CN105692609A - Preparation method of nano-diamond with relatively good liquid suspension stability - Google Patents
Preparation method of nano-diamond with relatively good liquid suspension stability Download PDFInfo
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- CN105692609A CN105692609A CN201610070519.6A CN201610070519A CN105692609A CN 105692609 A CN105692609 A CN 105692609A CN 201610070519 A CN201610070519 A CN 201610070519A CN 105692609 A CN105692609 A CN 105692609A
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- diamond
- nano
- liquid suspension
- nano diamond
- suspension stability
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- 239000002113 nanodiamond Substances 0.000 title claims abstract description 38
- 239000006194 liquid suspension Substances 0.000 title claims abstract description 14
- 238000002360 preparation method Methods 0.000 title abstract 5
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000002244 precipitate Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 18
- 238000005119 centrifugation Methods 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 8
- 239000010432 diamond Substances 0.000 claims description 8
- 229910003460 diamond Inorganic materials 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000002242 deionisation method Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 6
- 239000000243 solution Substances 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000008367 deionised water Substances 0.000 abstract 1
- 229910021641 deionized water Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 229960001484 edetic acid Drugs 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000000725 suspension Substances 0.000 description 30
- 239000000203 mixture Substances 0.000 description 11
- 239000012530 fluid Substances 0.000 description 10
- 239000007788 liquid Substances 0.000 description 7
- 239000006200 vaporizer Substances 0.000 description 7
- 239000000284 extract Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000008131 herbal destillate Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a preparation method of nano-diamond with relatively good liquid suspension stability. The preparation method is characterized by comprising the following steps: (1) putting selected nano-diamond powder into a reaction container, and adding deionized water into the reaction container, so as to obtain a mixed solution; (2) adding the mixed solution into an ultrasonic disperser, and processing by virtue of the ultrasonic disperser, so as to obtain a nano-diamond water solution; (3) adding ethylene dinitrilotetra-acetic acid EDTA into the nano-diamond water solution; (4) centrifugally separating required precipitates; and (5) heating and concentrating the obtained precipitates under the vacuum condition until the precipitates are powdery. According to the preparation method, the water addition, the drying and the reduction can be repeatedly carried out, and surface impurities of the obtained nano-diamond particles become less and less. The preparation method has the beneficial effect that the nano-diamond particles with relatively good liquid suspension stability can be effectively picked.
Description
Technical field
The present invention relates to Nano diamond field of material technology, a kind of method that particularly prepared by good Nano diamond of liquid suspension stability。Obtaining the problem that the Nano diamond of high technology with new features is the present invention, new features are the hydrosols that can be formed and have higher liquid suspension and more high technology quality
Background technology
Known to injecting electrolyte method of diamonds separated from disperse medium, the composition of electrolyte is adsorbed on the surface of diamond, on the one hand, draws impurity and solidifies, on the other hand, allowing the diamond of higher sedimentation stability reveal in settled solution。
The method is characterized by, can cause a large amount of losses of diamond in supernatant liquid, and not possess enough yield owing to precipitate precipitates for a long time.
The dispersion diamond nano particle having pointed out is the ultrasonic scattering method dispersed powders in DDW of way use the most efficiently in liquid, adds the concentration electrolyte at 10-2-10-4, dilution water dispersion subsequently。
The weak point of the method is, uses nanoparticle suspension and the electrolytic solution of Cmin, and lacks the scattered separation of settlement stability and dry operation, it is impossible to obtains dry Nano diamond powder and studies its performance。
Summary of the invention
The invention aims to solve the problems referred to above, devise a kind of method prepared by good Nano diamond of liquid suspension stability。
Realize above-mentioned purpose the technical scheme is that, a kind of method prepared by good Nano diamond of liquid suspension stability, it is characterised in that the method comprises the following steps:
Step one, chooses Nano diamond powder and puts into reaction vessel, add the water of deionization, obtain mixed solution in reaction vessel；
Step 2, puts in ultrasonic disperser by above-mentioned mixed solution, obtains Nano diamond aqueous solution, ultrasonic dispersing time 3-8 minute after ultrasonic disperser is processed；
Step 3, adds editic acid EDTA concentration in above-mentioned diamond aqueous solution and reaches 0.015-0.5mol/L.；
Step 4, puts into centrifugal device and processes 2-10 minute under the effect of the centrifugal force of 3000-15000 rev/min；
Step 5, acquirement precipitate is heated under vacuum be concentrated into Powdered；
Step 6, repeats step one to step 5 and repeatedly。
