CN1217741C - Method of preparing superfine modified powder by composite grinding and modification - Google Patents
Method of preparing superfine modified powder by composite grinding and modification Download PDFInfo
- Publication number
- CN1217741C CN1217741C CN 03128258 CN03128258A CN1217741C CN 1217741 C CN1217741 C CN 1217741C CN 03128258 CN03128258 CN 03128258 CN 03128258 A CN03128258 A CN 03128258A CN 1217741 C CN1217741 C CN 1217741C
- Authority
- CN
- China
- Prior art keywords
- powder
- modification
- microwave
- effect
- modifier
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Disintegrating Or Milling (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention relates to the fields of powder science and engineering, particularly to modifying preparation techniques for preparing superfine powder. The present invention discloses a method for preparing superfine modified powder in a crushing and modifying mode, which is characterized in that fresh surfaces of granules generated by crushing form a large quantity of high activity points in the fluidized bed air flow crushing process since chemical bonds are cut off, and the granules and a modifying agent can generate the chemical bond linkage or the physical adsorption effect in time by the peculiar high turbulent flow effect and the dynamic-chemical effect of the air flow crushing so as to have the modifying effect of the air flow crushing; meanwhile, the present invention realizes the modifying-grinding assisting effect of microwaves by utilizing the heating effect and modification excitation effect on the powder and the modifying agent by microwaves, and the intercrystalline stress reinforcing effect on granules by microwaves. The present invention has the advantages that the present invention simplifies the preparation process and enhances the superfine grinding efficiency; the heating effect and the modification excitation effect on the powder and the modifying agent by the microwave field can enhance the intercrystalline stress of the granules and have the grinding assisting effect.
Description
Technical field
The present invention relates to powder scientific and engineering field, be specifically related to the superfine modified technology of preparing of powder.
Background technology
Powder is carried out ultra-fineization and surface modification treatment, and the chemical reactivity that can improve powder is beneficial to the synthetic of material; The interface affinity that improves powder is beneficial to the mechanical property of packing material; The various cohesiveness of regulation and control powder surface are beneficial to the dispersion of powder and use; Obtain powder surface specific physical performance and be beneficial to the functional powder preparation.Therefore, ultra-fineization of powder and surface modification are the important means of high performance material preparation process engineering, also are the important contents of new material, new technology and new product development.
Existing superfine modified powder preparation method, what mainly adopt is that the technology of running on foot, that is: first ultra-fine grinding, rear surface modification are divided in elder generation, back.
In superfine technique, it is the mechanical crushing method that can effectively obtain smallest particles of generally acknowledging at present that air-flow is pulverized.Air-flow is pulverized all multiple modes in concrete enforcement, wherein, the fluidized bed airflow grinding mode is used more and more aborning with its superior ultra-fine grinding performance.
In the superfine powder process for modifying surface, the method in having used or having studied roughly is divided into 6 kinds: 1. surperficial adsorption of modification; 2. theca externa modification; 3. high energy surface modification; 4. mechanical-chemical modification; 5. local graft modification; 6. precipitation reaction modification.3. and 5. what wherein 2. 1. method promptly adopted is the method for " first ultra-fine grinding, rear surface modification "; 6. method then is to carry out surface modification simultaneously in chemical method prepares the process of ultra-fine grain, but this method only is applicable to that some can carry out the material that precipitation reaction prepares superfine powder, and the exposure at new interface behind the super-dry desintegrate can reduce the modified effect of superfine powder; 4. method is to utilize the high energy medium mill, under higher mechanical energy input rate state, powder is carried out mechanical-chemical modification, does not add modifier usually, and exists the wearing and tearing doping pollution problem of abrasive media.Eliminating method 4. beyond, the concrete enforcement of above method of modifying is to carry out in reforming apparatus such as reactor, mixer, homogenizer, high speed kneader, liquid fluid bed.
Heating using microwave is a kind of new heat energy technology, and it promotes its dipole motion by to heated material internal radiation microwave electromagnetic field, makes it mutual collision, friction and living hot, and therefore, heating using microwave has following characteristics:
(1) heating using microwave is to excite the material interior molecules to do Action of Superhigh Frequency Vibration, friction, can realize " stirring " on the molecular level, and this " priming effect " begun to use in Polymer Synthesizing and curing reaction;
(2), therefore can carry out the selectivity heating, thereby improve the selectivity of reaction each component in the modification material because material absorbs the dielectric property that the ability of microwave energy depends on material self;
(3) heating using microwave does not have hysteresis effect, after closing microwave source, does not promptly have microwave energy and passes to material, utilizes this characteristic can carry out the modification processing high to temperature control requirement;
(4) heating using microwave is the volume heating that material causes because of dielectric loss own in electromagnetic field, therefore, heating using microwave not only capacity usage ratio very high, heat up rapidly, and have inversion degree gradient and specific functions such as zero-temperature coefficient gradient-heated, reduction reaction temperature, fast reaction speed.
