CN114515563A - 一种新型可回收水硬性硅酸盐复合生物炭材料的制备方法 - Google Patents
一种新型可回收水硬性硅酸盐复合生物炭材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种新型可回收的水硬性硅酸盐复合生物炭材料的制备方法,涉及土壤重金属污染修复领域。本发明克服了现有生物炭施加到土壤后无法与土壤进行良好分离的不足,提供一种新方法对原始生物炭进行改进,使之可以从土壤中分离再回收利用。制备方法包括以下步骤:(1)将秸秆在含纳米Fe3O4微粒的溶液中浸渍24h,待混合溶液稳定后,过滤烘干。(2)将烘干后的混合有纳米Fe3O4微粒的水稻秸秆置于立式热解炉中无氧环境下热解,升温速率为20℃/min,热解温度分别是600 oC,热解时间为1h。(3)将含纳米Fe3O4微粒的磁性生物炭和硅酸盐按照质量比1:5的比例添加到圆盘造粒设备中。设置造粒机转速为20转/分钟,制备出具有一定粒径的水硬性硅酸盐复合生物炭颗粒。
Description
技术领域
本发明涉及土壤重金属污染修复领域,具体涉及一种可回收水硬性硅酸盐复合生物炭材料的组成成分及结合方式、制备流程。
背景技术
镉(Cd)是毒性最强的重金属污染物之一。当前中国土壤中有7%超过镉的污染标准限值0.3mg/kg。由于镉的不可生物降解性,很容易通过食物链在人体中富集。一些研究表明,摄入或积累过量的Cd(II)会引起全身疼痛,骨骼结节变形,并使骨骼严重软化。对于土壤和水体中镉污染物的去除,生物炭吸附法,由于其经济性和效率高,被认为是处理Cd污染的好方法。生物炭具有高度多孔的结构和各种官能团(包括羧基和羟基),因此对重金属具有很好的亲和力,可以通过吸附和原位钝化来降低有毒金属的生物利用性。土壤中原位钝化修复的缺点是虽然镉的生物有效性降低了,但是镉依然在土壤中无法去除,随着外界条件的改变,镉可能会重新从生物炭中释放,被植物吸收。为了促进生物炭的分离,一种方法是将过渡金属或它们的氧化物引入生物炭基质中以形成磁性生物炭,利用磁场力加以分离。但在土壤的修复过程中,磁性生物炭和土壤混合在一起,依然无法分离。为了解决生物炭回收难的问题,本发明制备一种新型生物炭材料,此种材料可以运用于镉污染水体的修复,更能应用于镉污染土壤的修复;这种新型生物炭材料能克服普通生物炭难以从土壤分离的应用缺陷,非常方便的从土壤中进行分离,从而达到从土壤中去除重金属的作用,而不仅仅是对土壤重金属的钝化作用。
发明内容
本发明的目的在于克服现有生物炭材料施加到土壤中,修复完土壤后,无法与土壤进行良好分离的不足,提供一种方法对原始生物炭进行改进,使之可以从土壤环境中顺利分离,再回收利用。
具体的技术方案为:
将收集收割后的小麦秸秆于自然条件下风干,将干燥的水稻秸秆用剪刀处理为长约1~2cm的尺寸。再将10 g FeSO4和Fe2(SO4)3-nH2O加入到200 mL去离子水中混合均匀,然后用5 mol/L的NaOH溶液将混合溶液的pH调至10-11。向混合溶液中分别加入10.00g处理好的秸秆,浸渍24h,待混合溶液稳定后,用抽滤机抽去多余的水分,烘干。将烘干后的混合有纳米Fe3O4微粒的水稻秸秆置于立式热解炉中无氧环境下热解,升温速率为20℃/min,热解温度分别是600 oC,热解时间为1h,制备含纳米Fe3O4微粒的磁性生物炭。将含纳米Fe3O4微粒的磁性生物炭粉碎,然后和粘结剂硅酸盐按照质量比1:5的比例添加到造粒设备中。圆盘造粒机分为成球区、加料区、喷淋区;将生物炭和硅酸盐添加到加料区,设置造粒机顺时针旋转的转速为20转/分钟。在造粒机成球盘中,生物炭和硅酸盐混合物在重力、离心力、盘面摩擦力以及盘面支持力的作用下不断滚动,按照一定的运动轨迹做圆周运动。同时,在喷淋区喷洒蒸馏水,微小蒸馏水液滴粘附生物炭和硅酸盐,形成初始硅酸盐复合生物炭球核。初始球核在成球区进一步粘附更多的生物炭和硅酸盐,硅酸盐复合生物炭继续成长形成具有一定粒径的球状颗粒。最后将具有一定粒径的球状颗粒磁性硅酸盐复合生物炭过筛分离,静置风干48 h,待硅酸盐复合生物炭颗粒彻底硬化。
