into slug centrifugation de-oiling, centrifuged using tripod pendulum type batch centrifugal or Large Copacity tubular type
The grinding waste material centrifugation de-oiling of collection is obtained centrifuging bed material by machine etc.；Contain diamond, copper powder, phenolic aldehyde in gained centrifugation bed material
Resin, aluminum oxide, organic matter solvent etc..
Centrifugation de-oiling can grind waste material to the sapphire and carry out preliminary de-oiling, be easy to subsequent technique further to remove it
His impurity.
Preferably, the solvent includes petroleum ether or n-hexane.
It is further preferred that the boiling range of the petroleum ether is 60-90 DEG C.
It is further preferred that the amount ratio of centrifugation bed material and petroleum ether or n-hexane is 1kg：2-5L, preferably 1kg：3-
5L, more preferably 1kg：4L；It is dispersed with stirring uniformly, then carries out eccentric cleaning.
Using the petroleum ether of specific dosage, can fully dispersed gained centrifugation bed material, dissolve grease impurities, it is clear by centrifuging
Mode is washed, is easy to remove residual grease impurities.
Preferably, by gained centrifuge bed material dries pulverizing after again with sulfuric acid and perchloric acid impurity removal reaction.
Preferably, gained is centrifuged into bed material with during sulfuric acid and perchloric acid impurity removal reaction, gained centrifugation bed material is added
In reactor, the concentrated sulfuric acid is then added, the mass ratio for centrifuging bed material and the concentrated sulfuric acid is 0.8-2:30, preferably 1.2-1.6:30,
More preferably 1.4:30.
It is further preferred that perchloric acid is added dropwise during the course of the reaction, the mass ratio for centrifuging bed material and perchloric acid is 1-1.6:
3, preferably 1.2-1.4:3, more preferably 1.3:3.
Preferably, the mass fraction of the concentrated sulfuric acid is 95%-98%；The mass fraction of the perchloric acid is 70%-
75%.
It is further preferred that it is 180-240 by the reaction temperature of gained centrifugation bed material and sulfuric acid and perchloric acid impurity removal reaction
DEG C, reaction time 2-8h；Preferably, reaction temperature is 200-220 DEG C, reaction time 4-6h；It is further preferred that reaction
Temperature is 208-212 DEG C, reaction time 5h.
Will centrifugation bed material at a certain temperature, reacted with the sulfuric acid and perchloric acid of specific dosage, can effectively remove copper powder,
The impurity such as phenolic resin, organic solvent, it is easy to subsequent technique to carry out, improves the purity of gained diamond dust particle.
Preferably, into reacted material obtained by step (3), addition water carries out gravitational settling cleaning, until cleaning to slurry
The pH value of material is 6-7.
It is further preferred that the drying materials water removal after gained is cleaned, obtains dried material, wherein mainly containing Buddha's warrior attendant
Stone, aluminum oxide and large granular impurity.
Preferably, water is added into the material after cleaning, the mass ratio of material and water is 1:5-20, preferably 1:5-15,
More preferably 1:10；It is dispersed with stirring uniformly, obtains the suspension of diamond and aluminum oxide.
Preferably, the material carries out mass ratio calculating with its dry powder weight.
Preferably, finely dispersed suspension is collected, is centrifuged in centrifuge, isolates the fine grained diamond in material
And aluminum oxide.
Preferably, gained is centrifuged into bed material to react with sodium silicate aqueous solution, natural subsidence separation, isolated in centrifugation bed material
Non-diamond granule foreign.
Sodium metasilicate can be reacted with remaining alumina impurities, and reaction product can be by natural subsidence, with precipitation form
Remove.
Preferably, the mass fraction of the sodium silicate aqueous solution is 0.01%-0.1%, preferably 0.03%-0.07%,
More preferably 0.05%.
Preferably, centrifuge bed material described in each step of the present invention and mass ratio calculating is carried out with its dry powder weight.
Obtained gold is reclaimed using the above-mentioned method that recovery diamond in slug is ground from sapphire using above-mentioned
Hard rock powder particle.
