CN100491250C - Method for preparing mullite from gangue - Google Patents
Method for preparing mullite from gangue Download PDFInfo
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- CN100491250C CN100491250C CNB2007100516570A CN200710051657A CN100491250C CN 100491250 C CN100491250 C CN 100491250C CN B2007100516570 A CNB2007100516570 A CN B2007100516570A CN 200710051657 A CN200710051657 A CN 200710051657A CN 100491250 C CN100491250 C CN 100491250C
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- coal gangue
- mullite
- gangue powder
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Abstract
This invention relates to a method for preparing mullite by calcining coal gangue. The method comprises: (1) mixing coal gangue powder and additive uniformly; (2) heating the mixed raw materials at a rate of 2-10 deg.C/min to 1300 deg.C, and keeping the temperature for 3h to obtain the product. The additive is composite catalyst of NaF and La2O3. The addition amounts of NaF and La2O3 are 1-2 wt. % and 0.1-0.5 wt. % of coal gangue powder, respectively. The method has such advantages as low energy consumption and low cost. The mullite product does not contain quartz phase that is harmful to mullite properties.
Description
Technical field
The present invention relates to a kind of method for preparing mullite by calcining coal gangue.
Technical background
Coal gangue has become China's burden and year output maximum, has taken and pile up the maximum industrial waste in place as the by product in the coal production process.And mullite (mullite) is an aluminium silicate mineral, character such as have refractoriness height, good thermal shock, chemical resistance of concrete, creep resistance, refractoriness under load height, volume stability is good, electrical insulating property is strong, be the ideal high grade refractory, it is industrial to be widely used in metallurgy, glass, pottery, chemistry, electric power, national defence, combustion gas and cement etc.Coal gangue being prepared as needed in the market M45 type mullite refractory, not only can solving the pollution problem of coal gangue stacking to environment, can also create more economic benefit, is a kind of behavior of turning waste into wealth.
The production technique of producing at present M45 is: kaolin or Coaseries kaolin 1500 ℃ of calcinings, are incubated 10 hours.Domestic only have one piece of patent report (China Patent No. be 93114925.8, " a kind of method of rejecting cristobalite in precision casting sand and the refractory materials "), kaolin directly prepares mullite, and product does not contain the cristobalite phase of damaging the mullite performance, its method is: coal series kaolin rock is through being crushed to the 40-250 order, through high-temperature calcination more than 1400 ℃ more than 8 hours, then 1300 ℃ of constant temperature 2 hours, perhaps coal series kaolin rock is through being crushed to the 40-250 order, add 1% (quality) mineralizer, 1.5% (quality) fusing assistant is calcining more than 1350 ℃ 8 hours, then 1150 ℃ of constant temperature 2 hours, mineralizer is a magnesium oxide, and fusing assistant is a calcium sulfate.
Above its main drawback of method is the energy consumption height, and cost has high input.
Summary of the invention
The object of the present invention is to provide the method for the preparing mullite from gangue that a kind of energy consumption is low, cost is low.
To achieve these goals, technical scheme of the present invention is: a kind of method of preparing mullite from gangue is characterized in that it comprises the steps:
1), coal gangue powder and outer doping are mixed, must admixtion; Described additive is NaF and La
2O
3The composite catalyst of being formed, the add-on of NaF are 1%-2% of coal gangue powder quality, La
2O
3Add-on be 1 ‰-5 ‰ of coal gangue powder quality;
2), admixtion is heated to 1300 ℃ with the speed of 2 ℃-10 ℃ of per minutes, 1300 ℃ of calcining insulations 3 hours, make at last mullite greater than 55%, do not contain the product of cristobalite phase.
Described colliery powder particle diameter is less than 200 orders (0.074mm), and alumina content is greater than 35%.
Compared with prior art, owing to adopt outer doping---NaF and La
2O
3, the present invention has following outstanding beneficial effect:
1. raw material greatly reduces the requirement to raw material for being the coal gangue of main component with kaolin, has reduced cost;
With calcining temperature from present technology greater than 1500 ℃, be reduced to 1300 ℃, reduced energy consumption;
With soaking time from 10 hours, be reduced to 3 hours, reduced energy consumption.Meanwhile, the product of preparing is gone up mutually from thing and do not contained the cristobalite phase that diminishes the mullite performance, and is approaching with the product Molochite sand of the ECC of Britain leading company on the composition.
The present invention has made full use of resource, turns waste into wealth, and reduces environmental pollution, and reaches the minimizing energy consumption, the purpose that reduces production costs by the adding of outer doping.
Description of drawings
Fig. 1 is the XRD figure spectrum of the embodiment of the invention one [Yidu City's coal gangue powder (less than 200 orders) is adding 15 ‰ Sodium Fluorides, and 5 ‰ lanthanum trioxides were 1300 ℃ of calcining insulations 3 hours] gained.
