CN106829953B - A kind of method and product that diamond is recycled and recycled - Google Patents
A kind of method and product that diamond is recycled and recycled Download PDFInfo
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- CN106829953B CN106829953B CN201710078290.5A CN201710078290A CN106829953B CN 106829953 B CN106829953 B CN 106829953B CN 201710078290 A CN201710078290 A CN 201710078290A CN 106829953 B CN106829953 B CN 106829953B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
Abstract
The present invention provides a kind of from the sapphire method and product for recycling diamond in grinding slug.The method of the present invention process is simple, it can be ground in slug from sapphire and recycle diamond, the performance of diamond itself is not damaged, reuse diamond, efficiency is significantly promoted, and reduces generated dangerous waste when saponification step and petroleum ether cleaning, and do not increase additional dangerous waste product, it is more environmentally friendly, prevent the material flammability issues in drying link.Diamond dust particle purity of the present invention is high, can be repeated as many times and utilize, can be effectively reduced the cost of sapphire grinding process technique.
Description
Technical field
The present invention relates to technical field of mineral processing, a kind of method for recycling and recycling in particular to diamond
And product.
Background technique
Sapphire (Sapphire), mineral name corundum, trigonal system crystalline solid.Sapphire in industry is aluminium oxide
A kind of monocrystalline (α-Al2O3), Mohs' hardness reaches 9.0, is only second to diamond.And the special lattice structure of sapphire is also determined
It has been determined with excellent physical property and chemical stability, for example, fabulous thermal conductance, splendid electric insulating quality and light transmission
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 since the sapphire face C and GaN single crystal film lattice constant mismatch rate are small, meet simultaneously
Requirement resistant to high temperature in GaN single crystal film growth course, so, sapphire is again by as GaN/Al2O3Light emitting diode (LED) is most
For ideal substrate material, it is widely used in LED industry.In recent years, popularizing with smart phone, sapphire relies on again
Intensity, wearability and the resistance to marring of its superelevation have gradually been applied to mobile phone screen, Touch control key, rear cover cover glass and have taken the photograph
As head diaphragm etc..Above various application fields, 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
Thin slice with a thickness of 800 μm or so is cut into using the methods of diamond wire saw, then passes through grinding process and buffer again
Sequence is processed into the thin slice with a thickness of 600 μm or so.And it is the most key in sapphire process for grinding 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 with polycrystalline diamond (PCD) for abrasive material, then by itself and aqueous solvent (predominantly ethylene glycol) or oiliness
Solvent (predominantly white oil) is mixed in a certain ratio, and dispersing agent appropriate is added and is configured to certain density suspension, is passed through
The mechanical grinding effect of polycrystalline diamond reaches grinding and effect is thinned.Currently, PCD micro mist master used in sapphire process
There are several granularities such as 5-9 (D50=6.5 ± 0.3 μm), 4-8 (D50=5.6 ± 0.2 μm), 3-6 (D50=4.2 ± 0.2 μm)
Specification.During the grinding process, the particle of polycrystalline diamond can be tapered, and granularity can also gradually become smaller, these diamond particles
The formation of the liquid substances such as clast and abrasive solvents, auxiliary agent, cleaning agent is ground with copper powder, the aluminium oxide etc. generated in process of lapping to grind
Grind waste slurry.And for this partial mill waste slurry, the main methods of sapphire processing enterprise are exactly according to laws and regulations
Walk hazardous waste disposal program.Under current economic continuous downlink, the background that environmental protection pressure continues to increase, at this dangerous waste
Reason spending is undoubtedly a no small burden for enterprise, and also results in greatly digestion pressure to environment.If energy
It invents a kind of method the polycrystalline diamond micro mist in grinding waste slurry material recycle and repeats to recycle, can will not only save
The production cost of enterprise, can also greatly facilitate resource recycle and environmental protection.
The prior art can only pass through the complicated preceding road of technique recovery section sapphire in the subsequent processing of grinding waste slurry material
It is worth lower boron carbide particles in processing, and can not be recycled for being worth higher diamond particles substantially in the processing of rear road,
It can only be wasted in subsequent offal treatment process.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of method for recycling diamond from sapphire grinding slug, described
Slave sapphire grinding slug in recycle diamond method and process it is simple, can effectively from sapphire grinding waste material in recycle
The diamond dust particle of high-purity, the powder particle can be repeated as many times and utilize, and can be effectively reduced sapphire grinding and add
The cost of work technique.
The second object of the present invention, which is to provide, a kind of recycles diamond from sapphire grinding slug using above-mentioned
The diamond dust particle that recycles of method, the diamond dust particle purity is high, can be repeated as many times and utilize, energy
The cost of sapphire grinding process technique is enough effectively reduced.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A method of diamond being recycled from sapphire in grinding slug, is included the following steps:
(1) by sapphire grinding slug centrifugation de-oiling;
(2) gained centrifugation bottom material is subjected to vacuum drying processing;
(3) by gained material drying and sulfuric acid and perchloric acid impurity removal reaction;
(4) cleaning resulting material gravitational settling to pH is 6-7;
(5) resulting material is subjected to alkali process;
(6) cleaning resulting material gravitational settling to pH is 6-7, adds water and stirs and is uniformly dispersed, gained suspension is centrifuged;
(7) gained centrifugation bottom material is reacted with sodium silicate solution, natural subsidence obtains diamond dust particle.
