CN104495836A - Method for processing diamond micropowder - Google Patents

Method for processing diamond micropowder Download PDF

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Publication number
CN104495836A
CN104495836A CN201410706391.9A CN201410706391A CN104495836A CN 104495836 A CN104495836 A CN 104495836A CN 201410706391 A CN201410706391 A CN 201410706391A CN 104495836 A CN104495836 A CN 104495836A
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diadust
content
alkaline purification
diamond micropowder
ozone
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CN201410706391.9A
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CN104495836B (en
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王晓
李治海
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Henan Jingrui Superhard Material Co Ltd
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Henan Jingrui Superhard Material Co Ltd
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Abstract

The invention provides a method for processing diamond micropowder. The method comprises the following steps: carrying out alkali treatment on to-be-processed diamond micropowder to obtain alkali-treated diamond micropowder; carrying out hydrochloric acid treatment on the alkali-treated diamond micropowder, and introducing ozone to obtain a diamond micropowder intermediate; and drying the diamond micropowder intermediate to obtain diamond micropowder. According to the processing method provided by the invention, the ozone is introduced to process when the diamond micropowder is processed, so that use of strong oxidative acids is avoided; the cost is reduced; and the pollution to the environment is reduced. In addition, the diamond micropowder obtained by the method is relatively low in impurity content. An experiment result shows that the cobalt content of the diamond micropowder obtained by the processing method disclosed by the invention is smaller than or equal to 5ppm; the content of manganese is smaller than or equal to 10ppm; and the content of iron is smaller than or equal to 5ppm.

