Device and method for preparing heterogeneous reaction catalyst under extremely weak magnetic conditions

Abstract

A device and method for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, which can provide preparation conditions close to zero magnetism during the catalyst preparation process, and provide a new direction for the development of multiphase reaction catalysts. The device and method are characterized in that the device comprises a closed space surrounded by a permalloy magnetic shielding layer, wherein the geomagnetism in the closed space is shielded to ≤1nT, and a central space is formed in the closed space by a manganese-zinc ferrite low-noise magnetic shielding layer, wherein the manganese-zinc ferrite low-noise magnetic shielding layer shields the hysteresis loss noise and eddy current noise generated by the permalloy, thereby reducing the magnetic noise in the central space to ≤5. A reaction table for a multiphase reaction catalyst preparation device is arranged in the central space, and a catalyst synthesis reaction device is placed on the reaction table.

Description

Technical Field

[0001] The present invention belongs to the technical field of preparing multiphase reaction catalysts, and in particular relates to an apparatus and method for preparing multiphase reaction catalysts under extremely weak magnetic conditions, which can provide preparation conditions close to zero magnetic field during the catalyst preparation process, and provides a new direction for the research and development of multiphase reaction catalysts. Background Art

[0002] At present, the preparation of multiphase reaction catalysts often does not take into account the influence of geomagnetism. Under the conditions of the earth's magnetic field (about 50000nT), the magnetic field will have a certain impact on the preparation process of the catalyst. The magnetic field directly acts on the nucleus and extranuclear electrons, affecting the electron spin direction, movement direction, diffusion rate, etc. of chemical molecules, atoms, and ions. In addition, the magnetic field can also affect the electronic microstructure of the metal active center of the catalyst and the interaction between the metal and the carrier, causing certain differences. However, the current magnetic shielding method cannot be applied to catalyst preparation, so it is necessary to develop a catalyst preparation method and equipment that can be used under extremely weak magnetic conditions. Summary of the invention

[0003] In view of the defects or shortcomings of the prior art, the present invention provides an apparatus and method for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, which can provide preparation conditions close to zero magnetic field during the catalyst preparation process, and provides a new direction for the research and development of multiphase reaction catalysts.

[0004] The technical solution of the present invention is as follows:

[0005] A device for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, characterized in that it comprises a closed space surrounded by a permalloy magnetic shielding layer, the earth's magnetism in the closed space is shielded to ≤1nT, a central space is surrounded by a manganese-zinc ferrite low-noise magnetic shielding layer in the closed space, the manganese-zinc ferrite low-noise magnetic shielding layer shields the hysteresis loss noise and eddy current noise generated by the permalloy, and the magnetic noise of the central space is reduced to A reaction platform of a multiphase reaction catalyst preparation device is arranged in the central space, and a catalyst synthesis reaction device is placed on the reaction platform.

[0006] The catalyst synthesis reaction device is a beaker, a hydrothermal kettle, a watch glass or a crucible.

[0007] The upper and lower parts of the central space are provided with an upper opening and a lower opening respectively penetrating to the outside of the Permalloy magnetic shielding layer, and the left and right parts of the central space are provided with a left opening and a right opening respectively penetrating to the outside of the Permalloy magnetic shielding layer.

[0008] A mechanical stirring arm or a gas pipeline for gas bubbling stirring is arranged through the upper opening and / or the lower opening.

[0009] An incident light adjustment device or a cavity gas atmosphere adjustment device is arranged through the left opening and / or the right opening.

[0010] The permalloy magnetic shielding layer comprises a first permalloy magnetic shielding layer, a second permalloy magnetic shielding layer, a third permalloy magnetic shielding layer and a fourth permalloy magnetic shielding layer which are sequentially arranged from the inside to the outside.

[0011] A method for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, characterized in that the above-mentioned equipment for preparing a multiphase reaction catalyst under extremely weak magnetic conditions is used, and raw materials are placed in a catalyst synthesis reaction device to prepare a multiphase reaction catalyst under extremely weak magnetic conditions.

[0012] The multiphase reaction catalyst is MnOOH nanorods, and comprises the following preparation process: 1.56 g of MnCl2·4H2O and 4.8 g of NaOH are respectively dissolved in 40 mL of deionized water, and after the solution is clear and transparent, the NaOH solution is slowly dripped into the MnCl2 solution, and after the solution is evenly mixed, the solution is transferred into a polytetrafluoroethylene synthesis kettle, and placed on a reaction table of a multiphase reaction catalyst preparation device, and is heated to 120° C. by low-noise electricity, maintained for 4 hours, and washed and dried to obtain a final sample of MnOOH nanorods, without the presence of a mixed phase of MnOOH nanorods and Mn3O4 under normal geomagnetic conditions.

