CN112090371A - High-pressure reaction kettle and control method thereof - Google Patents
High-pressure reaction kettle and control method thereof Download PDFInfo
- Publication number
- CN112090371A CN112090371A CN202010951594.XA CN202010951594A CN112090371A CN 112090371 A CN112090371 A CN 112090371A CN 202010951594 A CN202010951594 A CN 202010951594A CN 112090371 A CN112090371 A CN 112090371A
- Authority
- CN
- China
- Prior art keywords
- autoclave
- pressure
- reaction kettle
- voltage electrode
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/087—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
- B01J19/088—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/10—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing sonic or ultrasonic vibrations
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention provides a high-pressure reaction kettle and a control method thereof, wherein the high-pressure reaction kettle comprises: the high-pressure reaction kettle cavity is used for accommodating biomass, solvent and water; the ultrasonic generating device is used for generating cavitation bubbles in the aqueous solution in the cavity of the high-pressure reaction kettle; the high-voltage electrode assembly is used for discharging in the high-voltage reaction kettle cavity to generate plasma; the ultrasonic generating device and the high-voltage electrode assembly act cooperatively, the cavitation bubbles are provided by the ultrasonic generating device, and the high-voltage electrode assembly discharges and loads on the cavitation bubbles to realize discharge and generate plasma, so that the cavitation bubble volume is increased, the solution heating efficiency is improved, and the liquefaction effect of the content of free radicals in the cavitation bubbles is improved.
Description
Technical Field
The invention belongs to the technical field of hydrothermal liquefaction, and relates to a reaction kettle structure for hydrothermal liquefaction, in particular to a high-pressure reaction kettle structure and a control method thereof.
Background
Thermochemical conversion is mostly achieved in the prior art by hydrothermal processes. Hydrothermal process refers to a thermochemical conversion process in which biomass is treated by heating water and a catalyst in a closed system (under a high temperature and high pressure system). Depending on the different parameters (temperature, pressure, solution composition, etc.), the products obtained by hydrothermal methods can be generally classified into three categories: (1) hydrothermal carbonization: when the temperature is 180 ℃ and 250 ℃, the product with the pressure less than 4MPa in the high-pressure kettle is mainly coke; (2) hydrothermal liquefaction: when the temperature of the solution is raised to 200-370 ℃, and the pressure in the high-pressure kettle is 4-20 MPa, the main product is the biological oil; (3) hydrothermal gasification: when the water molecules in the autoclave are in the supercritical condition (the solution temperature is 360-420 ℃, and the pressure in the autoclave is 25-40 MPa), the biomass is converted into the combustible gas H2CO and CH4And the critical point of water molecules is 374.3 ℃ and 22.1 MPa.
In the prior art, the hydrothermal liquefaction technology under the subcritical/supercritical condition does not need to dry the biomass, only water, a solvent and a catalyst need to be added, the structure and chemical properties of water molecules under high temperature and high pressure are greatly changed, macromolecules, hydrolysis products and intermediate products after the biomass degradation can be dissolved, the mass transfer influence is reduced, and the reaction rate is accelerated. The heat value of the liquefied product is as high as 30-35MJ/kg, the number of C atoms of the product is 9-11, and the heat value mainly comprises the following components: acid, glucose, fructose, methylglyoxal and furfural.
However, the hydrothermal liquefaction process under sub/supercritical conditions in the prior art has many disadvantages, most notably high energy consumption, up to 1.8 kilowatts per kilogram, low heating efficiency due to the limitation of conduction heating, more than 50% of the heat being lost during heat conduction, and secondly low efficiency, 45 minutes being required for heating to above 200 ℃, and the subsequent catalytic liquefaction also taking more than 120 minutes. The above disadvantages limit the spread of this technology.
In view of the above problems, an autoclave reactor with low energy consumption and high heating efficiency is a problem to be solved urgently in the industry.
Disclosure of Invention
The invention aims to provide an autoclave reactor and a control method, which improve the liquefaction rate of biomass and shorten the liquefaction time.