Gained diamond dust particle purity is high, can repeatedly utilize, can effectively reduce sapphire attrition process
The cost of technique.
Compared with prior art, beneficial effects of the present invention are：
The inventive method, using special process, it can be ground from sapphire in slug and reclaim diamond, not damage Buddha's warrior attendant
The performance of stone itself, reuses diamond, reduces the discharge capacity of harmful waste；Centrifugally operated successively is used, can be made solid
Liquid separation is thorough, and fluid organic material clearance is up to more than 80%；Reacted using sulfuric acid and perchloric acid with impurity, solid organic matters
(hard resin, copper powder) removal of impurity is up to more than 95%；Centrifuge and sedimentation separation combines, realize separation and purification, aoxidize
Up to more than 95%, gained diamond dust particle purity is high, can repeatedly utilize, can for aluminium and bentonite removal of impurity
Effectively reduce the cost of sapphire grinding process technique.
Embodiment
Technical scheme is clearly and completely described below in conjunction with embodiment, but ability
Field technique personnel will be understood that following described embodiment is part of the embodiment of the present invention, rather than whole embodiments,
The present invention is merely to illustrate, and is not construed as limiting the scope of the present invention.Based on the embodiment in the present invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.Unreceipted actual conditions person in embodiment, the condition suggested according to normal condition or manufacturer are carried out.Agents useful for same or instrument
Unreceipted production firm person, it is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
It is a kind of that the method that diamond is reclaimed in slug is ground from sapphire, comprise the following steps：
(1) using tripod pendulum type batch centrifugal by the grinding waste material centrifugation de-oiling of collection, obtain centrifuging bed material；Contain in centrifugation bed material
Diamond, copper powder, phenolic resin, aluminum oxide, organic matter solvent etc.；
(2) petroleum ether is added into the centrifugation bed material obtained by step 1 to be disperseed, centrifuge the amount ratio of bed material and petroleum ether
For 1kg：2L, the boiling range of petroleum ether is 60-90 DEG C；It is dispersed with stirring uniformly；
(3) slurry after being uniformly dispersed carries out eccentric cleaning using centrifuge, pours out the supernatant after centrifugation, is centrifuged
Bed material；Diamond, copper powder, phenolic resin, aluminum oxide etc. are mainly contained in gained centrifugation bed material；This step can isolate centrifugation
The most organic solvent remained in bed material；
(4) the centrifugation bed material after step (3) eccentric cleaning is dried, then crushed；
(5) the centrifugation bed material that step (4) crushes is put into quartz reaction kettle, add the concentrated sulfuric acid, centrifugation bed material with
The mass ratio of the concentrated sulfuric acid is 2:30, reaction temperature is 180-184 DEG C, reaction time 8h；Perchloric acid is added dropwise during the course of the reaction,
The mass ratio for centrifuging bed material and perchloric acid is 1.6:3；This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(6) pure water is added into step (5) reacted material and carries out gravitational settling cleaning, until cleaning to slurry
PH value is 6-7；
(7) the cleaned material of step (6) is dried into water removal again, obtains dried material；Wherein mainly contain diamond,
Aluminum oxide and large granular impurity；
(8) pure water is added in the dried material obtained to step (7), the mass ratio of material and pure water is 1:5, then
It is dispersed with stirring uniformly, obtains the suspension of diamond and aluminum oxide；
(9) finely dispersed suspension is taken to be centrifuged in centrifuge, to isolate fine grained diamond and the oxygen in material
Change aluminium；Gained centrifugation bed material is imported into glass beaker again, is added the sodium silicate solution that enough mass fractions are 0.01%, is carried out
Natural subsidence separates, to be separated off out the non-diamond granule foreign in centrifugation bed material；
(10) centrifugation bed material is collected by centrifugation in resulting solution again, and adds pure water and cleaned, and then drying goes to remove water
Point, you can obtain the diamond dust particle that can be reused.
