CN102674381A - Method for preparing nano mullite powder from coal-based kaolin - Google Patents
Method for preparing nano mullite powder from coal-based kaolin Download PDFInfo
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- CN102674381A CN102674381A CN2012101590844A CN201210159084A CN102674381A CN 102674381 A CN102674381 A CN 102674381A CN 2012101590844 A CN2012101590844 A CN 2012101590844A CN 201210159084 A CN201210159084 A CN 201210159084A CN 102674381 A CN102674381 A CN 102674381A
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Abstract
The invention discloses a method for preparing nano mullite powder from coal-based kaolin, which comprises the following steps: calcining to activate the raw material coal-based kaolin, and carrying out alkali fusion reaction to prepare the nano mullite powder. Compared with the existing preparation method, the product prepared by the method disclosed by the invention is single-phase nano mullite powder, the raw material is natural mineral which is cheap and accessible, and the invention has the advantages of simple equipment and short period, and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of method of utilizing Coaseries kaolin to prepare nano mullite powder, belong to nano material or technical field of ceramic material.
Background technology
Mullite is the alumina hydrochlorate mineral of aluminium, is SiO
2～Al
2O
3The crystalline compound of system unique stable existence under normal pressure.Mullite has the physicals of many excellences; Like low-expansion coefficient, low thermal conductance, low creep, low-k, high resistance to sudden heating and HS etc.; Not only can be used as engineering materials, can also be widely used in the industry such as metallurgy, glass, pottery, chemistry, electric power, national defence, combustion gas and cement as high grade refractory.
Yet the natural mullite ore deposit that does not have economically valuable in the world, industrial required mullite are artificial mullite synthesizing entirely.
Nano mullite not only has the premium properties of traditional mullite; And have higher high-temperature creep resistance, heat-shock resistance, good erosion resistance and resistance to air loss etc.; It is a kind of potential body material of nanometer composite diphase material; And the nano mullite material receives much concern in the application in fields such as shortening, electronic package material, fire-resistant coating, optical material in recent years.
At present, what the preparation nano mullite powder was relevant applies for a patent: prepare the method for nano mullite complex-phase nano crystal, publication number CN 1733604A with natural kaolin; A kind of preparation method of nano mullite, publication number CN 101182001A; A kind of method for preparing mullite single crystal nano belt, publication number CN 1587450A; A kind of preparation method of nano mullite powder, publication number CN101456561; A kind of method for preparing the mullite single crystal nano line, publication number CN1587450; Collosol and gel～sonochemical method prepares the method for nano mullite powder, publication number CN101700979A.
Preparing the maximum method of nano mullite employing is sol-gel method; Like publication number is CN1587450A, CN101456561 and CN101700979A etc., yet the preparation cycle of sol-gel method is longer relatively, contains a large amount of chemical reagent in the raw material; Cost is higher, is difficult to realize heavy dose of production.
Thereby; Part scholar begins to utilize natural mineral raw to prepare nano mullite; But because the chemical constitution of natural mineral or ore and thing phase composite more complicated all, mostly the synthetic nano mullite is the complex ore phase, such as the preparation method of publication number CN 1733604A.
Up to the present, do not see that yet the bibliographical information that utilizes natural crystal to prepare the single phase nano mullite powder is arranged.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the defective of prior art; A kind of method of utilizing Coaseries kaolin to prepare nano mullite powder is provided; It utilizes Coaseries kaolin to be raw material, after handling through fragmentation, fine grinding, decarburization, deironing etc., carries out calcining and activating; Dissolve reaction through alkali again, prepare nano mullite powder.Compare with existing preparation method, products obtained therefrom of the present invention is the single phase nano mullite powder, and raw materials used be natural mineral, cheap and easy to get, equipment is simple, the cycle is short, be fit to industrial production.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of method of utilizing Coaseries kaolin to prepare nano mullite powder, said method is raw material for utilizing Coaseries kaolin, and raw material is carried out calcining and activating, dissolves reaction through alkali again, prepares nano mullite powder.
Coaseries kaolin of the present invention is kaolin or coal gangue.
With kaolin is raw material, and concrete steps are:
1), raw material calcining and activating: kaolin powder is incubated 2～4h down at 1100～1400 ℃, and naturally cooling gets activation kaolin;
2) alkali dissolves reaction: the NaOH strength of solution is 2～5mol/L, by NaOH solution and activation kaolin than being the standard of 7～10mL/g; Activation kaolin is put into NaOH solution; Stir through the magnetic force heating stirrer and to be warming up to 80～100 ℃; Carry out arrest reaction 3～5h, thorough washing promptly obtains nano mullite powder to neutral after the vacuum filtration drying.
