CN111848166B - 一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒及其制备方法 - Google Patents

一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒及其制备方法 Download PDF

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CN111848166B
CN111848166B CN202010798524.5A CN202010798524A CN111848166B CN 111848166 B CN111848166 B CN 111848166B CN 202010798524 A CN202010798524 A CN 202010798524A CN 111848166 B CN111848166 B CN 111848166B
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李家科
刘欣
王艳香
郭平春
胡旭美
范学运
赵学国
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Jingdezhen Ceramic Institute
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Abstract

本发明公开了一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒，由基础原料和辅助原料组成；所述基础原料为伊利石粉料20～60wt％、低温熔剂粉料10～40wt％、核桃壳粉20～70wt％；相对于基础原料，所述辅助原料及其用量为TiO2粉体0～10wt％、羟丙基甲基纤维素4～6wt％、油酸0.5～1.5wt％、甘油3～6wt％、水40～50wt％；所述低温熔剂粉体的熔融温度为600～900℃。此外，还公开了上述柱状炭粒的制备方法。本发明以核桃壳粉为碳源，以伊利石为基料、结合低温熔剂作为结合剂而形成配方体系，能够在较低温度下制备出高强度高孔隙率的炭粒材料，制备方法工艺流程简单，易于产业化生产。

Description

一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒 及其制备方法
技术领域
本发明涉及炭材料技术领域，尤其涉及一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒及其制备方法。
背景技术
活性炭(AC)是一种性能优异的多孔材料，通常采用富碳物质(木质材料、竹质材料、果壳材料和高分子材料等)作为原料，经过热解(炭化)而得到的一类无定型物质。由于具有高度发达的多孔性能、高比表面积和催化性能，而被广泛应用于环保行业、医疗、化工、食品等相关领域。
然而，富碳材料热解得到的活性炭，由于颗粒强度较低，因而不能满足使用要求，或得到的活性炭呈粉末状，在使用过程会引起粉尘，同时也不便于回收，从而导致二次污染。为了克服以上不足，通常是采用碳源材料和辅助材料进行成形，通过烧结或热处理，从而获得具有一定强度和颗粒形状的炭粒，以满足使用性能和便于回收的要求。
目前制备炭粒的工艺流程为，将含炭材料(如煤泥、沥青、富含木质素、纤维素的木质、竹质、植物秸秆材料等)、结合剂(如粘土、长石等)和溶剂(如水、甘油等)按一定比例混合，然后经过成形、干燥、热解(炭化)，从而得到炭粒。由于坯料中以粘土、长石等作为成形和结合剂，为了使制备炭粒具有一定机械强度，一般热解(炭化)温度需要在1000℃以上。这样便存在着以下技术问题：第一，由于富碳材料(木质材料、竹质材料、果壳材料和高分子材料)一般在800℃就可以完全碳化而得到高孔隙率的炭材料，如果热解温度过高，会使碳材料过度热解而导致炭产率降低；第二，由于较高的热解温度，同样使得炭颗粒中的孔隙率(比表面积)减小，使炭粒的吸附性能降低；第三，较高的热解温度，也会增加能源消耗，增加生产成本。因此，如何在较低温度下(1000℃以内)制备出能够满足使用强度要求、高孔隙率的炭粒材料，是炭粒材料研究的重点。
发明内容
本发明的目的在于克服现有技术的不足，提供一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒，通过配方设计，以提高炭粒的机械强度、气孔率、含炭量和吸附性能。本发明的另一目的在于提供上述以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒的制备方法。
本发明的目的通过以下技术方案予以实现：
本发明提供的一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒，由基础原料和辅助原料组成；所述基础原料为伊利石粉料20～60wt％、低温熔剂粉料10～40wt％、核桃壳粉20～70wt％；相对于基础原料，所述辅助原料及其用量为TiO2粉体0～10wt％、羟丙基甲基纤维素4～6wt％、油酸0.5～1.5wt％、甘油3～6wt％、水40～50wt％；所述低温熔剂粉体的熔融温度为600～900℃。
进一步地，本发明所述低温熔剂粉料的配料组成为锂长石23～35wt％、碳酸锂5～15wt％、石英10～15wt％、ZnO 4～6wt％、碳酸钠9～12wt％、硼酸20～30wt％、磷酸钠6～12wt％。所述TiO2粉体的粒径为3～5μm。
进一步地，本发明所述柱状炭粒其抗折强度为10～26MPa、气孔率为35～63％、孔径分布为1.0～75μm、含碳量为15～45％、吸附性能≥90％。
本发明的另一目的通过以下技术方案予以实现：
本发明提供的上述以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒的制备方法；包括以下步骤：
(1)低温熔剂粉料的制备
按照所述低温熔剂粉料的配料组成进行球磨混料，经过熔制处理后的熔体用水淬冷，经球磨粉碎、干燥、过筛后，即得到低温熔剂粉体；
(2)炭粒的制备
