CN110740807A - 吸附剂和过滤器 - Google Patents

吸附剂和过滤器 Download PDF

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CN110740807A
CN110740807A CN201880036830.6A CN201880036830A CN110740807A CN 110740807 A CN110740807 A CN 110740807A CN 201880036830 A CN201880036830 A CN 201880036830A CN 110740807 A CN110740807 A CN 110740807A
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adsorbent
ethylene gas
ethylene
organic compound
precipitated silica
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Z·托帕利安
P·诺伯格
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Swedish Airlines
Svenska Aerogel AB
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Abstract

一种用于捕获乙烯气体的吸附剂，其包含BET表面积为至少200m2/g的无定形沉淀二氧化硅材料和结合至该无定形沉淀二氧化硅材料的表面的胺、亚胺或酰胺形式的有机化合物，其中所述有机化合物经配置用于化学吸附乙烯。用于冰箱的乙烯气体过滤系统包括含有吸附剂的乙烯气体过滤器和风扇，其中所述乙烯气体过滤器与所述风扇一起安装，使得气体借助于风扇主动循环通过乙烯气体过滤器。所述有机化合物可以是三异丙醇胺、聚乙烯亚胺或聚酰胺。

Description

吸附剂和过滤器
技术领域
本发明涉及一种用于捕获乙烯气体的吸附剂。本发明还涉及包含这种吸附剂的乙烯气体过滤器，涉及乙烯气体过滤系统，并且涉及所提出的吸附剂用于捕获乙烯气体的用途。
背景技术
近期研究表明，与食物供应链中产生的废物相关的经济成本中的一大部分发生在供应链末端的家庭中。废物的一种来源是储存在家用冰箱中的水果和蔬菜(生鲜产品)在食用前变质因而不得不丢弃。
在成熟过程中，许多水果和蔬菜天然地生成乙烯气体(C2H4)。它可以进一步刺激成熟，并增加生鲜产品的变质速度。可影响生鲜产品的乙烯浓度极低，因此，减少乙烯的存在或等效地减少其影响的方法可能有益于延长生鲜产品的货架期。
因此，减少家庭食物废物的重要补救措施是将乙烯控制技术与家用冰箱结合使用。已经存在一些技术，包括通过使用包含高锰酸钾的吸附剂包在冰箱中吸附乙烯，向冰箱中添加臭氧以充当乙烯控制剂，以及用1-甲基环丙烯形式的乙烯抑制剂处理生鲜产品。
然而，当冰箱温度被很好地控制并且由于开关门相对频繁地通风时，发现上述技术不太可能具有很大的益处。另外，在处理和储存食物的环境中使用上述化学品存在问题。
发明内容
本发明的主要目的是提供一种在至少某些方面改进的技术，借助该技术可以从储存生鲜产品的位置、例如从冰箱中去除乙烯气体。特别地，本发明的目的是提供这样一种技术，其可以相对有效地去除乙烯，而不必用化学品处理生鲜产品并且不使用有害物质例如高锰酸钾。另一个目的是提供一种捕获乙烯气体的吸附剂，该吸附剂可以经济有效地生产。