The fluidized bed airflow breaking method adopts compressed air to quicken the supersonic jet that the back produces by nozzle expansion, powder is quickened and produces violent impact, friction and pulverizes at the injection stream crossing place.The crushing process of this method carries out in an airtight device, and the motion class of gas and powder is similar to fluidized state, and forms high turbulent flow melange effect, and this makes to add modifier in the crushing process and be adsorbed in particle surface equably becomes possibility.Simultaneously, its airtight container-like structure becomes possibility for utilizing microwave field that powder, modifier are heated, excite modification and pulverizes grinding aid.
Summary of the invention
The objective of the invention is: in existing superfine modified powder preparation method, the technology that elder generation's ultra-fine grinding rear surface modification is carried out step by step, air-flow is pulverized the preparation process that a modification and microwave modification one compoundization of grinding-aid effect are used for superfine modified powder, ultra-fine grinding and surface modification are finished in the integrated apparatus of a step process simultaneously.
The technical solution used in the present invention is: the method for pulverizing and the superfine modified powder of compoundization of modification preparation, it is characterized in that in the fluidized bed airflow crushing process, adding modifier, and simultaneously, utilize microwave that powder and modifier are heated.
The present invention adopts in the fluidized bed airflow crushing process, utilize and pulverize the particle unsalted surface that is produced is blocked formation because of chemical bond a large amount of high activity points, pulverize high turbulent flow and power-chemical effect by air-flow, timely and modifier produces chemical bonding or physisorption, realizes air-flow pulverizing-modified effect; Simultaneously, utilize microwave, realize microwave modification-grinding-aid effect the heating of powder and modifier, the modifying function that excites and microwave intergranular stress humidification to particle.
The present invention compares with existing powder surface modification method, has the following advantages:
One, overcome in the existing superfine modified powder preparation method, the shortcoming that elder generation's ultra-fine grinding rear surface modification is carried out step by step, ultra-fine grinding and surface modification are finished in the integrated apparatus of a step process simultaneously, and this has not only simplified superfine modified powder preparation technology, and, can prevent that powder is after ultra-fine grinding, because of surface-active improves greatly, cause reuniting or, bring difficulty for follow-up surface modification because other particles such as hydrone in the absorbed air make the powder surface passivation.
They are two years old, in superfine modified air-flow crushing process, add modifier, not only can realize the modification of powder surface is handled, and in time balance is blocked formed unsaturated one-tenth bonding force because of pulverizing causes the particle surface chemical bond, powder is pulverized under good dispersity, simultaneously, modifier has grinding-aid effect usually, and these can effectively improve ultra-fine grinding efficient.
Its three, in superfine modified air-flow crushing process, introduce microwave field, not only can heat and excite modification, and can strengthen the particle intergranular stress powder and modifier, play grinding-aid effect.
The specific embodiment
The present invention specifically implements in the following manner:
(1) on the basis of fluidized bed air flow crushing device, a modifier weigh feeder is set, modifier is sprayed in the reducing mechanism through the supersonic airstream atomizing by pulverizing nozzle; Microwave rf generator is symmetricly set in the middle part of reducing mechanism, and the bottom is provided with the multi-point temp sensor; Whole device meets the micro-wave screening requirement.
(2) microwave rf generator power configuration principle: 2～3 kilowatts of volume configurations are pulverized in per 500 liters of modifications, can adjust the allocating power of microwave in the enforcement according to the difference of powder microwave-medium; Heating using microwave is carried out with intermittent mode, and action time and intermittent time are adjustable, and with container in the interlock control of temperature sensor design temperature, the modifying process temperature is controlled at modifier decomposition temperature following (common 60 ~ 95 ℃).
When (3) modification was pulverized, modifier sprayed in the reducing mechanism by the required adding proportion of modification, and set microwave heating time and intermittent time according to modification temperature, carried out microwave Aided Modification air-flow and pulverized.
(4) pulverize the superfine modified powder that obtains by microwave Aided Modification air-flow, its granularity is controlled by the high-speed turbine grader rotating speed on the reducing mechanism.
