CN113772670A - Preparation method of nano-diamond dispersion liquid - Google Patents
Preparation method of nano-diamond dispersion liquid Download PDFInfo
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- CN113772670A CN113772670A CN202111131002.0A CN202111131002A CN113772670A CN 113772670 A CN113772670 A CN 113772670A CN 202111131002 A CN202111131002 A CN 202111131002A CN 113772670 A CN113772670 A CN 113772670A
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- 239000002113 nanodiamond Substances 0.000 title claims abstract description 80
- 239000006185 dispersion Substances 0.000 title claims abstract description 34
- 239000007788 liquid Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 27
- 150000003839 salts Chemical class 0.000 claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 25
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 18
- 239000010432 diamond Substances 0.000 claims abstract description 18
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 17
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 9
- 238000010306 acid treatment Methods 0.000 claims abstract description 8
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 230000004048 modification Effects 0.000 claims abstract description 4
- 238000012986 modification Methods 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 14
- 239000000725 suspension Substances 0.000 claims description 14
- 235000011164 potassium chloride Nutrition 0.000 claims description 11
- 239000001103 potassium chloride Substances 0.000 claims description 11
- 239000011780 sodium chloride Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims 3
- 239000007864 aqueous solution Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 12
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 12
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 11
- 235000011941 Tilia x europaea Nutrition 0.000 description 11
- 239000004571 lime Substances 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 239000002253 acid Substances 0.000 description 6
- 229910001573 adamantine Inorganic materials 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- ORILYTVJVMAKLC-UHFFFAOYSA-N adamantane Chemical compound C1C(C2)CC3CC1CC2C3 ORILYTVJVMAKLC-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000011325 microbead Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011324 bead Substances 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005474 detonation Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000004176 ammonification Methods 0.000 description 1
- 230000021523 carboxylation Effects 0.000 description 1
- 238000006473 carboxylation reaction Methods 0.000 description 1
- 125000003636 chemical group Chemical group 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 201000007750 congenital bile acid synthesis defect Diseases 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the field of diamond dispersion liquid, and particularly relates to a preparation method of nano diamond dispersion liquid. The method comprises the following steps: (1) carrying out acid treatment on the agglomerated nano-diamond to realize carboxyl modification on the surface of the diamond and obtain a carboxyl modified diamond; (2) carrying out planetary grinding on the carboxyl modified diamond in a saturated salt solution containing salt crystals, and deagglomerating the agglomerated diamond under the grinding action of the salt crystals; (3) dissolving salt crystal after planetary grinding, separating solid from liquid, and re-dispersing with solvent. The preparation method of the nano-diamond dispersion liquid can not introduce pollutants which cannot be removed or are difficult to remove into the final nano-diamond; and due to the collision effect during sanding and the dissolution-precipitation process of salt crystals in the aqueous solution, the desired size similarity of the grinding media (salt crystals) and the nanodiamond agglomerates is maintained, thereby maintaining the processing efficiency at a stable value throughout.
Description
Technical Field
The invention belongs to the field of diamond dispersion liquid, and particularly relates to a preparation method of nano diamond dispersion liquid.
Background
The nano-diamond has the excellent characteristics of high hardness, high thermal conductivity, high surface activity, good chemical stability, regular appearance, no toxicity, good biocompatibility and the like. These characteristics make it widely used in the fields of machinery, energy, materials and biomedicine.
However, the detonation method of nanodiamonds is particularly easy to form agglomerates, and the agglomerates are difficult to deagglomerate by conventional methods such as ultrasound, ball milling, etc. The difficulty in deagglomeration may be due to the abundance of chemical groups on the surface of the nanodiamond. The surface of the nano-diamond has various surface functional groups, such as carboxyl, hydroxyl, lactone and the like, and the functional groups can cause multiple hydrogen bonds and even covalent bonds to be formed between adjacent nano-diamond particles, so that the nano-diamond particles are difficult to de-agglomerate. The strong agglomerates severely limit many potential uses of nanodiamonds.
Since the conventional dispersion technique is not effective for deagglomeration of nanodiamonds, a specific deagglomeration technique has been developed. In order to obtain monodisperse nano-diamond particles, the commonly used nano-diamond deagglomeration technology in the industry at present is mainly a bead-assisted ultrasonic deagglomeration technology (BASD), and the prior art such as CN105452164A, CN105531228A, CN106536407A and the like respectively obtain single-particle nano-diamond dispersions of carboxylation, hydrogenation and ammonification by using the method.
