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CN112642404A - 一种可降解吸附剂及其制备方法、应用 - Google Patents

一种可降解吸附剂及其制备方法、应用 Download PDF

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CN112642404A
CN112642404A CN202011381180.4A CN202011381180A CN112642404A CN 112642404 A CN112642404 A CN 112642404A CN 202011381180 A CN202011381180 A CN 202011381180A CN 112642404 A CN112642404 A CN 112642404A
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周大钊
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Anhui Hongchang Sugar Industry Technology Co ltd
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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    • C13B20/00Purification of sugar juices
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    • C13BPRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00Purification of sugar juices
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J2220/00Aspects relating to sorbent materials
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Abstract

本发明公开了一种可降解吸附剂的制备方法,包括如下步骤:将活性炭在明胶水溶液中分散均匀得到溶液A,将溶液A与有机溶剂、表面活性剂混匀乳化得到乳化液,然后用交联剂固化,固液分离,真空冷冻干燥得到可降解吸附剂。本发明还公开了一种可降解吸附剂,按照上述可降解吸附剂的制备方法制得。本发明还公开了上述可降解吸附剂在甘蔗糖液除杂脱色中的应用。本发明具有良好的吸附性能,可重复利用,且可以降解不会污染环境。

Description

一种可降解吸附剂及其制备方法、应用
技术领域
本发明涉及吸附剂技术领域,尤其涉及一种可降解吸附剂及其制备方法、应用。
背景技术
在蔗糖,是食糖的主要成分。广泛应用于各行各业,尤其是食品和药用辅料中。在蔗糖制备工艺中,常需要对蔗汁、糖浆等物料进行澄清处理。
目前甘蔗糖厂常采用亚硫酸法澄清生产工艺,以二氧化硫与石灰乳反应生成的亚硫酸钙为主要的澄清剂和脱色剂,所产白糖存在残硫问题,不能满足医药、食品的需求。另外,蔗糖制糖过程中,会产生大量甘蔗渣,其堆积和废弃会污染环境。
发明内容
基于背景技术存在的技术问题,本发明提出了一种可降解吸附剂及其制备方法、应用,本发明具有良好的吸附性能,可重复利用,且可以降解不会污染环境。
本发明提出的一种可降解吸附剂的制备方法,包括如下步骤:将活性炭在明胶水溶液中分散均匀得到溶液A,将溶液A与有机溶剂、表面活性剂混匀乳化得到乳化液,然后用交联剂固化,固液分离,真空冷冻干燥得到可降解吸附剂。
优选地,活性炭的粒径≤3μm。
优选地,活性炭是用甘蔗渣制备的活性炭。
上述活性炭的制备方法可以按照本领域常规生物质活性炭的制备方法制得。
优选地,活性炭、明胶的重量比为0.06-0.08:1。
优选地,溶液A、有机溶剂的体积比为12.5-20:80。
优选地,有机溶剂和表面活性剂的体积重量比为80ml:0.1-0.3g。
优选地,明胶和交联剂的重量比为1:0.15-0.2。
优选地,明胶水溶液的质量分数为5-8wt%。
优选地,于室温固化2.5-3h。
优选地,真空冷冻干燥的温度为-15至-10℃。
优选地,有机溶剂为乙酸乙酯、甲苯、液体石蜡中的至少一种。
优选地,表面活性剂为失水山梨醇脂肪酸酯、山梨醇酐单月桂酸酯聚氧乙烯醚中的至少一种。
上述失水山梨醇脂肪酸酯可以选用司盘80等,山梨醇酐单月桂酸酯聚氧乙烯醚可选用吐温20等。
优选地,交联剂为甲醛、戊二醛中的至少一种。
上述水均为去离子水。
本发明还提出了一种可降解吸附剂,按照上述可降解吸附剂的制备方法制得。
本发明还提出了上述可降解吸附剂在甘蔗糖液除杂脱色中的应用。
有益效果:
本发明选用明胶水溶液和适宜粒径的活性炭混匀,然后制备乳化液,并用交联剂交联固化得到明胶微球,明胶分子链上含有丰富的氨基、羧基和羟基,具有一定的吸附性能,在明胶微球中引入活性炭,使得明胶微球表面呈粗糙多孔状态,进而大幅提高其吸附性能,经冷冻干燥使得微球具有交联网络与活性炭的多孔状态相互配合,进一步提高本发明的吸附性能;另外将明胶微球化,改善其遇水易溶胀的问题,提高吸附性能的稳定性,使得本发明可以重复利用;还有明胶可以自然降解,不会污染环境;选用甘蔗渣制备活性炭,可以解决在制糖过程中,剩余甘蔗渣容易污染环境的问题,可降低原料成本。发明人惊喜的发现,本发明可以很好的去除甘蔗糖液中杂质和色素,脱盐脱色,解决残硫问题。
具体实施方式
下面,通过具体实施例对本发明的技术方案进行详细说明。
实施例1
一种可降解吸附剂的制备方法,包括如下步骤:将0.06g粒径≤3μm的活性炭(甘蔗渣制备的活性炭)加入20ml质量分数为5wt%明胶水溶液中,超声分散均匀得到溶液A,
将20ml溶液A、0.1g司盘80加入80ml乙酸乙酯中,混匀乳化2h得到乳化液,然后滴加0.2g戊二醛于室温固化2.5h,过滤,用乙醇、水依次洗涤4次,然后于-10℃真空冷冻干燥得到可降解吸附剂,其平均粒径为61μm。
实施例2
一种可降解吸附剂的制备方法,包括如下步骤:将0.08g粒径≤3μm的活性炭(甘蔗渣制备的活性炭)加入12.5ml质量分数为8wt%明胶水溶液中,超声分散均匀得到溶液A,
将12.5ml溶液A、0.3g司盘80加入80ml甲苯中,混匀乳化2h得到乳化液,然后滴加0.15g戊二醛于室温固化3h,过滤,用乙醇、水依次洗涤4次,然后于-15℃真空冷冻干燥得到可降解吸附剂,其平均粒径为70μm。
实施例3
一种可降解吸附剂的制备方法,包括如下步骤:将0.07g粒径≤3μm的活性炭(甘蔗渣制备的活性炭)加入16ml质量分数为6.5wt%明胶水溶液中,超声分散均匀得到溶液A,
将16ml溶液A、0.2g司盘80加入80ml液体石蜡中,混匀乳化2h得到乳化液,然后滴加0.17g戊二醛于室温固化2.8h,过滤,用乙醇、水依次洗涤4次,然后于-13℃真空冷冻干燥得到可降解吸附剂,其平均粒径为65μm。
对比例1
一种明胶微球的制备方法为:将16ml质量分数为6.5wt%明胶水溶液、0.2g司盘80加入80ml液体石蜡中,混匀乳化2h得到乳化液,然后滴加0.17g戊二醛于室温固化2.8h,过滤,用乙醇、水依次洗涤4次,然后于-13℃真空冷冻干燥即得,其平均粒径为50μm。
对比例2
同实施例3的活性炭。
实验1
取甘蔗混合汁过200目滤网,然后加入磷酸(其浓度为300mg/L),用石灰乳调节pH=6.6,等分成6份,每份均为100ml,
取5份均加热至50℃,然后分别加入实施例1-3、对比例1-2(实施例1-3和对比例1-2的质量分数均为2wt%)分别记为实验组1-3、对照组1-2,然后用石灰乳调节pH=7.0,加热至90℃,再加入聚丙酰胺(每组浓度均为2mg/L),保温沉降,固液分离得到清汁;
第6份通入20ml SO2(记为对照组3),加热至90℃,再加入聚丙酰胺(浓度为2mg/L),保温沉降,固液分离得到清汁。
按照《甘蔗制糖化学管理分析方法》检测混合汁和清汁的纯度差△G.P、脱色率,结果如表1所示。
△G.P=清汁的重力纯度-混合汁的重力纯度。
脱色率=(IU清汁-IU混合汁)/IU混合汁*100%,其中,于420nm检测色值IU。
表1检测结果
分组 纯度差% 脱色率%
实验组1 2.7 73
实验组2 2.7 75
实验组3 2.8 74
对照组1 0.8 40
对照组2 0.4 28
对照组3 1.3 50
由表1可以看出,经本发明处理后,甘蔗混合汁和清汁的纯度差、脱色率均优于单独的明胶微球、活性炭和亚硫酸法,且没有残硫问题;本发明可以很好的去除甘蔗糖液中杂质和色素。
实验2
取实施例3制得的吸附剂,按照实验1的方法处理得到清汁;并经3次吸附-脱附循环,考察每次获得清汁的纯度差和脱色率,结果如表2所示。
脱附处理方法为:将使用后的吸附剂加入5g/L的氢氧化钠溶液中,于20-25℃保温振荡40min即可。
表2循环性能
Figure BDA0002809356710000051
Figure BDA0002809356710000061
由上表可以看出:本发明经3次吸附-脱附循环,清汁的纯度差和脱色率均优于亚硫酸法(如实验1中对照组3的数据),本发明可以重复使用。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。

