CN101045829A - Diamond powder modification method and equipment - Google Patents
Diamond powder modification method and equipment Download PDFInfo
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- CN101045829A CN101045829A CN 200710051630 CN200710051630A CN101045829A CN 101045829 A CN101045829 A CN 101045829A CN 200710051630 CN200710051630 CN 200710051630 CN 200710051630 A CN200710051630 A CN 200710051630A CN 101045829 A CN101045829 A CN 101045829A
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Abstract
This invention relates to modify method and modify equipment of a kind of diamond. The steps: first use mechanical and high energy ultrasonic cell disruptor to decompose micron or nanometer level diamond powder coacervate or particulate material; adopt n-butanol and oleic acid to blend chemical modified agent, adopt microwave radiation to heat chemical reactant, to carry out oil-phil and water drain chemical modification to surface of diamond powder particulate material. The equipment is a kind of modified cavity body structural microwave oven. This equipment can high speed whip modified material and carry out microwave radiation heating at the same time. The diamond powder particulate material modified by this method has no coacervate. So the dispersibility, stability, uniformity as well as dielectric compatibility all obtain prodigious advance.
Description
Technical field
The present invention relates to micron order or nano-diamond coacervate or particle surface oleophilic drainage performance chemical modification method and modification and handle used a kind of microwave oven equipment.
Background technology
Micron order or nano-diamond powder body material, not only has the same superhard characteristic of bulky diamond, also have high-specific surface area, and characteristics such as sphere or elliposoidal shape are arranged, cause micron order or nano-diamond powder body material to have good application prospects.Some applied research practices show that Nano diamond is used for the Ultraprecise polished of hard disc magnetic head, and the filler reinforcement of lubricating oil additive and plastic, rubber etc. all has good effect.Because the particular requirement of Ultraprecise polished technology generally needs to adopt non-water base polishing fluid-oil base polishing fluid.As polishing material, can reduce the roughness on polished surface with micron order or nano-diamond powder, processed substrate surface roughness reaches micron order or Subnano-class.The key problem in technology that contains the preparation of micron order or nano-diamond oil base polishing fluid is the stable dispersion of diamond particles in system.But, still undesirable in the field application situation of developing, an important reasons is exactly in these non-aqueous systems, the dispersiveness of micron order or nano-diamond, stability, degree of uniformity and also be not well solved with problems such as dielectric compatibility.
Nanoparticle surface has extremely strong activity, make its formation together that is easy to reunite have the larger-size coacervate of some weak linkage interfaces, this will reduce even eliminate the practical application effect of nano particle greatly, simultaneously because the hydrophilic oleophobic of nanoparticle surface, in organic polymer resin, be difficult to homodisperse, the space can appear on the interface, when entering the space, airborne moisture will cause the degraded of superpolymer at the interface, embrittlement, cause material property to descend, so must carry out surface modification to nanoparticle, weaken or the elimination agglomeration, improve the dispersiveness of nanoparticle in organic polymer.Present optimal method is that employing is ultrasonic or/and the vibration mill pulverization process, and micron order or nano-diamond carried out surface modification, utilize mechanical force and surfactants synergism, when pulverizing the diamond coacervate effectively, newly-generated surface in micron order or nano-diamond particle surface, the especially crushing process is modified.Separate and add polymeric dispersant in the collecting process, micron order or nano-diamond surface are carried out modification, regulate the hydrophilic and hydrophobic energy of particle surface, increase intergranular repulsive interaction, thereby realize the stable dispersion of diamond particles in oily medium or resene medium.Therefore, realize Nano diamond separate reunite and stable dispersion for bringing into play its premium properties, promote its application in some technical fields and have great importance.Therefore, in non-aqueous system, micron order or nano-diamond particulate dispersiveness, stability, degree of uniformity and be still with problems such as dielectric compatibility and be badly in need of very much improved problem.
