Joule thermal reactor for treating aerogel materials

Abstract

The utility model belongs to the field of nano material preparation, and particularly discloses a Joule thermal reactor for treating aerogel materials, which comprises an aluminum oxide frame, a first electrode, a second electrode, a third electrode, a fourth electrode and a fifth electrode, and the aluminum oxide frame is provided with a reaction cavity in the middle and is used for containing the aerogel materials; the first carbon paper and the second carbon paper are attached to the upper surface and the lower surface of the aluminum oxide frame respectively; the graphite fixing seats are used for fixing the aluminum oxide frame, the first carbon paper and the second carbon paper, and the graphite fixing seats are arranged at the two ends of the aluminum oxide frame; the Joule heat device comprises an electrode clamp and a power supply, two ends of the first carbon paper and two ends of the second carbon paper are connected with the electrode clamp, and the first carbon paper and the second carbon paper generate Joule heat after being electrified and are used for performing Joule heat treatment on the aerogel material in the reaction cavity. The Joule thermal reactor for treating the aerogel material can be used for efficiently heating and collecting the aerogel material.

Description

TECHNICAL FIELD

[0001] The utility model belongs to aerogel material processing field especially relates to the joule heat reactor for processing aerogel material. BACKGROUND

[0002] At present, the joule heat heating technology shows great potential in the field of material preparation. By applying current to the conductive material, a large amount of heat can be generated in a short time by using its own resistance, which can realize rapid and efficient heating. It has the characteristics of ultra-fast heating, ultra-short holding, ultra-fast cooling and self-heating high temperature, so it can realize a large degree of overheating and supercooling, inhibit grain growth, migration, ripening and agglomeration, and also realize non-equilibrium thermodynamics and extreme environment thermodynamics, and prepare some materials that cannot be prepared by conventional methods. Moreover, this method can achieve local ultra-high temperature and achieve a very high energy utilization rate; this method also has a large heating temperature range, which can meet the needs of different material preparation.

[0003] Aerogel material has a large specific surface area due to its porous structure, and aerogel is considered as one of the future materials due to its light weight, heat insulation, high specific surface area and controllable chemical properties. It shows great potential in the fields of energy, environmental protection, electronics and other fields. Joule heat treatment can make beneficial modification to aerogel material, however, the current joule heat heating technology mainly focuses on self-heating and using other materials (such as graphite sheet, tungsten sheet, etc.) to heat shock the sample to be treated, but it is difficult to heat and collect the fluffy aerogel material efficiently. Because in the short heating process, the gas expands under the influence of heat, the aerogel is affected and is difficult to collect. At present, it is urgent to design a reactor that can process fluffy aerogel material and realize efficient heating and collection of aerogel material. UTILITY MODEL CONTENTS

[0004] The technical problem to be solved by the utility model is to overcome the deficiencies and defects mentioned in the above background technology, and to provide a joule heat reactor capable of efficiently processing aerogel material and collecting products.

[0005] To solve the above technical problems, the technical scheme provided by the utility model is as follows: a joule heat reactor for processing aerogel material, comprising:

[0006] An aluminum oxide frame is formed with a reaction cavity in the middle, and the reaction cavity is used to hold aerogel material;

[0007] The first carbon paper and the second carbon paper are respectively attached to the upper surface and the lower surface of the aluminum oxide frame;

[0008] A graphite fixing seat is used to fix the aluminum oxide frame, the first carbon paper and the second carbon paper, and the graphite fixing seat is arranged at both ends of the aluminum oxide frame;

[0009] A joule heat device comprises an electrode clamp and a power supply, two ends of the first carbon paper and the second carbon paper are connected with the electrode clamp, and the first carbon paper and the second carbon paper generate joule heat after being electrified, which is used for joule heat treatment of the aerogel material in the reaction cavity.

[0010] In an embodiment, the thickness of the first carbon paper and the second carbon paper is 1.8-3mm, the density is 0.4-0.5g / cm 3 , the transverse conductivity is 100-120S / cm, and the thermal conductivity is 10-20W / m·K.

[0011] In an embodiment, the alumina frame comprises a frame body and a protruding part arranged at two ends of the frame body, the shapes of the first carbon paper and the second carbon paper are adapted to the shape of the alumina frame, two ends of the first carbon paper and the second carbon paper form clamping ends at the adapted parts of the protruding parts, and the clamping ends are connected with the electrode clamp.

[0012] In an embodiment, the graphite fixing seat comprises a graphite base, a graphite sheet and a graphite screw, the graphite base is arranged at the bottom of the protruding part of the alumina frame, the graphite sheet is arranged at the top of the protruding part, and the graphite screw passes through the graphite sheet, the first carbon paper, the protruding part, the second carbon paper and is locked on the graphite base.