本发明具有以下优势:
在不改变生物炭物理化学性质的条件下,引入粘结剂硅酸盐将生物炭颗粒粘连起来形成硅酸盐复合生物炭材料。此种硅酸盐复合生物炭为水硬性材料,具有良好的抗压强度,在水体和土壤中会保持完好的形态。在水体和土壤中留存一段时间后,还可以将硅酸盐复合生物炭材料完好的从水体和土壤中分离出来。生物炭材料为农业废弃物秸秆无氧条件下热解制备,生物炭热解原料秸秆来源广泛,对农业废弃物二次利用。粘结剂普通硅酸盐水泥价格便宜,来源广泛。硅酸盐复合生物炭制备过程简单,所需制备设备价格便宜,易操作,易生产。硅酸盐复合生物炭易从土壤中回收,对土壤中的硅酸盐复合生物炭进行磁分选和过筛分离,即可从土壤中分离出硅酸盐复合生物炭颗粒。
附图说明:
图1是重金属吸附量随吸附次数变化关系图。
图2是循环次数对生物炭回收率的影响图。
图3是新型水硬性生物炭制备流程图。
图4是新型颗粒生物炭磁铁吸附图。
图3中:1—惰性气体钢瓶,2—阀门,3—温控箱,4—气体流量计,5—热解炉,6—造粒机成球区,7—造粒机喷淋区,8—造粒机,9—造粒机加料区,10—造粒机电机,11—造粒机底座,12—出料口,13—筛分机,14—筛分电机,15—出料口,16—储料斗。
具体实施方式:
以下结合附图和具体实施例对本发明的技术方案做进一步描述。
如图1所示,将100g制备好的磁性硅酸盐复合生物炭颗粒(含纯生物20g)施加到重金属镉污染的土壤中(1000g)。污染土壤取自中国广西桂林市阳朔县铅锌矿矿区表层重金属污染土壤,土壤的镉含量为17.50mg/kg。土壤和生物炭颗粒混合均匀后,静置7天,期间根据土壤含水量变化,适当添加蒸馏水。7天后分离回收新型生物炭颗粒。对土壤中重金属镉吸附三次,图1中数据表示每一次的新型生物炭颗粒的吸附量及三次总吸附量。
如图2所示,将混有硅酸复合生物炭的土壤自然风干,风干后土壤和硅酸盐复合生物炭呈现离散状态时,磁性硅酸盐复合生物炭直接利用磁场分离,图2表示三次循环使用中新型生物炭颗粒每次回收量(单位:克g)和三次循环使用后新型生物炭颗粒总回收率。
如图4所示, a为生物炭材料浸水前状态,b为浸水后状态;c表示颗粒粒径大小均一,在4-6mm之间。图(d, e)表示浸水前和浸水后新型生物炭材料均可有效被磁铁吸附。
实例1:将收集收割后的小麦秸秆于自然条件下风干,将干燥的水稻秸秆用剪刀处理为长约1~2cm的尺寸。再将10 g FeSO4和Fe2(SO4)3-nH2O加入到200 mL去离子水中混合均匀,然后用5 mol/L的NaOH溶液将混合溶液的pH调至10-11。向混合溶液中分别加入10.00g处理好的秸秆,浸渍24h,待混合溶液稳定后,用抽滤机抽去多余的水分,烘干。
实例2:将实例1中烘干后的混合有纳米Fe3O4微粒的水稻秸秆置于立式热解炉5中无氧环境下热解,升温速率为20℃/min,热解温度分别是600 oC,热解时间为1h,制备含纳米Fe3O4微粒的磁性生物炭。
实例3:将实例2制备的含纳米Fe3O4微粒的磁性生物炭粉碎,然后和粘结剂硅酸盐按照质量比1:5的比例添加到造粒机8中。将生物炭和硅酸盐添加到加料区9中,设置造粒机顺时针旋转的转速为20转/分钟。同时,在喷淋区9喷洒蒸馏水,微小蒸馏水液滴粘附生物炭和硅酸盐,形成初始硅酸盐复合生物炭球核。初始球核在成球区6进一步粘附更多的生物炭和硅酸盐,硅酸盐复合生物炭继续成长形成具有一定粒径的球状颗粒。
