CN104495836B - A kind of processing method of diadust - Google Patents
A kind of processing method of diadust Download PDFInfo
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- CN104495836B CN104495836B CN201410706391.9A CN201410706391A CN104495836B CN 104495836 B CN104495836 B CN 104495836B CN 201410706391 A CN201410706391 A CN 201410706391A CN 104495836 B CN104495836 B CN 104495836B
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- 238000003672 processing method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 64
- 239000003513 alkali Substances 0.000 claims abstract description 55
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims abstract description 40
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000004575 stone Substances 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 16
- 229910017052 cobalt Inorganic materials 0.000 abstract description 15
- 239000010941 cobalt Substances 0.000 abstract description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract description 15
- 239000012535 impurity Substances 0.000 abstract description 10
- 239000010432 diamond Substances 0.000 abstract description 9
- 229910003460 diamond Inorganic materials 0.000 abstract description 9
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 7
- 230000001590 oxidative effect Effects 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 7
- 230000007423 decrease Effects 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 6
- 229910052748 manganese Inorganic materials 0.000 description 6
- 239000011572 manganese Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 238000010306 acid treatment Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 1
- 239000010437 gem Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen Sodium oxide Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Catalysts (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides the processing method of a kind of diadust, comprise the following steps: pending diadust is carried out alkali process, obtain alkali and process diadust；Alkali is processed diadust and carries out HCl treatment and logical ozone, obtain diadust intermediate；Described diadust intermediate is dried, obtains diadust.Processed by logical ozone during the disposal methods diadust that the present invention provides, it is to avoid the use of acid with strong oxidizing property, saved cost, decrease the pollution to environment.It addition, the impurities from diamond micro powder content that the present invention obtains is relatively low.Test result indicate that: the content≤5ppm, the content≤10ppm of manganese, the content≤5ppm of ferrum of the middle cobalt of the diadust that the disposal methods that the present invention provides obtains.
Description
Technical field
The invention belongs to diadust technical field, particularly relate to the processing method of a kind of diadust.
Background technology
Diadust refers to that granularity is narrower than the diamond particles of 36/54 micron, diadust hardness
Height, wearability are good, can be widely used for cutting, grinding, probing etc., are grinding and polishing hard alloy, pottery
The desirable feedstock of the high hardness materials such as porcelain, gem, optical glass.It addition, used by synthesis polycrystalline diamond
Diadust is higher to the requirement of impurity content, and requires its good dispersion, in order to batch mixing is equal
Even.
Conventional diadust processing method is acid-alkali treatment, is first placed on by pending diadust
In melted sodium hydroxide, under conditions of temperature is 800 DEG C, remove the pyrophillite composition in building-up process,
Mainly include the element such as aluminum, silicon；Second step, places it in the strong oxidizing property of hydrochloric acid and perchloric acid or nitric acid
Acid solution boils, to remove metal impurities and the graphite-phases such as manganese therein, cobalt, ferrum；3rd step,
Clean with pure water, put and be dried in 100 DEG C in an oven, obtain diadust.In above-mentioned processing procedure,
Use the acid with strong oxidizing property such as substantial amounts of perchloric acid or nitric acid, pollute environment, and human body is worked the mischief.
Summary of the invention
In view of this, it is an object of the invention to provide the processing method of a kind of diadust, the present invention
The use of acid with strong oxidizing property is provided during the disposal methods diadust provided.
The invention provides the processing method of a kind of diadust, comprise the following steps:
Pending diadust is carried out alkali process, obtains alkali and process diadust；
Described alkali process diadust is carried out HCl treatment and logical ozone, obtains in the middle of diadust
Body；
Described diadust intermediate is dried, obtains diadust.
Preferably, described alkali processes and uses alkaline matter；
Described alkaline matter includes sodium hydroxide and/or potassium hydroxide.
Preferably, the mass ratio of described pending diadust and alkaline matter is 1:2.8～3.3.
Preferably, the temperature that described alkali processes is 780 DEG C～830 DEG C.
Preferably, the time that described alkali processes is 1.5h～2.5h.
Preferably, described alkali processes diadust and the mass ratio 1:2.8～3.3 of hydrochloric acid.
Preferably, the temperature of described logical ozone is 95 DEG C～100 DEG C.
Preferably, the time of described logical ozone is 1h～30h.
Preferably, the mass concentration of the ozone used during described logical ozone is 20mg/L～25mg/L.
Preferably, described dry temperature is 60 DEG C～150 DEG C；
The described dry time is 1h～8h.
