铝交联累托石的制备与应用研究
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摘要
累托石是一种具有独特结构的矿物。本文以开发利用累托石矿为背景,系统地研究了累托石的成型、交联、表征与吸附性能。对累托石矿进行了成型及交联改性,给出了最优的成型与交联条件。研究了改性累托石作为吸附剂处理氨氮、氟、磷和染料废水的可行性,探索了累托石负载硅钨酸催化剂的制备和对乙酸丁酯反应的催化性能,主要的研究成果如下:
⑴ 天然累托石(不论是钙基还是钠基)在水中易于崩解、扩散、形成胶体溶液,不易与溶液分离;采用高温煅烧和交联的方法对累托石进行处理,能够明显地改善累托石在水溶液中的沉降性,使之容易与溶液分离,从而为累托石在废水处理中的应用创造了条件。
⑵ 提出了一种新的制备交联累托石的方法-微波强化交联法。实验结果表明微波强化交联的方法可以缩短反应时间,提高交联产品的底面间距和热稳定性,增加可反应的累托石泥浆和铝溶胶浓度,从而为实现工业化生产提供了新工艺。微波强化交联反应的优化条件是累托石泥浆浓度为4%、铝溶胶浓度为2.5 mol/L(Al)、每克累托石用4 mmol的Al 溶胶柱撑、微波反应时间7min。确定了采用常规加热方法对累托石进行铝交联时,影响产品底面间距的主要因素为累托石泥浆浓度和铝溶胶浓度。
⑶ 研究了煅烧、成型、交联改性等方法处理后的累托石对NH4+、Cd2+等阳离子的吸附性能,讨论了它们的吸附机理。累托石吸附阳离子的作用机理主要是基于累托石层间阳离子的交换作用,采用碱液洗涤法可以使用过的累托石再生。300(C煅烧后的钙基累托石对Cd2+具有较强的吸附作用,其吸附等温线符合Freundlich方程。
⑷ 研究了不同形态的原矿、煅烧及交联后的累托石对氟离子的吸附作用。结果表明煅烧和交联都能够明显提高钠基累托石对氟离子的吸附能力。改性后的钠基累托石对氟离子的吸附性能优于钙基累托石。用交联累托石制备的直径为1mm的球型颗粒,600(C煅烧3小时后具有较大的吸附氟离子的能力,同时具有在水中不崩解、易于分离和再生的优点,因而可用于实际的含氟废水的处理。
[5] 以除去水体中的痕量磷为目的,研究了改性累托石的除磷性能。试验表明煅烧和交联的方法均能提高累托石对磷的吸附能力,在200-800(C 的范围内,500(C煅烧后所制得的累托石的除磷性能最好。羟基、氟离子等阴离子对磷的吸附有竞争作用,而COD和氨氮则有协同作用。
[6] 研究了CTMAB改性累托石和铝交联累托石对酸性蓝GL废水的脱色作用。结果表明这两种改性方法都能够明显提高累托石对酸性蓝GL废水的脱色效率。对于初始浓度为50mg/L的废水,铝交联累托石对酸性蓝GL的吸附量可达21mgg-1,CTMAB改性的交联累托石的最大吸附量可达18mgg-1。其吸附规律可较好的符合Freundlich 吸附等温式。与CTMAB改性累托石相比,铝交联累托石具有吸附速度快、容量大、可以再生的优点。
[7]研究了交联累托石负载硅钨酸催化剂—SiW12/P-Rec的制备和催化性能。用XRD及IR对SiW12/P-Rec 及不同负载量和焙烧温度的负载催化剂进行了表征,发现通过浸渍的方法能将硅钨酸固载在交联累托石上,从而提高交联累托石的酸性。负载了硅钨酸的交联累托石对乙酸丁酯的合成反应具有良好的催化性能。
以上研究结果说明交联能够提高累托石的比表面积和底面间距、改变层间域的性质,提高累托石对废水中的阴、阳离子和有机分子的吸附能力。所以,交联累托石能够作为废水深度处理时的吸附剂;同时,由于交联累托石在800(C煅烧后仍然具有在水中不崩解、比表面积大、层间距大的优点,具备了作为催化剂载体的必要条件,有望在精细化工和石油化工中获得应用。
Rectorite is a mineral with specific texture. In order to find ways to use the rectorite friendly environment, we present a method formation of rectorite, synthesis and characterizations of aluminum-pillared rectorite, and adsorption capacity of pillared rectorite to ammonia, phosphate, COD, acid blue, in this paper. We also present the catalytic characteristics of pillared rectorite immobilized with SiW12-Heteropolyacid. The main conclusions are as follows:
⑴ Natural rectorite, whether Na-rectorite or Ca-rectorite, is easy to scatter and form gel solution with water. We found that rectorite became easy to separate with water after calcination and pillaring. It means that calcined and pillared rectorite could be better than natural rectorite used to treat wastewater.