Summary of the invention
An object of the present invention is to provide a kind of micron order or nano-diamond coacervate or granule modified method.Modification is the oleophilic drainage performance of regulating micron order or nano-diamond particle surface, improves dispersiveness, stability, degree of uniformity and and dielectric compatibility in non-aqueous system.
Another object of the present invention provides and is applicable to that micron order or nano-diamond coacervate or particle carry out the microwave oven equipment that modification is handled.Can be implemented in this microwave oven that limit microwave radiation heating edge stirs material when diamond coacervate or particle carried out the modification of oleophilic drainage performance and handle.
Diamond powder oleophilic drainage performance method of modifying step of the present invention is:
1), the diamond powder dispersion of materials is handled: with micron order or nano-diamond powder agglomerates or particulate material, use mechanical disintegration, carry out purifying treatment with concentrated nitric acid or concentrated hydrochloric acid, filter and be neutral, place ethanol or deionized water, adopt high-energy ultrasound cell pulverization machine to carry out dispersion treatment with the washed with de-ionized water, filter and with washed with de-ionized water, place ethanol to dewater again, after the drying, sub-sieve, classification are standby;
2), diamond powder material surface chemical modification is handled: get analytical pure propyl carbinol and oleic acid, mix and be uniform mixing liquid, in room temperature, under the condition of normal pressure, add the classification bortz powder powder material that step 1) obtains, stir into distributed slurry, move in the special microwave oven, use mechanical stirrer to stir slip after 1 hour, do not stopping under the agitation condition, adjust the microwave oven microwave radiation to full power microwave radiation 2～5 minutes, the low power microwave radiation heating is 25～55 minutes then, take out slip, filter, filter cake dehydrated alcohol filter wash 1～2 time, 30～80 ℃ of following dryings, promptly obtain the lipophilic-hydrophobic property diamond powder particulate material of surface chemical modification then.
Wherein said mechanical disintegration is to adopt vibration mill or ball milling or other mechanical disintegration; Oleic acid and propyl carbinol volume ratio=0,5～1 in described propyl carbinol and the oleic acid mixed solution, 3: 1,2～2,6 mixed solution, every gram micron order or nano-diamond powdered material use 20～95 milliliters of oleic acid amounts.
In above-mentioned steps 2) in, do not stopping under the agitation condition, adjust the microwave irradiation power to 700 watt of microwave oven～1300 watts microwave radiation 2～5 minutes, adjust microwave irradiation power to 50 watt～120 watts carry out microwave radiation heating 30～50 minutes then, take out slip, filter, filter cake dehydrated alcohol filter wash 1～2 time, 60 ℃ of following dryings, promptly obtain the lipophilic-hydrophobic property diamond powder particulate material of surface chemical modification then.
The equipment (seeing accompanying drawing 1) that is used for the modification of diamond powder oleophilic drainage performance among the present invention, comprise industry or household microwave oven 5, cantilever agitator 1, stir and hold in both hands 2, chemical reaction kettle 4, above the cavity center of industry or household microwave oven 5, processed a hole 3, above the hole, install cantilever agitator 1 additional, chemical reaction kettle 4 is placed in the microwave oven cavity center, stir to hold in both hands and vertically stretch in the chemical reaction kettle 4 by hole 3 by the outer top of microwave oven, stirring the handful upper end is fixed on the cantilever agitator, the electrical control system of cantilever agitator is placed in outside the microwave oven equipment in addition, and original chassis swivel arrangement is not removed and use as usual in family expenses or the industrial microwave oven body.
Above-mentioned industry or cavity of household microwave oven hit exactly diameter 2-3 centimetre of upper aperture 3, and the diameter of stirring rod is 1-2 centimetre, with microwave oven and cantilever agitator the material in the chemical reaction kettle are carried out to heat while stirring and finish chemical reaction.Stirring rod is the tetrafluoroethylene material.