Description

A kind for the treatment of process of diadust
Technical field
The invention belongs to diadust technical field, particularly relate to a kind for the treatment of process of diadust.
Background technology
Diadust refers to that granularity is narrower than the diamond particles of 36/54 micron, diadust hardness is high, wear resistance good, can be widely used in cutting, grinding, probing etc., be the desirable feedstock of the high hardness materials such as grinding and polishing Wimet, pottery, jewel, opticglass.In addition, the requirement of synthesis polycrystalline diamond diadust used to foreign matter content is higher, and requires its good dispersity, so that batch mixing is even.
Conventional diadust treatment process is acid-alkali treatment, is first placed in the sodium hydroxide of melting by pending diadust, is the agalmatolite composition removed under the condition of 800 DEG C in building-up process, mainly comprises the element such as aluminium, silicon in temperature; Second step, places it in the strong oxidizing property acid solution of hydrochloric acid and perchloric acid or nitric acid and boils, to remove metallic impurity and the graphite-phase such as manganese, cobalt, iron wherein; 3rd step, with pure water cleaning, puts in an oven in 100 DEG C of dryings, obtains diadust.In above-mentioned treating processes, use the acid with strong oxidizing property such as a large amount of perchloric acid or nitric acid, contaminate environment, and human body is worked the mischief.
Summary of the invention
In view of this, the object of the present invention is to provide a kind for the treatment of process of diadust, during disposal methods diadust provided by the invention, avoid the use of acid with strong oxidizing property.
The invention provides a kind for the treatment of process of diadust, comprise the following steps:
Pending diadust is carried out alkaline purification, obtains alkaline purification diadust;
Described alkaline purification diadust is carried out HCl treatment and logical ozone, obtains diadust intermediate;
Described diadust intermediate is carried out drying, obtains diadust.
Preferably, described alkaline purification adopts alkaline matter;
Described alkaline matter comprises 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 of described alkaline purification is 780 DEG C ~ 830 DEG C.
Preferably, the time of described alkaline purification is 1.5h ~ 2.5h.
Preferably, mass ratio 1:2.8 ~ 3.3 of described alkaline purification diadust and 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 adopted during described logical ozone is 20mg/L ~ 25mg/L.
Preferably, the temperature of described drying is 60 DEG C ~ 150 DEG C;
The time of described drying is 1h ~ 8h.
The invention provides a kind for the treatment of process of diadust, comprise the following steps: pending diadust is carried out alkaline purification, obtain alkaline purification diadust; Alkaline purification diadust is carried out HCl treatment and logical ozone, obtain diadust intermediate; Described diadust intermediate is carried out drying, obtains diadust.By logical ozonize during disposal methods process diadust provided by the invention, avoid the use of acid with strong oxidizing property, saved cost, decrease the pollution to environment.In addition, the impurities from diamond micro powder content that obtains of the present invention is lower.Experimental result shows: the content≤5ppm of cobalt in the diadust that disposal methods provided by the invention obtains, the content≤10ppm of manganese, the content≤5ppm of iron.
Embodiment
The invention provides a kind for the treatment of process of diadust, comprise the following steps:
Pending diadust is carried out alkaline purification, obtains alkaline purification diadust;
Alkaline purification diadust is carried out HCl treatment and logical ozone, obtain diadust intermediate;
Described diadust intermediate is carried out drying, obtains diadust.
Pending diadust is carried out alkaline purification by the present invention, obtains alkaline purification diadust.In the present invention, the granularity of described pending diadust is preferably 1 μm ~ 50 μm, is more preferably 2 μm ~ 40 μm, most preferably is 4 μm ~ 10 μm; In described pending diadust, the content of cobalt is 80ppm ~ 150ppm, and the content of iron is 110ppm ~ 150ppm; The content of manganese is 50ppm ~ 60ppm.The source of the present invention to described pending diadust does not have special restriction, adopts pending diadust well known to those skilled in the art, as adopted its commercial goods.
In the present invention, described alkaline purification preferably adopts alkaline matter, and described alkaline matter preferably includes sodium hydroxide and/or potassium hydroxide; The mass ratio of described pending diadust and alkaline matter is preferably 1:2.8 ~ 3.3, is more preferably 1:2.9 ~ 3.2, most preferably is 1:3.
In the present invention, described alkaline matter is molten state when alkaline purification; The temperature of described alkaline purification is preferably 780 DEG C ~ 830 DEG C, is more preferably 790 DEG C ~ 820 DEG C, most preferably is 795 DEG C ~ 805 DEG C; The time of described alkaline purification is preferably 1.5h ~ 2.5h, is more preferably 1.8h ~ 2.3h, most preferably is 1.9h ~ 2.1h.
The present invention does not have special restriction to the equipment adopted during alkaline purification, preferably pending diadust is placed in Stainless Steel Crucible well known to those skilled in the art and carries out alkaline purification.
After obtaining alkaline purification diadust, described alkaline purification diadust is carried out acid treatment and logical ozone by the present invention, obtains diadust intermediate.Alkaline purification diadust, before alkaline purification diadust carries out acid treatment, preferably carries out cooling and washing by the present invention successively.Alkaline purification diadust is preferably cooled to room temperature by the present invention.The present invention preferably adopts deionized water to wash; Preferred washing 3 times ~ 4 times.
In the present invention, the massfraction of described hydrochloric acid is 36% ~ 38%; The mass ratio of described alkaline purification diadust and hydrochloric acid is preferably 1:2.8 ~ 3.3, is more preferably 1:2.9 ~ 3.2, most preferably is 1:3.
The present invention preferably carries out the HCl treatment of alkaline purification diadust under the condition stirred.In the present invention, the speed of described stirring is preferably 170 revs/min ~ 190 revs/min.
