CN110773079B - Method for preparing superfine powder balls by ultrasonic spraying method - Google Patents
Method for preparing superfine powder balls by ultrasonic spraying method Download PDFInfo
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- CN110773079B CN110773079B CN201911124683.0A CN201911124683A CN110773079B CN 110773079 B CN110773079 B CN 110773079B CN 201911124683 A CN201911124683 A CN 201911124683A CN 110773079 B CN110773079 B CN 110773079B
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- 239000000843 powder Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000005507 spraying Methods 0.000 title claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 20
- 239000011858 nanopowder Substances 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 46
- 238000001694 spray drying Methods 0.000 claims description 10
- 239000002270 dispersing agent Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 239000002086 nanomaterial Substances 0.000 claims description 3
- 238000010009 beating Methods 0.000 claims description 2
- 230000009172 bursting Effects 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000005416 organic matter Substances 0.000 claims description 2
- 238000004537 pulping Methods 0.000 claims description 2
- 238000005096 rolling process Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 5
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 230000002776 aggregation Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000000889 atomisation Methods 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000010146 3D printing Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 239000011358 absorbing material Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920000058 polyacrylate Polymers 0.000 description 3
- 238000000635 electron micrograph Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
- B01D1/18—Evaporating by spraying to obtain dry solids
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Glanulating (AREA)
Abstract
The invention discloses a method for preparing superfine powder balls by an ultrasonic spraying method, which adopts ultrasonic high-speed atomization drying after double-solution dispersion, and the internal structure of the powder balls has the microscopic effect of nano powder; the powder balls have stable properties, no agglomeration phenomenon, high dispersity and particularly good fluidity; the invention has the advantages of convenient adjustment of process parameters, simple process and low cost.
Description
Technical Field
The invention relates to a technology for preparing a nano material, in particular to a preparation method of superfine powder balls, belonging to the field of nanotechnology.
Background
Along with the rapid development of the 3D printing and wave-absorbing material technology, the requirement on the superfine powder material is higher and higher, the 3D printing material requires that the used powder additive has good fluidity and low-temperature rapid forming so as to ensure that the powder spraying port is smooth and free from blockage in powder spraying, and the required heating source is not at too high temperature so as to prevent the formed part from being influenced by too high temperature and the service life of the heating source is not long. The wave-absorbing material is required to effectively absorb electromagnetic waves and convert the electromagnetic waves into heat energy, so that the reflection quantity is reduced.
The two purposes both put forward higher requirements on the used powder, the invention is in order to develop a powder ball, the powder ball is formed by a large amount of nano-scale powder agglomeration, the size of the powder ball is micron-scale, the larger size ensures that when the powder ball is used, the powder ball keeps good fluidity in a dry powder state to ensure the requirement of powder spraying when used for 3D printing, the powder ball keeps good stability in a slurry state, and when the powder spraying is formed, because the internal structure is the nano-scale powder, the surface melting point is very low, the powder ball can be quickly formed at a lower heating source temperature; when the material is attached to the surface of an object as a wave-absorbing material, the internal structure is powder aggregate, so that electromagnetic waves can be absorbed into the powder ball to effectively reduce reflection, and after the electromagnetic waves are absorbed into the powder ball, the electromagnetic waves are reflected and absorbed back and forth in the powder ball to be converted into heat energy, thereby achieving the wave-absorbing effect.
Disclosure of Invention
The invention provides a method for preparing superfine powder balls by an ultrasonic spraying method aiming at the application requirements of the powder balls in the background technology, which aims to: the method for preparing the superfine powder ball has the advantages of high dispersity, good fluidity and uniform size, and the internal structure of the superfine powder ball is nano powder, the appearance of the superfine powder ball is micro powder level powder ball.