The present invention adopts the carry out microwave radiation heating slip, and microwave radiation is low dose of power.After the slip heated by microwave, the oleic acid temperature reaches 100～130 ℃ very soon, and the temperature rise of slip endoparticle material is lower than oleic acid.
Utilize the microwave radiation slip that heats while stirring, particulate material under microwave radiation with propyl carbinol and elaidin reaction, oleic acid is as a kind of water-fast tensio-active agent, oleic acid molecular connects micron order or nano-diamond powder particle material, oleic hydrophilic radical at first adsorbs with particulate material, and its lipophilic group is exposed in the propyl carbinol, and so forth, therefore be adsorbed with the micron order or the nano-diamond particulate material of oleic acid molecular, easier being distributed in the organic solvent propyl carbinol.
The diamond powder particulate material that is coated with propyl carbinol and oleic acid polymkeric substance has been modified on this surface, and no coacervate exists.Therefore, the dispersiveness in non-aqueous system, stability, degree of uniformity and be greatly improved with dielectric compatibility etc.This to micron order or nano-diamond powder particle materials chemistry surface modification treatment technology, have very strong quality-advantage and modern technique advantage.
Description of drawings
The microwave oven equipment structure chart that Fig. 1 uses for the modification of diamond powder oleophilic drainage performance
Among the figure: 1 cantilever agitator, 2 stir handful, 3 holes, 4 chemical reaction kettles, 5 industry or household microwave oven.
Embodiment
The device structure that the modification of diamond powder oleophilic drainage performance is used among the following embodiment as shown in Figure 1.It is a kind of through improving the microwave oven equipment of cavity configuration.This equipment is above the cavity center of industry or household microwave oven 5, mechanical workout 2～3 centimetres of holes 3, an aperture, direction installs cantilever agitator 1 additional on hole 3, stirring handful 2 is vertically stretched in the chemical reaction kettle 4 that is placed in the microwave oven cavity center by hole 3 by the outer top of microwave oven, stir to hold in both hands and hold in both hands to tetrafluoroethylene stirs, 1～2 centimetre of diameter, stirring the handful upper end is fixed on the cantilever agitator 1, the electrical control system of agitator 1 is placed in outside the microwave oven equipment in addition, with microwave oven and stirring handful material in the chemical reaction kettle is carried out to heat while stirring and finishes chemical reaction.
Embodiment 1
The modification of coacervate nano-diamond powder oleophilic drainage performance
Operation steps is as follows:
1), the nano-diamond powdered material purifies dispersion treatment
Get 11 gram coacervate nano-diamond powdered materials, vibration mill with routine is pulverized, and places in 100 milliliters of concentrated nitric acids, stirs 60 minutes, adopt filter cloth to filter and be neutral with the washed with de-ionized water, place deionized water, adopt high-energy ultrasound cell pulverization machine to separate to reunite and handle, again with the filter cloth filtration and with washed with de-ionized water, place ethanol to dewater again, after the drying, sub-sieve, classification, thus finish nano-diamond powdered material dispersion treatment;
2), surface chemical modification
Get 500 milliliters of 250 milliliters of analytical pure oleic acid and propyl carbinols, mechanical stirring is a uniform mixing liquid in glass beaker, in room temperature, under the condition of normal pressure, the nano-diamond powder material that obtains is handled in adding through step 1), become distributed slurry with magnetic stirrer, move in the special microwave oven, use mechanical stirrer, adopt the tetrafluoroethylene stirring rod, medium speed does not stop under the condition in stirring after distributed slurry is stirred 1 hour, adjust the microwave oven microwave radiation to full power, used microwave radiation 2 minutes, the low power microwave radiation heating is 55 minutes then, takes out slip, behind vacuum filtration, with dehydrated alcohol diafiltration sample, dry sample under 60 ℃ of conditions then promptly obtains the oleophilic drainage nano-diamond particulate material of surface chemical modification.
