CN114522714B - Platinum-series catalyst with hydroxylated boron nitride as carrier and preparation method thereof - Google Patents
Platinum-series catalyst with hydroxylated boron nitride as carrier and preparation method thereof Download PDFInfo
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- CN114522714B CN114522714B CN202210277907.7A CN202210277907A CN114522714B CN 114522714 B CN114522714 B CN 114522714B CN 202210277907 A CN202210277907 A CN 202210277907A CN 114522714 B CN114522714 B CN 114522714B
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Abstract
The invention discloses a preparation method of a platinum catalyst taking hydroxylated boron nitride as a carrier. The method comprises the steps of treating a prepared boron nitride material by using a strong acid solution, and then roasting the boron nitride material in an inert gas at a high temperature to obtain a hydroxylated boron nitride carrier; then carrying out platinum and tin double loading on the platinum-containing compound solution and the tin-containing compound, drying in inert gas, and then reducing. The obtained catalyst is used for dehydrogenation reaction of low-carbon alkane and has higher activity. And the prior literature and patents do not find similar materials to be used in the direct dehydrogenation reaction of propane, so the method has very novel research significance.
Description
Technical Field
The invention belongs to the technical field of low-carbon alkane dehydrogenation catalysts, and particularly relates to a catalyst taking hydroxylated boron nitride as a carrier, and a preparation method and application thereof.
Background
With the large-scale development of shale gas in the united states, the dehydrogenation of propane to propylene is an industrial technology which has attracted much attention in recent years. With the development of dehydrogenation technology, the efficient adsorption/activation of propane on the surface of heterogeneous catalysts and the subsequent desorption of propylene remains a scientific challenge. Supported Pt and CrOx catalysts have been used as active catalysts for dehydrogenation reactions. However, problems of catalyst deactivation, high platinum value, chromium toxicity, etc. have prevented their widespread use. Therefore, the development of a novel dehydrogenation catalyst system with high efficiency, low cost and environmental friendliness is of great significance.
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. In recent years, more and more novel vectors have been extensively studied.
Disclosure of Invention
The invention aims to provide a preparation method of a platinum-based catalyst with hydroxylated boron nitride as a carrier, which adopts strong acid solution to treat a boron nitride material, bakes the boron nitride material at high temperature in inert gas, then carries out platinum and tin double loading, and has high catalytic activity and high selectivity when being applied to low-carbon alkane dehydrogenation reaction.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a platinum catalyst taking hydroxylated boron nitride as a carrier comprises the steps of dispersing a boron nitride material in a strong acid solution, and preparing the hydroxylated boron nitride carrier through acidification, centrifugation, washing, drying and calcination; and carrying out platinum loading on the platinum-containing precursor solution, carrying out tin loading on the tin-containing precursor solution, and then reducing to obtain the catalyst, namely the platinum-based catalyst taking the hydroxylated boron nitride as the carrier.
Preferably, the loading amount of the platinum accounts for 0 to 5 percent of the total weight of the catalyst and is not 0; the loading amount of the tin accounts for 0 to 5 percent of the total weight of the catalyst, and is not 0.
Preferably, the strong acid solution is one or more of nitric acid, sulfuric acid, hydrochloric acid, nitrous acid.
Preferably, the temperature in the acidification process is 25-100 ℃, and the acidification time is 1-10 h.
Preferably, the calcination is carried out for 1 to 5 hours at the temperature of 300 to 900 ℃ in an inert gas atmosphere; the inert gas is argon, nitrogen or helium.
Preferably, the platinum-containing precursor is platinum nitrate, chloroplatinic acid, potassium chloroplatinate, platinum tetraammine dichloride or platinum acetylacetonate; the platinum-containing precursor solution is prepared by one or more solvents of deionized water, ethanol, acetone or isopropanol.
Preferably, the tin-containing precursor is stannic chloride, stannic acetate, stannic tetrachloride, stannous sulfate or trichloromethyl tin; the tin-containing precursor solution is prepared by one or more solvents of deionized water, ethanol, methanol or isopropanol.
Preferably, the platinum load and the tin load are both treated by stirring and ultrasonic treatment, and then treated by stirring and dipping; the ultrasonic treatment time is 0.5 to 5 hours, and the stirring and dipping time is 0 to 5 hours.
Preferably, the reduction is carried out by adopting a reducing agent or hydrogen in a reducing atmosphere, the reducing agent is any one or more of ethylene glycol, C1-C3 carboxylic acid or C1-C3 sodium carboxylate, and when hydrogen is used for reduction, the reduction temperature is 500-600 ℃, and the reduction time is 0.5-10 h.