With the coal gangue is raw material, and concrete steps are:
1), raw material calcining and activating:
(1) coal gangue is just handled: coal gangue is broken, fully fine grinding;
(2) coal gangue carbonization treatment: the coal gangue powder is incubated 3～5h, naturally cooling down at 800～1000 ℃;
(3) the coal gangue deironing is handled: be 15～35% hydrochloric acid with mass concentration; Mix with the coal gangue powder of carbonization treatment according to 4: 1 to 6: 1 ratio of liquid-solid ratio; Under 70～90 ℃ of conditions, carry out constant temperature and stir, extremely neutral with the zero(ppm) water repetitive scrubbing to powder behind 1～2h, suction filtration is also dry;
(4) calcining and activating: deironing coal gangue powder is incubated 2～4h down at 1100～1400 ℃, and naturally cooling gets active coal gangue;
2) alkali dissolves reaction: the NaOH strength of solution is 2～5mol/L, by NaOH solution and active coal gangue than being the standard of 7～10mL/g; Active coal gangue is put into NaOH solution; Stir through the magnetic force heating stirrer and to be warming up to 80～100 ℃; Carry out arrest reaction 3～5h, thorough washing promptly obtains nano mullite powder to neutral after the vacuum filtration drying.
The present invention is to be that alkali dissolves the reaction precursor body with the Coaseries kaolin behind the calcining and activating, is reaction medium with NaOH, dissolves reaction back acquisition nano mullite powder through alkali.
China's Coaseries kaolin aboundresources, distribution are extensively; Coaseries kaolin mainly comprises kaolin and coal gangue; Kaolin ore is clay or the tonstein that kaolinite subtribe clay mineral reaches content capable of using; Because of it has many good use characteristics, be widely used in departments such as papermaking, pottery, coating, rubber, plastics, refractory materials, chemical industry, agricultural chemicals, medicine, weaving, oil, building materials and national defence.Coal gangue is the solid waste of being discharged in coal mining and the coal washing process; Be a kind of lower with the carbon content of coal seam association in the coal-forming process, than the hard black graystone of coal; Its main thing is quartz and kaolinite mutually, has similar thermal activation reaction process with kaolin ore.At present, the main mode of the recycling of coal gangue is that low calorie fuels, colliery wastes brick, coal gangue are reclaimed to build up fields and built the road and underground filling etc.
The present invention adopts and contains higher Al in the Coaseries kaolin chemical ingredients
2O
3And SiO
2, and its loss on ignition is bigger, is mainly materials such as carbon.Main thing in the coal gangue is kaolin mutually, thing phase change and the kaolin families of coal gangue in the high-temperature calcination process seemingly, through the metakaolin stage and to the mullite inversion of phases.
The activation temperature that the present invention selectes is 1100～1400 ℃, and the Coaseries kaolin after activation this moment has changed the mixed oxide of mullite and quartz or cristobalite into.Alkali dissolves in the reaction process; NaOH strength of solution, alkali dissolve temperature of reaction, alkali dissolves the key that the reaction times all is control generation single phase nano mullite powder; Wherein to the influence degree that generates the single phase nano mullite by by force to a little less than be respectively, alkali solubility temperature＞NaOH strength of solution＞alkali dissolves the time.Under the situation of, overlong time too high in excessive concentration, temperature, hydro-thermal reaction is prone to generate unsettled zeolite facies.According to experiment repeatedly, alkali of the present invention dissolves condition and is decided to be: NaOH strength of solution 2～5mol/L, and alkali dissolves 80～100 ℃ of temperature of reaction, and alkali dissolves reaction times 3～5h.Dissolve under the condition at alkali; Active bigger quartz and cristobalite phased soln are in solution in the activation Coaseries kaolin; Calcine the mullite that forms down through 1100～1400 ℃ and be not sufficiently complete owing to crystallization, the common relatively mullite of activity is higher, and dissolving under the condition at this technological alkali has certain dissolving; Crystal grain reduces, and forms the nano level mullite crystal.In stirring is warming up to 80～100 ℃ process; The solubleness of quartz or cristobalite phase is bigger; But mullite crystal is not dissolving almost; But the pattern of mullite crystal just begins to change after alkali dissolves reaction beginning certain hour, and reach the Al in 2～5h afterreaction system when the reaction times
2O
3/ SiO
2Ratio tends towards stability, and forms the single-phase powder of nano mullite, and solubilizing reaction finishes.In the reaction process when noticing that alkali dissolves the solubilizing reaction influence of condition to quartz or cristobalite phase; Also should dissolve condition according to the morphology change control alkali of mullite crystal; Avoid part crystal excessive dissolution or crystalline regrowth, also should note avoiding the generation of dephasigns such as zeolite.
