CN113600233B - Metal-doped palladium molecular sieve catalyst, and preparation method and application thereof - Google Patents

Metal-doped palladium molecular sieve catalyst, and preparation method and application thereof Download PDF

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CN113600233B
CN113600233B CN202111016544.3A CN202111016544A CN113600233B CN 113600233 B CN113600233 B CN 113600233B CN 202111016544 A CN202111016544 A CN 202111016544A CN 113600233 B CN113600233 B CN 113600233B
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molecular sieve
mixture
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sieve catalyst
rotary mixing
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CN113600233A (en
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郑琴
庞磊
王睿
杨帆
刘诗逸
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Dongfeng Commercial Vehicle Co Ltd
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Abstract

The application relates to the technical field of automobile exhaust treatment, in particular to a metal-doped palladium molecular sieve catalyst, and a preparation method and application thereof. The preparation method of the metal-doped palladium molecular sieve catalyst comprises the following steps: placing a molecular sieve and a first metal salt in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing carrier gas to continue to perform rotary mixing to obtain a first mixture; the first metal salt is palladium salt; adding a second metal salt into the first mixture, carrying out rotary mixing and vacuumizing, and continuously carrying out rotary mixing after carrier gas is introduced to obtain a second mixture; and calcining the second mixture to obtain the metal-doped palladium molecular sieve catalyst. The molecular sieve catalyst obtained by the preparation method provided by the application has uniform particle distribution and excellent catalytic performance.

Description

Metal-doped palladium molecular sieve catalyst, and preparation method and application thereof
Technical Field
The application relates to the technical field of automobile exhaust treatment, in particular to a metal-doped palladium molecular sieve catalyst, and a preparation method and application thereof.
Background
Nitrogen oxides NO emitted by combustion of diesel engines x Can cause adverse effects on human health and environment, and reduce nitrogen oxide NO along with increasing tightening of national emission regulations x Becomes an important social problem.
Currently, selective catalytic reduction of SCR and NO x The storage reduction NSR technology has been successfully used to reduce NOx NO in diesel vehicles x And (4) discharging. Selective catalytic reduction of SCR and NO at operating temperatures above 200 DEG C x The storage reduction NSR technology can effectively reduce NO x . However, during cold start of vehicle operation, exhaust temperatures are well below 200 ℃, at which time the NSR catalyst is unable to oxidize NO to NO 2 Urea cannot be completely decomposed to NH in SCR systems 3 To convert NO x Resulting in selective catalytic reduction of SCR and NO x The storage reduction NSR technique fails.
In order to solve the problem of the above two technologies failing during the cold start of vehicle operation, researchers have developed passive NOx adsorbers PNA, which are generally used as the adsorbing material in two categories: (1) noble metal supported rare earth oxides; (2) The noble metal loaded molecular sieve material has wide application of Pd loaded molecular sieve catalyst, and the method for preparing the adsorbing material mainly comprises an impregnation method and an ion exchange method, wherein the impregnation method has the defects of incomplete exchange, uneven distribution of catalyst particles and poor catalytic performance; the ion exchange method has the disadvantages of long period and complicated steps.
Based on the above analysis, it is very important to provide a method for preparing a molecular sieve catalyst with uniform particle distribution and excellent catalytic performance.
Disclosure of Invention
The embodiment of the application provides a preparation method of a metal-doped palladium molecular sieve catalyst, and the molecular sieve catalyst obtained by the preparation method is uniform in particle distribution and excellent in catalytic performance.
In a first aspect, an embodiment of the present application provides a preparation method of a metal-doped palladium molecular sieve catalyst, including the following steps:
s101, placing a molecular sieve and a first metal salt in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing carrier gas to continue to perform rotary mixing to obtain a first mixture; the first metal salt is palladium salt;
step S102, adding a second metal salt into the first mixture, carrying out rotary mixing and vacuumizing, and continuously carrying out rotary mixing after carrier gas is introduced to obtain a second mixture;
and step S103, calcining the second mixture to obtain the metal-doped palladium molecular sieve catalyst.
In some examples, the molecular sieve in step S101 is SAPO-18 molecular sieve.
