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CN1344671A - Catalyst for reforming mathand and carbon dioxide to synthesize gas - Google Patents

Catalyst for reforming mathand and carbon dioxide to synthesize gas Download PDF

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CN1344671A
CN1344671A CN 01135912 CN01135912A CN1344671A CN 1344671 A CN1344671 A CN 1344671A CN 01135912 CN01135912 CN 01135912 CN 01135912 A CN01135912 A CN 01135912A CN 1344671 A CN1344671 A CN 1344671A
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catalyst
carbon dioxide
methane
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王晓来
�田宏
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明公开了一种甲烷和二氧化碳重整制合成气催化剂及其制备方法。甲烷和二氧化碳重整制合成气催化剂以SiO2或γ－Al2O3为载体,含Ni6%～13%重量,同时含MoO3或WO3,其含量为1.5%～3.5%重量。该催化剂采用浸渍法制备,具有活性高,抗烧结、积炭能力强等特点。本发明的催化剂在常压下、780℃,空速为8400ml·g－1·h－1,甲烷与二氧化碳比为1的条件下,甲烷和二氧化碳的转化率在20h的反应过程中始终保持在90%以上。The invention discloses a catalyst for producing synthesis gas by reforming methane and carbon dioxide and a preparation method thereof. The catalyst for reforming methane and carbon dioxide to produce synthesis gas uses SiO 2 or γ-Al 2 O 3 as a carrier, contains 6% to 13% by weight of Ni, and simultaneously contains MoO 3 or WO 3 at a content of 1.5% to 3.5% by weight. The catalyst is prepared by an impregnation method, and has the characteristics of high activity, anti-sintering and strong carbon deposition ability. The catalyst of the present invention is under the conditions of normal pressure, 780°C, space velocity of 8400ml·g -1 ·h -1 , and ratio of methane to carbon dioxide of 1, the conversion rate of methane and carbon dioxide is always kept at More than 90.

Description

甲烷和二氧化碳重整制合成气催化剂Catalyst for reforming methane and carbon dioxide to synthesis gas

本发明涉及一种甲烷和二氧化碳重整制合成气用催化剂及其制备方法。The invention relates to a catalyst for reforming methane and carbon dioxide to produce synthesis gas and a preparation method thereof.

甲烷和二氧化碳重整制合成气，不仅能催化活化丰富价廉的甲烷和二氧化碳制取富一氧化碳的合成气，还由于该反应的强吸热性在化学储能方面有着广阔的应用前景，使得该反应在有效利用天然气、减轻温室效应、减缓能源危机等方面都具有重要的现实意义。The reforming of methane and carbon dioxide to synthesis gas can not only catalyze and activate abundant and cheap methane and carbon dioxide to produce carbon monoxide-rich synthesis gas, but also has broad application prospects in chemical energy storage due to the strong endothermic nature of the reaction, making this Response has important practical significance in the effective use of natural gas, mitigation of greenhouse effect, and mitigation of energy crisis.

目前用于甲烷和二氧化碳重整制合成气的催化剂主要有Pt族贵金属催化剂和Fe系过渡金属催化剂。贵金属催化剂的优点是催化活性高，抗积炭性能强，不足之处是贵金属催化剂价格昂贵。负载型镍基催化剂具有良好的催化活性，但由于积炭、烧结以及与载体间的固相反应等缺点，导致催化剂活性很快下降。因此，改变廉价过渡金属Ni基催化剂的存在状态，提高其催化活性和稳定性，是目前这一领域急待解决的问题之一。At present, the catalysts used for the reforming of methane and carbon dioxide to produce synthesis gas mainly include Pt-group noble metal catalysts and Fe-based transition metal catalysts. The advantages of noble metal catalysts are high catalytic activity and strong anti-coking performance, but the disadvantage is that noble metal catalysts are expensive. Supported nickel-based catalysts have good catalytic activity, but due to the disadvantages of carbon deposition, sintering, and solid-state reaction with the support, the catalyst activity decreases rapidly. Therefore, changing the existence state of cheap transition metal Ni-based catalysts and improving their catalytic activity and stability is one of the urgent problems to be solved in this field.

