CN113058632B - Platinum-based catalyst with hexagonal boron carbon nitrogen as carrier and preparation method thereof - Google Patents
Platinum-based catalyst with hexagonal boron carbon nitrogen as carrier and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of preparation of low-carbon alkane dehydrogenation catalysts, and particularly relates to a platinum catalyst taking hexagonal boron carbon nitrogen as a carrier and a preparation method thereof. The catalyst specifically comprises 1.0-10.0 mass% of platinum and 90-99 mass% of hexagonal boron carbon nitrogen. The specific preparation method comprises the steps of mixing a boron source, a nitrogen source and a carbon source according to the proportion of 1: 1-10, roasting the mixture in inert gas at 900-1400 ℃ to obtain a hexagonal boron carbon nitrogen coarse body, washing the hexagonal boron carbon nitrogen coarse body with hydrochloric acid with a certain concentration to obtain a hexagonal boron carbon nitrogen pure body, soaking the hexagonal boron carbon nitrogen pure body with a platinum-containing compound solution, drying the hexagonal boron carbon nitrogen pure body in the inert gas, and reducing the hexagonal boron carbon nitrogen pure body. The obtained catalyst is used for dehydrogenation reaction of low-carbon alkane, and has high activity and stability.
Description
Technical Field
The invention belongs to the field of preparation of low-carbon alkane dehydrogenation catalysts, and particularly relates to a platinum catalyst taking hexagonal boron carbon nitrogen as a carrier and a preparation method thereof.
Background
The propane dehydrogenation catalyst is commonly used in Pt-series and Cr-series catalysts, wherein the active center Cr and compounds thereof of the Cr-series catalyst are heavy metals, have toxicity and easily cause pollution to the environment, so the use of the catalyst is limited to a certain extent. Although the Pt-based catalyst is relatively expensive, it has high activity and stability.
The carrier is a solid which plays a role in supporting active components in the catalyst. With the improvement of the requirements of people on the catalytic performance, the research on the carrier is more and more. For propane dehydrogenation, a support having good thermal stability, a high surface area, and a uniform pore structure is required.
The carbon material itself has catalytic properties in the dehydrogenation of alkanes, while boron nitride exhibits excellent stability properties in the dehydrogenation of alkanes. By doping carbon element into the structure of boron nitride, the carbon element and the boron nitride have synergistic effect so as to obtain the best propane dehydrogenation performance. The carbon element can be easily doped into the BN nano-sheet, which is a feasible method for changing the physicochemical property of BN to prepare a new material, namely ternary ceramic Boron Carbide (BCN). The synthesized BCN material shows complementary properties with graphene and h-BN materials, so that the electronic structure, properties and application have rich diversity. BCN nanoplates can form layered hybrid structures because of their close lattice parameters. C-doped BNNSs with tuned dielectric band gap are used as an excellent metal-free catalyst. The BCN nanosheet has the advantages of large specific surface area, abundant O-containing groups on the surface, obvious defects (vacancies and edges), excellent durability and adsorption capacity, and is a promising metal-free catalyst, even superior to a noble metal Pt/C catalyst.
Guo et al (GUO F S, YANG P J, PAN Z M, et al. Carbon-dot BN Nanosheets for the Oxidative Dehydrogenation of Ethylbenzene [ J ]. Angewandte Chemie-International Edition,2017,56(28):8231-8235.) reported the synthesis, characterization and application of BCN nanosheet porous structure as Oxidative Dehydrogenation reaction catalyst. This BCN nanosheet consists of hybrid, randomly distributed domains of h-BN and C phases, with C, B and N being demonstrated as covalent bonds in the graphene layer. Research shows that BCN shows high activity and selectivity and excellent oxidation resistance in the process of preparing styrene by oxidative dehydrogenation of ethylbenzene.