根据本发明的第一方面，通过权利要求1所述的用于捕获乙烯气体的吸附剂来实现至少上述主要目的。所述吸附剂包含：
-BET表面积为至少200m2/g的无定形沉淀二氧化硅材料；和
-结合至无定形沉淀二氧化硅材料的表面的胺、亚胺或酰胺形式的有机化合物，其中所述有机化合物经配置用于化学吸附乙烯。
根据本发明的吸附剂可用于从储存生鲜产品的任何环境中去除乙烯气体。吸附剂可以借助化学吸附有效地从例如冰箱中去除乙烯气体而不使用高锰酸钾。由于无定形沉淀二氧化硅材料的大的BET表面积，在乙烯的化学吸附方面具有活性的有机化合物可以散布在大的表面上，从而在吸收乙烯时变得有活性。进而，通过将碱金属硅酸盐与盐溶液混合然后进行常压干燥可以经济有效地生产该吸附剂，例如先前在WO2006/071183中所述，其中可以将有机化合物在二氧化硅沉淀之前加入到盐溶液中，或在洗涤和脱水后加入沉淀二氧化硅。在这两种情况下，在生产过程中可以有效地包括用有机化合物掺杂无定形沉淀二氧化硅。
有机化合物应该是一种能够与乙烯进行化学反应并形成表面结合的反应产物从而将其捕获在吸附剂的多孔结构中的化合物。由于有机化合物起化学吸附乙烯气体的作用，因此在例如温度和/或乙烯气体浓度变化时，捕获在吸附剂内的乙烯不释放。根据本发明，已发现当酰胺、亚胺或胺形式的有机化合物结合到无定形沉淀二氧化硅材料的表面时适用于此目的。优选地，吸附剂不包含除所述酰胺、亚胺或胺形式的有机化合物以外的其他有机化合物。
根据一个实施方式，无定形沉淀二氧化硅材料的BET表面积为至少300m2/g，优选至少400m2/g。相对大的BET表面积有利于吸附剂的吸附效率并增加乙烯吸收。
根据一个实施方式，无定形沉淀二氧化硅材料是包括根据式MeyO×m SiO2的多孔颗粒的聚集物的介孔材料，其中Me表示选自Ca、Mg、Cu、Zn、Mn、Cd、Pb、Ni、Fe、Cr、Al、Ti、V、Co、Mo、Sn、Sb、Sr、Ba和W的任意两种以上的金属，y表示金属成分与氧的摩尔比，且m表示SiO2/MeyO的摩尔比。先前已经在WO2006/071183中描述了这种无定形沉淀二氧化硅材料的制造方法。已知根据该式的沉淀二氧化硅材料具有相对大的BET表面积，并且可以在介孔范围内(即2-50nm)以合适的孔径制造。m的值可以在1-4之间变化，或者最好在2-3.7之间变化，例如m＝3.35。取决于金属的价态，y的值可能会在0.5-2的范围内变化。
根据一个实施方式，Me表示Ca和Mg。已经证明，Ca和Mg的组合在BET表面积、孔径分布和二氧化硅材料与有机化合物的掺杂性方面给出良好的结果。Ca/Mg的摩尔比可以例如为35/65或32/68，但是当然可以优化该摩尔比以实现对所选有机化合物的期望掺杂性。优选地，Ca/Mg的摩尔比在0.05＜Ca/Mg＜1.0的范围内变化。
根据一个实施方式，有机化合物在吸附剂中的存在量为1-20重量％，优选为2-12重量％，更优选为5-10重量％。在此，该量以占吸附剂总重量的干物质的重量百分比(重量％)给出。通过包含至少1重量％、优选至少2重量％、且更优选至少5重量％，可以实现所需的乙烯吸附水平。通过将所述量限制为20重量％、优选12重量％、更优选10重量％，可以避免对吸附剂的BET表面积、孔径和机械强度的负面影响。
根据一个实施方式，有机化合物是聚酰胺。已发现包含聚酰胺(PA)的吸附剂在乙烯捕获方面显示出有前景的结果。在这种情况下，聚酰胺包括脂族聚酰胺，例如尼龙6((C6H11NO)n)和尼龙6,6等。在该实施方式中，通过在向盐溶液加入PA然后与碱金属硅酸盐溶液混合并随后沉淀出二氧化硅，可以经济有效地生产吸附剂。因此，可以在生产过程中有效地包括用有机化合物掺杂的无定形沉淀二氧化硅，而无需额外的干燥步骤。