The invention provides the processing method of a kind of diadust, comprise the following steps: by pending gold
Hard rock micropowder carries out alkali process, obtains alkali and processes diadust；Alkali is processed diadust and carries out salt
Acid treatment and logical ozone, obtain diadust intermediate；Described diadust intermediate is done
Dry, obtain diadust.By leading to when the disposal methods that the present invention provides processes diadust
Ozone processes, it is to avoid the use of acid with strong oxidizing property, has saved cost, decreases the pollution to environment.
It addition, the impurities from diamond micro powder content that the present invention obtains is relatively low.Test result indicate that: the present invention carries
Content≤the 5ppm of cobalt in the diadust that the disposal methods of confession obtains, the content≤10ppm of manganese,
Content≤the 5ppm of ferrum.
Detailed description of the invention
The invention provides the processing method of a kind of diadust, comprise the following steps:
Pending diadust is carried out alkali process, obtains alkali and process diadust；
Alkali is processed diadust and carries out HCl treatment and logical ozone, obtain diadust intermediate；
Described diadust intermediate is dried, obtains diadust.
Pending diadust is carried out alkali process by the present invention, obtains alkali and processes diadust.At this
In invention, the granularity of described pending diadust is preferably 1 μm～50 μm, more preferably
2 μm～40 μm, most preferably 4 μm～10 μm；In described pending diadust, the content of cobalt is 80
Ppm～150ppm, the content of ferrum is 110ppm～150ppm；The content of manganese is 50ppm～60ppm.
The present invention does not has special restriction to the source of described pending diadust, uses people in the art
Pending diadust known to Yuan, as used its commercial goods.
In the present invention, described alkali processes and preferably employs alkaline matter, and described alkaline matter preferably includes hydrogen
Sodium oxide and/or potassium hydroxide；The mass ratio of described pending diadust and alkaline matter is preferably
1:2.8～3.3, more preferably 1:2.9～3.2, most preferably 1:3.
In the present invention, described alkaline matter is molten condition when alkali processes；The temperature that described alkali processes
It is preferably 780 DEG C～830 DEG C, more preferably 790 DEG C～820 DEG C, most preferably 795 DEG C～805 DEG C；Described
The time that alkali processes is preferably 1.5h～2.5h, more preferably 1.8h～2.3h, most preferably 1.9h～2.1h.
The equipment used when alkali is processed by the present invention does not has special restriction, preferably by micro-for pending diamond
Powder is placed in stainless steel crucible well known to those skilled in the art and carries out alkali process.
After obtaining alkali process diadust, described alkali process diadust is carried out acid treatment by the present invention
With logical ozone, obtain diadust intermediate.The present invention processes diadust at alkali and carries out acid treatment
Before, preferably alkali is processed diadust and cools down successively and wash.Alkali is preferably processed gold by the present invention
Hard rock micropowder is cooled to room temperature.Present invention preferably employs deionized water to wash；Preferably washing 3 times～4
Secondary.
In the present invention, the mass fraction of described hydrochloric acid is 36%～38%；Described alkali processes diadust
It is preferably 1:2.8～3.3, more preferably 1:2.9～3.2, most preferably 1:3 with the mass ratio of hydrochloric acid.
The present invention preferably carries out alkali under conditions of stirring and processes the HCl treatment of diadust.At this
In bright, the speed of described stirring is preferably 170 revs/min～190 revs/min.
The order that the present invention carries out HCl treatment and logical ozone to alkali process diadust does not has special limit
System, the present invention can carry out HCl treatment simultaneously and logical ozone processes, it is also possible to first carries out HCl treatment again
Logical ozone, it is also possible to first lead to ozone and carrying out HCl treatment.The present invention preferably logical ozone after hydrochloric acid seethes with excitement,
Obtain diadust intermediate.In the present invention, alkali can be processed diamond micro-for described HCl treatment
Manganese, cobalt and ferrous metal impurity part in powder are removed；It is micro-that described logical ozone can remove alkali process diamond
Graphite-phase in powder.In the present invention, the mass concentration of the ozone used during described logical ozone is
20mg/L～25mg/L；The flow of the ozone used during described logical ozone is
100mL/min～1000mL/min, the temperature of described logical ozone is preferably 95 DEG C～105 DEG C, more preferably
98 DEG C～103 DEG C, most preferably 100 DEG C；The time of described logical ozone is preferably 1h～30h, more preferably
4h～20h.
After completing logical ozone, the diadust after logical ozone is preferably processed by the present invention is carried out；This
Invention preferably employs deionized water and is carried out；Preferably clean no less than 5 times.