In order to achieve the purpose, the technical solution of the invention is as follows:
a method for preparing superfine powder balls by an ultrasonic spraying method specifically comprises the following steps:
firstly, obtaining target nano powder;
adding the nano powder in the step (one) into a dispersing agent, and fully mixing to obtain a dispersion liquid, wherein the specific concentration is determined by the required powder, and the smaller the diameter of the required powder ball is, the smaller the concentration of the dispersion liquid is;
thirdly, adding the powder dispersion liquid prepared in the step (II) into a volatile liquid, wherein the volatile liquid and the dispersion liquid are required not to be mutually dissolved;
turning on ultrasonic waves, carrying out ultrasonic treatment on the mixed liquid prepared in the step (three), and beating the dispersion liquid into tiny liquid drops to be suspended in the volatile liquid through tiny balloon bursting force formed by the ultrasonic waves until the size of the tiny liquid drops can reach the millimeter level or below;
and (V) rapidly passing the mixed solution through a high-speed atomizing motor, carrying out spray drying in a spray drying device, rapidly evaporating the volatile liquid, rapidly evaporating the dispersion liquid in high-temperature airflow of the spray drying device, concentrating and agglomerating the nano powder dispersed in the dispersion liquid into powder balls, and forming micron-sized agglomerated superfine powder balls through the high-temperature airflow of the spray drying device.
Furthermore, the dispersant required in the step (II) is organic matter and has good dispersibility for the nano powder.
Further, in the step (two), in the process of fully mixing, a stirring device, an ultrasonic dispersion device or a rolling pulping device can be used.
Furthermore, the volatile liquid in the step (three) is water or alcohol type low molecular weight liquid, does not dissolve with the dispersant used in the step (two), and has good volatility.
Preferably, the powder used in the step (one) may be a mixture of a plurality of nanomaterials, thereby preparing powder balls with more excellent performance.
Preferably, the ultrasonic wave used in the step (four) is installed at a position close to the high-speed atomizing motor used in the step (five) to prevent the dispersed liquid droplets in the mixed liquid from being aggregated.
The invention has the beneficial effects that: the invention adopts ultrasonic high-speed atomization drying after double-solution dispersion, and has the following advantages:
1) the internal structure of the powder ball has the microscopic effect of the nano powder;
2) the powder balls have stable properties, no agglomeration phenomenon, high dispersity and particularly good fluidity;
3) the technological parameters are convenient to adjust, the process is simple, and the cost is low.
Drawings
FIG. 1 is an electron micrograph of nickel powders required for preparation examples.
FIG. 2 is an enlarged electron micrograph of the prepared powder ball.
Detailed Description
The present invention will be further described with reference to the following examples and the accompanying drawings.
Examples
A method for preparing superfine powder balls by an ultrasonic spraying method comprises the following specific steps:
1. and adding 10L of ammonium polyacrylate into a collection system communicated with the production system, starting an emulsifying machine for stirring, wherein the rotating speed of a motor is 1390r/min, the transmission ratio is 1:1, and then adding 1 kg of 80nm nickel powder to prepare the ammonium polyacrylate dispersion liquid of the nickel powder with the concentration of 10%.
2. After an ultrasonic production system is started, adding the ammonium polyacrylate dispersion liquid of nickel powder into 50L of alcohol solution, starting ultrasonic waves, and fully stirring and uniformly mixing the dispersion liquid in the alcohol solution to form micro-droplet suspension.
3. And starting the heating airflow of the spray drying equipment until the temperature in the spray drying equipment reaches the temperature and airflow speed required by drying.
4. The mixed liquid is added into a high-speed atomizing motor through a metering pump, and the mixed liquid is rapidly sprayed out from a liquid spraying port of the atomizing motor to form a mist shape by using the rotating speed of 18000 r/min.
5. The size of the atomized liquid can reach millimeter level, the size of the nickel powder dispersion liquid drop in the liquid is smaller, the volatile liquid is firstly evaporated through high-temperature drying gas, the dispersing agent is gradually evaporated, the nickel powder in the dispersing agent is gradually concentrated at the moment, and the nickel powder self-agglomerates into a spherical shape under the action of the surface tension of the dispersing agent and is dried in a high-temperature drying atmosphere to form an agglomerated powder ball.
Claims (6)
1. A method for preparing superfine powder balls by an ultrasonic spraying method is characterized by comprising the following steps: the method specifically comprises the following steps:
firstly, obtaining target nano powder;
adding the nano powder in the step (one) into a dispersing agent, and fully mixing to obtain a dispersion liquid, wherein the specific concentration is determined by the required powder ball, and the smaller the diameter of the required powder ball is, the smaller the concentration of the dispersion liquid is;
thirdly, adding the powder dispersion liquid prepared in the step (II) into a volatile liquid, wherein the volatile liquid and the dispersion liquid are required not to be mutually dissolved;
turning on ultrasonic waves, carrying out ultrasonic treatment on the mixed liquid prepared in the step (three), and beating the dispersion liquid into tiny liquid drops to be suspended in the volatile liquid through tiny balloon bursting force formed by the ultrasonic waves until the size of the tiny liquid drops can reach the millimeter level or below;
and (V) rapidly passing the mixed solution through a high-speed atomizing motor, carrying out spray drying in a spray drying device, rapidly evaporating the volatile liquid, rapidly evaporating the dispersion liquid in high-temperature airflow of the spray drying device, concentrating and agglomerating the nano powder dispersed in the dispersion liquid into powder balls, and forming micron-sized agglomerated superfine powder balls through the high-temperature airflow of the spray drying device.
