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Advanced Materials Research Vol. 549 (2012) pp 762-765 Online available since 2012/Jul/09 at www.scientific.net © (2012) Trans Tech Publications, Switzerland doi:10.4028/www.scientific.net/AMR.549.762

Semi-dry desulfurization ash modification and application in autoclaved brick Fu Ying-li1,a, Mu Yan1,b , Zhao Feng-qing1,3,c
1 2

Chemical Department, Hebei University of Sci.&Tec. , Shijiazhuang 050018 P.R. China

Hebei Research Center of Pharmaceutical and Chemical Engineering, Shijiazhuang, P.R. China
3

Hebei Engineering and Research Center of Solid Waste Utilization, Shijiazhuang, P.R. China

a

dreamslink0809@126.com, btoto8001@gmail.com,czhaofq3366@126.com (corresponding author)

Keywords: Semi-dry desulfurization ash, calcium sulfite, modification, autoclaved brick

Abstract. The modification of calcium sulfite in semi-dry desulfurization ash was studied. By the combining use of catalyst and oxidant, the content of calcium sulfite in the modified desulfurized ash was greatly reduced. In this way, the calcium oxide and calcium sulfate in the modified desulfurization ash were used to partially replace the lime, gypsum and other materials in the process of autoclaved brick production. The hydration reaction mechanism was discussed. Introduction It is common knowledge that sulfur dioxide is a main cause of acid rain. Removal of SO2 from flue gas emitted in the combustion of fossil fuels has been a worldwide concern since the 1970s [1]. To minimize the negative environment impact of SO2 emissions, much effort has been put on the development of flue gas desulfurization (FDG) technologies over the past decades [2,5].With the desulphurization system in install continually, more and more the desulfurization ash is produced, and the comprehensive utilization of desulfurization ash has become a serious problem to be solved. The semi-dry desulfurization ash has a complicated composition with higher content of calcium sulfite, which is harmful to construction and building materials. In this article the Catalytic Oxidation of calcium sulfite in desulfurization ash was investigated, aiming to oxidize the calcium sulfite in the semi-dry desulfurization ash partially. In this way, the calcium oxide and calcium sulfate in the modified desulfurization ash can be used to replace lime, gypsum and other materials in the production of autoclaved bricks. Experimental Materials.The desulfurization ash used in this paper is supplied by Fengfeng power plant with the composition: CaO-43.11%,MgO-3.28%, SiO2 -18.34%, Fe2O3 -0.60%, Al2O3-0.076%, SO3-2.25% and ignition loss of 17.0%. The fly ash is from Xibaipo Power Plant with the composition: SiO2 -56.5%, Al2O3 -25.3%, Fe2O3-1.68%, CaO-4.71%, MgO-1.24%, SO3 -0.69%, and ignition loss of 6.79%. The lime is from Jingxing Chemicals with 67% of CaO. The sand used is river sand with not over 5.0 mm particle size with the fineness modulus of 2.6. Catalysts used in this work are TiO2, MnO2, Al2O3, Cr2O3,Fe2O3 and V2O5. The Oxidant is hydrogen peroxide. Modification of the desulfurization ash.Appropriate amounts of catalyst, oxidant and water were added to the desulfurization ash with the water-solid ratio of 0.10. After mixed evenly, the mixture was pressed formed at 20 MPa. The specimen was autoclaved 6 hours at 174.5℃ in the autoclave. The conversion of calcium sulfite in the desulfurization ash was determined after the specimen was ground and dried. Autoclaved brick from the modified desulfurization ash.Fixed amounts of catalyst (2.0%) and oxidant (0.20%) were added to the modified desulfurization ash. Then the desulfurization ash is mixed evenly with fly ash, lime, gypsum, water and others. The mixed materials were pressed to produce bricks at 20 MPa, then cured at 174.5℃ for 6 hours in the autoclave, the mechanical strength was tested.
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Results and discussion Effects of catalyst.On the condition of low temperature and dry atmosphere, calcium sulfite will hardly be oxidized to calcium sulfate. However, the addition of catalyst can promote the reaction [6,7] . We choose six metal oxides as catalysts. They were added into desulfurization ash. The effects on the calcium sulfite conversion were studied in the autoclave with fixed water-solid ratio (0.10). The results are shown in Fig. 1.

