CN102107878A - Method for synthesizing fly ash zeolite by alkali fusion-microwave process - Google Patents
Method for synthesizing fly ash zeolite by alkali fusion-microwave process Download PDFInfo
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- CN102107878A CN102107878A CN2010105375087A CN201010537508A CN102107878A CN 102107878 A CN102107878 A CN 102107878A CN 2010105375087 A CN2010105375087 A CN 2010105375087A CN 201010537508 A CN201010537508 A CN 201010537508A CN 102107878 A CN102107878 A CN 102107878A
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Abstract
The invention relates to a method for synthesizing fly ash zeolite by an alkali fusion-microwave process, particularly a method for synthesizing zeolite by utilizing industrial solid waste fly ash. In the invention, fly ash is used as a main raw material, NaOH is used as an activating agent, and an alkali fusion-microwave process is used for preparing the zeolite product. In the method, an ultrasonic dispersion process enables the activating agent to sufficiently contact the fly ash, and calcination enables the fusion reaction of the fly ash and the activating agent at high temperature, thereby increasing the conversion rate of the zeolite; the introduction of the 4A zeolite can enhance the purity of the 4A fly ash zeolite and reduce the generation of impure crystals; and microwaves are used for heating in the crystallization process, thereby greatly shortening the crystallization time of the zeolite. The method is simple to operate, has the advantages of simple equipment, short reaction time and energy saving, is convenient, feasible and practical, is suitable for industrial production of synthetic zeolite from fly ash, and develops a new way for comprehensive and cyclic utilization of fly ash.
Description
Technical field:
The present invention relates to a kind of alkali melts-and microwave method is synthesized the method for coal ash zeolite, specifically, mainly is the method for utilizing industrial solid castoff flyash synthetic zeolite.
Background technology:
Flyash is a kind of particulate dispersed industrial solid castoff behind the pulverized coal friring, and its major ingredient is SiO
2And Al
2O
3, the total content of the two is more than 70%.At present, the quantity discharged of the annual flyash of China surpasses 1.6 hundred million tons, and is ascendant trend year by year.According to relevant, China's utilization of coal ash rate is mainly used in and builds the road, builds brickmaking and soil improvement etc. less than 40% at present.Flyash has the volcanic ash characteristic, is to make flyash turn waste into wealth, obtain the effective way of high value added product with the flyash synthetic zeolite.
The research of flyash synthetic zeolite begins the history in existing more than 20 year so far from Holler and Wrisching.At present, the technology of utilizing the flyash synthetic zeolite is comparative maturity, its main synthetic method has hydrothermal synthesis method, microwave-assisted synthesis method, alkali fusion method, the hot method of salt, mixes alkali gas phase synthesis method, trace water system solid-phase synthesis etc., but existing synthetic method shortcomings such as also the ubiquity reaction times is long, cost is too high, the zeolite transformation efficiency is low, product performance are not ideal enough.
Hydrothermal synthesis method is present widely used a kind of prior synthesizing method, but its exist aging take long, temperature of reaction is high, energy consumption is big, zeolite transformation efficiency low (a large amount of quartz and mullites can not dissolve in the flyash) and zeolite product be with shortcomings such as by product generations.Microwave assisting method is to be based upon on the basis of traditional water thermal synthesis method, though improved the speed of flyash crystallization process, shortened generated time greatly, reduced synthetic cost to a certain extent, but still can't break away from the problem of the intrinsic existence of traditional water thermal synthesis method, the transformation efficiency of zeolite product is low.The alkali fusion method can make the silane agent major part in the flyash be converted into zeolite, do not contain mullite and quartz in the product, improved the utilization of coal ash rate greatly, and can obtain the higher zeolite of purity by regulating silica alumina ratio and optimizing synthesis condition, but this method activates, the heated and stirred time is longer, when reacting in non-encloses container, the moisture in the reaction system is volatile to be fallen.Though the hot method of salt need not add water in the salt thermal process, contain a large amount of salt in its synthetics, its product needed is washed with a large amount of water, as handles and badly easily environment is polluted, and the performance of temperature of reaction height, zeolite product is also desirable not to the utmost.Mixing the alkali gas phase synthesis method and the most of silane agent in the flyash can be comprised that mullite is converted into cancrinite with quartz crystals material mutually, is a kind of comparatively easy synthetic method, but there are shortcomings such as length consuming time, efficient are low in it.Trace water system solid-phase synthesis since in the reaction system water yield few, mix inhomogeneously, so be difficult to react completely, flyash transformation efficiency and zeolite product performance are all undesirable.
Summary of the invention
The object of the present invention is to provide a kind of zeolite transformation efficiency height, crystallization time is short, and the alkali that cost is low melts-method of the synthetic coal ash zeolite of microwave method.
