CN1475310A - 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
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- CN1475310A CN1475310A CNA03128258XA CN03128258A CN1475310A CN 1475310 A CN1475310 A CN 1475310A CN A03128258X A CNA03128258X A CN A03128258XA CN 03128258 A CN03128258 A CN 03128258A CN 1475310 A CN1475310 A CN 1475310A
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Abstract
A process for preparing modified superfine powder by pulverizing and modifying features airflow pulverizing on fluidized bed while reacting on modifier by chemical bonding and physical adsorption. Said modifier is heated by microwave before reaction. Its advantages are simple process and high 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 fine 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, the fine 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 to divide first, afterwards the technique of running on foot, that is: first ultra-fine grinding, rear surface modification.
In superfine technique, air-flow crushing is the mechanical crushing method that can effectively obtain smallest particles of generally acknowledging at present. Air-flow crushing has all multiple modes in concrete enforcement, wherein, the fluid bed airflow milling 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. adsorption 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 namely adopted is the method for " first ultra-fine grinding, rear surface modification "; 6. method then is to carry out simultaneously surface modification in chemical method prepares the process of ultra-fine grain, can carry out the material that precipitation reaction prepares superfine powder but this method is only applicable to some, 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 usually add modifier, and exists the wearing and tearing doping pollution problem of abrasive media. Eliminating method 4. beyond, the implementation of above method of modifying is to carry out in the reforming apparatus such as reactor, mixer, homogenizer, high-speed kneading machine, 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) because the ability of material absorbing microwave energy depends on the dielectric property of material self, therefore can each component in the modification material selectively be heated, thereby improve the selective of reaction;
(3) heating using microwave, namely passes to material without microwave energy after closing microwave source without hysteresis effect, utilizes this characteristic can carry out the modification high to temperature control requirement;
(4) heating using microwave is the volume heating that material causes because of dielectric loss own at elect magnetic field, therefore, heating using microwave not only capacity usage ratio very high, heat up rapidly, and have inversion degree gradient and the specific functions such as zero-temperature coefficient gradient-heated, reduction reaction temperature, fast reaction speed.
The fluid bed airflow milling method, the supersonic jet that produces after adopting compressed air to accelerate by nozzle expansion is accelerated powder and is produced violent impact, friction and pulverize at the injection stream crossing place. The crushing process of the method carries out in an airtight device, and the motion class of gas and powder is similar to fluidized state, and forms distinctive high turbulent flow melange effect, and this makes to add modifier in the crushing process and be adsorbed in equably particle surface becomes possibility. Simultaneously, its airtight container-like structure is for utilizing microwave field to heat, excite modification and powder crushing grinding aid to become possibility to powder, modifier.
Summary of the invention
The objective of the invention is: in existing superfine modified powder preparation method, the technique that elder generation's ultra-fine grinding rear surface modification is carried out step by step, air-flow crushing-modification and microwave modification-grinding-aid effect Composite are used for the preparation process of 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: pulverize the method for preparing superfine modified powder with the modification Composite, it is characterized in that in the fluid bed airflow milling process, utilize and pulverize the particle unsalted surface that produces is truncated formation because of chemical bond a large amount of high activity points, by the distinctive high turbulent flow of air-flow crushing and power-chemical effect, timely and modifier produces chemical bonding or physisorption, realizes air-flow crushing-modified effect; Simultaneously, utilize microwave to the heating of powder and modifier, the modifying function that excites and the microwave intergranular stress humidification to particle, realize microwave modification-grinding-aid effect.
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 surface-active improves greatly, cause reuniting or because other particles such as hydrone in the absorbed air make the powder surface passivation, bring difficulty for follow-up surface modification.
They are two years old, in superfine modified Crushing with Jet Mill, add modifier, not only can realize the modification to powder surface, and in time balance is truncated formed unsaturated one-tenth bonding force because 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 Crushing with Jet Mill, introduce microwave field, not only can heat and excite modification powder and modifier, and can strengthen the particle intergranular stress, play grinding-aid effect.
The specific embodiment
The present invention is implementation 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 arranges multipoint temperature 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 according to the difference of powder microwave-medium the allocating power of microwave in the enforcement; Heating using microwave is carried out with intermittent mode, and action time and intermittent time can be regulated and control, 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 crushing.
