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CN107377008A - One kind carries palladium fiber base catalyst and its production and use - Google Patents

One kind carries palladium fiber base catalyst and its production and use Download PDF

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Publication number
CN107377008A
CN107377008A CN201710610999.5A CN201710610999A CN107377008A CN 107377008 A CN107377008 A CN 107377008A CN 201710610999 A CN201710610999 A CN 201710610999A CN 107377008 A CN107377008 A CN 107377008A
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palladium
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temperature
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贺泓
邓华
单文坡
李要彬
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Ningbo Urban Environment Observation And Research Station-Nueors Chinese Academy Of Sciences
Institute of Urban Environment of CAS
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Ningbo Urban Environment Observation And Research Station-Nueors Chinese Academy Of Sciences
Institute of Urban Environment of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/50Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/58Fabrics or filaments
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44Palladium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/60Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61Surface area
    • B01J35/61310-100 m2/g
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02Impregnation, coating or precipitation
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    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment
    • B01J37/082Decomposition and pyrolysis
    • B01J37/088Decomposition of a metal salt
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/16Reducing
    • B01J37/18Reducing with gases containing free hydrogen
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/34Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
    • B01J37/341Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
    • B01J37/343Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23GCREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F23G7/07Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material

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Abstract

本发明提供了一种载钯纤维基催化剂及其制备方法和用途。本发明的载钯纤维基催化剂,所述催化剂的载体为纤维,活性组分为负载在所述载体上的钯,以所述载体的质量为100%计,所述钯的质量为0.05~2%。本发明以纤维作为载体,利用纤维材料空隙率高、传质效率高等优点,以其为载体负载活性贵金属钯制备燃烧净化苯的载钯纤维基催化剂,可高效降解剧毒挥发性有机物苯,该催化剂具有空隙率高、传质效率高、成型容易、降解苯反应温度低等优点,具有较好的应用前景,广泛适用于冶炼厂、炼油厂、化工厂等固定源所排放废气中含苯的净化处理。

The invention provides a palladium-loaded fiber-based catalyst, a preparation method and application thereof. In the palladium-loaded fiber-based catalyst of the present invention, the carrier of the catalyst is fiber, the active component is palladium loaded on the carrier, and the mass of the palladium is 0.05 to 2% based on the mass of the carrier as 100%. %. In the present invention, the fiber is used as a carrier, and the advantages of high porosity and high mass transfer efficiency of the fiber material are utilized, and the active precious metal palladium is loaded on the fiber material to prepare a palladium-loaded fiber-based catalyst for burning and purifying benzene, which can efficiently degrade the highly toxic volatile organic compound benzene. The catalyst has the advantages of high porosity, high mass transfer efficiency, easy molding, and low reaction temperature for benzene degradation. Purification treatment.

Description

一种载钯纤维基催化剂及其制备方法和用途A kind of palladium-loaded fiber-based catalyst and its preparation method and application

技术领域technical field

本发明属于催化剂技术领域,涉及一种载钯纤维基催化剂及其制备方法和用途,尤其涉及一种用于挥发性有机物的催化燃烧的载钯纤维基催化剂及其制备方法,特别涉及一种用于苯的催化燃烧的载钯纤维基催化剂及其制备方法。The invention belongs to the technical field of catalysts, and relates to a palladium-loaded fiber-based catalyst and its preparation method and application, in particular to a palladium-loaded fiber-based catalyst for catalytic combustion of volatile organic compounds and a preparation method thereof, in particular to a Palladium-loaded fiber-based catalyst for catalytic combustion of benzene and its preparation method.

背景技术Background technique

随着人类工业活动的强度增加,大量的挥发性有机物(Volatile OrganicCompound,简称VOCs)排放到大气环境中,通过系列化学反应引发环境污染。例如,一些活性强的VOCs可以与另一种大气污染物氮氧化物(NOx)发生光化学反应,引起地表臭氧浓度升高,形成光化学烟雾污染;一些蒸汽压低的VOCs也可以经过复杂过程成核长大形成二次有机气溶胶,而二次有机气溶胶正是细颗粒物PM2.5的重要组成部分。可见VOCs是形成光化学污染和大气灰霾的重要前驱物质。除此之外,VOCs本身对人体健康也能构成巨大威胁。例如,常见的VOCs如甲醛、苯、甲苯等具有致癌、致畸的危害。因此,要去除光化学烟雾,降低颗粒物污染,提高城市空气质量,保护民众的身体健康,VOCs排放控制和去除势在必行。As the intensity of human industrial activities increases, a large amount of volatile organic compounds (Volatile Organic Compounds, VOCs for short) are discharged into the atmosphere, causing environmental pollution through a series of chemical reactions. For example, some highly active VOCs can react photochemically with another atmospheric pollutant, nitrogen oxides (NO x ), causing an increase in the concentration of surface ozone and forming photochemical smog pollution; some VOCs with low vapor pressure can also nucleate through complex processes It grows up to form secondary organic aerosol, and secondary organic aerosol is an important part of fine particulate matter PM2.5. It can be seen that VOCs are important precursors for the formation of photochemical pollution and atmospheric haze. In addition, VOCs themselves can pose a huge threat to human health. For example, common VOCs such as formaldehyde, benzene, toluene, etc. have carcinogenic and teratogenic hazards. Therefore, to remove photochemical smog, reduce particle pollution, improve urban air quality, and protect people's health, it is imperative to control and remove VOCs emissions.

VOCs的来源广泛,主要包括了石油、化工、医药、包装、印刷、涂装等,以涂装行业为例,其VOCs排放量将近700万吨/年,约占VOCs总排放量的1/3。在涂装行业VOCs消除净化领域,西方主要发达国家以及日本起步较早。在1955年美国就已颁布了《空气污染控制法》,对空气污染物排放类别和总量做了详细的规定,后来又颁布了《洁净空气法》,并于1970年和1990年做了两次修订;在1966年还专门为涂装行业的VOCs排放制定了专门性法规,即“66法规”。在法律的强制约束和企业利益的推动下,不同消除VOCs的技术被研发和使用。VOCs come from a wide range of sources, mainly including petroleum, chemical industry, medicine, packaging, printing, coating, etc. Taking the coating industry as an example, its VOCs emissions are nearly 7 million tons per year, accounting for about 1/3 of the total VOCs emissions . In the field of VOCs elimination and purification in the coating industry, major western developed countries and Japan started earlier. In 1955, the United States promulgated the "Air Pollution Control Act", which made detailed regulations on the types and total amount of air pollutant emissions. In 1966, special regulations were formulated specifically for VOCs emissions in the coating industry, namely "Regulation 66". Driven by legal constraints and corporate interests, different technologies for eliminating VOCs have been developed and used.