Goyal et al (GOYAL R, SARKAR B, BAG A, et al. Single-step synthesis of iterative BxCN: a metal-free catalyst for low-temperature oxidative dehydrogenation of propane [ J ] Mater Chem A,2016,4(47):18559-18569.) synthesized a boron-nitrogen mesoporous co-doped carbon material with a hierarchical pore structure by a nano-casting method using a novel boron precursor as a raw material. The result shows that the BxCN material has excellent specific surface area, general pore diameter and large pore diameter. In addition, the pore size can be adjusted by varying the amount of boron source used. The N-B-C type structure of the material is characterized by adopting solid nuclear magnetic resonance and XPS technology. The material has good stability in an oxygen environment, and the catalytic capability of the newly developed material in a carbon-hydrogen bond activation reaction is also proved. The mesoporous BxCN material has certain catalytic activity (6.7%) on the oxidative dehydrogenation of propane and excellent selectivity (84.6%) on propylene. The reports disclosed therein on the oxidative dehydrogenation of propane and the direct dehydrogenation of propane according to the invention differ considerably in two completely different types of reaction. Oxidative dehydrogenation is a method of reducing dehydrogenation reaction conditions (especially temperature, the reaction temperature of oxidative dehydrogenation is about 400 ℃ generally) by adding an oxidant, one difficulty of the reaction is the safety of the process, and the other difficulty is how to improve the selectivity of a target product. For the direct dehydrogenation reaction of propane, the reaction is typically characterized by a high reaction temperature, which is generally higher than 450 ℃, and the phenomena of catalyst coking, sintering and further inactivation easily occur, so that the problem of improving the stability of the reaction catalyst is a problem recognized in the industry. For example, Goyal et al use BxCN for oxidative dehydrogenation, by activating propane C-H under an oxygen atmosphere using the B-N-C structure, propane is first combined with oxygen and finally water molecules are removed to produce propylene. However, the prepared hexagonal boron carbon nitrogen is used as a carrier, and active metal platinum is loaded on the carrier, so that charge effect can be generated between the hexagonal boron carbon nitrogen used as the carrier and the active metal platinum, thereby leading the platinum atoms and the hexagonal boron carbon nitrogen carrier to have strong metal carrier interaction (SMSI), the strong interaction between the metal carriers ensures that the platinum atoms are very stable in the reaction, the propane can be directly adsorbed on the surface of the carrier, the C-H bond of the propane is directly broken to generate the propylene by the participation of the platinum atoms in the reaction, in addition, the hexagonal boron nitride prepared by the method can uniformly disperse metal platinum atoms on the surface of the hexagonal boron nitride, and is more beneficial to the stability of the platinum atoms in a high-temperature reaction, so that the catalyst has very excellent stability in the reaction.
In view of the fact that the boron carbon nitrogen material has general catalytic activity when being used for propane oxidative dehydrogenation reaction, and no literature or patent reports that the boron carbon nitrogen material can be used in propane direct dehydrogenation reaction until now exist, the cubic boron carbon nitrogen nanosheet synthesized by the method can be applied to propane direct dehydrogenation catalytic reaction and has very good properties.
Disclosure of Invention
The invention aims to provide a platinum catalyst taking hexagonal boron carbon nitrogen as a carrier and a preparation method thereof, wherein a boron source, a nitrogen source and a carbon source are mixed according to a proportion to prepare a hexagonal boron carbon nitrogen pure body, and then platinum loading is carried out, so that the catalyst has high catalytic activity, high selectivity and high stability when being applied to the dehydrogenation reaction of low-carbon alkane.
In order to realize the purpose, the invention adopts the following technical scheme:
the platinum-based catalyst with the hexagonal boron carbon nitrogen as the carrier comprises the hexagonal boron carbon nitrogen and platinum, and preferably comprises 1.0-10.0 mass% of Pt and 90.0-99.0 mass% of the hexagonal boron carbon nitrogen.
The preparation method of the platinum-based catalyst taking hexagonal boron carbon nitrogen as a carrier specifically comprises the steps of mixing a boron source, a nitrogen source and a carbon source according to the mass ratio of 1: 1-10, roasting the mixture in inert gas at 900-1400 ℃ to obtain a hexagonal boron carbon nitrogen coarse body, washing and drying the hexagonal boron carbon nitrogen coarse body with hydrochloric acid with a certain concentration to obtain a hexagonal boron carbon nitrogen pure body, soaking the hexagonal boron carbon nitrogen pure body with a platinum-containing compound solution, drying the hexagonal boron carbon nitrogen pure body in inert gas, and reducing the hexagonal boron carbon nitrogen pure body.
In the method, the boron source is simple substance boron, boric acid, diboron trioxide or sodium tetraborate, preferably boric acid;
the nitrogen source is ammonium bicarbonate, ammonium chloride, dopamine hydrochloride or melamine, preferably melamine;
the carbon source used is glucose, fructose, starch or cellulose, preferably glucose.
Preferably, the mass ratio of the glucose to the boric acid is 1-6, the mass ratio of the melamine to the boric acid is 1-3,
in the method, the concentration of the washing hydrochloric acid is 0.5-1 mol/L.
In the method, the roasting temperature of the mixture in the inert gas is preferably 800-1100 ℃. The inert gas is argon, helium or nitrogen. The inert gas is preferably nitrogen.
In the method, the roasting time is preferably 2-20 hours, and more preferably 2-8 hours.
In the above method, the platinum-containing compound is any one selected from platinum nitrate, chloroplatinic acid, potassium chloroplatinate, tetraammineplatinum dichloride and platinum acetylacetonate. In the above method, the liquid/solid ratio at the time of immersion is preferably 10 to 50 mL/g.
In the method, the platinum-containing precursor solution used for impregnation is prepared by one or more solvents of deionized water, ethanol, acetone or isopropanol. The platinum content in the platinum-containing compound solution is preferably 1-10 mg/mL.