[0013] The multiphase reaction catalyst is a CoNi / SiO2 alloy catalytic material, which includes the following preparation process: dissolving 0.18g Ni(NO3)2·6H2O, 0.18g Co(NO3)2·6H2O and 8.32g TEOS into 200mL of a solution, wherein the solution contains ethanol and water in a volume ratio of 1:3, then adding 15mL of an aqueous ammonia solution, then placing a beaker on a reaction table of a multiphase reaction catalyst preparation device, introducing 100mL / min of nitrogen through an upper hole, stirring for more than 8 hours in a gas bubbling manner, then filtering and washing the sample, drying it in an oven at 100°C overnight, and then calcining it in an air atmosphere at 500°C for 4 hours to obtain a uniformly dispersed CoNi / SiO2 alloy catalytic material without the presence of a mixed phase of CoNi alloy, Co nanoparticles and Ni particles under normal geomagnetic conditions.

[0014] The technical effects of the present invention are as follows: The present invention provides a device and method for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, shielding the earth's magnetic field through a Permalloy magnetic shielding structure, and then using manganese-zinc ferrite to shield the hysteresis loss noise and eddy current noise generated by the Permalloy layer. A hollow layer is constructed to place a catalyst synthesis device, and different stirring methods and other conditions are set according to the reaction conditions to achieve catalyst preparation under extremely weak magnetic field conditions.

[0015] The advantages of the present invention over the prior art are as follows: (1) The present invention shields the earth's magnetic field through a Permalloy magnetic shielding structure, and then uses manganese-zinc ferrite to shield the hysteresis loss noise and eddy current noise generated by the Permalloy layer. The catalyst synthesis equipment is placed in the hollow layer, and different stirring methods and other conditions are set according to the reaction conditions to achieve catalyst preparation under extremely weak magnetic field conditions. (2) The method of the present invention is reasonable and the experimental operation is simple, which provides a basis for the development of multiphase reaction catalysts under extremely weak magnetic conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 The present invention is a schematic diagram of the structure of a device for preparing a multiphase reaction catalyst under extremely weak magnetic conditions.

[0017] The illustrations are as follows: A1-fourth Permalloy magnetic shielding layer; A2-third Permalloy magnetic shielding layer; A3-second Permalloy magnetic shielding layer; A4-first Permalloy magnetic shielding layer; B1-manganese zinc ferrite low noise magnetic shielding layer; C1-catalyst synthesis reaction device; C2-reaction table of multiphase reaction catalyst preparation device. DETAILED DESCRIPTION

[0018] Below is the attached figure ( Figure 1 ) and Examples illustrate the present invention.

[0019] Figure 1 This is a schematic diagram of the structure of an apparatus for preparing a multiphase reaction catalyst under extremely weak magnetic conditions according to the present invention. Figure 1 As shown, a device for preparing a multiphase reaction catalyst under extremely weak magnetic conditions comprises a closed space surrounded by a permalloy magnetic shielding layer, wherein the earth's magnetism in the closed space is shielded to ≤1nT, and a central space is surrounded by a manganese-zinc ferrite low-noise magnetic shielding layer B1 in the closed space, wherein the manganese-zinc ferrite low-noise magnetic shielding layer shields the hysteresis loss noise and eddy current noise generated by the permalloy, so that the magnetic noise in the central space is reduced to A multiphase reaction catalyst preparation device reaction table C2 is arranged in the central space, and a catalyst synthesis reaction device C1 is placed on the reaction table.

[0020] The catalyst synthesis reaction device C1 is a beaker, a hydrothermal kettle, a watch glass or a crucible. The upper and lower parts of the central space are provided with an upper opening and a lower opening respectively extending to the outside of the permalloy magnetic shielding layer, and the left and right parts of the central space are provided with a left opening and a right opening respectively extending to the outside of the permalloy magnetic shielding layer. A mechanical stirring arm or a gas pipeline for gas bubbling stirring is arranged through the upper opening and / or the lower opening. An incident light adjustment device or a cavity gas atmosphere adjustment device is arranged through the left opening and / or the right opening. The permalloy magnetic shielding layer includes a first permalloy magnetic shielding layer A4, a second permalloy magnetic shielding layer A3, a third permalloy magnetic shielding layer A2 and a fourth permalloy magnetic shielding layer A1 arranged in sequence from the inside to the outside.

[0021] A method for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, using the above-mentioned equipment for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, placing raw materials into a catalyst synthesis reaction device to prepare a multiphase reaction catalyst under extremely weak magnetic conditions.

