CN101516497A - 酸浸渍的活性炭及其形成与使用方法 - Google Patents
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Abstract
通过添加无机酸,由含碳材料形成的酸浸渍的活性炭基体,它可用于从气流中化学吸附氨气。氨气与酸反应,形成肥料盐。废的基体可用作肥料,或者可从基体中淘洗肥料盐。
Description
发明领域
本发明涉及含用无机酸浸渍的活性炭基体的组合物及其生产与使用方法。
发明背景
氨水是工业和农业上重要的化学品。它用于制备许多聚合物和纺织品,且是氮肥的重要的基本成分。
在空气或水中发现的氨水可来自于尿素、蛋白质和其他含氮有机物的分解,或者来自于在工业或农业中使用氨水的过程中其偶然逃逸。空气中的氨水在百万分之25-500份的浓度下对人类和动物有毒,这取决于可接受的暴露时间。在任何浓度下,空气中的氨水结合酸性组分,例如二氧化硫,形成直径小于2.5微米(PM2.5)的粒状物质,这种粒状物质是尤其有毒的污染物,它可深深地渗透到人类呼吸道内。另外,气载氨水会引起金属结构腐蚀且被视为气味问题的主要贡献因子。
氨水在水中高度可溶,其中在高浓度下,它可引起鱼死亡且通过刺激藻类种群的生长造成富营养化和氧气的消耗。
可通过数种方法从空气中除去氨水。首先且最便宜的是,用低浓度氨水稀释负载氨水的空气,以便实现可接受的水平。然而,这一“稀释”方法在较宽的区域内分配氨水,因此造成形成PM2.5。在其中因动物尿液沉积导致累积有毒程度的氨水的封闭(confined)的牲畜作业中,排出内部空气和外部空气作为“补充空气”进入。然而,在寒冷的气候条件下,除去负载氨水的空气要求加热置换空气以保持畜栏内均匀的温度。
另一选择是通过在水中鼓泡,从空气中除去氨气,从而以氨水和铵离子(NH4 +)形式捕获氨气。然而,当氨含量增加时,水的pH增加且氨气再次释放到空气内。而且,稀释的氨化水没有价值,且也必须弃置。第三个选择,和可能最常见的是使负载氨气的空气鼓泡通过无机酸,例如硫酸或盐酸或硝酸。氨气转化成相当的盐(硫酸铵、氯化铵或硝酸铵)。第三个选择的缺点是:(a)空气鼓泡通过液体的结果是形成显著大的反压,和(b)所形成的盐与液体酸混合且难以分离,从而限制了副产物的用途。
另一选择是通过电化学处理,还原氨气成氮气(N2)。然而,这一方法的缺点是,操作成本高且要求复杂的加工设备。
若必须从水,例如从将再引入到天然水体内的废水中除去氨气,则将氨气从水中汽提到空气内,其中再次出现除去空气问题。因此,以上讨论的从空气中除去氨气的所有技术同样可应用到在水中处理氨气。
因此,本领域需要从空气中除去氨气的活性炭基体,它可减少现有技术中出现的一些或所有难题。
发明概述
本发明涉及一种新型组合物,它包括酸浸渍的活性炭,所述活性炭可通过将含碳材料转化成活性炭基体同时在活性炭基体内灌入酸而生产。另外,本发明可包括使用酸浸渍的活性炭,从气流中除去氨气的方法,和由废介质生产肥料物质的方法。此外,本发明可包括将酸浸渍的活性炭基体和肥料盐浸渍的副产物转化成活性炭的方法。
因此,在一个方面中,本发明可包括固体组合物,所述组合物包括用无机酸浸渍的活性炭基体,它可用于化学吸附氨气。在一个实施方案中,无机酸包括硫酸、盐酸、磷酸或硝酸之一。该固体组合物优选表面积为至少约10m2/g,更优选至少约30m2/g,和最优选至少约500m2/g。
在一个实施方案中,通过添加无机酸到含碳材料中,由含碳材料形成活性炭基体,其中活性炭基体的表面积为含碳材料的至少约5倍,和优选为含碳材料表面积的约10倍,和更优选约100倍,和最优选约300倍。含碳材料包括生物物质材料,所述生物物质材料包括曾经存活的有机物或由曾经存活的有机物,例如木材、动物废物或泥煤苔形成的任何材料。