In the BASD technique, high-density zirconia micro-beads are propelled by energy generated by cavitation to collide and crush the nanodiamond aggregate trapped between two zirconia micro-beads, thereby obtaining a monodisperse nanodiamond colloid. However, the zirconia microspheres wear during this process and occasionally break down, leaving zirconia contaminants in the nanodiamond dispersion that are difficult to remove. Although zirconia contamination is considered non-toxic, the difficulty of controlling residual amounts and removing from the nanodiamond dispersion reduces the likelihood that BASD-produced nanodiamond is approved by clinical medicine. Meanwhile, expensive zirconia beads are used as grinding media in the BASD technology, so that additional cost is increased. Moreover, after the nano-diamond aggregate is reduced from micron level to 50-30nm by the BASD technology, the nano-diamond aggregate is smaller and smaller due to grinding, the difference of grinding micro-beads on the size of the aggregate is larger and larger, and the efficiency of the processing process is reduced.
Disclosure of Invention
An object of the present invention is to provide a method for preparing a nanodiamond dispersion liquid without introducing contaminants that cannot be removed or are difficult to remove into the final nanodiamond.
In order to achieve the above purpose, the technical scheme of the preparation method of the nano-diamond dispersion liquid is as follows:
a method for preparing a nanodiamond dispersion liquid comprises the following steps:
(1) carrying out acid treatment on the agglomerated nano-diamond to realize carboxyl modification on the surface of the diamond and obtain a carboxyl modified diamond;
(2) carrying out planetary grinding on the carboxyl modified diamond in a saturated salt solution containing salt crystals, and deagglomerating the agglomerated diamond under the grinding action of the salt crystals;
(3) dissolving salt crystal after planetary grinding, separating solid from liquid, and re-dispersing with solvent.
The preparation method of the nano-diamond dispersion liquid can not introduce pollutants which cannot be removed or are difficult to remove into the final nano-diamond; and due to the collision effect during sanding and the dissolution-precipitation process of salt crystals in the aqueous solution, the desired size similarity of the grinding media (salt crystals) and the nanodiamond agglomerates is maintained, thereby maintaining the processing efficiency at a stable value throughout. The monodisperse nanodiamond dispersion liquid obtained by the method has more obvious advantages particularly in biomedical application.
Preferably, in the step (1), the average particle size of the agglomerated nano-diamond is 150-200 nm.
In view of cost, it is preferable that the salt crystals and the salt in the saturated salt solution in step (2) are the same type and are sodium chloride or potassium chloride. More preferably, 5 parts of the agglomerated nanodiamond is used in an amount corresponding to 100 parts of salt and 20 parts of water.
Preferably, in the step (2), the ball milling is planetary ball milling, the rotating speed of the planetary ball milling is controlled at 1000r/min, 20min of planetary ball milling is performed each time, the planetary ball milling is kept for 20min and is cooled, and the total working time of the planetary ball milling is 1-1.5 h.
Providing a more convenient way to obtain a mixed solution convenient for ball milling, preferably, in step (2), constructing a mixed solution in which a saturated salt solution, salt crystals and carboxyl modified diamond exist by the following method: grinding salt and carboxyl modified diamond, adding water and ultrasonically stirring to obtain a uniformly mixed suspension; subjecting the suspension to the planetary mill. More preferably, the ultrasonic power of the ultrasonic stirring is 500-1500W, and the frequency is 40 kHz; the stirring speed is 500-800 r/min.
Preferably, in the step (3), the salt crystals are dissolved by adding water to the system. The amount of water added is sufficient to dissolve the salt crystals in the system.
Preferably, in step (3), the solvent used for the redispersion is water. More preferably, 100 parts of the agglomerated nanodiamond is used in an amount of 12 parts with respect to water.
Drawings
FIG. 1 is a raw material particle size distribution diagram of an agglomerated state nanodiamond;
fig. 2 is a particle size distribution diagram of a monodisperse nanodiamond dispersion obtained by the method of example 1 of the present invention.
Detailed Description
In the invention, a new, efficient and cheap technology is adopted to obtain the nano-diamond colloidal dispersion which is monodisperse in water.
The agglomerated nano diamond is nano diamond black powder obtained by primarily purifying nano diamond obtained by a detonation method.
In the step (1), the prior art can be referred to for the modification mode of obtaining carboxyl-rich groups on the surface by acid treatment. Preferably, in the step (1), the acid treatment is a mixed acid composed of nitric acid, sulfuric acid and perchloric acid, and the volume ratio of the nitric acid to the sulfuric acid to the perchloric acid in the mixed acid is 1.5: 15: 2.5. the amount of the agglomerated nano-diamond corresponding to each liter of mixed acid is 2500ct, and the nano-diamond lime powder rich in carboxyl is obtained after acid treatment.
