CN112547059B - Ru/3DOM SnO with good stability 2 Preparation method and application of catalyst - Google Patents

Ru/3DOM SnO with good stability 2 Preparation method and application of catalyst Download PDF

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CN112547059B
CN112547059B CN202010930806.6A CN202010930806A CN112547059B CN 112547059 B CN112547059 B CN 112547059B CN 202010930806 A CN202010930806 A CN 202010930806A CN 112547059 B CN112547059 B CN 112547059B
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戴洪兴
余晓慧
邓积光
刘雨溪
敬林
张兴
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Beijing University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
    • B01J23/622—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead
    • B01J23/626—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead with tin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8659—Removing halogens or halogen compounds
    • B01D53/8662—Organic halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/16—Reducing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/206—Organic halogen compounds
    • B01D2257/2064—Chlorine

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Abstract

Ru/3DOM SnO with good stability 2 A preparation method and application of a catalyst, belonging to the technical field of functional material synthesis. Firstly, preparing three-dimensional ordered macroporous tin dioxide (3 DOM SnO) by using polymethyl methacrylate (PMMA) colloidal crystal template 2 ) The carrier is prepared by loading Ru nano particles to 3DOM SnO by a sodium borohydride reduction method protected by polyvinyl alcohol (PVA) 2 Drying and roasting the surface of the carrier to obtain xRu/3DOM SnO 2 A catalyst. The invention has simple operation process, and the prepared xRu/3DOM SnO 2 The catalyst has high specific surface area and excellent catalytic activity and stability for trichloroethylene oxidation reaction.