目前我国高度重视VOCs的污染问题,要求到2020年,基本实现VOCs从原料到产品、从生产到消费的全过程减排。因此,VOCs的减排技术得到了广泛的研究探索。At present, my country attaches great importance to the pollution of VOCs, and requires that by 2020, the whole process of VOCs emission reduction from raw materials to products, from production to consumption will be basically realized. Therefore, VOCs emission reduction technologies have been extensively researched and explored.

苯是挥发性有机物中毒性较大的一种,《民用建筑工程室内环境污染控制规范》GB50325-2001中对其浓度进行了严格限量,要求其低于0.09mg/m3。因此对排放源含苯的尾气进行处理十分必要。催化燃烧苯是目前较为高效的控制技术,但是,目前传统粉末催化剂存在成型困难和传质阻力大等缺点。Benzene is one of the most toxic volatile organic compounds. The "Code for Indoor Environmental Pollution Control of Civil Construction Engineering" GB50325-2001 strictly limits its concentration, requiring its concentration to be less than 0.09mg/m 3 . Therefore, it is very necessary to treat the tail gas containing benzene from the emission source. Catalytic combustion of benzene is a more efficient control technology at present, but the traditional powder catalysts have disadvantages such as difficult molding and large mass transfer resistance.

发明内容Contents of the invention

针对现有技术的不足,本发明的目的之一在于提供一种载钯纤维基催化剂,催化活性高、空隙率高、传质效率高、成型容易、降解苯反应温度低。In view of the deficiencies in the prior art, one of the objectives of the present invention is to provide a palladium-loaded fiber-based catalyst with high catalytic activity, high porosity, high mass transfer efficiency, easy molding, and low reaction temperature for benzene degradation.

为达此目的,本发明采用以下技术方案:For reaching this purpose, the present invention adopts following technical scheme:

一种载钯纤维基催化剂,所述催化剂的载体为纤维,活性组分为负载在所述载体上的钯,以所述载体的质量为100%计,所述钯的质量为0.05~2%。A palladium-loaded fiber-based catalyst, the carrier of the catalyst is fiber, the active component is palladium loaded on the carrier, and the mass of the palladium is 0.05-2% based on the mass of the carrier as 100% .

本发明以纤维作为载体,利用纤维材料空隙率高、传质效率高等优点,以其为载体负载活性贵金属钯制备燃烧净化苯的载钯纤维基催化剂,可高效降解剧毒挥发性有机物苯,该催化剂具有空隙率高、传质效率高、成型容易、降解苯反应温度低等优点,具有较好的应用前景。In the present invention, the fiber is used as a carrier, and the advantages of high porosity and high mass transfer efficiency of the fiber material are utilized, and the active precious metal palladium is loaded on the fiber material to prepare a palladium-loaded fiber-based catalyst for burning and purifying benzene, which can efficiently degrade the highly toxic volatile organic compound benzene. The catalyst has the advantages of high porosity, high mass transfer efficiency, easy molding, and low reaction temperature for benzene degradation, and has a good application prospect.

本发明所述的纤维为陶瓷纤维、玻璃纤维、金属纤维、活性炭纤维中的一种或至少两种的混合物;所述混合物典型但非限制的混合物为两种纤维的混合物,例如陶瓷纤维、玻璃纤维的混合物,陶瓷纤维、金属纤维的混合物,陶瓷纤维、活性炭纤维的混合物,玻璃纤维、金属纤维的混合物,玻璃纤维、活性炭纤维的混合物,金属纤维、活性炭纤维的混合物;所述混合物可以为三种纤维的混合物,例如陶瓷纤维、玻璃纤维、金属纤维的混合物,陶瓷纤维、玻璃纤维、活性炭纤维的混合物,玻璃纤维、金属纤维、活性炭纤维的混合物;所述混合物可以为四种纤维的混合物,例如陶瓷纤维、玻璃纤维、金属纤维、活性炭纤维的混合物。优选地,所述纤维为玻璃纤维和陶瓷纤维的混合物,所述玻璃纤维与所述陶瓷纤维的质量比为(7~9):(1~3),例如7:3、8:2、9:1,优选为8:2。The fiber described in the present invention is one or a mixture of at least two of ceramic fibers, glass fibers, metal fibers, and activated carbon fibers; a typical but non-limiting mixture of the mixture is a mixture of two fibers, such as ceramic fibers, glass A mixture of fibers, a mixture of ceramic fibers and metal fibers, a mixture of ceramic fibers and activated carbon fibers, a mixture of glass fibers and metal fibers, a mixture of glass fibers and activated carbon fibers, a mixture of metal fibers and activated carbon fibers; the mixture can be three A mixture of fibers, such as a mixture of ceramic fibers, glass fibers, metal fibers, a mixture of ceramic fibers, glass fibers, activated carbon fibers, a mixture of glass fibers, metal fibers, activated carbon fibers; the mixture can be a mixture of four fibers, For example, a mixture of ceramic fibers, glass fibers, metal fibers, activated carbon fibers. Preferably, the fibers are a mixture of glass fibers and ceramic fibers, and the mass ratio of the glass fibers to the ceramic fibers is (7-9):(1-3), such as 7:3, 8:2, 9 :1, preferably 8:2.

本发明中,以所述载体的质量为100%计,所述钯的质量为0.05~2%,例如所述钯的质量为0.05%、0.06%、0.07%、0.08%、0.09%、1%、1.1%、1.2%、1.3%、1.4%、1.5%、1.6%、1.7%、1.8%、1.9%、2%,优选地,以所述载体的质量为100%计,所述钯的质量为1%。In the present invention, based on the mass of the carrier as 100%, the mass of the palladium is 0.05-2%, for example, the mass of the palladium is 0.05%, 0.06%, 0.07%, 0.08%, 0.09%, 1%. , 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, 2%, preferably, based on the mass of the carrier being 100%, the mass of the palladium 1%.