The present invention is from the sapphire method for recycling diamond in grinding slug, and using special process, process is simple, energy
It is enough to recycle diamond from sapphire grinding slug, the performance of diamond itself is not damaged, reuses diamond, efficiency
It is significantly promoted, reduces generated dangerous waste when saponification step and petroleum ether cleaning, and do not increase additional dangerous waste product, more ring
It protects, has prevented the material flammability issues in drying link.Vacuum drying processing, liquid are carried out to centrifugation bottom material using vacuum oven
Body organic removal rate is up to 95% or more;It is reacted using sulfuric acid and perchloric acid with impurity, solid organic matters (hard resin, copper powder)
For removal of impurity up to 95% or more, purification process has more controllability, and material overflows the risk of reaction kettle when reducing purification, reduces
Sulfuric acid dosage;Centrifuge separation and sedimentation separation combine, and realize separation and purification, aluminium oxide and bentonite removal of impurity up to 95%
More than, gained diamond dust particle purity is high, can be repeated as many times and utilize, can be effectively reduced sapphire grinding process technique
Cost.
Preferably, the drying temperature of the vacuum drying processing is 100-500 DEG C, preferably 200-300 DEG C, further excellent
It is selected as 240 DEG C.
Preferably, the vacuum degree of the vacuum drying is -0.005MPa hereinafter, preferably -0.08MPa is hereinafter, further
Preferably -0.1MPa or less.
Preferably, the drying time of the vacuum drying is 2-8h, preferably 2-4h, further preferably 2h.
Preferably, by gained centrifugation bottom material crush after again with sulfuric acid and perchloric acid impurity removal reaction.
Preferably, the concentration of the sulfuric acid be 75wt% or more, preferably 75wt%-90wt%, further preferably
80wt%.
Preferably, by during gained material drying and sulfuric acid and perchloric acid impurity removal reaction, gained material drying is added
In reactor, the concentrated sulfuric acid is then added, the mass ratio for being centrifuged bottom material and sulfuric acid is 1-2:30, preferably 1.2-1.8:30, into one
Step is preferably 1.5:30.
Preferably, it is added dropwise perchloric acid during the reaction, the mass ratio of material drying and perchloric acid is 0.5-1:1, preferably
For 0.6-0.8:1, further preferably 0.7:1.
It preferably, is 150-280 DEG C by the reaction temperature of gained material drying and sulfuric acid and perchloric acid impurity removal reaction, preferably
It is 180-240 DEG C, further preferably 210 DEG C.
It preferably, is 3-6h, preferably 4- by the reaction time of gained material drying and sulfuric acid and perchloric acid impurity removal reaction
6h, further preferably 5h.
Preferably, it includes one of inorganic base and organic base or more for resulting material being carried out alkali used in alkali process
Kind, preferably one of inorganic base or a variety of, further preferably one of sodium hydroxide and potassium hydroxide or a variety of.
It preferably, include heating after mixing material with water and alkali by resulting material progress alkali process.
It is further preferred that resulting material is carried out in alkali process, the mass ratio of material and water is 1-2:15, preferably 1-
1.5:15 preferably 1:15.
It is further preferred that resulting material is carried out in alkali process, the mass ratio of material and alkali is 0.5-2:1, preferably
0.8-1.2:1, further preferably 1:1.
It is further preferred that by resulting material carry out alkali process in, temperature be 40 DEG C or more, preferably 40-80 DEG C, into one
Preferably 60 DEG C of step.
It is further preferred that by resulting material carry out alkali process in, the time be 20min or more, preferably 20-60min, into
One step is preferably 30min.
Preferably, resulting material gravitational settling is cleaned to pH is 6-7, adds water and stirs and is uniformly dispersed, by gained suspension
In centrifugation, the mass ratio of material and water is 1:5-20, preferably 1:5-15, further preferably 1:10.
Preferably, resulting material gravitational settling is cleaned to pH is 6-7, adds water and stirs and is uniformly dispersed, by gained suspension
In centrifugation, centrifugal rotational speed is 300r/min or more, preferably 300-500r/min, further preferably 400r/min.
Preferably, resulting material gravitational settling is cleaned to pH is 6-7, adds water and stirs and is uniformly dispersed, by gained suspension
In centrifugation, centrifugation time is 4min or more, preferably 4-7min, further preferably 5min.
Preferably, gained centrifugation bottom material is reacted with sodium silicate solution, in natural subsidence, the concentration of sodium silicate solution is
0.01wt%-0.1wt%, preferably 0.03wt%-0.07wt%, further preferably 0.05wt%.
Preferably, gained centrifugation bottom material to be reacted with sodium silicate solution, in natural subsidence, the sedimentation time is 0.5h or more,
Preferably 0.5-1h, further preferably 1h.
Preferably, gained centrifugation bottom material is reacted with sodium silicate solution, in natural subsidence, is repeatedly settled as needed
Classification.
Using a kind of above-mentioned diamond recycled from sapphire with the method for diamond is recycled in grinding slug
Powder particle.
Diamond dust particle purity of the present invention is high, can be repeated as many times and utilize, and can be effectively reduced sapphire grinding and adds
The cost of work technique.
Compared with prior art, the invention has the benefit that
The present invention is from the sapphire method for recycling diamond in grinding slug, and using special process, process is simple, energy
It is enough to recycle diamond from sapphire grinding slug, the performance of diamond itself is not damaged, reuses diamond, efficiency
It is significantly promoted, reduces generated dangerous waste when saponification step and petroleum ether cleaning, and do not increase additional dangerous waste product, more ring
It protects.Vacuum drying processing is carried out to centrifugation bottom material in the method for the present invention second step, so that organic matter is handled completely completely, prevents
It is safer in the material flammability issues of drying link;Vacuum drying processing, liquid are carried out to centrifugation bottom material using vacuum oven
Body organic removal rate is up to 99% or more;It is reacted using sulfuric acid and perchloric acid with impurity, solid organic matters (hard resin, copper powder)
For removal of impurity up to 95% or more, purification process has more controllability, and material overflows the risk of reaction kettle when reducing purification, reduces
Sulfuric acid dosage;Centrifuge separation and sedimentation separation combine, and realize separation and purification, aluminium oxide and bentonite removal of impurity up to 95%
More than, gained diamond dust particle purity is high, can be repeated as many times and utilize, can be effectively reduced sapphire grinding process technique
Cost.Gained diamond dust particle purity is high, can be repeated as many times and utilize, can be effectively reduced sapphire attrition process work
The cost of skill.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with specific embodiment, but ability
Field technique personnel will be understood that following described embodiments are some of the embodiments of the present invention, instead of all the embodiments,
It is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same or instrument
Production firm person is not specified, is the conventional products that can be obtained by commercially available purchase.