The invention provides a high-pressure reaction kettle, which comprises: the high-pressure reaction kettle cavity is used for accommodating biomass, solvent and water; the ultrasonic generating device is used for generating cavitation bubbles in the aqueous solution in the cavity of the high-pressure reaction kettle; the high-voltage electrode assembly is used for discharging in the high-voltage reaction kettle cavity to generate plasma; the ultrasonic generating device and the high-voltage electrode assembly act cooperatively, the cavitation bubbles are provided by the ultrasonic generating device, and the high-voltage electrode assembly discharges and loads on the cavitation bubbles to realize discharge and generate plasma, so that the cavitation bubble volume is increased, the solution heating efficiency is improved, and the liquefaction effect of the content of free radicals in the cavitation bubbles is improved.
As an embodiment of the present invention, the high voltage electrode assembly includes a high voltage electrode and an insulating ceramic plate, wherein the insulating ceramic plate is provided with a circular groove, and the high voltage electrode is embedded therein.
The electrode assembly as another embodiment of the present invention is passed out of the autoclave through an electrode lead assembly, which includes a high voltage electrode lead and an insulating ceramic bushing.
As another embodiment of the present invention, the pressure sensor assembly further comprises a pressure sensor and an insulating ceramic sleeve of the pressure sensor, wherein the pressure sensor is used for measuring the pressure in the high-pressure reaction kettle, and the insulating ceramic sleeve of the pressure sensor is used for isolating the high-pressure reaction kettle from the pressure sensor.
As another embodiment of the present invention, the temperature sensor assembly further comprises a temperature sensor and an insulating ceramic bushing of the temperature sensor, wherein the temperature sensor is used for measuring the temperature of the high-pressure reaction kettle, and the insulating ceramic bushing of the temperature sensor is used for isolating the high-pressure reaction kettle from the temperature sensor.
As another embodiment of the invention, the ultrasonic generating assembly comprises a high-voltage resistant ultrasonic generator, a cylindrical insulating ceramic layer, a cylindrical ground electrode and a high-voltage resistant insulating ceramic sleeve.
In yet another embodiment of the present invention, a high pressure relief valve is further included.
The plasma generator further comprises a plasma power supply, wherein the plasma power supply is loaded on the vacuole through the high-voltage electrode group to discharge to generate plasma.
The ultrasonic generator further comprises an ultrasonic generator power supply, wherein the ultrasonic generator power supply is connected with the ultrasonic generator and is used for driving the ultrasonic generator to output ultrasonic waves.
As another embodiment of the present invention, the biomass is one or more of straw, fat, animal liver, the solvent is one or more of methanol, ethanol, formaldehyde, and acetaldehyde, and the water is one of purified water and distilled water.
The invention also provides a control method of the high-pressure reaction kettle, which comprises the steps of preparing the solution according to the proportion and filling the solution into the cavity of the high-pressure reaction kettle; applying voltage 600-800V to the high-voltage electrode through a plasma power supply; after the solution reaches the first state, regulating the voltage output of the plasma power supply to 1200-1500V; after the solution reaches the second state, continuing for a certain time, completing the liquefaction of the biomass, and gradually reducing the voltage to be closed; the solution was cooled and liquefaction was complete.
As an embodiment of the present invention, the solution reaches the first state, where the solution temperature is 284-505 ℃, the pressure is less than 2.4MPa, and the corresponding loop current is decreased to 0.05-0.1A.
As another embodiment of the present invention, the solution reaches the second state where the solution temperature is 364-.
According to the invention, the ultrasonic generating device and the plasma device are arranged in the high-pressure reaction kettle, so that the ultrasonic and the plasma are in synergistic action in the high-pressure reaction kettle, the content of free radicals is increased, the biological quality is improved, the high-efficiency liquefaction of biomass is realized, the hydrothermal liquefaction time is shortened, and the thermalization efficiency is improved.