The platinum-based catalyst taking the hydroxylated boron nitride as the carrier can be used for dehydrogenation of low-carbon alkane, and 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 to 650 ℃, and the pressure is 0.1 to 0.5 MPa. The low-carbon alkane is C3-C5 alkane, such as propane, butane or pentane.
Drawings
FIG. 1 is an XRD pattern of a support hydroxylated boron nitride of the invention.
Detailed Description
The method comprises the steps of dispersing a boron nitride material in a strong acid solution, and preparing a hydroxylated boron nitride carrier through acidification, centrifugation, washing, drying and calcination; and carrying out platinum loading on the platinum-containing precursor solution, carrying out tin loading on the tin-containing precursor solution, and reducing the platinum-containing precursor solution by using a reducing agent or hydrogen to prepare the catalyst, thus obtaining the platinum-based catalyst taking the hydroxylated boron nitride as the carrier. The obtained catalyst is used for dehydrogenation reaction of low-carbon alkane, and has high activity and selectivity. The load capacity of the platinum accounts for 0 to 5 percent of the total weight of the catalyst; the loading amount of the tin accounts for 0 to 5 percent of the total weight of the catalyst.
The added strong acid solution is one or more of nitric acid, sulfuric acid, hydrochloric acid and nitrous acid.
The temperature in the acidification process is 25-100 ℃, and the acidification time is 1-10 h.
The calcining process is calcining for 1 to 5 hours at the temperature of 300 to 900 ℃ in an inert gas atmosphere; the inert gas is argon, nitrogen or helium.
The platinum-containing precursor is platinum nitrate, chloroplatinic acid, potassium chloroplatinate, dichlorotetramine platinum or acetylacetone platinum.
The platinum-containing precursor solution is prepared by one or more solvents of deionized water, ethanol, acetone or isopropanol.
The tin-containing precursor is stannic chloride, stannic acetate, stannic tetrachloride, stannous sulfate or trichloromethyl tin.
The tin-containing precursor solution is prepared by one or more solvents of deionized water, ethanol, methanol or isopropanol.
The platinum and tin load is firstly treated by stirring and ultrasonic wave and then treated by stirring and dipping; the ultrasonic treatment time is preferably 0.5 to 5 hours, and the stirring and soaking time is preferably 0 to 5 hours.
The reduction is carried out by adopting a reducing agent or reducing atmosphere hydrogen, and the reducing agent is selected from glycol and C 1 ~C 3 Carboxylic acid or C 1 ~C 3 Any one or more of the sodium carboxylates. When hydrogen is used for reduction, the reduction temperature is preferably 500 to 600 ℃, and the reduction time is preferably 0.5 to 10 hours.
The invention provides a method for dehydrogenating low-carbon alkane, and a packageThe method comprises the step of contacting and reacting the low-carbon alkane with the catalyst under the dehydrogenation reaction condition. The dehydrogenation reaction temperature is 500 to 650 ℃, and the pressure is 0.1 to 0.5 MPa. The lower alkane is C 3 ~C 5 Such as propane, butane or pentane.
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
Adding boric acid and melamine into 80 mL of methanol aqueous solution according to the mass ratio of 1. And (3) placing the precursor in a tube furnace, heating to 950 ℃, preserving heat for 6 h, cooling the tube furnace, taking out a sample, and grinding to obtain the white BN carrier.
2 g of boron nitride were stirred in a 500 mL round bottom flask with 200 mL of 65% nitric acid for 3 h at room temperature. The diluted mixture was then filtered and washed with excess deionized water until the pH reached 7, and the resulting sample was dried at 120 ℃ overnight and N 2 Roasting for 2h at 700 ℃ in the atmosphere. Weighing 0.5 g of the prepared hydroxylated boron nitride carrier, putting the carrier into 5 mL of chloroplatinic acid solution with Pt content of 5 mg/mL and 15 mL of ethanol, firstly stirring for 1 h at 25 ℃, carrying out ultrasonic treatment for 3 h, adding 3 mL of stannic chloride solution with Sn content of 5 mg/mL, stirring for 1 h, completely evaporating the ethanol in the system at 80 ℃, putting the system into N 2 Calcining at 550 ℃ for 2h in the atmosphere. Then reducing for 1 h at 580 ℃ under the hydrogen atmosphere to obtain the catalyst A. In catalyst A, the platinum loading was 5 wt%; tin loading was 3 wt%.