The present invention provides a kind of from the sapphire method for recycling diamond in grinding slug, includes the following steps:
(1) by sapphire grinding slug centrifugation de-oiling;
(2) gained centrifugation bottom material is subjected to vacuum drying processing;
(3) by gained material drying and sulfuric acid and perchloric acid impurity removal reaction;
(4) cleaning resulting material gravitational settling to pH is 6-7;
(5) resulting material is subjected to alkali process;
(6) cleaning resulting material gravitational settling to pH is 6-7, adds water and stirs and is uniformly dispersed, gained suspension is centrifuged;
(7) gained centrifugation bottom material is reacted with sodium silicate solution, natural subsidence obtains diamond dust particle.
The present invention is from the sapphire method for recycling diamond in grinding slug, and using special process, process is simple, energy
It is enough to recycle diamond from sapphire grinding slug, the performance of diamond itself is not damaged, reuses diamond, efficiency
It is significantly promoted, reduces generated dangerous waste when saponification step and petroleum ether cleaning, and do not increase additional dangerous waste product, more ring
It protects, has prevented the material flammability issues in drying link.Vacuum drying processing, liquid are carried out to centrifugation bottom material using vacuum oven
Body organic removal rate is up to 95% or more;It is reacted using sulfuric acid and perchloric acid with impurity, solid organic matters (hard resin, copper powder)
For removal of impurity up to 95% or more, purification process has more controllability, and material overflows the risk of reaction kettle when reducing purification, reduces
Sulfuric acid dosage;Centrifuge separation and sedimentation separation combine, and realize separation and purification, aluminium oxide and bentonite removal of impurity up to 95%
More than, gained diamond dust particle purity is high, can be repeated as many times and utilize, can be effectively reduced sapphire grinding process technique
Cost.
In a kind of preferred embodiment of the present invention, the drying temperature of the vacuum drying processing is 100-500 DEG C,
Preferably 200-300 DEG C, further preferably 240 DEG C.
In a kind of preferred embodiment of the present invention, the vacuum degree of the vacuum drying is -0.005MPa hereinafter, excellent
- 0.08MPa is selected as hereinafter, further preferably -0.1MPa or less.
In a kind of preferred embodiment of the present invention, the drying time of the vacuum drying is 2-8h, preferably 2-
4h, further preferably 2h.
Using specific vacuum drying condition, liquid phase organic matter solvent whole in centrifugation bottom material can be isolated, further
The removal effect of liquid phase organic matter is improved, is carried out convenient for subsequent technique, the purity of gained diamond dust particle is improved.
It is anti-with sulfuric acid and perchloric acid again after gained centrifugation bottom material is crushed in a kind of preferred embodiment of the present invention
It should clean.
In a kind of preferred embodiment of the present invention, the concentration of the sulfuric acid is 75wt% or more, preferably
75wt%-90wt%, further preferably 80wt%.
In a kind of preferred embodiment of the present invention, by gained material drying and sulfuric acid and perchloric acid impurity removal reaction mistake
Gained material drying is added in reactor Cheng Zhong, and the concentrated sulfuric acid is then added, and the mass ratio for being centrifuged bottom material and sulfuric acid is 1-2:
30, preferably 1.2-1.8:30, further preferably 1.5:30.
In a kind of preferred embodiment of the present invention, perchloric acid, material drying and high chlorine are added dropwise during the reaction
The mass ratio of acid is 0.5-1:1, preferably 0.6-0.8:1, further preferably 0.7:1.
In a kind of preferred embodiment of the present invention, by gained material drying and sulfuric acid and perchloric acid impurity removal reaction
Reaction temperature is 150-280 DEG C, preferably 180-240 DEG C, further preferably 210 DEG C.
In a kind of preferred embodiment of the present invention, by gained material drying and sulfuric acid and perchloric acid impurity removal reaction
Reaction time is 3-6h, preferably 4-6h, further preferably 5h.
Will centrifugation bottom material at a certain temperature, reacted with the sulfuric acid of specific dosage and perchloric acid, can effectively remove copper powder,
The impurity such as phenolic resin, organic solvent carry out convenient for subsequent technique, improve the purity of gained diamond dust particle.
In a kind of preferred embodiment of the present invention, it includes inorganic that resulting material, which is carried out alkali used in alkali process,
One of alkali and organic base are a variety of, preferably one of inorganic base or a variety of, further preferably sodium hydroxide and hydrogen
One of potassium oxide is a variety of.
It include by material and water and alkali by resulting material progress alkali process in a kind of preferred embodiment of the present invention
Heat after mixing.
Preferably, resulting material is carried out in alkali process, the mass ratio of material and water is 1-2:15, preferably 1-1.5:
15, preferably 1:15.
Preferably, resulting material is carried out in alkali process, the mass ratio of material and alkali is 0.5-2:1, preferably 0.8-
1.2:1 further preferably 1:1.
Preferably, by resulting material carry out alkali process in, temperature be 40 DEG C or more, preferably 40-80 DEG C, further preferably
It is 60 DEG C.
Preferably, by resulting material carry out alkali process in, the time be 20min or more, preferably 20-60min, further it is excellent
It is selected as 30min.
Using specific alkali pretreatment, helps effectively to remove the silica solution impurity in material, be carried out convenient for subsequent technique,
Improve the purity of gained diamond dust particle.