Drawings
FIG. 1 is a first schematic structural view of a high-pressure reactor according to the present invention;
FIG. 2 is a schematic structural diagram II of a high-pressure reaction kettle according to the present invention;
FIG. 3 is a schematic structural view of an ultrasound generating assembly of the present invention;
FIG. 4 is a schematic top view of a ground electrode of the present invention;
FIG. 5 is a schematic diagram of a ground electrode of the present invention in cross-section;
FIG. 6 is an overall cross-sectional view of an ultrasound generating assembly of the present invention;
FIG. 7 is a schematic structural view of a temperature sensor assembly according to the present invention;
FIG. 8 is a schematic diagram of the pressure sensor assembly of the present invention;
FIG. 9 is a schematic view of a high voltage electrode assembly of the present invention;
FIG. 10 is a schematic view of an electrode lead out assembly according to the present invention;
FIG. 11 is a graph of discharge current for a first state of the present invention;
FIG. 12 is a second state discharge current graph according to the present invention.
Detailed Description
In order to overcome the defects of large energy loss, low heating efficiency, low free radical content, low bio-oil quality and the like in the conduction heating process, the invention improves the high-pressure autoclave reactor and the control method thereof, and the invention is specifically described by combining the attached drawings as follows:
the structure of the high-pressure kettle reactor is improved, the high-pressure kettle reactor is provided with a high-voltage electrode, a ground electrode, an ultrasonic device, a pressure sensing device and a temperature detection device, water, biomass and a solvent are added into the reaction kettle, and parameters between the ultrasonic device and the high-voltage electrode and between the high-voltage electrode and the ground electrode are adjusted to realize the synergistic effect of the ultrasonic and the plasma, so that the efficient liquefaction of the biomass is realized. The synergistic process can increase the content of free radicals and improve the quality of the bio-oil, and the specific synergistic process is as follows:
when the ultrasonic device is started, the water solution can generate vacuoles with the diameter less than 10 microns in the reaction kettle under the ultrasonic action,wherein the vacuole contains gaseous water molecules, electrons, -OH, -H and-HO as main components2Equal free radical (content about 10)16m3) The ultrasound device is not capable of heating the solution, but the ultrasound may provide bubbles to the solution, which provide the gas needed for the discharge for the plasma discharge, when the bubbles are located between the high voltage electrode and the ground electrode, the bubbles are ionized to generate plasma, and the plasma generated by the discharge can significantly increase the volume and the free radical content (the content is about 10) of the bubbles23m3). Meanwhile, the process of plasma generated by discharge can effectively heat the solution, so that the temperature is rapidly increased to realize liquefaction. Therefore, when the ultrasonic device and the plasma act together, firstly, the ultrasonic action provides cavitation bubbles, and the plasma power supply 9 loads the output signals of the high-voltage electrode and the ground electrode on the cavitation bubbles to realize discharge so as to generate plasma. The plasma not only obviously increases the volume of the vacuole and effectively heats the solution, but also increases the liquefaction effect of the content of free radicals in the vacuole.
The following are respectively specific descriptions of the structures of the present invention:
the high-pressure reaction kettle of the invention has a specific structure as shown in figure 1, and is provided with a high-pressure reaction kettle cavity 1, a high-pressure electrode assembly 2, a high-pressure electrode 2-1, an insulating ceramic plate 2-2, an electrode lead-out wire assembly 3, an electrode lead-out wire 3-1, an insulating ceramic bushing 3-2, a high-pressure resistant insulating ceramic bushing 4, an ultrasonic generating assembly 5, a high-pressure resistant ultrasonic generator 5-1, a cylindrical insulating ceramic layer 5-2, a cylindrical ground electrode 5-3, a high-pressure resistant insulating ceramic bushing 5-4, a temperature sensor assembly 6, a temperature sensor 6-1, an insulating ceramic bushing 6-2 of a temperature sensor, a pressure sensor assembly 7, a pressure sensor 7-1, an insulating ceramic bushing 7-2 of a pressure sensor, a high-pressure safety valve 8, a plasma power supply 9 and, a temperature sensor power supply 11, a pressure sensor power supply 12; the autoclave reaction cavity 1 is filled with biomass, solvent and water for reaction, wherein the cylindrical ground electrode wrapping layer 5-3 is connected with the ground electrode of the plasma power supply 9, and the electrode leading-out wire 3-1 is connected with the ground electrode of the plasma power supply 9.