Compare with existing preparation method; The present invention utilizes the chemical ingredients and the thing phase composite advantage of Coaseries kaolin; Strict control presoma calcining and activating and alkali dissolve technology, thereby brilliant granularity and the purity of control nano mullite is prepared single phase nano level mullite powder.Products obtained therefrom of the present invention is the single phase nano mullite powder, and raw materials used be natural mineral, equipment is simple, the cycle is short, is fit to industrial production.
Thereby the present invention is simple for process, easy handling, less energy consumption, equipment is simple, reaction time is short and raw material resources are abundant, cheap being easy to get.The nano mullite powder of preparing is well-crystallized's column crystal, and crystallographic dimension is even, and all below 200nm, diameter is all below 55nm for length.
Description of drawings
Fig. 1 is the XRD figure of kaolin raw material among the embodiment 1～3.
Fig. 2 is the XRD figure of coal gangue raw material among the embodiment 4.
Fig. 3 is the XRD analysis figure of the embodiment of the invention 1 to embodiment 4 prepared powder.
Fig. 4 is the SEM figure of the embodiment of the invention 1 prepared powder.
Fig. 5 is the TEM figure of the embodiment of the invention 4 prepared powders.
Embodiment
Embodiment 1
Activation kaolin: with kaolin is raw material, rises to 1000 ℃ with the temperature rise rate of 10 ℃/min, and the temperature rise rate with 5 ℃/min rises to 1400 ℃ again, naturally cooling behind the insulation 2h.
10g is a benchmark with activation kaolin, gets NaOH 16g, zero(ppm) water 100mL; Activation kaolin is put into the beaker that NaOH solution is housed, stir with glass stick; Beaker sealed to be placed on the magnetic force heating stirrer stir intensification; When temperature when room temperature rises to 100 ℃, beaker moved in 100 ℃ the water-bath, carry out the thermostat(t)ed water thermal response; Take out beaker behind the 4h, the powder in the beaker is carried out thorough washing to neutral, vacuum filtration also can obtain nano mullite powder behind 105 ℃ of following complete dryinies.
Embodiment 2
Activation kaolin: with kaolin is raw material, rises to 1000 ℃ with the temperature rise rate of 10 ℃/min, and the temperature rise rate with 5 ℃/min rises to 1400 ℃ again, naturally cooling behind the insulation 2h.
10g is a benchmark with activation kaolin, gets NaOH 12g, zero(ppm) water 100mL; Activation kaolin is put into the beaker that NaOH solution is housed, stir with glass stick; Beaker sealed to be placed on the magnetic force heating stirrer stir intensification; When temperature when room temperature rises to 80 ℃, beaker moved in 80 ℃ the water-bath, carry out the thermostat(t)ed water thermal response; Take out beaker behind the 5h, the powder in the beaker is carried out thorough washing to neutral, vacuum filtration also can obtain nano mullite powder behind 105 ℃ of following complete dryinies.
Embodiment 3
Activation kaolin: with kaolin is raw material, rises to 1000 ℃ with the temperature rise rate of 10 ℃/min, and the temperature rise rate with 5 ℃/min rises to 1400 ℃ again, naturally cooling behind the insulation 2h.
10g is a benchmark with activation kaolin, gets NaOH 16g, zero(ppm) water 100mL; Activation kaolin is put into the beaker that NaOH solution is housed, stir with glass stick; Beaker sealed to be placed on the magnetic force heating stirrer stir intensification; When temperature when room temperature rises to 100 ℃, beaker moved in 100 ℃ the water-bath, carry out the thermostat(t)ed water thermal response; Take out beaker behind the 3h, the powder in the beaker is carried out thorough washing to neutral, vacuum filtration also can obtain nano mullite powder behind 105 ℃ of following complete dryinies.