Embodiment 2
It is a kind of that the method that diamond is reclaimed in slug is ground from sapphire, comprise the following steps：
(1) using tripod pendulum type batch centrifugal by the grinding waste material centrifugation de-oiling of collection, obtain centrifuging bed material；Contain in centrifugation bed material
Diamond, copper powder, phenolic resin, aluminum oxide, organic matter solvent etc.；
(2) n-hexane is added into the centrifugation bed material obtained by step 1 to be disperseed, centrifuge the amount ratio of bed material and n-hexane
For 1kg：5L；It is dispersed with stirring uniformly；
(3) slurry after being uniformly dispersed carries out eccentric cleaning using centrifuge, pours out the supernatant after centrifugation, is centrifuged
Bed material；Diamond, copper powder, phenolic resin, aluminum oxide etc. are mainly contained in gained centrifugation bed material；This step can isolate centrifugation
The most organic solvent remained in bed material；
(4) the centrifugation bed material after step (3) eccentric cleaning is dried, then crushed；
(5) the centrifugation bed material that step (4) crushes is put into quartz reaction kettle, add the concentrated sulfuric acid, centrifugation bed material with
The mass ratio of the concentrated sulfuric acid is 0.8:30；Reaction temperature is 236-240 DEG C, reaction time 2h；High chlorine is added dropwise during the course of the reaction
Acid, the mass ratio for centrifuging bed material and perchloric acid is 1:3；This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(6) pure water is added into step (5) reacted material and carries out gravitational settling cleaning, until cleaning to slurry
PH value is 6-7；
(7) the cleaned material of step (6) is dried into water removal again, obtains dried material；Wherein mainly contain diamond,
Aluminum oxide and large granular impurity；
(8) pure water is added in the dried material obtained to step (7), the mass ratio of material and pure water is 1:20, so
After be dispersed with stirring uniformly, obtain the suspension of diamond and aluminum oxide；
(9) finely dispersed suspension is taken to be centrifuged in centrifuge, to isolate fine grained diamond and the oxygen in material
Change aluminium；Gained centrifugation bed material is imported into glass beaker again, is added the sodium silicate solution that enough mass fractions are 0.1%, is carried out
Natural subsidence separates, to be separated off out the non-diamond granule foreign in centrifugation bed material；
(10) centrifugation bed material is collected by centrifugation in resulting solution again, and adds pure water and cleaned, and then drying goes to remove water
Point, you can obtain the diamond dust particle that can be reused.
Embodiment 3
It is a kind of that the method that diamond is reclaimed in slug is ground from sapphire, comprise the following steps：
(1) using tripod pendulum type batch centrifugal by the grinding waste material centrifugation de-oiling of collection, obtain centrifuging bed material；Contain in centrifugation bed material
Diamond, copper powder, phenolic resin, aluminum oxide, organic matter solvent etc.；
(2) petroleum ether is added into the centrifugation bed material obtained by step 1 to be disperseed, centrifuge the amount ratio of bed material and petroleum ether
For 1kg：3L, the boiling range of petroleum ether is 60-90 DEG C；It is dispersed with stirring uniformly；
(3) slurry after being uniformly dispersed carries out eccentric cleaning using centrifuge, pours out the supernatant after centrifugation, is centrifuged
Bed material；Diamond, copper powder, phenolic resin, aluminum oxide etc. are mainly contained in gained centrifugation bed material；This step can isolate centrifugation
The most organic solvent remained in bed material；
(4) the centrifugation bed material after step (3) eccentric cleaning is dried, then crushed；
(5) the centrifugation bed material that step (4) crushes is put into quartz reaction kettle, add the concentrated sulfuric acid, centrifugation bed material with
The mass ratio of the concentrated sulfuric acid is 1.6:30；Reaction temperature is 198-202 DEG C, reaction time 6h；High chlorine is added dropwise during the course of the reaction
Acid, the mass ratio for centrifuging bed material and perchloric acid is 1.4:3；This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(6) pure water is added into step (5) reacted material and carries out gravitational settling cleaning, until cleaning to slurry
PH value is 6-7；
(7) the cleaned material of step (6) is dried into water removal again, obtains dried material；Wherein mainly contain diamond,
Aluminum oxide and large granular impurity；
(8) pure water is added in the dried material obtained to step (7), the mass ratio of material and pure water is 1:5, then
It is dispersed with stirring uniformly, obtains the suspension of diamond and aluminum oxide；
(9) finely dispersed suspension is taken to be centrifuged in centrifuge, to isolate fine grained diamond and the oxygen in material
Change aluminium；Gained centrifugation bed material is imported into glass beaker again, is added the sodium silicate solution that enough mass fractions are 0.03%, is carried out
Natural subsidence separates, to be separated off out the non-diamond granule foreign in centrifugation bed material；
(10) centrifugation bed material is collected by centrifugation in resulting solution again, and adds pure water and cleaned, and then drying goes to remove water
Point, you can obtain the diamond dust particle that can be reused.