The following examples are provided to further illustrate the practice of the invention.
The specific examples of the method for preparing the nanodiamond dispersion liquid of the present invention are as follows:
example 1
The method for preparing the nano-diamond dispersion liquid of the embodiment comprises the following steps:
(1) nano-diamond lime powder (agglomerated nano-diamond with the average particle size of 170nm) is used as a raw material, carboxyl groups are enriched on the surface of the nano-diamond lime powder after the treatment of nitric acid, sulfuric acid and perchloric acid, and the particle size distribution diagram of the raw material is shown in figure 1.
The volume ratio of nitric acid, sulfuric acid and perchloric acid in the acid treatment is 1.5: 15: 2.5. the dosage of the agglomerated nano-diamond corresponding to each liter of mixed acid is 2500 ct.
(2) 100 parts of analytically pure sodium chloride crystals and 5 parts of the nanodiamond powder obtained in step (1) were weighed, ground using a mortar, and preliminarily mixed.
(3) Adding the preliminarily mixed nano-adamantine lime powder and sodium chloride crystals into a glass beaker, adding 20 parts of water, and carrying out ultrasonic stirring to uniformly mix the nano-adamantine lime powder, the sodium chloride crystals and the sodium chloride crystals, wherein the ultrasonic power is 1000W, the frequency is 40kHz, the stirring speed is 500rpm, and the ultrasonic time is 30min to obtain a uniformly mixed suspension, and a sodium chloride saturated aqueous solution, the sodium chloride crystals and the nano-adamantine lime powder are stored in the suspension;
(4) and (4) putting the uniformly mixed suspension in the step (3) into a polytetrafluoroethylene tank, carrying out planetary grinding, controlling the rotating speed of the planetary grinding to be 1000r/min, and keeping the planetary grinding for 20min for liquid cooling in order to prevent water evaporation caused by serious process heating, wherein the total time of the planetary grinding is 1 h.
(5) Adding 1500 parts of water into the suspension obtained in the step (4), ultrasonically stirring to completely dissolve sodium chloride crystals, wherein the ultrasonic power is 1000W, the frequency is 40kHz, stirring is carried out at 300rpm to obtain a nano-diamond suspension, centrifuging by using a high-speed refrigerated centrifuge, the rotating speed of the centrifuge is 6000r/min, the centrifuging time is 30min, and pouring out the upper clear sodium chloride solution after centrifuging;
the nano-diamond abrasive at the bottom of the centrifuge cup is redispersed in 1500 parts of aqueous solution in an ultrasonic stirring mode (the ultrasonic power is 1000W, the frequency is 40kHz), the upper yellowish sodium chloride solution is poured out after the centrifugation is carried out again, the rotating speed of the centrifuge is 11000r/min and 60min, 12 parts of water is added into the abrasive at the bottom of the centrifuge cup, the abrasive is uniformly dispersed by ultrasonic stirring (the ultrasonic power is 1000W, the frequency is 40kHz, and the rotating speed is 500rpm), and a monodisperse nano-diamond dispersion liquid is obtained, wherein the particle size distribution of the monodisperse nano-diamond dispersion liquid is shown in figure 2.
As can be seen by comparing with the attached drawings, the parameters of the average particle size and the like in FIG. 1 are 170 nm. In FIG. 2, the average particle size and other parameters were 25 nm.
Example 2
(1) Nano-diamond lime powder (agglomerated nano-diamond with the average particle size of 100nm) is used as a raw material, and the surface of the nano-diamond lime powder is treated by nitric-sulfuric mixed acid and perchloric acid to be rich in carboxyl groups.
The volume ratio of nitric acid, sulfuric acid and perchloric acid in the acid treatment is 1.5: 15: 2.5. the dosage of the agglomerated nano-diamond corresponding to each liter of mixed acid is 2500 ct.
(2) 100 parts of analytically pure potassium chloride crystals and 5 parts of the nanodiamond powder obtained in step (1) were weighed, and ground using a mortar to preliminarily mix them.