[0013] In an embodiment, a joule heat instrument is further included, the joule heat instrument comprises a reaction cabin and a vacuum pump connected with the reaction cabin, the vacuum pump is used for extracting air in the reaction cabin and filling inert gas, and the alumina frame is detachably fixed in the reaction cabin.

[0014] In an embodiment, the inert gas is nitrogen or argon.

[0015] In an embodiment, the temperature rising rate of the reaction cavity of the alumina frame is 500-1500K / s, and the temperature falling rate is 800K / s.

[0016] In an embodiment, the aerogel material is carbon aerogel, silica aerogel, polymer aerogel or biomass aerogel.

[0017] Compared with the prior art, the beneficial effects of the utility model are that: the utility model adopts the sandwich structure joule heat heating mode, the first carbon paper and the second carbon paper arranged on the top and bottom of the alumina frame top and bottom carry out joule heat treatment, and the aerogel material is filled in the reaction cavity of the alumina frame, so that efficient joule heat treatment can be realized, the first carbon paper and the second carbon paper can ensure that the aerogel material is heated uniformly and the repeatability of material preparation is ensured, and the larger heating area can ensure that the product amount prepared each time is larger. BRIEF DESCRIPTION OF DRAWINGS

[0018] In order to more clearly illustrate the technical scheme in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced as follows. Obviously, the drawings in the following description are some embodiments of the present application, and for those skilled in the art, other drawings can also be obtained without creative labor on the basis of these drawings.

[0019] Fig. 1 It is a structural schematic view of the joule heat reactor for processing aerogel material in an embodiment.

[0020] Fig. 2 It is a structural schematic view of the joule heat reactor for processing aerogel material in another embodiment.

[0021] Fig. 3 It is a temperature rising and falling rate schematic view of the joule heat reactor for processing aerogel material in an embodiment.

[0022] The drawings show that: 10 is an alumina frame; 12 is a reaction cavity; 14 is a protruding part; 16 is a frame body; 20 is a first carbon paper; 30 is a second carbon paper; 22 is a clamping end; 40 is a graphite fixing seat; 42 is a graphite base; 44 is a graphite sheet; 46 is a graphite screw; and the aerogel material 100. DETAILED DESCRIPTION

[0023] In order to facilitate the understanding of the present application, the following will combine the drawings of the specification and the preferred embodiments to make a more comprehensive and detailed description of the present application, but the protection scope of the present application is not limited to the following specific embodiments.

[0024] Unless otherwise defined, all terms used in the description herein, including technical terms, have the same meaning as commonly understood by one of ordinary skill in the art. The terms used herein are for the purpose of describing specific embodiments only and are not intended to limit the scope of the present application.

[0025] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present application can be purchased from the market or prepared by the existing method.

[0026] As shown in Figs. 1-3 An embodiment of the present application provides a Joule heat reactor for processing aerogel material, which comprises an alumina frame 10, a first carbon paper 20, a second carbon paper 30, a graphite fixing seat 40 and a Joule heat device (not shown in the figure). Specifically, a reaction cavity 12 is formed in the middle of the alumina frame 10, which is used to hold the aerogel material. The first carbon paper 20 and the second carbon paper 30 are respectively attached to the upper surface and the lower surface of the alumina frame 10. The graphite fixing seat 40 is used to fix the alumina frame 10, the first carbon paper 20 and the second carbon paper 30, and is arranged at both ends of the alumina frame 10. The Joule heat device comprises an electrode clamp and a power supply, and both ends of the first carbon paper 20 and the second carbon paper 30 are connected to the electrode clamp. After being electrified, the first carbon paper 20 and the second carbon paper 30 generate Joule heat, which is used to perform Joule heat treatment on the aerogel material in the reaction cavity 12. Specifically, in an embodiment, the aerogel material is carbon aerogel, silica aerogel, polymer aerogel or biomass aerogel. Of course, it is not limited to the above-mentioned aerogel materials, and the above-mentioned materials are currently commonly used materials. The aerogel material is shaped in the reaction cavity of the alumina frame 10 after Joule heat.

[0027] The present application adopts a sandwich structure of Joule heat heating mode. The first carbon paper 20 and the second carbon paper 30 arranged at the top and the bottom of the alumina frame 10 perform Joule heat treatment. The aerogel material is filled into the reaction cavity 12 of the alumina frame 10, so that efficient Joule heat treatment can be achieved. Since the first carbon paper 20 and the second carbon paper 30 can ensure uniform heating of the aerogel material and ensure the repeatability of material preparation, a larger heating area can ensure a larger amount of products prepared each time. Further, in the aerogel heat treatment, the first carbon paper 20 and the second carbon paper 30 close the reaction cavity 12 of the alumina frame 10, so that the aerogel in the reaction cavity 12 will not fly out due to gas expansion, solving the problem that the fluffy aerogel material is easy to fly out during the Joule heat treatment process and cannot be collected.