Application example of the present invention:
Used powder is pulverized in modification: talcum
Modifier: silane coupler NH
2-C
3H
6-Si (OC
2H
5)
3
Grader rotating speed: 7500r.p.m.; Nozzle is pulverized pressure: 0.8～0.88MPa;
Modifier addition: 12ml/kg powder;
Modification control temperature: 70 ± 8 ℃; Microwave action time-temperature sensor is controlled automatically;
The disposal ability that modification is pulverized; 19.5kg/hr;
Microwave power: 1500W; Microwave frequency: 2450MHz.
The superfine modified talcum powder performance test value of the present invention's preparation
| The fluidized bed jet mill comminuting method | The present invention | Explanation | |
| 4 hours turbidity (%) in isopropyl alcohol | 18.30 | 46.87 | Modification is pulverized back powder turbidity value in isopropyl alcohol and is significantly improved, promptly form stable dispersion, show that the present invention has reached the modified effect of expection. |
| Oil absorbency (%) | 45.2 | 28.4 | Oil absorbency obviously reduces, and promptly lipophile increases, and shows that the present invention has reached the modified effect of expection. | |
| Infrared spectrum analysis | Infrared spectrum analysis shows, adopts the resulting talcum powder of the present invention, at 2919cm -1And 2840cm -1Absworption peak appears in the place, and this is by silane coupler [NH 2-C 3H 6-Si (OC 2H 5) 3] in-CH 2-asymmetric stretching vibration and symmetrical stretching vibration cause; At 1440cm -1Peak, place spectrum is obviously widened, and shows-CH 2-NH 2Functional group and [CO 3] 2-Characteristic peak formed the coupling vibrational band.Therefore, the talcum powder surface has formed chemisorbed with silane coupler, i.e. the present invention has reached the modified effect of expection. | |||
| X-ray diffraction analysis | X-ray diffraction spectrum figure shows, adopt the resulting talcum powder of the present invention, interlamellar spacing d value is that the peak of 4.6916 (004) crystal faces obviously weakens, the d value is that the peak of 2.3411 (008) crystal faces disappears, show that talcum is along (004), (008) crystal face cleavage, crystal face is destroyed, also promptly show in modification crushing process of the present invention, caused the generation of crystal displacement and distortion. | |||
| Change of granularity | Before modification is pulverized: d 50=14.16 microns; d 97Back: d is pulverized in=41.30 microns modifications 50=3.01 microns; d 97=6.62 microns | Before and after modification is pulverized, change of granularity is remarkable, promptly shows to pulverize the effect that has reached ultra-fine grinding with the method for the superfine modified powder of compoundization of modification preparation. | ||
Claims (2)
1. the method for pulverizing and the superfine modified powder of compoundization of modification preparation is characterized in that adding modifier in the fluidized bed airflow crushing process, simultaneously, utilizes microwave that powder and modifier are heated.
2. the method for pulverizing according to claim 1 and the superfine modified powder of compoundization of modification preparation, it is characterized in that specific implementation method is: (1) is on the basis of fluidized bed air flow crushing device, one modifier weigh feeder is set, modifier is sprayed in the reducing mechanism through the supersonic airstream atomizing by pulverizing nozzle; Microwave rf generator is symmetricly set in the middle part of reducing mechanism, and the bottom is provided with the multi-point temp sensor; Whole device meets the micro-wave screening requirement;
(2) microwave rf generator power configuration principle: 2～3 kilowatts of volume configurations are pulverized in per 500 liters of modifications, can adjust the allocating power of microwave in the enforcement according to the difference of powder microwave-medium; Heating using microwave is carried out with intermittent mode, and action time and intermittent time are adjustable, and with container in the interlock control of temperature sensor design temperature, the modifying process temperature is controlled at 60～95 ℃;
When (3) modification was pulverized, modifier sprayed in the reducing mechanism by the required adding proportion of modification, and set microwave heating time and intermittent time according to modification temperature, carried out microwave Aided Modification air-flow and pulverized;
(4) pulverize the superfine modified powder that obtains by microwave Aided Modification air-flow, its granularity is controlled by the high-speed turbine grader rotating speed on the reducing mechanism.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03128258 CN1217741C (en) | 2003-07-01 | 2003-07-01 | Method of preparing superfine modified powder by composite grinding and modification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03128258 CN1217741C (en) | 2003-07-01 | 2003-07-01 | Method of preparing superfine modified powder by composite grinding and modification |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1475310A CN1475310A (en) | 2004-02-18 |