Embodiment 2
The modification of coacervate micron order diamond powder oleophilic drainage performance
Operation steps is as follows:
1), diamond powder materials purification dispersion treatment
Get 11 gram coacervate micron order bortz powder powder materials, vibration mill with routine is pulverized, and places in 100 milliliters of concentrated nitric acids, stirs 60 minutes, adopt filter cloth to filter and be neutral with the washed with de-ionized water, place deionized water, adopt high-energy ultrasound cell pulverization machine to separate to reunite and handle, again with the filter cloth filtration and with washed with de-ionized water, place ethanol to dewater again, after the drying, sub-sieve, classification are handled thereby finish micron order diamond powder dispersion of materials;
2), surface chemical modification
Get 528 milliliters of 220 milliliters of analytical pure oleic acid and propyl carbinols, mechanical stirring is a uniform mixing liquid in glass beaker, in room temperature, under the condition of normal pressure, the micron order grade diamond powder material that obtains is handled in adding through step 1), become distributed slurry with magnetic stirrer, move in the special microwave oven, use mechanical stirrer, adopt the tetrafluoroethylene stirring rod, after medium speed stirs 1 hour to distributed slurry, do not stop under the condition in stirring, adjust microwave oven microwave irradiation power to 700 watt radiation 5 minutes, adjusting microwave irradiation power then is 120 watts, radiation 30 minutes, take out slip, behind vacuum filtration, with dehydrated alcohol diafiltration sample, then under 60 ℃ of conditions, dry sample promptly obtains the oleophilic drainage micron order diamond powder particulate material of surface chemical modification.
Embodiment 3
The modification of diamond powder surface oleophilic drainage performance
Operation steps is as follows:
1), diamond powder materials purification dispersion treatment
Get 11 gram bortz powder powder materials, vibration mill with routine is pulverized, and places in 100 milliliters of concentrated nitric acids, stirs 60 minutes, adopt filter cloth to filter and be neutral with the washed with de-ionized water, place deionized water, adopt high-energy ultrasound cell pulverization machine to separate to reunite and handle, again with the filter cloth filtration and with washed with de-ionized water, place ethanol to dewater again, after the drying, sub-sieve, classification are handled thereby finish the diamond powder dispersion of materials;
2), surface chemical modification
Get 1000 milliliters of 1000 milliliters of analytical pure oleic acid and propyl carbinols, in suitable capacity glass beaker, mechanical stirring is a uniform mixing liquid, in room temperature, under the condition of normal pressure, the bortz powder powder material that obtains is handled in adding through step 1), become distributed slurry with magnetic stirrer, move in the special microwave oven, use mechanical stirrer, adopt the tetrafluoroethylene stirring rod, medium speed does not stop under the condition in stirring after distributed slurry is stirred 1 hour, adjusts microwave oven microwave irradiation power to 700 watt radiation 5 minutes, adjusting microwave irradiation power then is 80 watts, radiation 30 minutes is taken out slip, behind vacuum filtration, with dehydrated alcohol diafiltration sample, then under 60 ℃ of conditions, dry sample promptly obtains the oleophilic drainage bortz powder powder material of surface chemical modification.
Claims (7)
1, a kind of oleophilic drainage performance method of modifying of diamond powder is characterized in that the method for modifying step is:
1) the diamond powder dispersion of materials is handled: with coacervate micron order or nano-diamond powder or particulate material, use mechanical disintegration, carry out purifying treatment with concentrated nitric acid or concentrated hydrochloric acid, filter and be neutral, place ethanol or deionized water, adopt high-energy ultrasound cell pulverization machine to carry out dispersion treatment with the washed with de-ionized water, filter and with washed with de-ionized water, place ethanol to dewater again, after the drying, sub-sieve, classification are standby;
2), diamond powder material surface chemical modification is handled: get analytical pure propyl carbinol and oleic acid, mix and be uniform mixing liquid, in room temperature, under the condition of normal pressure, add the classification bortz powder powder material that step 1 obtains, stir into distributed slurry, move in the special microwave oven, use mechanical stirrer to stir slip after 1 hour, do not stopping under the agitation condition, adjust the microwave oven microwave radiation to full power microwave radiation 2-5 minute, low power microwave radiation heating 25-55 minute then, take out slip, filter, filter cake dehydrated alcohol filter wash 1～2 time, 30～80 ℃ of following dryings, promptly obtain the lipophilic-hydrophobic property diamond powder particulate material of surface chemical modification then.