Al2O3
32 30 28

Cr2O3 M 2 nO TiO2 Fe2O3 V2O5

Conversion of CaSO3/%

26 24 22 20 18 16 14 12 10 8 0.5 1.0 1.5 2.0 2.5

The amount of catalyst /%

Fig. 1 Effects of catalysts on the conversion of calcium sulfite On the autoclaved condition, the catalyst can promote the conversion of calcium sulfite. However, the six catalysts have different effects. Though V2O5 show the best performance, its price is higher. And take the price and conversion into consideration, TiO2 behaves best. So TiO2 was chosen as the catalyst for the subsequent study. Fig.1 shows that with 2.0% TiO2 addition, the calcium sulfite conversion is 26.52%. When the dosage increased to 2.5%, the conversion increased little. So the optimal dosage of TiO2 was fixed at 2.0%. Effects of oxidant. Adding oxidants can supplement the oxygen loss in the autoclaved process. Hydrogen peroxide is preferred, because it can release oxygen and generate no harmful by-products in the process. The catalytic oxidation experiments of calcium sulfite in desulfurization ash were carried out on the autoclaved condition. After diluted to 10%, hydrogen peroxide was added to the desulfurization ash. The results were shown in Fig. 2.
44 42

Conversion of CaSO3 /%

40 38 36 34 32 30 28 26 0.00 0.05 0.10 0.15 0.20 0.25

The amount of oxidant /%

Fig. 2 Effects of the oxidant on the conversion of calcium sulfite

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Chemical Engineering and Material Properties II

With the increase of oxidant, the conversion of calcium sulfite increased. While hydrogen peroxide is corrosive to the equipment, affecting the service life of equipment, the dosage of catalyst and oxidant were fixed at 2.0% and 0.20% respectively.Under this condition, the conversion is 41.25%. Effects of modified desulfurization ash.The brick was produced in steam curing of 174.5℃ with the regime: Firstly heating for 2h, then keep the temperature for 6h, cooling for 2h. The dosage of catalyst and oxidant were fixed at 2.0% and 0.20%. The effect of modified and unmodified desulfurization ash on the mechanical strength of autoclaved bricks was shown in Table 1. Table 1 Effects of modified desulfurization ash on the strength of bricks Modified Unmodified Fly ash Lime Gypsum Sand Compressive desulfurization desulfurization /% /% /% /% Strength ash /% ash /% /MPa 20 / 40 10 2 25 13.6 / 20 40 10 2 25 10.5

No.

A1 A2

We can see clearly from the Tab. 1 that the bricks’ compressive strength made from the modified desulfurization ash is 13.6MPa, and can meet the Grade MU10 of JC239-2001 (fly ash brick, China Construction Material Professional Standard). The bricks’ compressive strength made from the unmodified desulfurization was 22.8 % lower. Effects of CaO dosage.The desulfurization ash used in this study contains some CaO, which can be used to partly replace lime. The effect of lime on the strength of autoclaved brick was studied on the condition with the proportioning: fly ash- 40%, river sand-30% and water-solid ratio of 0.10. The results were given in Fig. 3
20