In the method, the method for impregnating the hexagonal boron carbon nitrogen carrier with the platinum-containing compound solution can be static impregnation or stirring impregnation, and the preferable method comprises the steps of firstly stirring, then performing ultrasonic treatment, and then stirring and impregnating, wherein the ultrasonic treatment temperature is 15-45 ℃, and the time is 0.5-5 hours; the temperature during stirring is 20-100 ℃, and the time is 0-5 h. The ultrasonic treatment time is preferably 0.5-5 h, the ultrasonic treatment temperature is preferably 18-25 ℃, the stirring and dipping time is preferably 0-5 h, and the stirring and dipping temperature is preferably 40-80 ℃.
In the method, after the impregnation and loading of platinum, the hexagonal boron carbon nitrogen carrier is dried in inert gas, wherein the inert gas is preferably nitrogen, and the roasting time is preferably 2-20 h, more preferably 2-8 h. The drying temperature is preferably 500-700 ℃, and reduction is carried out after drying.
In the above method, the reduction may be carried out by using hydrogen. When hydrogen is used for reduction, the reduction temperature is preferably 500-600 ℃, and the reduction time is preferably 0.5-10 h.
The method for dehydrogenating the low-carbon alkane provided by the invention comprises the step of carrying out contact reaction on the low-carbon alkane and the catalyst under the dehydrogenation reaction condition. The dehydrogenation reaction temperature is 500-650 ℃, and the pressure is 0.1-0.5 MPa. The low-carbon alkane is C3-C5 alkane, such as propane, butane or pentane.
The invention has the remarkable advantages that:
the hexagonal boron carbon nitrogen nanosheet prepared by the invention is used as a carrier of a propane dehydrogenation catalyst, active metal Pt is loaded on the surface of the hexagonal boron carbon nitrogen nanosheet, active metal platinum atoms have stable properties at high temperature through the interaction between the hexagonal boron carbon nitrogen carrier and active metal and the strong carrier and metal, and the obtained catalyst is used for low-carbon alkane dehydrogenation reaction and has high activity and stability.
Drawings
FIG. 1 is an XRD pattern of hexagonal boron carbon nitride of the carrier of the invention.
FIG. 2 is an SEM image of hexagonal boron carbon nitrogen of the carrier of the invention.
Detailed Description
For further disclosure, but not limitation, the present invention is further described in detail below with reference to examples.
The invention is further illustrated below by way of examples, without being limited thereto.
Example 1
Preparation of the catalyst of the invention and evaluation of propane dehydrogenation Performance
(1) Preparation of the catalyst
1g of boric acid, 3g of melamine and 3g of glucose were thoroughly ground in an agate mortar. And then putting the mixed precursor into a horizontal tube furnace. Before heating, discharging all oxygen in the tube for about 30min, calcining at 950 ℃ for 6h, and washing the obtained product in hot water by using 0.1M HCl to obtain the hexagonal boron carbon nitrogen carrier. 0.5g of hexagonal boron carbon nitrogen carrier is taken and put into 5mL of chloroplatinic acid solution with 5mg/mL of Pt content and 5mL of ethanol. Stirring for 3h at 25 deg.C, ultrasonic treating for 3h, stirring for 3h, evaporating ethanol in the system at 80 deg.C, and drying at 80 deg.C overnight. Placing it in N2Calcining for 2h at 500 ℃ in the atmosphere to obtain the catalyst A. The platinum content of catalyst A, the ratio of boric acid, melamine and glucose used are shown in Table 1.
(2) Evaluation of catalyst Performance
0.2g of catalyst A was charged in a microreaction device and propane and N were added in a volume fraction of 5% based on propane2The mixture of (A) is used as a reaction raw material, the reaction is carried out for 10 hours under the conditions of 600 ℃, 0.1MPa and 1.8h < -1 > of propane feeding mass space velocity, the conversion rate of propane at the initial reaction and the selectivity value of propylene are calculated, and the reaction result is shown in Table 1. The results of the reaction for 10 hours are shown in Table 2.
Example 2
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1 except that the mass of glucose in the step (1) was 1g, and the content of platinum element in the obtained catalyst B, the ratio of boric acid, melamine and glucose used and the results of propane dehydrogenation reaction were shown in Table 1. The results of the reaction for 10 hours are shown in Table 3.
Example 3
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1 except that the mass of glucose in the step (1) was 2g, and the content of platinum element in the obtained catalyst C, the ratio of boric acid, melamine and glucose used and the reaction result of propane dehydrogenation were as shown in Table 1. The results of the reaction for 10 hours are shown in Table 4.
Example 4
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1 except that the mass of glucose in the step (1) was 6g, and the content of platinum element in the obtained catalyst D, the ratio of boric acid, melamine and glucose used and the reaction result of propane dehydrogenation were as shown in Table 1. The results of the reaction for 10 hours are shown in Table 5.