本发明的目的是提供一种活性高且抗积炭、烧结能力强的甲烷和二氧化碳重整制合成气的催化剂及其制备方法。The object of the present invention is to provide a catalyst for reforming synthesis gas from methane and carbon dioxide with high activity, anti-coking and strong sintering ability and its preparation method.

本发明的催化剂载体为SiO2或γ-Al2O3，活性组分由6％～13％重量Ni，1.5％～3.5％重量MoO3或WO3组成。The catalyst carrier of the present invention is SiO 2 or γ-Al 2 O 3 , and the active component is composed of 6%-13% by weight of Ni and 1.5%-3.5% by weight of MoO 3 or WO 3 .

本发明的催化剂采用浸渍法制备，其特征在于先将Ni的盐类配成其氨络合物溶液，再加入用氨水促溶的Mo或W的盐溶液，配成的混合物作为浸渍液来浸渍载体。经100～120℃干燥后，再经500～800℃焙烧4-8小时，最后用氢气600～800℃下还原活化，制得催化剂。The catalyst of the present invention is prepared by an impregnation method, which is characterized in that the salt of Ni is prepared as its ammonia complex solution, and then the salt solution of Mo or W that is promoted with ammonia water is added, and the prepared mixture is impregnated as an impregnating solution. carrier. After drying at 100-120°C, calcining at 500-800°C for 4-8 hours, and finally reducing and activating with hydrogen at 600-800°C to obtain the catalyst.

本发明的催化剂所用镍相应的盐类为硝酸镍。所用的Mo或W盐分别是钼酸铵和钨酸铵。本催化剂所用载体为SiO2或γ-Al2O3。采用固定床为反应器，气时空速为8400ml·g-1·h-1，常压下反应，780℃下，甲烷和二氧化碳的转化率在20小时的反应过程中都保持在90％以上。The corresponding salt of nickel used in the catalyst of the present invention is nickel nitrate. The Mo or W salts used are ammonium molybdate and ammonium tungstate, respectively. The carrier used in the catalyst is SiO 2 or γ-Al 2 O 3 . A fixed bed is used as the reactor, the gas hourly space velocity is 8400ml·g -1 ·h -1 , and the reaction is carried out under normal pressure. At 780°C, the conversion rates of methane and carbon dioxide are maintained above 90% during the 20-hour reaction process.

实施例1：采用2.0gSiO2载体，其形状和尺寸为30～60目的颗粒。将0.8919g硝酸镍配成其氨络合物溶液，然后加入用氨水促溶的0.0602(NH4)6Mo7O24·4H2O，配成的混合物作为浸渍液浸渍载体。搅拌均匀，100～120℃下干燥2小时，再经600℃焙烧4-8小时，即得到成品催化剂。Embodiment 1: adopt 2.0g SiO 2 carrier, its shape and size are 30～60 mesh particles. 0.8919g of nickel nitrate is made into its ammonium complex solution, and then 0.0602(NH 4 ) 6 Mo 7 O 24 ·4H 2 O, which is promoted with ammonia water, is added, and the prepared mixture is used as the impregnating solution to impregnate the carrier. Stir evenly, dry at 100-120°C for 2 hours, and then roast at 600°C for 4-8 hours to obtain the finished catalyst.

取0.3g30～60目该催化剂置于φ6mm的石英管反应器中。通入1∶1的CH4和CO2反应气，其空速为8400ml·g-1·h-1，780℃常压下连续反应20h。反应结果列于表1。Take 0.3g of the 30-60 mesh catalyst and place it in a φ6mm quartz tube reactor. A 1:1 reaction gas of CH 4 and CO 2 was introduced with a space velocity of 8400 ml·g -1 ·h -1 , and the reaction was continued for 20 h at 780°C under normal pressure. The reaction results are listed in Table 1.