Description

Ru/3DOM SnO with good stability 2 Preparation method and application of catalyst
Technical Field
The invention relates to Ru/3DOM SnO 2 Preparation method and application of catalyst, namely, polymethyl methacrylate (PMMA) is used as hard template, and polyvinyl alcohol (PVA) is used for protectionNaBH 4 Preparation of Ru particles by reduction method and loading of Ru particles to three-dimensional ordered macroporous SnO 2 (3DOM SnO 2 ) The surface of the carrier is dried and baked to obtain xRu/3DOM SnO 2 (x=0.09-1.65 wt%) and finally can be used for high-effective catalytic oxidation of trichloroethylene. Belonging to the technical field of functional material synthesis.
Background
In recent years, chlorine-Containing Volatile Organic Compounds (CVOCs) discharged in the mechanical manufacturing, petrochemical, pharmaceutical, and spray industries not only destroy the atmospheric ozone layer, form photochemical smog, and generate global warming, etc., but also pose a great threat to human health. Research has shown that catalytic combustion is a more promising and economical process than traditional physical and other chemical processes. Currently, there are three main types of catalysts for eliminating CVOCs, namely noble metal catalysts, transition metal oxide catalysts and zeolite catalysts. Among them, the supported noble metal catalyst is attracting attention for its high activity and excellent antitoxic performance. For example, wang et al (Y.Lao, et al Catalysis Science)&Technology 8 (2018) 4797-4811) studied 1, 2-dichlorobenzene in Ru/Co 3 O 4 The oxidation reaction mechanism on the catalyst shows that the addition of Ru can improve the utilization rate of active oxygen, thereby improving the catalytic activity. Ru/CeO research by Wang group of topics 2 (H.Huang,et al.,Applied Catalysis B:Environmental158-159(2014)96-105)、Ru/Ce x Al y (Y. Gu et al, ACS Omega 3 (2018) 8460-8470), ru/SBA-15 (Q. Dai et al, applied Catalysis B: environmental 126 (2012) 64-75) catalyst effect on CVOCs degradation. The result shows that Ru is used as an active component with better stability, and the prepared supported Ru catalyst has excellent catalytic performance.
SnO 2 Has abundant oxygen vacancies, acidic species and active oxygen species, has been used in the catalytic field, such as CO oxidation, methane combustion, toluene oxidation and NH 3 Selective reduction of NO x Etc. Researchers have studied the key factors that determine the activity of the catalyst. Kamiuchi et al (N.Kamiuchi, H.Muroyama, T.Matsui, R.Kikuchi, K.Eguchi, applied Catalysis A: general 379 (2010) 148-154) found Pd/SnO 2 Core-shell structure of catalyst becomesThe conversion leads to a difference in catalytic activity. Reduced or oxidized Pt/SnO 2 Is also an important factor in causing differences in catalytic activity (N.Kamiuchi, K.Taguchi, T.Matsui, R.Kikuchi, K.Eguchi, applied Catalysis B: environmental 89 (2009) 65-72). Liu et al (Y. Liu et al, industrial)&Engineering Chemistry Research 57 (2018) 14052-14063) showed that the deep oxidation of toluene was due to more surface active oxygen and acid site exposure.
In recent years, catalysts with different morphologies have been studied for the catalytic performance of oxidation of different VOCs, such as benzene, toluene, methane, trichloroethylene, and the like. The three-dimensional ordered macroporous (3 DOM) structure shows excellent catalytic activity on the catalytic oxidation of VOCs due to the unique pore structure and the high specific surface area. However, few studies have attempted to produce SnO 2 The material is applied to CVOCs catalytic oxidation. At present, no document reports Ru/3DOM SnO 2 Catalytic oxidation of trichloroethylene oxidation.
Disclosure of Invention
The invention aims to provide Ru/3DOM SnO which has high specific surface area, is simple and convenient to operate and can efficiently catalyze the oxidation of trichloroethylene 2 A method for preparing the catalyst.
The invention synthesizes 3DOM SnO by polymethyl methacrylate (PMMA) colloidal crystal template method 2 NaBH protected with polyvinyl alcohol (PVA) 4 Ru particles were prepared by the reduction method and loaded to 3DOM SnO 2 The surface of the carrier is dried and baked to obtain xRu/3DOM SnO 2 A catalyst; wherein the value range of the mass percent load x is more than 0% and less than or equal to 2%.
The method specifically comprises the following steps: dissolving stannous chloride in deionized water, and stirring until the stannous chloride is completely dissolved; placing the above solution in ice bath, and then dropwise adding H 2 O 2 The solution is changed from transparent to yellow-green, and then is changed into transparent again; when the temperature is reached to room temperature, the PMMA template is infiltrated into the precursor solution for a period of time. Vacuum filtering and drying at room temperature, and heating to 280-350deg.C, preferably 300deg.C at a rate of 5deg.C/min in nitrogen atmosphere for 2 hr; after cooling to room temperature, in an air atmosphere (150 mL/min)Heating to 480-520 ℃ at a speed of 5 ℃/min, preferably 500 ℃, and keeping for 6 hours to obtain 3DOM SnO 2 A carrier;
NaBH protected by PVA 4 Reduction method for preparing Ru/3DOM SnO 2 Catalyst: ruCl is to be processed 3 The aqueous solution was added to the PVA solution in an ice-water bath, and after 30 minutes, naBH dissolved in deionized water was added to the PVA solution with Ru/PVA mass ratio=1.0:1.2 4 Rapidly adding the mixture into the solution, and vigorously stirring for 30 minutes; then adding 3DOM SnO 2 The method comprises the steps of carrying out a first treatment on the surface of the At this time, the stirring rate was lowered to prevent damage to the support macropore structure. After slowly stirring for 6h, vacuum filtering, drying at 60deg.C for 12h, heating to 450-550deg.C, preferably 500deg.C at a rate of 5deg.C/min in air atmosphere, and maintaining for 2h to obtain Ru/3DOM SnO 2 A catalyst.
xRu/3DOM SnO prepared by the invention 2 The catalyst has excellent catalytic performance on trichloroethylene oxidation reaction.
Drawings
Fig. 1 is an XRD spectrum of the prepared catalyst. Wherein the curve (a, c-e) is xRu/3DOM SnO 2 XRD patterns of the catalyst (x=0, 0.19wt%,0.58wt%,0.98 wt%) and curves (f) and (b) were XRD patterns of example 1 and example 2, respectively.
FIG. 2 shows the 3DOM SnO obtained 2 SEM photographs of (2).
FIG. 3 shows the prepared xRu/3DOM SnO 2 A TEM photograph of (c). Wherein (a) and (b) (c) are 3DOM SnO 2 TEM photograph of (d), (e) and (f) being 0.98Ru/3DOM SnO 2 A TEM photograph of (c).
FIG. 4 shows the catalytic activity of the catalyst prepared for the oxidation of trichloroethylene. The reaction conditions were 1000ppm of trichloroethylene, O 2 Concentration of 20vol%, N 2 To balance the gas, the space velocity was 40000 mL/(g h).
Detailed Description
In order to further illustrate the invention, a detailed description is provided below in connection with the practice.
Example 1
8.4g anhydrous stannous chloride was dissolved in 20mL deionized water and stirred until completely dissolved. The above solution was placed in an ice bath, and then 6.0g was added dropwise via syringe H 2 O 2 The solution (30 wt% aqueous solution) changed from transparent to yellowish green, and then to transparent again. When cooled to room temperature, 5.0g of PMMA template was infiltrated into the precursor solution for about 4 hours. After vacuum filtration and room temperature drying for 48h, the temperature was raised to 300℃at a rate of 5℃per minute in a nitrogen atmosphere (200 mL/min) and maintained for 2h. After cooling to room temperature, heating to 500 ℃ at a rate of 5 ℃/min in an air atmosphere (150 mL/min), and maintaining for 6 hours to obtain 3DOM SnO 2 A carrier.
NaBH protected by PVA (molecular weight 10000 g/mol) 4 Preparation of 1.65Ru/3DOM SnO by reduction method 2 Catalyst (theoretical loading 2 wt%). 9.9mL RuCl 3 The (0.010 mol/L) aqueous solution was added to 6.0mL PVA (2 g/L) in an ice-water bath (Ru/PVA mass ratio=1.0:1.2). After 30 minutes, 9.3mL NaBH dissolved in deionized water was added 4 (2 g/L) was added rapidly to the above solution and vigorously stirred for 30 minutes. Then 0.5g of 3DOM SnO is added 2 . At this time, the stirring rate was lowered to prevent damage to the support macropore structure. After slowly stirring for 6 hours, vacuum filtering, drying at 60 ℃ for 12 hours, heating to 500 ℃ at a speed of 5 ℃/min in air atmosphere, and keeping for 2 hours to obtain 1.65Ru/3DOM SnO 2 A catalyst.
The catalyst obtained by the invention is applied to the catalytic oxidation of trichloroethylene, and the main reaction products are as follows: carbon dioxide, water, HCl, chlorine, and the like. At a trichloroethylene concentration of 1000ppm, O 2 Concentration of 20vol%, N 2 The activity and stability of the catalyst were tested for equilibrium gas and space velocity of 40000 mL/(g h). The catalyst T 50％ (reaction temperature required for 50% conversion of trichloroethylene) 270 ℃ C., T 90％ (reaction temperature required for 90% conversion of trichloroethylene) was 300℃and catalyst T 95％ (the reaction temperature required when the trichloroethylene conversion rate reaches 95%) is 320 ℃, the activity is stable in 30 hours of continuous test, and the catalyst has good stability.
Example 2
NaBH protected by PVA (molecular weight 10000 g/mol) 4 Preparation of 0.09Ru/3DOM SnO by reduction method 2 Catalytic reactionAgent (theoretical loading 0.10 wt%). Will 0.50mL RuCl 3 The (0.010 mol/L) aqueous solution was added to 0.3mL PVA (2 g/L) of an ice-water bath (Ru/PVA mass ratio=1.0:1.2). After 30 minutes, 0.47mL NaBH dissolved in deionized water was added 4 (2 g/L) was added rapidly to the above solution and vigorously stirred for 30 minutes. Then 0.5g of 3DOM SnO is added 2 . At this time, the stirring rate was lowered to prevent damage to the support macropore structure. After slowly stirring for 6 hours, vacuum filtering, drying at 60 ℃ for 12 hours, heating to 500 ℃ at a speed of 5 ℃/min in air atmosphere, and keeping for 2 hours to obtain 0.09Ru/3DOM SnO 2 A catalyst.
The catalyst obtained by the invention is applied to the catalytic oxidation of trichloroethylene. At a trichloroethylene concentration of 1000ppm, O 2 Concentration of 20vol%, N 2 T of the catalyst under conditions of equilibrium gas and space velocity of 40000 mL/(g h) 50％ At 333 ℃, T 90％ 378 ℃.
The invention has simple operation process, the prepared catalyst has high specific surface area and xRu/3DOM SnO 2 The catalyst has excellent catalytic performance on trichloroethylene oxidation.