Embodiment 4
It is a kind of that the method that diamond is reclaimed in slug is ground from sapphire, comprise the following steps：
(1) using tripod pendulum type batch centrifugal by the grinding waste material centrifugation de-oiling of collection, obtain centrifuging bed material；Contain in centrifugation bed material
Diamond, copper powder, phenolic resin, aluminum oxide, organic matter solvent etc.；
(2) n-hexane is added into the centrifugation bed material obtained by step 1 to be disperseed, centrifuge the amount ratio of bed material and n-hexane
For 1kg：5L；It is dispersed with stirring uniformly；
(3) slurry after being uniformly dispersed carries out eccentric cleaning using centrifuge, pours out the supernatant after centrifugation, is centrifuged
Bed material；Diamond, copper powder, phenolic resin, aluminum oxide etc. are mainly contained in gained centrifugation bed material；This step can isolate centrifugation
The most organic solvent remained in bed material；
(4) the centrifugation bed material after step (3) eccentric cleaning is dried, then crushed；
(5) the centrifugation bed material that step (4) crushes is put into quartz reaction kettle, add the concentrated sulfuric acid, centrifugation bed material with
The mass ratio of the concentrated sulfuric acid is 1.2:30, more preferably 1.4:30；Reaction temperature is 218-222 DEG C, reaction time 4h；
Perchloric acid is added dropwise in course of reaction, the mass ratio for centrifuging bed material and perchloric acid is 1.2:3；This step can remove copper powder, phenolic aldehyde tree
The impurity such as fat, organic solvent；
(6) pure water is added into step (5) reacted material and carries out gravitational settling cleaning, until cleaning to slurry
PH value is 6-7；
(7) the cleaned material of step (6) is dried into water removal again, obtains dried material；Wherein mainly contain diamond,
Aluminum oxide and large granular impurity；
(8) pure water is added in the dried material obtained to step (7), the mass ratio of material and pure water is 1:15, so
After be dispersed with stirring uniformly, obtain the suspension of diamond and aluminum oxide；
(9) finely dispersed suspension is taken to be centrifuged in centrifuge, to isolate fine grained diamond and the oxygen in material
Change aluminium；Gained centrifugation bed material is imported into glass beaker again, is added the sodium silicate solution that enough mass fractions are 0.07%, is carried out
Natural subsidence separates, to be separated off out the non-diamond granule foreign in centrifugation bed material；
(10) centrifugation bed material is collected by centrifugation in resulting solution again, and adds pure water and cleaned, and then drying goes to remove water
Point, you can obtain the diamond dust particle that can be reused.
