Waste biochar regeneration method based on microwave heating and non-heating effects
Technical Field
The invention relates to a waste biochar regeneration method, and belongs to the technical field of waste recycling.
Background
Biochar is widely applied in the fields of wastewater treatment, soil remediation, plant root growth and the like due to the excellent pore structure and rich functional groups. At present, the raw materials for preparing the biochar are extremely wide in source, wherein sludge (sewage sludge, papermaking sludge, printing and dyeing sludge and the like) and biomass (lignin, rice hulls, rice and the like) are mainly used. Pyrolysis is used as a low-carbon and high-efficiency biochar material synthesis technology and becomes a technical means commonly adopted in academia and industry.
Currently, application research on biochar is mainly focused on aspects of pollutant adsorption efficiency, toxicity release risk and the like. Although the biochar has good application results in practical engineering, neglecting the subsequent regeneration and utilization thereof leads to a significant technical bottleneck in the large-scale production of the biochar market. The key points of the difficulty in the recycling of the biochar are in two aspects of pore structure blockage and toxicity release of adsorbed pollutants. Therefore, the development of the biochar recycling technology is important to the improvement of the core technical status of China internationally owned.
Microwaves cause the dipole molecules to rotate frequently by emitting electromagnetic waves at frequencies between 300 megahertz and 3000 gigahertz. Then, friction of adjacent dipole molecules generates a large amount of heat, and finally quick temperature rise of the biochar is realized. Microplasmas and hot spots caused by microwave heating proved to have excellent catalytic effects. Based on this, it is speculated herein that the internal components of the biochar pore structure will be further catalytically cracked. Meanwhile, the non-thermal effect caused by microwaves accelerates the decomposition of components in the pores into small molecular components by the rotation and vibration of dipole molecules, and finally solves the problem of the blockage of the pore structure of the waste biochar. In addition, the biochar pore structure is further carbonized, so that the pollutant fixing effect is effectively improved. The invention has important practical significance for realizing the recycling of the waste biochar.
Disclosure of Invention
The invention provides a waste biochar regeneration method based on microwave heat and non-heat effect, which aims to solve the problem of the blocking of waste biochar pores and the insufficient pollutant fixing effect. The biochar pore structure initially forms new carbon at 300 ℃ and develops into a complete carbon pore structure at 500 ℃. Based on the method, a gradient heating experimental group is arranged, and the structural change of waste biochar holes subjected to microwave treatment at 300-700 ℃ is observed, so that the optimal experimental conditions are determined.
The invention adopts the technical proposal for solving the problems that the method comprises the following steps:
step 1, respectively placing samples in quartz reactors in a microwave device;
Step 2, raising the temperature in the quartz reactor to 500 ℃ and 700 ℃ respectively;
Step 3, carrying out microwave radiation on the sample;
And 4, collecting the biochar cooled to room temperature.
Further, the temperature rising speed in the quartz reactor in the step 2 is 100 ℃ per min.
Further, in step 3, electromagnetic waves having a frequency between 300 megahertz and 3000 gigahertz are emitted to the sample.
Further, in order to maintain a strict inert atmosphere in the quartz reactor, pure argon is continuously injected into the quartz reactor to discharge oxygen, the microwave device is closed after a specified reaction time is reached, and high-purity argon is injected into the quartz reactor again to remove residual gas.
Furthermore, the microwave non-thermal effect causes the dipole molecules of the biochar to rotate through high-frequency electromagnetic waves, so that new pores are generated in the biochar, the pore volume and pore size distribution of the new biochar are obviously increased, and finally the regeneration and the utilization of the waste biochar are realized.
Further, in order to maintain a strict inert atmosphere in the quartz reactor, pure argon was continuously injected into the quartz reactor at a flow rate of 10L/min for 20 minutes.
Further, after the specified reaction time is reached, the microwave device is turned off, and high-purity argon is again injected into the quartz reactor for 20 minutes.
Further, the ideal effects are obtained at 500 ℃ and 700 ℃, and under the condition, the application of high-frequency electromagnetic waves is beneficial to remarkably improving the hole structure of the waste biochar.