实例4:将实例3中的具有一定粒径的球状颗粒磁性硅酸盐复合生物炭添加到筛分机13中,符合粒径的硅酸盐复合生物炭颗粒从出料口15分离,静置风干48 h,待硅酸盐复合生物炭颗粒彻底硬化。粒径达不到要求的硅酸盐复合生物炭颗粒从出料口12分离,继续加到造粒机8中。
Claims (9)
1.一种新型可回收的水硬性硅酸盐复合生物炭材料制备方法,其特征在于以下步骤:
收集收割后的小麦秸秆于自然条件下风干,将干燥的水稻秸秆用剪刀处理为长约1~2cm的尺寸;将10 g FeSO4和Fe2(SO4)3-nH2O加入到200 mL去离子水中混合均匀,然后用5mol/L的NaOH溶液将混合溶液的pH调至10-11;向混合溶液中分别加入10.00g处理好的秸秆,浸渍24h,待混合溶液稳定后,用抽滤机抽去多余的水分,烘干;将烘干后的混合有纳米Fe3O4微粒的水稻秸秆置于立式热解炉中无氧环境下热解,升温速率为20℃/min,热解温度分别是600 oC,热解时间为1h,制备含纳米Fe3O4微粒的磁性生物炭;将含纳米Fe3O4微粒的磁性生物炭粉碎,然后和粘结剂硅酸盐按照质量比1:5的比例添加到造粒设备中;圆盘造粒机分为成球区、加料区、喷淋区;将生物炭和硅酸盐添加到加料区,设置造粒机顺时针旋转的转速为20转/分钟;在造粒机成球盘中,生物炭和硅酸盐混合物在重力、离心力、盘面摩擦力以及盘面支持力的作用下不断滚动,按照一定的运动轨迹做圆周运动;同时,在喷淋区喷洒蒸馏水,微小蒸馏水液滴粘附生物炭和硅酸盐,形成初始硅酸盐复合生物炭球核。
2.初始球核在成球区进一步粘附更多的生物炭和硅酸盐,硅酸盐复合生物炭继续成长形成具有一定粒径的球状颗粒。
3.将具有一定粒径的球状颗粒磁性硅酸盐复合生物炭过筛分离,静置风干48 h,待硅酸盐复合生物炭颗粒彻底硬化。
4.根据权利要求1所述的新型可回收的水硬性硅酸盐复合生物炭材料的制备方法,其特征在于:含纳米Fe3O4微粒的磁性生物炭的热解条件为:无氧环境,升温速率为20℃/min,热解温度分别是600 oC,热解时间为1h。
5.根据权利要求1所述的新型可回收的水硬性硅酸盐复合生物炭材料的制备方法,其特征在于:粘结剂为水硬性凝胶材料硅酸盐水泥,基本参数:初凝时间≥45min;终凝时间≤390min;3天抗压强度≥27.0MPa,28天抗压强度≥52.5MPa。
6.根据权利要求1所述的新型可回收的水硬性硅酸盐复合生物炭材料的制备方法,其特征在于:粘结剂水硬性材料硅酸盐水泥和生物炭的质量比为5:1。
7.根据权利要求1所述的新型可回收的水硬性硅酸盐复合生物炭材料的制备方法,其特征在于:造粒机为圆盘造粒机,造粒机顺时针旋转的转速为20转/分钟,并在造粒机旋转的过程中向硅酸盐和生物炭的混合物喷洒蒸馏水。
8.根据权利要求4所述的新型可回收的水硬性硅酸盐复合生物炭材料的结合方式,其特征在于:粘结剂硅酸盐的主要成分硅酸三钙(3CaO·SiO2,)和硅酸二钙(β-2CaO·SiO2)与水发生水化反应产生具有粘结力的胶态水化产物(CaO)x–SiO2–(H2O)y (简称C-S-H gel) ,这种纤维状C-S-H凝胶能够嵌入到生物炭的孔隙中将生物炭牢牢地胶连起来。
9.根据权利要求1所述新型可回收的水硬性硅酸盐复合生物炭材料的用途,其特征在于:新型可回收的水硬性硅酸盐复合生物炭材料用于土壤中重金属的吸附。
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