CN-115591477-B - Device and method for large-scale production of boron nitride nano material

Abstract

The invention relates to the technical field of chemical production and discloses a device and a method for large-scale production of boron nitride nano materials, wherein the device comprises a vacuum chamber, a cooling water circulation system, a vacuum air extraction system, an exhaust system, an air path, an automatic stirring device, a material reaction container and a heating device, wherein the automatic stirring device is used for controlling material mixing and stirring, the material reaction container is connected with a plurality of evenly distributed air inlets, and the heating device surrounds the material reaction container and is used for controlling reaction temperature. According to the invention, the automatic stirring device and the multi-point densely distributed air inlet channels are arranged in the material reaction container, so that the heat treatment effect and the chemical reaction efficiency of the raw materials in the gas are improved, the single treatment quality and the single treatment quantity of the materials are effectively improved, and the production efficiency of the boron nitride nano material is improved. The invention has the advantages of simple device, low manufacturing cost, easy realization of large-scale production, simple production method, low energy consumption and no pollution, and meets the requirement of large-scale preparation of the boron nitride nano material.

Inventors

• YIN HONG
• GAO JINLING
• ZHAN WEI
• GAO WEI

Assignees

• 吉林大学

Dates

Publication Date

20260505

Application Date

20221020

Claims (8)

1. 1. The device for large-scale production of the boron nitride nano material is characterized by comprising a vacuum chamber, a cooling water circulation system, a vacuum air extraction system, an exhaust system, an air path, an automatic stirring device, a material reaction container and a heating device; the vacuum chamber is provided with a switch door, a quartz observation window, a vacuum sealing rubber ring and a lock are arranged on the door, and the outer wall of the chamber is a cooling water circulation cold wall for integrally cooling the vacuum chamber; The automatic stirring device comprises a rotary driving piece, a lifting rod and a stirring blade, wherein the upper end of the stirring blade is fixed on the vacuum chamber, the external part of the stirring blade is connected with a frequency converter, a lifting motor and a stirring motor and is used for controlling the mixing and stirring of materials, and the stirring blade is arranged in a material reaction container and is used for continuously mixing and stirring the materials; a plurality of air inlets are uniformly distributed on the side wall of the material reaction container along the axis in a surrounding manner; The heating device surrounds the side surface and the bottom of the material reaction container and is used for controlling the material reaction temperature; the top of the material reaction container is provided with a container upper cover, and a gap is reserved between the container upper cover and a lifting rod of the stirring device to form an air outlet for escape of reaction gas.
2. 2. The apparatus for mass production of boron nitride nanomaterials according to claim 1, wherein the number of air inlets is greater than 1, each air inlet is spaced apart from 30-800 mm, and each air inlet can be independently opened and closed.
3. 3. The device for mass production of boron nitride nano-materials according to claim 1, wherein the material reaction vessel is cylindrical, and is made of quartz, corundum and zirconia, and the diameter of the material reaction vessel is 50-500 mm.
4. 4. The device for mass production of boron nitride nano-materials according to claim 1, wherein the back vacuum of the vacuum chamber can reach 10 -2 Pa, and the working pressure during the reaction is 1-10 5 Pa.
5. 5. The apparatus for mass production of boron nitride nanomaterial according to claim 1, wherein the heating temperature of the heating apparatus is from room temperature to 1200 o C.
6. 6. The apparatus for the mass production of boron nitride nanomaterials according to claim 1, wherein the apparatus is useful for mass production of materials including, but not limited to, boron nitride nanofibers, boron nitride nanorods, boron nitride nanotubes, boron nitride nanoplatelets, and porous boron nitride nanomaterials.
7. 7. A method for mass production of boron nitride nanomaterials, characterized in that the device according to any one of claims 1 to 6 is used, comprising the steps of: 1) Opening a vacuum chamber door, placing raw materials in a material reaction container, and closing a container upper cover; 2) Closing a vacuum chamber door, starting vacuumizing, closing an air extraction port until the appointed back vacuum ensures that gas impurities are removed, closing a vacuum pump, introducing inert gas until the atmospheric pressure is reached, opening an air outlet, starting a cooling water circulation system, starting heating, starting an automatic stirring device, performing up-and-down rotary mixing stirring on materials in a material reaction container, and simultaneously, introducing reaction gas after heating to the appointed reaction temperature, and starting reaction; 3) After the reaction is finished, closing the reaction gas, cooling until the temperature is reduced to room temperature, stopping stirring, closing the inert gas, and closing the cooling water circulation system; 4) And opening a vacuum chamber door, opening a container upper cover, and taking out the reacted material to obtain the boron nitride nano material.
8. 8. The method of claim 7, wherein the method is applicable to mass production of boron nitride nanomaterials including, but not limited to, boron nitride nanofibers, boron nitride nanorods, boron nitride nanotubes, boron nitride nanoplatelets, and porous boron nitride nanomaterials.