In a kind of preferred embodiment of the present invention, it is 6-7 that resulting material gravitational settling, which is cleaned to pH, and water is added to stir
It mixes and is uniformly dispersed, by the centrifugation of gained suspension, the mass ratio of material and water is 1:5-20, preferably 1:5-15, further excellent
It is selected as 1:10.
In a kind of preferred embodiment of the present invention, it is 6-7 that resulting material gravitational settling, which is cleaned to pH, and water is added to stir
It mixes and is uniformly dispersed, by the centrifugation of gained suspension, centrifugal rotational speed is 300r/min or more, preferably 300-500r/min, into one
Step is preferably 400r/min.
In a kind of preferred embodiment of the present invention, it is 6-7 that resulting material gravitational settling, which is cleaned to pH, and water is added to stir
Mix and be uniformly dispersed, by gained suspension centrifugation in, centrifugation time be 4min or more, preferably 4-7min, further preferably
5min。
Using the operating procedure of specific sedimentation cleaning, dispersion, suspension centrifugation, help effectively to remove the oxidation in material
Aluminium impurity carries out convenient for subsequent technique, improves the purity of gained diamond dust particle.
In a kind of preferred embodiment of the present invention, gained centrifugation bottom material is reacted with sodium silicate solution, it is naturally heavy
In drop, the concentration of sodium silicate solution is 0.01wt%-0.1wt%, preferably 0.03wt%-0.07wt%, further preferably
0.05wt%.
In a kind of preferred embodiment of the present invention, gained centrifugation bottom material is reacted with sodium silicate solution, it is naturally heavy
In drop, the sedimentation time is 0.5h or more, preferably 0.5-1h, further preferably 1h.
Using specific sodium metasilicate reaction treatment technique, help effectively to remove the expense diamond large granular impurity in material
(bentonite etc.) further increases the purity of gained diamond dust particle.
In a kind of preferred embodiment of the present invention, gained centrifugation bottom material is reacted with sodium silicate solution, it is naturally heavy
In drop, multiple classification of sedimentation is carried out as needed.
Using multiple fractionation, the high-purity polycrystalline diamond micro mist for obtaining required granularity can be collected.
In a kind of preferred embodiment of the present invention, centrifugation bottom material is with its dry powder weight described in each step of the present invention
Carry out mass ratio calculating.
In a kind of preferred embodiment of the present invention, the water includes the purifying such as deionized water, distilled water, pure water
Water.
Using a kind of above-mentioned diamond recycled from sapphire with the method for diamond is recycled in grinding slug
Powder particle.
Diamond dust particle purity of the present invention is high, can be repeated as many times and utilize, and can be effectively reduced sapphire grinding and adds
The cost of work technique.
Embodiment 1
A method of diamond being recycled from sapphire in grinding slug, is included the following steps:
(1) the grinding waste material centrifugation de-oiling of collection is obtained into centrifugation bottom material using tripod pendulum type batch centrifugal;Gained is centrifuged in bottom material
Contain polycrystalline diamond, copper powder, phenolic resin, aluminium oxide, organic matter solvent etc.;
(2) the resulting centrifugation bottom material of step (1) is subjected to vacuum drying processing using vacuum oven, drying temperature is
100 DEG C, vacuum degree is -0.005MPa, drying time 8h;
(3) step (2) resulting material drying is crushed using pulverizer;Contain polycrystalline gold in smashed material
Hard rock, copper powder, phenolic resin, aluminium oxide etc.;
(4) material that step (3) crushes is put into quartz reaction kettle, it is molten that the sulfuric acid that concentration is 75wt% is added
The mass ratio of liquid, material and sulfuric acid solution is 1:30, and reaction temperature is 150 DEG C, and perchloric acid solution, object are added dropwise during the reaction
The mass ratio of material and perchloric acid solution is 0.5:1, and the W-response time is 6h;This step can remove in step (3) resulting material
The impurity such as copper powder, phenolic resin, polycrystalline diamond, silica solution that aluminium oxide, reaction generate etc. are contained in obtained material;
(5) pure water is added into the material after step (4) reaction and carries out gravitational settling cleaning, until cleaning to slurry
PH value is in 6-7;
(6) the cleaned drying materials of step (5) are removed water, obtains dried material;Wherein mainly contain polycrystalline diamond,
Aluminium oxide, silica solution, non-diamond large granular impurity etc.;
(7) it is added pure water in the dried material obtained to step (6), the mass ratio of material and pure water is 1:15, then
It is added suitable analysis pure cerium hydroxide sodium solid particle, the mass ratio of material and sodium hydroxide is 0.5:1;It then will be mixed
Slurry, which is put into water-bath, carries out heating water bath, and heating temperature is 40 DEG C, and heating time 60min heats while stirring, and carries out
Alkali process operation;This step can remove the silica solution impurity in step (6) material, contain polycrystalline diamond in obtained material
Stone, aluminium oxide, non-diamond large granular impurity etc.;
(8) pure water is added into step (7) resulting material and carries out gravitational settling cleaning, until pH of the cleaning to slurry
Value is in 6-7;
(9) it is cleaned to step (8) and suitable pure water, the quality of dried material and pure water is added into neutral slurry
Than for 1:5, being then dispersed with stirring uniformly, the suspension of polycrystalline diamond, aluminium oxide, non-diamond large granular impurity etc. is obtained;
(10) finely dispersed suspension is placed in centrifuge and does centrifugation and removes subfractionation, to isolate thin in material
Grain polycrystalline diamond and aluminium oxide;The revolving speed of centrifugal classification is 300r/min, centrifugation time 7min;This step can be with remover
Alumina impurities in material contain polycrystalline diamond, non-diamond large granular impurity etc. in obtained material;
(11) it goes the centrifugation bottom material carefully completed to imported into glass beaker again, it is molten that the sodium metasilicate that concentration is 0.01wt% is added
Liquid carries out natural subsidence and removes rough classification, to isolate the non-diamond large granular impurity in material;The time of classification of sedimentation is
0.5h carries out multiple fractionation as needed, until granularity reaches standard requirements;This step can remove the non-diamond in material
Large granular impurity obtains the higher polycrystalline diamond micro mist of purity;
(12) pure water is added again and is cleaned for the material after the completion of going slightly, and then moisture removal is removed in drying, can be obtained
The polycrystalline diamond micro mist that can be reused.