Technical solution: the inventive method step is as follows:
1) flyash is carried out ball milling, and cross 200 order molecular sieves;
2) flyash after ball milling sieves in sodium hydroxide powder and the step 1) is by 1~1.4: 1 mass ratio mixes;
3) to step 2) mixture in add entry, solid-to-liquid ratio is 1: 1~5, ultra-sonic dispersion 5~20 minutes, then with resultant solid water mixture 100 ℃ dry 1~2 hour down;
4) resulting mixture in the step 3) is packed into plumbago crucible in atmosphere furnace, feeds nitrogen with the speed of 0.05~1L/min, 600~700 ℃ of roasting temperatures 45~75 minutes, cools to room temperature with the furnace and obtains alkali fusion flyash grog;
5) with after obtaining grog in the step 4) and being ground to powder, be that 1: 5~15 ratio adds entry in solid-to-liquid ratio, add sodium aluminate and adjust silica alumina ratio extremely: n (SiO
2)/n (Al
2O
3)=1.44~2.16 add particle diameter then: 0.4~0.6 purpose 4A zeolite seed crystal, add-on by quality than grog: 4A zeolite seed crystal=100: 1-10, and stir ageing 8~16 hours;
6) with the mixture that obtains in the step 5) in microwave oven under 90~100 ℃ of temperature crystallization after washing, drying, obtain the zeolite product after 5~30 minutes.
Flyash main component of the present invention includes: SiO
2, Al
2O
3, all the other are impurity, wherein: press mass percent, SiO
2And Al
2O
3Total content 〉=70%.
The present invention is a main raw material with flyash, is activator with NaOH, adopt alkali melt-microwave method prepared zeolite product.Ultrasonic dispersion makes activator fully contact with flyash in the method, and calcining makes flyash and activator that frit reaction at high temperature take place, and has improved the transformation efficiency of zeolite; The 4A zeolite seed crystal is introduced, and can improve the purity of 4A coal ash zeolite, reduces the generation of stray crystal; In crystallization process, use microwave heating, shortened the crystallization time of zeolite greatly.This method has been avoided the shortcoming of existing flyash synthetic zeolite method, coal ash zeolite product purity and transformation efficiency have been improved, have easy and simple to handle, equipment is simple, reaction times is short, advantage such as save energy and non-secondary pollution is a kind of simple and feasible practical approach, is applicable to the suitability for industrialized production of fly-ash Preparation synthetic zeolite.
The present invention is the comprehensive utilization of resources to industrial solid castoff, has not only reduced the production cost of zeolite, has reduced environmental pollution, and disposes for flyash and to have opened up a new way.Utilize industrial residue to belong to environmental protection project, can also enjoy the treatment of reduction or remission of taxes, reduce the production cost of zeolite.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is the coal ash zeolite XRD diffractogram of the embodiment of the invention 1;
Fig. 3 is the coal ash zeolite XRD diffractogram of the embodiment of the invention 2;
Fig. 4 is the coal ash zeolite XRD diffractogram of the embodiment of the invention 3.
Embodiment
Use XRD and xrf analysis method to analyze testing used flyash, main component includes in the flyash: SiO
2And Al
2O
3, wherein: SiO
2And Al
2O
3Total content 〉=70% (mass percent).
Utilize alkali fusion-microwave method to synthesize the method for coal ash zeolite according to the present invention, it specifically may further comprise the steps:
Embodiment 1:
Flyash is chosen from suburbs, packet header first heat power plant, and its chemical constitution is as shown in table 1.
(1) flyash is carried out ball milling, and cross 200 order molecular sieves;
(2) flyash after sieving with ball milling in plastic containers weighing sodium hydroxide powder and the step (1) mixes by 1.2: 1 mass ratio;
(3) add entry in the mixture of step (2), solid-to-liquid ratio is 1: 1, ultra-sonic dispersion 10 minutes, then with resultant solid water mixture 100 ℃ dry 1 hour down;
(4) resulting mixture in the step (3) is packed into plumbago crucible feeds nitrogen in 600 ℃ of following roastings 45 minutes in atmosphere furnace, cool to room temperature with the furnace and obtain alkali fusion flyash grog;
(5) with after obtaining grog in the step (4) and being ground to powder, taking by weighing the grog powder, is to add entry at 1: 8 by solid-to-liquid ratio, and adding sodium aluminate, to adjust silica alumina ratio be 1.6, add grog in mass ratio: the ratio of 4A zeolite seed crystal=100: 1 is mixed, and stirs ageing 8 hours;
(6) in 90~100 ℃ of following crystallization 5 minutes, being washed with water to pH value was 7~8 in microwave oven for mixture that ageing in the step (5) is good, 100 ℃ down dryings obtain the zeolite product after 6 hours.
The XRD figure spectrum of above-mentioned technology synthetic coal ash zeolite is seen accompanying drawing 2.Performance index are: CEC value: 396.5mmol/100g, specific surface area is at 468.28m
2/ g, mean pore size is at 4.114nm, and pore volume 0.3812cc/g, zeolite transformation efficiency are 70.6%.
Embodiment 2:
Flyash is chosen from Xi'an despot's bridge heat power plant, and its chemical constitution is as shown in table 2.