根据一个实施方式，有机化合物是三异丙醇胺。与例如基于高锰酸钾的吸附剂相比，包含三异丙醇胺(TIPA)的吸附剂在乙烯捕获方面显示出非常有前景的结果。
根据一个实施方式，有机化合物是聚乙烯亚胺。包含聚乙烯亚胺(PEI)的吸附剂在乙烯捕获方面显示出有前景的结果。优选地，在该实施方式中，吸附剂包含10-20重量％的聚乙烯亚胺。
本发明还涉及一种用于冰箱的乙烯气体过滤器，该乙烯气体过滤器包括根据上述实施方式中的任一个所提出的吸附剂。乙烯气体过滤器可包括用于保持吸附剂的气体渗透性载体。冰箱可以是家用或商用冰箱。
本发明的另一个目的是实现与被动式乙烯气槽相比对冰箱中乙烯吸收的改善。该目的通过权利要求10所述的用于冰箱的乙烯气体过滤系统来实现。乙烯气体过滤系统包括所提出的乙烯气体过滤器，其与风扇一起安装，从而使得气体能够借助风扇主动循环通过乙烯气体过滤器。风扇可以例如是蒸发器风扇，其适于吹动空气经过冰箱的蒸发器盘管并以比自然对流更有效的方式将其分配到整个冰箱内部。
根据本发明，风扇与所提出的乙烯气体过滤器结合使用，该乙烯气体过滤器包含上述实施方式中的任一个所述的吸附剂，从而乙烯的吸收比仅利用被动吸附更加有效。通过使冰箱的内部空气通过过滤器再循环，若干冰箱体积的空气可以通过过滤器，从而可以改善对储存在冰箱中的生鲜产品产生的不希望的乙烯的吸收。
本公开还涉及根据上述实施方式中任一项所提出的吸附剂在捕获乙烯气体中的用途。优选但非排他地，本公开涉及所述吸附剂在冰箱中用于捕获乙烯气体的用途。
从下文的详细描述中，本发明的其他优点和有利特征将变得明显。
附图说明
下文中将参照附图描述本发明的实施方式，其中：
图1示出了对于200ppm的乙烯气体浓度，根据本发明的吸附剂的去除效率对时间的函数，以及
图2显示了对于10ppm的乙烯气体浓度，根据本发明的吸附剂的去除效率对时间的函数。
具体实施方式
根据本发明的一个实施方式的用于捕获乙烯气体的吸附剂包括具有通式MeyO×mSiO2的沉淀二氧化硅材料，其中Me表示选自Ca、Mg、Cu、Zn、Mn、Cd、Pb、Ni、Fe、Cr、Al、Ti、V、Co、Mo、Sn、Sb、Sr、Ba和W的任意两种以上的金属，y表示金属成分与氧的摩尔比，且m表示SiO2/MeyO的摩尔比。无定形沉淀二氧化硅材料可以是CMS型
Figure BDA0002300353850000041
材料的形式，其可以写为(Ca0.35,Mg0.65)O×3.35SiO2，即Me＝(Ca0.35,Mg0.65)，y＝1，且m＝3.35。
在WO 2006/071183中公开了通过将碱金属硅酸盐与盐溶液混合来制造该材料的方法。该材料通过将碱金属硅酸盐与盐溶液混合而作为沉淀物形成。此后以各种方式处理沉淀物，以获得在孔径、粒径、表面积、密度等方面具有所需性质的最终产物。用于根据本发明实施方式的吸附剂的无定形沉淀二氧化硅材料具有介孔结构，其BET表面积为至少200m2/g，优选至少300m2/g或更优选至少400m2/g。
无定形沉淀二氧化硅材料掺杂有结合到无定形沉淀二氧化硅材料的表面的胺、亚胺或酰胺形式的有机化合物，其中有机化合物被配置用于化学吸附乙烯。有机化合物可以优选地为三异丙醇胺(TIPA)的形式，而且已发现聚酰胺(PA)和聚乙烯亚胺(PEI)也有益于捕获乙烯气体。有机化合物在吸附剂中的存在量优选为1-20重量％，更优选为2-12重量％，甚至更优选为5-10重量％。但是，这取决于例如使用哪种有机化合物、掺杂方法、无定形沉淀二氧化硅材料的可用BET表面积以及该材料的孔径。