Embodiment 2
A method of diamond being recycled from sapphire in grinding slug, is included the following steps:
(1) the grinding waste material centrifugation de-oiling of collection is obtained into centrifugation bottom material using tripod pendulum type batch centrifugal;Gained is centrifuged in bottom material
Contain polycrystalline diamond, copper powder, phenolic resin, aluminium oxide, organic matter solvent etc.;
(2) the resulting centrifugation bottom material of step (1) is subjected to vacuum drying processing using vacuum oven, drying temperature is
500 DEG C, vacuum degree is -0.08MPa, drying time 2h;
(3) step (2) resulting material drying is crushed using pulverizer;Contain polycrystalline gold in smashed material
Hard rock, copper powder, phenolic resin, aluminium oxide etc.;
(4) material that step (3) crushes is put into quartz reaction kettle, it is molten that the sulfuric acid that concentration is 90wt% is added
The mass ratio of liquid, material and sulfuric acid solution is 2:30, and reaction temperature is 280 DEG C, and perchloric acid solution, object are added dropwise during the reaction
The mass ratio of material and perchloric acid solution is 1:1, and the W-response time is 3h;This step can remove in step (3) resulting material
The impurity such as copper powder, phenolic resin contain polycrystalline diamond, silica solution that aluminium oxide, reaction generate etc. in obtained material;
(5) pure water is added into the material after step (4) reaction and carries out gravitational settling cleaning, until cleaning to slurry
PH value is in 6-7;
(6) the cleaned drying materials of step (5) are removed water, obtains dried material;Wherein mainly contain polycrystalline diamond,
Aluminium oxide, silica solution, non-diamond large granular impurity etc.;
(7) it is added pure water in the dried material obtained to step (6), the mass ratio of material and pure water is 2:15, then
It is added suitable analysis pure cerium hydroxide potassium solid particle, the mass ratio of material and potassium hydroxide is 2:1;Then by mixed slurry
Material, which is put into water-bath, carries out heating water bath, and heating temperature is 80 DEG C, and heating time 20min heats while stirring, and carries out alkali
Processing operation;This step can remove the silica solution impurity in step (6) material, in obtained material containing polycrystalline diamond,
Aluminium oxide, non-diamond large granular impurity etc.;
(8) pure water is added into step (7) resulting material and carries out gravitational settling cleaning, until pH of the cleaning to slurry
Value is in 6-7;
(9) it is cleaned to step (8) and suitable pure water, the quality of dried material and pure water is added into neutral slurry
Than for 1:20, being then dispersed with stirring uniformly, the suspension of polycrystalline diamond, aluminium oxide, non-diamond large granular impurity etc. is obtained;
(10) finely dispersed suspension is placed in centrifuge and does centrifugation and removes subfractionation, to isolate thin in material
Grain polycrystalline diamond and aluminium oxide;The revolving speed of centrifugal classification is 500r/min, and centrifugation time is 4min or more;This step can be gone
Except the alumina impurities in material, polycrystalline diamond, non-diamond large granular impurity etc. are contained in obtained material;
(11) it goes the centrifugation bottom material carefully completed to imported into glass beaker again, it is molten that the sodium metasilicate that concentration is 0.1wt% is added
Liquid carries out natural subsidence and removes rough classification, to isolate the non-diamond large granular impurity in material;The time of classification of sedimentation is
1h carries out multiple fractionation as needed, until granularity reaches standard requirements;The non-diamond that this step can remove in material is big
Granule foreign obtains the higher polycrystalline diamond micro mist of purity;
(12) pure water is added again and is cleaned for the material after the completion of going slightly, and then moisture removal is removed in drying, can be obtained
The polycrystalline diamond micro mist that can be reused.
Embodiment 3
A method of diamond being recycled from sapphire in grinding slug, is included the following steps:
(1) the grinding waste material centrifugation de-oiling of collection is obtained into centrifugation bottom material using tripod pendulum type batch centrifugal;Gained is centrifuged in bottom material
Contain polycrystalline diamond, copper powder, phenolic resin, aluminium oxide, organic matter solvent etc.;
(2) the resulting centrifugation bottom material of step (1) is subjected to vacuum drying processing using vacuum oven, drying temperature is
200 DEG C, further preferably 240 DEG C, vacuum degree are -0.1MPa, drying time 4h;
(3) step (2) resulting material drying is crushed using pulverizer;Contain polycrystalline gold in smashed material
Hard rock, copper powder, phenolic resin, aluminium oxide etc.;
(4) material that step (3) crushes is put into quartz reaction kettle, it is molten that the sulfuric acid that concentration is 80wt% is added
The mass ratio of liquid, material and sulfuric acid solution is 1.2:30, and reaction temperature is 180 DEG C, and perchloric acid solution is added dropwise during the reaction,
The mass ratio of material and perchloric acid solution is 0.6:1, and the W-response time is 6h;This step can remove step (3) resulting material
In the impurity such as copper powder, phenolic resin, polycrystalline diamond, silica solution that aluminium oxide, reaction generate etc. are contained in obtained material;
(5) pure water is added into the material after step (4) reaction and carries out gravitational settling cleaning, until cleaning to slurry
PH value is in 6-7;
(6) the cleaned drying materials of step (5) are removed water, obtains dried material;Wherein mainly contain polycrystalline diamond,
Aluminium oxide, silica solution, non-diamond large granular impurity etc.;
(7) it is added pure water in the dried material obtained to step (6), the mass ratio of material and pure water is 1:15, then
It is added suitable analysis pure cerium hydroxide sodium solid particle, the mass ratio of material and sodium hydroxide is 0.8:1;It then will be mixed
