CN105712429B - 一种水杨醛改性壳聚糖吸附氧钒离子的方法 - Google Patents

一种水杨醛改性壳聚糖吸附氧钒离子的方法 Download PDF

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CN105712429B
CN105712429B CN201610214724.5A CN201610214724A CN105712429B CN 105712429 B CN105712429 B CN 105712429B CN 201610214724 A CN201610214724 A CN 201610214724A CN 105712429 B CN105712429 B CN 105712429B
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chitosan
vanadyl
salicylide
ion
modification
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CN105712429A (zh
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曾庆乐
黄艺
倪师军
周悦
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Chengdu Univeristy of Technology
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

氧钒(IV)离子存在于含钒废水、废渣和一些催化体系。改性的壳聚糖作为多种重金属离子的吸附材料，但未见用于吸附氧钒(IV)离子。本发明采用水杨醛改性的壳聚糖吸附材料用于吸附氧钒(IV)离子，对于50至200毫克/升的氧钒(IV)离子溶液，吸附率超过98%，残留浓度低于2毫克/升。该处理方法具有一定的应用前景。

Description

一种水杨醛改性壳聚糖吸附氧钒离子的方法
技术领域
该专利涉及高分子合成、环境保护的研究领域，具体的讲，就是一种用水杨醛改性壳聚糖的吸附材料吸附氧钒离子的方法。
背景技术
壳聚糖通过改性，可以有效地提高它对过渡金属离子的吸附性能。已经有不少文献报道了水杨醛改性的壳聚糖的制备方法(《化学研究》，2005年，16卷，29-31页)，也有不少文献报道了水杨醛改性的壳聚糖对多种过渡金属离子的吸附性能，例如Hg2+、Cd2+、Pb2+、Au3 +、Ag+、Cr3+、Ni2+、Zn2+、Co2+(《化学研究》，2005年，16卷，29-31页；Carbohydrate Polymers2004年，55卷，77–93；《环境化学》，1997年，16卷，55-59页)。
对五价钒提取回收的文献比较多。例如，有文献报道了通过戊二醛交联的壳聚糖改性高分子，用于吸附钒酸根负离子(Ind.Eng.Chem.Res.1998年,37卷,1454-1463页)；环氧氯丙烷交联的壳聚糖用于偏钒(V)酸铵的吸附(分析科学学报，2004年，20卷，534-536页)；弱碱性阴离子交换树脂用于吸附含钒矿浆中的钒酸根阴离子(申请号:CN98112468.2，申请日:1998.05.08，公开(公告)号:CN1235201A，公开(公告)日:1999.11.17)。
氧钒(IV)离子，即VO2+存在于钒钛矿渣和含钒废水(水处理技术，1991,17,333-337)和多种催化体系(化工时刊，2007年,21卷,22-24)之中。但是，用于吸附氧钒(IV)离子的吸附材料，特别是水杨醛改性的壳聚糖用于吸附正四价的氧钒离子未见报道。因此，我们提供一种通过吸附脱除氧钒(IV)离子的方法。
发明内容
本发明公开一种水杨醛改性的壳聚糖用于吸附的氧钒(IV)离子的方法。
结合下面的实施例更详细地阐述本发明，并不认为它们是对本发明范围的限制。
具体实施方式
实施例一
水杨醛改性壳聚糖的合成工艺：称取1克壳聚糖(脱乙酰度≥95％，粘度100-200mpa.s)装到100毫升圆底烧瓶里，加入20毫升无水乙醇中，放到80℃预热的油浴锅中溶胀2小时，加入3.7克水杨醛，继续反应5至6小时。然后，将反应得到的产物转到锥形瓶中，放到超声波里超声30分钟，接着转移到布氏漏斗上抽滤，用水洗、95％乙醇洗。然后，再加入95％乙醇，超声30分钟，进一步水洗、95％乙醇洗、抽滤，再重复超声、洗涤、抽滤两次，除去未反应的水杨醛以及附着在高分子上未反应的水杨醛，最后将得到的改性高分子在70℃烘箱中干燥24小时，得到1.3克最终的水杨醛改性的壳聚糖。
实施例二
水杨醛改性壳聚糖吸附氧钒离子的工艺：称取高分子材料0.125克于100毫升的锥形瓶中，用移液管移取25毫升的氧钒(IV)离子储备液(钒(IV)离子浓度为130毫克/升)于此锥形瓶中，封口，震荡30分钟，再静置24小时。然后将吸附完成后的液体用每分钟4000转的速度离心30分钟，得到上清液，最后通过ICP-OES检测，得到吸附后溶液里钒(IV)离子的残留浓度为1.0毫克/升。
实施例三
水杨醛改性壳聚糖吸附氧钒离子的工艺：称取高分子材料0.125克于100毫升的锥形瓶中，用移液管移取25毫升的氧钒(IV)离子储备液(钒(IV)离子浓度为200毫克/升)于此锥形瓶中，封口，震荡30分钟，再静置24小时。然后将吸附完成后的液体用每分钟4000转的速度离心30分钟，得到上清液，最后通过ICP-OES检测，得到吸附后溶液里钒(IV)离子的残留浓度为1.9毫克/升。
实施例四
水杨醛改性壳聚糖吸附氧钒离子的工艺：称取高分子材料0.125克于100毫升的锥形瓶中，用移液管移取25毫升的氧钒(IV)离子储备液(钒(IV)离子浓度为50毫克/升)于此锥形瓶中，封口，震荡30分钟，再静置24小时。然后将吸附完成后的液体用每分钟4000转的速度离心30分钟，得到上清液，最后通过ICP-OES检测，得到吸附后溶液里钒(IV)离子的残留浓度为0.6毫克/升。

Claims (1)

1.一种水杨醛改性壳聚糖吸附氧钒(IV)离子的方法，其特征在于：用和含氧钒(IV)离子溶液的质量体积比为1:200，单位为克/毫升的水杨醛改性壳聚糖处理含氧钒(IV)离子浓度在50至200毫克/升的溶液，水杨醛改性壳聚糖对氧钒(IV)离子的吸附率达到98%以上，溶液中含氧钒(IV)离子的残留浓度低于2毫克/升；其中，水杨醛改性壳聚糖的合成工艺如下：称取1克壳聚糖，脱乙酰度≥95％，粘度100-200mpa.s，装到100毫升圆底烧瓶里，加入20毫升无水乙醇中，放到80℃预热的油浴锅中溶胀2小时， 加入3.7克水杨醛，继续反应5至6小时。然后，将反应得到的产物转到锥形瓶中，放到超 声波里超声30分钟，接着转移到布氏漏斗上抽滤，用水洗、95％乙醇洗。然后，再加入 95％乙醇，超声30分钟，进一步水洗、95％乙醇洗、抽滤，再重复超声、洗涤、抽滤两次，除去未反应的水杨醛以及附着在高分子上未反应的水杨醛，最后将得到的改性高分子在 70℃烘箱中干燥24小时，得到1.3克最终的水杨醛改性的壳聚糖。
CN201610214724.5A 2016-04-08 2016-04-08 一种水杨醛改性壳聚糖吸附氧钒离子的方法 Expired - Fee Related CN105712429B (zh)

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