在另一方面中,本发明可包括生产用无机酸浸渍的活性炭基体的方法,该方法包括下述步骤:
(a)视需要,干燥含碳材料到合适的含湿量;
(b)粉碎含碳材料成合适的粒度范围;和
(c)在混合这两种组分的同时,施加无机酸到含碳材料上。
在一个实施方案中,含碳材料可包括木材、动物废物或泥煤苔。可在施加无机酸之前,对含碳材料造粒,或者可对用无机酸浸渍的活性炭基体造粒。在一个实施方案中,可用水淘洗用无机酸浸渍的活性炭基体,在氨气化学吸附之后洗出肥料盐。
在另一方面中,本发明可包括从气流中化学吸附氨气的方法,该方法包括下述步骤:在用无机酸浸渍的活性炭基体上使气流通过或者使气流流经它。在一个实施方案中,该方法可包括下述步骤:
(a)将用无机酸浸渍的活性炭基体放置在反应器内;和
(b)使含氨的气体流经该反应器。
在一个实施方案中,在气体流动过程中扰动用无机酸浸渍的活性炭基体并且它可以是造粒或颗粒形式。
在另一方面中,本发明可包括将酸浸渍的活性炭基体转化成肥料产品的方法,该方法包括下述步骤:
1.通过将废活性炭基体暴露于氨气下,将活性炭基体内的酸转化成其相应的盐;和
2.筛选活性炭基体到所需的粒度范围或者对活性炭基体造粒,以实现所需的粒度范围。
在一个实施方案中,该方法进一步包括从活性炭基体中淘洗肥料产品,留下活性炭的步骤。
附图简述
通过例举的实施方案,参考简化的未成比例画出的附图,阐述本发明。在附图中:
图1示出了显示流动的气体的临界速度对活性炭基体所要求的床深度关系以维持所需的最小压降的图表。
发明详述
本发明涉及由用酸浸渍的含碳材料生产的固体多孔介质,和通过使气体流经用酸浸渍的固体多孔介质,从气流中除去氨气的装置,和使氨气与活性炭基体内浸渍的酸反应的副产物这一组合物。当描述本发明时,下述术语具有下述含义,除非另有说明。此处没有定义的所有术语具有其常见领域认识到的含义。
在下述说明是本发明的具体实施方案或特定用途的程度上,本发明仅仅是阐述目的,而不是限制要求保护的发明。下述说明拟覆盖包括在本发明的精神和范围内的在所附权利要求中定义的所有替代、改性和等价方案。
“含碳材料”应当是指任何生物物质材料,它包括最新或曾经存活的生物材料,例如植物、动物、藻类或微生物,或者由曾经存活的有机物洗出的任何材料或残渣。含碳材料可没有限制地包括木材和其他木质纤维素材料、动物废物或副产物,例如消化或堆肥(composted)的动物粪肥、农用副产物、泥煤苔、稻草、城市固体废物、含粪肥的垫底(bedding)材料、坚果壳、椰子皮纤维以及石化燃料和石化燃料副产物,例如煤和石油焦炭。
“液体酸”是指任何无机酸,其中包括,但不限于,硫酸、磷酸、硝酸或盐酸。
“活性炭”是指具有高表面积的固体微孔材料,它主要由元素碳组成且含有最初在活性炭由其形成的含碳材料内发现的小量其他元素,所述其他元素可包括,但不限于,诸如氧、氢、氮、硫、硅、铝、铁、钙、镁、钠和钾之类的元素。
“活性炭基体”是指足够多孔的固体形式的活性炭,以允许气体穿过其内部空间。
“气体”是指在标准温度和压力下以气态存在的任何物质或物质的结合物。
“化学吸附”是指固定或吸收气体分子在固体或液体表面上且可以接着发生在气体分子和固体或液体之间的任何反应。
发明人已发现,含碳材料将与液体酸反应,形成用酸浸渍的活性炭基体。这一反应可在环境条件下发生。
在一般的意义上,可通过下述形成酸浸渍的活性炭基体:
1.视需要,调节含碳材料的含湿量到所需的水平;
2.调节含碳材料的粒度到所需的范围;