⑵ We present the synthesis and characterization of aluminum-pillared rectorite. The synthesis was conducted with both conventional heating and microwave irradiation. Microwave irradiation was found to enhance the intercalation and ion-exchange during synthesis, and produced rectorite with larger d001 and better uniformity. The specific surface area is 180m2/g and basal spacing is 3.2 nm. The optimized synthesis conditions with microwave irradiation are:
Rectorite slurry was 4%(wt), concentration of aluminum was 2.5 mol/l, ratio of rectorite with aluminum was 4mmol/g(dry base), microwave reaction time was 7 min.
We found main factors that affect synthesis with conventional heating are concentrations of rectorite slurry and aluminum gel.
⑶ The adsorption capacity of modified rectorite with calcinations, pillaring and formation to NH4+、Cd2+ were studied. The results show that mechanism of removal ion like NH4+ and Cd2+ is ion-exchange with modified-rectorite. Saturated rectorite can be reprocessed with hydroxy. Rectorite calcined at 300℃ for 3h has stronger adsorption to Cd2+, and its isotherm fit Freundlich equation.
⑷ The adsorption capacity of Ca-rectorite , Na-rectorite and modified rectorite with calcination and pillaring towere tested. The results show that both calcinations and
pillaring can improve capability of modified rectorite to adsorb F-. After calcinations, Na-rectorite has larger capability to adsorb F- than Ca-rectorite.
⑸ For the purpose of removal trace phosphates from water body, we test the capability of modified rectorite. The results show that both calcinations and pillaring can improve capability of rectorite to adsorb phosphates. Calcined rectorite at 500℃ for 3h has largest adsorption to phosphates from 200℃ to 800℃. We found that hydroxy and F- reduce the adsorption capability of modified rectorite, and that both ammonia and COD increase it under the same conditions.
[6] Removal of acid blue GL from water by using modified rectorite was investigated. The results show that modified rectorite both organorectorite and pillared rectorite have strong adsorbed capacity to adsorb acid blue GL. The adsorbed capacity of organorectorite and pillared rectorite reached 18mgg-1 and 21mgg-1 for acid blue GL, respectively. Adsorption isotherms both of them fit Freundlich equation. Al-pillared rectorite has characteristics of larger adsorbed capacity, low cost, high speed adsorbing rate, capable of regeneration compared with CTMAB-rectorite.
[7] A new type solid acid of SiW12/P-Rec was prepared through impregnation method and used to catalyze the esterification of acetic acid and butanol. XRD, IR are used to characterize supported catalysts with different loadings and calcined at different SiW12 immobilized on P-Rec. And in the esterification of n-butanol by acetic acid, it can be found that the loaded amount of SiW12 and calcination temperature have a significant effect on catalytic property.
As above all, cross-linking can increase specific surface area, basal space, change the interlayer properties; improve adsorption capacity to ion and organic materials of rectorite. Hence, it can be used as adsorbents to treat wastewater that contains ion and organic materials. Meanwhile, owing to its high thermal stability, pi
⑴ 天然累托石(不论是钙基还是钠基)在水中易于崩解、扩散、形成胶体溶液,不易与溶液分离;采用高温煅烧和交联的方法对累托石进行处理,能够明显地改善累托石在水溶液中的沉降性,使之容易与溶液分离,从而为累托石在废水处理中的应用创造了条件。
⑵ 提出了一种新的制备交联累托石的方法-微波强化交联法。实验结果表明微波强化交联的方法可以缩短反应时间,提高交联产品的底面间距和热稳定性,增加可反应的累托石泥浆和铝溶胶浓度,从而为实现工业化生产提供了新工艺。微波强化交联反应的优化条件是累托石泥浆浓度为4%、铝溶胶浓度为2.5 mol/L(Al)、每克累托石用4 mmol的Al 溶胶柱撑、微波反应时间7min。确定了采用常规加热方法对累托石进行铝交联时,影响产品底面间距的主要因素为累托石泥浆浓度和铝溶胶浓度。
⑶ 研究了煅烧、成型、交联改性等方法处理后的累托石对NH4+、Cd2+等阳离子的吸附性能,讨论了它们的吸附机理。累托石吸附阳离子的作用机理主要是基于累托石层间阳离子的交换作用,采用碱液洗涤法可以使用过的累托石再生。300(C煅烧后的钙基累托石对Cd2+具有较强的吸附作用,其吸附等温线符合Freundlich方程。
⑷ 研究了不同形态的原矿、煅烧及交联后的累托石对氟离子的吸附作用。结果表明煅烧和交联都能够明显提高钠基累托石对氟离子的吸附能力。改性后的钠基累托石对氟离子的吸附性能优于钙基累托石。用交联累托石制备的直径为1mm的球型颗粒,600(C煅烧3小时后具有较大的吸附氟离子的能力,同时具有在水中不崩解、易于分离和再生的优点,因而可用于实际的含氟废水的处理。
[5] 以除去水体中的痕量磷为目的,研究了改性累托石的除磷性能。试验表明煅烧和交联的方法均能提高累托石对磷的吸附能力,在200-800(C 的范围内,500(C煅烧后所制得的累托石的除磷性能最好。羟基、氟离子等阴离子对磷的吸附有竞争作用,而COD和氨氮则有协同作用。
[6] 研究了CTMAB改性累托石和铝交联累托石对酸性蓝GL废水的脱色作用。结果表明这两种改性方法都能够明显提高累托石对酸性蓝GL废水的脱色效率。对于初始浓度为50mg/L的废水,铝交联累托石对酸性蓝GL的吸附量可达21mgg-1,CTMAB改性的交联累托石的最大吸附量可达18mgg-1。其吸附规律可较好的符合Freundlich 吸附等温式。与CTMAB改性累托石相比,铝交联累托石具有吸附速度快、容量大、可以再生的优点。