     表1.甲烷和二氧化碳的转化率和收率随反应时间的变化   时间(h)   XCH4(％)   XCO2(％)   YCO(％)   YH2(％)     0     95.5     95.9     95.7     95.4     2     96.0     97.0     96.5     95.5     4     96.2     97.2     96.7     95.7     6     96.1     96.9     96.5     95.7     8     96.5     97.4     96.9     96.0    10     96.2     96.6     96.3     95.9    12     95.5     96.4     95.9     95.0    14     95.5     96.3     95.9     95.1    16     95.7     96.3     96.0     95.4    18     96.5     96.5     96.5     96.5    20     96.2     96.6     96.4     96.0 Table 1. Conversion and yield of methane and carbon dioxide as a function of reaction time time (h) X CH4 (%) X CO2 (%) Y CO (%) Y H2 (%) 0 95.5 95.9 95.7 95.4 2 96.0 97.0 96.5 95.5 4 96.2 97.2 96.7 95.7 6 96.1 96.9 96.5 95.7 8 96.5 97.4 96.9 96.0 10 96.2 96.6 96.3 95.9 12 95.5 96.4 95.9 95.0 14 95.5 96.3 95.9 95.1 16 95.7 96.3 96.0 95.4 18 96.5 96.5 96.5 96.5 20 96.2 96.6 96.4 96.0

XCH4：CH4转化率 XCO2：CO2转化率  YCO：CO收率   YH2：H2收率X CH4 : CH4 conversion X CO2 : CO2 conversion Y CO : CO yield Y H2 : H2 yield

实施例2：采用2.0gSiO2载体，其形状和尺寸为30～60目的颗粒。将0.8919g硝酸镍配成其氨络合物溶液，然后加入用氨水促溶的0.0910g(NH4)5H5[H2(WO4)6]·4H2O，下面的步骤同实施例1。取0.3g30～60目该催化剂，采用实施例1的反应装置和反应条件。反应结果列于表2。Embodiment 2: adopt 2.0g SiO 2 carrier, its shape and size are 30～60 mesh particles. Make 0.8919g of nickel nitrate into its ammonium complex solution, then add 0.0910g of (NH 4 ) 5 H 5 [H 2 (WO 4 ) 6 ]·4H 2 O, which is solubilized with ammonia water, and the following steps are the same as in the examples 1. Get 0.3g of this catalyst of 30～60 meshes, adopt the reaction apparatus and reaction conditions of embodiment 1. The reaction results are listed in Table 2.

      表2.甲烷和二氧化碳的转化率和收率随反应时间的变化   时间(h)   XCH4(％)   XCO2(％)   YCO(％)   YH2(％)      0     89.7     91.6     90.6     88.7      2     89.4     92.0     90.7     88.0      4     92.1     93.8     92.9     91.3      6     92.3     94.5     93.4     91.2      8     92.1     94.2     93.2     91.0     10     92.4     94.5     93.4     91.4     12     92.5     94.5     93.5     91.5     14     92.5     94.0     93.2     91.7     16     92.9     94.3     93.6     92.2     18     93.2     93.6     93.4     92.9     20     92.8     94.4     93.6     92.6 Table 2. Conversion and yield of methane and carbon dioxide as a function of reaction time time (h) X CH4 (%) X CO2 (%) Y CO (%) Y H2 (%) 0 89.7 91.6 90.6 88.7 2 89.4 92.0 90.7 88.0 4 92.1 93.8 92.9 91.3 6 92.3 94.5 93.4 91.2 8 92.1 94.2 93.2 91.0 10 92.4 94.5 93.4 91.4 12 92.5 94.5 93.5 91.5 14 92.5 94.0 93.2 91.7 16 92.9 94.3 93.6 92.2 18 93.2 93.6 93.4 92.9 20 92.8 94.4 93.6 92.6

XCH4：CH4转化率  XCO2：CO2转化率  YCO：CO收率  YH2：H2收率X CH4 : CH4 conversion X CO2 : CO2 conversion Y CO : CO yield Y H2 : H2 yield

实施例3：采用2.0gγ-Al2O3载体，其形状和尺寸为30～60目的颗粒。下面的步骤同实施例1。Example 3: 2.0 g of γ-Al 2 O 3 carrier is used, the shape and size of which are 30-60 mesh particles. The following steps are the same as in Example 1.

取0.3g30～60目该催化剂，采用实施例1的反应装置和反应条件。反应结果列于表3。Get 0.3g of this catalyst of 30～60 meshes, adopt the reaction apparatus and reaction conditions of embodiment 1. The reaction results are listed in Table 3.