本发明的目的之二在于提供一种如上所述的载钯纤维基催化剂的制备方法,该催化剂制备方法简单、制得的催化剂活性优良,具有较好的应用潜力,所述制备方法包括如下步骤:The second object of the present invention is to provide a method for preparing the palladium-supported fiber-based catalyst as described above. The preparation method of the catalyst is simple, the catalyst activity is excellent, and it has good application potential. The preparation method includes the following steps :

1)将载体纤维进行酸洗;1) pickling the carrier fiber;

2)将步骤1)酸洗后的载体纤维置于含钯溶液中浸渍,然后进行蒸发、烘干处理;2) impregnating the carrier fiber after pickling in step 1) in a solution containing palladium, then evaporating and drying;

3)将步骤2)烘干后的产物进行焙烧处理;3) roasting the dried product in step 2);

4)将步骤3)焙烧处理后的产物进行高温还原再处理,得到载钯纤维基催化剂。4) The product after the roasting treatment in step 3) is subjected to high-temperature reduction and retreatment to obtain a palladium-supported fiber-based catalyst.

载体纤维的表面比较光滑,本发明通过酸洗载体纤维,使纤维的表面经过酸洗后形成不饱和位点等表面缺陷,这些不饱和位点会结合更多的贵金属钯,使负载的钯不至于团聚在一起形成大颗粒,钯更均匀地负载于载体纤维上,从而提高催化剂的活性。本发明的步骤1)中,所述酸洗的过程为,将载体纤维浸于酸中,在真空滴滤瓶中逐滴抽滤淋洗液体。The surface of the carrier fiber is relatively smooth. The present invention makes the surface of the fiber form unsaturated sites and other surface defects after pickling by pickling the carrier fiber. These unsaturated sites will bind more precious metal palladium, so that the loaded palladium will As for the agglomeration together to form large particles, the palladium is more uniformly loaded on the support fibers, thereby improving the activity of the catalyst. In the step 1) of the present invention, the pickling process includes immersing the carrier fiber in acid, and suctioning and filtering the rinsing liquid drop by drop in a vacuum drip filter bottle.

优选地,所述酸的质量百分数为10~60%,例如10%、20%、30%、40%、50%、60%,优选为50%。Preferably, the mass percentage of the acid is 10-60%, such as 10%, 20%, 30%, 40%, 50%, 60%, preferably 50%.

优选地,所述酸为硫酸或硝酸,优选为硫酸。Preferably, the acid is sulfuric acid or nitric acid, preferably sulfuric acid.

优选地,所述载体纤维与所述酸的固液比为1/100~1/10g/mL,例如所述载体纤维与所述酸的固液比为1/100、1/90、1/80、1/70、1/60、1/50、1/40、1/30、1/20、1/10,优选为1/50g/mL。Preferably, the solid-to-liquid ratio of the carrier fiber to the acid is 1/100 to 1/10 g/mL, for example, the solid-to-liquid ratio of the carrier fiber to the acid is 1/100, 1/90, 1/10 80, 1/70, 1/60, 1/50, 1/40, 1/30, 1/20, 1/10, preferably 1/50 g/mL.

优选地,所述淋洗的时间为20~40min,例如淋洗的时间为20min、25min、30min、35min、40min,优选为30min,所述淋洗的次数为1~3次。Preferably, the rinsing time is 20-40 min, for example, 20 min, 25 min, 30 min, 35 min, 40 min, preferably 30 min, and the rinsing times are 1-3 times.

步骤1)中,经所述酸洗后的纤维进行去离子水冲洗,所述去离子水冲洗后的pH值为中性。In step 1), the acid-washed fiber is rinsed with deionized water, and the pH value of the rinsed deionized water is neutral.

优选地,所述去离子水冲洗后还包括干燥的步骤;Preferably, after the deionized water is rinsed, a drying step is also included;

优选地,所述干燥是在烘箱中进行的,所述干燥的温度为100~150℃,例如干燥的温度为100℃、110℃、120℃、130℃、140℃、150℃,优选为120℃。Preferably, the drying is carried out in an oven, the drying temperature is 100-150°C, for example, the drying temperature is 100°C, 110°C, 120°C, 130°C, 140°C, 150°C, preferably 120°C ℃.

优选地,所述干燥的时间为5~24h,例如5h、6h、7h、8h、9h、10h、11h、12h、13h、14h、15h、16h、17h、18h、19h、20h,优选为12h。Preferably, the drying time is 5-24 hours, such as 5 hours, 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, 17 hours, 18 hours, 19 hours, 20 hours, preferably 12 hours.

步骤2)中,所述含钯溶液为二水硝酸钯溶液、氯化钯溶液、乙酸钯溶液中的一种。In step 2), the palladium-containing solution is one of palladium nitrate dihydrate solution, palladium chloride solution and palladium acetate solution.

优选地,所述浸渍为超声辅助浸渍,所述超声辅助浸渍的具体过程为:将酸洗后的载体纤维置于含钯溶液中得到固液体系,将所述固液体系置于超声波池中进行超声辅助浸渍,所述超声辅助浸渍的温度为室温,优选为23~27℃,例如23℃、24℃、25℃、26℃、27℃;所述超声辅助浸渍的超声的频率为40~50kHz,例如超声的频率为40kHz、41kHz、42kHz、43kHz、44kHz、45kHz、46kHz、47kHz、48kHz、49kHz、50kHz,优选为44kHz,所述超声辅助浸渍的时间为10~60min,例如10min、20min、30min、40min、50min、60min,优选为30min。Preferably, the impregnation is ultrasonic-assisted impregnation, and the specific process of the ultrasonic-assisted impregnation is: placing the pickled carrier fiber in a palladium-containing solution to obtain a solid-liquid system, and placing the solid-liquid system in an ultrasonic pool Perform ultrasonic-assisted impregnation, the temperature of the ultrasonic-assisted impregnation is room temperature, preferably 23-27°C, such as 23°C, 24°C, 25°C, 26°C, 27°C; the ultrasonic frequency of the ultrasonic-assisted impregnation is 40-27°C. 50kHz, for example, the frequency of ultrasound is 40kHz, 41kHz, 42kHz, 43kHz, 44kHz, 45kHz, 46kHz, 47kHz, 48kHz, 49kHz, 50kHz, preferably 44kHz, and the time of ultrasonic-assisted impregnation is 10 to 60min, such as 10min, 20min, 30min, 40min, 50min, 60min, preferably 30min.