(3) Adding the preliminarily mixed nano-scale adamantine lime powder and potassium chloride crystals into a glass beaker, adding 20 parts of water, and carrying out ultrasonic stirring to uniformly mix the nano-scale adamantine lime powder, the potassium chloride crystals and the potassium chloride crystals, wherein the ultrasonic power is 1000W, the frequency is 40kHz, the stirring speed is 800r/min, and the ultrasonic time is 1 hour to obtain a uniformly mixed suspension, and a saturated aqueous solution of potassium chloride, the potassium chloride crystals and the nano-scale adamantine lime powder are stored in the suspension;
(4) and (4) putting the uniformly mixed suspension in the step (3) into a polytetrafluoroethylene tank, carrying out planetary grinding, controlling the rotating speed of the planetary grinding to be 1000r/min, and keeping the planetary grinding for 20min for each planetary grinding for liquid cooling, wherein the total working time of the planetary grinding is 1.2h, so as to prevent water evaporation caused by serious process heating.
(5) Adding 1500 parts of water into the suspension obtained in the step (4), ultrasonically stirring to completely dissolve potassium chloride crystals, wherein the ultrasonic power is 1000W, the frequency is 40kHz, stirring is carried out at 300rpm to obtain a nano-diamond suspension, centrifuging by using a high-speed refrigerated centrifuge, the rotating speed of the centrifuge is 6000r/min, the centrifuging time is 30min, and pouring out the upper clear potassium chloride solution after centrifuging;
the nano-diamond abrasive at the bottom of the centrifugal cup is redispersed in 1500 parts of aqueous solution in an ultrasonic stirring mode (the ultrasonic power is 1000W, the frequency is 40kHz), the yellowish potassium chloride solution at the upper layer is poured out after the centrifugation is carried out again, the rotating speed of the centrifuge is 11000r/min and 60min, 12 parts of water is added into the abrasive at the bottom of the centrifugal cup, the abrasive is uniformly dispersed by ultrasonic stirring (the ultrasonic power is 1000W, the frequency is 40kHz and the rotating speed is 400rpm), and monodisperse nano-diamond dispersion liquid is obtained, wherein the average particle size of the monodisperse nano-diamond dispersion liquid is 18 nm.
Claims (10)
1. A method for preparing a nanodiamond dispersion liquid is characterized by comprising the following steps:
(1) carrying out acid treatment on the agglomerated nano-diamond to realize carboxyl modification on the surface of the diamond and obtain a carboxyl modified diamond;
(2) carrying out planetary grinding on the carboxyl modified diamond in a saturated salt solution containing salt crystals, and deagglomerating the agglomerated diamond under the grinding action of the salt crystals;
(3) dissolving salt crystal after planetary grinding, separating solid from liquid, and re-dispersing with solvent.
2. The method of preparing the nanodiamond dispersion liquid according to claim 1, wherein in the step (1), the average particle size of the agglomerated nanodiamond is 150 to 200 nm.
3. The method of preparing a nanodiamond dispersion liquid according to claim 1, wherein in the step (2), the salt crystal and the salt in the saturated salt solution are the same type and are sodium chloride or potassium chloride.
4. The method of preparing a nanodiamond dispersion liquid according to claim 3, wherein in the step (2), 5 parts of the agglomerated nanodiamond is used in an amount corresponding to 100 parts of salt and 20 parts of water.
5. The method for preparing a nanodiamond dispersion liquid according to claim 1, wherein in the step (2), the ball milling is planetary ball milling, the rotational speed of the planetary ball milling is controlled at 1000r/min, 20min is performed for each planetary ball milling, the planetary ball milling is kept for 20min and then cooled, and the total working time of the planetary ball milling is 1-1.5 h.
6. The method for producing a nanodiamond dispersion liquid according to any one of claims 1 to 5, wherein in the step (2), a mixed liquid in which a saturated salt solution, salt crystals, and carboxyl-modified diamond exist is constructed by: grinding salt and carboxyl modified diamond, adding water and ultrasonically stirring to obtain a uniformly mixed suspension; subjecting the suspension to the planetary mill.
7. The method for preparing the nano-diamond dispersion liquid according to claim 6, wherein the ultrasonic power of the ultrasonic stirring is 500-1500W, and the frequency is 40 kHz; the stirring speed is 500-800 r/min.
8. The method for producing a nanodiamond dispersion liquid according to claim 1, wherein in the step (3), the salt crystal is dissolved by adding water to the system.
9. The method for producing a nanodiamond dispersion liquid according to claim 1, wherein the solvent used in the re-dispersion in the step (3) is water.
10. The method of producing a nanodiamond dispersion liquid according to claim 9, wherein the amount of water used is 12 parts per 100 parts of the agglomerated nanodiamond.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114686171A (en) * | 2022-05-19 | 2022-07-01 | 中国振华集团云科电子有限公司 | Suspensible diamond grinding fluid and preparation process thereof |
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Application publication date: 20211210 |