(4) the superfine modified powder that obtains by microwave Aided Modification air-flow crushing, 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 NH2-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 ℃; The microwave action time is controlled automatically by temperature sensor;
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 | Powder turbidity value in isopropyl alcohol significantly improved after modification was pulverized, and namely formed stable dispersion, showed that the present invention has reached the modified effect of expection. |
| Oil absorbency (%) | 45.2 | 28.4 | Oil absorbency obviously reduces, and namely 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 [NH2-C 3H 6-Si(OC 2H 5) 3] in-CH2-asymmetric stretching vibration and symmetrical stretching vibration cause; At 1440cm-1Peak, place spectrum is obviously widened, and shows-CH2-NH 2Functional group and [CO3] 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, and also namely shows in modification crushing process of the present invention, has caused the generation of crystal displacement and distortion. | |||
| Change of granularity | Before modification is pulverized: d50=14.16 microns; d97After=41.30 microns modifications are pulverized: d50=3.01 microns; d97=6.62 microns | Before and after modification was pulverized, change of granularity was remarkable, namely showed to pulverize the effect that the method for preparing superfine modified powder with the modification Composite has reached ultra-fine grinding. | ||
Claims (2)
1, pulverizing and modification Composite prepare the method for superfine modified powder, it is characterized in that in the fluid bed airflow milling process, utilize and pulverize the particle unsalted surface that produces is truncated formation because of chemical bond a large amount of high activity points, by the distinctive high turbulent flow of air-flow crushing and power-chemical effect, timely and modifier produces chemical bonding or physisorption, realizes air-flow crushing-modified effect; Simultaneously, utilize microwave to the heating of powder and modifier, the modifying function that excites and the microwave intergranular stress humidification to particle, realize microwave modification-grinding-aid effect.
2, pulverizing according to claim 1 and modification Composite prepare the method for superfine modified powder, 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 arranges multipoint temperature 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 according to the difference of powder microwave-medium the allocating power of microwave in the enforcement; Heating using microwave is carried out with intermittent mode, and action time and intermittent time can be regulated and control, 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 crushing;
(4) the superfine modified powder that obtains by microwave Aided Modification air-flow crushing, its granularity is controlled by the high-speed turbine grader rotating speed on the reducing mechanism.
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| CN 03128258 CN1217741C (en) | 2003-07-01 | 2003-07-01 | Method of preparing superfine modified powder by composite grinding and modification |
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Cited By (9)
| 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 |
| CN101648154B (en) * | 2009-09-08 | 2011-06-08 | 武汉理工大学 | Airflow mill of multifunctional fluidized bed |
| CN101531835B (en) * | 2009-04-24 | 2012-05-23 | 吉林大学 | Wollastonite powder surface wet modification method assisted by microwave |
| WO2015197005A1 (en) * | 2014-06-26 | 2015-12-30 | 山东大展纳米材料有限公司 | Method for quickly preparing cyclopentadiene-modified carbon nanotube in gas-solid phase |
| CN107446388A (en) * | 2017-08-04 | 2017-12-08 | 西藏亚吐克工贸有限公司 | The special titanium dioxide process of powdery paints |
| CN108947580A (en) * | 2018-07-26 | 2018-12-07 | 塔里木大学 | A kind of exfoliated vermiculite raw powder's production technology |
| 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 |
| 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 (12)
| 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 |
| WO2015197005A1 (en) * | 2014-06-26 | 2015-12-30 | 山东大展纳米材料有限公司 | Method for quickly preparing cyclopentadiene-modified carbon nanotube in gas-solid phase |
| CN107446388A (en) * | 2017-08-04 | 2017-12-08 | 西藏亚吐克工贸有限公司 | The special titanium dioxide process of powdery paints |
| 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 |
| CN108947580A (en) * | 2018-07-26 | 2018-12-07 | 塔里木大学 | A kind of exfoliated vermiculite raw powder's production technology |
| CN108947580B (en) * | 2018-07-26 | 2020-12-08 | 塔里木大学 | Preparation method of layered vermiculite powder |
| 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 |
| 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 |
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|---|---|
| CN1217741C (en) | 2005-09-07 |
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