步骤2)中,所述蒸发处理是在旋转蒸发瓶中进行的,所述旋转蒸发的旋转频率为20~200r/min,例如旋转频率为20r/min、30r/min、40r/min、50r/min、60r/min、70r/min、80r/min、90r/min、100r/min、110r/min、120r/min、130r/min、140r/min、150r/min、160r/min、170r/min、180r/min、190r/min、200r/min,优选为60r/min,所述旋转蒸发的温度为50~70℃,例如旋转蒸发的温度为50℃、51℃、52℃、53℃、54℃、55℃、56℃、57℃、58℃、59℃、60℃、61℃、62℃、63℃、64℃、65℃、66℃、67℃、68℃、69℃、70℃,优选为60℃。In step 2), the evaporation treatment is carried out in a rotary evaporating flask, and the rotation frequency of the rotary evaporation is 20 to 200r/min, for example, the rotation frequency is 20r/min, 30r/min, 40r/min, 50r/min. min, 60r/min, 70r/min, 80r/min, 90r/min, 100r/min, 110r/min, 120r/min, 130r/min, 140r/min, 150r/min, 160r/min, 170r/min, 180r/min, 190r/min, 200r/min, preferably 60r/min, the temperature of the rotary evaporation is 50-70°C, for example, the temperature of the rotary evaporation is 50°C, 51°C, 52°C, 53°C, 54°C , 55°C, 56°C, 57°C, 58°C, 59°C, 60°C, 61°C, 62°C, 63°C, 64°C, 65°C, 66°C, 67°C, 68°C, 69°C, 70°C, preferably is 60°C.

优选的,步骤2)中,所述烘干处理是在烘箱中进行的,所述烘干的温度为80~120℃,例如烘干的温度为80℃、90℃、100℃、110℃、120℃,优选为100℃,所述烘干的时间为10~15h,例如烘干的时间为10h、11h、12h、13h、14h、15h,优选为12h。Preferably, in step 2), the drying treatment is carried out in an oven, and the drying temperature is 80-120°C, for example, the drying temperature is 80°C, 90°C, 100°C, 110°C, 120°C, preferably 100°C, the drying time is 10-15h, for example, the drying time is 10h, 11h, 12h, 13h, 14h, 15h, preferably 12h.

步骤3)中,所述焙烧处理的温度为400~600℃,例如焙烧的温度为400℃、410℃、420℃、430℃、440℃、450℃、460℃、470℃、480℃、490℃、500℃、510℃、520℃、530℃、540℃、550℃、560℃、570℃、580℃、590℃、600℃,优选为550℃;所述焙烧的时间为2~5h,例如焙烧时间为2h、3h、4h、5h,优选为3h;所述焙烧的升温速率为2~10℃/min,例如升温速率为2℃/min、3℃/min、4℃/min、5℃/min、6℃/min、7℃/min、8℃/min、9℃/min、10℃/min。In step 3), the temperature of the calcination treatment is 400-600°C, for example, the calcination temperature is 400°C, 410°C, 420°C, 430°C, 440°C, 450°C, 460°C, 470°C, 480°C, 490°C °C, 500 °C, 510 °C, 520 °C, 530 °C, 540 °C, 550 °C, 560 °C, 570 °C, 580 °C, 590 °C, 600 °C, preferably 550 °C; the roasting time is 2 to 5 hours, For example, the roasting time is 2h, 3h, 4h, 5h, preferably 3h; the heating rate of the roasting is 2-10°C/min, for example, the heating rate is 2°C/min, 3°C/min, 4°C/min, 5°C. °C/min, 6°C/min, 7°C/min, 8°C/min, 9°C/min, 10°C/min.

步骤4)中,所述高温还原再处理的过程为:将经步骤3)焙烧处理的产物放入气氛炉中进行升温还原处理。In step 4), the high-temperature reduction retreatment process is: put the roasted product in step 3) into an atmosphere furnace for temperature-rising reduction treatment.

优选地,所述气氛炉中的气氛为还原气氛,以氮气作为平衡气,优选地,所述还原气氛为氢气,所述氢气所占的体积比为1~100%,例如氢气的体积比为1%、10%、20%、30%、40%、50%、60%、70%、80%、90%、100%,优选为5%。Preferably, the atmosphere in the atmosphere furnace is a reducing atmosphere, and nitrogen is used as a balance gas. Preferably, the reducing atmosphere is hydrogen, and the volume ratio of the hydrogen is 1 to 100%, for example, the volume ratio of hydrogen is 1%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, 100%, preferably 5%.

优选地,所述升温还原的升温速率为2~10℃/min,例如升温速率为2℃/min、3℃/min、4℃/min、5℃/min、6℃/min、7℃/min、8℃/min、9℃/min、10℃/min,优选为5℃/min;所述升温后的温度为200~400℃,例如升温后的温度为200℃、210℃、220℃、230℃、240℃、250℃、260℃、270℃、280℃、290℃、300℃、310℃、320℃、330℃、340℃、350℃、360℃、370℃、380℃、390℃、400℃,优选为300℃;优选地,所述高温还原再处理的时间为2~5h,例如焙烧时间为2h、3h、4h、5h,优选为2h。经过还原处理的催化剂可直接用于挥发性有机物苯的催化燃烧。Preferably, the heating rate of the heating reduction is 2-10°C/min, for example, the heating rate is 2°C/min, 3°C/min, 4°C/min, 5°C/min, 6°C/min, 7°C/min min, 8°C/min, 9°C/min, 10°C/min, preferably 5°C/min; the temperature after the heating is 200-400°C, for example, the temperature after the heating is 200°C, 210°C, 220°C , 230°C, 240°C, 250°C, 260°C, 270°C, 280°C, 290°C, 300°C, 310°C, 320°C, 330°C, 340°C, 350°C, 360°C, 370°C, 380°C, 390°C °C, 400 °C, preferably 300 °C; preferably, the time for the high-temperature reduction retreatment is 2-5 h, for example, the roasting time is 2 h, 3 h, 4 h, 5 h, preferably 2 h. The reduced catalyst can be directly used for the catalytic combustion of benzene, a volatile organic compound.

本发明的目的之三在于提供一种载钯纤维基催化剂的用途,将所述载钯纤维基催化剂用于挥发性有机物苯的催化燃烧。The third object of the present invention is to provide a use of a palladium-loaded fiber-based catalyst, which is used for catalytic combustion of volatile organic compound benzene.