[0022] The multiphase reaction catalyst is MnOOH nanorods, and comprises the following preparation process: 1.56 g of MnCl2·4H2O and 4.8 g of NaOH are respectively dissolved in 40 mL of deionized water, and after the solution is clear and transparent, the NaOH solution is slowly dripped into the MnCl2 solution, and after the solution is evenly mixed, the solution is transferred into a polytetrafluoroethylene synthesis kettle, and placed on a reaction table of a multiphase reaction catalyst preparation device, and is heated to 120° C. by low-noise electricity, maintained for 4 hours, and washed and dried to obtain a final sample of MnOOH nanorods, without the presence of a mixed phase of MnOOH nanorods and Mn3O4 under normal geomagnetic conditions.

[0023] The multiphase reaction catalyst is a CoNi / SiO2 alloy catalytic material, which includes the following preparation process: dissolving 0.18g Ni(NO3)2·6H2O, 0.18g Co(NO3)2·6H2O and 8.32g TEOS (TEOS, Tetraethyl orthosilicate, tetraethoxysilane) into 200mL of solution, wherein the solution contains ethanol and water in a volume ratio of 1:3, then adding 15mL of ammonia solution, then placing the beaker on the reaction table of a multiphase reaction catalyst preparation device, introducing 100mL / min of nitrogen through the upper hole, stirring for more than 8 hours in a gas bubbling manner, then filtering and washing the sample, drying it in an oven at 100°C overnight, and then calcining it in an air atmosphere at 500°C for 4 hours to obtain a uniformly dispersed CoNi / SiO2 alloy catalytic material without the presence of a mixed phase of CoNi alloy, Co nanoparticles and Ni particles under normal geomagnetic conditions.

[0024] A method and device capable of preparing a multiphase reaction catalyst under extremely weak magnetic conditions. The method and device are reasonable in method, simple in experimental operation, can accurately provide near-zero magnetic reaction conditions, and provide a basis for the development of multiphase reaction catalysts under extremely weak magnetic conditions.

[0025] A method and device for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, characterized by combining an earth magnetic field shielding device with a multiphase reaction catalytic device to achieve catalyst preparation under extremely weak magnetic field conditions.

[0026] A method and apparatus for preparing a heterogeneous reaction catalyst under extremely weak magnetic conditions, comprising:

[0027] The four-layer Permalloy magnetic shielding structure shields the earth's magnetic field to less than 1nT. The middle core is a layer of manganese-zinc ferrite low-noise magnetic shielding layer to shield the hysteresis loss noise and eddy current noise generated by the Permalloy, reducing the central magnetic noise to Inside.

[0028] The catalyst preparation device is placed in the center of the magnetic shielding device. The upper and lower openings of the device are suitable for different types of stirring, such as placing a mechanical stirring arm for physical stirring or placing a gas pipeline for gas bubbling stirring. The horizontal openings on both sides are suitable for adjusting external influencing conditions, such as light and cavity gas atmosphere.

[0029] The specific implementation structure of the present invention is as follows Figure 1 As shown, the technical solution of the present invention is a method and device for preparing a multiphase reaction catalyst under extremely weak magnetic conditions, comprising the following steps:

[0030] Step (1): Establish a model according to the reaction requirements and prepare an earth magnetic field shielding device with a certain cavity volume that can be prepared using a catalyst.

[0031] Step (2): Measure the magnetic field strength in the cavity.

[0032] Step (3): Place the catalyst synthesis device according to the reaction conditions, including a beaker, a hydrothermal reactor, a watch glass, a crucible, etc.

[0033] Step (4): Different stirring methods are selected according to the reaction requirements and conditions, including physical stirring through a mechanical stirring arm, gas bubbling stirring through a gas pipeline, etc.

[0034] Step (5): Adjust different chamber atmospheres, light intensity, etc. according to reaction requirements and conditions.

[0035] Step (6): preparing a catalyst.

[0036] Example 1

[0037] 1.56 g MnCl2·4H2O and 4.8 g NaOH were dissolved in 40 mL of deionized water respectively. After the solution became clear and transparent, the NaOH solution was slowly dripped into the MnCl2 solution. After being evenly mixed, the solution was transferred into a polytetrafluoroethylene synthesis reactor and placed on the reaction table of a multiphase reaction catalyst preparation device. The solution was heated to 120°C by an electric coil and maintained for 4 hours. After washing and drying, the final sample was MnOOH nanorods.

[0038] Example 2

[0039] 1.56 g MnCl2·4H2O and 4.8 g NaOH were dissolved in 40 mL deionized water respectively. After the solution became clear and transparent, the NaOH solution was slowly dripped into the MnCl2 solution. After being evenly mixed, the solution was transferred into a polytetrafluoroethylene synthesis kettle and placed in an oven under the earth's magnetic field conditions at 120°C for 4 hours. After washing and drying, the final sample was a mixed phase of MnOOH nanorods and Mn3O4.