   表3甲烷和二氧化碳的转化率和收率随反应时间的变化   时间(h)   XCH4(％)   XCO2(％)   YCO(％)   YH2(％)      0     95.5     96.3     96.0     95.4      2     95.6     96.5     96.2     95.5      4     95.1     95.9     95.5     95.0      6     95.0     95.9     95.5     95.0      8     94.7     96.2     95.5     94.6     10     94.5     95.7     95.1     94.4     12     93.5     94.8     94.1     93.5 Table 3 The conversion and yield of methane and carbon dioxide as a function of reaction time time (h) X CH4 (%) X CO2 (%) Y CO (%) Y H2 (%) 0 95.5 96.3 96.0 95.4 2 95.6 96.5 96.2 95.5 4 95.1 95.9 95.5 95.0 6 95.0 95.9 95.5 95.0 8 94.7 96.2 95.5 94.6 10 94.5 95.7 95.1 94.4 12 93.5 94.8 94.1 93.5

  时间(h) Time (h)   XCH4(％)X CH4 (%)   XCO2(％)X CO2 (%)   YCO(％)Y CO (%)   YH2(％)Y H2 (%)     14 14     93.9 93.9     95.2 95.2     94.6 94.6     93.9 93.9     16 16     93.9 93.9     95.3 95.3     94.6 94.6     93.9 93.9     18 18     93.9 93.9     95.2 95.2     94.5 94.5     93.8 93.8     20 20     92.6 92.6     94.4 94.4     93.5 93.5     92.4 92.4

XCH4：CH4转化率  XCO2：CO2转化率  YCO：CO收率  YH2：H2收率X CH4 : CH4 conversion X CO2 : CO2 conversion Y CO : CO yield Y H2 : H2 yield

实施例4：采用2.0gγ-Al2O3载体，其形状和尺寸为30～60目的颗粒。下面的步骤同实施例2。Example 4: 2.0 g of γ-Al 2 O 3 carrier is used, the shape and size of which are 30-60 mesh particles. The following steps are the same as in Example 2.

取0.3g30～60目该催化剂，采用实施例1的反应装置和反应条件。反应结果列于表4。Get 0.3g of this catalyst of 30～60 meshes, adopt the reaction apparatus and reaction conditions of embodiment 1. The reaction results are listed in Table 4.

   表4.甲烷和二氧化碳的转化率和收率随反应时间的变化   时间(h)   XCH4(％)   XCO2(％)   YCO(％)   YH2(％)      0     91.6     92.0     90.5     90.0      2     91.6     92.1     91.5     90.2      4     91.7     92.3     91.6     90.0      6     91.5     92.0     91.4     90.6      8     91.7     92.4     91.5     90.3     10     91.7     92.3     91.2     90.1     12     91.7     92.3     91.5     90.5     14     90.4     90.9     90.3     90.1     16     90.4     91.0     90.4     90.2     18     90.3     91.2     90.5     90.3     20     90.1     90.9     90.7     90.0 XCH4：CH4转化率  XCO2：CO2转化率  YCO：CO收率  YH2：H2收率Table 4. Conversion and yield of methane and carbon dioxide as a function of reaction time time (h) X CH4 (%) X CO2 (%) Y CO (%) Y H2 (%) 0 91.6 92.0 90.5 90.0 2 91.6 92.1 91.5 90.2 4 91.7 92.3 91.6 90.0 6 91.5 92.0 91.4 90.6 8 91.7 92.4 91.5 90.3 10 91.7 92.3 91.2 90.1 12 91.7 92.3 91.5 90.5 14 90.4 90.9 90.3 90.1 16 90.4 91.0 90.4 90.2 18 90.3 91.2 90.5 90.3 20 90.1 90.9 90.7 90.0 X CH4 : CH4 conversion X CO2 : CO2 conversion Y CO : CO yield Y H2 : H2 yield

Claims (2)

