CN105692609B - The method of the preferable Nano diamond preparation of liquid suspension stability - Google Patents
The method of the preferable Nano diamond preparation of liquid suspension stability Download PDFInfo
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- CN105692609B CN105692609B CN201610070519.6A CN201610070519A CN105692609B CN 105692609 B CN105692609 B CN 105692609B CN 201610070519 A CN201610070519 A CN 201610070519A CN 105692609 B CN105692609 B CN 105692609B
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- nano diamond
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- 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
Abstract
The invention discloses a kind of methods of the preferable Nano diamond preparation of liquid suspension stability, it is characterized in that, method includes the following steps: step 1, chooses Nano diamond powder and is put into reaction vessel, the water of deionization is added into reaction vessel, obtains mixed solution；Above-mentioned mixed solution is put into ultrasonic disperser by step 2, and Nano diamond aqueous solution is obtained after ultrasonic disperser is processed；Ethylenediaminetetraacetic acid EDTA is added in Xiang Shangshu diamond aqueous solution for step 3；Step 4 isolates the sediment of needs by centrifugation.Step 5 by obtain sediment heat under vacuum conditions be concentrated into it is powdered.The surface impurity for the nanodiamond particle that water, drying and reduction can be added to obtain repeatedly can be reduced increasingly.The invention has the advantages that the Nano diamond particle with preferable liquid suspension stability can be selected effectively.
Description
Technical field
The present invention relates to Nano diamond field of material technology, especially a kind of preferable nanogold of liquid suspension stability
The method of hard rock preparation.It is project of the invention that obtaining, which has the Nano diamond of the high technology of new features, and new features are can
To form the hydrosol with higher liquid suspension and more high technology quality
Background technique
The known method that diamond is separated from decentralized medium by injecting electrolyte, the ingredient of electrolyte are adsorbed on Buddha's warrior attendant
The surface of stone, on the one hand, draw impurity and simultaneously solidify, on the other hand, allow the Buddha's warrior attendant for having higher sedimentation stability in clear solution
Stone reveals.
This method is characterized in, will cause a large amount of losses of diamond in supernatant liquid, and since sediment is prolonged
Precipitating is without having enough yield
Most efficiently method uses ultrasonic scattering method double to the dispersion diamond nano particle having proposed in liquid
Dispersion powders in distilled water are added concentration in the electrolyte of 10-2-10-4, then dilute water dispersion.
The shortcoming of this method is, using the nanoparticle suspension and electrolytic solution of Cmin, and lacks and sinks
The process for dropping separation and the drying of stable dispersion, can not obtain dry Nano diamond powder and study its performance.
Summary of the invention
The purpose of the present invention is to solve the above problems, devise a kind of preferable nanometer Buddha's warrior attendant of liquid suspension stability
Standby method made of stones.
Realize above-mentioned purpose the technical scheme is that, a kind of preferable Nano diamond preparation of liquid suspension stability
Method, which is characterized in that method includes the following steps:
Step 1 is chosen Nano diamond powder and is put into reaction vessel, the water of deionization is added into reaction vessel, obtains
To mixed solution；
Above-mentioned mixed solution is put into ultrasonic disperser by step 2, is received after ultrasonic disperser is processed
Rice diamond aqueous solution, ultrasonic dispersing time 3-8 minutes；
Ethylenediaminetetraacetic acid EDTA concentration is added in Xiang Shangshu diamond aqueous solution and reaches 0.015-0.5 mol/ for step 3
L.；
Step 4 is put into centrifugal device and handles 2-10 minutes under the action of 3000-15000 revs/min of centrifugal force；
Step 5, by obtain sediment heat under vacuum conditions be concentrated into it is powdered；
Step 6 repeats step 1 to step 5 and multiple.
Using the method for the preferable Nano diamond preparation of liquid suspension stability that technical solution of the present invention makes, lead to
It crosses the introducing electrolyte in suspension and obtains the Nano diamond with higher liquid suspension stability, water is then added, sufficiently
Stirring, isolates the hydrosol, and finally dehydration obtains Nano diamond powder.