Utilize method prepared by the good Nano diamond of liquid suspension stability that technical scheme makes, by introducing the Nano diamond that electrolyte obtains having higher liquid suspension stability in suspension, it is subsequently adding water, it is sufficiently stirred for, isolating the hydrosol, last dehydration obtains Nano diamond powder。
Accompanying drawing explanation
Fig. 1 is the impurity content percentage ratio form of the Nano diamond powder after of the present invention initial and processing；
Fig. 2 is of the present invention when initial conditions are all different, adopts the effective performance reference table that the Nano diamond that this method obtains has。
Detailed description of the invention
Below in conjunction with accompanying drawing 1, embodiments of the invention are specifically described；
Case 1. laboratory extracts the Nano diamond powder of blast synthesis, extracts lot number No.11。Y З Д Т 2T type (Russia) ultrasonic disperse equipment is used to make the suspension of mass concentration 2%. in suspension, add editic acid reach concentration 0.015-0.5mol/L. use BeckmanJ21B (U.S.) centrifuge with 6000 revs/min of these mixture of centrifugation in 3 minutes. remove supermatant fluid, in precipitate, add water and stir. use BeckmanJ21B centrifuge with 15000 revs/min of these mixture of centrifugation in 10 minutes, obtain supermatant fluid (nanodiamond suspension) and precipitate. collect suspension and be dried in Unipan350P (Poland) vacuum rotary evaporator. formulate the content of residue water according to demand, to obtain concentrated suspension liquid, the intermediate products of filtering residue or black powder form. similarly precipitate is dried in vacuum spin chuck vaporizer Unipan350P, obtain bright powder. particle distribution 40-45% in suspension, particle distribution 55-60%. in precipitate
Case 2. laboratory extracts the Nano diamond powder of blast synthesis, extracts lot number No.7。Y З Д Т 2T type (Russia) ultrasonic disperse equipment is used to make the suspension of mass concentration 1%. in suspension, add editic acid reach concentration 0.125mol/L. use BeckmanJ21B (U.S.) centrifuge with 10000 revs/min of these mixture of centrifugation in 3 minutes. throw except supermatant fluid. in precipitate, add water and stir. use BeckmanJ21B centrifuge with 15000 revs/min of these mixture of centrifugation in 10 minutes, obtain supermatant fluid (nanodiamond suspension) and precipitate. collect suspension and be dried in Unipan350P (Poland) rotating disk vaporizer. obtain concentrated suspension liquid according to the content of residue water, filtering residue or black dry powder. similarly precipitate is dried in vacuum spin chuck vaporizer Unipan350P, obtaining bright powder. in suspension, original powder nanometer particle appears and reaches 65 ± 3%.
Case 3. extracts lot number 7 in the Nano diamond powder that Peter Krass Noah Er Sike scientific center synthesizes, y З Д Т 2T type (Russia) ultrasonic disperse equipment is used to make the suspension of mass concentration 1%. in suspension, add editic acid reach concentration 0.125mol/L. use BeckmanJ21B (U.S.) centrifuge with 10000 revs/min of these mixture of centrifugation in 3 minutes. throw except supermatant fluid. in precipitate, add water and stir. use BeckmanJ21B centrifuge with 15000 revs/min of these mixture of centrifugation in 10 minutes. acquirement supermatant fluid (nanodiamond suspension) and precipitate. collect suspension and be also dried in Unipan350P (Poland) rotating disk vaporizer. obtain concentrated suspension liquid according to the content of residue water, filtering residue or black dry powder. similarly precipitate is dried in vacuum spin chuck vaporizer Unipan350P, obtain bright powder. original powder nanometer particle 50 ± 5%. in suspension
Case 4. extracts super frangible diamond-C in the Nano diamond powder of " Altay " (than this gram) federal research and production center synthesis, y З Д Т 2T type (Russia) ultrasonic disperse equipment is used to make the suspension of mass concentration 1%. in suspension, add editic acid reach concentration 0.015-0.5mol/L. use BeckmanJ21B (U.S.) centrifuge with 3000 revs/min of these mixture of centrifugation in 2 minutes. throw except supermatant fluid. in precipitate, add water and stir. use BeckmanJ21B centrifuge with 15000 revs/min of these mixture of centrifugation in 10 minutes. acquirement supermatant fluid (nanodiamond suspension) and precipitate. collect suspension and be also dried in Unipan350P (Poland) rotating disk vaporizer. obtain concentrated suspension liquid according to the content of residue water, filtering residue or black dry powder. equally precipitate is dried, obtaining bright powder. the population of suspension is 70 ± 5%.
Case 5. is at the super frangible diamond of the lot number-C nano diamond dry powder of " Altay " (than this gram) federal research and production center synthesis, adding editic acid in the ratio of 1:4 uses BeckmanJ21B (U.S.) centrifuge with 3000 revs/min of these mixture of centrifugation in 2 minutes to concentration 0.5mol/L.. throw except supermatant fluid. and in precipitate, add water and stir. use BeckmanJ21B centrifuge with 15000 revs/min of these mixture of centrifugation in 10 minutes, obtain supermatant fluid (nanodiamond suspension) and precipitate. collect suspension and be dried in Unipan350P (Poland) rotating disk vaporizer. obtain concentrated suspension liquid according to the content of residue water, filtering residue or black dry powder. equally precipitate is dried, obtaining bright powder. the population of suspension is 70 ± 5%.