After obtaining diadust intermediate, described diadust intermediate is dried by the present invention,
Obtain diadust.In the present invention, described dry temperature is preferably 60 DEG C～150 DEG C；Described dry
Dry time 1h～8h, more preferably 3h～6h.
The present invention uses the flame atomic absorption spectrometry method diadust to obtaining to carry out cobalt content
Test, the test of Fe content and the test of iron content, test result is: the content≤5ppm of cobalt, manganese
Content≤10ppm, the content≤5ppm of ferrum.
The invention provides the processing method of a kind of diadust, comprise the following steps: by pending gold
Hard rock micropowder carries out alkali process, obtains alkali and processes diadust；Alkali is processed diadust and carries out salt
Acid treatment and logical ozone, obtain diadust intermediate；Described diadust intermediate is done
Dry, obtain diadust.By leading to when the disposal methods that the present invention provides processes diadust
Ozone processes, it is to avoid the use of acid with strong oxidizing property, has saved cost, decreases the pollution to environment.
It addition, the impurities from diamond micro powder content that the present invention obtains is relatively low.Test result indicate that: the present invention carries
Content≤the 5ppm of cobalt in the diadust that the disposal methods of confession obtains, the content≤10ppm of manganese,
Content≤the 5ppm of ferrum.
In order to further illustrate the present invention, a kind of diamond provided the present invention below in conjunction with embodiment is micro-
The processing method of powder is described in detail, but they can not be interpreted as the limit to scope
Fixed.
Embodiment 1
By 500ct (content of cobalt is 100ppm, and the content of ferrum is 144ppm, and the content of manganese is 55ppm)
Granularity is 2 μm～the pending diadust of 4 μm and sodium hydroxide is put into stainless according to the mass ratio of 1:3
In steel crucible, 800 DEG C are boiled 2 hours, obtain alkali and process diadust；
Alkali is processed diadust cooling, takes out and clean no less than 3 times with deionized water；
Alkali after cleaning processes diadust and puts in beaker, and adds quality according to the mass ratio of 1:3
Mark is the hydrochloric acid of 38%, stirring, and mixing speed is 180 revs/min, 100 DEG C boil after start to be passed through smelly
Oxygen, the concentration of ozone is 10mg/L, and the gas flow of ozone is 100mL/min, takes out after 4 hours,
And clean no less than 5 times with deionized water, obtain diadust intermediate；
The diadust intermediate obtained is put in baking oven and is dried, take out after being dried 6 hours at 80 DEG C,
Obtain diadust.
The impurity that the present invention measures diadust surface according to method of testing described in technique scheme contains
Amount, measurement result is: the content≤5ppm of cobalt, the content≤5ppm of manganese, and the content≤5ppm of ferrum does not has
Graphite-phase detected.
Embodiment 2
By 500ct (content of cobalt is 150ppm, and the content of ferrum is 124ppm, and the content of manganese is 60ppm)
Granularity is the pending diadust of 5～10 μm and sodium hydroxide puts into rustless steel according to the mass ratio of 1:3
In crucible, 800 DEG C are boiled 2 hours, obtain alkali and process diadust；
Alkali is processed diadust cooling, takes out and clean no less than 3 times with deionized water；
Alkali after cleaning processes diadust and puts in beaker, and adds quality according to the mass ratio of 1:3
Mark is the hydrochloric acid of 36%, stirring, and mixing speed is 180 revs/min, 100 DEG C boil after start to be passed through smelly
Oxygen, the concentration of ozone is 20mg/L, and the gas flow of ozone is 500mL/min, takes out after 1 hour,
And clean no less than 5 times with deionized water, obtain diadust intermediate；
The diadust intermediate obtained is put in baking oven and is dried, be dried 3.5 hours at 120 DEG C
Rear taking-up, obtains diadust.
The impurity that the present invention measures diadust surface according to method of testing described in technique scheme contains
Amount, measurement result is: the content≤5ppm of cobalt, the content≤10ppm of manganese, the content≤5ppm of ferrum,
It is not detected by graphite-phase.
Embodiment 3
By 500ct (content of cobalt is 122ppm, and the content of ferrum is 140ppm, and the content of manganese is 50ppm)
Granularity is the pending diadust of 4～8 μm and sodium hydroxide puts into rustless steel according to the mass ratio of 1:3
In crucible, 800 DEG C are boiled 2 hours, obtain alkali and process diadust；
Cool down out and diadust is taken out and cleans no less than 3 times with deionized water；
Diadust after cleaning is put in beaker, and according to the mass ratio addition mass fraction of 1:3 is
The hydrochloric acid of 37%, stirring, mixing speed is 180 revs/min, 100 DEG C boil after start to be passed through ozone, smelly
The concentration of oxygen is 30mg/L, and the gas flow of ozone is 1000mL/min, takes out, and use after 30 hours
Deionized water cleans no less than 5 times, obtains diadust intermediate；
The diadust intermediate obtained is put in baking oven and is dried, after being dried 4 hours at 100 DEG C
Take out, obtain diadust.