The high-pressure autoclave reaction cavity 1 of the reaction kettle is cylindrical, the diameter is 10-50cm, the thickness is more than 12mm, and the reaction cavity can be made of one of stainless steel, tungsten-molybdenum alloy and the like. The high-voltage electrode assembly 2 is composed of two parts, a high-voltage electrode 2-1 is embedded in an insulating ceramic plate 2-2 provided with a circular groove, and the high-voltage electrode 2-1 can be made of one of tungsten, molybdenum, tungsten-molybdenum alloy and the like. The electrode lead-out wire assembly 3 comprises two parts, one is a high-voltage electrode lead-out wire 3-1, and the other is an insulating ceramic sleeve 3-2; the high-voltage electrode lead-out wire 3-1 is connected with the high-voltage electrode 2-1 from the side surface, the outer part of the high-voltage electrode lead-out wire is sleeved with an insulating ceramic sleeve 3-2, the insulating ceramic sleeve 3-2 passing through the high-voltage resistant electrode penetrates out of the high-voltage reaction kettle and is connected with the high-voltage output end of the plasma power supply 9. Wherein the high-voltage electrode lead-out wire 3-1 can be one of copper, steel, aluminum, tungsten, molybdenum, tungsten-molybdenum alloy and the like; the insulating ceramic sleeve 3-2 can be one of insulating inert inorganic materials such as ceramics, corundum and the like; the high-voltage electrode lead-out wire 3-1 is tightly matched with the insulating ceramic sleeve 3-2, and the middle part is fixed by high-temperature and high-voltage resistant ceramic glue; the insulating ceramic sleeve 3-2 can be made of insulating inert inorganic materials such as ceramics, corundum and the like.
The ultrasonic generating assembly 5 comprises four components of a high-voltage resistant ultrasonic generator 5-1, a cylindrical insulating ceramic layer 5-2, a cylindrical ground electrode 5-3 and a high-voltage resistant insulating ceramic sleeve 5-4, wherein the output power of the high-voltage resistant ultrasonic generator 5-1 is 200-2000 watts, the frequency is 25-130 kHz, when the power is lower than 200 watts, enough cavitation bubbles cannot be provided, and when the power is higher than 2000 watts, the cavitation bubble combination phenomenon occurs, so that the synergistic effect of plasma and cavitation bubbles is not facilitated. The cylindrical insulating ceramic layer 5-2 is used for isolating the ultrasonic generating device from a ground electrode, so that the ultrasonic generating device is prevented from being influenced by the current of the ground electrode, the material used by the cylindrical insulating ceramic layer 5-2 can be ceramic, corundum and other insulating inert inorganic materials, the cylindrical insulating ceramic layer is tightly matched with the high-pressure resistant ultrasonic generator 5-1, and the middle part of the cylindrical insulating ceramic layer is filled and fixed by high-temperature and high-pressure resistant ceramic glue. The cylindrical ground electrode 5-3 is tightly matched with the cylindrical insulating ceramic layer 5-2, the material can be one of tungsten, molybdenum and tungsten-molybdenum alloy materials, and the middle part is filled and fixed by high-temperature and high-pressure resistant ceramic glue. The high-voltage resistant insulating ceramic sleeve 5-4 can be made of insulating inert inorganic materials such as ceramics, corundum and the like, and is tightly matched with the cylindrical ground electrode 5-3 and the high-pressure reaction kettle.