Claims (2)

1. Application of three-dimensional ordered macroporous tin dioxide supported ruthenium catalyst for catalytic oxidation of trichloroethylene, wherein the catalyst synthesizes 3DOM SnO by polymethyl methacrylate colloidal crystal template method 2 NaBH protected by polyvinyl alcohol 4 Ru particles were prepared by the reduction method and loaded to 3DOM SnO 2 The surface of the carrier is dried and baked to obtainxRu/3DOM SnO 2 A catalyst; wherein the value range of the mass percent load x is more than or equal to 0.58% and less than or equal to 2%;
the specific preparation method of the three-dimensional ordered macroporous tin dioxide supported ruthenium catalyst comprises the following steps:
dissolving stannous chloride in deionized water, and stirring until the stannous chloride is completely dissolved; placing the above solution in ice bath, and then dropwise adding H 2 O 2 The solution is changed from transparent to yellow-green, and then is changed into transparent again; penetrating PMMA template into the precursor solution for a period of time when the temperature is reached to room temperatureThe method comprises the steps of carrying out a first treatment on the surface of the Vacuum filtering and drying at room temperature, and heating to 280-350deg.C at a rate of 5deg.C/min in nitrogen atmosphere, and maintaining at 2h; after cooling to room temperature, heating to 480-520 ℃ at a speed of 5 ℃/min in air atmosphere, and keeping 6h to obtain 3DOM SnO 2 A carrier;
NaBH protected by PVA 4 Reduction method for preparing Ru/3DOM SnO 2 Catalyst: ruCl is to be processed 3 The aqueous solution was added to a PVA solution in an ice-water bath, the Ru/PVA mass ratio=1.0:1.2, after 30 minutes, naBH dissolved in deionized water 4 Rapidly adding the mixture into the solution, and vigorously stirring for 30 minutes; then adding 3DOM SnO 2 The method comprises the steps of carrying out a first treatment on the surface of the At this time, the stirring rate is lowered to prevent damage to the macroporous structure of the carrier; after slowly stirring for 6h, vacuum filtering, drying at 60deg.C for 12h, heating to 500deg.C at a rate of 5deg.C/min in air atmosphere, and maintaining for 2h to obtain Ru/3DOM SnO 2 A catalyst.
2. Use according to claim 1, characterized in that it is raised to 300 ℃ at a rate of 5 ℃/min in a nitrogen atmosphere; the temperature was raised to 500℃at a rate of 5℃per minute in an air atmosphere.
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