The present invention does not have special restriction to the order that alkaline purification diadust carries out HCl treatment and logical ozone, the present invention can carry out HCl treatment and logical ozonize simultaneously, also first can carry out HCl treatment logical ozone again, first can also lead to ozone and carry out HCl treatment.The present invention is logical ozone after hydrochloric acid boiling preferably, obtains diadust intermediate.In the present invention, the manganese in alkaline purification diadust, cobalt and ferrous metal impurity portion can be removed by described HCl treatment; Described logical ozone can remove the graphite-phase in alkaline purification diadust.In the present invention, the mass concentration of the ozone adopted during described logical ozone is 20mg/L ~ 25mg/L; The flow of the ozone adopted during described logical ozone is 100mL/min ~ 1000mL/min, and the temperature of described logical ozone is preferably 95 DEG C ~ 105 DEG C, is more preferably 98 DEG C ~ 103 DEG C, most preferably is 100 DEG C; The time of described logical ozone is preferably 1h ~ 30h, is more preferably 4h ~ 20h.
After completing logical ozone, the diadust after logical ozonize preferably cleans by the present invention; The present invention preferably adopts deionized water to clean; Preferred cleaning is no less than 5 times.
After obtaining diadust intermediate, described diadust intermediate is carried out drying by the present invention, obtains diadust.In the present invention, the temperature of described drying is preferably 60 DEG C ~ 150 DEG C; Time 1h ~ the 8h of described drying, is more preferably 3h ~ 6h.
The present invention adopts flame atomic absorption spectrometry method to carry out the test of the test of cobalt contents, the test of Fe content and iron level to the diadust obtained, and test result is: the content≤5ppm of cobalt, the content≤10ppm of manganese, the content≤5ppm of iron.
The invention provides a kind for the treatment of process of diadust, comprise the following steps: pending diadust is carried out alkaline purification, obtain alkaline purification diadust; Alkaline purification diadust is carried out HCl treatment and logical ozone, obtain diadust intermediate; Described diadust intermediate is carried out drying, obtains diadust.By logical ozonize during disposal methods process diadust provided by the invention, avoid the use of acid with strong oxidizing property, saved cost, decrease the pollution to environment.In addition, the impurities from diamond micro powder content that obtains of the present invention is lower.Experimental result shows: the content≤5ppm of cobalt in the diadust that disposal methods provided by the invention obtains, the content≤10ppm of manganese, the content≤5ppm of iron.
In order to further illustrate the present invention, being described in detail below in conjunction with the treatment process of embodiment to a kind of diadust provided by the invention, but they can not being interpreted as limiting the scope of the present invention.
Embodiment 1
By 500ct, (content of cobalt is 100ppm, the content of iron is 144ppm, the content of manganese is 55ppm) granularity is that the pending diadust of 2 μm ~ 4 μm and sodium hydroxide put into Stainless Steel Crucible according to the mass ratio of 1:3,800 DEG C are boiled 2 hours, obtain alkaline purification diadust;
Alkaline purification diadust is cooled, takes out and be no less than 3 times by washed with de-ionized water;
Alkaline purification diadust after cleaning is put into beaker, and add according to the mass ratio of 1:3 the hydrochloric acid that massfraction is 38%, stir, stirring velocity is 180 revs/min, 100 DEG C boil after start to pass into ozone, the concentration of ozone is 10mg/L, the gas flow of ozone is 100mL/min, take out after 4 hours, and be no less than 5 times by washed with de-ionized water, obtain diadust intermediate;
The diadust intermediate obtained is put into baking oven dry, take out after dry 6 hours at 80 DEG C, obtain diadust.
The present invention's testing method according to technique scheme measures the foreign matter content on diadust surface, and measuring result is: the content≤5ppm of cobalt, the content≤5ppm of manganese, and the content≤5ppm of iron, does not detect graphite-phase.
Embodiment 2
By 500ct, (content of cobalt is 150ppm, the content of iron is 124ppm, the content of manganese is 60ppm) granularity is that the pending diadust of 5 ~ 10 μm and sodium hydroxide put into Stainless Steel Crucible according to the mass ratio of 1:3,800 DEG C are boiled 2 hours, obtain alkaline purification diadust;
Alkaline purification diadust is cooled, takes out and be no less than 3 times by washed with de-ionized water;
Alkaline purification diadust after cleaning is put into beaker, and add according to the mass ratio of 1:3 the hydrochloric acid that massfraction is 36%, stir, stirring velocity is 180 revs/min, 100 DEG C boil after start to pass into ozone, the concentration of ozone is 20mg/L, the gas flow of ozone is 500mL/min, take out after 1 hour, and be no less than 5 times by washed with de-ionized water, obtain diadust intermediate;
The diadust intermediate obtained is put into baking oven and carries out drying, take out after dry 3.5 hours at 120 DEG C, obtain diadust.
The present invention's testing method according to technique scheme measures the foreign matter content on diadust surface, and measuring result is: the content≤5ppm of cobalt, the content≤10ppm of manganese, and the content≤5ppm of iron, does not detect graphite-phase.
Embodiment 3
By 500ct, (content of cobalt is 122ppm, the content of iron is 140ppm, the content of manganese is 50ppm) granularity is that the pending diadust of 4 ~ 8 μm and sodium hydroxide put into Stainless Steel Crucible according to the mass ratio of 1:3,800 DEG C are boiled 2 hours, obtain alkaline purification diadust;
Cool out diadust taking-up and be no less than 3 times by washed with de-ionized water;
Diadust after cleaning is put into beaker, and add according to the mass ratio of 1:3 the hydrochloric acid that massfraction is 37%, stir, stirring velocity is 180 revs/min, 100 DEG C boil after start to pass into ozone, the concentration of ozone is 30mg/L, the gas flow of ozone is 1000mL/min, take out after 30 hours, and be no less than 5 times by washed with de-ionized water, obtain diadust intermediate;
The diadust intermediate obtained is put into baking oven and carries out drying, take out after dry 4 hours at 100 DEG C, obtain diadust.
The present invention is testing method according to technique scheme, and measure the foreign matter content on diadust surface, test result is: the content≤5ppm of cobalt, the content≤10ppm of manganese, and the content≤5ppm of iron, does not detect graphite-phase.
As seen from the above embodiment, the invention provides a kind for the treatment of process of diadust, comprise the following steps: pending diadust is carried out alkaline purification, obtain alkaline purification diadust; Alkaline purification diadust is carried out HCl treatment and logical ozone, obtain diadust intermediate; Described diadust intermediate is carried out drying, obtains diadust.By logical ozonize during disposal methods diadust provided by the invention, avoid the use of acid with strong oxidizing property, saved cost, decrease the pollution to environment.In addition, the foreign matter content of diadust that obtains of process of the present invention is lower.Experimental result shows: the content≤5ppm of cobalt in the diadust that disposal methods provided by the invention obtains, the content≤10ppm of manganese, the content≤5ppm of iron.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.