In some embodiments, in step S101, palladium chloride is used as the palladium salt.
In some embodiments, in steps S101 and S102, the carrier gas is a mixture of argon and oxygen, and the flow rate of the carrier gas is 600mL/min; the carrier gas does not damage the structure of the carrier molecular sieve, the oxygen plasma can activate the surface of the molecular sieve, and the argon plasma generates etching action on the surface of the molecular sieve, so that the surface of the particles becomes rough, fine pits and gullies are formed, and the specific surface area is increased.
In some embodiments, the second metal salt is selected from a chloride salt or a nitrate salt of any one or more of chromium (Cr), iron (Fe), nickel (Ni), copper (Cu), zinc (Zn), barium (Ba), cobalt (Co), manganese (Mn), tin (Sn), and the like.
In some embodiments, the temperature of the calcination in step S103 is 450-650 ℃.
In some embodiments, the metal-doped palladium molecular sieve catalyst has a palladium content to molecular sieve mass ratio of 0.5% to 2%:1.
in some embodiments, in the metal-doped palladium molecular sieve catalyst, the mass ratio of the doping amount of the metal in the second metal salt to the molecular sieve is 0.3% -1.5%:1.
In a second aspect, the embodiments of the present application provide a metal-doped palladium molecular sieve catalyst prepared by the above preparation method.
In a third aspect, embodiments of the present application provide an application of the metal-doped palladium molecular sieve catalyst, where the metal-doped palladium molecular sieve catalyst can be used for adsorbing nitrogen oxides in automobile exhaust.
The method provided by the application adopts a plasma method to prepare the metal-loaded and palladium-loaded molecular sieve catalyst, the plasma is in a fourth form except a gaseous state, a liquid state and a solid state, and is generated by applying sufficient energy to gas under a certain pressure condition by using a high-voltage power supply.
The beneficial effect that technical scheme that this application provided brought includes: the preparation method provided by the application is simple and feasible, and can realize 360-degree dead-angle-free plasma treatment by adopting plasma equipment to rotationally mix the molecular sieve, the palladium salt and the second metal salt, so that the problems of incomplete and uneven treatment of a powder sample are solved, the thorough mixing of all components is ensured, the catalyst particles are uniformly distributed, and the catalyst has an excellent adsorption effect on nitrogen oxides; the molecular sieve catalyst prepared by the preparation method provided by the application has excellent high thermal stability, low temperature performance and hydrothermal stability.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic flow diagram of a process for preparing a metal-doped palladium molecular sieve catalyst provided in an embodiment of the present application;
FIG. 2 is a scanning electron microscope image of PdZn-SAPO-18 catalyst prepared in example 5 of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The embodiment of the application provides a preparation method of a metal-doped palladium molecular sieve catalyst, and the molecular sieve catalyst obtained by the preparation method is uniform in particle distribution and excellent in catalytic performance.
Fig. 1 is a schematic flow diagram of a method of making a metal-doped palladium molecular sieve catalyst provided herein, and with reference to fig. 1, the method of making provided herein comprises the steps of:
s101, placing a molecular sieve and a first metal salt in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing a mixture of argon and oxygen at a gas flow rate of 600mL/min to continue to perform rotary mixing for 10-15min to obtain a first mixture; wherein the first metal salt is palladium chloride; the molecular sieve is SAPO-18 molecular sieve; after argon and oxygen are introduced, oxygen plasma and argon plasma are excited, the oxygen plasma can activate the surface of the molecular sieve, and the argon plasma generates an etching effect on the surface of the molecular sieve, so that the surface of particles becomes rough, fine pits and ravines are formed, and the specific surface area is increased;
step S102, adding a second metal salt into the first mixture, carrying out rotary mixing and vacuum pumping, introducing a mixture of argon and oxygen at a gas flow rate of 600mL/min, and continuously carrying out rotary mixing for 10-15min to obtain a second mixture; the second metal salt is selected from chloride or nitrate of any one or more of chromium (Cr), iron (Fe), nickel (Ni), copper (Cu), zinc (Zn), barium (Ba), cobalt (Co), manganese (Mn), tin (Sn) and the like;
step S103, calcining the second mixture at the temperature of 450-650 ℃ to obtain a metal-doped palladium molecular sieve catalyst; in the metal-doped palladium molecular sieve catalyst, the doping amount of Pd is 0.5-2wt% and the doping amount of metal in the second metal salt is 0.3-1.5wt% based on the mass of the molecular sieve.