Although the initial condition in above-mentioned classification case is all different, the Nano diamond obtained by proposed method has all of effective performance (with reference to Fig. 2).
Technique scheme only embodies the optimal technical scheme of technical solution of the present invention, and some variations that some of which part is likely to make by those skilled in the art all embody principles of the invention, belong within protection scope of the present invention。
Claims (4)
1. the method that prepared by the good Nano diamond of liquid suspension stability, it is characterised in that the method comprises the following steps:
Step one, chooses Nano diamond powder and puts into reaction vessel, add the water of deionization, obtain mixed solution in reaction vessel；
Step 2, puts in ultrasonic disperser by above-mentioned mixed solution, obtains Nano diamond aqueous solution after ultrasonic disperser is processed；
Step 3, adds editic acid EDTA concentration in above-mentioned diamond aqueous solution and reaches 0.015-0.5mol/L.；
Step 4, isolates precipitate by centrifugation；
Step 5, acquirement precipitate is heated under vacuum be concentrated into Powdered；
Step 6, repeats step one to step 5 and repeatedly。
2. the method that prepared by the good Nano diamond of liquid suspension stability according to claim 1, it is characterised in that in described step 2 mixed solution put into ultrasonic disperser processing time be 3-8 minute。
3. the method that prepared by the good Nano diamond of liquid suspension stability according to claim 1, it is characterised in that in described step 3, editic acid EDTA concentration is 0.015-0.5mol/L.。
4. the method that prepared by the good Nano diamond of liquid suspension stability according to claim 1, it is characterised in that in described step 4, precipitate is put into centrifugal device and processed 2-10 minute under the effect of the centrifugal force of 3000-15000 rev/min。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610070519.6A CN105692609B (en) | 2016-03-10 | 2016-03-10 | The method of the preferable Nano diamond preparation of liquid suspension stability |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610070519.6A CN105692609B (en) | 2016-03-10 | 2016-03-10 | The method of the preferable Nano diamond preparation of liquid suspension stability |
Publications (2)
| Publication Number | Publication Date |
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| CN105692609A true CN105692609A (en) | 2016-06-22 |
| CN105692609B CN105692609B (en) | 2019-10-25 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1439451A (en) * | 2002-11-18 | 2003-09-03 | 长沙矿冶研究院 | Nano-diamond deagglomeration and grading method |
| CN1560161A (en) * | 2004-03-01 | 2005-01-05 | 长沙矿冶研究院 | Water-based nano diamond polishing solution and preparation method thereof |
| CN1695779A (en) * | 2004-05-14 | 2005-11-16 | 深圳市金刚源新材料发展有限公司 | Surface treatment method for Nano diamond fine particles added to lubricant |
| CN101007252A (en) * | 2006-01-24 | 2007-08-01 | 河南省联合磨料磨具有限公司 | Apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond and its producing method |
| CN101045829A (en) * | 2007-03-08 | 2007-10-03 | 武汉理工大学 | Diamond powder modification method and equipment |
| CN104085888A (en) * | 2014-07-17 | 2014-10-08 | 长沙矿冶研究院有限责任公司 | Method for preparing detonation nanometer diamond dispersion |
-
2016
- 2016-03-10 CN CN201610070519.6A patent/CN105692609B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1439451A (en) * | 2002-11-18 | 2003-09-03 | 长沙矿冶研究院 | Nano-diamond deagglomeration and grading method |
| CN1560161A (en) * | 2004-03-01 | 2005-01-05 | 长沙矿冶研究院 | Water-based nano diamond polishing solution and preparation method thereof |
| CN1695779A (en) * | 2004-05-14 | 2005-11-16 | 深圳市金刚源新材料发展有限公司 | Surface treatment method for Nano diamond fine particles added to lubricant |
| CN101007252A (en) * | 2006-01-24 | 2007-08-01 | 河南省联合磨料磨具有限公司 | Apparent particle size controllable ultra-fine and ultra-dispersed micropowder of nanocrystalline diamond and its producing method |
| CN101045829A (en) * | 2007-03-08 | 2007-10-03 | 武汉理工大学 | Diamond powder modification method and equipment |
| CN104085888A (en) * | 2014-07-17 | 2014-10-08 | 长沙矿冶研究院有限责任公司 | Method for preparing detonation nanometer diamond dispersion |
Non-Patent Citations (1)
| Title |
|---|
| 阚伟等: "《物理化学理论与应用研究》", 30 April 2014, 中国水利水电出版社 * |
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| CN105692609B (en) | 2019-10-25 |
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Effective date of registration: 20230801 Address after: 503, 5th floor, Building B, Tianlangyuan, Chaoyang District, Beijing, 100000 Patentee after: Beijing Junchuan New Century Trading Co.,Ltd. Address before: 533-34, No. 18 Fuyuan Road, Development Zone, Wuqing District, Tianjin, 301700 (centralized office area) Patentee before: TIANJIN DIMAI AIKE TECHNOLOGY Co.,Ltd. |
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