金属丝网负载分子筛膜催化剂的制备、表征与裂解催化性能的研究
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摘要
随着航空航天技术的发展,对燃料提出了更高的要求。高密度碳氢燃料和吸热型碳氢燃料是当前燃料发展的两个主要方向。为了增强吸热型碳氢燃料的化学吸热能力、改善高密度碳氢燃料的点火燃烧性能,提出了燃料在进入燃烧室前预先在金属丝网负载分子筛膜作用下催化裂解的新概念,本文主要对金属丝网负载分子筛膜催化剂的制备、表征和催化性能进行了研究,并取得了一些研究成果：
(1)采用不含有机模板剂的反应体系,研究了亚微米Y分子筛的合成。研究结果表明,反应体系的n(Na2O)/n(SiO2)影响结晶产物Y分子筛的粒径。Y分子筛的粒径随n(Na2O)/n(SiO2)的增大先减小后增大。Y分子筛的硅铝比n(Si) /n(Al)随n(Na2O)/n(SiO2)的增大先减小后几乎不变,当n(Na2O)/n(SiO2)≥1.04时,产物的硅铝比约为2.0。硅源对Y分子筛粒径也有影响。以硅溶胶和固体纳米二氧化硅为硅源合成得到的Y分子筛粒径分布较均匀,平均粒径分别约为300nm和500nm；以硅酸钠为硅源合成的Y分子筛粒径呈二元分布,大颗粒的平均粒径约为1000nm,小颗粒的平均粒径在100nm左右。当反应液的n(SiO2)/n(Al2O3)由25减小为5时,得到了粒径在50-100nm左右的Y分子筛颗粒。微波加热可以提高反应速率,但是对于减小产物粒径没有明显的作用。
(2)优化并确定了适合于FAU分子筛结晶的澄清反应体系,并研究了该澄清体系用于制备FeCrAl合金丝网负载的FAU分子筛涂层(膜)的可行性。研究发现,载体表面预先涂覆晶种后有利于提高分子筛负载量、涂层的连续性和均匀性。反应液老化对FAU分子筛结晶及成膜均有影响。FAU分子筛涂层具有一定的裂解催化活性。在500℃时,正辛烷的热裂解转化率为4.4%,而在FAU分子筛涂层作用下,其初始裂解转化率为13.2%,但活性随TOS急剧变小
(3)通过稀土金属离子改性,得到的FAU分子筛膜具有更高的催化活性。离子交换的顺序对于所合成的膜的催化活性有很大的影响。铵型分子筛膜中的铵离子可以较容易被稀土金属离子交换下来,而氢型分子筛膜中氢离子很难被稀土金属离子交换。使用0.125 mol/L、0.25 mol/L和0.50 mol/L硝酸铈溶液交换的分子筛膜,催化裂解性能基本相同。Ce3+和La3+稀土金属离子对分子筛膜的催化性能影响基本一致。
(4)研究了JP-10在多种类型分子筛催化剂上的催化裂解。发现孔径大小对于JP-10的催化裂解有较大的影响。对于分子筛孔径大于JP-10分子的HY、HUSY以及Hβ三种氢型分子筛催化剂而言,气体产率较高；而对于分子筛孔径小于JP-10分子的HZSM-5分子筛而言,气体产率较低。
比较了HZSM-5、碱处理HZSM-5(HZSM-5-OH)和酸处理HZSM-5 (HZSM-5-H)三种催化剂对JP-10裂解反应的催化效果。研究发现,JP-10在三种催化剂作用下的裂解转化率分别为67.15%、75.86%和71.74%。气态裂解产物收率大小顺序为HZSM-5-H>HZSM-5>HZSM-5-OH,而液态裂解产物的收率大小刚好相反。在任一催化剂作用下,气态裂解产物的主要成分均为乙烯、丙烷、丙烯和异丁烷,这些组分的相对含量依催化剂的不同而不同,但基本遵循丙烯>乙烯>异丁烯>丙烷的顺序。相对于HZSM-5催化剂而言,JP-10在HZSM-5-OH催化剂上裂解时气体产物收率下降但液体产物收率增加；在HZSM-5-H催化剂上裂解时则刚好相反,气体产物收率增加但液体产物收率下降。
(5)采用水热合成法制备了不锈钢负载的ZSM-5分子筛涂层。考察了不锈钢载体表面处理对分子筛与载体之间结合力的影响。研究结果表明,与酸处理或洗涤剂清洗处理相比,高温热处理更加有利于提高分子筛与不锈钢载体之间的结合力,且热处理效果与温度有关,最佳处理温度为850℃,在该温度下处理5h后的载体,所得到的分子筛/不锈钢复合材料,不仅具有最大的分子筛表面覆盖率,而且在焙烧过程中分子筛几乎不脱落。热处理后的载体在反应液中进一步浸泡同样会影响分子筛的覆盖率及结合力,影响大小与载体热处理温度有关。
With the development of technology in Aero-Space field, high energy density fuels and endothermic hydrocarbon fuels are two main aims in fuels development. The new conception of zeolitic film supported on metallic mesh using as catalytic cracking catalysts has been submitted, in order to increase the heat-absorbing capacity of endothermic hydrocarbon fuels and improve ignition and combustion behaviors of high energy density fuels. For these reasons, preparation, characterization and catalytic properties for cracking of zeolitic film catalysts supported on metallic mesh have been researched by us in this thesis. The results which were got by us from our research are as below:
(1) Synthesis of submicron sized zeolite Y has been studied without the presence of organic templates. The size of zeolite NaY crystals is influenced by n(Na2O)/n(SiO2) of the synthesis mixture. The size of NaY zeolite crystals decreases initiallyand then increases with increasing n(Na2O)/n(SiO2). The n(Si)/n(Al) ratio of Y zeolite crystals decreases initially and then almost keeps constant with increasing n(Na2O)/n(SiO2). The n(Si)/n(Al) ratio of the Y crystals is about 2.0 at n(Na2O)/n(SiO2)≥1.04. Silica source is another factor influencing the particle size. The zeolite crystals which are synthesized from silica sol and nano silica have uniform size distribution, and the average sizes of the crystals are 300nm and 500nm, respectively. When sodium silicate is used as silica source, the particle size appears a dual mode distribution (big particles are about 1000nm while small particles are around 100nm). When n(SiO2)/n(Al2O3) of synthesis mixture is changed from 25 to 5, zeolite Y particles with the size of 50nm-100nm are obtained. Microwave heating can accelerate the formation rate of NaY crystals compared with conventional heating, but it has no influence on the particle size.