The metal-doped palladium molecular sieve catalyst and the preparation method thereof provided by the present application are described in detail below with reference to examples.
Example 1:
embodiment 1 of the present application provides a preparation method of a PdCr-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 5g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, adding 0.125g of chromium nitrate Cr (NO) to the first mixture 3 ) 3 Rotating, mixing, vacuumizing, introducing argon and oxygen at a gas flow of 600mL/min, and continuously rotating and mixing for 12min to obtain a second solutionMixing;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdCr-SAPO-18 molecular sieve catalyst.
Example 2:
embodiment 2 of the present application provides a preparation method of a PdFe-SAPO-18 molecular sieve catalyst, which comprises the following steps:
step S101, mixing 5g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 12min to obtain a first mixture;
in step S102, 0.055g of iron nitrate Fe (NO) was added to the first mixture 3 ) 3 Carrying out rotary mixing and vacuum pumping, and introducing argon and oxygen at the gas flow of 600mL/min to continue to carry out rotary mixing for 10min to obtain a second mixture;
and step S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdFe-SAPO-18 molecular sieve based catalyst.
Example 3:
embodiment 3 of the present application provides a method for preparing a PdNi-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 5g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continuously perform rotary mixing for 10min to obtain a first mixture;
step S102, 0.085g of nickel nitrate Ni (NO) was added to the first mixture 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 15min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdNi-SAPO-18 molecular sieve catalyst.
Example 4:
embodiment 4 of the present application provides a preparation method of a PdCu-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 5g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continuously perform rotary mixing for 13min to obtain a first mixture;
in step S102, 0.115g of copper nitrate Cu (NO) is added to the first mixture 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 15min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdCu-SAPO-18 molecular sieve catalyst.
Example 5:
embodiment 5 of the present application provides a preparation method of a PdZn-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 5gH-SAPO-18 molecular sieve and 1gPdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 12min to obtain a first mixture;
step S102, 0.076g of zinc nitrate Zn (NO) is added to the first mixture 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 14min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdZn-SAPO-18 molecular sieve catalyst.
The scanning electron microscope images of the PdZn-SAPO-18 molecular sieve catalyst prepared in example 5 under different times are shown in FIG. 2, pd and Zn are loaded on the surface of the SAPO-18 molecular sieve catalyst in oxide form, and as can be seen from FIG. 2a and FIG. 2b, the palladium oxide and the zinc oxide are uniformly dispersed, the particle size is smaller, and the doping of the auxiliary metal does not affect the framework structure of the molecular sieve.
Example 6:
embodiment 6 of the present application provides a preparation method of a PdBa-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, 0.085g of barium nitrate Ba (NO) is added to the first mixture 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdBa-SAPO-18 molecular sieve catalyst.
The molecular sieve catalysts prepared in examples 1 to 6 were evaluated for nitrogen oxide adsorption performance by the following methods: 200mg of the molecular sieve catalysts prepared in examples 1 to 6 were charged into a reactor, respectively, to investigate the adsorption and desorption properties of the catalysts on nitrogen oxides NOx; charging into the reactor 5% 2 、10％H 2 O and N 2 The reaction space velocity is 30000h -1 Pretreating for 30min, introducing 300ppmNO at different temperatures x Carrying out NO x Storage of NO x After a period of storage, NO is switched off x And (3) carrying out gas flow and temperature programmed desorption, and obtaining the results shown in table 1.
Table 1: examples 1-6 adsorption and desorption performance of nitrogen oxides by molecular sieve catalysts prepared in examples 1
Examples Adsorption amount (. Mu. Mol. G) -1 ) Desorption amount (. Mu. Mol. G) -1 )
Example 1 72 67
Example 2 58 50
Example 3 65 60
Example 4 60 51
Example 5 82 76
Example 6 74 65
As can be seen from table 1, the molecular sieve catalysts prepared in examples 1 to 6 have good adsorption and desorption properties for nitrogen oxides, and are suitable for use as the adsorption material of the passive NOx adsorber PNA.