3.施加液体酸到含碳材料上;和
4.混合含碳材料与液体酸,直到化学反应完成。
含碳材料可包括任何合适的生物物质材料,其中包括木材和其他木质纤维素材料、动物废物或副产物,例如消化或堆肥的动物粪肥、泥煤苔、稻草、城市固体废物、含粪肥的垫底材料、坚果壳、椰子皮纤维、煤和石油焦炭。木材碎片或刨花是尤其优选的含碳材料。
含碳材料的含湿量取决于原料和粒度,且范围可以是基于湿的物料,约0-50%,优选约5-35%,和更优选约15-25%。若含湿量高于所需水平,则可干燥含碳材料,或者可将水加入到含碳材料中,以达到该湿度水平。
可通过任何合适的方式,其中包括例如短切、粉碎、切割,或用其他方法降低粒度,将含碳材料加工成合适尺寸的颗粒,这取决于打算的应用和原料。另外,若原料由非常小的颗粒组成,则颗粒可能会聚集,产生合适尺寸的较大颗粒。含碳材料的粒度的平均范围可以是约0.1mm-10mm,优选约1-5mm,和更优选约3mm。
液体酸可以是任何合适的无机酸,例如硫酸、磷酸、盐酸或硝酸。若酸与化学吸附的分子反应,则酸的选择当然会改变所形成的盐。因此,若使用该材料从气流中除去氨气,则使用硫酸将导致形成硫酸铵。
所使用的液体酸的浓度取决于含碳材料的含湿量,较低的浓度适合于较低的含湿量,且范围可以是约20-100%,优选约75-100%,和更优选100%(其中100%是酸的浓形式)。所使用的液体酸的用量部分取决于含碳材料的粒度和所使用的酸的浓度,且范围可以是相对于1份较小颗粒的含碳材料(以重量计)约1份酸,到相对于1份最大(约10mm)颗粒10份酸。优选地,酸与含碳材料之比为约2∶1到5∶1,和更优选约4∶1(以重量计)。
混合含碳材料与液体酸,直到反应基本上完成,其时间长度取决于含湿量、粒度、酸浓度和酸/原料比,但典型地为约2-35分钟,优选约5-25分钟,和更优选约15分钟。在一个实施方案中,可通过温度来监控反应的完成。当反应启动时,温度典型地升高,达到最大值,和当反应完成时,温度下降。
在一个实施方案中,当进行混合时,将液体酸喷洒在含碳材料上。在另一实施方案中,将含碳材料形成为粒料,然后施加液体酸到含碳材料的造粒形式上。
酸将含碳材料转化到活性炭基体内,和过量酸本身浸渍在活性炭基体上。即使存在在碳基体内浸渍的大量酸,产物看起来且行为象固体材料。含大量强酸的固体基体在科学和商业上是重要的,因为与流经相同量的液体相比,气体可更加有效和便宜地流经多孔的活性炭基体。
在一个实施方案中,一步发生含碳材料转化成活性炭和酸的浸渍。此外,在用作化学吸附剂之前,不要求进一步加工酸浸渍的活性炭基体。因此,不要求或希望热处理、洗涤或中和步骤,或最后的气体磺化步骤。
结果,酸浸渍的碳基体可用作化学吸附剂材料,这是因为它具有微孔性和大的表面积。因此,流经该材料的气体内的任何碱性成分可更加有效地除去并转化成固体副产物。
在一个实施方案中,可使用该材料从气流中除去氨气。氨气与无机酸反应,形成相应的铵盐,且当气体流经时,被固体材料保留。
含氨气的气流可被导引通过或者固体、颗粒或者粒料形式的含酸浸渍的活性炭基体的密封反应腔室。活性炭基体可包括固定床或者可被气流或机械机构,例如用流化床或假流化床干扰。优选地,提供周期性更新或替代活性炭基体的机构。
通过酸浸渍的活性炭基体化学吸附氨气并转化成残留酸度很小且具有仅仅小量碳和其他元素的肥料盐。因此,废活性炭基体是一种农业和园艺应用的选择营养物的有用来源。正因为如此,除去氨气的成本下降且产生具有附加值的副产物。
可使用常规方法造粒废的活性炭基体,形成肥料的粒料或者用其他方法加工成有用的农业或园艺形式。若以颗粒形式造粒或加工,则粒料可提供铵盐肥料用缓释机构。