本发明的吸附剂可以有利地包括在放置在冰箱中的乙烯气体过滤器中，旨在从冰箱的内部环境中去除乙烯气体。为此，吸附剂可以承载在气体渗透性载体上，例如在过滤盒中。乙烯气体过滤器可以优选地形成用于冰箱的乙烯气体过滤系统的一部分，该乙烯气体过滤系统除了乙烯气体过滤器之外还包括风扇，例如冰箱的蒸发器风扇。在这种情况下，乙烯气体过滤器位于风扇的上游或下游，从而含乙烯气体的空气借助于风扇主动循环通过乙烯气体过滤器。当包含低浓度(如1-10ppm)的乙烯气体的空气通过乙烯气体过滤器时，乙烯气体被吸附剂化学吸附，从而从冰箱的内部环境中去除。
实施例
制造了多个根据本发明实施方式的示例性乙烯吸附剂S1-S4并与参照的现有技术吸附剂Ref1-Ref3一起进行测试。经测试的吸附剂列于表I。
Figure BDA0002300353850000051
表I
S1-S4的无定形沉淀二氧化硅材料是CMS型材料。根据WO 2006/071183中所述的方法制备吸附剂S1、S3和S4，其中将钙和镁源添加至稀的活性硅酸钠水溶液中。以68mol％的Mg和32mol％的Ca的比例制备包含MgCl2和CaCl2的盐溶液。将盐溶液倒在1.5M(相对于SiO2)的硅酸钠溶液上，并在室温搅拌所得混合物。随后发生凝结，然后将形成的浆料洗涤并通过真空抽吸在滤布上脱水以变成饼或凝胶。将包含TIPA和PEI之一的稀溶液添加到获得的凝胶中。充分混合后，将经掺杂的凝胶干燥以获得粉末或颗粒形式的吸附剂。
含有PA的吸附剂S2根据略有不同的方案制备。在该情形中，首先按照先前B.Sun，“Study on the mechanism of nylon 6,6dissolving process using CaCl2/MeOH asthe solvent”,Chinese Journal of Polymer Science,vol.12，p57,1994中描述的方法将PA溶解在甲醇/CaCl2溶液中。此后，作为第一步，将包含PA的甲醇/CaCl2溶液与硅酸钠溶液混合，导致掺杂有PA的无定形二氧化硅沉淀。随后，将MgCl2溶液添加到混合溶液中以使反应完成。此后可以洗涤、过滤和干燥凝胶以获得粉末或颗粒形式的吸附剂。
表I中列出的吸附剂被分成每个3g的样品。此后，在第一轮测试中对样品S1-S3和Ref1-Ref3进行测试，其通过在7℃的温度和70％RH的相对湿度下使包含200ppm乙烯气体的空气通过样品进行。该温度和相对湿度类似于冰箱中的条件，但是通常可预期在冰箱中乙烯浓度会低得多，例如1ppm量级。空气的体积流量为0.9l/min。以百分比计的去除效率对时间的函数如图1所示。如图1的图中可见，包含10重量％的TIPA的吸附剂S1在这些条件下具有随时间推移明显高于其他样品的去除效率。一小时后，去除效率约为25％，两小时后约为20％，六小时后约为10％。因此，六小时后，该吸附剂仍具有剩余容量。所有其他吸附剂均显示出相似的去除效率。
表I中显示了在第一轮测试期间在200ppm的乙烯下不同吸附剂的以mg计的乙烯总吸收量。含10重量％TIPA的样品S1的总吸收最高，而含40重量％PEI的样品S4也相对较高。