Embodiment 4
Active coal gangue: with the coal gangue is raw material, and raw material with crusher in crushing and with the abundant fine grinding of vibration mill, is risen to 900 ℃ with the powder that obtains after the fine grinding with the temperature rise rate of 10 ℃/min, insulation 3h, naturally cooling;
With mass concentration 20% hydrochloric acid; Mix with calcining back powder according to liquid-solid ratio 4: 1; And constant temperature stirs under 80 ℃ of conditions, and is extremely neutral with the zero(ppm) water repetitive scrubbing to powder behind the 1h, and suction filtration and dry back rise to 1150 ℃ with the temperature rise rate of 10 ℃/min; Naturally cooling behind the insulation 2h gets active coal gangue;
Active coal gangue 10g with behind the ball milling is a benchmark, gets NaOH 8g, zero(ppm) water 100mL; Active coal gangue is put into the beaker that NaOH solution is housed, stir with glass stick; Beaker sealed to be placed on the magnetic force heating stirrer stir intensification; When temperature rises to 80 ℃, beaker moved in 80 ℃ the water-bath, carry out the thermostat(t)ed water thermal response; Take out beaker behind the 3h, the powder in the beaker is carried out thorough washing to neutral, vacuum filtration also can obtain nano mullite powder behind 105 ℃ of following complete dryinies.
The embodiment interpretation of result
To the nano mullite powder that the present invention utilizes Coaseries kaolin to prepare, utilization powder crystal X-ray diffraction (XRD), transmission electron microscope (TEM) and sem means such as (SEM) are analyzed.
As shown in Figure 1, be the XRD figure of kaolin raw material among the embodiment 1～3, Fig. 2 is the XRD figure of coal gangue raw material among the embodiment 4, and among Fig. 2, K is a kaolin, and Q is quartzy.
The result shows; Embodiment 1～4 prepared powder is a mullite crystal; Be illustrated in figure 3 as the XRD analysis figure of the embodiment of the invention 1 to embodiment 4 prepared powder; Among Fig. 3, be respectively the XRD analysis figure of embodiment 1, embodiment 2, embodiment 3 and embodiment 4 prepared powders from bottom to top, wherein the nano mullite crystal structure Du Genggao of the relative coal gangue preparation of the nano mullite crystal prepared of kaolin.
Be illustrated in figure 4 as the SEM figure of the embodiment of the invention 1 prepared powder, the mullite crystal of kaolin preparation is well-crystallized's a styloid, and all below 200nm, diameter is all below 55nm for length.
Be illustrated in figure 5 as the TEM figure of the embodiment of the invention 4 prepared powders; In the nano mullite powder of coal gangue preparation; Exist the uniform short cylinder crystal of taking measurements greatly; These crystal lengths are about 30～70nm, width is about 10～20nm, and other has the littler styloid of size to appear at around the big styloid, and the trend of the oriented outgrowth of the incomplete little styloid of this growth.
What should explain at last is: obviously, the foregoing description only be for clearly the present invention is described and is done for example, and be not qualification to embodiment.For the those of ordinary skill in affiliated field, on the basis of above-mentioned explanation, can also make other multi-form variation or change.Here need not also can't give exhaustive to all embodiments.And conspicuous variation of being amplified out thus or change still are among protection scope of the present invention.
Claims (4)
1. a method of utilizing Coaseries kaolin to prepare nano mullite powder is characterized in that, said method is raw material for utilizing Coaseries kaolin, and raw material is carried out calcining and activating, dissolves reaction through alkali again, prepares nano mullite powder.
2. the method for utilizing Coaseries kaolin to prepare nano mullite powder as claimed in claim 1 is characterized in that: said Coaseries kaolin is kaolin or coal gangue.
3. the method for utilizing Coaseries kaolin to prepare nano mullite powder as claimed in claim 2 is characterized in that, is raw material with kaolin, and concrete steps are:
1), raw material calcining and activating: kaolin powder is incubated 2～4h down at 1100～1400 ℃, and naturally cooling gets activation kaolin;
2), alkali dissolves reaction: the NaOH strength of solution is 2～5mol/L, by NaOH solution and activation kaolin than being the standard of 7～10mL/g; Activation kaolin is put into NaOH solution; Stir through the magnetic force heating stirrer and to be warming up to 80～100 ℃; Carry out arrest reaction 3～5h, thorough washing promptly obtains nano mullite powder to neutral after the vacuum filtration drying.
