CN108067181B - 一氧化碳高选择性吸收剂及其制造方法 - Google Patents
一氧化碳高选择性吸收剂及其制造方法 Download PDFInfo
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Abstract
本发明涉及一氧化碳高选择性吸收剂及其制造方法,更具体地,涉及包括铜化合物被分散的勃姆石或假勃姆石支撑体的一氧化碳高选择性吸收剂及其制造方法。
Description
技术领域
本发明涉及选择性地吸收一氧化碳,且用于分离及提炼的一氧化碳高选择性吸收剂及其制造方法。
背景技术
在钢铁厂的炼钢工程发生的废气林茨-多纳维茨气体(LDG,Linz-Donawits Gas)包括一氧化碳(65~80%)、二氧化碳(5~7%)、微量的氮气,且高炉煤气(BFG,BlastFurnace Gas)包括一氧化碳(20~36%)、二氧化碳(4~13%)、氮气(55~61%)、氢气(1.5~8%),经所述废气发生的一氧化碳年产为300万吨,但现在排出的大部分一氧化碳不被回收,并成为热源燃烧。
正在形成一氧化碳生产源及发生源的多变化,对资源回收及高价值化产品(乙酸酯、聚氨酯、聚碳酸酯、甲酸、丙烯酸、光气等)适用的关心增加,因此,用于吸收及分离一氧化碳技术开发的要求变高。
当前,作为分离一氧化碳的技术,主要利用低温法、吸收法、吸附法等,且在这中吸附法是利用一氧化碳吸收剂,在费用侧面对中小规模的一氧化碳分离,具有有利的优点。
LDG、BFG等在钢铁厂的炼钢工程发生的废气的构成成分,由多量的一氧化碳和二氧化碳及微量气体构成,因此,为了吸收多量的一氧化碳,在常温常压要求一氧化碳吸收量和二氧化碳对比一氧化碳的选择度优秀的吸收剂。
通常,一氧化碳吸收剂作为沉积亚铜的形态,被用于从由氢气和一氧化碳构成的蒸汽重整气体、合成气体等,选择性地吸收一氧化碳并分离。亚铜化合物不溶解在一般溶剂,因此,这些一氧化碳吸收剂很难均匀地分散,利用将正铜盐在固体支撑体上沉着之后进行还原,转换为亚铜状态或将亚铜盐在固体支撑体上,进行汽化之后粘贴(粘附)方法等,但具有亚铜盐在固体支撑体上不均匀地分散或对一氧化碳的吸收特性低的问题。
发明内容
技术方案
本发明是为了解决如上述问题,涉及具有对一氧化碳的高选择性,包括分散有铜化合物的勃姆石或假勃姆石支撑体的一氧化碳高选择性吸收剂。
此外,本发明涉及经本发明的一氧化碳高选择性吸收剂的制造方法。
本发明要解决的课题不限定于上述提及的课题,没有被提及的其他课题,可从以下记载明确地被技术人员理解。
本发明的一个方面,涉及一氧化碳高选择性吸收剂,其包括:分散有铜化合物的勃姆石或假勃姆石支撑体。
根据本发明的一个实施例,所述勃姆石或假勃姆石支撑体是AlOX(OH)(3-2X)(H2O)Z(x<1.5),且所述勃姆石或假勃姆石支撑体的比表面积可以是300m2g-1以上。
根据本发明的一个实施例,所述勃姆石或者假勃姆石支撑体的孔隙容量可以是0.2m2g-1以上。
根据本发明的一个实施例,所述勃姆石或假勃姆石支撑体,可包括20nm以下的孔隙大小。
根据本发明的一个实施例,所述铜化合物可包括从氯化亚铜、氟化亚铜、碘化亚铜、溴化亚铜、氮氧化亚铜、醋酸亚铜、硫氰酸亚铜、硫苯甲酸铜、丁硫铜、苯甲酸亚铜、硫酸铜及硫代硫酸亚铜组成的组中选择的一种以上。
根据本发明的一个实施例,对于所述一氧化碳高选择性吸收剂,10wt%至50wt%的所述铜化合物,可分散在所述勃姆石或假勃姆石支撑体上。
根据本发明的一个实施例,所述一氧化碳高选择性吸收剂对二氧化碳的一氧化碳纯成分选择度(CO吸收量/CO2吸收量,20℃及1条吸收量比率基准)可以为4以上。
根据本发明的一个实施例,所述一氧化碳高选择性吸收剂在常温(20℃至30℃),每单位质量一氧化碳吸收量可以为1.35mmol/g以上,每单位质量二氧化碳吸收量为0.20mmol/g以下。
本发明的另一方面,涉及一氧化碳高选择性吸收剂的制造方法,其步骤包括:制造勃姆石或假勃姆石支撑体及铜化合物的混合物;及在勃姆石或假勃姆石支撑体上,热分散铜化合物。
根据本发明的一个实施例,所述热分散步骤可以在热分散温度250℃至350℃,下进行1小时至48小时。
根据本发明的一个实施例,所述热分散步骤可以在真空;或惰性气体、
还原气体或包括这两个的气氛下进行。
本发明的另一方面,涉及一氧化碳高选择性吸收剂的制造方法,其步骤包括:制造包括铜化合物及溶剂的浸渍溶液;接触勃姆石或假勃姆石支撑体与浸渍溶液,在支撑体浸渍铜化合物;烘干被浸渍的支撑体;及热处理被浸渍的支撑体。
根据本发明的一个实施例,所述烘干步骤在30℃至60℃的温度及真空;或者惰性气体、还原气体或包括这两个气氛,进行1小时至50小时,且所述热处理步骤在110℃至400℃的温度及真空;或者惰性气体、还原气体或包括这两个气氛,可进行10分钟至20小时。
根据本发明的一个实施例,所述浸渍的步骤,可利用初湿含浸法,在15℃至60℃温度进行。
根据本发明的一个实施例,所述溶剂可包括从水、甲苯、乙酸乙酯及乙腈组成的组中选择的一个以上,且所述浸渍溶液还包括从氨、硝酸、盐酸及硫酸组成的组中选择的一种以上。
附图说明
图1是示出根据本发明的一个实施例,是由本发明的一氧化碳高选择性吸收剂制造方法的流程图。
图2是示出根据本发明的其他实施例,是由本发明的一氧化碳高选择性吸收剂制造方法的流程图。
图3是示出根据本发明的实验例1,对制造的一氧化碳高选择性吸收剂的一氧化碳及二氧化碳的吸收量。
具体实施方式
以下,参照附图详细地说明本发明的实施例。在说明本发明的过程中,判断对有关公知功能或构成的具体说明不必要的模糊本发明的要点时,可省略其详细地说明。此外,在本说明书使用的用语(terminology)作为适当地表现本发明的优选实施例而被使用的用语,其可根据用户、运营者的意图或者本发明所属领域的惯例等而不同。因此,对本用语的定义,以本说明书整个内容为基础下定义。在各图提示的相同参照符号显示相同的部件。
本发明涉及一氧化碳高选择性吸收剂,根据本发明的一个实施例,经本发明的一氧化碳高选择性吸收剂,可提供在混合气体内,对一氧化碳的吸收选择度高,对一氧化碳高的吸收量。
根据本发明的一个实施例,经本发明的一氧化碳高选择性吸收剂,可包括铜化合物及勃姆石(Boehmite)或假勃姆石支撑体。
作为本发明的一个示例,所述一氧化碳高选择性吸收剂,可包括铜化合物分散在勃姆石或假勃姆石支撑体上的孔隙、表面或这两个,例如,在所述支撑体的孔隙、表面或这两个分散的铜化合物的勃姆石或假勃姆石支撑体。或者,在所述支撑体的表面、孔隙、表面,或者这两个,可包括铜化合物浸渍的勃姆石或假勃姆石支撑体。所述一氧化碳高选择性吸收剂,同时具有铜化合物和勃姆石或假勃姆石支撑体的特性,因此,比起适用现有沸石或者氧化铝支撑体的一氧化碳吸收剂,可提供更高的一氧化碳的选择度。
例如,所述勃姆石或假勃姆石支撑体可以是AlOX(OH)(3-2X)(H2O)Z,所述勃姆石或假勃姆石支撑体是铝氧化物,例如,比起结晶结构或非结晶结构铝氧化物或沸石等,可提供更好地一氧化碳的吸收性和选择度。例如,在AlOX(OH)(3-2X)(H2O)Z中,X是未满1.5、0以上及未满1.5,或者0.88以上及未满1.5范围内的实数,Z是0至1以下的实数。包括在所述范围内,铜化合物可均匀地分散在支撑体的孔隙、表面,或者这两个。
例如,所述勃姆石或假勃姆石支撑体的比表面积可以是300m2g-1以上,或者300m2g-1至500m2g-1。包括在所述比表面积范围内,增加一氧化碳的吸收面积,可提高对一氧化碳的吸收特性。
例如,所述勃姆石或假勃姆石支撑体的孔隙容量,可以是0.2cm3g-1以上,或者0.2cm3g-1至0.5cm3g-1。包括在所述孔隙容量范围内,可提高在所述勃姆石或假勃姆石支撑体上的铜化合物的分散含量。
例如,所述勃姆石或假勃姆石支撑体,可包括20nm以下、2nm至20nm,或者3nm至10nm的孔隙大小。包括在所述范围内,铜化合物均匀地分散在所述勃姆石或假勃姆石的孔隙、表面,或者这两个,可提供优秀的一氧化碳吸收特性。
例如,所述铜化合物可以是亚铜盐,且作为所述亚铜盐的示例,可包括从氯化亚铜、氟化亚铜、碘化亚铜、溴化亚铜、氮氧化亚铜、醋酸亚铜、硫氰酸亚铜、硫苯甲酸铜、丁硫铜、苯甲酸亚铜、硫酸铜及硫代硫酸亚铜组成的组中选择的一种以上。
例如,所述铜化合物对所述一氧化碳高选择性吸收剂,以10wt%至50wt%,或者25wt%至35wt%含量,可分散在所述勃姆石或假勃姆石支撑体。包括在所述含量范围内,高含量的铜化合物均匀地分散在所述支撑体上,因此,可提高对一氧化碳的吸收特性。
根据本发明的一个实施例,所述一氧化碳高选择性吸收剂对二氧化碳的一氧化碳的纯成分选择度(CO吸收量/CO2吸收量),可以是4以上、5以上,或者8以上。例如,所述一氧化碳高选择性吸收剂在常温(20℃至30℃),每单位质量的一氧化碳吸收量为1.35mmol/g以上,每单位质量二氧化碳吸收量,可以是0.20mmol/g以下。
本发明涉及经本发明的一氧化碳高选择性吸收剂的制造方法,根据本发明的一个实施例,经本发明的一氧化碳高选择性吸收剂的制造方法,可在勃姆石或勃姆石支撑体上均匀地分散高浓度的铜化合物,且可提供对一氧化碳吸收特性优秀的一氧化碳高选择性吸收剂。
根据本发明的一个实施例,经本发明的一氧化碳高选择性吸收剂的制造方法,可包括步骤110:制造勃姆石或假勃姆石支撑体及铜化合物的混合物;及步骤120:在勃姆石或假勃姆石支撑体上,热分散铜化合物。
作为本发明的一个示例,步骤110:制造勃姆石或假勃姆石支撑体及铜化合物的混合物,可磨碎勃姆石或假勃姆石及铜化合物,并进行混合。所述磨碎及混合,可利用在本发明的技术领域使用的装置,例如,可以是球磨机、搅拌器等。例如,步骤110:制造勃姆石或假勃姆石及铜化合物的混合物,可由勃姆石或假勃姆石对铜化合物为90:10~50:50,或者75:25~65:35(质量比)被混合。
作为本发明的一个示例,步骤120:在勃姆石或假勃姆石支撑体上,热分散铜化合物,在热分散温度250℃至350℃、250℃至330℃,或者270℃至300℃的温度,可由非活性气体气氛进行热分散。包括在所述温度范围内,防止AlOOH、结晶结构或非结晶结构铝氧化物的转换,维持勃姆石或假勃姆石支撑体的特性的同时,可在所述支撑体的孔隙、表面,或者这两个,诱导高浓度的铜化合物的均匀热分散。此外,防止转换为根据温度增加的铜化合物的金属铜(Cu),可使在一氧化碳吸收剂维持铜化合物的特性。
例如,步骤120:在勃姆石或假勃姆石支撑体上,热分散铜化合物,可进行1小时至48小时,且包括在所述事件范围内,维持铜化合物的特性的同时,可均匀地热分散在勃姆石或假勃姆石支撑体上。
作为本发明的一个示例,热分散步骤可在排除氧气和水分的环境下进行,例如,真空,或者氮气、氩、氦等惰性气体,或者氢气、一氧化碳等还原气体,或者包括这两个的气氛。
根据本发明的其他实施例,经本发明的一氧化碳高选择性吸收剂的制造方法,可包括步骤210:制造包括铜化合物及溶剂的浸渍溶液;步骤220:接触勃姆石或假勃姆石支撑体与浸渍溶液,在支撑体浸渍铜化合物;步骤230:烘干被浸渍的支撑体;及步骤240:热处理被浸渍的支撑体。