在一个实施方案中,用水从活性炭基体中淘洗铵盐,例如硫酸铵。然后可浓缩硫酸铵并形成为肥料,从而留下活性炭基体。
实施例-下述实施例拟阐述,但不限制要求保护的发明。
以从约2.5∶1到约4.5∶1变化的重量比将浓硫酸加入到含碳材料中。监控该材料的温度,并记录该材料中最终的酸含量。下表1中示出了结果。
表1在添加硫酸到碳源中之后,最终的酸含量和在活性炭基体内达到的最大温度
酸与碳源之比 | 最大温度(℃) | 最终酸含量(%) |
2.5 | 166.0 | 71.0 |
3.0 | 155.0 | 74.0 |
3.5 | 125.0 | 80.2 |
4.0 | 96.5 | 78.9 |
4.5 | 86.0 | 82.6 |
根据表1,也可看出,液体酸不仅将含碳材料转化成活性炭,而且导致在活化的碳基体内浸渍酸。取决于液体酸与含碳材料之比,多达82wt%的所得活性炭基体由酸组成。
而且,表1示出了当酸与含碳材料之比增加时反应的最大温度下降。尽管在表1中没有示出,但无一试验导致质量损失大于5%,也就是说,在反应以生产固体产物过程中,含碳材料和酸的损失之和没有超过5%。
数种含碳材料与硫酸反应的程度被量化。通过表面积大的变化来证明数种含碳材料转化成含活性炭的多孔活性炭基体。
表2添加浓硫酸(2.5份)到含碳材料(1份)中对表面积的影响
(1)衍生于厌氧消化
使含碳材料与液体酸反应将导致碳基体,特别是木材表面积大的增加。在反应之前,木材碎片的表面积为约2m2/g;在反应之后,表面积增加到大于600m2/g。这代表表面积约300倍的增加。应当注意,用硫酸处理的结果是,来自于牛粪的厌氧消化的生物固体显示出表面积约10倍增加,而在相同处理之后,商业泥煤苔显示出表面积约5倍的增加。
现已令人惊奇地发现,在气流内任何浓度的氨气将完全且快速地被酸浸渍的活性炭基体化学吸附。
表3载体气体特征和入口气体中NH3浓度对NH3吸附的影响
(1)相对湿度
(2)衍生于厌氧消化
表3列出的结果表明范围为百万分之95体积份-百万分之150,000体积份的气流中的氨气被活性炭基体化学吸附,以便氨气的出口浓度小于百万分之1份。而且,表3表明改变气体的温度或相对湿度没有影响氨气的化学吸附,条件是温度没有出现明显下降。
为了测定关键的应答变量,进行试验,以测定吸附100%存在于气流内的氨气所要求的最小床深和反应时间。
表4活性炭基体特征和气体温度对关键应答变量的影响
(1)关键应答变量是吸附100%NH3所要求的最小参数值
(2)衍生于厌氧消化
表4示出了需要仅仅7-11mm酸浸渍的活性炭基体,以快速(60-109ms)在10-17cm/s流动的气体中化学吸附所有氨气(约百万分之2000体积份)。我们的结论是,氨气的化学吸附非常快速且需要非常少地暴露于酸浸渍的活性炭基体物料内以供完全除去。表4示出了高的气体温度(60℃)没有影响化学吸附氨气所需的保留时间,只要当该气体流经活性炭基体时,它没有温降即可(在它们各自的温度下,所有气流用湿气饱和)。还值得注意的是,表3和表4示出了含碳材料源,不管它来自于木材刨花或者来自于牛粪的生物固体,没有显著影响氨气化学吸附所要求的保留时间。
通过试验,我们测定到酸浸渍的活性炭基体,甚至当它转化成其肥料盐时,和甚至当流速高时,会加速气体流动且最小压降均匀。图1所示的图表示出了对于已经通过化学吸附氨气转化成其肥料盐的非造粒的酸浸渍的活性炭基体来说,甚至采用80cm/s的流速流经10cm活性炭基体的情况下,压降没有超过1.5kPa。图1同样显而易见的是,当流速下降时,活性炭基体床的深度可呈指数增加,且没有引起大于1.5kPa的压降。此外,试验测定到,在相同的气体流速(以表面速度形式测量)下,扰动床(即周期性振动的床)引起的压降小于“固定”床(即在测试过程中没有扰动的床)。
