CN111644195A - 一种电催化降解肼类环境污染物同时产氢的催化剂的制备方法 - Google Patents
一种电催化降解肼类环境污染物同时产氢的催化剂的制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims description 26
- 238000002360 preparation method Methods 0.000 title claims description 13
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- 238000000034 method Methods 0.000 claims abstract description 6
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
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- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 4
- 229910003178 Mo2C Inorganic materials 0.000 claims description 4
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- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
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- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- -1 ammonium molybdate heptahydrate Chemical class 0.000 claims description 2
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims description 2
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- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- QIJNJJZPYXGIQM-UHFFFAOYSA-N 1lambda4,2lambda4-dimolybdacyclopropa-1,2,3-triene Chemical compound [Mo]=C=[Mo] QIJNJJZPYXGIQM-UHFFFAOYSA-N 0.000 claims 1
- 229910039444 MoC Inorganic materials 0.000 claims 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 6
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
- C02F2001/46133—Electrodes characterised by the material
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- C02F2001/46142—Catalytic coating
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
肼,又称联氨,是一种无色发烟的、具有腐蚀性和强还原性的无色油状液体。肼类污染物催化降解是环境催化化学领域的热点问题,电催化降解肼类污染物同时产生氢气对评价环境生态学具有重要的科学和实践意义。肼类有机污染物在水体中造成的污染,严重危害生态环境和人民生命安全。该电催化过程阴极用于产生氢气,阳极用于肼类有机污染物的电催化降解,不仅实现了肼的零污染降解,而且为构建资源节约型社会提供了新思路。
Description
技术领域
本发明涉及多种非金属掺杂一种催化剂的制备方法及应用领域,具体涉及一种制备N,P-Mo2C多孔纳米针催化剂的方法及其在电催化降解肼类环境污染物同时产氢的领域的应用。
背景技术
能源是人类发展的保障,是社会进步的重要支撑。当前社会的能源主要来源为煤、石油、页岩气等化石燃料,但是这些化石燃料面临储量下降、开采困难、不可再生等问题,同时还造成环境污染,威胁人类健康。氢能作为清洁、高效的可再生能源受到了科研工作者的关注。氢气燃烧产物是水,不仅零污染,而且其热量高,来源广,是最理想的传统化石燃料替代能源。电解水催化制氢被认为有效的产氢方法。
肼类污染物催化降解是环境催化化学领域的热点问题,电催化降解肼类污染物同时产生氢气对评价环境生态学具有重要的科学和实践意义。肼类有机污染物在水体中造成的污染,严重危害生态环境和人民生命安全。该电催化过程阴极用于产生氢气,阳极用于肼类有机污染物的电催化降解,不仅实现了肼的零污染降解,而且为构建资源节约型社会提供了新思路。
多功能催化剂的研发对于纳米材料、环境催化等领域具有重要意义。传统的单一催化剂面临着催化效率不高,催化效果不好等问题,因此发展高效的掺杂态催化剂对催化领域有着重要的指导意义。
发明内容
本发明的目的之一是一种N,P-Mo2C多孔纳米针催化剂的新型制备方法。
本发明的目的之二是将所合成的纳米针催化剂应用于电催化降解肼类有机污染物。
本发明的目的之三是将所合成的纳米针催化剂应用于电催化降解有机污染物同时产氢体系。
本发明的技术方案如下:
1.N,P-Mo2C多孔纳米针催化剂的制备:是将钼源试剂、0 ~ 50 g的植酸、和0 ~ 50 g的苯胺加入到100 mL的去离子水中,并加入1 M的盐酸0 ~ 50 mL,强力搅拌均匀,使溶液的pH控制在1.5 ~ 8.5 之间,得到催化剂的制备液;将上述得到的制备液温度控制在40 ~ 80℃之间,并强力搅拌3 ~ 10 h,然后将其离心分析,得到的固体产品用乙醇清洗,干燥后即可得到氮,磷-双掺杂的催化剂前驱体;将上述得到的氮,磷-双掺杂的催化剂前驱体在650~ 1200 ℃之间进行退火3 ~ 20 h,即可得到N,P-Mo2C多孔纳米针催化剂。
2. 该方案的N,P-Mo2C多孔纳米针催化剂尚属首次合成,巧妙运用植酸、苯胺和钼源试剂中的非金属元素,实现了较低温度下的前驱体掺杂,较传统的直接高温掺杂,节约了大量的能源,且达到了非常好的掺杂效果。
3. N,P-Mo2C多孔纳米针催化剂的制备方法中,钼源试剂为七水钼酸铵、钼酸铵、钼酸钠、硫代钼酸铵、氧化钼中一种或几种的组合,钼源试剂含量为0.01 ~ 100 mol。
4. 电催化降解肼类环境污染物过程同时产氢,采用三电极系统进行测试,在电化学工作站上进行电催化降解肼类环境污染物性能测试;将一定浓度的污染物液体加入到催化底液中,以涂有N,P-Mo2C多孔纳米针催化剂的玻碳电极为工作电极,以碳棒为对电极,以Ag/AgCl电极为参比电极,以0.1 ~ 10 mol/L的硫酸盐缓冲溶液为催化底液。
具体实施例方式
为了进一步了解本发明,下面结合实施例对本发明优选实施方案进行描述,这些描述只是为进一步说明本发明的特征和优点,而不是对本发明权利要求的限制。
实施例1
将钼源试剂、25 g的植酸、和0 ~ 50 g的苯胺加入到100 mL的去离子水中,并加入1 M的盐酸0 ~ 50 mL,强力搅拌均匀,使溶液的pH控制在5.5左右,得到催化剂的制备液。
实施例2
将得到的制备液温度控制在60 ℃,并强力搅拌3 h,然后将其离心分析,得到的固体产品用乙醇清洗,干燥后即可得到氮,磷-双掺杂的催化剂前驱体。
实施例3
将得到的氮,磷-双掺杂的催化剂前驱体在850 ℃进行退火10 h,即可得到N,P-Mo2C多孔纳米针催化剂。
实施例4
采用三电极系统进行测试,在电化学工作站上进行电催化降解肼类环境污染物性能测试;将一定浓度的污染物液体加入到催化底液中,以涂有N,P-Mo2C多孔纳米针催化剂的玻碳电极为工作电极,以碳棒为对电极,以Ag/AgCl电极为参比电极,以0.5 mol/L的硫酸盐缓冲溶液为催化底液。
Claims (3)
1.一种电催化降解肼类环境污染物同时产氢的催化剂的制备方法,所涉及的氮,磷-双掺杂碳化钼N,P-Mo2C多孔纳米针催化剂,其特征在于,制备步骤如下:
(1)将钼源试剂、0 ~ 50 g的植酸、和0 ~ 50 g的苯胺加入到100 mL的去离子水中,并加入1 M的盐酸0 ~ 50 mL,强力搅拌均匀,使溶液的pH控制在1.5 ~ 8.5 之间,得到催化剂的制备液;
(2)将上述得到的制备液温度控制在40 ~ 80 ℃之间,并强力搅拌3 ~ 10 h,然后将其离心分析,得到的固体产品用乙醇清洗,干燥后即可得到氮,磷-双掺杂的催化剂前驱体;
(3)将上述得到的氮,磷-双掺杂的催化剂前驱体在650 ~ 1200 ℃之间进行退火3 ~20 h,即可得到N,P-Mo2C多孔纳米针催化剂。
2.如权利要求1所述的N,P-Mo2C多孔纳米针催化剂的制备方法,其特征在于,所述步骤(1)中,钼源试剂为七水钼酸铵、钼酸铵、钼酸钠、硫代钼酸铵、氧化钼中一种或几种的组合,钼源试剂含量为0.01 ~ 100 mol。
3.一种电催化降解肼类环境污染物同时产氢的催化剂的制备方法,所述的电催化降解肼类环境污染物过程同时产氢,其特征在于,包含如下步骤:采用三电极系统进行测试,在电化学工作站上进行电催化降解肼类环境污染物性能测试;将一定浓度的污染物液体加入到催化底液中,以涂有N,P-Mo2C多孔纳米针催化剂的玻碳电极为工作电极,以碳棒为对电极,以Ag/AgCl电极为参比电极,以0.1 ~ 10 mol/L的硫酸盐缓冲溶液为催化底液。
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Cited By (3)
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CN113351219A (zh) * | 2021-07-15 | 2021-09-07 | 西南大学 | 一种纳米棒状FeV3O8制备方法及其光催化应用 |
CN113481517A (zh) * | 2021-08-12 | 2021-10-08 | 济南大学 | 一种降解环境污染物肼的双功能催化剂的制备方法 |
CN113750987A (zh) * | 2021-09-16 | 2021-12-07 | 南京信息工程大学 | 一种正交相MoO3电催化剂及其制备方法和应用 |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113351219A (zh) * | 2021-07-15 | 2021-09-07 | 西南大学 | 一种纳米棒状FeV3O8制备方法及其光催化应用 |
CN113481517A (zh) * | 2021-08-12 | 2021-10-08 | 济南大学 | 一种降解环境污染物肼的双功能催化剂的制备方法 |
CN113750987A (zh) * | 2021-09-16 | 2021-12-07 | 南京信息工程大学 | 一种正交相MoO3电催化剂及其制备方法和应用 |
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