(2) Evaluation of catalyst Performance
Filling 0.2 g of catalyst A in a micro-reactor, taking a mixture of propane and nitrogen with the volume fraction of 5 percent of propane as a reaction raw material, and feeding propane at the temperature of 600 ℃, the pressure of 0.1 MPa and the mass space velocity of 1.8 h -1 Under the conditions of (1) dehydrogenation reaction10 The performance data in h are shown in Table 1.
Example 2
A catalyst B having a platinum loading of 5 wt% and a tin loading of 3 wt% was prepared by preparing a catalyst and performing a propane dehydrogenation reaction according to the procedure of example 1, except that 200 mL of 98% sulfuric acid was used in the step (1).
The performance data over 10 h of the reaction are shown in Table 2.
Example 3
A catalyst was prepared and subjected to propane dehydrogenation reaction in the same manner as in example 1, except that 200 mL of deionized water was used in the step (1). In the catalyst C obtained, the amount of platinum supported was 5 wt% and the amount of tin supported was 3 wt%.
The performance data in 10 h of the reaction are shown in Table 3.
Comparative example 1
A catalyst was prepared as in example 1, except that the sample obtained in step (1) was dried at 120 ℃ overnight and then subjected to N 2 No calcination was carried out in the atmosphere, and the platinum loading in the prepared catalyst D was 5 wt%, and the tin loading was 3 wt%.
The propane conversion after 0.5 h of reaction was 34.75%.
Comparative example 2
A catalyst was prepared as in example 1, except that the sample obtained in step (1) was dried at 120 ℃ overnight under N 2 Roasting for 2h at 900 ℃ in the atmosphere to obtain the catalyst E, wherein the platinum loading capacity is 5 wt%, and the tin loading capacity is 3 wt%.
The propane conversion after 0.5 h of reaction was 29.96%.
Comparative example 3
A catalyst was prepared as in example 1, except that in step (1) 2 g of boron nitride nanotubes were stirred in a 500 mL round bottom flask with 200 mL of 65% nitric acid at room temperature for 1 h, resulting in catalyst F with 5 wt% platinum and 3 wt% tin loading.
The propane conversion after 0.5 h of reaction was 35.78%.
Comparative example 4
A catalyst was prepared as in example 1 except that in step (1) 2G of boron nitride nanotubes were stirred in a 500 mL round bottom flask with 200 mL of 65% nitric acid at room temperature for 6 h to produce catalyst G with a platinum loading of 5 wt% and a tin loading of 3 wt%.
The conversion of propane after 0.5 h of reaction was 38.79%.
Comparative example 5
A catalyst was prepared as in example 1, except that after the hydroxylated boron nitride support obtained in step (1) was obtained, no further tin was loaded, and catalyst H was prepared with a platinum loading of 5 wt% and a tin loading of 0wt%.
The conversion of propane after 0.5 h of reaction was 12.18%.
Comparative example 6
A catalyst was prepared as in example 1, except that no platinum was loaded after the hydroxylated boron nitride support was obtained in step (1), and catalyst I was prepared with a platinum loading of 0wt% and a tin loading of 3 wt%.
The conversion of propane after 0.5 h of reaction was 5.78%.
Comparing the propane dehydrogenation performance of the catalysts prepared in the catalyst examples and the comparative examples, the catalyst has the advantages that the hydroxylated boron nitride carrier obtained by treating the boron nitride material with strong acid has very high catalytic performance after being loaded with platinum and tin metals, the best catalytic performance can be achieved when the strong acid solution is 65% concentrated nitric acid, the roasting temperature is 700 ℃, and the acidification time is 3 hours, and the dehydrogenation performance of the catalyst is higher than that of the catalyst which is not treated and is loaded with the same metals.
From comparative examples 1 and 2, it can be seen that the calcination temperature has some effect on the hydroxylated boron nitride catalyst. The data show that the catalytic performance of the catalyst after roasting treatment is superior to that of the catalyst without roasting treatment, because the unstable oxygen-containing functional group on the surface of the carrier is decomposed by high-temperature roasting, the active site is more stable, and the pore structure of BNOH can be changed after roasting, which is beneficial to the release of propylene from a pore system. When the calcination temperature reaches 900 ℃, the initial activity of the catalyst is reduced, because the excessive temperature can affect the deposition rate of-OH on the surface of boron nitride, and the deposition rate is far greater than the generation rate of active sites, thereby inactivating the catalyst. From comparative examples 3 and 4, the effect of acid treatment time on catalyst performance was examined. The data show that as the acid treatment time increases, the reaction progresses, and the number of active sites for B-OH produced increases, thereby increasing the propane conversion. And as can be seen from the data of comparative example 4, the catalytic activity is not greatly influenced after the acid treatment time is prolonged to 6 hours, which indicates that the active sites are saturated, and the introduction of hydroxyl is no longer a main factor influencing the catalytic activity.