1.一种甲烷和二氧化碳重整制合成气催化剂，其特征在于载体为SiO2或γ-Al2O3，活性组分由6％～13％重量Ni，1.5％～3.5％重量MoO3或WO3组成。1. A catalyst for reforming synthesis gas from methane and carbon dioxide, characterized in that the carrier is SiO 2 or γ-Al 2 O 3 , and the active components are 6% to 13% by weight Ni, 1.5% to 3.5% by weight MoO or WO 3 composition. 2.如权利要求1所述的催化剂的制备方法，采用浸渍法制备，其特征在于先将硝酸镍配成其氨络合物溶液，再加入用氨水促溶的钼酸铵或钨酸铵的盐溶液，配成的混合物作为浸渍液来浸渍载体；经100～120℃干燥后，再经500～800℃焙烧4-8小时，最后用氢气600～800℃下还原活化，制得催化剂。2. the preparation method of catalyzer as claimed in claim 1 adopts dipping method to prepare, it is characterized in that nickel nitrate is made into its ammonium complex solution earlier, then add the ammonium molybdate or ammonium tungstate with ammoniacal liquor promoting dissolution Saline solution, the prepared mixture is used as impregnating solution to impregnate the carrier; after drying at 100-120°C, calcining at 500-800°C for 4-8 hours, and finally reducing and activating with hydrogen at 600-800°C to obtain the catalyst.
CN 01135912 2001-10-17 2001-10-17 Catalyst for reforming mathand and carbon dioxide to synthesize gas Pending CN1344671A (en)

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CN102745648A (en) * 2011-04-22 2012-10-24 太原理工大学 Preparation method of catalyst for producing synthetic gas by methane and carbon dioxide reformation
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CN103055868A (en) * 2011-10-24 2013-04-24 中国石油化工股份有限公司 Nickel-based catalyst and preparation method thereof
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CN101347735B (en) * 2007-07-19 2013-02-06 中国石油化工股份有限公司 Methanation catalyst for removing trace amounts of oxycarbide
CN102745648A (en) * 2011-04-22 2012-10-24 太原理工大学 Preparation method of catalyst for producing synthetic gas by methane and carbon dioxide reformation
CN103055868A (en) * 2011-10-24 2013-04-24 中国石油化工股份有限公司 Nickel-based catalyst and preparation method thereof
CN103058138A (en) * 2011-10-24 2013-04-24 中国石油化工股份有限公司 Preparation method of synthesis gas
CN103058138B (en) * 2011-10-24 2014-12-10 中国石油化工股份有限公司 Preparation method of synthesis gas
WO2016011970A1 (en) * 2014-07-25 2016-01-28 苏州汉瀚储能科技有限公司 Use of tungsten-containing material
CN104971784A (en) * 2015-07-07 2015-10-14 厦门大学 Preparation method of supported metal catalysts
CN106944071B (en) * 2016-01-07 2019-07-12 中国石油化工股份有限公司 The preparation method of methane portion oxidation synthesis gas catalyst
CN106944071A (en) * 2016-01-07 2017-07-14 中国石油化工股份有限公司 The preparation method of methane portion oxidation synthesis gas catalyst
CN109718799A (en) * 2017-10-31 2019-05-07 中国石油化工股份有限公司 The method of loaded catalyst and its preparation method and application and methane dry reforming preparing synthetic gas
CN110980639A (en) * 2019-12-31 2020-04-10 湘潭大学 Method for directly producing hydrogen by methane conversion under microwave catalysis
CN110980639B (en) * 2019-12-31 2021-10-26 湘潭大学 Method for directly producing hydrogen by methane conversion under microwave catalysis
CN116322981A (en) * 2020-04-03 2023-06-23 巴西石油公司 Catalyst for production of hydrogen and/or synthesis gas, method for obtaining same and use in steam reforming process
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CN112275293B (en) * 2020-09-07 2024-03-15 昆明理工大学 Preparation method and reforming method of catalyst for low-carbon alkane reforming hydrogen production and application of catalyst
CN115999564A (en) * 2022-06-30 2023-04-25 湘潭大学 A Ni-Mo/SiO2 catalyst for catalyzing bio-oil hydrodeoxygenation to prepare hydrocarbon fuels
CN115999564B (en) * 2022-06-30 2024-10-18 湘潭大学 A Ni-Mo/SiO2 catalyst for catalyzing the hydrodeoxygenation of bio-oil to produce hydrocarbon fuel

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