通过单位质量的活性炭基体吸附的氨气比率来测量通过酸浸渍的活性炭基体吸附的氨气量。表6示出了酸浸渍的活性炭基体吸附200-223mg氨气/g活性炭基体,这代表20-23重量%氨气。
表6:相对于起始粒度,吸附的全部NH3(每克活性炭基体)和‘废’的酸浸渍的活性炭基体的堆积密度
粒度(mm) | 吸附的NH3(mg/g) | 堆积密度(kg/m3) |
<0.5 | 200 | 513 |
0.5-1.0 | 230 | 614 |
1.0-1.7 | 220 | 628 |
1.7-2.0 | 220 | 623 |
2.0-2.8 | 220 | 547 |
2.8-3.4 | 230 | 636 |
3.4-4.0 | 220 | 610 |
>4.0 | 230 | 680 |
表6还示出了在化学吸附氨气之后活性炭基体的堆积密度增加到约500-700kg/cm3。
进行测试,以测定在化学吸附氨气之后,酸浸渍的活性炭基体的化学组成。充分转化的酸浸渍的介质被称为“废”的活性炭基体。表7示出了在完成充分化学吸附氨气之后废的活性炭基体的化学组成。根据图7可看出,在完成氨气的化学吸附之后,肥料盐包括84重量%废活性炭基体。
表7在完成NH3的吸附之后,在酸浸渍的活性炭基体内的组分
组分 | 用量(%) |
硫酸铵 | 84.0 |
元素组成(1) | |
氮 | 18.0 |
硫 | 11.2 |
碳 | 5.9 |
氧 | 40.0 |
其他 | 4.3 |
残留酸 | 0.6 |
(1)包括硫酸铵中的元素和来自于吸附剂基体的残渣
而且,表7示出了仅仅0.6%原始的酸保留在废的活性炭基体内。废活性炭基体的元素组成与大比例的肥料盐一致,其中在得到表7列出数据的试验中,所述肥料盐是硫酸铵。由原始的木材刨花或其他含碳材料保留的碳含量小于6wt%。
Claims (23)
1.化学吸附氨气的固体组合物,它包括通过混合酸与含碳材料形成的用无机酸浸渍的活性炭基体。
2.权利要求1的固体组合物,其中无机酸包括硫酸、盐酸、磷酸或硝酸之一。
3.权利要求1的固体组合物,其中活性炭基体的表面积为至少约10m2/g。
4.权利要求3的固体组合物,其中活性炭基体的表面积为至少约30m2/g。
5.权利要求4的固体组合物,其中活性炭基体的表面积为至少约500m2/g。
6.权利要求1的固体组合物,其中活性炭基体的表面积为含碳材料的至少约5倍。
7.权利要求1的固体组合物,它为颗粒或粒料形式。
8.权利要求6的固体组合物,其中含碳材料包括木材、消化或堆肥的动物粪肥、泥煤苔、稻草、城市固体废物、含粪肥的垫底(bedding)材料、坚果壳、椰子皮纤维、煤或石油焦炭。
9.生产用无机酸浸渍的活性炭基体的方法,该方法包括下述步骤:
(a)视需要,干燥含碳材料到合适的含湿量;
(b)视需要,粉碎含碳材料成合适的粒度范围;和
(c)在混合这两种组分的同时,施加无机酸到含碳材料上。
10.权利要求9的方法,其中含碳材料包括木材、消化或堆肥的动物粪肥、泥煤苔、稻草、城市固体废物、含粪肥的垫底材料、坚果壳、椰子皮纤维、煤或石油焦炭。
11.权利要求9的方法,进一步包括在施加无机酸之前,对含碳材料造粒的步骤。
12.权利要求9的方法,进一步包括对用无机酸浸渍的活性炭基体造粒的步骤。
13.权利要求9的方法,其中无机酸包括硫酸、硝酸、磷酸或盐酸。
14.权利要求13的方法,其中无机酸包括浓硫酸。