2, the oleophilic drainage performance method of modifying of diamond powder as claimed in claim 1 is characterized in that volume ratio=0,5～1 of oleic acid and propyl carbinol in described propyl carbinol and the oleic acid mixed solution, 3: 1, and 2～2,6.
3, the oleophilic drainage performance method of modifying of diamond powder as claimed in claim 1 is characterized in that every gram micron order or nano-diamond powdered material use the oleic acid amount to be the 20-95 milliliter.
4, the oleophilic drainage performance method of modifying of diamond powder as claimed in claim 1, it is characterized in that: in step 2) in, do not stopping under the agitation condition, adjust the microwave irradiation power to 700 watts-1300 watts of microwave oven, with microwave radiation 2-5 minute, adjusted microwave irradiation power to 50 watts-120 watts then carry out microwave radiation heating 30-50 minute, take out slip, filter, filter cake dehydrated alcohol filter wash 1～2 time, 50～60 ℃ of following dryings, promptly obtain the lipophilic-hydrophobic property diamond powder particulate material of surface chemical modification then.
5, the equipment that the modification of the described diamond powder oleophilic drainage of claim 1 performance is used, it is characterized in that comprising industry or household microwave oven (5), cantilever agitator (1), stir and hold in both hands (2), chemical reaction kettle (4), top, cavity center at industry or household microwave oven (5), processed a hole (3), the outer top of (3) installs cantilever agitator (1) additional in the hole, chemical reaction kettle (4) is placed in the microwave oven cavity center, stirring handful (2) is vertically stretched in the chemical reaction kettle (4) by hole (3) by the outer top of microwave oven, stirring the handful upper end is fixed on the cantilever agitator (1), the electrical control system of cantilever agitator (1) is placed in outside the microwave oven equipment in addition, and original chassis swivel arrangement is not removed and use as usual in family expenses or industrial microwave oven (5) body.
6, the equipment used of diamond powder oleophilic drainage performance as claimed in claim 5 modification, the diameter that it is characterized in that described hole (3) is 2～3 centimetres, stirring the diameter of holding in both hands (2) is 1～2 centimetre.
7, the equipment used of diamond powder oleophilic drainage performance as claimed in claim 5 modification is characterized in that described stirring holds in both hands (2) and be the tetrafluoroethylene material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100516301A CN100572457C (en) | 2007-03-08 | 2007-03-08 | Bortz powder method of modifying and modified device |
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| CNB2007100516301A CN100572457C (en) | 2007-03-08 | 2007-03-08 | Bortz powder method of modifying and modified device |
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| CN101045829A true CN101045829A (en) | 2007-10-03 |
| CN100572457C CN100572457C (en) | 2009-12-23 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531835B (en) * | 2009-04-24 | 2012-05-23 | 吉林大学 | Wollastonite powder surface wet modification method assisted by microwave |
| CN102602882A (en) * | 2011-01-21 | 2012-07-25 | 曾亚东 | High-speed centrifugal nanoparticle preparation method |
| TWI398507B (en) * | 2009-07-03 | 2013-06-11 | Kinik Co | Thermal paste with modified diamond particles and manufacture method thereof |
