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Further increase in the grinding times to 6 (for PAL-6, PAL-8 and PAL- 10 samples), the intensity of the characteristic diffraction peak at 2θ=8.38° (d=10.6 Å  [24] remarkably decreased and the otherpeaks had no obvious change, indicating that the repeated grinding treatment with high intensity would affect the crystal structure of PAL to certain extent and slightly reduced its order–disorder structural degree [26], which was an advantageous property for well-defined adsorbents [27], as validated by the following adsorption results for MB. The intensity of the peak at 2θ=8.38° (d=10.6 Å [24] forPAL-6 was lowest, increased for PAL-8 and decreased for PAL-10. This may be according to following reasons: for PAL-6, the crystal aggregates were dissociated and crystal rods were shortened, thusleading to large degree of destructiveness in crystal structure; for PAL-8, more stressing force acted on the sample, and then crystal structure was further affected. The crystal rods would rearrange due to minimum energy principle, leading to the crystal structure was recovered to a certain extent; whereas for PAL-10, superabundant stressing force operated on the sample, and then crystal structure was affected so serious that it was difficult to be recovered 3.4. Effect of grinding treatment on specific surface area Specific surface area is one of the most crucial physical-chemical properties of an adsorbent as to remove heavy metal ions and dyes. Liu et al. [28] found that the specific surface area of CTA+-REC had significant effect on the removal of anionic dye Congo red, and the similar results were reported by Chen et al. [29]. Thus, the effect of grinding times on specific surface area of PAL was investigated and shown in Table 1. SBET and Smicro of PAL-0 were only 153 and 28 m2/g, respectively. The SBET was greatly enhanced after grinding treatment. The SBET firstly increased to 229 m2/g for PAL-2, and then decreased to 184 m2/g for PAL-6. With further increasing the grinding times to 8, the SBET increased to 213 m2/g and kept constant. Furthermore, the tendency of Sext/SBET ratio versus grinding times was quite the reverse of the SBET and only little change in the value of Sext can be found. For PAL samples with grinding treatment, the Sext/SBET ratio increased until PAL-6 and then decreased with increasing grinding times due to the change in the SBET, indicating grinding treatment had insignificant effect on the Sext. The tendencies in Smicro and the Smicro/SBET ratio with grinding timeswere in linewith the obtained for SBET. Itwas also clearly observed that Smicro increased with the grinding times until PAL-2 and then decreased until PAL-6 and finally increased. The Smicro of PAL with grinding treatment was higher than that initial PAL-0 value. In all, the SBET of grinding treated PAL was obviously higher than that of PAL-0 due to the increase in Smicro. This was attributed to that the rod-like crystals of PAL become shorter after grinding treatment as validated by FESEMimages, which led to the increase inmicroparticles, and then resulted in the increase of Smicro 3.5. Effect of grinding treatment on pore-size distribution The pore size of an adsorbent material exhibits great influence on the adsorption capacity for dyes or metal ions, especially for adsorbates with large and complex molecular structures. In this case, the effect of grinding treatment on pore-size distribution for PAL samples was studied and illustrated in Fig. 4. As shown in the inset of Fig. 4, the first peak at about 3.5 nm for PAL-0, 3.6 nm for PAL-2 and PAL- 4, 3.8 nm for PAL-6, PAL-8 and PAL-10 was ascribed to the mesopores between layers of PAL and furthermore, as pore size was in the range of 0 and 8.0 nm, the peak area was in the order of