CN114950351A - 一种掺杂改性ZSM-5分子筛强化吸附VOCs的方法与应用 - Google Patents
一种掺杂改性ZSM-5分子筛强化吸附VOCs的方法与应用 Download PDFInfo
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 55
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- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 12
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- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 4
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- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims 1
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims 1
- 229910052746 lanthanum Inorganic materials 0.000 claims 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims 1
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical compound [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 claims 1
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims 1
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 abstract description 21
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
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- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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Abstract
本发明提供了一种改性ZSM‑5分子筛的方法，将金属阳离子掺杂入ZSM‑5分子筛骨架结构中，改善其吸附VOCs的性能。具体实验步骤为：取1g ZSM‑5分子筛，加入配制好的金属盐溶液，置于烘箱中进行离子交换负载。自然冷却至常温，经过滤、干燥、煅烧后即可得到金属阳离子掺杂改性的分子筛。所述改性分子筛的合成条件温和、操作简便、易于控制，与未掺杂改性的空白ZSM‑5吸附性能对比发现，改性后的分子筛对于典型VOCs苯的吸附性能有明显提升。
Description
技术领域
本发明具体涉及一种掺杂改性ZSM-5分子筛强化吸附VOCs的方法与应用，属于材料与环境化工领域。
背景技术
挥发性有机物（VOCs）不仅有害人类身体健康，而且还是导致大气污染如光化学烟雾形成的主要成分。作为富集、分离净化VOCs的有效方法之一，吸附法拥有操作简单和经济可行等优点，而其与蓄热式催化燃烧（RCO）结合的综合处理技术是目前VOCs处理行业的重点推广的工艺。沸石转轮是现今吸附技术应用的典型设备，它能有效避免吸附材料加热再生时潜在的安全风险。其关键核心材料为分子筛，而ZSM-5分子筛对VOCs的吸附性能并不够好，尤其是对苯。作为一种吸附材料，分子筛吸附目标分子属于物理性吸附，其影响吸附性能的因素包括分子筛孔径、有机物极性以及表面结构和化学性质。而不同的硅铝比例往往会造成分子筛表面酸碱性的差异，从而影响其吸附和催化性能。而在分子筛吸附VOCs时会涉及与水分子的竞争吸附，单一从调节分子筛硅铝比无法达到理想的VOCs吸附效果。中国专利CN202010533312.4一种基于酸碱改性的稀土掺杂HZSM-5分子筛的制备方法，改性后的分子筛具有高活性、高选择性、较大比表面积等特点。传统ZSM-5分子筛内部存在表面积很大并且排列规整的空穴，这一特殊结构加上金属离子的反应活性，有望提高分子筛吸附和催化性能。中国专利CN201410488803.6将分子筛在一定温度下活化后再与可溶性金属盐或杂多酸等进行负载或交换改性，提高了分子筛吸附量。Yang等人通过浸渍法制备了掺杂Ce离子的改性ZSM-5分子筛，发现Ce和Cr的引入能提高ZSM-5分子筛对氯代挥发性有机物的催化活性和抗积碳能力(Chemical Engineering Journal,2013,234.)。Qin等人通过两阶段变温水热法，成功合成了一种具有分级孔结构的均匀纳米棒状晶体组装的铁掺杂ZSM-5微球，表现出优异的吸附能力和对氯苯的降解效率，但成本高不利于工业生成(Journal of Hazardous Materials,2020,385.)。涂等人发现金属离子Cu、Zn、Ce的负载可以增加ZSM-5分子筛的活性中心，而适量的Ce掺杂以及采用溶胶凝胶法制备可以使金属氧化物颗粒分散均匀，但此方法需要先进行碱液处理，较为繁琐(材料导报,2017,31(24):114-119)。可以看出金属离子掺杂改性分子筛可以强化吸附性能，但采用较简单的条件有效的提高其对VOCs的吸附的制备方法仍需进一步研究。
发明内容
本发明克服了制备条件繁琐、成本高、VOCs吸附性能较差等缺点，提出一种成本低、易于产业化的分子筛改性方法，并提高了分子筛的VOCs吸附性能。技术方案包括以下步骤：
利用掺杂改性ZSM-5分子筛强化吸附VOCs的方法与应用，包括以下步骤:
(1)分别配制50ml Cu2+、La2+、Ce3+等金属离子的盐溶液；
(2)取1g ZSM-5分子筛加入到上述盐溶液，并移至水热反应釜中，升温到80-150℃，反应4-10h；
(3)过滤分离出沉淀，经干燥、煅烧后得到金属阳离子掺杂改性分子筛；
(4)对改性后的分子筛进行典型VOCs吸附性能测试。
优选地，步骤(1)所述的溶液浓度为0.2mol/L。
优选地，步骤(1)所述的铜盐为硫酸铜、镧盐为硝酸镧、铈盐为硝酸铈。
优选地，步骤(2)所述的分子筛硅铝比为500。
优选地，步骤(2)所述的反应温度为120 ℃。
优选地，步骤(4)所述的典型VOCs为苯系物。
与现有技术相比，本发明具有以下优点:
（1）改性后的分子筛具有较大的比表面积、丰富的微孔结构，使得活性组分分散度高。再加上金属离子与分子筛结合力强且具有协同作用，可以强化VOCs吸附性能。（2）制备步骤简单，降低了吸附剂的制备成本，易于工业化生产。
附图说明
图1为本发明实例1的XRD图。
图2为本发明实例2的扫描电镜图。
图3为本发明实例3的BJH孔径分布图（小）与N2吸脱附等温曲线。
图4为本发明实例4的苯吸附的浓度变化曲线（空速为120000 mL g−1 h−1）。
具体实施方式
实施例1
(1)配制50ml 0.2mol/L的硫酸铜溶液；
(2)取1g 硅铝比为500的 ZSM-5分子筛，加入到硫酸铜溶液，并将混合物移至水热反应釜中，升温到120 ℃，反应6h；
(3)过滤分离出沉淀，干燥后在450 ℃下煅烧2h，得到金属阳离子掺杂改性分子筛；
(4)取50 mg改性后的分子筛进行苯吸附性能测试。
实施例2
(1)配制50ml 0.2mol/L的硝酸镧溶液；
(2)取1g 硅铝比为500的 ZSM-5分子筛，加入到硝酸镧溶液，并将混合物移至水热反应釜中，升温到120 ℃，反应6h；
(3)过滤分离出沉淀，干燥后在450 ℃下煅烧2h，得到金属阳离子掺杂改性分子筛；
(4)取50 mg改性后的分子筛进行苯吸附性能测试。
实施例3
(1)配制50ml 0.2mol/L的硝酸铈溶液；
(2)取1g 硅铝比为500的 ZSM-5分子筛，加入到硝酸铈溶液，并将混合物移至水热反应釜中，升温到120 ℃，反应6h；
(3)过滤分离出沉淀，干燥后在450 ℃下煅烧2h，得到金属阳离子掺杂改性分子筛；
(4)取50 mg改性后的分子筛进行苯吸附性能测试。
实施例4
(1)配制50ml 0.2mol/L的硝酸铈溶液；
(2)取1g 硅铝比为500的 ZSM-5分子筛，加入到硝酸铈溶液，并将混合物移至水热反应釜中，升温到80 ℃，反应6h；
(3)过滤分离出沉淀，干燥后在450 ℃下煅烧2h，得到金属阳离子掺杂改性分子筛；
(4)取50 mg改性后的分子筛进行苯吸附性能测试。
Claims (3)
1.一种掺杂改性ZSM-5分子筛强化吸附VOCs的方法与应用，其特征在于：(1)配制50 ml铜或铈或镧等金属离子的单一或混合盐溶液；(2)取1g ZSM-5分子筛加入到上述盐溶液，并移至水热反应釜中，升温到80-150 ℃，反应4-10 h；(3)待自然冷却至室温后过滤分离出分子筛固体，经干燥、煅烧后得到金属阳离子掺杂改性分子筛产品；(4)对改性后的分子筛进行典型VOCs吸附性能测试。
2.根据权利要求1所述的一种利用掺杂改性ZSM-5分子筛强化吸附VOCs的方法与应用，其特征在于所述步骤(1)中铜盐为醋酸铜、硫酸铜、硝酸铜或氯化铜中的一种或多种；所述的镧盐为硝酸镧、醋酸镧或氯化镧中的一种或多种；所述的铈盐为硝酸铈、醋酸铈、硫酸亚铈或氯化亚铈中的一种或多种；盐溶液浓度为0.025-0. 200 mol/L。
3.根据权利要求1所述的一种利用掺杂改性ZSM-5分子筛强化吸附VOCs的方法与应用，其特征在于所述步骤(3)中煅烧的升温速率为0.5-5 ℃/min，煅烧温度为450-600 ℃。
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