Fig. 2 is the XRD figure spectrum of the embodiment of the invention two [Yidu City's coal gangue powder (less than 200 orders) is adding 15 ‰ Sodium Fluorides, and 3 ‰ lanthanum trioxides were 1300 ℃ of calcining insulations 3 hours] gained.
Fig. 3 is the XRD figure spectrum of the embodiment of the invention three [Yidu City's coal gangue powder (less than 200 orders) is adding 18 ‰ Sodium Fluorides, and 2 ‰ lanthanum trioxides were 1300 ℃ of calcining insulations 3 hours] gained.
Fig. 4 is the XRD figure spectrum of the embodiment of the invention four [Yidu City's coal gangue powder (less than 200 orders) is adding 17 ‰ Sodium Fluorides, and 3 ‰ lanthanum trioxides were 1300 ℃ of calcining insulations 3 hours] gained.
Fig. 5 is the XRD figure spectrum of the embodiment of the invention five [Yidu City's coal gangue powder (less than 200 orders) is adding 16 ‰ Sodium Fluorides, and 4 ‰ lanthanum trioxides were 1300 ℃ of calcining insulations 3 hours] gained.
Fig. 6 is the XRD figure spectrum of the embodiment of the invention six [Yidu City's coal gangue powder (less than 200 orders) is adding 19 ‰ Sodium Fluorides, and 3 ‰ lanthanum trioxides were 1300 ℃ of calcining insulations 3 hours] gained.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment one:
Get Yidu City's coal gangue powder (less than 200 orders) 3.00g, add the Sodium Fluoride of coal gangue powder quality 15 ‰, add the lanthanum trioxide of coal gangue powder quality 5 ‰, mix, put into corundum crucible, crucible is put in the Si-Mo rod chamber type electric resistance furnace, be warming up to 1300 ℃, in the XRD figure spectrum of 3 hours gained of 1300 ℃ of calcining insulations with the speed of 4 ℃ of per minutes.Mullite is 55-60% mutually as can be seen from X ray diffracting spectrum that sample is done (Fig. 1), does not contain cristobalite, and other is an amorphous phase.
Embodiment two:
Get Yidu City's coal gangue powder (less than 200 orders) 3.00g, add the Sodium Fluoride of coal gangue powder quality 15 ‰, add the lanthanum trioxide of coal gangue powder quality 3 ‰, mix, put into corundum crucible, crucible is put in the Si-Mo rod chamber type electric resistance furnace, be warming up to 1300 ℃, in the XRD figure spectrum of 3 hours gained of 1300 ℃ of calcining insulations with the speed of 4 ℃ of per minutes.Mullite is 55-60% mutually as can be seen from X ray diffracting spectrum that sample is done (Fig. 2), does not contain cristobalite, and other is an amorphous phase.
Embodiment three:
Get Yidu City's coal gangue powder (less than 200 orders) 3.00g, add the Sodium Fluoride of coal gangue powder quality 18 ‰, add the lanthanum trioxide of coal gangue powder quality 2 ‰, mix, put into corundum crucible, crucible is put in the Si-Mo rod chamber type electric resistance furnace, be warming up to 1300 ℃, in the XRD figure spectrum of 3 hours gained of 1300 ℃ of calcining insulations with the speed of 4 ℃ of per minutes.Mullite is 55-60% mutually as can be seen from X ray diffracting spectrum that sample is done (Fig. 3), does not contain cristobalite, and other is an amorphous phase.
Embodiment four:
Get Yidu City's coal gangue powder (less than 200 orders) 3.00g, add the Sodium Fluoride of coal gangue powder quality 17 ‰, add the lanthanum trioxide of coal gangue powder quality 3 ‰, mix, put into corundum crucible, crucible is put in the Si-Mo rod chamber type electric resistance furnace, be warming up to 1300 ℃, in the XRD figure spectrum of 3 hours gained of 1300 ℃ of calcining insulations with the speed of 4 ℃ of per minutes.Mullite is 55-60% mutually as can be seen from X ray diffracting spectrum that sample is done (Fig. 4), does not contain cristobalite, and other is an amorphous phase.
Embodiment five:
Get Yidu City's coal gangue powder (less than 200 orders) 3.00g, add the Sodium Fluoride of coal gangue powder quality 16 ‰, add the lanthanum trioxide of coal gangue powder quality 4 ‰, mix, put into corundum crucible, crucible is put in the Si-Mo rod chamber type electric resistance furnace, be warming up to 1300 ℃, in the XRD figure spectrum of 3 hours gained of 1300 ℃ of calcining insulations with the speed of 4 ℃ of per minutes.Mullite is 55-60% mutually as can be seen from X ray diffracting spectrum that sample is done (Fig. 5), does not contain cristobalite, and other is an amorphous phase.