Detailed description of the invention
Fig. 1 is the impurity content percentage table of the Nano diamond powder after of the present invention initial and processing；
Fig. 2 is of the present invention in the case where initial conditions are all different, is had using the Nano diamond that this method obtains
Some effective performances are referring to table.
Specific embodiment
1 pair of the embodiment of the present invention is specifically described with reference to the accompanying drawing；
The Nano diamond powder that explosion synthesis is extracted in 1. laboratory of case, extracts lot number No.11.With y З Д Т
The suspension that mass concentration 2% is made in 2T type (Russia) ultrasonic disperse equipment adds ethylenediaminetetraacetic acid into suspension and reaches
With 6000 revs/min, centrifuge separation should in 3 minutes using Beckman J21B (U.S.) centrifuge by concentration 0.015-0.5mol/L.
Mixture remove supermatant fluid, into sediment add water and stir using Beckman J21B centrifuge with 15000 revs/min
Be centrifugated the mixture in 10 minutes, obtain supermatant fluid (nanodiamond suspension) and sediment collection suspension and
The content that formulates remaining water according to demand is dried in Unipan 350P (Poland) vacuum rotary evaporator, to obtain concentration
The intermediate products of suspension, filter residue or black powder form is similarly by sediment in vacuum spin chuck evaporator Unipan
It is dried in 350P, obtains particle distribution 40-45% in bright powder suspension, the particle distribution 55- in sediment
60%.
The Nano diamond powder that explosion synthesis is extracted in 2. laboratory of case, extracts lot number No.7.With y З Д Т 2T
The suspension that mass concentration 1% is made in type (Russia) ultrasonic disperse equipment adds ethylenediaminetetraacetic acid into suspension up to dense
Degree 0.125mol/L. is centrifugated the mixing using Beckman J21B (U.S.) centrifuge with 10000 revs/min in 3 minutes
Object is thrown uses Beckman J21B centrifuge with 15000 revs/min at 10 points except supermatant fluid adds water into sediment and stirs
The mixture is centrifugated in clock, obtain supermatant fluid (nanodiamond suspension) and sediment collection suspension and
Be dried in Unipan 350P (Poland) turntable evaporator according to the content of remaining water obtain concentrated suspension liquid, filter residue or
Similarly sediment is dried in vacuum spin chuck evaporator Unipan 350P by black dry powder, and it is outstanding to obtain bright powder
Original powder nanometer particle appears up to 65 ± 3%. in supernatant liquid
Case 3. extracts lot number 7 in the Nano diamond powder that Peter Krass Noah Er Sike scientific center synthesizes, and uses
The suspension that mass concentration 1% is made in y З Д Т 2T type (Russia) ultrasonic disperse equipment adds ethylenediamine tetraacetic into suspension
Acetic acid is up to concentration 0.125mol/L. using Beckman J21B (U.S.) centrifuge with 10000 revs/min of centrifugations point in 3 minutes
From mixture throw except supermatant fluid add water into sediment and stir use Beckman J21B centrifuge with 15000 turns/
Divide and is centrifugated mixture acquirement supermatant fluid (nanodiamond suspension) and sediment collection suspension in 10 minutes
And is dried in Unipan 350P (Poland) turntable evaporator, concentrated suspension liquid, filter residue are obtained according to the content of remaining water
Or similarly sediment is dried in vacuum spin chuck evaporator Unipan 350P by black dry powder, obtains bright powder
Original powder nanometer particle 50 ± 5%. in last suspension
Case 4. is extracted super in the Nano diamond powder of " Altay " (than this gram) federal research and production center synthesis
The suspension of mass concentration 1% is made to outstanding with y З Д Т 2T type (Russia) ultrasonic disperse equipment in frangible diamond-C
Ethylenediaminetetraacetic acid is added in supernatant liquid uses Beckman J21B (U.S.) centrifuge with 3000 up to concentration 0.015-0.5mol/L.