Example 5
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1 except that the mass of melamine in the step (1) was 2g, and the platinum element content, the ratio of boric acid, melamine and glucose used and the propane dehydrogenation reaction result in the catalyst E obtained were as shown in Table 1. The results of the reaction for 10 hours are shown in Table 6.
Example 6
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1 except that the mass of melamine in the step (1) was 1g, and the platinum element content in the obtained catalyst F, the ratio of boric acid, melamine and glucose used and the reaction results of propane dehydrogenation were shown in Table 1. The results of the reaction for 10 hours are shown in Table 7.
Comparative example 1
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1, except that no glucose was added in the step (1), and catalyst G was obtained in which the content of platinum element, the ratio of boric acid, melamine and glucose used and the results of propane dehydrogenation reaction were shown in Table 1.
Comparative example 2
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1, except that boric acid was not added in the step (1), and the catalyst H obtained had a platinum content, a ratio of boric acid, melamine and glucose used and propane dehydrogenation reaction results as shown in Table 1.
Comparative example 3
A catalyst was prepared and subjected to propane dehydrogenation according to the procedure of example 1, except that melamine was not added in the step (1), and catalyst I was obtained in which the content of platinum element, the ratio of boric acid, melamine and glucose used and the results of propane dehydrogenation are shown in Table 1.
Comparative example 4
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1 except that the calcination temperature in the step (1) was changed to 800 ℃ to obtain catalyst J having a platinum element content, a ratio of boric acid, melamine and glucose used and propane dehydrogenation reaction results as shown in Table 1.
Comparative example 5
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1, except that the calcination temperature in the step (1) was changed to 1100 deg.C, and the platinum element content, the ratio of boric acid, melamine and glucose used and the propane dehydrogenation reaction results were obtained as shown in Table 1.
Comparing the propane dehydrogenation performance of the catalysts prepared in the catalyst examples and the comparative examples, the catalyst prepared by using hexagonal boron carbon nitride and glucose prepared by the mass ratio of 3:1:3 and the calcining temperature of 950 ℃ as the carrier has the best propane dehydrogenation performance, and the dehydrogenation performance is higher than that of the catalyst prepared by using the carrier only containing boron carbon, boron nitrogen or carbon nitrogen and then loading platinum.
TABLE 1
TABLE 2
TABLE 3
TABLE 4
TABLE 5
TABLE 6
TABLE 7
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (4)
1. The application of a platinum catalyst taking hexagonal boron carbon nitride as a carrier in the direct dehydrogenation of low-carbon alkane is characterized in that: mixing a boron source, a nitrogen source and a carbon source according to a ratio, roasting at a high temperature in inert gas to obtain a hexagonal boron carbon nitrogen coarse body, washing with hydrochloric acid to obtain a hexagonal boron carbon nitrogen pure body, soaking with a platinum-containing compound solution, and finally drying in the inert gas and then reducing; obtaining the platinum catalyst taking hexagonal boron carbon nitrogen as a carrier; wherein the mass ratio of the carbon source to the boron source to the nitrogen source is 3:1: 3; the doping amount of the platinum is 5.0 percent of the weight of the carrier; the boron source used is boric acid; the nitrogen source used is melamine; the carbon source is glucose, wherein the high-temperature roasting temperature is 950 ℃, and the time is 2-20 hours; wherein the dipping by the platinum-containing compound solution is to adopt ultrasonic treatment firstly and then dip under stirring; the ultrasonic treatment temperature is 15-45 ℃, and the time is 0.5-5 h; the temperature during stirring is 20-100 ℃, and the time is 0-5 h;
The method for directly dehydrogenating the low-carbon alkane comprises the following steps: carrying out contact reaction on low-carbon alkane and a platinum catalyst taking hexagonal boron carbon nitrogen as a carrier under a dehydrogenation reaction condition; the reaction temperature is 500-650 ℃, and the pressure is 0.1-0.5 MPa; the lower alkane is propane, butane or pentane.
2. Use according to claim 1, characterized in that: the concentration of the hydrochloric acid used for washing is 0.5-1.5M.
3. Use according to claim 1, characterized in that: the platinum-containing compound is any one of platinum nitrate, chloroplatinic acid, potassium chloroplatinate, dichlorotetramine platinum or acetylacetone platinum; the platinum-containing compound solution is prepared by one or more solvents of deionized water, ethanol, acetone or isopropanol; the platinum content in the platinum-containing compound solution is 1-10 mg/mL.
4. Use according to claim 1, characterized in that: the reduction is carried out by adopting a reducing agent or reducing atmosphere hydrogen, and the reducing agent is selected from glycol and C1~C3Carboxylic acid or C1~C3Any one or more of the sodium carboxylates described above.
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