首先将伊利石粉料、低温熔剂粉料、核桃壳粉、TiO2粉体和羟丙基甲基纤维素混合均匀，然后加入油酸、甘油和水，经过搅拌、练泥、陈腐后进行挤出成形为柱状坯体，经干燥后，在氮气气氛中进行以下热解处理：以3℃/min升温到热解温度700～900℃，保温时间为60～90min，保温结束以2℃/min降到室温，即得到柱状炭粒。
进一步地，本发明制备方法所述步骤(1)中熔制温度为1250～1300℃，保温时间为30～60min。所述步骤(2)中柱状坯体的尺寸为Φ6mm×(10～12)mm。
本发明具有以下有益效果：
(1)本发明以核桃壳粉为碳源，以伊利石为基料、结合低温熔剂(熔融温度600～900℃)作为结合剂，并辅以TiO2(光催化剂、提高吸附性能)、羟丙基甲基纤维素(成形助剂)、油酸(分散剂)、甘油(成形助剂)、水而形成配方体系，从而在较低温度下(700～900℃)制备出能够满足使用强度要求、高孔隙率的炭粒材料。
(2)伊利石作为一种常见的粘土矿物﹐由白云母﹑钾长石风化而成﹐并产于泥质岩中﹐或由其它矿物蚀变形成，属于粘土类矿物，具有较好的可塑性。本发明利用伊利石在炭粒坯体成形过程中起到结合剂作用，在热解阶段起到骨架作用。
(3)TiO2是一种半导体材料，具有光催化性能。本发明在配方体系中TiO2作为辅助原料引入，利用其具有光催化性能可有效降解污染物，从而进一步提高炭粒的吸附性能。
(4)本发明制备方法具有热解温度低、工艺流程简单、易操作，低成本低和高性能等特点，易于产业化生产。
下面将结合实施例对本发明作进一步的详细描述。
具体实施方式
本发明实施例一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒，由基料原料和辅助原料组成；其中，基料原料为伊利石粉料20～60wt％、低温熔剂粉料10～40wt％、核桃壳粉20～70wt％；相对于基料原料，辅助原料及其用量为TiO2粉体0～10wt％、羟丙基甲基纤维素(HPMC)4～6wt％、油酸0.5～1.5wt％、甘油3～6wt％、水40～50wt％；低温熔剂粉料的配料组成为锂长石23～35wt％、碳酸锂5～15wt％、石英10～15wt％、ZnO 4～6wt％、碳酸钠9～12wt％、硼酸20～30wt％、磷酸钠6～12wt％。
本发明实施例伊利石来自于河北承德人和矿业有限公司，矿区位于承德市围场满族蒙古族自治县境内，其化学组成为：Al2O315.11％、SiO272.55％、K2O+Na2O6.85％、Fe2O31.22％、CaO 0.11％、TiO20.27％、IL3.89％，经过球磨粉碎、干燥、过250目筛得到伊利石粉料。
核桃壳是核桃加工过程中产生的附属料，是一类硬质果壳原料，经过球磨破碎、过250目筛得到核桃壳粉。
本发明实施例一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒的制备方法，其步骤如下：
(1)低温熔剂粉料的制备
按照上述低温熔剂粉料的配料组成进行球磨混料30min，然后将混合料装入到立式窑中进行熔制而得到熔体，熔制温度为1250～1300℃、保温时间为30～60min，保温结束后将熔体倒入到水中进行淬冷，经球磨粉碎30min、干燥、过250目筛后，即得到低温熔剂粉体；
本发明实施例所用低温熔剂粉体的配料组成、熔制参数及所制备熔剂的熔融温度如表1所示；
(2)炭粒的制备
首先将伊利石粉料、低温熔剂粉料、核桃壳粉、粒径为3～5μm的TiO2粉体和羟丙基甲基纤维素(HPMC)放入到捏合机中进行混料，混料时间为30min，然后加入油酸、甘油和水继续混料30min得到泥料，经练泥得到的泥段放置在阴暗处陈腐12h后，放入成形机中挤出成形为柱状坯体(尺寸规格为Φ6mm×(10～12)mm)；将柱状坯体首先自然干燥8h，然后放置在80℃烘箱中干燥12h后，在氮气气氛中进行以下热解处理：以3℃/min升温到热解温度700～900℃，保温时间为60～90min，保温结束以2℃/min降到室温，即得到柱状炭粒(尺寸规格为Φ(5～5.5)mm×(9～11)mm)。
各实施例柱状炭粒的原料组成、热解工艺参数如表2所示。
表1本发明实施例所用低温熔剂粉体的配料组成、熔制参数及所制备熔剂的熔融温度
Figure BDA0002626502100000041
*低温熔剂熔融温度的测定：将低温熔剂粉体压制成规格Φ2×3mm的小圆柱，采用高温显微镜检测熔融温度范围。
表2本发明各实施例柱状炭粒的原料组成、热解工艺参数
Figure BDA0002626502100000042
Figure BDA0002626502100000051
*辅助原料的用量为相对于基料原料
对本发明各实施例制得的柱状炭粒进行以下性能测试：
1、抗折强度：采用材料试验机检测炭粒试样的抗折强度(MPa)。
2、气孔率：采用阿基米德排水法检测炭粒试样的气孔率(％)。将干燥试样放入有适量水的烧杯中，然后进行抽真空30min，以便排出试样中气体，抽真空结束，取出试样测量相应质量，计算试样的气孔率。
气孔率(％)＝(m1-m2)/m3×100％，
m1干燥试样的质量(g)，m2饱和试样在空气中的质量(g)，m3饱和试样在水中的质量(g)。
3、孔径：采用压汞法检测炭粒材料的孔径分布。
4、含碳量：采用质量差值法检测炭粒中的中的碳含量。将炭粒试样在马弗炉中煅烧，煅烧温度为900℃，保温时间为2h，使试样中的炭全部氧化。
含碳量(％)＝(m1-m2)/m1×100％，
m1煅烧前试样质量(g)，m2煅烧后试样质量(g)。
5、吸附性能：采用亚甲蓝为模拟物，检测炭粒试样的吸附能力。将100ml亚甲蓝水溶液(浓度10mg/L)放置于烧杯中，然后把质量为0.5g炭粒放置上述溶液中，并进行搅拌，经过30min吸附后，检测亚甲蓝溶液浓度变化。
吸附性能(％)＝(M1-M2)/M1×100％，
M1吸附前亚甲蓝溶液浓度(mg/L)，M2吸附后亚甲蓝溶液浓度(mg/L)。
本发明各实施例制得的柱状炭粒的性能测试结果如表3所示。
表3本发明各实施例制得的柱状炭粒的性能指标
Figure BDA0002626502100000052
Figure BDA0002626502100000061