PAL-4>PAL-2> PAL-0>PAL-6>PAL-8>PAL-10, suggesting the mesopore volume had the same sequence except PAL-0 and PAL-4. It was clear from Fig. 4 that another peak at 30 nm for PAL-0 and 28 nm for PAL-2, PAL-4, PAL-6 and PAL-8 and 29 nm for PAL-10 was corresponding to non-structural pores between microparticles of PAL. In addition, the first set of peaks were small and narrow attributed to the inner surface area, while the second set of peaks were large and broad attributed to the outer surface area of PAL. This means that the pores present an irregular size distribution [30,31]. Furthermore, the results suggested that the non-structural pores among microparticles of PAL were dominant and responsible for the large proportion of the pore volume and specific surface area. It can be also seen from Fig. 4 the non-structural pore of PAL-2, PAL-4, PAL-6, PAL-8 and PAL-10 was a little smaller than that of PAL-0. This may be due to that the change of crystal aggregates and the break of rod-like crystals of PAL. The strong compression and shearing action resulting from the stone miller disc led to the rearrangement of crystal bundles and the stack of crystals became compact, which caused a small decrease in nonstructural pores of PAL-2, PAL-4, PAL-6, PAL-8 and PAL-10 and thechange in structure of crystal aggregates. Due to strong shearing forces induced by the stone miller operating on the PAL, crystal aggregates, bundles were dissociated and part of single crystals were shortened. According to the Van der Waals forces and hydrogen bonds, part of dissociated crystal aggregates, bundles and single crystals would rearrange and part of the interstitial spaces between the crystal aggregates would change according to minimum energy principle. Under these conditions, shortened crystals would be more compact. A slight decrease of intensity in the second peak set and the increase of intensity in the first peak set with grinding treatment were observed. Thus there was a slight change in pore volume of PAL after grinding treatment and the extent in change depended on the decreasing extent in the second set of peak and increasing extent in the first set of peak |
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xiaoyingwv
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愛與雨下: 金幣+2 2012-10-20 07:10:26
oink: 金幣+30, 翻譯EPI+1, ★★★★★最佳答案 2012-10-21 15:31:21
愛與雨下: 金幣+2 2012-10-20 07:10:26
oink: 金幣+30, 翻譯EPI+1, ★★★★★最佳答案 2012-10-21 15:31:21
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將樣品的研磨次數(shù)增加到六次（PAL-6，PAL-8，PAL-10），在2θ=8.38°處的特征峰強度顯著減弱，而其他衍射峰強度 沒有明顯變化，說明高強度的重復研磨能在一定程度上影響PAL的晶型，降低PAL的有序-無序的結(jié)構比例，這是較好吸附 劑的優(yōu)良性質(zhì)，下面對MB的吸附試驗也證實了PAL的這一優(yōu)良性質(zhì)。 在2θ=8.38°處的特征峰強度，PAL-6的峰強度最低，PAL-8的峰強度增加了而PAL-10的峰強度降低了。原因可能如下： 對PAL-6而言，聚集的晶體解離，棒狀晶體縮短，進而導致晶體結(jié)構在很大程度上遭到破壞；對于PAL-8，由于對樣品施 加了更大的壓力，晶體結(jié)構受到了更大的影響。根據(jù)最低能量法則，晶體棒會重新排列，從而導致晶體結(jié)構在一定程度上 回復。然而對于PAL-10而言，由于對樣品施加了過多的壓力，嚴重影響了其晶體結(jié)構，這種影響很難回復。 3.4 研磨程度能影響樣品的比表面積，比表面積是吸附劑在吸附重金屬離子和燃料時的，一個很重要的物理化學性質(zhì)。 Liu等人發(fā)現(xiàn)吸附劑CTA+REC在除剛果紅時，其比表面積對吸附效果影響很大，Chen等人也報道過類似的結(jié)論。 因此，研磨次數(shù)對PAL比表面的的影響效果已測試，結(jié)果見表1.PAL-0的比表面積和Smicro分別為153,28平方米每克。研 磨后比表面積顯著增強，PAL-2的比表面積首先增加到229平方米每克，PAL-6的比表面積又降低到184平方米每克.研磨次 數(shù)增加到8，比表面積增加到213平方米每克并且保持不變。此外，Sext/比表面積的比例隨著研磨次數(shù)的增加反而降低， 而且Sext的含量很少改變。 研磨PAL樣品，直至PAL-6樣品Sext/比表面積的比例一直增加，然而由于比表面積的改變，隨著研磨次數(shù)的增加Sext/比 表面積的值反而降低，說明研磨次數(shù)對Sext有較大影響。 Smicro 和 Smicro/比表面積 的值與研磨次數(shù)的均符合所得到的比表面積。PAL-2之前Smicro隨著研磨次數(shù)增加而增加 ，到PAL-6會減少，最后又會增加。 PAL的Smicro隨研磨后均高于PAL-0，總之，由于Smicro的增加，研磨過的PAL的比較表面都明顯比PAL-0的比表面積高。 FESEM圖像證實，這是由于研磨后棒狀PAL晶體變短，導致微小粒子增多進而導致Smicro增加。 附注：3.5之前的均已翻譯過，部分專業(yè)詞匯可能翻譯不是很準確（例如Smicro; Sext ;），僅供參考 |
2樓2012-10-19 23:00:02
xiaoyingwv
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3樓2012-10-19 23:02:36
愛與雨下: 請勿點擊"確認回帖應助" 2012-10-20 07:11:39
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