(2) Clear solutions were optimized for crystallization of FAU-type zeolite. The clear solution was also used for preparation of FAU-type zeolite coatings on the grids made of FeCrAl alloys. Crystal seeds are beneficial to produce continuous and uniform coatings on grids. Seeds can also increase the amount of the crystals on grids. The ageing of the synthesis mixture is considered as another important factor. The as-synthesized FAU coatings have catalytic activities with the initial conversion of about 13.2% for JP-10 cracking at 500℃, while the conversion of thermal cracking is 4.4%. Unfortunately, the catalytic activity decreases rapidly with time on stream.
(3) FAU coatings with higher catalytic activities are obtained by modification of rare earth ions. The order for ion exchange is important. NH4+ ions in zeolite can be replaced by Ce3+ ions easily, whereas it is very difficult to exchange H+ ions by Ce3+ ions. The concentration of the rare earth salt solution has little influence on the catalytic cracking of n-octane over FAU zeolite coatings. There is almost no difference in the catalytic activities between Ce3+ and La3+ ions-exchanged FAU coatings.
(4) Catalytic cracking of JP-10 has been investigated over many types of zeolite. Pore size of zeolite is an important factor influencing JP-10 cracking. The yield of gas products is higher over HY, HUSY and Hβcatalysts than that on HZSM-5. In order to improve the catalytic properties of HZSM-5, HZSM-5-OH and HZSM-5-H were prepared by treating HZSM-5 crystals in basic and acidic solutions, respectively. The average conversions of JP-10 cracking are 67.15%、75.86% and 71.74% for HZSM-5、HZSM-5-OH and HZSM-5-H catalysts, respectively. The gaseous cracking products for each catalyst are mainly consisted of ethylene, propane, propylene and iso-butane. Their yields depend on the catalyst preparation method. The magnitude of these four components of gas products follows propylene>ethylene>iso-butane >propane for each catalyst. The yield of gas products decreases over HZSM-5-OH catalyst while the yield of liquid products increases. The yield of gas products increases over HZSM-5-H catalyst while the yield of liquid products decreases.
(5) ZSM-5 coatings on stainless steel foils were synthesized by hydrothermal synthesis. The influence of support surface pretreatment was studied on the adhesion strength between zeolite crystals and stainless steel support. The results have shown that high-temperature pretreatment has more favorable effect on adhesion strength of zeolite coatings compared to acid treatment or cleansing with detergent, the degree of which depends on the temperature. ZSM-5 coatings with the highest coverage and the strongest adhesion strength were achieved on stainless steel support that was pretreated at 850℃for 5h. The immersion of high-temperature pretreated support in the synthesis solution also imposes influence on surface coverage and adhesion strength of zeolite coatings, the degree of which depends on pretreatment temperature.