Claims (2)

1.一种以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒的制备方法，其特征在于：所述柱状炭粒由基础原料和辅助原料组成；所述基础原料为伊利石粉料20～60wt%、低温熔剂粉料10～40wt%、核桃壳粉20～70wt%；相对于基础原料，所述辅助原料及其用量为粒径3～5μm的TiO2粉体0～10wt%、羟丙基甲基纤维素4～6wt%、油酸0.5～1.5wt%、甘油3～6wt%、水40～50wt%；所述低温熔剂粉体的熔融温度为600～900℃，其配料组成为锂长石23～35wt%、碳酸锂5～15wt%、石英10～15wt%、ZnO 4～6wt%、碳酸钠9～12wt%、硼酸20～30wt%、磷酸钠6～12wt%；制备方法包括以下步骤：
(1) 低温熔剂粉料的制备
按照所述低温熔剂粉料的配料组成进行球磨混料，经过1250～1300℃熔制处理30～60min后的熔体用水淬冷，经球磨粉碎、干燥、过筛后，即得到低温熔剂粉体；
(2) 炭粒的制备
首先将伊利石粉料、低温熔剂粉料、核桃壳粉、TiO2粉体和羟丙基甲基纤维素混合均匀，然后加入油酸、甘油和水，经过搅拌、练泥、陈腐后进行挤出成形为柱状坯体，经干燥后，在氮气气氛中进行以下热解处理：以3℃/min升温到热解温度700～900℃，保温时间为60～90min，保温结束以2℃/min降到室温，即得到柱状炭粒；所述柱状炭粒其抗折强度为10～26MPa、气孔率为35～63%、孔径分布为1.0～75μm、含碳量为15～45%、吸附性能≥90%。
2.根据权利要求1所述的以伊利石、低温熔剂和核桃壳粉为主要原料的柱状炭粒的制备方法，其特征在于：所述步骤(2)中柱状坯体的尺寸为Φ6mm×(10～12)mm。
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