[7]研究了交联累托石负载硅钨酸催化剂—SiW12/P-Rec的制备和催化性能。用XRD及IR对SiW12/P-Rec 及不同负载量和焙烧温度的负载催化剂进行了表征,发现通过浸渍的方法能将硅钨酸固载在交联累托石上,从而提高交联累托石的酸性。负载了硅钨酸的交联累托石对乙酸丁酯的合成反应具有良好的催化性能。
以上研究结果说明交联能够提高累托石的比表面积和底面间距、改变层间域的性质,提高累托石对废水中的阴、阳离子和有机分子的吸附能力。所以,交联累托石能够作为废水深度处理时的吸附剂;同时,由于交联累托石在800(C煅烧后仍然具有在水中不崩解、比表面积大、层间距大的优点,具备了作为催化剂载体的必要条件,有望在精细化工和石油化工中获得应用。
Rectorite is a mineral with specific texture. In order to find ways to use the rectorite friendly environment, we present a method formation of rectorite, synthesis and characterizations of aluminum-pillared rectorite, and adsorption capacity of pillared rectorite to ammonia, phosphate, COD, acid blue, in this paper. We also present the catalytic characteristics of pillared rectorite immobilized with SiW12-Heteropolyacid. The main conclusions are as follows:
⑴ Natural rectorite, whether Na-rectorite or Ca-rectorite, is easy to scatter and form gel solution with water. We found that rectorite became easy to separate with water after calcination and pillaring. It means that calcined and pillared rectorite could be better than natural rectorite used to treat wastewater.
⑵ We present the synthesis and characterization of aluminum-pillared rectorite. The synthesis was conducted with both conventional heating and microwave irradiation. Microwave irradiation was found to enhance the intercalation and ion-exchange during synthesis, and produced rectorite with larger d001 and better uniformity. The specific surface area is 180m2/g and basal spacing is 3.2 nm. The optimized synthesis conditions with microwave irradiation are:
Rectorite slurry was 4%(wt), concentration of aluminum was 2.5 mol/l, ratio of rectorite with aluminum was 4mmol/g(dry base), microwave reaction time was 7 min.
We found main factors that affect synthesis with conventional heating are concentrations of rectorite slurry and aluminum gel.
⑶ The adsorption capacity of modified rectorite with calcinations, pillaring and formation to NH4+、Cd2+ were studied. The results show that mechanism of removal ion like NH4+ and Cd2+ is ion-exchange with modified-rectorite. Saturated rectorite can be reprocessed with hydroxy. Rectorite calcined at 300℃ for 3h has stronger adsorption to Cd2+, and its isotherm fit Freundlich equation.
⑷ The adsorption capacity of Ca-rectorite , Na-rectorite and modified rectorite with calcination and pillaring towere tested. The results show that both calcinations and
pillaring can improve capability of modified rectorite to adsorb F-. After calcinations, Na-rectorite has larger capability to adsorb F- than Ca-rectorite.
⑸ For the purpose of removal trace phosphates from water body, we test the capability of modified rectorite. The results show that both calcinations and pillaring can improve capability of rectorite to adsorb phosphates. Calcined rectorite at 500℃ for 3h has largest adsorption to phosphates from 200℃ to 800℃. We found that hydroxy and F- reduce the adsorption capability of modified rectorite, and that both ammonia and COD increase it under the same conditions.
[6] Removal of acid blue GL from water by using modified rectorite was investigated. The results show that modified rectorite both organorectorite and pillared rectorite have strong adsorbed capacity to adsorb acid blue GL. The adsorbed capacity of organorectorite and pillared rectorite reached 18mgg-1 and 21mgg-1 for acid blue GL, respectively. Adsorption isotherms both of them fit Freundlich equation. Al-pillared rectorite has characteristics of larger adsorbed capacity, low cost, high speed adsorbing rate, capable of regeneration compared with CTMAB-rectorite.
[7] A new type solid acid of SiW12/P-Rec was prepared through impregnation method and used to catalyze the esterification of acetic acid and butanol. XRD, IR are used to characterize supported catalysts with different loadings and calcined at different SiW12 immobilized on P-Rec. And in the esterification of n-butanol by acetic acid, it can be found that the loaded amount of SiW12 and calcination temperature have a significant effect on catalytic property.
As above all, cross-linking can increase specific surface area, basal space, change the interlayer properties; improve adsorption capacity to ion and organic materials of rectorite. Hence, it can be used as adsorbents to treat wastewater that contains ion and organic materials. Meanwhile, owing to its high thermal stability, pi
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