[0028] In combination with Fig. 3It can be seen that in specific use, the heating rate of the reaction cavity 12 of the aluminum oxide frame 10 is 500-1500 K / s, and the cooling rate is 800 K / s. The Joule heat reactor of the present application has the characteristics of high superheat and high subcooling, which is beneficial to the structure optimization of aerogel, improves the heat conduction performance, enhances the adsorption / desorption capacity, improves the catalytic performance, and improves the stability of the material.

[0029] Specifically, in an embodiment, the thickness of the first carbon paper 20 and the second carbon paper 30 is 1.8-3mm, the density is 0.4-0.5g / cm3, the transverse conductivity is 100-120S / cm, and the thermal conductivity is 10-20W / m·K. The first carbon paper 20 and the second carbon paper 30 generate a large amount of heat instantaneously due to their own resistance when passing through the current, and perform carbon thermal impact on the aerogel material sandwiched in the aluminum oxide frame 10. The aluminum oxide frame 10 mainly plays a limiting role in this process, which can prevent the carbon paper from affecting the structure of the aerogel. Because the first carbon paper 20 and the second carbon paper 30 have a certain rigidity, when they are clamped together with the aluminum oxide frame 10, they play a certain sealing role. After the aluminum oxide frame 10, the first carbon paper 20 and the second carbon paper 30 are fixed by the graphite fixing seat 40, the dispersion of the aerogel is limited, and the waste caused by the flying of the aerogel material during the heating process is prevented.

[0030] Specifically, in an embodiment, the aluminum oxide frame 10 includes a frame body 16 and a protruding portion 14 arranged at both ends of the frame body 16, the shapes of the first carbon paper 20 and the second carbon paper 30 are adapted to the shape of the aluminum oxide frame 10, and the ends of the first carbon paper 20 and the second carbon paper 30 are adapted to the protruding portion 14 to form clamping ends 22, and the clamping ends 22 are connected with the electrode clamps.

[0031] Specifically, in an embodiment, the graphite fixing seat 40 includes a graphite base 42, a graphite sheet 44 and a graphite screw 46, the graphite base 42 is arranged at the bottom of the protruding portion 14 of the aluminum oxide frame 10, the graphite sheet 44 is arranged at the top of the protruding portion 14, and the graphite screw 46 passes through the graphite sheet 44, the first carbon paper 20, the protruding portion 14, the second carbon paper 30 and is locked on the graphite base 44.

[0032] Specifically, in an embodiment, the device further comprises a Joule heat instrument, the Joule heat instrument comprises a reaction chamber, a vacuum pump connected with the reaction chamber, the vacuum pump is used for extracting air in the reaction chamber, and after vacuumizing, inert gas is filled from another gas inlet according to needs, and the alumina frame 10 is detachably fixed in the reaction chamber. The reaction atmosphere can be inert gas according to the requirements of the aerogel material itself, or air or oxygen. The graphite base 42 of the graphite fixing seat 40 is connected to the Joule heat instrument. Preferably, the inert gas is nitrogen or argon. The device can be applied to various aerogel materials, such as carbon aerogel, silica aerogel, polymer aerogel, biomass aerogel, etc.

[0033] The use method of the Joule heat reactor for processing aerogel materials of the utility model is disclosed in combination with the specific embodiments as follows:

[0034] Example 1: The graphene supported ruthenium nanoparticles are obtained by using the Joule heat reactor for processing aerogel materials of the present application to process graphene oxide supported ruthenium aerogel

[0035] Specifically, the following steps are included: using graphene oxide supported ruthenium to prepare aerogel, and performing Joule heat treatment under argon atmosphere.

[0036] The graphene oxide supported ruthenium aerogel is prepared in advance, the mass ratio of graphene oxide to ruthenium in the aerogel is 0.12, and the aerogel is prepared by freeze-drying method.

[0037] The aerogel material is placed in the reaction cavity 12 of the alumina frame 10, the alumina frame 10 is clamped by the first carbon paper 20 and the second carbon paper 30 from top to bottom, and is fixed at both ends by the graphite fixing seat 40, and the first carbon paper 20 and the second carbon paper 30 used in this example are TGP-H-060 type carbon paper of Toray.

[0038] The device and the material are fixed in the reaction chamber of the Joule heat instrument, the air in the reaction chamber of the Joule heat instrument is extracted by using a vacuum pump, then nitrogen is filled, and the operation is repeated for 3 times to ensure that the purity of argon in the reaction chamber is high enough to avoid the occurrence of side reactions.