The temperature sensor assembly 6 is composed of a temperature sensor 6-1 and an insulating ceramic sleeve 6-2 of the temperature sensor, wherein the temperature sensor 6-1 can be one of a platinum resistance thermometer, a thermocouple thermometer and a semiconductor thermometer and is used for measuring the temperature in the high-pressure reaction kettle. The insulating ceramic sleeve 6-2 of the temperature sensor is used for isolating the high-pressure reaction kettle from the temperature sensor 6-1, the material of the insulating ceramic sleeve can be ceramic, corundum and other insulating inert inorganic materials, the insulating ceramic sleeve is tightly matched with the temperature sensor, and the middle of the insulating ceramic sleeve is filled and fixed by high-temperature and high-pressure resistant ceramic glue. The temperature measuring range of the temperature sensor is-10-600 ℃.
The pressure sensor assembly 7 is composed of a pressure sensor 7-1 and an insulating ceramic sleeve 7-2 of the pressure sensor, wherein the pressure sensor 7-1 is used for measuring the pressure in the high-pressure reaction kettle and can be one of a semiconductor piezoelectric resistance type pressure transmitter, a static capacitance type pressure transmitter and a diffused silicon pressure transmitter. The insulating ceramic sleeve 7-2 of the pressure sensor is used for isolating the high-pressure reaction kettle from the pressure sensor, the material of the insulating ceramic sleeve can be ceramic, corundum and other insulating inert inorganic materials, the insulating ceramic sleeve is tightly matched with the pressure sensor, and the middle of the insulating ceramic sleeve is filled and fixed by high-temperature and high-pressure resistant ceramic glue.
The reaction kettle can also be provided with a high-pressure safety valve 8, wherein the high-pressure safety valve 8 is a safety protection valve and is used for preventing the high-pressure reaction kettle from bursting due to overhigh pressure, and the opening pressure of the high-pressure reaction kettle is not lower than 10 MPa. It may be selected from one of a hammer type, a lever type, a spring type and a pilot type, and in a preferred embodiment of the present invention is one of DN 6-200.
The plasma power supply 9 of the invention is loaded on the vacuole (generated by the ultrasonic generating device) through the high-voltage electrode and the ground electrode to generate discharge plasma, and the output parameters of the power supply can be selected as follows: can be 200-2000V, the frequency is 50 Hz-50 kHz, and stable plasma can be generated in the solution; the volume of the vacuole generated by the ultrasonic generating device can be obviously reduced along with the increase of the temperature and the pressure in the high-pressure reaction kettle, the voltage needs to be increased to continuously discharge, and the discharge parameters are as follows: can be 1200-1500V, the frequency is 50 Hz-50 kHz, the output power is 2000-10000W, and the output waveform can be one of sine wave, square wave and the like.
The power supply of the ultrasonic generating device is connected with the ultrasonic generating device and used for driving the ultrasonic generating device to output ultrasonic waves, and the parameters are as follows: DC-1 MHz, maximum output voltage 1000Vpp, output current 0-1.5A, output power 200 + 1000W, and the output waveform can be one of sine wave, square wave, etc., and can be automatically matched with an ultrasonic generating device.
The temperature sensor power supply 11 of the invention is connected with the temperature sensor 6-1, and can be adapted to the corresponding power supply according to the type of the temperature sensor. The pressure sensor power supply 12 of the invention is connected with the pressure sensor 7-1, the pressure sensor is used for converting the detected pressure signal into pressure intensity, and the measuring range of the pressure sensor is as follows: 0 to 10 MPa.
The reaction kettle comprises a reaction cavity 1 for accommodating reacted biomass, a solvent and water, wherein the biomass can be one or more of straws, excrement, fat and animal livers; the solvent can be one or more of methanol, ethanol, formaldehyde and acetaldehyde; the water may be one of purified water and distilled water.