Embodiment 5
It is a kind of that the method that diamond is reclaimed in slug is ground from sapphire, comprise the following steps：
(1) using tripod pendulum type batch centrifugal by the grinding waste material centrifugation de-oiling of collection, obtain centrifuging bed material；Contain in centrifugation bed material
Diamond, copper powder, phenolic resin, aluminum oxide, organic matter solvent etc.；
(2) petroleum ether is added into the centrifugation bed material obtained by step 1 to be disperseed, centrifuge the amount ratio of bed material and petroleum ether
For 1kg：4L, the boiling range of petroleum ether is 60-90 DEG C；It is dispersed with stirring uniformly；
(3) slurry after being uniformly dispersed carries out eccentric cleaning using centrifuge, pours out the supernatant after centrifugation, is centrifuged
Bed material；Diamond, copper powder, phenolic resin, aluminum oxide etc. are mainly contained in gained centrifugation bed material；This step can isolate centrifugation
The most organic solvent remained in bed material；
(4) the centrifugation bed material after step (3) eccentric cleaning is dried, then crushed；
(5) the centrifugation bed material that step (4) crushes is put into quartz reaction kettle, add the concentrated sulfuric acid, centrifugation bed material with
The mass ratio of the concentrated sulfuric acid is 1.4:30；Reaction temperature is 208-212 DEG C, reaction time 5h；High chlorine is added dropwise during the course of the reaction
Acid, the mass ratio for centrifuging bed material and perchloric acid is 1.3:3；This step can remove the impurity such as copper powder, phenolic resin, organic solvent；
(6) pure water is added into step (5) reacted material and carries out gravitational settling cleaning, until cleaning to slurry
PH value is 6-7；
(7) the cleaned material of step (6) is dried into water removal again, obtains dried material；Wherein mainly contain diamond,
Aluminum oxide and large granular impurity；
(8) pure water is added in the dried material obtained to step (7), the mass ratio of material and pure water is 1:10, so
After be dispersed with stirring uniformly, obtain the suspension of diamond and aluminum oxide；
(9) finely dispersed suspension is taken to be centrifuged in centrifuge, to isolate fine grained diamond and the oxygen in material
Change aluminium；Gained centrifugation bed material is imported into glass beaker again, is added the sodium silicate solution that enough mass fractions are 0.05%, is carried out
Natural subsidence separates, to be separated off out the non-diamond granule foreign in centrifugation bed material；
(10) centrifugation bed material is collected by centrifugation in resulting solution again, and adds pure water and cleaned, and then drying goes to remove water
Point, you can obtain the diamond dust particle that can be reused.
Diamond dust particulate component (mass fraction) obtained by 1-5 of embodiment of the present invention methods is detected, as a result such as
Under：
The present invention of table 1 grinds the diamond components testing result reclaimed in slug from sapphire
It can be seen from Table 1 that the present invention grinds the method that diamond is reclaimed in slug from sapphire, can effectively go
Except the impurity such as the copper powder in sapphire grinding slug, phenolic resin, aluminum oxide, bentonite, organic matter solvent, gained diamond
Powder particle purity is high, can repeatedly utilize, can effectively reduce the cost of sapphire grinding process technique.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that various embodiments above is only used
To illustrate technical scheme, rather than its limitations；It will be understood by those within the art that：Without departing substantially from this hair
In the case of bright spirit and scope, the technical scheme described in foregoing embodiments can be modified, or to wherein
Some or all of technical characteristic carries out equivalent substitution；And these are changed or are replaced, the essence of appropriate technical solution is not made
Depart from the scope of various embodiments of the present invention technical scheme；It is, therefore, intended that include belonging to the present invention in the following claims
In the range of all these substitutions and modifications.
Claims (21)
1. a kind of grind the method that diamond is reclaimed in slug from sapphire, it is characterised in that comprises the following steps：
(1) sapphire is ground into slug centrifugation de-oiling；
(2) gained centrifugation bed material is disperseed with solvent, eccentric cleaning；
(3) gained is centrifuged into bed material and sulfuric acid and perchloric acid impurity removal reaction；
(4) it is 6-7 to clean resulting material gravitational settling to pH, adds water to be dispersed with stirring uniformly, gained suspension is centrifuged；
(5) gained being centrifuged into bed material to react with sodium silicate solution, centrifugation bed material is collected by centrifugation in natural subsidence, resulting solution again,
The cleaning of gained centrifugation bed material, drying, obtain diamond dust particle.
A kind of 2. method that recovery diamond in slug is ground from sapphire according to claim 1, it is characterised in that
The solvent includes petroleum ether or n-hexane.
A kind of 3. method that recovery diamond in slug is ground from sapphire according to claim 2, it is characterised in that
The amount ratio for centrifuging bed material and petroleum ether or n-hexane is 1kg：2-5L.