Embodiment six:
Get Yidu City's coal gangue powder (less than 200 orders) 3.00g, add the Sodium Fluoride of coal gangue powder quality 19 ‰, add the lanthanum trioxide of coal gangue powder quality 3 ‰, mix, put into corundum crucible, crucible is put in the Si-Mo rod chamber type electric resistance furnace, be warming up to 1300 ℃, in the XRD figure spectrum of 3 hours gained of 1300 ℃ of calcining insulations with the speed of 4 ℃ of per minutes.Mullite is 55-60% mutually as can be seen from X ray diffracting spectrum that sample is done (Fig. 6), does not contain cristobalite, and other is an amorphous phase.
Embodiment seven:
A kind of method of preparing mullite from gangue, it comprises the steps:
1), coal gangue powder and outer doping are mixed, must admixtion; Described additive is NaF and La
2O
3The composite catalyst of being formed, the add-on of NaF are 1% of coal gangue powder quality, La
2O
3Add-on be 1 ‰ of coal gangue powder quality; Described colliery powder particle diameter is less than 200 orders, and alumina content is greater than 35%.
2), admixtion is heated to 1300 ℃ with the speed of 2 ℃ of per minutes, 1300 ℃ of calcining insulations 3 hours, make at last mullite greater than 55%, do not contain the product of cristobalite phase.
Embodiment eight:
A kind of method of preparing mullite from gangue, it comprises the steps:
1), coal gangue powder and outer doping are mixed, must admixtion; Described additive is NaF and La
2O
3The composite catalyst of being formed, the add-on of NaF are 2% of coal gangue powder quality, La
2O
3Add-on be 5 ‰ of coal gangue powder quality; Described colliery powder particle diameter is less than 200 orders, and alumina content is greater than 35%.
2), admixtion is heated to 1300 ℃ with the speed of 10 ℃ of per minutes, 1300 ℃ of calcining insulations 3 hours, make at last mullite greater than 55%, do not contain the product of cristobalite phase.
Claims (2)
1. the method for a preparing mullite from gangue is characterized in that it comprises the steps:
1), coal gangue powder and outer doping are mixed, must admixtion; Described additive is NaF and La
2O
3The composite catalyst of being formed, the add-on of NaF are 1%-2% of coal gangue powder quality, La
2O
3Add-on be 1 ‰-5 ‰ of coal gangue powder quality;
2), admixtion is heated to 1300 ℃ with the speed of 2 ℃-10 ℃ of per minutes, 1300 ℃ of calcining insulations 3 hours, product.
2. the method for a kind of preparing mullite from gangue according to claim 1, it is characterized in that: described colliery powder particle diameter is less than 200 orders, and alumina content is greater than 35%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100516570A CN100491250C (en) | 2007-03-13 | 2007-03-13 | Method for preparing mullite from gangue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100516570A CN100491250C (en) | 2007-03-13 | 2007-03-13 | Method for preparing mullite from gangue |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101049938A CN101049938A (en) | 2007-10-10 |
| CN100491250C true CN100491250C (en) | 2009-05-27 |
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|---|---|---|---|
| CNB2007100516570A Expired - Fee Related CN100491250C (en) | 2007-03-13 | 2007-03-13 | Method for preparing mullite from gangue |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102229501A (en) * | 2011-04-21 | 2011-11-02 | 河南省冶金研究所有限责任公司 | Method for preparing cristobalite-mullite composite refractory |
| CN104947177B (en) * | 2015-05-29 | 2017-10-20 | 景德镇陶瓷大学 | One kind is without V2O5The method for preparing mullite crystal whisker with gangue and aluminium hydroxide growth in situ under the conditions of dry-pressing |
| CN106064092B (en) * | 2016-08-03 | 2018-06-26 | 荆楚理工学院 | Application of the gangue in dangerous waste is burned |
| CN106336200B (en) * | 2016-08-21 | 2019-06-11 | 长兴盟友耐火材料有限公司 | A kind of inorfil toughening refractory material and its preparation process |
| CN108558431A (en) * | 2017-12-12 | 2018-09-21 | 醴陵友立特种陶瓷有限公司 | Biological particles object borrosion hole lightweight refracrory and preparation method thereof |
| CN109455733B (en) * | 2018-12-29 | 2021-11-09 | 东北大学 | Method for preparing high-quality mullite by coal gangue electrothermal method |
| 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 |
| CN113307282B (en) * | 2021-06-25 | 2022-11-15 | 太原理工大学 | Method for synthesizing sodalite zeolite molecular sieve from coal gangue solid waste |
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2007
- 2007-03-13 CN CNB2007100516570A patent/CN100491250C/en not_active Expired - Fee Related
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| CN101049938A (en) | 2007-10-10 |
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Granted publication date: 20090527 Termination date: 20100313 |