本发明制得的载钯纤维基催化剂呈丝状堆叠,容易成型处理,填充后呈棉花状,相对于粉状、颗粒状催化剂其透气性好,便于填装,无粉尘等二次污染,且催化剂效率高,广泛适用于冶炼厂、炼油厂、化工厂等固定源所排放废气中含苯的净化处理,经催化燃烧剧毒污染物苯能全部分解为无毒无害的二氧化碳和水。The palladium-loaded fiber-based catalyst prepared in the present invention is stacked in filaments, easy to form and process, and is cotton-like after filling. Compared with powdery and granular catalysts, it has good air permeability, is easy to fill, and has no secondary pollution such as dust, and The catalyst has high efficiency and is widely used in the purification treatment of benzene contained in the waste gas emitted by stationary sources such as smelters, oil refineries, and chemical plants. After catalytic combustion, the highly toxic pollutant benzene can be completely decomposed into non-toxic and harmless carbon dioxide and water.

与现有技术相比,本发明的有益效果为:Compared with prior art, the beneficial effect of the present invention is:

(1)本发明的载钯纤维基催化剂呈丝状堆叠,透气性好,容易成型处理,无粉尘等二次污染。(1) The palladium-loaded fiber-based catalyst of the present invention is stacked in a filamentary shape, has good air permeability, is easy to form and handle, and has no secondary pollution such as dust.

(2)本发明的载钯纤维基催化剂制备方法简单易行,制得的载钯纤维基催化剂广泛适用于冶炼厂、炼油厂、化工厂等固定源所排放废气中含苯的净化处理,经催化燃烧剧毒污染物苯能全部分解为无毒无害的二氧化碳和水。(2) The preparation method of the palladium-loaded fiber-based catalyst of the present invention is simple and easy, and the prepared palladium-loaded fiber-based catalyst is widely applicable to the purification treatment of benzene in exhaust gases discharged from stationary sources such as smelters, oil refineries, and chemical plants. Catalytic combustion of highly toxic pollutant benzene can be completely decomposed into non-toxic and harmless carbon dioxide and water.

(3)本发明的载钯纤维基催化剂用于挥发性有机物苯的催化燃烧时,具有空隙率高、传质效率高、成型容易、降解苯反应温度低、催化剂效率高的优点,空速为90L/(g·h)时,反应温度在250℃时苯的转化率就能达到95%以上。(3) When the palladium-loaded fiber-based catalyst of the present invention is used for the catalytic combustion of volatile organic compound benzene, it has the advantages of high porosity, high mass transfer efficiency, easy molding, low reaction temperature for degrading benzene, and high catalyst efficiency. The space velocity is 90L/(g·h), the conversion rate of benzene can reach more than 95% when the reaction temperature is 250°C.

附图说明Description of drawings

图1为本发明的实施例1制得的催化剂用于挥发性有机物苯的催化燃烧时的苯净化曲线和二氧化碳产率曲线示意图;1 is a schematic diagram of the benzene purification curve and the carbon dioxide yield curve when the catalyst prepared in Example 1 of the present invention is used for the catalytic combustion of volatile organic compound benzene;

图2为本发明的实施例2制得的催化剂用于挥发性有机物苯的催化燃烧时的苯净化曲线和二氧化碳产率曲线示意图;2 is a schematic diagram of the benzene purification curve and the carbon dioxide yield curve when the catalyst prepared in Example 2 of the present invention is used for the catalytic combustion of volatile organic compound benzene;

图3为本发明的实施例3制得的催化剂用于挥发性有机物苯的催化燃烧时的苯净化曲线和二氧化碳产率曲线示意图;3 is a schematic diagram of the benzene purification curve and the carbon dioxide yield curve when the catalyst prepared in Example 3 of the present invention is used for the catalytic combustion of volatile organic compound benzene;

图4为本发明的实施例4制得的催化剂用于挥发性有机物苯的催化燃烧时的苯净化曲线和二氧化碳产率曲线示意图;4 is a schematic diagram of the benzene purification curve and the carbon dioxide yield curve when the catalyst prepared in Example 4 of the present invention is used for the catalytic combustion of volatile organic compound benzene;

图5为本发明的实施例1-6制得的催化剂用于挥发性有机物苯的催化燃烧时的苯的转化率的对比图;Fig. 5 is the comparison chart of the conversion rate of benzene when the catalyst prepared by the embodiments of the present invention 1-6 is used for the catalytic combustion of volatile organic compound benzene;

图6为本发明的实施例3、7、8制得的催化剂用于挥发性有机物苯的催化燃烧时的苯的转化率的对比图;Fig. 6 is the comparison chart of the conversion rate of benzene when the catalysts prepared by the embodiments of the present invention 3, 7, and 8 are used for the catalytic combustion of volatile organic compound benzene;

图7为本发明的实施例3制得的催化剂的SEM图;Fig. 7 is the SEM figure of the catalyst that the embodiment of the present invention 3 makes;

图8为本发明的实施例4制得的催化剂的SEM图;Fig. 8 is the SEM figure of the catalyst that the embodiment of the present invention 4 makes;

图9为本发明的实施例8制得的催化剂的N2吸附表征图。Fig. 9 is a N 2 adsorption characterization diagram of the catalyst prepared in Example 8 of the present invention.

具体实施方式detailed description

下面结合附图1-9并通过具体实施方式来进一步说明本发明的技术方案。The technical solution of the present invention will be further described below in conjunction with the accompanying drawings 1-9 and through specific embodiments.

实施例1Example 1

A.称量陶瓷纤维10g,(Fisher Chemical Triton Kaowool ceramic fiber.Code:T/3740/48)一次用500ml去离子水,由布氏漏斗抽滤反复淋洗,一次淋洗约30分钟,样品抽干备用;称量二水硝酸钯0.25g,放入100ml去离子水中,搅拌混匀。将上述陶瓷纤维加入100ml溶液之中。再置入超声清洗槽里超声辅助浸渍。超声频率44KHz,浸渍1h。将上述固液体系转入旋转蒸发瓶中,由室温逐渐升温至60℃,将溶剂蒸发干净。之后将浸渍后的产物放入烘箱,100℃继续烘干12h。然后取出,降至室温,放入马弗炉内焙烧,升温速率5℃每分到500℃恒温3h。然后自然降温,备用。A. Weigh 10g of ceramic fiber, (Fisher Chemical Triton Kaowool ceramic fiber.Code: T/3740/48) once with 500ml of deionized water, filter and rinse repeatedly through Buchner funnel, rinse for about 30 minutes once, and drain the sample Standby; weigh 0.25 g of palladium nitrate dihydrate, put it into 100 ml of deionized water, and stir to mix. The above ceramic fiber was added to 100ml of the solution. Then put it into the ultrasonic cleaning tank for ultrasonic assisted impregnation. Ultrasonic frequency 44KHz, impregnation 1h. The above solid-liquid system was transferred into a rotary evaporating flask, and the temperature was gradually raised from room temperature to 60°C to evaporate the solvent. Afterwards, put the impregnated product into an oven, and continue drying at 100° C. for 12 hours. Then take it out, lower it to room temperature, put it into a muffle furnace for roasting, and heat up at a rate of 5°C per minute to 500°C for 3 hours. Then cool down naturally and set aside.