A kind of 4. method that recovery diamond in slug is ground from sapphire according to claim 3, it is characterised in that
The amount ratio for centrifuging bed material and petroleum ether or n-hexane is 1kg：3-5L.
A kind of 5. method that recovery diamond in slug is ground from sapphire according to claim 4, it is characterised in that
The amount ratio for centrifuging bed material and petroleum ether or n-hexane is 1kg：4L.
A kind of 6. method that recovery diamond in slug is ground from sapphire according to claim 1, it is characterised in that
By gained centrifuge bed material dries pulverizing after again with sulfuric acid and perchloric acid impurity removal reaction.
A kind of 7. method that recovery diamond in slug is ground from sapphire according to claim 1, it is characterised in that
By gained centrifugation bed material with during sulfuric acid and perchloric acid impurity removal reaction, gained centrifugation bed material being added in reactor, Ran Houjia
Enter the concentrated sulfuric acid, the mass ratio for centrifuging bed material and the concentrated sulfuric acid is 0.8-2:30.
A kind of 8. method that recovery diamond in slug is ground from sapphire according to claim 7, it is characterised in that
The mass ratio of the centrifugation bed material and the concentrated sulfuric acid is 1.2-1.6:30.
A kind of 9. method that recovery diamond in slug is ground from sapphire according to claim 8, it is characterised in that
The mass ratio of the centrifugation bed material and the concentrated sulfuric acid is 1.4:30.
10. a kind of method that recovery diamond in slug is ground from sapphire according to claim 7, its feature exist
In being added dropwise perchloric acid during the course of the reaction, the mass ratio for centrifuging bed material and perchloric acid is 1-1.6:3.
11. a kind of method that recovery diamond in slug is ground from sapphire according to claim 10, its feature exist
In the mass ratio of the centrifugation bed material and perchloric acid is 1.2-1.4:3.
12. a kind of method that recovery diamond in slug is ground from sapphire according to claim 11, its feature exist
In the mass ratio of the centrifugation bed material and perchloric acid is 1.3:3.
13. a kind of method that recovery diamond in slug is ground from sapphire according to claim 1, its feature exist
In it is 180-240 DEG C that gained is centrifuged into bed material with the reaction temperature of sulfuric acid and perchloric acid impurity removal reaction, reaction time 2-8h.
14. a kind of method that recovery diamond in slug is ground from sapphire according to claim 13, its feature exist
In it is 200-220 DEG C that gained is centrifuged into bed material with the reaction temperature of sulfuric acid and perchloric acid impurity removal reaction, reaction time 4-6h.
15. a kind of method that recovery diamond in slug is ground from sapphire according to claim 14, its feature exist
In it is 208-212 DEG C that gained is centrifuged into bed material with the reaction temperature of sulfuric acid and perchloric acid impurity removal reaction, reaction time 5h.
16. a kind of method that recovery diamond in slug is ground from sapphire according to claim 1, its feature exist
In it is 6-7 to clean resulting material gravitational settling to pH, adds water to be dispersed with stirring uniformly, and the mass ratio of material and water is 1:5-20；
It is dispersed with stirring uniformly, obtains the suspension of diamond and aluminum oxide.
17. a kind of method that recovery diamond in slug is ground from sapphire according to claim 16, its feature exist
In the mass ratio of the material and water is 1:5-15.
18. a kind of method that recovery diamond in slug is ground from sapphire according to claim 17, its feature exist
In the mass ratio of the material and water is 1:10.
19. a kind of method that recovery diamond in slug is ground from sapphire according to claim 1, its feature exist
In the mass fraction of the sodium silicate aqueous solution is 0.01%-0.1%.
20. a kind of method that recovery diamond in slug is ground from sapphire according to claim 19, its feature exist
In the mass fraction of the sodium silicate aqueous solution is 0.03%-0.07%.