Example 7:
embodiment 7 of the present application provides a preparation method of a PdCo-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, adding into the first mixture0.065g of cobalt nitrate Co (NO) was added 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 12min to obtain a second mixture;
and S103, calcining the second mixture at 500 ℃ for 5 hours to obtain the PdCo-SAPO-18 molecular sieve catalyst.
Example 8:
embodiment 8 of the present application provides a preparation method of a PdMn-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continuously perform rotary mixing for 13min to obtain a first mixture;
in step S102, 0.075g of manganese nitrate Mn (NO) is added to the first mixture 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 12min to obtain a second mixture;
and step S103, calcining the second mixture for 5 hours at 450 ℃ to obtain the PdMn-SAPO-18 molecular sieve based catalyst.
Example 9:
embodiment 9 of the present application provides a preparation method of a PdSn-SAPO-18 molecular sieve catalyst, which comprises the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, 0.065g of tin (Sn) Nitrate (NO) is added to the first mixture 3 ) 4 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdSn-SAPO-18 molecular sieve catalyst.
Example 10:
embodiment 10 of the present application provides a preparation method of a PdFe-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 12min to obtain a first mixture;
step S102, adding 0.08g of FeCl into the first mixture 3 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 12min to obtain a second mixture;
and S103, calcining the second mixture at 580 ℃ for 5 hours to obtain the PdFe-SAPO-18 molecular sieve catalyst.
Example 11:
embodiment 11 of the present application provides a preparation method of a PdCu-SAPO-18 molecular sieve catalyst, comprising the steps of:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continuously perform rotary mixing for 13min to obtain a first mixture;
step S102, adding 0.095g of copper chloride (CuCl) to the first mixture 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 15min to obtain a second mixture;
and S103, calcining the second mixture at 560 ℃ for 5 hours to obtain the PdCu-SAPO-18 molecular sieve catalyst.
Example 12:
embodiment 12 of the present application provides a preparation method of a PdCo-SAPO-18 molecular sieve catalyst, including the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing in a cavity of a plasma device, mixing while rotating, vacuumizing, and introducing argon and oxygen at a gas flow rate of 600mL/minContinuously rotating and mixing for 15min to obtain a first mixture;
step S102, 0.085g of cobalt chloride CoCl was added to the first mixture 2 Carrying out rotary mixing and vacuum pumping, and introducing argon and oxygen at the gas flow of 600mL/min to continue to carry out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 560 ℃ for 5 hours to obtain the PdCo-SAPO-18 molecular sieve catalyst.
Example 13:
embodiment 13 of the present application provides a method for preparing a PdMn-SAPO-18 molecular sieve catalyst, comprising the steps of:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, adding 0.045g MnCl into the first mixture 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 15min to obtain a second mixture;
and S103, calcining the second mixture at 580 ℃ for 5 hours to obtain the PdMn-SAPO-18 molecular sieve catalyst.
Example 14:
embodiment 14 of the present application provides a method for preparing a pdbai-SAPO-18 molecular sieve catalyst, comprising the steps of:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, 0.055g of barium nitrate Ba (NO) was added to the first mixture 3 ) 2 0.025g of Ni (NO) nitrate 3 ) 2 Carrying out rotary mixing and vacuum pumping, and introducing argon and oxygen at the gas flow of 600mL/min to continue to carry out rotary mixing for 10min to obtain a second mixture;
and step S103, calcining the second mixture for 5 hours at the temperature of 600 ℃ to obtain the PdBaNi-SAPO-18 molecular sieve based catalyst.
Example 15:
embodiment 15 of the present application provides a preparation method of a PdZnNi-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, 0.035g of zinc nitrate Zn (NO) is added to the first mixture 3 ) 2 And 0.045g of nickel nitrate Ni (NO) 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and step S103, calcining the second mixture for 5 hours at 570 ℃ to obtain the PdZnNi-SAPO-18 molecular sieve catalyst.