通过在7℃的温度和70％RH、50％RH和18％RH的不同相对湿度浓度下使包含10ppm乙烯气体的空气通过样品，对一些样品进行了进一步测试。结果显示在表II中，列出了以mg乙烯/克吸附剂表示的吸收量。对于包含10重量％TIPA的吸附剂S1，对于70％RH的总乙烯吸收量为0.30mg乙烯/克吸附剂，对于50％RH为0.34mg/克吸附剂，对于18％RH为0.04mg/克吸附剂。换言之，包含TIPA的吸附剂S1需要一定量的相对湿度才能发挥最佳作用。在乙烯浓度为10ppm且相对湿度为50％RH时对包含PA的吸附剂S1、S2和Ref3的比较表明，含TIPA的吸附剂S1的总吸收量最高(0.034mg/克吸附剂)，其次是含PA的吸附剂S2(0.05mg/克吸附剂)，而参照吸附剂Ref3在该浓度下的总吸收量低得多(0.004mg/克吸附剂)，尽管其比样品S2在200ppm乙烯时的乙烯吸收量略高。
表II
样品 10ppm，70％RH 10ppm，50％RH 10ppm，18％RH
S1 0.30 0.34 0.04
S2 0.05
S4 0.04
Ref3 0.004
还测试了是否可以通过在50％RH和7℃下使用10ppm乙烯气体的两轮测试之间使吸附剂静置来重新使用包含10％TIPA的吸附剂S1。第一轮测试导致重量减轻了22％，这是由于水分损失造成的。经17天静置期后，向吸附剂添加相应量的水以补偿该重量损失，然后在相同条件下对吸附剂进行第二轮测试。结果如图2所示，显示了两轮测试的去除效率对时间的函数。发现吸附剂在第二轮测试中的效果几乎与第一轮测试一样好。
总而言之，实验结果表明，所有吸附剂S1-S4都可以在类似于冰箱中的条件下发挥捕获乙烯气体的作用。
当然，本发明绝不限于上述实施方式。相反，在不背离诸如所附权利要求书所限定的本发明的基本构思的情况下，许多可能的对其的修改对于本领域普通技术人员将是显而易见的。

Claims (11)

1.一种用于捕获乙烯气体的吸附剂，其包含：
-BET表面积为至少200m2/g的无定形沉淀二氧化硅材料；和
-结合至所述无定形沉淀二氧化硅材料的表面的胺、亚胺或酰胺形式的有机化合物，其中所述有机化合物经配置用于化学吸附乙烯。
2.如权利要求1所述的吸附剂，其中，所述无定形沉淀二氧化硅材料的BET表面积为至少300m2/g，优选至少400m2/g。
3.如权利要求1或2所述的吸附剂，其中，所述无定形沉淀二氧化硅材料是包括根据式MeyO×m SiO2的多孔颗粒的聚集物的介孔材料，其中Me表示选自Ca、Mg、Cu、Zn、Mn、Cd、Pb、Ni、Fe、Cr、Al、Ti、V、Co、Mo、Sn、Sb、Sr、Ba和W的任意两种以上的金属，y表示金属成分与氧的摩尔比，且m表示SiO2/MeyO的摩尔比。
4.如权利要求3所述的吸附剂，其中，Me表示Ca和Mg。
5.如前述权利要求中任一项所述的吸附剂，其中，所述有机化合物在所述吸附剂中的存在量为1重量％至20重量％，优选为2重量％至12重量％，并且更优选为5重量％至10重量％。
6.如前述权利要求中任一项所述的吸附剂，其中，所述有机化合物是聚酰胺。
7.如权利要求1至5中任一项所述的吸附剂，其中，所述有机化合物是三异丙醇胺。
8.如权利要求1至5中任一项所述的吸附剂，其中，所述有机化合物是聚乙烯亚胺。
9.一种用于冰箱的乙烯气体过滤器，其包含前述权利要求中任一项所述的吸附剂。
10.一种用于冰箱的乙烯气体过滤系统，其包括权利要求9所述的乙烯气体过滤器和风扇，其中，所述乙烯气体过滤器与所述风扇一起安装，使得气体借助所述风扇主动循环通过所述乙烯气体过滤器。
11.权利要求1-8中任一项所述的吸附剂在捕获乙烯气体中的用途。
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