Slurry, which is put into water-bath, carries out heating water bath, and heating temperature is 60 DEG C, and heating time 30min heats while stirring, and carries out
Alkali process operation;This step can remove the silica solution impurity in step (6) material, contain polycrystalline diamond in obtained material
Stone, aluminium oxide, non-diamond large granular impurity etc.;
(8) pure water is added into step (7) resulting material and carries out gravitational settling cleaning, until pH of the cleaning to slurry
Value is in 6-7;
(9) it is cleaned to step (8) and suitable pure water, the quality of dried material and pure water is added into neutral slurry
Than for 1:5, being then dispersed with stirring uniformly, the suspension of polycrystalline diamond, aluminium oxide, non-diamond large granular impurity etc. is obtained;
(10) finely dispersed suspension is placed in centrifuge and does centrifugation and removes subfractionation, to isolate thin in material
Grain polycrystalline diamond and aluminium oxide;The revolving speed of centrifugal classification is 400r/min, centrifugation time 5min;This step can be with remover
Alumina impurities in material contain polycrystalline diamond, non-diamond large granular impurity etc. in obtained material;
(11) it goes the centrifugation bottom material carefully completed to imported into glass beaker again, it is molten that the sodium metasilicate that concentration is 0.03wt% is added
Liquid carries out natural subsidence and removes rough classification, to isolate the non-diamond large granular impurity in material;The time of classification of sedimentation is
1h carries out multiple fractionation as needed, until granularity reaches standard requirements;The non-diamond that this step can remove in material is big
Granule foreign obtains the higher polycrystalline diamond micro mist of purity;
(12) pure water is added again and is cleaned for the material after the completion of going slightly, and then moisture removal is removed in drying, can be obtained
The polycrystalline diamond micro mist that can be reused.
Embodiment 4
A method of diamond being recycled from sapphire in grinding slug, is included the following steps:
(1) the grinding waste material centrifugation de-oiling of collection is obtained into centrifugation bottom material using tripod pendulum type batch centrifugal;Gained is centrifuged in bottom material
Contain polycrystalline diamond, copper powder, phenolic resin, aluminium oxide, organic matter solvent etc.;
(2) the resulting centrifugation bottom material of step (1) is subjected to vacuum drying processing using vacuum oven, drying temperature is
300 DEG C, vacuum degree is -0.1MPa, drying time 2h;
(3) step (2) resulting material drying is crushed using pulverizer;Contain polycrystalline gold in smashed material
Hard rock, copper powder, phenolic resin, aluminium oxide etc.;
(4) material that step (3) crushes is put into quartz reaction kettle, it is molten that the sulfuric acid that concentration is 80wt% is added
The mass ratio of liquid, material and sulfuric acid solution is 1.8:30, and reaction temperature is 240 DEG C, and perchloric acid solution is added dropwise during the reaction,
The mass ratio of material and perchloric acid solution is 0.8:1, and the W-response time is 4h;This step can remove step (3) resulting material
In the impurity such as copper powder, phenolic resin, polycrystalline diamond, silica solution that aluminium oxide, reaction generate etc. are contained in obtained material;
(5) pure water is added into the material after step (4) reaction and carries out gravitational settling cleaning, until cleaning to slurry
PH value is in 6-7;
(6) the cleaned drying materials of step (5) are removed water, obtains dried material;Wherein mainly contain polycrystalline diamond,
Aluminium oxide, silica solution, non-diamond large granular impurity etc.;
(7) it is added pure water in the dried material obtained to step (6), the mass ratio of material and pure water is 1.5:15,
Add suitable analysis pure cerium hydroxide potassium solid particle, the mass ratio of material and potassium hydroxide is 1.2:1;Then after mixing
Slurry be put into water-bath and carry out heating water bath, heating temperature is 60 DEG C, and heating time 30min heats while stirring, into
The operation of row alkali process;This step can remove the silica solution impurity in step (6) material, contain polycrystalline diamond in obtained material
Stone, aluminium oxide, non-diamond large granular impurity etc.;
(8) pure water is added into step (7) resulting material and carries out gravitational settling cleaning, until pH of the cleaning to slurry
Value is in 6-7;
(9) it is cleaned to step (8) and suitable pure water, the quality of dried material and pure water is added into neutral slurry
Than for 1:15, being then dispersed with stirring uniformly, the suspension of polycrystalline diamond, aluminium oxide, non-diamond large granular impurity etc. is obtained;
(10) finely dispersed suspension is placed in centrifuge and does centrifugation and removes subfractionation, to isolate thin in material
Grain polycrystalline diamond and aluminium oxide;The revolving speed of centrifugal classification is 400r/min, centrifugation time 5min;This step can be with remover
Alumina impurities in material contain polycrystalline diamond, non-diamond large granular impurity etc. in obtained material;
(11) it goes the centrifugation bottom material carefully completed to imported into glass beaker again, it is molten that the sodium metasilicate that concentration is 0.07wt% is added
Liquid carries out natural subsidence and removes rough classification, to isolate the non-diamond large granular impurity in material;The time of classification of sedimentation is
1h carries out multiple fractionation as needed, until granularity reaches standard requirements;The non-diamond that this step can remove in material is big
Granule foreign obtains the higher polycrystalline diamond micro mist of purity;
(12) pure water is added again and is cleaned for the material after the completion of going slightly, and then moisture removal is removed in drying, can be obtained
The polycrystalline diamond micro mist that can be reused.
