CN102107878B - 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 PDF

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CN102107878B
CN102107878B CN2010105375087A CN201010537508A CN102107878B CN 102107878 B CN102107878 B CN 102107878B CN 2010105375087 A CN2010105375087 A CN 2010105375087A CN 201010537508 A CN201010537508 A CN 201010537508A CN 102107878 B CN102107878 B CN 102107878B
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fly ash
flyash
grog
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张雪峰
贾晓林
郭俊温
杨文焕
林忠
贺通
张宏微
张凯丰
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Zhengzhou University
Inner Mongolia University of Science and Technology
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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

Alkali melts-method of the synthetic coal ash zeolite of microwave method
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 the industrial solid castoff synthetic zeolite from flyash.
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 year by year ascendant trend.According to relevant, the utilization ratio of China's flyash is mainly used in building 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 synthetic zeolite from flyash.
The research of synthetic zeolite from flyash begins to have so far the history in more than 20 year from Holler and Wrisching.At present, the technology of utilizing synthetic zeolite from flyash is comparative maturity, its main synthetic method has hydrothermal synthesis method, microwave-assisted synthesis method, preparation, the hot method of salt, mixed alkali gas phase synthesis method, trace water system solid-phase synthesis etc., but the existing synthetic method shortcomings such as also long, high cost of ubiquity reaction times, zeolite low conversion rate, product performance be 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 large, zeolite low conversion rate (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 hydrothermal synthesis method, although improved the speed of flyash crystallization process, greatly shortened generated time, reduced to a certain extent synthetic cost, but still can't break away from the problem of the intrinsic existence of traditional hydrothermal synthesis method, the low conversion rate of zeolite product.Preparation can make the silane agent major part in the flyash be converted into zeolite, do not contain mullite and quartz in the product, greatly improved the utilization ratio of flyash, and can obtain the higher zeolite of purity by regulating silica alumina ratio and optimizing synthesis condition, but the 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 processes badly easily to environment, and temperature of reaction is high, the performance of zeolite product is also desirable not to the utmost.Mixed alkali gas phase synthesis method can comprise the most of silane agent in the flyash that mullite is cancrinite with quartz crystals Substance Transformation mutually, is a kind of comparatively easy synthetic method, but there are the 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 high, 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) sodium hydroxide powder and step 1) in the flyash of ball milling after sieving 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 is then lower dry 1～2 hour at 100 ℃ with resulting solid water mixture;
4) with step 3) in the resulting mixture plumbago crucible of packing into, in atmosphere furnace, pass into nitrogen with the speed of 0.05～1L/min, 600～700 ℃ of roasting temperatures 45～75 minutes, cool to room temperature with the furnace and obtain alkali fusion flyash grog;
5) with step 4) in obtain grog and be ground to powder after, 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 3Then)=1.44～2.16 add the 4A zeolite seed crystal, and add-on is grog in mass ratio: 4A zeolite seed crystal=100: 1-10, and stir ageing 8～16 hours;
6) with step 5) in the mixture that obtains 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 take flyash as main raw material, take NaOH as activator, 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 occur, 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, greatly shortened the crystallization time of zeolite.The method has been avoided the shortcoming of existing synthetic zeolite from flyash 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, the 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 the standby synthetic zeolite of coal ash for manufacturing.
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 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:
EXAMPLE l:
Flyash is chosen from suburbs, packet header the 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 l: 1, ultra-sonic dispersion 10 minutes, then that resulting solid water mixture is lower dry 1 hour at 100 ℃;
(4) resulting mixture in the step (3) is packed into plumbago crucible passes into nitrogen in 600 ℃ of lower 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 in mass ratio grog: the ratio of 4A zeolite seed crystal=100: l is mixed, and stirs ageing 8 hours;
(6) in 90～100 ℃ of lower crystallization 5 minutes, be washed with water to pH value was 7～8 to the mixture that ageing in the step (5) is good, obtains the zeolite product 100 ℃ of lower dryings after 6 hours in microwave oven.
The XRD figure spectrum of the coal ash zeolite that above-mentioned technique is synthetic 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 then lower dry 2 hours at 100 ℃ with resulting solid water mixture;
(4) resulting mixture in the step (3) is packed into plumbago crucible passes into nitrogen in 650 ℃ of lower 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 in mass ratio grog: 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 lower crystallization 15 minutes, is washed with water to pH most 7～8, obtain the zeolite product at 100 ℃ after lower dry 6 hours in microwave oven.
The XRD figure spectrum of the coal ash zeolite that above-mentioned technique is synthetic 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 then lower dry 1.5 hours at 100 ℃ with resulting solid water mixture;
(4) resulting mixture in the step (3) is packed into plumbago crucible passes into nitrogen in 700 ℃ of lower 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 in mass ratio grog: 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 lower crystallization 20 minutes, is washed with water to pH most 7～8, obtain the zeolite product at 100 ℃ after lower dry 6 hours in microwave oven.
The XRD figure spectrum of the coal ash zeolite that above-mentioned technique is synthetic 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 the first heat power plant)
Figure GSB00000934986000041
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)
Figure GSB00000934986000052

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) sodium hydroxide powder and step 1) in the flyash of ball milling after sieving 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 is then lower dry 1～2 hour at 100 ℃ with resulting solid water mixture;
4) with step 3) in the resulting mixture plumbago crucible of packing into, in atmosphere furnace, pass into nitrogen with the speed of 0.05～1L/min, 600～700 ℃ of roasting temperatures 45～75 minutes, cool to room temperature with the furnace and obtain alkali fusion flyash grog;
5) with step 4) in obtain grog and be ground to powder after, 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 3Then)=1.44～2.16 add the 4A zeolite seed crystal, and add-on is grog in mass ratio: 4A zeolite seed crystal=100: 1～10, and stir ageing 8～16 hours;
6) with step 5) in the mixture that obtains 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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