(1)采用不含有机模板剂的反应体系,研究了亚微米Y分子筛的合成。研究结果表明,反应体系的n(Na2O)/n(SiO2)影响结晶产物Y分子筛的粒径。Y分子筛的粒径随n(Na2O)/n(SiO2)的增大先减小后增大。Y分子筛的硅铝比n(Si) /n(Al)随n(Na2O)/n(SiO2)的增大先减小后几乎不变,当n(Na2O)/n(SiO2)≥1.04时,产物的硅铝比约为2.0。硅源对Y分子筛粒径也有影响。以硅溶胶和固体纳米二氧化硅为硅源合成得到的Y分子筛粒径分布较均匀,平均粒径分别约为300nm和500nm；以硅酸钠为硅源合成的Y分子筛粒径呈二元分布,大颗粒的平均粒径约为1000nm,小颗粒的平均粒径在100nm左右。当反应液的n(SiO2)/n(Al2O3)由25减小为5时,得到了粒径在50-100nm左右的Y分子筛颗粒。微波加热可以提高反应速率,但是对于减小产物粒径没有明显的作用。
(2)优化并确定了适合于FAU分子筛结晶的澄清反应体系,并研究了该澄清体系用于制备FeCrAl合金丝网负载的FAU分子筛涂层(膜)的可行性。研究发现,载体表面预先涂覆晶种后有利于提高分子筛负载量、涂层的连续性和均匀性。反应液老化对FAU分子筛结晶及成膜均有影响。FAU分子筛涂层具有一定的裂解催化活性。在500℃时,正辛烷的热裂解转化率为4.4%,而在FAU分子筛涂层作用下,其初始裂解转化率为13.2%,但活性随TOS急剧变小
(3)通过稀土金属离子改性,得到的FAU分子筛膜具有更高的催化活性。离子交换的顺序对于所合成的膜的催化活性有很大的影响。铵型分子筛膜中的铵离子可以较容易被稀土金属离子交换下来,而氢型分子筛膜中氢离子很难被稀土金属离子交换。使用0.125 mol/L、0.25 mol/L和0.50 mol/L硝酸铈溶液交换的分子筛膜,催化裂解性能基本相同。Ce3+和La3+稀土金属离子对分子筛膜的催化性能影响基本一致。
(4)研究了JP-10在多种类型分子筛催化剂上的催化裂解。发现孔径大小对于JP-10的催化裂解有较大的影响。对于分子筛孔径大于JP-10分子的HY、HUSY以及Hβ三种氢型分子筛催化剂而言,气体产率较高；而对于分子筛孔径小于JP-10分子的HZSM-5分子筛而言,气体产率较低。
比较了HZSM-5、碱处理HZSM-5(HZSM-5-OH)和酸处理HZSM-5 (HZSM-5-H)三种催化剂对JP-10裂解反应的催化效果。研究发现,JP-10在三种催化剂作用下的裂解转化率分别为67.15%、75.86%和71.74%。气态裂解产物收率大小顺序为HZSM-5-H>HZSM-5>HZSM-5-OH,而液态裂解产物的收率大小刚好相反。在任一催化剂作用下,气态裂解产物的主要成分均为乙烯、丙烷、丙烯和异丁烷,这些组分的相对含量依催化剂的不同而不同,但基本遵循丙烯>乙烯>异丁烯>丙烷的顺序。相对于HZSM-5催化剂而言,JP-10在HZSM-5-OH催化剂上裂解时气体产物收率下降但液体产物收率增加；在HZSM-5-H催化剂上裂解时则刚好相反,气体产物收率增加但液体产物收率下降。
(5)采用水热合成法制备了不锈钢负载的ZSM-5分子筛涂层。考察了不锈钢载体表面处理对分子筛与载体之间结合力的影响。研究结果表明,与酸处理或洗涤剂清洗处理相比,高温热处理更加有利于提高分子筛与不锈钢载体之间的结合力,且热处理效果与温度有关,最佳处理温度为850℃,在该温度下处理5h后的载体,所得到的分子筛/不锈钢复合材料,不仅具有最大的分子筛表面覆盖率,而且在焙烧过程中分子筛几乎不脱落。热处理后的载体在反应液中进一步浸泡同样会影响分子筛的覆盖率及结合力,影响大小与载体热处理温度有关。
With the development of technology in Aero-Space field, high energy density fuels and endothermic hydrocarbon fuels are two main aims in fuels development. The new conception of zeolitic film supported on metallic mesh using as catalytic cracking catalysts has been submitted, in order to increase the heat-absorbing capacity of endothermic hydrocarbon fuels and improve ignition and combustion behaviors of high energy density fuels. For these reasons, preparation, characterization and catalytic properties for cracking of zeolitic film catalysts supported on metallic mesh have been researched by us in this thesis. The results which were got by us from our research are as below:
(1) Synthesis of submicron sized zeolite Y has been studied without the presence of organic templates. The size of zeolite NaY crystals is influenced by n(Na2O)/n(SiO2) of the synthesis mixture. The size of NaY zeolite crystals decreases initiallyand then increases with increasing n(Na2O)/n(SiO2). The n(Si)/n(Al) ratio of Y zeolite crystals decreases initially and then almost keeps constant with increasing n(Na2O)/n(SiO2). The n(Si)/n(Al) ratio of the Y crystals is about 2.0 at n(Na2O)/n(SiO2)≥1.04. Silica source is another factor influencing the particle size. The zeolite crystals which are synthesized from silica sol and nano silica have uniform size distribution, and the average sizes of the crystals are 300nm and 500nm, respectively. When sodium silicate is used as silica source, the particle size appears a dual mode distribution (big particles are about 1000nm while small particles are around 100nm). When n(SiO2)/n(Al2O3) of synthesis mixture is changed from 25 to 5, zeolite Y particles with the size of 50nm-100nm are obtained. Microwave heating can accelerate the formation rate of NaY crystals compared with conventional heating, but it has no influence on the particle size.
