CN1054315C - 甲烷直接合成芳烃的双组分催化剂及其制备方法 - Google Patents
甲烷直接合成芳烃的双组分催化剂及其制备方法 Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 48
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims description 5
- 230000002194 synthesizing effect Effects 0.000 title abstract 2
- 239000004215 Carbon black (E152) Substances 0.000 title 1
- 229930195733 hydrocarbon Natural products 0.000 title 1
- 150000002430 hydrocarbons Chemical class 0.000 title 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000010457 zeolite Substances 0.000 claims abstract description 5
- 238000007654 immersion Methods 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 7
- 239000011609 ammonium molybdate Substances 0.000 claims description 7
- 229940010552 ammonium molybdate Drugs 0.000 claims description 7
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 7
- 238000005498 polishing Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 8
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract 5
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 abstract 2
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 abstract 2
- 238000000227 grinding Methods 0.000 abstract 1
- 239000011701 zinc Substances 0.000 description 9
- 239000010949 copper Substances 0.000 description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 230000009257 reactivity Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000001802 infusion Methods 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910019614 (NH4)6 Mo7 O24.4H2 O Inorganic materials 0.000 description 1
- 229910017315 Mo—Cu Inorganic materials 0.000 description 1
- 229910017318 Mo—Ni Inorganic materials 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- AIYYMMQIMJOTBM-UHFFFAOYSA-L nickel(ii) acetate Chemical compound [Ni+2].CC([O-])=O.CC([O-])=O AIYYMMQIMJOTBM-UHFFFAOYSA-L 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
一种甲烷直接合成芳烃的催化剂，其特征在于用MoO3为第一改性物质，ZnO、WO3、CuO、Cr2O3、NiO的其中一种为第二改性物质，改性HZSM-5沸石，组分含量为Mo6+含量为3-6%，第二组分与第一组分Mn+/Mo6+摩尔比为0.01-0.11，余量为HZSM-5。
本发明的催化剂采用浸渍法或固态研磨法制备，制备工艺简单，与单组分催化剂相比，提高了甲烷转化率。
Description
本发明涉及甲烷直接合成芳烃的技术，具体涉及一种甲烷在无氧条件下转化成芳烃甲烷直接合成芳烃的双组分催化剂及催化剂的制备方法。
中国专利93115889.3公开了一种甲烷直接合成芳烃的催化剂，该催化剂为MoO3改性的HZSM-5沸石，用该催化剂在连续进料的固定床式反应器上，甲烷转化率达到7-7.5％。由于是单组分，甲烷转化率需要进一步提高，以满足工业化生产的需要。
本发明目的是在上述Mo(VI)/HZSM-5催化剂的基础上，改进活性组分，得到进一步提高甲烷转化率的甲烷直接合成芳烃的双组分催化剂及其制备方法。
本发明提供的甲烷直接合成芳烃的双组分催化剂，采用双组分改性HZSM-5沸石，以MoO3为第一改性物质，分别以ZnO、WO3、CuO、Cr2O3、NiO为第二改性物质，HZSM-5的SiO2/Al2O3比为50-70，本发明催化剂组分含量为(重量百分比)，第一活性组分Mo6+含量3-6％，第二活性组分Mn+与第一活性组分Mo6+之摩尔比为0.01-0.11，余量为HZSM-5沸石。