[0040] Example 3

[0041] 0.18g Ni(NO3)2·6H2O, 0.18g Co(NO3)2·6H2O and 8.32g TEOS were dissolved in 200mL solution (the solution contained ethanol and water in a volume ratio of 1:3), and then 15mL ammonia solution was added. The beaker was then placed on the reaction table of the multiphase reaction catalyst preparation device, 100mL / min nitrogen was introduced through the upper hole, and the gas bubbling method was stirred for more than 8 hours, and then the sample was filtered, washed, dried in an oven at 100℃ overnight, and then calcined at 500℃ in air atmosphere for 4 hours to obtain a uniformly dispersed CoNi / SiO2 alloy catalyst material.

[0042] Example 4

[0043] 0.18g Ni(NO3)2·6H2O, 0.18g Co(NO3)2·6H2O and 8.32g TEOS were dissolved in 200mL solution (the solution contained ethanol and water in a volume ratio of 1:3), and then 15mL ammonia solution was added. The beaker was then placed in a magnetic stirrer under the earth's magnetic field and stirred for more than 8 hours, and then the sample was filtered, washed, dried in an oven at 100°C overnight, and then calcined at 500°C in air atmosphere for 4 hours. The metal phase of the obtained CoNi / SiO2 catalytic material was a mixed phase of CoNi alloy, Co nanoparticles and Ni particles.

[0044] The contents not described in detail in the specification of the present invention belong to the prior art known to the professional and technical personnel in the field. It is pointed out here that the above description helps those skilled in the art to understand the invention, but does not limit the protection scope of the invention. Any equivalent replacement, modification and / or simplification of the above description without departing from the essence of the invention falls within the protection scope of the invention.

Claims

1. A method for preparing a heterogeneous reaction catalyst under extremely weak magnetic conditions, characterized in that: A device for preparing a multiphase reaction catalyst under extremely weak magnetic conditions is used, the device comprising a closed space surrounded by a permalloy magnetic shielding layer, the earth's magnetism in the closed space is shielded to ≤1nT, a central space is surrounded by a manganese-zinc ferrite low-noise magnetic shielding layer in the closed space, the manganese-zinc ferrite low-noise magnetic shielding layer shields the hysteresis loss noise and eddy current noise generated by the permalloy, A reaction table for a multiphase reaction catalyst preparation device is arranged in the central space, and a catalyst synthesis reaction device is placed on the reaction table; The raw materials are placed in a catalyst synthesis reaction device to prepare a heterogeneous reaction catalyst under extremely weak magnetic conditions; The multiphase reaction catalyst is a CoNi / SiO2 alloy catalytic material, which includes the following preparation process: dissolving 0.18g Ni(NO3)2·6H2O, 0.18g Co(NO3)2·6H2O and 8.32g TEOS into 200mL of a solution, wherein the solution contains ethanol and water in a volume ratio of 1:3, then adding 15mL of an aqueous ammonia solution, then placing a beaker on a reaction table of a multiphase reaction catalyst preparation device, introducing 100mL / min of nitrogen through an upper hole, stirring for more than 8 hours in a gas bubbling manner, then filtering and washing the sample, drying it in an oven at 100°C overnight, and then calcining it in an air atmosphere at 500°C for 4 hours to obtain a uniformly dispersed CoNi / SiO2 alloy catalytic material without the presence of a mixed phase of CoNi alloy, Co nanoparticles and Ni particles under normal geomagnetic conditions.

2. The method for preparing a heterogeneous reaction catalyst under extremely weak magnetic conditions according to claim 1, characterized in that: The catalyst synthesis reaction device is a beaker, a hydrothermal kettle, a watch glass or a crucible.

3. The method for preparing a heterogeneous reaction catalyst under extremely weak magnetic conditions according to claim 1, characterized in that: The upper and lower parts of the central space are provided with an upper opening and a lower opening respectively penetrating to the outside of the Permalloy magnetic shielding layer, and the left and right parts of the central space are provided with a left opening and a right opening respectively penetrating to the outside of the Permalloy magnetic shielding layer.

4. The method for preparing a heterogeneous reaction catalyst under extremely weak magnetic conditions according to claim 3, characterized in that: A mechanical stirring arm or a gas pipeline for gas bubbling stirring is arranged through the upper opening and / or the lower opening.

5. The method for preparing a heterogeneous reaction catalyst under extremely weak magnetic conditions according to claim 3, characterized in that: An incident light adjustment device or a cavity gas atmosphere adjustment device is arranged through the left opening and / or the right opening.

6. The method for preparing a heterogeneous reaction catalyst under extremely weak magnetic conditions according to claim 1, characterized in that: The permalloy magnetic shielding layer comprises a first permalloy magnetic shielding layer, a second permalloy magnetic shielding layer, a third permalloy magnetic shielding layer and a fourth permalloy magnetic shielding layer which are sequentially arranged from the inside to the outside.

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