B.反应混合气的组成为:苯[C6H6]=1500ppm,[O2]=20%,N2作平衡气,气体总流量为300mL/min,空速为90L/(g·h),反应温度150~400℃。苯、二氧化碳、氧气等气体浓度利用气相色谱仪(安捷伦-7980B,FID和TCD)测定;B. The composition of the reaction mixture gas is: benzene [C 6 H 6 ]=1500ppm, [O 2 ]=20%, N 2 is used as the balance gas, the total gas flow rate is 300mL/min, and the space velocity is 90L/(g·h ), the reaction temperature is 150-400°C. The concentration of gases such as benzene, carbon dioxide, and oxygen was measured by gas chromatography (Agilent-7980B, FID and TCD);

C.上述催化剂用量为0.2g,在反应评价之前,需先用H2还原处理。条件为:H2=5%,N2作平衡气,气体总流量为400mL/min,升温速率10℃每分,在300℃恒温保持2h,之后降至室温开始升温评价;得到苯净化曲线和二氧化碳产率曲线如图1所示。C. The amount of the above-mentioned catalyst is 0.2g, and before the reaction evaluation, it needs to be treated with H2 reduction. The conditions are: H 2 =5%, N 2 as the balance gas, the total gas flow rate is 400mL/min, the heating rate is 10°C per minute, the constant temperature is maintained at 300°C for 2 hours, and then the temperature rises to evaluate after cooling down to room temperature; the benzene purification curve and The carbon dioxide yield curve is shown in Fig. 1.

实施例2Example 2

称量母体为:玻璃纤维10g,(ACROS Organic Glass wool,Code:386062500),其他操作参数如上实施例1。得到苯净化曲线和二氧化碳产率曲线如图2所示。The weighing matrix is: glass fiber 10g, (ACROS Organic Glass wool, Code: 386062500), and other operating parameters are as in Example 1 above. The obtained benzene purification curve and carbon dioxide yield curve are shown in Fig. 2 .

实施例3Example 3

称量陶瓷纤维10g,配置50(wet)%H2SO4溶液,一次用500ml去离子水,由布氏漏斗抽滤反复淋洗,一次淋洗约30分钟,用去离子洗至中性。样品抽干备用;其他制备与评价方法和实施例1一样,得到苯净化曲线和二氧化碳产率曲线如图3所示。对本实施例制得的催化剂的形貌进行电镜扫描,SEM图如图7所示。Weigh 10g of ceramic fiber, configure 50(wet)% H 2 SO 4 solution, use 500ml of deionized water once, filter and wash repeatedly through Buchner funnel, rinse for about 30 minutes once, and wash with deionized water until neutral. The sample was drained for later use; other preparation and evaluation methods were the same as in Example 1, and the benzene purification curve and carbon dioxide yield curve were obtained as shown in Figure 3. The morphology of the catalyst prepared in this example was scanned by an electron microscope, and the SEM image is shown in FIG. 7 .

实施例4Example 4

称量玻璃纤维10g,配置50(wet)%H2SO4溶液,一次用500ml去离子水,由布氏漏斗抽滤反复淋洗,一次淋洗约30分钟,用去离子洗至中性。样品抽干备用;其他制备与评价方法和实施例1一样。得到苯净化曲线和二氧化碳产率曲线如图4所示。对本实施例制得的催化剂的形貌进行电镜扫描,SEM图如图8所示。Weigh 10g of glass fiber, configure 50(wet)% H 2 SO 4 solution, use 500ml of deionized water once, filter through Buchner funnel repeatedly, rinse for about 30 minutes once, and wash with deionized water until neutral. The sample was drained for later use; other preparation and evaluation methods were the same as in Example 1. The obtained benzene purification curve and carbon dioxide yield curve are shown in Figure 4. The morphology of the catalyst prepared in this example was scanned by an electron microscope, and the SEM image is shown in FIG. 8 .

实施例5Example 5

称量玻璃纤维10g,配置50(wet)%HNO3溶液,一次用500ml去离子水,由布氏漏斗抽滤反复淋洗,一次淋洗约30分钟,用去离子洗至中性。样品抽干备用;其他制备与评价方法和实施例1一样,评价结果如图5所示。Weigh 10g of glass fiber, configure 50(wet)% HNO 3 solution, use 500ml of deionized water once, filter and rinse repeatedly through Buchner funnel, rinse for about 30 minutes once, and wash with deionized water until neutral. The sample was drained for later use; other preparation and evaluation methods were the same as in Example 1, and the evaluation results were shown in Figure 5.

实施例6Example 6

称量陶瓷纤维10g,配置50(wet)%HNO3溶液,一次用500ml去离子水,由布氏漏斗抽滤反复淋洗,一次淋洗约30分钟,用去离子洗至中性。样品抽干备用;其他制备与评价方法和实施例1一样,评价结果如图6所示。Weigh 10g of ceramic fiber, configure 50(wet)% HNO 3 solution, use 500ml deionized water once, filter and rinse repeatedly through Buchner funnel, rinse once for about 30 minutes, and wash with deionized water until neutral. The sample was drained for later use; other preparation and evaluation methods were the same as in Example 1, and the evaluation results were shown in Figure 6.