(2) Clear solutions were optimized for crystallization of FAU-type zeolite. The clear solution was also used for preparation of FAU-type zeolite coatings on the grids made of FeCrAl alloys. Crystal seeds are beneficial to produce continuous and uniform coatings on grids. Seeds can also increase the amount of the crystals on grids. The ageing of the synthesis mixture is considered as another important factor. The as-synthesized FAU coatings have catalytic activities with the initial conversion of about 13.2% for JP-10 cracking at 500℃, while the conversion of thermal cracking is 4.4%. Unfortunately, the catalytic activity decreases rapidly with time on stream.
(3) FAU coatings with higher catalytic activities are obtained by modification of rare earth ions. The order for ion exchange is important. NH4+ ions in zeolite can be replaced by Ce3+ ions easily, whereas it is very difficult to exchange H+ ions by Ce3+ ions. The concentration of the rare earth salt solution has little influence on the catalytic cracking of n-octane over FAU zeolite coatings. There is almost no difference in the catalytic activities between Ce3+ and La3+ ions-exchanged FAU coatings.
(4) Catalytic cracking of JP-10 has been investigated over many types of zeolite. Pore size of zeolite is an important factor influencing JP-10 cracking. The yield of gas products is higher over HY, HUSY and Hβcatalysts than that on HZSM-5. In order to improve the catalytic properties of HZSM-5, HZSM-5-OH and HZSM-5-H were prepared by treating HZSM-5 crystals in basic and acidic solutions, respectively. The average conversions of JP-10 cracking are 67.15%、75.86% and 71.74% for HZSM-5、HZSM-5-OH and HZSM-5-H catalysts, respectively. The gaseous cracking products for each catalyst are mainly consisted of ethylene, propane, propylene and iso-butane. Their yields depend on the catalyst preparation method. The magnitude of these four components of gas products follows propylene>ethylene>iso-butane >propane for each catalyst. The yield of gas products decreases over HZSM-5-OH catalyst while the yield of liquid products increases. The yield of gas products increases over HZSM-5-H catalyst while the yield of liquid products decreases.
(5) ZSM-5 coatings on stainless steel foils were synthesized by hydrothermal synthesis. The influence of support surface pretreatment was studied on the adhesion strength between zeolite crystals and stainless steel support. The results have shown that high-temperature pretreatment has more favorable effect on adhesion strength of zeolite coatings compared to acid treatment or cleansing with detergent, the degree of which depends on the temperature. ZSM-5 coatings with the highest coverage and the strongest adhesion strength were achieved on stainless steel support that was pretreated at 850℃for 5h. The immersion of high-temperature pretreated support in the synthesis solution also imposes influence on surface coverage and adhesion strength of zeolite coatings, the degree of which depends on pretreatment temperature.
引文
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