| CN104961945A (en) * | 2015-07-27 | 2015-10-07 | 四川理工学院 | Method for reinforcing rubber by using nano diamond powder |
| CN105004669A (en) * | 2015-07-27 | 2015-10-28 | 四川理工学院 | Method for directly measuring reinforcement mechanical properties of rubber |
| CN105131842A (en) * | 2015-10-13 | 2015-12-09 | 郑州磨料磨具磨削研究所有限公司 | Shape dressing method for nanodiamond aggregate in polishing solution |
| CN105153942A (en) * | 2015-07-28 | 2015-12-16 | 郑州磨料磨具磨削研究所有限公司 | Control method for grain size of abrasive material in nano diamond polishing solution |
| CN105692609A (en) * | 2016-03-10 | 2016-06-22 | 天津迪麦爱科科技有限公司 | Preparation method of nano-diamond with relatively good liquid suspension stability |
| CN107502003A (en) * | 2016-06-14 | 2017-12-22 | 中国科学院理化技术研究所 | A kind of preparation method of hydrophobic inorganic powder body material |
| CN112191360A (en) * | 2020-10-09 | 2021-01-08 | 河南工业大学 | Diamond powder particle size grading method |
| CN113717691A (en) * | 2021-08-31 | 2021-11-30 | 昆山捷纳电子材料有限公司 | Preparation method and application of polyethylene polyamine modified diamond composite abrasive particles |
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2007
- 2007-03-08 CN CNB2007100516301A patent/CN100572457C/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531835B (en) * | 2009-04-24 | 2012-05-23 | 吉林大学 | Wollastonite powder surface wet modification method assisted by microwave |
| TWI398507B (en) * | 2009-07-03 | 2013-06-11 | Kinik Co | Thermal paste with modified diamond particles and manufacture method thereof |
| CN102602882A (en) * | 2011-01-21 | 2012-07-25 | 曾亚东 | High-speed centrifugal nanoparticle preparation method |
| CN104961945A (en) * | 2015-07-27 | 2015-10-07 | 四川理工学院 | Method for reinforcing rubber by using nano diamond powder |
| CN105004669A (en) * | 2015-07-27 | 2015-10-28 | 四川理工学院 | Method for directly measuring reinforcement mechanical properties of rubber |
| CN105004669B (en) * | 2015-07-27 | 2017-09-01 | 四川理工学院 | A kind of method of direct measurement reinforcing rubber mechanical property |
| CN105153942A (en) * | 2015-07-28 | 2015-12-16 | 郑州磨料磨具磨削研究所有限公司 | Control method for grain size of abrasive material in nano diamond polishing solution |
| CN105131842A (en) * | 2015-10-13 | 2015-12-09 | 郑州磨料磨具磨削研究所有限公司 | Shape dressing method for nanodiamond aggregate in polishing solution |
| CN105131842B (en) * | 2015-10-13 | 2018-03-09 | 郑州磨料磨具磨削研究所有限公司 | Nano diamond aggregate pattern dressing method in polishing fluid |
| CN105692609A (en) * | 2016-03-10 | 2016-06-22 | 天津迪麦爱科科技有限公司 | Preparation method of nano-diamond with relatively good liquid suspension stability |
| CN105692609B (en) * | 2016-03-10 | 2019-10-25 | 天津迪麦爱科科技有限公司 | The method of the preferable Nano diamond preparation of liquid suspension stability |
| CN107502003A (en) * | 2016-06-14 | 2017-12-22 | 中国科学院理化技术研究所 | A kind of preparation method of hydrophobic inorganic powder body material |
| CN107502003B (en) * | 2016-06-14 | 2020-06-02 | 中国科学院理化技术研究所 | Preparation method of hydrophobic inorganic powder material |
| CN112191360A (en) * | 2020-10-09 | 2021-01-08 | 河南工业大学 | Diamond powder particle size grading method |
| CN113717691A (en) * | 2021-08-31 | 2021-11-30 | 昆山捷纳电子材料有限公司 | Preparation method and application of polyethylene polyamine modified diamond composite abrasive particles |
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| CN100572457C (en) | 2009-12-23 |
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