| CN1217741C true CN1217741C (en) | 2005-09-07 |
Family
ID=34153298
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 03128258 Expired - Fee Related CN1217741C (en) | 2003-07-01 | 2003-07-01 | Method of preparing superfine modified powder by composite grinding and modification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1217741C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665615A (en) * | 2019-10-10 | 2020-01-10 | 青岛瓷兴新材料有限公司 | Preparation method of superfine silicon powder |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100362058C (en) * | 2005-12-20 | 2008-01-16 | 中国地质大学（武汉） | Dry process mechanical force and chemical modification method of superfine calcium carbonate |
| CN101030454B (en) * | 2006-03-03 | 2010-12-22 | 西南科技大学 | Production and usage for electromagnetic shielding functional metaprimitive |
| CN101531835B (en) * | 2009-04-24 | 2012-05-23 | 吉林大学 | Wollastonite powder surface wet modification method assisted by microwave |
| CN101648154B (en) * | 2009-09-08 | 2011-06-08 | 武汉理工大学 | Airflow mill of multifunctional fluidized bed |
| CN105236381B (en) * | 2014-06-26 | 2019-01-11 | 山东大展纳米材料有限公司 | The method that gas-solid mutually quickly prepares cyclopentadiene modified carbon nano-tube |
| CN107446388B (en) * | 2017-08-04 | 2019-08-20 | 西藏亚吐克工贸有限公司 | The dedicated titanium dioxide process of powdery paints |
| CN108947580B (en) * | 2018-07-26 | 2020-12-08 | 塔里木大学 | Preparation method of layered vermiculite powder |
| CN113278306A (en) * | 2021-05-12 | 2021-08-20 | 广西科学院 | Microwave wet-method modified artificial granite waste residue and recycling process method thereof |
-
2003
- 2003-07-01 CN CN 03128258 patent/CN1217741C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665615A (en) * | 2019-10-10 | 2020-01-10 | 青岛瓷兴新材料有限公司 | Preparation method of superfine silicon powder |
| CN110665615B (en) * | 2019-10-10 | 2022-04-19 | 青岛瓷兴新材料有限公司 | Preparation method of superfine silicon powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1475310A (en) | 2004-02-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Pinjari et al. | Cavitation milling of natural cellulose to nanofibrils | |
| CN1217741C (en) | Method of preparing superfine modified powder by composite grinding and modification | |
| WO2021109729A1 (en) | Inorganic powder modification system | |
| CN1176142C (en) | Polymer/carbon nano pipe composite powder and its solid phase shear break up preparation method | |
| KR101487475B1 (en) | Method of fabricating nano cellulose fiber and apparatus for fabricating the same | |
| KR900005175B1 (en) | Particulate material treating apparatus | |
| CN201186212Y (en) | Multifunction phonochemical reaction equipment | |
| NZ531480A (en) | Process for micronizing materials | |
| CN102732063A (en) | Modified fly ash, preparation method thereof, and preparation apparatus thereof | |
| CN109810323A (en) | The preparation method and nano hybridization filler of a kind of white carbon black/stannic oxide/graphene nano hydridization filler and its application | |
| CN101942233B (en) | Surface treatment method of inorganic nano-particles and application | |
| CN110117394B (en) | Nano toughening wear-resistant plastic master batch and preparation method thereof | |
| WO2022205791A1 (en) | Graphene modified pet film material and preparation method therefor | |
| JP2011219344A (en) | Method for producing metal hydroxide fine particle | |
| Hielscher | Ultrasonic milling and dispersing technology for nano-particles | |
| US7108207B2 (en) | Process and apparatus for comminuting particle rubber | |
| CN108545718A (en) | A kind of dispersing method of carbon nanotube | |
| CN110694559B (en) | Preparation method and application of two-dimensional material nanosheet coated microspheres | |
| CN102372815A (en) | Preparation method for organic/inorganic nano composite resin | |
| CN107010651A (en) | The surface modifying method of nano zine oxide | |
| CN107118592A (en) | A kind of preparation method of modified nano zinc oxide | |
| CN107129596A (en) | The method of modifying of nano zine oxide | |
| CN1256391C (en) | Powder surface imcrowave auxiliary modification method | |
| Badgujar et al. | Ultrasound assisted organic pigment dispersion: Advantages of ultrasound method over conventional method | |
| KR100665042B1 (en) | Polymer macroparticle of which surface is modified by mesoparticle and nanoparticle, nanoparticle-polymer composite using the same, and preparation thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |