CN114073961A - 具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法 - Google Patents
具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 30
- 239000010949 copper Substances 0.000 claims abstract description 32
- 239000000243 solution Substances 0.000 claims abstract description 26
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 17
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001354 calcination Methods 0.000 claims abstract description 17
- 239000011651 chromium Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 17
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000047 product Substances 0.000 claims abstract description 16
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 150000001879 copper Chemical class 0.000 claims abstract description 9
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 8
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 8
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- ZZBBCSFCMKWYQR-UHFFFAOYSA-N copper;dioxido(oxo)silane Chemical compound [Cu+2].[O-][Si]([O-])=O ZZBBCSFCMKWYQR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
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- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims description 10
- 229910001431 copper ion Inorganic materials 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 7
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- PMJNEQWWZRSFCE-UHFFFAOYSA-N 3-ethoxy-3-oxo-2-(thiophen-2-ylmethyl)propanoic acid Chemical compound CCOC(=O)C(C(O)=O)CC1=CC=CS1 PMJNEQWWZRSFCE-UHFFFAOYSA-N 0.000 claims description 3
- JOSWYUNQBRPBDN-UHFFFAOYSA-P ammonium dichromate Chemical compound [NH4+].[NH4+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O JOSWYUNQBRPBDN-UHFFFAOYSA-P 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 claims description 3
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 1
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- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 238000001833 catalytic reforming Methods 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
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- 239000011148 porous material Substances 0.000 description 1
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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Abstract
本发明属催化剂制备领域,尤其涉及一种具有脱砷性能的Cr‑Cu/SiO2催化剂的制备方法,具体步骤包括:(1)在铜盐水溶液中加入氨水,形成铜氨络合物;(2)在所得产物中加入硅溶胶溶液,经室温搅拌、水浴加热及抽滤干燥后得到沉淀物硅酸铜前驱体;(3)将所得产物在马弗炉中煅烧,得到Cu/SiO2多孔载体;(4)将所得产物浸渍在含金属铬溶液中,经干燥、煅烧后即得目的产物。本发明可得到具有较大比表面积和良好Cr负载量的Cr‑Cu/SiO2催化剂复合材料,有利于脱砷率的提高。
Description
技术领域
本发明属催化剂制备领域,尤其涉及一种具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法。
背景技术
在石油中广泛存在着砷元素,随着当前石油开采力度的加大,原油逐渐趋于劣质化,砷含量也呈现逐渐增多的趋势。砷在石油中一般与烃基形成有机化合物,在原油的后续加工过程中,砷化物会在裂解、加氢及催化重整的工艺步骤中产生有毒有害物质,不仅会影响生产过程中催化剂的活性,导致催化剂的失活从而影响装置的稳定性和生产周期,还对人体健康产生重大威胁。因此原油加工程序中砷元素的脱除成为了不可忽视的重要一环。
传统的脱砷催化剂主要利用的原理是物理吸附,但是存在砷容小,选择性差,稳定性差等问题。如果以多孔材料作为基本载体,并在基体中搭配上不同的活性组分,同时结合物理吸附和化学吸附,就能够在脱砷的过程中增强催化剂对于砷化物的选择针对性。
中国专利文件CN111036220A公开了一种脱砷剂的制备方法,该方法分别在铜盐、锌盐、铝盐和镁盐中加入沉淀剂,通过共沉淀法制备出活性组分和载体,再将二者混合、成型、焙烧得到最终的脱砷剂。但该方法的制备工艺复杂,生产周期较长,不适合工业化生产,并且仅体现了产品砷容的大小,脱砷率未见报道。因此,开发脱砷能力强、制备工艺简单、生产周期短的催化剂材料,成为本领域研究的热点问题。
发明内容
本发明旨在克服现有技术的不足之处而提供一种生产成本低、工艺流程简单,目的产物活性高、氧化还原性能好、脱砷性能强,具有较大比表面积和良好Cr负载量的具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法。
为解决上述技术问题,本发明是这样实现的:
一种具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,包括如下步骤:
(1)在铜盐水溶液中加入氨水,形成铜氨络合物;
(2)在步骤(1)所得产物中加入硅溶胶溶液,经室温搅拌、水浴加热及抽滤干燥后得到沉淀物硅酸铜前驱体;
(3)将步骤(2)所得产物在马弗炉中煅烧,得到Cu/SiO2多孔载体;
(4)将步骤(3)所得产物浸渍在金属铬溶液中,经干燥、煅烧后即得目的产物。
作为一种优选方案,本发明步骤(1)中,所述铜盐为硝酸铜、醋酸铜或硫酸铜中的一种或两种以上的混合物。
进一步地,本发明所述铜盐为硝酸铜。
进一步地,本发明步骤(1)中,所述氨水与铜离子的摩尔比为4 ~ 12:1。
进一步地,本发明所述氨水和铜离子的摩尔比为8:1。
进一步地,本发明步骤(2)中,所述硅溶胶与铜离子的摩尔比为1 ~ 4:1。
进一步地,本发明所述硅溶胶与铜离子的摩尔比为2:1。
进一步地,本发明步骤(3)中,所述煅烧温度为375℃,煅烧时间为2小时。
进一步地,本发明步骤(4)中,含金属铬溶液为铬酸纳、铬酸钾、重铬酸钾、铬酸铵、重铬酸铵溶液中的一种或两种以上的混合物;金属铬占含金属铬溶液的体积比为5 ~ 15vol.%;含金属铬溶液与步骤(3)所得Cu/SiO2多孔载体的质量比为2 ~ 4:1。
进一步地,本发明步骤(4)中,煅烧温度为375℃,煅烧时间为1小时。
与现有技术相比,本发明的有益效果:
本发明生产成本低、工艺流程简单,目的产物活性高、氧化还原性能好,脱砷性能强,通过采用浸渍-煅烧的方法,首先将Cu/SiO2设计成具有多孔结构的基体,不仅能够有效降低材料的密度,还可以增加负载金属铬离子和吸附砷元素的比表面积,从而提高材料的砷吸附能力,得到脱砷性能优异的Cr-Cu/SiO2催化剂复合材料。
附图说明
图1 为本发明实施例1所得Cr-Cu/SiO2催化剂的TEM图。
具体实施方式
下面结合实施例对本发明的技术方案做进一步说明,但本发明所保护范围不限于此。实施例中所用原料均为常规原料,所用设备均为常规设备,市购产品。表1为实施例1所得Cr-Cu/SiO2催化剂的性能数据表。
实施例1
一种具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,包括如下步骤:
(1)称取一定量硝酸铜加入去离子水400ml,室温搅拌至完全溶解;
(2)按照氨水和铜离子摩尔比为8的比例,加入氨水,形成铜氨络合物;
(3)按照硅溶胶和铜离子的摩尔比为2的比例,加入硅溶胶溶液,室温搅拌并且经过水浴加热蒸出氨气,抽滤并干燥后得到沉淀物硅酸铜前驱体;
(4)将步骤(3)中得到的沉淀物硅酸铜前驱体在马弗炉中经375℃煅烧2小时,得到Cu/SiO2多孔载体;
(5)按照金属铬所占含金属铬溶液的体积比为10 vol.%,且含金属铬溶液与Cu/SiO2多孔载体的质量比为3的比例,配制一定质量的重铬酸钾溶液,并将Cu/SiO2多孔载体浸渍在溶液中;
(6)将步骤(5)中浸渍后的Cu/SiO2多孔载体进行干燥,并在马弗炉中以375℃煅烧1小时,得到具有脱砷性能的Cr-Cu/SiO2催化剂。表1为实施例1所得Cr-Cu/SiO2催化剂的性能数据表。
表1
实施例2
其它内容同实施例1,不同的是:
步骤(5)中所配溶液为铬酸纳与铬酸钾的混合溶液,且铬所占溶液的体积比为15vol.%,溶液与载体的质量比为4。
实施例3:
如实施例1所述,不同的是:
步骤(5)中所配溶液为铬酸铵与重铬酸铵的混合溶液,且铬所占溶液的体积比为8vol.%,溶液与载体的质量比为2.5。
实施例4:
其它内容同实施例1,不同的是:步骤(1)中铜盐为硝酸铜与硫酸铜的混合物。
需要说明的是,以上列举的仅是本发明的若干个具体实施例,显然本发明不仅仅限于以上实施例,还可以有其他变形。本领域的技术人员从本发明公开内容直接导出或间接引申的所有变形,均应认为是本发明的保护范围。
Claims (10)
1.一种具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于,包括如下步骤:
(1)在铜盐水溶液中加入氨水,形成铜氨络合物;
(2)在步骤(1)所得产物中加入硅溶胶溶液,经室温搅拌、水浴加热及抽滤干燥后得到沉淀物硅酸铜前驱体;
(3)将步骤(2)所得产物在马弗炉中煅烧,得到Cu/SiO2多孔载体;
(4)将步骤(3)所得产物浸渍在含金属铬溶液中,经干燥、煅烧后即得目的产物。
2.根据权利要求1所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:步骤(1)中,所述铜盐为硝酸铜、醋酸铜或硫酸铜中的一种或两种以上的混合物。
3.根据权利要求2所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:所述铜盐为硝酸铜。
4.根据权利要求3所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:步骤(1)中,所述氨水与铜离子的摩尔比为4 ~ 12:1。
5.根据权利要求4所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:所述氨水和铜离子的摩尔比为8:1。
6.根据权利要求5所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:步骤(2)中,所述硅溶胶与铜离子的摩尔比为1 ~ 4:1。
7.根据权利要求6所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:所述硅溶胶与铜离子的摩尔比为2:1。
8.根据权利要求7所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:步骤(3)中,所述煅烧温度为375℃,煅烧时间为2小时。
9.根据权利要求8所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:步骤(4)中,含金属铬溶液为铬酸纳、铬酸钾、重铬酸钾、铬酸铵、重铬酸铵溶液中的一种或两种以上的混合物;金属铬占含金属铬溶液的体积比为5 ~ 15 vol.%;含金属铬溶液与步骤(3)所得Cu/SiO2多孔载体的质量比为2 ~ 4:1。
10.根据权利要求9所述具有脱砷性能的Cr-Cu/SiO2催化剂的制备方法,其特征在于:步骤(4)中,煅烧温度为375℃,煅烧时间为1小时。
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