(1) flyash is carried out ball milling, and cross 200 order molecular sieves;
(2) flyash after sieving with ball milling in plastic containers weighing sodium hydroxide powder and the step (1) mixes by 1.3: 1 mass ratio;
(3) add entry in the mixture of step (2), solid-to-liquid ratio is 1: 3, and ultra-sonic dispersion 15 minutes is following dry 2 hours at 100 ℃ with resultant solid water mixture then;
(4) resulting mixture in the step (3) is packed into plumbago crucible feeds nitrogen in 650 ℃ of following roastings 60 minutes in atmosphere furnace, cool to room temperature with the furnace and obtain alkali fusion flyash grog;
(5) with after obtaining grog in the step (4) and being ground to powder, taking by weighing the grog powder, is to add entry at 1: 12 by solid-to-liquid ratio, and adding sodium aluminate, to adjust silica alumina ratio be 2, add grog in mass ratio: the ratio of 4A zeolite seed crystal=100: 5 is mixed, and stirs ageing 12 hours;
(6) mixture that ageing in the step (5) is good in 90~100 ℃ of following crystallization 15 minutes, is washed with water to pH most 7~8, obtain the zeolite product after dry 6 hours down at 100 ℃ in microwave oven.
The XRD figure spectrum of above-mentioned technology synthetic coal ash zeolite is seen accompanying drawing 3.Performance index are: CEC value: 423.8mmol/100g, specific surface area is at 476.4m
2/ g, mean pore size is at 4.126nm, and pore volume 3.952cc/g, zeolite transformation efficiency are 72.1%.
Embodiment 3:
Flyash is chosen from Luoyang, Henan power plant, and its chemical constitution is as shown in table 3.
(1) flyash is carried out ball milling, and cross 200 order molecular sieves;
(2) flyash after sieving with ball milling in plastic containers weighing sodium hydroxide powder and the step (1) mixes by 1.4: 1 mass ratio;
(3) add entry in the mixture of step (2), solid-to-liquid ratio is 1: 5, and ultra-sonic dispersion 20 minutes is following dry 1.5 hours at 100 ℃ with resultant solid water mixture then;
(4) resulting mixture in the step (3) is packed into plumbago crucible feeds nitrogen in 700 ℃ of following roastings 75 minutes in atmosphere furnace, cool to room temperature with the furnace and obtain alkali fusion flyash grog;
(5) with after obtaining grog in the step (4) and being ground to powder, taking by weighing the grog powder, is to add entry at 1: 14 by solid-to-liquid ratio, and adding sodium aluminate, to adjust silica alumina ratio be 2.1, add grog in mass ratio: the ratio of 4A zeolite seed crystal=100: 10 is mixed, and stirs ageing 14 hours;
(6) mixture that ageing in (5) is good in 90~100 ℃ of following crystallization 20 minutes, is washed with water to pH most 7~8, obtain the zeolite product after dry 6 hours down at 100 ℃ in microwave oven.
The XRD figure spectrum of above-mentioned technology synthetic coal ash zeolite is seen accompanying drawing 4.Performance index are: CEC value: 416.3mmol/100g,
Specific surface area is at 472m
2/ g, mean pore size is at 4.121nm, and pore volume 3.824cc/g, zeolite transformation efficiency are 71.2%.
Table 1 chemical composition of PCA/wt% (taking from suburbs, packet header first heat power plant)
Table 2 chemical composition of PCA/wt% (taking from Xi'an despot's bridge heat power plant)
Table 3 chemical composition of PCA/wt% (taking from Luoyang, Henan power plant)
Claims (2)
1. alkali melts-method of the synthetic coal ash zeolite of microwave method, and it is characterized in that: method steps is as follows:
1) flyash is carried out ball milling, and cross 200 order molecular sieves;
2) flyash after ball milling sieves in sodium hydroxide powder and the step 1) is by sodium hydroxide powder: flyash=1~1.4: 1 mass ratio mixes;
3) to step 2) mixture in add entry, solid-to-liquid ratio is 1: 1~5, ultra-sonic dispersion 5~20 minutes, then with resultant solid water mixture 100 ℃ dry 1~2 hour down;
4) resulting mixture in the step 3) is packed into plumbago crucible in atmosphere furnace, feeds nitrogen with the speed of 0.05~1L/min, 600~700 ℃ of roasting temperatures 45~75 minutes, cools to room temperature with the furnace and obtains alkali fusion flyash grog;
5) with after obtaining grog in the step 4) and being ground to powder, be that 1: 5~15 ratio adds entry in solid-to-liquid ratio, add sodium aluminate and adjust silica alumina ratio extremely: n (SiO
2)/n (Al
2O
3)=1.44~2.16 add particle diameter then: 0.4~0.6 purpose 4A zeolite seed crystal, add-on by quality than grog: 4A zeolite seed crystal=100: 1~10, and stir ageing 8~16 hours;
6) with the mixture that obtains in the step 5) in microwave oven under 90~100 ℃ of temperature crystallization after washing, drying, obtain the zeolite product after 5~30 minutes.
2. alkali according to claim 1 melts-method of the synthetic coal ash zeolite of microwave method, it is characterized in that the flyash main component includes: SiO
2, Al
2O
3, all the other are impurity, wherein: press mass percent, SiO
2And Al
2O
3Total content 〉=70%.
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