Description

Device and method for large-scale production of boron nitride nano material Technical Field The invention belongs to the technical field of chemical production, and particularly relates to a device and a method for large-scale production of boron nitride nano materials. Background The boron nitride nano material has strong mechanical property, excellent thermal property and chemical stability of boron nitride, also has special properties of the nano material, such as specific high specific surface area and small size, presents multiple structural properties and rich functionalities, and has great application requirements in the aspects of filtration, adsorption, catalytic carrier, hydrogen storage, drug delivery, composite material addition modification and the like. The high-grade boron nitride core technology is monopolized abroad for a long time, the existing large-scale production process is generally lagged, the product specification is few, the stability is poor, the yield and the productivity of the high-quality boron nitride nano material are urgently required to be improved, and the large-scale production is accelerated. The size and the morphology of the nano material play a decisive role in the performance and the application of the material, so that the large-scale synthesis of the boron nitride nano material with controllable morphology and uniform size is a key for truly realizing the commercial value. At present, the preparation process of the boron nitride nano material in a laboratory is improved to the greatest extent, and a special device and a special technology applied to the mass production of the high-quality boron nitride nano material are not available in the market. The synthesis of nanomaterials is generally carried out by using a high temperature furnace device with gas participation reaction, and mainly comprises a tubular furnace, an atmosphere furnace and a pit furnace. The tubular furnace is generally suitable for heat treatment of small workpieces or a small amount of experimental samples, adopts various different atmosphere environments of vacuum, protective gas, oxidation and reduction, has strong sealing performance, is similar to the synthesis of functions of a box furnace and the tubular furnace, has ventilation property on the basis of the box furnace, is used for treating larger samples needing gas participation, and has a generally circular hearth, a door is opened and closed in the vertical direction, and the mechanism is similar to a crucible high-temperature furnace. For experimental reaction involving gas, a tube furnace is mostly selected, the gas in the tube is exhausted to reach a higher vacuum state before the reaction starts, and then the reaction gas is introduced to remove the influence of impurity molecules in the air, but the limited reaction space and reaction temperature zone limit the single material handling capacity. Especially for the treatment of powder materials, under the condition that the reaction space is limited, if the condition that the contact of the materials with the reaction gas is incomplete, the reaction is insufficient and the like occurs when the powder is placed too much at a time, the quality and the quantity of the single material treatment are further reduced, if an atmosphere furnace is used, the gas is only contacted with the upper layer powder sample after entering, the problems that the powder sample is too few in the single synthetic treatment, the reaction quality of the lower layer sample is poor and the like are also faced, meanwhile, the utilization rate of the gas introduced into the furnace is lower, the waste is easily caused, the requirement on the tail gas treatment is high, and the use cost is increased. Therefore, how to mass produce boron nitride nano-materials and simultaneously meet the high-quality preparation with controllable structure and uniform size is a problem to be solved at present, and a reaction device with large capacity, ventilation, heating, improving the utilization rate of reaction gas and increasing the thermal reaction efficiency and chemical reaction efficiency of materials is a key to realize macro and high-quality synthesis and process of powder samples. Disclosure of Invention In view of the above, the invention aims to provide a device and a method for mass production of boron nitride nano materials, which can be used for synthesizing and heat-treating a large amount of powder materials needing to be participated by gas in a single process by adding a material reaction container with an automatic stirring device and a heating device and carrying out multi-point and high-density uniform ventilation, and has the advantages of simple structure and low cost, and solves the problems of limited single powder material treatment capacity, uneven contact between reaction gas and powder, low material chemical reaction efficiency and the like of the conventional high-temperature furnace technolog