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 (7)
1. A preparation method of a platinum catalyst taking hydroxylated boron nitride as a carrier is characterized by comprising the following steps: dispersing a boron nitride material in a strong acid solution, and preparing a hydroxylated boron nitride carrier through acidification, centrifugation, washing, drying and calcination; carrying out platinum loading on the platinum-containing precursor solution, carrying out tin loading on the tin-containing precursor solution, and then reducing to obtain a catalyst, namely the platinum-based catalyst taking the hydroxylated boron nitride as a carrier;
the load amount of the platinum accounts for 0 to 5 percent of the total weight of the catalyst and is not 0; the loading amount of the tin accounts for 0 to 5 percent of the total weight of the catalyst and is not 0;
the strong acid solution is nitric acid; the calcination is carried out for 2h at 700 ℃ in an inert gas atmosphere; the inert gas is argon, nitrogen or helium.
2. The preparation method according to claim 1, wherein the temperature in the acidification process is 25-100 ℃, and the acidification time is 1-10 h.
3. The preparation method according to claim 1, wherein the platinum-containing precursor is platinum nitrate, chloroplatinic acid, potassium chloroplatinate, tetraammineplatinum dichloride or platinum acetylacetonate; the platinum-containing precursor solution is prepared from one or more solvents of deionized water, ethanol, acetone or isopropanol.
4. The preparation method according to claim 1, wherein the tin-containing precursor is tin chloride, tin acetate, tin tetrachloride, stannous sulfate, or trichloromethyl tin; the tin-containing precursor solution is prepared by one or more solvents of deionized water, ethanol, methanol or isopropanol.
5. The preparation method according to claim 1, wherein the platinum load and the tin load are both treated by stirring and ultrasonic treatment, and then treated by stirring and dipping; the ultrasonic treatment time is 0.5 to 5 hours, and the stirring and soaking time is 0 to 5 hours.
6. The method of claim 1, wherein the reduction is carried out with a reducing agent selected from the group consisting of ethylene glycol and C, or with hydrogen in a reducing atmosphere 1 ~C 3 Carboxylic acid or C 1 ~C 3 When reducing with hydrogen, the reducing temperature is 500 to 600 ℃, and the reducing time is 0.5 to 10 hours.
7. A platinum-based catalyst supported on hydroxylated boron nitride obtained by the process according to any one of claims 1 to 6.
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| CN109692713A (en) * | 2019-01-25 | 2019-04-30 | 福州大学 | A kind of catalyst for dehydrogenation of low-carbon paraffin and the preparation method and application thereof |
| CN109939719A (en) * | 2019-04-16 | 2019-06-28 | 中国科学技术大学 | A kind of modified boron nitride nanometer material of hydroxylating, preparation method and application |
| CN113058632A (en) * | 2021-03-26 | 2021-07-02 | 福州大学 | Platinum-series catalyst with hexagonal boron carbon nitride as carrier and preparation method thereof |
| CN114192180A (en) * | 2021-12-31 | 2022-03-18 | 上海大学 | Modified boron nitride loaded nickel-based methane dry reforming catalyst, and preparation method and application thereof |
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| CN109692713A (en) * | 2019-01-25 | 2019-04-30 | 福州大学 | A kind of catalyst for dehydrogenation of low-carbon paraffin and the preparation method and application thereof |
| CN109939719A (en) * | 2019-04-16 | 2019-06-28 | 中国科学技术大学 | A kind of modified boron nitride nanometer material of hydroxylating, preparation method and application |
| CN113058632A (en) * | 2021-03-26 | 2021-07-02 | 福州大学 | Platinum-series catalyst with hexagonal boron carbon nitride as carrier and preparation method thereof |
| CN114192180A (en) * | 2021-12-31 | 2022-03-18 | 上海大学 | Modified boron nitride loaded nickel-based methane dry reforming catalyst, and preparation method and application thereof |
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| Title |
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| Yi Wang et al.，.γ-Radiation synthesis of ultrasmall noble metal (Pd, Au, Pt) nanoparticles embedded on boron nitride nanosheets for high-performance catalysis.《Ceramics International》.2021,第47卷第26963–26970页. * |
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