15.从气流中化学吸附氨气的方法,该方法包括下述步骤:
(a)将用无机酸浸渍的活性炭基体置于反应器内;和
(b)使含氨气的气体流经该反应器。
16.权利要求15的方法,其中在气体流动过程中,扰动用无机酸浸渍的活性炭基体。
17.权利要求15的方法,其中用无机酸浸渍的活性炭基体为粒料或颗粒形式。
18.权利要求17的方法,其中在气体流动过程中,扰动用无机酸浸渍的活性炭基体的粒料或颗粒。
19.权利要求15的方法,其中无机酸包括硫酸、硝酸、磷酸或盐酸。
20.将酸浸渍的活性炭基体转化成肥料产品的方法,该方法包括下述步骤:
(a)通过将废活性炭基体暴露于氨气下,将活性炭基体内的酸转化成其相应的盐;和
(b)筛分活性炭基体到所需的粒度范围,或者对活性炭基体造粒,以实现所需的粒度范围。
21.权利要求20的方法,进一步包括从活性炭基体中淘洗肥料产品的步骤。
22.通过权利要求20的方法生产的肥料组合物。
23.通过权利要求21的方法生产的活性炭。
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Publication number | Publication date |
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JP2014205143A (ja) | 2014-10-30 |
AU2007288097B2 (en) | 2012-05-03 |
RU2595658C2 (ru) | 2016-08-27 |
RU2463107C2 (ru) | 2012-10-10 |
ES2588212T3 (es) | 2016-10-31 |
US20080047313A1 (en) | 2008-02-28 |
RU2009110159A (ru) | 2010-09-27 |
WO2008022461A1 (en) | 2008-02-28 |
RU2012121877A (ru) | 2013-11-27 |
US20120137744A1 (en) | 2012-06-07 |
EG26217A (en) | 2013-04-29 |
CA2845374A1 (en) | 2008-02-28 |
AU2007288097A1 (en) | 2008-02-28 |
US9114358B2 (en) | 2015-08-25 |
EP2081676B1 (en) | 2016-05-25 |
EP2081676A1 (en) | 2009-07-29 |
MX353962B (es) | 2018-02-06 |
UA99599C2 (ru) | 2012-09-10 |
CA2666727A1 (en) | 2008-02-28 |
CN103949210A (zh) | 2014-07-30 |
MX2009001945A (es) | 2009-04-14 |
CN101516497B (zh) | 2015-09-16 |
EP2081676A4 (en) | 2009-10-28 |
CA2666727C (en) | 2014-05-27 |
PL2081676T3 (pl) | 2016-12-30 |
CA2845374C (en) | 2015-12-22 |
JP2010501320A (ja) | 2010-01-21 |
US8198211B2 (en) | 2012-06-12 |
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