本发明的双组分催化剂组分含量以Mo6+含量3.3-4％为佳，Mn+的含量与Mo6+之摩尔比以Zn/Mo0.02-0.06为佳，Cu/Mo0.02-0.06为佳，W/Mo0.04-0.06为佳，Cr/Mo0.02-0.08为佳，Ni/Mo0.03-0.08为佳。
本发明的双组分催化剂采用浸渍法或固态研磨法制备。浸渍法制备过程为：按上述双组分含量和双组分摩尔比的钼酸铵和硝酸盐或乙酸盐的混合溶液浸渍HZSM-5载体，室温干燥后393K烘4小时，再于723K焙烧4小时，即得到不同Mn+、Mo6+含量的双组分甲烷直接合成芳烃的浸渍法催化剂。固态研磨法制备过程为：按上述双组分含量和双组分摩尔比的钼酸铵和硝酸盐或乙酸盐的混合溶液混和HZSM-5载体，研磨，于723K焙烧4小时，即得到不同Mn+、Mo6+含量的双组分甲烷直接合成芳烃的研磨法催化剂。
本发明的双组分催化剂在973K反应温度，1200ml/g.hr的空速下，甲烷转化率达到9-13％，更适合于工业化生产。采用浸渍法和固态研磨法制备催化剂工艺简单，操作方便。
以下通过实施例对本发明作详细的描述。实施例1、浸渍法制备本发明的双组分催化剂。
原料：钼酸铵 (NH4)6Mo7O24.4H2O
铵型ZSM-5载体 SiO2/Al2O3＝50-70
钨酸铵 (NH4)5H5(H2(WO4)6).H2O
乙酸锌 Zn(CH3COO)2.2H2O
乙酸铜 Cu(CH3COO)2.H2O
硝酸铬 Cr(NO3)3.9H2O
乙酸镍 Ni(CH3COO)2.4H2O
将上述铵型载体于813K马福炉中空气氛下焙烧3小时，即成HZSM-5载体，取不同比例的钼酸铵和含W、Cu、Zn、Cr、Ni的原料中的一种，加一定量的水成混合溶液，浸渍一定量的HZSM-5载体。Mo含量3-6％，Mn+/Mo6+之摩尔比为0.01-0.11(Mn+为W、Cu、Zn、Cr、Ni离子中的一种)，其它为HZSM-5载体，室温干燥后393K烘4小时，再于723K焙烧4小时，即成本发明的双组分催化剂。实施例2、固态研磨法制备本发明的双组分催化剂
参照实施例1中的原料和含量，将不同比例的钼酸铵和含W、Cu、Zn、Cr、Ni的原料中的一种与一定量的HZSM-5载体研磨，于723K焙烧4小时，即得到不同含钼量和Mn+/Mo6+摩尔比的双组分催化剂。实施例3、固态研磨法制备不同Cu/Mo摩尔比的Mo-Cu/HZSM-5双组分催化剂催化反应实验。在连续进料的固定床反应器中进行反应，反应温度为973K，空速1200ml/g.hr，结果见表1。
表1、不同Cu/Mo比催化剂的反应性能催化剂 CH4 选择性(％)(Cu/Mo摩尔比) 转化率(％) C6H6 CH3-C6H5 C2H4 C2H60.01 12.97 91.51 6.01 1.65 0.830.03 13.15 91.78 5.84 1.63 0.750.05 13.33 93.71 4.27 1.32 0.710.07 12.71 91.90 5.40 1.95 0.750.09 12.26 91.13 6.10 1.88 0.890.11 11.90 90.15 6.61 2.28 0.97实施例4、浸渍法制备不同Zn/Mo摩尔比的Mo-Zn/HZSM-5双组分催化剂催化反应实验。反应在实施例3的条件下进行，结果见表2 。
表2、不同Zn/Mo比催化剂的反应性能催化剂 CH4 选择性(％)(Zn/Mo摩尔比) 转化率(％) C6H6 CH3-C6H5 C2H4 C2H60.01 10.25 90.88 5.90 2.22 1.000.03 10.91 90.01 6.73 2.25 1.010.05 10.49 87.33 9.31 2.37 0.990.07 10.31 89.94 6.57 2.42 1.070.09 10.25 89.17 5.87 2.15 2.810.11 10.00 89.61 5.68 2.61 2.10实施例5、浸渍法制备不同W/Mo摩尔比的Mo-W/HZSM-5双组分催化剂催化反应实验。反应在实施例3的条件下进行，结果见表3。
表3、不同W/Mo比催化剂的反应性能催化剂 CH4 选择性(％)(W/Mo摩尔比) 转化率(％) C6H6 CH3-C6H5 C2H4 C2H60.01 9.28 90.65 5.82 2.43 1.100.03 9.45 90.19 6.15 2.60 1.060.05 10.23 89.80 6.47 2.61 1.120.07 9.60 90.07 6.17 2.64 1.120.09 9.40 89.82 6.16 2.81 1.210.11 8.95 88.10 6.57 3.95 1.38实施例6、浸渍法制备不同Cr/Mo摩尔比的Mo-Cr/HZSM-5双组分催化剂催化反应实验。反应在实施例3的条件下进行，结果见表4。
表4、不同Cr/Mo比催化剂的反应性能催化剂 CH4 选择性(％)(Cr/Mo摩尔比) 转化率(％) C6H6 CH3-C6H5 C2H4 C2H60.01 9.20 90.64 5.96 2.27 1.130.03 10.68 91.54 5.85 1.77 0.840.05 11.18 91.75 5.40 1.93 0.920.07 11.64 91.15 6.04 1.91 0.900.09 9.80 90.91 5.87 2.10 1.120.11 9.42 90.69 5.46 2.62 1.23实施例7、浸渍法制备不同Ni/Mo摩尔比的Mo-Ni/HZSM-5双组分催化剂催化反应实验。反应在实施例3的条件下进行，结果见表5。