Claims (10)

1. a treatment process for diadust, comprises the following steps:
Pending diadust is carried out alkaline purification, obtains alkaline purification diadust;
Described alkaline purification diadust is carried out HCl treatment and logical ozone, obtains diadust intermediate;
Described diadust intermediate is carried out drying, obtains diadust.
2. treatment process according to claim 1, is characterized in that, described alkaline purification adopts alkaline matter;
Described alkaline matter comprises sodium hydroxide and/or potassium hydroxide.
3. treatment process according to claim 2, is characterized in that, the mass ratio of described pending diadust and alkaline matter is 1:2.8 ~ 3.3.
4. treatment process according to claim 1, is characterized in that, the temperature of described alkaline purification is 780 DEG C ~ 830 DEG C.
5. treatment process according to claim 1, is characterized in that, the time of described alkaline purification is 1.5h ~ 2.5h.
6. treatment process according to claim 1, is characterized in that, mass ratio 1:2.8 ~ 3.3 of described alkaline purification diadust and hydrochloric acid.
7. treatment process according to claim 1, is characterized in that, the temperature of described logical ozone is 95 DEG C ~ 105 DEG C.
8. treatment process according to claim 1, is characterized in that, the time of described logical ozone is 1h ~ 30h.
9. treatment process according to claim 1, is characterized in that, the mass concentration of the ozone adopted during described logical ozone is 20mg/L ~ 25mg/L.
10. treatment process according to claim 1, is characterized in that, the temperature of described drying is 60 DEG C ~ 150 DEG C;
The time of described drying is 1h ~ 8h.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271218A (en) * 2015-10-28 2016-01-27 山田研磨材料有限公司 Production method of diamond micro-powder
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
CN109305676A (en) * 2018-11-26 2019-02-05 南京金瑞立丰硬质材料科技有限公司 The minimizing technology of graphitic carbon in a kind of nano diamond ash material being simple and efficient
CN111620336A (en) * 2020-06-09 2020-09-04 三门峡天钻晶体材料有限公司 Diamond micro powder, method and equipment for cleaning diamond single crystal

Citations (3)

* Cited by examiner, † Cited by third party
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
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
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
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

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105271218A (en) * 2015-10-28 2016-01-27 山田研磨材料有限公司 Production method of diamond micro-powder
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
CN109305676A (en) * 2018-11-26 2019-02-05 南京金瑞立丰硬质材料科技有限公司 The minimizing technology of graphitic carbon in a kind of nano diamond ash material being simple and efficient
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
CN111620336A (en) * 2020-06-09 2020-09-04 三门峡天钻晶体材料有限公司 Diamond micro powder, method and equipment for cleaning diamond single crystal
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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