作为本发明的一个示例,步骤210:制造包括铜化合物及溶剂的浸渍溶液,混合包括从所述提及的铜化合物及水、甲苯、乙酸乙酯及乙腈组成的组中选择的一种以上的溶剂,可制造浸渍溶液。
例如,所述浸渍溶液溶解铜化合物,为了在支撑体诱导铜化合物的均匀浸渍,还可包括酸及碱,例如,可包括从氨基、硝酸、盐酸及硫酸组成的组中选择的一种以上,优选地,所述氨可以是20%至30%的氨水溶液,且1N至5N的硝酸、盐酸及硫酸的水溶液。
例如,步骤210:制造包括铜化合物及溶剂的浸渍溶液,可将所述铜化合物及所述溶剂,在常温至40℃温度,搅拌30分至4小时,制造浸渍溶液。
作为本发明的一个示例,浸渍的步骤220利用初湿含浸法,在15℃至60℃温度,或者30℃至40℃温度,可进行1小时至20小时。
作为本发明的一个示例,烘干的步骤230在浸渍的步骤220之后,滤过浸渍的支撑体,且在30℃至60℃温度,或者40℃至50℃温度及真空,或者惰性气体、还原气体或包括这两个的气氛,可烘干1小时至50小时,优选地,5小时至20小时。
作为本发明的一个示例,焙烧步骤240在烘干的步骤230之后,将浸渍的支撑体在如电炉等焙烧装置,流入真空,或者惰性气体、还原气体或者包括这两个的气氛,可在110℃至400℃温度,或者250℃至330℃温度,可焙烧10分钟至20小时,优选地,5小时至15小时。
根据本发明的一个实施例,经本发明的一氧化碳高选择性吸收剂的制造方法,还可包括在本发明的技术领域利用的磨碎、清洗等后处理工程等,但在本说明书不具体地提及。
参照本发明的优选实施例进行了说明,但本发明不限定于此,且不脱离以下的权利要求及记载在发明的详细说明的本发明的思想及领域范围内,对本发明可进行多样修改及变更。
实施例1
在勃姆石(7g)添加CuCl(3g),由球磨机磨碎并混合10分钟。其次,放入反应器在真空气氛,以300℃温度热分散24小时,由常温进行冷却获得吸收剂。
实施例2
将勃姆石(7g)在150℃烘干24小时。在氨水溶液(28%)10ml,混合CuCl(3g)之后,以密封的状态在常温搅拌1小时。利用初湿含浸法(incipient wetness impregnation)在常温将混合溶液,浸渍在所述准备的支撑体,在密封容器保管30分钟。之后,在维持40℃的真空炉,24小时放入氮气进行烘干。被烘干的吸收剂在氮气气氛的加热炉,以300℃焙烧12小时之后,保管在密封容器。
比较例1
将CuCl(3g)及氧化铝(7g)由球磨机磨碎并混合10分钟。其次,放入反应器在真空气氛,以300℃温度热分散24小时,由常温进行冷却获得吸收剂。
比较例2
将CuCl(3g)及沸石(13X,7g)由球磨机磨碎并混合10分钟。其次,放入反应器在真空气氛,以300℃温度热分散24小时,由常温进行冷却获得吸收剂。
比较例3
将CuCl(3g)及沸石(Y,7g)由球磨机磨碎并混合10分钟。其次,放入反应器在真空气氛,以300℃温度热分散24小时,由常温进行冷却获得吸收剂。
实验例1
在实施例及比较例制造的吸收剂,在测量吸收量之前,在300℃真空前处理3小时,去除不纯物等。CO(99.999%)的吸收量利用容量测定,分别在293K及101kPa气压进行测量,其结果在表1及图3显示。
【表1】
观察表1及图3,可确认经本发明的铜化合物包括分散的勃姆石支撑体的一氧化碳高选择性吸收剂,比起利用比较例1至3的氧化铝支撑体及沸石支撑体的吸收剂,一氧化碳选择度更好地增加。这使实施例的一氧化碳高选择性吸收剂,同时维持勃姆石支撑体及铜化合物的特性,分散铜化合物,因此,可提供对一氧化碳的高选择性。
实施例3至6
将显示在表2的勃姆石(AlOX(OH)(3-2X)(H2O)Z,7g)分别在150℃进行24小时烘干。在所述勃姆石添加CuCl(3g)由球磨机磨碎并混合10分钟。其次,放入反应器在真空气氛,以250℃、270℃、330℃及350℃温度,分别进行热分散24小时,由常温进行冷却获得吸收剂。
实施例2
在实施例3至6制造的吸收剂在在测量吸收量前,在300℃真空前处理3小时,去除不纯物等。CO(99.999%)的吸收量利用容量测定,分别在293K及101kPa气压进行测量,其结果在表2显示。
【表2】
观察表2,可确认经本发明的铜化合物包括分散的勃姆石或假勃姆石支撑体的一氧化碳高选择性吸收剂,提供优秀的一氧化碳选择度。
本发明提供铜化合物包括分散的勃姆石或假勃姆石支撑体的一氧化碳高选择性吸收剂,所述一氧化碳高选择性吸收剂,比起现有的吸收剂,可显示二氧化碳对比一氧化碳选择度更高的特性。
本发明可提供一氧化碳高选择性吸收剂,其适用勃姆石(Boehmite)或假勃姆石支撑体,对一氧化碳具有优秀的吸收量,且具有低二氧化碳吸收量。
经本发明的一氧化碳高选择性吸收剂,在混合气体内提高二氧化碳对比一氧化碳的选择度,可有效地适用在一氧化碳的选择性吸收及分离。
Claims (10)
1.一种一氧化碳高选择性吸收剂,其包括:
分散有铜化合物的勃姆石或假勃姆石支撑体,
其中所述铜化合物是热分散在所述支撑体上的亚铜盐,
其中所述勃姆石或假勃姆石支撑体是AlOX (OH)(3-2X)(H2O)Z ,其中x<1.5,
其中所述勃姆石或假勃姆石支撑体包括20nm以下的孔隙大小,
其中所述亚铜盐包括从氯化亚铜、氟化亚铜、碘化亚铜、溴化亚铜、醋酸亚铜、硫氰酸亚铜、苯甲酸亚铜及硫代硫酸亚铜组成的组中选择的一种以上。
2.根据权利要求1所述的一氧化碳高选择性吸收剂,其中,
所述勃姆石或假勃姆石支撑体的比表面积是300m2g-1 以上。
3.根据权利要求1所述的一氧化碳高选择性吸收剂,其中,所述勃姆石或假勃姆石支撑体的孔隙容量是0.2 cm3g-1以上。
4.根据权利要求1所述的一氧化碳高选择性吸收剂,其中,所述铜化合物热分散在所述勃姆石或假勃姆石支撑体的表面上;所述铜化合物热分散在所述勃姆石或假勃姆石支撑体的孔隙中;或所述铜化合物热分散在所述勃姆石或假勃姆石支撑体的表面上以及孔隙中。
5.根据权利要求1所述的一氧化碳高选择性吸收剂,其中,对于所述一氧化碳高选择性吸收剂,10wt%至50wt%的所述铜化合物分散在所述勃姆石或假勃姆石支撑体上。
6.根据权利要求1所述的一氧化碳高选择性吸收剂,其中,相对于二氧化碳,所述一氧化碳高选择性吸收剂对一氧化碳的纯成分选择性,即CO吸收量/CO2 吸收量为4以上。
7.根据权利要求1所述的一氧化碳高选择性吸收剂,其中,所述一氧化碳高选择性吸收剂在常温,即20℃至30℃下,每单位质量一氧化碳吸收量为1.35mmol/g以上,每单位质量二氧化碳吸收量为0.20mmol/g以下。
8.一种一氧化碳高选择性吸收剂的制造方法,其步骤包括:
制造勃姆石或假勃姆石及铜化合物的混合物;及
在所述勃姆石或假勃姆石上,热分散铜化合物,
其中所述勃姆石或假勃姆石支撑体是AlOX(OH)(3-2X)(H2O)Z ,其中x<1.5,
其中所述勃姆石或假勃姆石支撑体包括20nm以下的孔隙大小,
其中所述铜化合物是亚铜盐,
其中所述亚铜盐包括从氯化亚铜、氟化亚铜、碘化亚铜、溴化亚铜、醋酸亚铜、硫氰酸亚铜、苯甲酸亚铜及硫代硫酸亚铜组成的组中选择的一种以上。
9.根据权利要求8所述的一氧化碳高选择性吸收剂的制造方法,其中,所述热分散在热分散温度250℃至350℃进行1小时至48小时。
10.根据权利要求8所述的一氧化碳高选择性吸收剂的制造方法,其中,所述热分散在真空;惰性气体或还原气体的气氛;或者惰性气体和还原气体的气氛中进行。
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