Example 16:
embodiment 16 of the present application provides a preparation method of a pdcrccu-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, adding 0.025g of chromium nitrate Cr (NO) to the first mixture 3 ) 2 0.065g of Cu (NO) copper nitrate 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 580 ℃ for 5 hours to obtain the PdCrCu-SAPO-18 molecular sieve catalyst.
Example 17:
embodiment 17 of the present application provides a preparation method of a PdZnCu-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, 0.055g of CuCl was added to the first mixture 2 And 0.035g of ZnCl 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture for 5 hours at 590 ℃ to obtain the PdZnCu-SAPO-18 molecular sieve catalyst.
Example 18:
an embodiment 18 of the present application provides a preparation method of a PdCoCu-SAPO-18 molecular sieve catalyst, including the steps of:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, adding 0.025g of cobalt nitrate Co (NO) to the first mixture 3 ) 2 And 0.035g of Cu (NO) copper nitrate 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 12min to obtain a second mixture;
and step S103, calcining the second mixture for 5 hours at 585 ℃ to obtain the PdCoCu-SAPO-18 molecular sieve catalyst.
Example 19:
embodiment 19 of the present application provides a preparation method of a PdCrNi-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing in a cavity of a plasma device, rotating and mixing while vacuumizing, and introducing argon at a gas flow rate of 600mL/minContinuously rotating and mixing the gas and the oxygen for 15min to obtain a first mixture;
step S102, adding 0.055g of chromium chloride CrCl into the first mixture 2 And 0.035g of nickel chloride NiCl 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdCrNi-SAPO-18 molecular sieve catalyst.
Example 20:
embodiment 20 of the present application provides a preparation method of a PdCrCo-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
in step S102, 0.075g of chromium nitrate Cr (NO) is added to the first mixture 3 ) 2 0.025g of cobalt nitrate Co (NO) 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and step S103, calcining the second mixture at 565 ℃ for 5 hours to obtain the PdCrCo-SAPO-18 molecular sieve based catalyst.
Example 21:
embodiment 21 of the present application provides a preparation method of a PdNiSn-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, adding 0.025g of nickel nitrate Ni (NO) to the first mixture 3 ) 2 And 0.05g of tin nitrate Sn (NO) 3 ) 4 Rotating, mixing, vacuumizing at 600mL/minIntroducing argon and oxygen into the gas flow, and continuously rotating and mixing for 10min to obtain a second mixture;
and step S103, calcining the second mixture for 5 hours at 580 ℃ to obtain the PdNiSn-SAPO-18 molecular sieve catalyst.
Example 22:
embodiment 22 of the present application provides a preparation method of a PdZnFe-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
in step S102, 0.085g of zinc nitrate Zn (NO) was added to the first mixture 3 ) 2 0.015g of Fe (NO) nitrate 3 ) 3 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and step S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdZnFe-SAPO-18 molecular sieve catalyst.
Example 23:
embodiment 23 of the present application provides a method for preparing a PdCoCu-SAPO-18 molecular sieve catalyst, comprising the steps of:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
in step S102, 0.035g of copper nitrate Cu (NO) was added to the first mixture 3 ) 2 And 0.055g of cobalt nitrate Co (NO) 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdCoCu-SAPO-18 molecular sieve catalyst.
Example 24:
embodiment 24 of the present application provides a method for preparing a PdCoMn-SAPO-18 molecular sieve catalyst, comprising the steps of:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, adding 0.025g of cobalt nitrate Co (NO) to the first mixture 3 ) 2 And 0.065g of manganese Mn Nitrate (NO) 3 ) 2 Carrying out rotary mixing and vacuum pumping, and introducing argon and oxygen at the gas flow of 600mL/min to continue to carry out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdCOMN-SAPO-18 molecular sieve catalyst.
Example 25:
embodiment 25 of the present application provides a preparation method of a PdZnCr-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
in step S102, 0.05g of zinc nitrate Zn (NO) is added to the first mixture 3 ) 2 0.02g of chromium nitrate Cr (NO) 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and step S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdZnCr-SAPO-18 molecular sieve based catalyst.
Example 26:
embodiment 26 of the present application provides a preparation method of a PdNiSn-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, 10gH-SAPO-18 minutesSub-sieves and 1gPdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, 0.055g of nickel nitrate Ni (NO) was added to the first mixture 3 ) 2 And 0.035g of tin nitrate Sn (NO) 3 ) 4 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdNiSn-SAPO-18 molecular sieve catalyst.