4. the method for utilizing Coaseries kaolin to prepare nano mullite powder as claimed in claim 2 is characterized in that, is raw material with the coal gangue, and concrete steps are:
1), raw material calcining and activating:
(1) coal gangue is just handled: coal gangue is broken, fully fine grinding;
(2) coal gangue carbonization treatment: the coal gangue powder is incubated 3～5h, naturally cooling down at 800～1000 ℃;
(3) the coal gangue deironing is handled: be 15～35% hydrochloric acid with mass concentration; Mix with the coal gangue powder of carbonization treatment according to 4: 1 to 6: 1 ratio of liquid-solid ratio; Under 70～90 ℃ of conditions, carry out constant temperature and stir, extremely neutral with the zero(ppm) water repetitive scrubbing to powder behind 1～2h, suction filtration is also dry;
(4) calcining and activating: deironing coal gangue powder is incubated 2～4h down at 1100～1400 ℃, and naturally cooling gets active coal gangue;
2), alkali dissolves reaction: the NaOH strength of solution is 2～5mol/L, by NaOH solution and active coal gangue than being the standard of 7～10mL/g; Active coal gangue is put into NaOH solution; Stir through the magnetic force heating stirrer and to be warming up to 80～100 ℃; Carry out arrest reaction 3～5h, thorough washing promptly obtains nano mullite powder to neutral after the vacuum filtration drying.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967196A (en) * | 2016-05-05 | 2016-09-28 | 江西理工大学 | Method for synthesis of sodalite from kaolinite |
| CN106904955A (en) * | 2017-01-17 | 2017-06-30 | 安徽理工大学 | A kind of method with gangue as raw material molten-salt growth method low temperature mullite synthesizing powder |
| CN108017405A (en) * | 2017-11-22 | 2018-05-11 | 马鞍山科润冶金材料有限公司 | A kind of preparation method of In-situ Mullite Whisker ceramic material |
| CN109455733A (en) * | 2018-12-29 | 2019-03-12 | 东北大学 | A kind of method of gangue electrothermal way preparation high-quality mullite |
| CN109970434A (en) * | 2019-04-17 | 2019-07-05 | 郑州市新郑梅久实业有限公司 | A kind of ceramsite sand and its production technology |
| CN110436907A (en) * | 2019-08-26 | 2019-11-12 | 湖南德景源科技有限公司 | A method of utilizing preparing mullite from gangue |
| CN113912414A (en) * | 2021-10-28 | 2022-01-11 | 韶关学院 | Method for preparing mullite porous heat-insulating material by using coal gangue |
| CN114272916A (en) * | 2022-01-06 | 2022-04-05 | 中国科学院宁波材料技术与工程研究所 | High-catalytic-activity mullite material, and preparation method and application thereof |
| CN117550617A (en) * | 2023-12-29 | 2024-02-13 | 安徽金岩高岭土新材料股份有限公司 | Technology for preparing mullite by taking coal-series kaolinite as raw material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105967196A (en) * | 2016-05-05 | 2016-09-28 | 江西理工大学 | Method for synthesis of sodalite from kaolinite |
| CN106904955B (en) * | 2017-01-17 | 2020-04-03 | 安徽理工大学 | Method for synthesizing mullite powder at low temperature by using coal gangue as raw material through molten salt growth method |
| CN106904955A (en) * | 2017-01-17 | 2017-06-30 | 安徽理工大学 | A kind of method with gangue as raw material molten-salt growth method low temperature mullite synthesizing powder |
| CN108017405A (en) * | 2017-11-22 | 2018-05-11 | 马鞍山科润冶金材料有限公司 | A kind of preparation method of In-situ Mullite Whisker ceramic material |
| CN109455733A (en) * | 2018-12-29 | 2019-03-12 | 东北大学 | A kind of method of gangue electrothermal way preparation high-quality mullite |
| CN109970434A (en) * | 2019-04-17 | 2019-07-05 | 郑州市新郑梅久实业有限公司 | A kind of ceramsite sand and its production technology |
| CN109970434B (en) * | 2019-04-17 | 2021-09-24 | 郑州市新郑梅久实业有限公司 | Ceramsite sand and production process thereof |
| CN110436907A (en) * | 2019-08-26 | 2019-11-12 | 湖南德景源科技有限公司 | A method of utilizing preparing mullite from gangue |
| CN113912414A (en) * | 2021-10-28 | 2022-01-11 | 韶关学院 | Method for preparing mullite porous heat-insulating material by using coal gangue |
| CN114272916A (en) * | 2022-01-06 | 2022-04-05 | 中国科学院宁波材料技术与工程研究所 | High-catalytic-activity mullite material, and preparation method and application thereof |
| CN114272916B (en) * | 2022-01-06 | 2022-07-12 | 中国科学院宁波材料技术与工程研究所 | High-catalytic-activity mullite material, and preparation method and application thereof |
| CN117550617A (en) * | 2023-12-29 | 2024-02-13 | 安徽金岩高岭土新材料股份有限公司 | Technology for preparing mullite by taking coal-series kaolinite as raw material |
| CN117550617B (en) * | 2023-12-29 | 2024-07-16 | 安徽金岩高岭土新材料股份有限公司 | Technology for preparing mullite by taking coal-series kaolinite as raw material |
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Application publication date: 20120919 |