The beneficial effects of the invention are as follows:
(1) The micro-plasmas and hot spots caused by microwave heating have catalytic effects, so that the carbonization of the surface of the waste biochar is effectively accelerated, and the pollutant fixing effect is improved. Further, the microwave non-thermal effect causes the dipole molecules of the biochar to rotate through high-frequency electromagnetic waves, so that new pores are generated in the biochar, and finally, the regeneration and the utilization of the waste biochar are realized.
(2) Carrying out microwave treatment on the charcoal which is pyrolyzed at 500 ℃ and 700 ℃, analyzing the pore characteristics of the charcoal by adopting a physical and chemical adsorption instrument, and finding that the pore volume of the new charcoal is obviously increased and the pore size distribution is further enlarged after the microwave treatment; the invention determines 500 ℃ as the optimal condition, and the 700 ℃ carbon pore structure is obviously improved, solves the engineering bottleneck problem of insufficient pollutant fixing effect due to the blocking of the waste biochar pores, and realizes the development of the waste biochar recycling technology.
Drawings
FIG. 1 is a schematic diagram of the structural features of a 500 ℃ biochar pore;
FIG. 2 is a schematic diagram of the pore structure characteristics of a biochar at 700 ℃.
Detailed Description
The first embodiment is as shown in fig. 1, the method for regenerating the waste biochar based on the microwave heat and non-heat effect comprises the following specific steps:
step 1, respectively placing samples in quartz reactors in a microwave device;
step 2, respectively increasing the temperature in the quartz reactor to 500 ℃ and 700 ℃, wherein the temperature increasing speed in the quartz reactor is 100 ℃ per minute;
Step 3, carrying out microwave radiation on the sample, and transmitting electromagnetic waves with the frequency of 300 megahertz to 3000 gigahertz to the sample;
And 4, collecting the biochar cooled to room temperature.
In the second embodiment, as shown in fig. 1, in order to maintain a strict inert atmosphere in the quartz reactor, pure argon is continuously injected into the quartz reactor to discharge oxygen, the microwave device is closed after a specified reaction time is reached, and high-purity argon is re-injected into the quartz reactor to remove residual gas.
Wherein, in order to maintain a strict inert atmosphere in the quartz reactor, pure argon gas was continuously injected into the quartz reactor at a flow rate of 10L/min for 20 minutes.
After the specified reaction time is reached, the microwave device is turned off, and high-purity argon is injected into the quartz reactor again for 20 minutes.
In the embodiment, the waste biochar is widely sourced and comprises biochar prepared by taking sludge, lignin, rice hulls, rice and the like as materials, and specifically waste biochar generated by engineering such as industrial wastewater treatment, soil remediation and the like is used;
the microwave device comprises a microwave cavity, a quartz reactor, a wave guide pipe, a magnetron, a PC fuzzy logic algorithm, a power regulator, an infrared thermometer and a gas flowmeter;
waste biochar microwave test process:
step one, collecting waste biochar generated in different engineering application scenes as an experiment set by taking newly prepared biochar as a control set, and carrying out batch experiments by setting different microwave frequencies as variables;
Step two, respectively placing the samples in quartz reactors in a microwave chamber;
and step three, the temperature is increased to 300-700 ℃ at a speed of 100 ℃ per minute. After the set temperature is reached, carrying out microwave radiation on the sample, and emitting electromagnetic waves with the frequency of 300 megahertz to 3000 gigahertz, wherein the electromagnetic waves cause the dipole molecules of the waste biochar to rotate, so that new pores are generated in the biochar;
And step four, collecting the biochar cooled to room temperature for performance evaluation.
The microwave non-thermal effect causes the dipole molecules of the biochar to rotate through high-frequency electromagnetic waves, new pores are generated in the biochar, the pore volume and the pore size distribution of the new biochar are obviously increased, and finally the regeneration and the utilization of the waste biochar are realized.
Wherein, 500 ℃ and 700 ℃ are ideal pyrolysis conditions, and the high-frequency electromagnetic wave is applied under the conditions, thereby being beneficial to remarkably improving the hole structure of the waste biochar.
The present invention is not limited to the preferred embodiments, and the present invention is described above in any way, but is not limited to the preferred embodiments, and any person skilled in the art will appreciate that the present invention is not limited to the embodiments described above, while the invention has been described with respect to specific examples including presently preferred modes of carrying out the invention, those skilled in the art will appreciate that there are numerous variations and permutations of the above described embodiments that fall within the spirit and scope of the invention as set forth in the appended claims.