Example 27:
embodiment 27 of the present application provides a preparation method of a PdZnMn-SAPO-18 molecular sieve catalyst, comprising the following steps:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102, 0.02g of zinc nitrate Zn (NO) is added to the first mixture 3 ) 2 And 0.04g of manganese nitrate Mn (NO) 3 ) 2 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 550 ℃ for 5 hours to obtain the PdZnMn-SAPO-18 molecular sieve catalyst.
Example 28:
embodiment 28 of the present application provides a method for preparing a PdBaSn-SAPO-18 molecular sieve catalyst, comprising the steps of:
step S101, mixing 10g of H-SAPO-18 molecular sieve and 1g of PdCl 2 Placing the mixture in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing argon and oxygen at the gas flow of 600mL/min to continue to perform rotary mixing for 15min to obtain a first mixture;
step S102To the first mixture was added 0.035g of barium nitrate Ba (NO) 3 ) 2 And 0.04g of tin nitrate Sn (NO) 3 ) 4 Carrying out rotary mixing and vacuum pumping, introducing argon and oxygen at the gas flow of 600mL/min, and continuously carrying out rotary mixing for 10min to obtain a second mixture;
and S103, calcining the second mixture at 600 ℃ for 5 hours to obtain the PdBaSn-SAPO-18 molecular sieve catalyst.
In the description of the present specification, reference to the description of "one embodiment/mode", "some embodiments/modes", "example", "specific example" or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment/mode or example is included in at least one embodiment/mode or example of the present application. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment/mode or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/aspects or examples and features of the various embodiments/aspects or examples described in this specification can be combined and combined by one skilled in the art without conflicting therewith.
It is noted that, in the present application, relational terms such as "first" and "second", and the like, are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising a," "8230," "8230," or "comprising" does not exclude the presence of additional like elements in a process, method, article, or apparatus that comprises the element. In this application, "plurality" means at least two, e.g., two, three, etc., unless specifically stated otherwise.
The above description is merely exemplary of the present application and is presented to enable those skilled in the art to understand and practice the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (9)

1. A preparation method of a metal-doped palladium molecular sieve catalyst is characterized by comprising the following steps:
placing a molecular sieve and a first metal salt in a cavity of plasma equipment, performing rotary mixing and vacuumizing, and then introducing carrier gas to continue to perform rotary mixing to obtain a first mixture; the first metal salt is palladium salt;
adding a second metal salt into the first mixture, carrying out rotary mixing and vacuumizing, and continuously carrying out rotary mixing after carrier gas is introduced to obtain a second mixture;
calcining the second mixture to obtain a metal-doped palladium molecular sieve catalyst;
the carrier gas is a mixture of argon and oxygen.
2. The method of claim 1, wherein the molecular sieve is a SAPO-18 molecular sieve.
3. The method of claim 1, wherein the palladium salt is palladium chloride.
4. The method for preparing the metal-doped palladium molecular sieve catalyst according to claim 1, wherein the second metal salt is chloride or nitrate of any one or more of chromium, iron, nickel, copper, zinc, barium, cobalt, manganese and tin.
5. The method of claim 1, wherein the calcination is at a temperature of 450-650 ℃.
6. The method for preparing a metal-doped palladium molecular sieve catalyst according to claim 1, wherein the mass ratio of the palladium content to the molecular sieve in the metal-doped palladium molecular sieve catalyst is 0.5 to 2%:1.
7. the method of claim 1, wherein the mass ratio of the metal doping amount of the second metal salt to the molecular sieve in the metal-doped palladium molecular sieve catalyst is 0.3% -1.5%:1.
8. A metal-doped palladium molecular sieve catalyst, wherein the metal-doped palladium molecular sieve catalyst is prepared by the preparation method of any one of claims 1 to 7.
9. The use of the metal-doped palladium molecular sieve catalyst of claim 8, wherein the metal-doped palladium molecular sieve catalyst is used for adsorption of nitrogen oxides in automobile exhaust.
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