2. The method for preparing the superfine powder ball by the ultrasonic spraying method according to claim 1, wherein the method comprises the following steps: the dispersant required in the step (II) is an organic matter, and has good dispersibility for the nano powder.
3. The method for preparing the superfine powder ball by the ultrasonic spraying method according to claim 1, wherein the method comprises the following steps: and (II) in the fully mixing process, stirring equipment, ultrasonic dispersion equipment or rolling pulping equipment is used.
4. The method for preparing the superfine powder ball by the ultrasonic spraying method according to claim 1, wherein the method comprises the following steps: the volatile liquid in the step (III) is water or alcohol low molecular weight liquid, does not dissolve with the dispersant used in the step (II), and has good volatility.
5. The method for preparing the superfine powder ball by the ultrasonic spraying method according to claim 1, wherein the method comprises the following steps: the powder used in the step (one) is a mixture of a plurality of nano materials.
6. The method for preparing the superfine powder ball by the ultrasonic spraying method according to claim 1, wherein the method comprises the following steps: and (4) the ultrasonic wave used in the step (four) is arranged at a position close to the high-speed atomizing motor used in the step (five) so as to prevent the dispersed liquid drops in the mixed liquid from being aggregated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911124683.0A CN110773079B (en) | 2019-11-18 | 2019-11-18 | Method for preparing superfine powder balls by ultrasonic spraying method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911124683.0A CN110773079B (en) | 2019-11-18 | 2019-11-18 | Method for preparing superfine powder balls by ultrasonic spraying method |
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| Publication Number | Publication Date |
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| CN110773079A CN110773079A (en) | 2020-02-11 |
| CN110773079B true CN110773079B (en) | 2022-03-01 |
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| CN201911124683.0A Active CN110773079B (en) | 2019-11-18 | 2019-11-18 | Method for preparing superfine powder balls by ultrasonic spraying method |
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| CN111515000B (en) * | 2020-04-30 | 2022-02-01 | 厦门高容纳米新材料科技有限公司 | Method for dispersing nano powder |
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| US6538164B1 (en) * | 1999-09-30 | 2003-03-25 | E. I. Du Pont De Nemours And Company | Recovery process for volatile compounds from solids in aqueous solution |
| KR20060033033A (en) * | 2003-08-04 | 2006-04-18 | 화이자 프로덕츠 인크. | Formulations provide controlled release of cholesteryl ester transfer protein inhibitors and transient release of HMV-COA reductase inhibitors |
| GB0705159D0 (en) * | 2007-03-19 | 2007-04-25 | Prosonix Ltd | Process for making crystals |
| CN101279232B (en) * | 2008-01-11 | 2010-10-06 | 东南大学 | Preparation of microballoons based on microfluid |
| PT106237B (en) * | 2012-03-30 | 2015-03-19 | Hovione Farmaci Ncia S A | PRODUCTION OF SUBSTANCIALLY MONO-BUILT PARTICLES USING GRINDING AND MEMBRANE SEPARATION |
| DK3082771T3 (en) * | 2013-12-19 | 2019-09-02 | Aerosol Therapeutics Llc | COMPOSITIONS AND METHODS FOR ATMOSPHERIC SPRAY FREEZER DRYING |
| JP2017094239A (en) * | 2015-11-19 | 2017-06-01 | 株式会社日清製粉グループ本社 | Granule and production method of the granule |
| CN107522206A (en) * | 2016-06-21 | 2017-12-29 | 张家港市思杰五金工具有限公司 | The preparation method of conglobation molybdenum silicide powder |
| CN108516805A (en) * | 2018-06-21 | 2018-09-11 | 西北工业大学 | The preparation method of eutectic composition oxide ceramics spheric granules |
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