Embodiment 5
A method of diamond being recycled from sapphire in grinding slug, is included the following steps:
(1) the grinding waste material centrifugation de-oiling of collection is obtained into centrifugation bottom material using tripod pendulum type batch centrifugal;Gained is centrifuged in bottom material
Contain polycrystalline diamond, copper powder, phenolic resin, aluminium oxide, organic matter solvent etc.;
(2) the resulting centrifugation bottom material of step (1) is subjected to vacuum drying processing using vacuum oven, drying temperature is
240 DEG C, vacuum degree is -0.1MPa, drying time 2h;
(3) step (2) resulting material drying is crushed using pulverizer;Contain polycrystalline gold in smashed material
Hard rock, copper powder, phenolic resin, aluminium oxide etc.;
(4) material that step (3) crushes is put into quartz reaction kettle, addition concentration is 75wt% or more, preferably
For the sulfuric acid solution of 80wt%, the mass ratio of material and sulfuric acid solution is 1.5:30, and reaction temperature is 210 DEG C, in reaction process
The mass ratio of middle dropwise addition perchloric acid solution, material and perchloric acid solution is 0.7:1, and the W-response time is 5h;This step can be removed
It removes the impurity such as copper powder, the phenolic resin in step (3) resulting material, polycrystalline diamond, aluminium oxide, anti-is contained in obtained material
The silica solution etc. that should be generated;
(5) pure water is added into the material after step (4) reaction and carries out gravitational settling cleaning, until cleaning to slurry
PH value is in 6-7;
(6) the cleaned drying materials of step (5) are removed water, obtains dried material;Wherein mainly contain polycrystalline diamond,
Aluminium oxide, silica solution, non-diamond large granular impurity etc.;
(7) it is added pure water in the dried material obtained to step (6), the mass ratio of material and pure water is 1:15, then
It is added suitable analysis pure cerium hydroxide sodium solid particle, the mass ratio of material and sodium hydroxide is 1:1;Then by mixed slurry
Material, which is put into water-bath, carries out heating water bath, and heating temperature is 60 DEG C, and heating time 30min heats while stirring, and carries out alkali
Processing operation;This step can remove the silica solution impurity in step (6) material, in obtained material containing polycrystalline diamond,
Aluminium oxide, non-diamond large granular impurity etc.;
(8) pure water is added into step (7) resulting material and carries out gravitational settling cleaning, until pH of the cleaning to slurry
Value is in 6-7;
(9) it is cleaned to step (8) and suitable pure water, the quality of dried material and pure water is added into neutral slurry
Than for 1:10, being then dispersed with stirring uniformly, the suspension of polycrystalline diamond, aluminium oxide, non-diamond large granular impurity etc. is obtained;
(10) finely dispersed suspension is placed in centrifuge and does centrifugation and removes subfractionation, to isolate thin in material
Grain polycrystalline diamond and aluminium oxide;The revolving speed of centrifugal classification is 400r/min, centrifugation time 5min;This step can be with remover
Alumina impurities in material contain polycrystalline diamond, non-diamond large granular impurity etc. in obtained material;
(11) it goes the centrifugation bottom material carefully completed to imported into glass beaker again, it is molten that the sodium metasilicate that concentration is 0.05wt% is added
Liquid carries out natural subsidence and removes rough classification, to isolate the non-diamond large granular impurity in material;The time of classification of sedimentation is
1h carries out multiple fractionation as needed, until granularity reaches standard requirements;The non-diamond that this step can remove in material is big
Granule foreign obtains the higher polycrystalline diamond micro mist of purity;
(12) pure water is added again and is cleaned for the material after the completion of going slightly, and then moisture removal is removed in drying, can be obtained
The polycrystalline diamond micro mist that can be reused.
Diamond dust particulate component (mass fraction) obtained by 1-5 of embodiment of the present invention method is detected, as a result such as
Under:
The diamond components testing result that 1 present invention of table is recycled from sapphire grinding slug
It can be seen from Table 1 that the present invention uses the method that diamond is recycled in grinding slug from sapphire, it can be effective
Remove the impurity such as copper powder, phenolic resin, aluminium oxide, bentonite, the organic matter solvent in sapphire grinding slug, gained Buddha's warrior attendant
Stone powder particle purity is high, can be repeated as many times and utilize, can be effectively reduced the cost of sapphire grinding process technique.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that the above various embodiments is only used
To illustrate technical solution of the present invention, rather than its limitations;Those skilled in the art should understand that: without departing substantially from this hair
It in the case where bright spirit and scope, is possible to modify the technical solutions described in the foregoing embodiments, or to wherein
Some or all of technical characteristic is equivalently replaced;And these are modified or replaceed, and do not make the essence of corresponding technical solution
It departs from the scope of the technical solutions of the embodiments of the present invention;It is, therefore, intended that in the following claims including belonging to the present invention
All these substitutions and modifications in range.
Claims (50)
1. a kind of from the sapphire method for recycling diamond in grinding slug, which comprises the steps of:
(1) by sapphire grinding slug centrifugation de-oiling;
(2) gained centrifugation bottom material is subjected to vacuum drying processing;
(3) by gained material drying and sulfuric acid and perchloric acid impurity removal reaction;
(4) cleaning resulting material gravitational settling to pH is 6-7;
(5) resulting material is subjected to alkali process;
(6) cleaning resulting material gravitational settling to pH is 6-7, adds water and stirs and is uniformly dispersed, gained suspension is centrifuged;
(7) gained centrifugation bottom material is reacted with sodium silicate solution, natural subsidence obtains diamond dust particle;
Wherein, the drying temperature of vacuum drying processing is 100-500 DEG C, the vacuum degree of the vacuum drying is-
0.005MPa is hereinafter, the drying time of the vacuum drying is 2-8h;
Include heating after mixing material with water and alkali by resulting material progress alkali process, resulting material is subjected to alkali process
In, the mass ratio of material and water is 1-2:15, and the mass ratio of material and alkali is 0.5-2:1, and temperature is 40 DEG C or more, and the time is
20min or more;
The content of diamond is 99.0%, 99.4%, 99.5%, 99.6% or 99.8% in the diamond dust particle.
2. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In the drying temperature of the vacuum drying processing is 200-300 DEG C.
3. according to claim 2 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In the drying temperature of the vacuum drying processing is 240 DEG C.
4. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In the vacuum degree of the vacuum drying is -0.08MPa or less.
5. according to claim 4 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In the vacuum degree of the vacuum drying is -0.1MPa or less.
6. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In the drying time of the vacuum drying is 2-4h.
7. according to claim 6 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In the drying time of the vacuum drying is 2h.
8. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In, by gained centrifugation bottom material crush after again with sulfuric acid and perchloric acid impurity removal reaction.
9. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In the concentration of the sulfuric acid is 75wt% or more.
10. according to claim 9 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In the concentration of the sulfuric acid is 75wt%-90wt%.
11. according to claim 10 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, the concentration of the sulfuric acid is 80wt%.
12. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In gained material drying being added in reactor, then during gained material drying and sulfuric acid and perchloric acid impurity removal reaction
The concentrated sulfuric acid is added, the mass ratio for being centrifuged bottom material and sulfuric acid is 1-2:30.
13. according to claim 12 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, the mass ratio for being centrifuged bottom material and sulfuric acid is 1.2-1.8:30.
14. according to claim 13 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, the mass ratio for being centrifuged bottom material and sulfuric acid is 1.5:30.
15. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In being added dropwise perchloric acid during the reaction, the mass ratio of material drying and perchloric acid is 0.5-1:1.
16. according to claim 15 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, the mass ratio of material drying and perchloric acid is 0.6-0.8:1.
17. according to claim 16 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, the mass ratio of material drying and perchloric acid is 0.7:1.
18. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In being 150-280 DEG C by the reaction temperature of gained material drying and sulfuric acid and perchloric acid impurity removal reaction.
19. according to claim 18 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, is 180-240 DEG C by the reaction temperature of gained material drying and sulfuric acid and perchloric acid impurity removal reaction.
20. according to claim 19 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, is 210 DEG C by the reaction temperature of gained material drying and sulfuric acid and perchloric acid impurity removal reaction.
21. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In being 3-6h by the reaction time of gained material drying and sulfuric acid and perchloric acid impurity removal reaction.
22. according to claim 21 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, is 4-6h by the reaction time of gained material drying and sulfuric acid and perchloric acid impurity removal reaction.
23. according to claim 22 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, is 5h by the reaction time of gained material drying and sulfuric acid and perchloric acid impurity removal reaction.
24. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In it includes one of inorganic base and organic base or a variety of that resulting material, which is carried out alkali used in alkali process,.
25. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In it is one of inorganic base or a variety of that resulting material, which is carried out alkali used in alkali process,.
26. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In it is one of sodium hydroxide and potassium hydroxide or a variety of that resulting material, which is carried out alkali used in alkali process,.
27. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In by resulting material progress alkali process, the mass ratio of material and water is 1-1.5:15.
28. according to claim 27 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, resulting material is carried out in alkali process, the mass ratio of material and water is 1:15.
29. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In by resulting material progress alkali process, the mass ratio of material and alkali is 0.8-1.2:1.
30. according to claim 29 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, resulting material is carried out in alkali process, the mass ratio of material and alkali is 1:1.
31. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In by resulting material progress alkali process, temperature is 40-80 DEG C.
32. according to claim 31 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, resulting material is carried out in alkali process, temperature is 60 DEG C.
33. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In, by resulting material carry out alkali process in, time 20-60min.
34. according to claim 33 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, resulting material is carried out in alkali process, time 30min.
35. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In, by resulting material gravitational settling clean to pH be 6-7, add water and stir and be uniformly dispersed, by gained suspension centrifugation in, material with
The mass ratio of water is 1:5-20.
36. according to claim 35 a kind of from the sapphire method for recycling diamond in grinding slug, feature
Be, by resulting material gravitational settling clean to pH be 6-7, add water and stir and be uniformly dispersed, by gained suspension centrifugation in, material
Mass ratio with water is 1:5-15.
37. according to claim 36 a kind of from the sapphire method for recycling diamond in grinding slug, feature
Be, by resulting material gravitational settling clean to pH be 6-7, add water and stir and be uniformly dispersed, by gained suspension centrifugation in, material
Mass ratio with water is 1:10.
38. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In cleaning resulting material gravitational settling to pH is 6-7, adds water and stirs and is uniformly dispersed, and by the centrifugation of gained suspension, centrifugation turns
Speed is 300r/min or more.
39. a kind of from the sapphire method for recycling diamond in grinding slug, feature according to claim 38
It is, centrifugal rotational speed 300-500r/min.
40. according to claim 39 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, centrifugal rotational speed 400r/min.
41. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In cleaning resulting material gravitational settling to pH is 6-7, adds water and stirs and is uniformly dispersed, by the centrifugation of gained suspension, when centrifugation
Between be 4min or more.
42. according to claim 41 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, centrifugation time 4-7min.
43. according to claim 42 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, centrifugation time 5min.
44. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In gained centrifugation bottom material being reacted with sodium silicate solution, in natural subsidence, the concentration of sodium silicate solution is 0.01wt%-
0.1wt%.
45. according to claim 44 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, the concentration of sodium silicate solution is 0.03wt%-0.07wt%.
46. according to claim 45 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, the concentration of sodium silicate solution is 0.05wt%.
47. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In gained centrifugation bottom material being reacted with sodium silicate solution, in natural subsidence, the sedimentation time is 0.5h or more.
48. according to claim 47 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, sedimentation time 0.5-1h.
49. according to claim 48 a kind of from the sapphire method for recycling diamond in grinding slug, feature
It is, sedimentation time 1h.
50. according to claim 1 a kind of from the sapphire method for recycling diamond in grinding slug, feature exists
In gained centrifugation bottom material is reacted with sodium silicate solution, in natural subsidence, carries out multiple classification of sedimentation as needed.
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