Compressive Flexural

15

Strength /MPa

10

5

0 0 2 4 6 8 10

The amount of lime/%

Fig. 3 Effects of CaO in modified desulfurization ash on the strength of autoclaved brick It is clear that the strength of brick increases with the amount of lime increased. The strength can reach 12.8 MPa when no lime is added. Therefore, the calcium oxide in desulfurization ash can be used to replace the lime to produce autoclaved bricks, reducing production cost and natural resources. Hydration reaction mechanism.A series of physical and chemical reaction occurred in the autoclaved process. Under hydrothermal conditions, lime will interact with fly ash, generating a series of hydration products such as hydrated calcium silicate, hydrated calcium aluminate, hydrated calcium aluminosilicate, and hydrated calcium aluminosulfate [8,9]. In temperature rising process, quick lime was hydrated into Ca(OH)2. The later interacted with the active SiO2 and Al2O3 in fly ash to generate C3AH6 slowly, then interacted with the CaSO4 to generate calcium aluminosilicate (Aft). With the temperature raised up to about 100℃, Ca(OH)2 reacts with active SiO2 to generate a high basicity hydration calcium silicate (C-S-H gel). With the

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dissolution of SiO2 sequentially, C-S-H gel produced from the hydration interacted with the lime and fly ash to generation CSH (Ⅰ). At the same time, calcium aluminosilicate (Aft) decomposed to calcium aluminosilicate (Afm). In the early stage of constant temperature, a lot of CSH (Ⅰ) formed[10]. Calcium aluminosilicate (Afm) is unstable, decomposing to form C3AH6 and CaSO4. With the extension of the constant temperature period, the crystallization of hydration calcium silicate improved continuously, and then mullite appeared. As the results, the main hydration products of the Lime-fly ash-gypsum-desulfurization ash system are CSH (Ⅰ), mullite, water garnet under the autoclave conditions. Fig. 4 is the scanning electron microscopy (SEM) photo of autoclaved brick particle. It is clear that there is a lot of flake mullite formed. Fig. 5 is the XRD diffraction spectrum of autoclaved brick particle. It is proved that the main hydration products are mullite ,CSH(Ⅰ), water garnet, as well as the un-reacted quartz and anhydrite.

Fig. 4 SEM of hydration products Summary

Fig. 5 XRD of hydration products

a. Without catalyst and oxidizer, the conversion of calcium sulfite to calcium sulfate in the desulfurization ash is only 2.14% at autoclaved conditions (175.4 ℃, autoclaved 6h). This situation can be improved significantly when the catalyst TiO2 and the oxidant H2O2 were used. With 2.0% of TiO2 and 0.20% of H2O2, the conversion reached 41.25%. b. The content of CaO and CaSO4 in modified desulfurization ash can be used to replace lime and gypsum for autoclaved brick preparation. The strength of prepared brick reached the strength grade of MU10. This approach provided a proper method to utilize semi-dry desulphurization ash. References [1] G.Xu, Q.Guo, T.Kaneko, et al, Advances in Environmental Research, Vol. 4 (2000), p. 9 [2] Cofala J, Amann M, Gyarfas F, Schoepp W, Boudri J C, Hordijk L, Kroeze C, Junfeng L, Lin D, Panwar T S, Gupta S, Environ. Manage. Vol. 72 (2004), p. 149 [3] Fernandez J, Renedo J, Garea A, Viguri J, Irabien J A, Powder Technol. Vol. 94 (1997) , p. 133 [4] Fernandez J, Renedo M J, Pesquera A, Irabien J A, Powder Technol. Vol.119(2001), p. 201 [5] Fernandez J, Renedo M J, Energ. Fuels Vol. 17(2003), p. 1330 [6] Yang Xinya, Zhang Liying, Liu Hongbo, Coal Ash China, Vol.4(2006), p. 10(In Chinese) [7] Guo Bin, Bian Jingfeng, Ren Ailing, Environmental Pollution & Control, Vol.7(2009), p. 1 (In Chinese) [8] Zhao feng-qing, zhao Jing, Liu hong-jie. Construction and Building Materials. Vol. 23(2009), p539 [9] Li Hao, Zhao feng-qing etal. Advanced Materials Research. Vol.217-218( 2010),p846 [10] H. EW.Taylor. Theehemistry of Cement. Aeademie Press, 1994

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Semi-Dry Desulfurization Ash Modification and Application in Autoclaved Brick 10.4028/www.scientific.net/AMR.549.762

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