The present invention contains according to method of testing described in technique scheme, the impurity measuring diadust surface
Amount, test result is: the content≤5ppm of cobalt, the content≤10ppm of manganese, the content≤5ppm of ferrum,
It is not detected by graphite-phase.
As seen from the above embodiment, the invention provides the processing method of a kind of diadust, including with
Lower step: pending diadust is carried out alkali process, obtains alkali and processes diadust；At alkali
Reason diadust carries out HCl treatment and logical ozone, obtains diadust intermediate；By described Buddha's warrior attendant
Stone micropowder intermediate is dried, and obtains diadust.The disposal methods Buddha's warrior attendant that the present invention provides
Processed by logical ozone during stone micropowder, it is to avoid the use of acid with strong oxidizing property, saved cost, decrease
Pollution to environment.It addition, the impurity content that the present invention processes the diadust obtained is relatively low.Experiment
Result shows: the content≤5ppm of cobalt in the diadust that the disposal methods that the present invention provides obtains,
Content≤the 10ppm of manganese, the content≤5ppm of ferrum.
The above is only the preferred embodiment of the present invention, it is noted that general for the art
For logical technical staff, under the premise without departing from the principles of the invention, it is also possible to make some improvement and profit
Decorations, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (5)
1. a processing method for diadust, comprises the following steps:
Pending diadust is carried out alkali process, obtains alkali and process diadust；
Described alkali process diadust is carried out HCl treatment and logical ozone, obtains diadust
Intermediate；
Described diadust intermediate is dried, obtains diadust；
Described alkali processes and uses alkaline matter；
Described alkaline matter is made up of sodium hydroxide and/or potassium hydroxide；
The temperature that described alkali processes is 780 DEG C～830 DEG C；
The time that described alkali processes is 1.5h～2.5h；
The temperature of described logical ozone is 95 DEG C～105 DEG C；
The time of described logical ozone is 1h～30h.
Processing method the most according to claim 1, it is characterised in that described pending Buddha's warrior attendant
The mass ratio of stone micropowder and alkaline matter is 1:2.8～3.3.
Processing method the most according to claim 1, it is characterised in that described alkali processes Buddha's warrior attendant
The mass ratio 1:2.8～3.3 of stone micropowder and hydrochloric acid.
Processing method the most according to claim 1, it is characterised in that adopt during described logical ozone
The mass concentration of ozone be 20mg/L～25mg/L.
Processing method the most according to claim 1, it is characterised in that described dry temperature
It it is 60 DEG C～150 DEG C；
The described dry time is 1h～8h.
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| CN105271218B (en) * | 2015-10-28 | 2017-12-22 | 山田研磨材料有限公司 | A kind of production method of diadust |
| CN107777710A (en) * | 2017-11-28 | 2018-03-09 | 黄冈师范学院 | With the method and device of nitrogen oxide potassium nitrate recovery diamond |
| CN109305676B (en) * | 2018-11-26 | 2021-08-03 | 南京金瑞立丰硬质材料科技有限公司 | Simple and efficient method for removing graphite carbon in nano diamond ash |
| CN111620336B (en) * | 2020-06-09 | 2022-04-08 | 河南天钻晶体材料有限公司 | Diamond micro powder, method and equipment for cleaning diamond single crystal |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324906A (en) * | 2000-05-16 | 2001-12-05 | 因芬尼昂技术股份公司 | Polishing liquid for structurizing treatment of metal and metal oxide and method thereof |
| CN102888584A (en) * | 2012-09-17 | 2013-01-23 | 上海大学 | Method for depositing CdTe thin film based on diamond thin film |
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| WO2014121819A1 (en) * | 2013-02-06 | 2014-08-14 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Folate functionalized nanodiamond particles, method for its preparation and their use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1324906A (en) * | 2000-05-16 | 2001-12-05 | 因芬尼昂技术股份公司 | Polishing liquid for structurizing treatment of metal and metal oxide and method thereof |
| CN102888584A (en) * | 2012-09-17 | 2013-01-23 | 上海大学 | Method for depositing CdTe thin film based on diamond thin film |
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