[0039] The current and time during Joule heat treatment are set, in this example, the current and time are 500 A and 0.4 s respectively, the Joule heat temperature is 1700 K, and the graphene supported nanoparticles are obtained. The product obtained in this embodiment is graphene oxide supported ruthenium nanoparticles, the nanoparticle size distribution is uniform, the average particle size is 1.2 nm, and no obvious aggregation phenomenon occurs, avoiding the particle aggregation in traditional thermal chemistry. Moreover, the preparation process flow is simple, the cost is low, and the graphene supported ultrafine ruthenium nanoparticles can be successfully prepared in a very short time (0.4 s).

[0040] Example 2: The graphene oxide supported ruthenium aerogel is treated in the joule heat reactor of the application to obtain the nanosheet of ruthenium / ruthenium oxide hetero-particle composition;

[0041] The aerogel is prepared in advance, and the mass ratio of graphene oxide to ruthenium is 0.25, and the aerogel is prepared by freeze-drying method;

[0042] The aerogel material is placed in the reaction cavity 12 of the alumina frame 10, the alumina frame 10 is clamped by the first carbon paper 20 and the second carbon paper 30, and is fixed at both ends by the graphite fixing seat 40, and the first carbon paper 20 and the second carbon paper 30 used in the example are AvCarb MGL280 type carbon paper;

[0043] The above device and material are fixed in the reaction cavity of the joule heat instrument, the current and time during joule heat treatment are set, the current and time are 500A and 0.5s respectively, the joule heat temperature is 1800K, and the nanosheet of ruthenium / ruthenium oxide hetero-particle composition is obtained. In the embodiment, the graphene oxide is completely pyrolyzed in the process of joule heat, the ruthenium also generates ruthenium oxide at high temperature, finally the hetero-nanosheet composed of ruthenium / ruthenium oxide is formed, the product has uniform particle size distribution, the average particle size is 3nm, and no obvious aggregation phenomenon occurs, avoiding the particle aggregation in the traditional thermochemistry. The process flow is simple, the cost is low, and the ruthenium / ruthenium oxide hetero-nanosheet can be successfully prepared in a very short time (0.5s).

[0044] The above only describes the preferred embodiments of the application, and does not limit the actual application of the application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the application shall be included in the protection scope of the application.

Claims

1. A Joule thermal reactor for processing aerogel materials, characterized in that, include: An alumina frame, wherein a reaction chamber is formed in the middle of the alumina frame, and the reaction chamber is used to hold aerogel material; The first carbon paper and the second carbon paper are respectively attached to the upper and lower surfaces of the alumina frame; Graphite holders are used to fix the alumina frame, the first carbon paper, and the second carbon paper. The graphite holders are located at both ends of the alumina frame. The Joule heating device includes an electrode clamp and a power supply. Both ends of the first carbon paper and the second carbon paper are connected to the electrode clamp. When the power is turned on, the first carbon paper and the second carbon paper generate Joule heat, which is used to perform Joule heat treatment on the aerogel material in the reaction chamber.

2. The Joule thermal reactor for processing aerogel materials according to claim 1, characterized in that, The thickness of the first and second carbon papers is 1.8-3 mm, and the density is 0.4-0.5 g / cm³. 3 Its lateral electrical conductivity is 100-120 S / cm, and its thermal conductivity is 10-20 W / m·K.

3. The Joule thermal reactor for processing aerogel materials according to claim 1, characterized in that, The alumina frame includes a frame body and protrusions at both ends of the frame body. The shapes of the first carbon paper and the second carbon paper are adapted to the shape of the alumina frame. The two ends of the first carbon paper and the second carbon paper are adapted to the protrusions to form clamping ends, which are connected to the electrode clamps.

4. The Joule thermal reactor for processing aerogel materials according to claim 3, characterized in that, The graphite fixing base includes a graphite base, a graphite sheet, and a graphite screw. The graphite base is located at the bottom of the protrusion of the alumina frame, the graphite sheet is located at the top of the protrusion, and the graphite screw passes through the graphite sheet, the first carbon paper, the protrusion, and the second carbon paper and is locked onto the graphite base.

5. The Joule thermal reactor for processing aerogel materials according to claim 1, characterized in that, It also includes a Joule heating instrument, which includes a reaction chamber and a vacuum pump connected to the reaction chamber. The vacuum pump is used to extract air from the reaction chamber and fill it with inert gas. The alumina frame is detachably fixed inside the reaction chamber.

6. The Joule thermal reactor for processing aerogel materials according to claim 5, characterized in that, The inert gas is nitrogen or argon.

7. The Joule thermal reactor for processing aerogel materials according to claim 1, characterized in that, The heating rate of the reaction chamber of the alumina frame is 500-1500 K / s, and the cooling rate is 800 K / s.

8. The Joule thermal reactor for processing aerogel materials according to claim 1, characterized in that, The aerogel material is carbon aerogel, silica aerogel, polymer aerogel, or biomass aerogel.

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