实施例7Example 7

称量陶瓷纤维7g加玻璃纤维3g,配置50(wet)%H2SO4溶液,一次用500ml去离子水,由布氏漏斗抽滤反复淋洗,一次淋洗约30分钟,用去离子洗至中性。样品抽干备用;其他制备与评价方法和实施例1一样,评价结果如图6所示。Weigh 7g of ceramic fiber and 3g of glass fiber, configure 50(wet)% H 2 SO 4 solution, use 500ml of deionized water at a time, filter and rinse repeatedly through a Buchner funnel, rinse for about 30 minutes once, and rinse with deionized water until neutral. The sample was drained for later use; other preparation and evaluation methods were the same as in Example 1, and the evaluation results were shown in Figure 6.

实施例8Example 8

称量陶瓷纤维8g加玻璃纤维2g,(产品出处)配置50(wet)%H2SO4溶液,一次用500ml去离子水,由布氏漏斗抽滤反复淋洗,一次淋洗约30分钟,用去离子洗至中性。样品抽干备用;其他制备与评价方法和实施例1一样,评价结果如图6所示,对本实施例制得的催化剂进行比表面积检测,实验结果如图9所示。Weigh ceramic fiber 8g plus glass fiber 2g, configure 50(wet)% H 2 SO 4 solution (source of product), once use 500ml deionized water, and repeatedly rinse by Buchner funnel suction filtration, once rinse for about 30 minutes, use Deionized wash to neutral. The sample was drained for later use; other preparation and evaluation methods were the same as in Example 1, and the evaluation results were shown in Figure 6. The specific surface area of the catalyst prepared in this example was tested, and the experimental results were shown in Figure 9.

综上实验,如图5所示,相对于实施例1的去离子水淋洗,实施例3、实施例4的酸洗对陶瓷纤维或玻璃纤维制成的催化剂的活性有了很大的提升。相对于实施例5、实施例6的硝酸淋洗,实施例3、实施例4的硫酸淋洗,可以看出,硫酸淋洗对陶瓷纤维或玻璃纤维制成的催化剂的活性提升最优。相对于实施例4的玻璃纤维相比,实施例3的陶瓷纤维相对玻璃纤维活性更优,但实施例7、实施例8的混合两种纤维制备的催化剂的活性最佳,如图6所示。In summary, as shown in Figure 5, compared with the deionized water rinsing in Example 1, the pickling in Example 3 and Example 4 has greatly improved the activity of the catalyst made of ceramic fibers or glass fibers . Compared with the nitric acid leaching in Example 5 and Example 6, and the sulfuric acid rinsing in Example 3 and Example 4, it can be seen that sulfuric acid rinsing has the best activity improvement for catalysts made of ceramic fibers or glass fibers. Compared with the glass fiber of Example 4, the activity of the ceramic fiber of Example 3 is better than that of glass fiber, but the activity of the catalyst prepared by mixing the two fibers of Example 7 and Example 8 is the best, as shown in Figure 6 .

由图7、8可以看出,载体纤维呈棒状排列,贵金属钯较均匀地负载于载体纤维的表面。It can be seen from Figures 7 and 8 that the carrier fibers are arranged in a rod shape, and the noble metal palladium is evenly loaded on the surface of the carrier fibers.

由图9可以看出,相对于陶瓷纤维或玻璃纤维的比表面积为2-3m2/g来说,实施例8制得的催化剂的比表面积有了很大的提高,为87.57m2/g,比表面积的增大有利于催化剂的活性。It can be seen from Figure 9 that the specific surface area of the catalyst prepared in Example 8 has been greatly improved, which is 87.57 m 2 /g, compared to the specific surface area of ceramic fibers or glass fibers of 2-3 m 2 /g , the increase of the specific surface area is beneficial to the activity of the catalyst.

以上实施例仅用来说明本发明的详细方法,本发明并不局限于上述详细方法,即不意味着本发明必须依赖上述详细方法才能实施。所属技术领域的技术人员应该明了,对本发明的任何改进,对本发明产品各原料的等效替换及辅助成分的添加、具体方式的选择等,均落在本发明的保护范围和公开范围之内。The above examples are only used to illustrate the detailed methods of the present invention, and the present invention is not limited to the above detailed methods, that is, it does not mean that the present invention can only be implemented depending on the above detailed methods. Those skilled in the art should understand that any improvement of the present invention, the equivalent replacement of each raw material of the product of the present invention, the addition of auxiliary components, the selection of specific methods, etc., all fall within the scope of protection and disclosure of the present invention.

Claims (10)