21. a kind of method that recovery diamond in slug is ground from sapphire according to claim 20, its feature exist
In the mass fraction of the sodium silicate aqueous solution is 0.05%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610621402.2A CN106241794B (en) | 2016-08-01 | 2016-08-01 | It is a kind of that the method and product that diamond is reclaimed in slug are ground from sapphire |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610621402.2A CN106241794B (en) | 2016-08-01 | 2016-08-01 | It is a kind of that the method and product that diamond is reclaimed in slug are ground from sapphire |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106241794A CN106241794A (en) | 2016-12-21 |
| CN106241794B true CN106241794B (en) | 2018-02-02 |
Family
ID=57605798
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610621402.2A Active CN106241794B (en) | 2016-08-01 | 2016-08-01 | It is a kind of that the method and product that diamond is reclaimed in slug are ground from sapphire |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106241794B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106829953B (en) * | 2017-02-14 | 2019-02-22 | 北京国瑞升科技股份有限公司 | A kind of method and product that diamond is recycled and recycled |
| 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 |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229113B (en) * | 2011-06-07 | 2013-08-28 | 王楚雯 | Method for recovering sapphire powder |
| CN103350996B (en) * | 2013-06-29 | 2015-07-29 | 开封恒锐新金刚石制品有限公司 | Adamantine method is reclaimed from liquid resin |
| CN103495505B (en) * | 2013-10-10 | 2015-05-27 | 安化县众旺钨业有限公司 | Floatation method of diamonds and application to separation and purification of artificial diamonds from grinding waste materials thereof |
-
2016
- 2016-08-01 CN CN201610621402.2A patent/CN106241794B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN106241794A (en) | 2016-12-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106006629B (en) | A kind of sapphire method and product that diamond is reclaimed in grinding slug | |
| US20130236387A1 (en) | Methods and Apparatus for Recovery of Silicon and Silicon Carbide from Spent Wafer-Sawing Slurry | |
| US20040144722A1 (en) | Method for treating an exhausted glycol-based slurry | |
| CN106241794B (en) | It is a kind of that the method and product that diamond is reclaimed in slug are ground from sapphire | |
| JP4980793B2 (en) | Silicon recovery method and silicon recovery apparatus | |
| KR101179521B1 (en) | The method and device for the recycling of waste silicon wafer sludge | |
| CN102167956A (en) | Method for recycling and reutilizing rare-earth polishing powder waste residue and waste liquor | |
| JP4520331B2 (en) | Method for producing hydrogen gas | |
| JP2007246367A (en) | Method for recovering silicon-containing material | |
| JP4966938B2 (en) | Silicon regeneration method | |
| KR101355816B1 (en) | Method for separation and recovery of silicon from silicon sludge | |
| JP4160930B2 (en) | Halosilane production method, solid content purification method | |
| JP2011218503A (en) | Method for disposing silicon-containing waste liquid | |
| KR20080036816A (en) | Reproduction method of spent abrasives for polishing a glass panel for display | |
| CN106829953B (en) | A kind of method and product that diamond is recycled and recycled | |
| EP3060521B1 (en) | Non-chemical method for recovering silicon carbide particles | |
| CN106583031A (en) | Process for purifying ganister sand from silicon carbide reclamation sand | |
| JP2007246366A (en) | Method for recovering silicon-containing material | |
| JP2002028866A (en) | Recovering method for abrasive grain and grinding slurry | |
| KR20130033290A (en) | Method for recovering a solid particle | |
| JP4414364B2 (en) | Method for recovering silicon-containing material | |
| CN104120026A (en) | Method for comprehensively recycling SiC cutting fluid waste mortar | |
| TWM469311U (en) | Silicon carbide recycling system | |
| CN104711107A (en) | Silicon waste slurry recovery system, coolant recovery solution, recovered abrasive grains and recovered cutting powder | |
| JP2005007541A (en) | Reusing system of slurry waste liquid for slicing hard/brittle material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210204 Address after: 124000 22, area a, incubation base of Fine Chemical Industrial Park, Shuangtaizi District, Panjin City, Liaoning Province Patentee after: Panjin Guoruisheng Technology Co.,Ltd. Address before: 102500 room 218, block C, no.6, Dongyi lane, yanshangang South Road, Fangshan District, Beijing Patentee before: BEIJING POLYSTAR HITECH Co.,Ltd. |