It it rev/min is centrifugated mixture in 2 minutes throws and use Beckman except supermatant fluid add water into sediment and stirs
J21B centrifuge is centrifugated mixture in 10 minutes with 15000 revs/min and obtains supermatant fluid (nanodiamond suspension)
Suspension is collected with sediment and is dried according to the content of remaining water in Unipan 350P (Poland) turntable evaporator
It obtains concentrated suspension liquid, filter residue or black dry powder equally sediment is dried, obtains the grain of bright powder suspension
Subnumber is 70 ± 5%.
Lot number super frangible diamond-C nano of the case 5. in " Altay " (than this gram) federal research and production center synthesis
Diamond dry powder, in 1:4 ratio add ethylenediaminetetraacetic acid to concentration 0.5mol/L. using Beckman J21B (U.S.) from
Scheming is centrifugated mixture and thrown with 3000 revs/min in 2 minutes to be made except supermatant fluid adds water into sediment and stirs
It is centrifugated the mixture in 10 minutes with 15000 revs/min with Beckman J21B centrifuge, obtains supermatant fluid (nanogold
Hard rock suspension) and sediment collect suspension and be dried in Unipan 350P (Poland) turntable evaporator according to
The content of remaining water obtains concentrated suspension liquid, filter residue or black dry powder and equally sediment is dried, and obtains bright powder
The population of last suspension is 70 ± 5%.
Although the initial condition in above-mentioned classification case is all different, have with the Nano diamond that the method proposed obtains
All effective performance (referring to Fig. 2)
Above-mentioned technical proposal only embodies the optimal technical scheme of technical solution of the present invention, those skilled in the art
The principle of the present invention is embodied to some variations that some of them part may be made, belongs to the scope of protection of the present invention it
It is interior.
Claims (3)
1. a kind of method of the preferable Nano diamond preparation of liquid suspension stability, which is characterized in that this method includes following
Step:
Step 1 is chosen Nano diamond powder and is put into reaction vessel, the water of deionization is added into reaction vessel, is mixed
Close solution；
Above-mentioned mixed solution is put into ultrasonic disperser by step 2, obtains nanogold after ultrasonic disperser is processed
Hard rock aqueous solution；
Ethylenediaminetetraacetic acid EDTA concentration is added in Xiang Shangshu diamond aqueous solution and reaches 0.015-0.5mol/L for step 3；
Step 4 isolates sediment by centrifugation；
Step 5, by obtain sediment heat under vacuum conditions be concentrated into it is powdered；
Step 6 repeats step 1 to step 5 and multiple；
Super frangible diamond-C is extracted in the Nano diamond powder of Altay federation research and production center synthesis, with y З
The suspension of mass concentration 1% is made in Д Т 2T type ultrasonic disperse machine, and ethylenediaminetetraacetic acid is added into suspension and reaches concentration
0.015-0.5mol/L；It is centrifugated the mixture in 2 minutes with 3000 revs/min using Beckman J21B centrifuge, throws
Except supermatant fluid, water is added into sediment and is stirred；Using Beckman J21B centrifuge with 15000 revs/min in 10 minutes
It is centrifugated the mixture, obtains supermatant fluid and sediment, collect suspension and is carried out in Unipan 350P turntable evaporator
It is dry；Concentrated suspension liquid, filter residue or black dry powder are obtained according to the content of remaining water, equally sediment is dried, is taken
Must become clear powder；The population of suspension is 70 ± 5%.
2. the method for the preferable Nano diamond preparation of liquid suspension stability according to claim 1, which is characterized in that
The time that mixed solution is put into the interior processing of ultrasonic disperser in the step 2 is 3-8 minutes.
3. the method for the preferable Nano diamond preparation of liquid suspension stability according to claim 1, which is characterized in that
Sediment is put into centrifugal device and handles 2-5 minutes under the action of the centrifugal force of 5000g in the step 4.
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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 |
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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. |