1.一种载钯纤维基催化剂,其特征在于,所述催化剂的载体为纤维,活性组分为负载在所述载体上的钯,以所述载体的质量为100%计,所述钯的质量为0.05~2%。1. a palladium-loaded fiber-based catalyst is characterized in that the carrier of the catalyst is a fiber, and the active component is palladium loaded on the carrier, and the mass of the carrier is 100% in terms of the palladium. The mass is 0.05 to 2%. 2.根据权利要求1所述的载钯纤维基催化剂,其特征在于,所述纤维为陶瓷纤维、玻璃纤维、金属纤维、活性炭纤维中的一种或至少两种的混合物;2. palladium-loaded fiber-based catalyst according to claim 1, is characterized in that, described fiber is the mixture of one or at least two in ceramic fiber, glass fiber, metal fiber, active carbon fiber; 优选地,所述纤维为玻璃纤维和陶瓷纤维的混合物,所述玻璃纤维与所述陶瓷纤维的质量比为(7~9):(1~3),优选为8:2;Preferably, the fibers are a mixture of glass fibers and ceramic fibers, and the mass ratio of the glass fibers to the ceramic fibers is (7-9):(1-3), preferably 8:2; 优选地,以所述载体的质量为100%计,所述钯的质量为1%。Preferably, the mass of the palladium is 1% based on 100% of the mass of the carrier. 3.一种如权利要求1或2所述的载钯纤维基催化剂的制备方法,其特征在于,所述制备方法包括如下步骤:3. a preparation method of palladium-loaded fiber-based catalyst as claimed in claim 1 or 2, is characterized in that, described preparation method comprises the steps: 1)将载体纤维进行酸洗;1) pickling the carrier fiber; 2)将步骤1)酸洗后的载体纤维置于含钯溶液中浸渍,然后进行蒸发、烘干处理;2) impregnating the carrier fiber after pickling in step 1) in a solution containing palladium, then evaporating and drying; 3)将步骤2)烘干后的产物进行焙烧处理;3) roasting the dried product in step 2); 4)将步骤3)焙烧处理后的产物进行高温还原再处理,得到载钯纤维基催化剂。4) The product after the roasting treatment in step 3) is subjected to high-temperature reduction and retreatment to obtain a palladium-supported fiber-based catalyst. 4.根据权利要求3所述的制备方法,其特征在于,步骤1)中,所述酸洗的过程为,将载体纤维浸于酸中,在真空滴滤瓶中逐滴抽滤淋洗液体;4. preparation method according to claim 3, is characterized in that, in step 1), the process of described pickling is, the carrier fiber is soaked in the acid, in the vacuum trickling filter bottle, suck and filter the rinsing liquid drop by drop ; 优选地,所述酸的质量百分数为10~60%,优选为50%;Preferably, the mass percentage of the acid is 10-60%, preferably 50%; 优选地,所述酸为硫酸或硝酸,优选为硫酸;Preferably, the acid is sulfuric acid or nitric acid, preferably sulfuric acid; 优选地,所述载体纤维与所述酸的固液比为1/100~1/10g/mL,优选为1/50g/mL;Preferably, the solid-to-liquid ratio of the carrier fiber to the acid is 1/100-1/10 g/mL, preferably 1/50 g/mL; 优选地,所述淋洗的时间为20~40min,优选为30min,所述淋洗的次数为1~3次。Preferably, the rinsing time is 20-40 min, preferably 30 min, and the rinsing times are 1-3 times. 5.根据权利要求3或4所述的制备方法,其特征在于,步骤1)中,经所述酸洗后的纤维进行去离子水冲洗,所述去离子水冲洗后的pH值为中性;5. according to the described preparation method of claim 3 or 4, it is characterized in that, in step 1), the fiber after described pickling is carried out deionized water rinse, and the pH value after described deionized water rinse is neutral ; 优选地,所述去离子水冲洗后还包括干燥的步骤;Preferably, after the deionized water is rinsed, a drying step is also included; 优选地,所述干燥是在烘箱中进行的,所述干燥的温度为100~150℃,优选为120℃;Preferably, the drying is carried out in an oven, and the drying temperature is 100-150°C, preferably 120°C; 优选地,所述干燥的时间为5~24h,优选为12h。Preferably, the drying time is 5-24 hours, preferably 12 hours. 6.根据权利要求3-5之一所述的制备方法,其特征在于,步骤2)中,所述含钯溶液为二水硝酸钯溶液、氯化钯溶液、乙酸钯溶液中的一种;6. according to the described preparation method of one of claim 3-5, it is characterized in that, in step 2), described palladium-containing solution is the one in dihydrate palladium nitrate solution, palladium chloride solution, palladium acetate solution; 优选地,所述浸渍为超声辅助浸渍,所述超声辅助浸渍的具体过程为:将酸洗后的载体纤维置于含钯溶液中得到固液体系,将所述固液体系置于超声波池中进行超声辅助浸渍,所述超声辅助浸渍的温度为23~27℃;所述超声辅助浸渍的超声的频率为40~50kHz,优选为44kHz;所述超声辅助浸渍的时间为10~60min,优选为30min。Preferably, the impregnation is ultrasonic-assisted impregnation, and the specific process of the ultrasonic-assisted impregnation is: placing the pickled carrier fiber in a palladium-containing solution to obtain a solid-liquid system, and placing the solid-liquid system in an ultrasonic pool Carry out ultrasonic assisted impregnation, the temperature of described ultrasonic assisted impregnation is 23~27 ℃; The ultrasonic frequency of described ultrasonic assisted impregnation is 40~50kHz, preferably 44kHz; The time of described ultrasonic assisted impregnation is 10~60min, preferably 30min. 7.根据权利要求3-6之一所述的制备方法,其特征在于,步骤2)中,所述蒸发处理是在旋转蒸发瓶中进行的,所述旋转蒸发的旋转频率为20~200r/min,优选为60r/min;所述旋转蒸发的温度为50~70℃,优选为60℃;7. The preparation method according to any one of claims 3-6, characterized in that, in step 2), the evaporation treatment is carried out in a rotary evaporation flask, and the rotation frequency of the rotary evaporation is 20-200r/ min, preferably 60r/min; the temperature of the rotary evaporation is 50-70°C, preferably 60°C; 优选的,步骤2)中,所述烘干处理是在烘箱中进行的,所述烘干的温度为80~120℃,优选为100℃;所述烘干的时间为10~15h,优选为12h。Preferably, in step 2), the drying process is carried out in an oven, the drying temperature is 80-120°C, preferably 100°C; the drying time is 10-15h, preferably 12h. 8.根据权利要求3-7之一所述的制备方法,其特征在于,步骤3)中,所述焙烧处理的温度为400~600℃,优选为550℃;所述焙烧的时间为2~5h,优选为3h;所述焙烧的升温速率为2~10℃/min。8. The preparation method according to any one of claims 3-7, characterized in that, in step 3), the temperature of the roasting treatment is 400-600° C., preferably 550° C.; the roasting time is 2-600° C. 5h, preferably 3h; the heating rate of the calcination is 2-10°C/min. 9.根据权利要求3-8之一所述的制备方法,其特征在于,步骤4)中,所述高温还原再处理的过程为:将经步骤3)焙烧处理的产物放入气氛炉中进行升温还原处理;9. The preparation method according to any one of claims 3-8, characterized in that, in step 4), the process of the high-temperature reduction retreatment is: putting the product roasted in step 3) into an atmosphere furnace Heating reduction treatment; 优选地,所述气氛炉中的气氛为氢气,所述氢气所占的体积比为1~100%,优选为5%;Preferably, the atmosphere in the atmosphere furnace is hydrogen, and the volume ratio of the hydrogen is 1-100%, preferably 5%; 优选地,所述升温还原的升温速率为2~10℃/min,优选为5℃/min,所述升温后的温度为200~400℃,优选为300℃;优选地,所述高温还原再处理的时间为2~5h,优选为2h。Preferably, the heating rate of the heating reduction is 2-10°C/min, preferably 5°C/min, and the temperature after the heating is 200-400°C, preferably 300°C; preferably, the high-temperature reduction is The treatment time is 2 to 5 hours, preferably 2 hours. 10.一种如权利要求1或2所述的载钯纤维基催化剂的用途,其特征在于,将所述载钯纤维基催化剂用于挥发性有机物苯的催化燃烧。10. A use of the palladium-loaded fiber-based catalyst as claimed in claim 1 or 2, characterized in that, the palladium-loaded fiber-based catalyst is used for catalytic combustion of volatile organic compound benzene.
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