表5、不同Ni/Mo比催化剂的反应性能催化剂 CH4 选择性(％)(Ni/Mo摩尔比) 转化率(％) C6H6 CH3-C6H5 C2H4 C2H60.01 8.74 89.67 7.18 1.99 1.160.03 9.75 91.54 5.53 1.92 1.010.05 11.29 91.48 5.65 1.93 0.940.07 10.92 92.55 5.70 1.83 0.920.09 9.56 91.90 5.42 1.71 0.970.11 8.40 92.54 4.28 2.14 1.04
Claims (8)
1、一种甲烷直接合成芳烃的双组分催化剂，其特征在于：用双组分改性HZSM-5沸石，以MoO3为第一改性物质，分别以ZnO、WO3、CuO、Cr2O3或NiO为第二改性物质，HZSM-5的SiO2/Al2O3比为50-70，其组分含量为(重量百分比)：第一组分Mo6+含量3-6％，第二组分Mn+/Mo6+之摩尔比为0.01-0.11，余量为HZSM-5，Mn+为Zn2+、W6+、Cu2+、Cr3+或Ni2+。
2、根据权利要求1所述的双组分催化剂，其特征是所述第二组分Zn2+与第一组分Mo6+含量的摩尔比为Zn2+/Mo6+＝0.02-0.06。
3、根据权利要求1所述的双组分催化剂，其特征是所述第二组分Cu2+与第一组分Mo6+含量的摩尔比为Cu2+/Mo6+＝0.02-0.06。
4、根据权利要求1所述的双组分催化剂，其特征是所述第二组分W6+与第一组分Mo6+含量的摩尔比为W6+/Mo6+＝0.04-0.06。
5、根据权利要求1所述的双组分催化剂，其特征是所述第二组分Cr3+与第一组分Mo6+含量的摩尔比为Cr3+/Mo6+＝0.02-0.08。
6、根据权利要求1所述的双组分催化剂，其特征是所述第二组分Ni2+与第一组分Mo6+含量的摩尔比为Ni2+/Mo6+＝0.03-0.08。
7、权利要求1所述的双组分催化剂制备方法，其特征是采用浸渍法制备，制备过程为：按权利要求1，2，3，4，5或6所述Mo6+含量和双组分Mn+与Mo6+的摩尔比，将钼酸铵和硝酸盐或乙酸盐的混合溶液浸渍HZSM-5载体，室温干燥后393K烘干4小时，再于723K焙烧4小时。
8、权利要求1所述的双组分催化剂制备方法，其特征是采用固态研磨法制备，制备过程为：按权利要求1，2，3，4，5或6所述Mo6+含量和双组分Mn+与Mo6+的摩尔比，将钼酸铵和硝酸盐或乙酸盐混和HZSM-5载体，研磨，于723K焙烧4小时，
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| CN1327961C (zh) * | 2004-06-02 | 2007-07-25 | 华东师范大学 | 一种负载型催化剂及其制备和应用 |
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| CN1293940C (zh) * | 2003-06-10 | 2007-01-10 | 太原理工大学 | 负载型氮氧化物净化催化剂及制备 |
| RU2514915C2 (ru) * | 2008-02-21 | 2014-05-10 | Эксонмобил Кемикэл Пейтентс Инк. | Получение ароматических соединений из метана |
| CN107626343A (zh) * | 2017-09-25 | 2018-01-26 | 华东理工大学 | 一种合成气一步法制备轻质芳烃的催化剂及其制备方法与应用 |
| CN108212204B (zh) * | 2018-03-23 | 2021-02-09 | 安徽理工大学 | 一种微波辅助甲烷直接制备高碳烯烃的催化剂及催化工艺 |
| CN111420700B (zh) * | 2020-04-13 | 2023-10-27 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | 一种铜掺杂复合催化剂及其制备方法和应用 |
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| US4808763A (en) * | 1987-08-05 | 1989-02-28 | Amoco Corporation | Process for upgrading light paraffins |
| US5026937A (en) * | 1989-12-29 | 1991-06-25 | Uop | Aromatization of methane using zeolite incorporated in a phosphorus-containing alumina |
| CN1102359A (zh) * | 1993-11-04 | 1995-05-10 | 中科院大连化学物理研究所 | 甲烷直接合成芳烃的催化剂及其在合成反应中的应用 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1327961C (zh) * | 2004-06-02 | 2007-07-25 | 华东师范大学 | 一种负载型催化剂及其制备和应用 |
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| CN1168815A (zh) | 1997-12-31 |
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