Claims (10)

1.一种可降解吸附剂的制备方法,其特征在于,包括如下步骤:将活性炭在明胶水溶液中分散均匀得到溶液A,将溶液A与有机溶剂、表面活性剂混匀乳化得到乳化液,然后用交联剂固化,固液分离,真空冷冻干燥得到可降解吸附剂。
2.根据权利要求1所述可降解吸附剂的制备方法,其特征在于,活性炭的粒径≤3μm;优选地,活性炭是用甘蔗渣制备的活性炭。
3.根据权利要求1或2所述可降解吸附剂的制备方法,其特征在于,活性炭、明胶的重量比为0.06-0.08:1。
4.根据权利要求1-3任一项所述可降解吸附剂的制备方法,其特征在于,溶液A、有机溶剂的体积比为12.5-20:80;优选地,有机溶剂和表面活性剂的体积重量比为80ml:0.1-0.3g;优选地,明胶和交联剂的重量比为1:0.15-0.2。
5.根据权利要求1-4任一项所述可降解吸附剂的制备方法,其特征在于,明胶水溶液的质量分数为5-8wt%。
6.根据权利要求1-5任一项所述可降解吸附剂的制备方法,其特征在于,于室温固化2.5-3h。
7.根据权利要求1-6任一项所述可降解吸附剂的制备方法,其特征在于,真空冷冻干燥的温度为-15至-10℃。
8.根据权利要求1-7任一项所述可降解吸附剂的制备方法,其特征在于,有机溶剂为乙酸乙酯、甲苯、液体石蜡中的至少一种;优选地,表面活性剂为失水山梨醇脂肪酸酯、山梨醇酐单月桂酸酯聚氧乙烯醚中的至少一种;优选地,交联剂为甲醛、戊二醛中的至少一种。
9.一种可降解吸附剂,其特征在于,按照权利要求1-8任一项所述可降解吸附剂的制备方法制得。
10.一种如权利要求9所述可降解吸附剂在甘蔗糖液除杂脱色中的应用。
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