In one embodiment, the reaction mixture contained in the reaction vessel of the present invention has the following composition ratio and reaction results: 5g of straws, 12ml of methanol and 8.4ml of purified water, and the specific gravity of the product is up to 82.2 percent after liquefaction, and the product is: acetic acids (5.8%), D-glucopyranose (7.6%), glucose (11.7%), levulinic acid (12.5%), fructose (9.2%), methylglyoxal (10.9%), furfural (20.8%), pyridine and the like.
In another embodiment, the reaction kettle of the present invention contains the following reaction substances according to the following composition ratio and the reaction result: 5g of straws, 12ml of mixed solution (2:1) of methanol and ethanol and 8.4ml of purified water, and the specific gravity of the product is up to 81.4 percent after liquefaction, wherein the product mainly comprises: acetic acids (4.2%), D-glucopyranose (4.8%), glucose (9.7%), levulinic acid (14.5%), fructose (8.2%), methylglyoxal (11.7%), furfural (27.4%), pyridine and the like.
In another embodiment, the reaction mixture contained in the reaction vessel of the present invention has the following composition ratio and reaction result: 5g of straws, 10ml of formaldehyde and 9.6ml of purified water, and the specific gravity of the product is up to 78.3 percent after liquefaction, and the product is: acetic acids (3.1%), D-glucopyranose (2.5%), glucose (8.8%), levulinic acid (19.5%), fructose (3.2%), methylglyoxal (16.7%), furfural (24.4%), pyridine and the like.
In another embodiment, the reaction mixture contained in the reaction vessel of the present invention has the following composition ratio and reaction results: 5g of straw, 10ml of mixed solution (2:1) of formaldehyde and acetaldehyde and 9.6ml of purified water, and the specific gravity of the product is up to 77.3 percent after liquefaction, and the product is: acetic acids (1.7%), D-glucopyranose (4.8%), glucose (9.7%), levulinic acid (14.5%), fructose (8.2%), methylglyoxal (11.7%), furfural (27.4%) and pyridine.
In another embodiment, the reaction mixture contained in the reaction vessel of the present invention has the following composition ratio and reaction results: 5g of straws, 10ml of mixed solution (2:1) of methanol and formaldehyde and 9.6ml of purified water, and the specific gravity of the product is up to 74.3 percent after liquefaction, and the product is: acetic acids (2.2%), D-glucopyranose (6.3%), glucose (7.9%), levulinic acid (11.8%), fructose (6.2%), methylglyoxal (16.9%), furfural (48.7%), pyridine and the like.
The specific operation and control method of the reaction kettle of the invention is as follows: preparing solution according to the proportion, putting the solution into a reaction cavity, applying voltage to the high-voltage electrode 2-1 through a plasma power supply 9, when the voltage is 800V for 600-. Then, the plasma power voltage is continuously increased to 1200-1500V, the frequency is increased to 500Hz, and the voltage-current curve diagram is shown in FIG. 12. Then the solution temperature and pressure are continuously increased, at this time, the solution in the high-pressure reaction kettle reaches a second state, the solution temperature in the high-pressure reaction kettle is 364-. After the state lasts for a certain time, the time is determined to be 30 minutes in the preferred embodiment of the invention, the biomass liquefaction is completed, the voltage is gradually reduced until the power supply is turned off, and the liquefaction is finished after the biomass is cooled for 120 minutes.
Aiming at the problems of high energy consumption and low heating efficiency of a high-pressure reaction kettle in the hydrothermal liquefaction process in the prior art, the structure of the high-pressure reaction kettle is improved, an ultrasonic device and a plasma power supply are arranged, the ultrasonic action and the plasma action are utilized to work cooperatively, cavitation bubbles are provided by the ultrasonic action, and the plasma power supply is loaded on the cavitation bubbles through a high-voltage electrode to realize discharge and generate plasma. The plasma not only obviously increases the volume of the vacuole and effectively heats the solution, but also increases the liquefaction effect of the content of free radicals in the vacuole, reduces the energy consumption and improves the heating efficiency.
The above embodiments are only specific illustrations for explaining the technical solutions of the present invention, and are not intended to limit the specific protection scope of the present invention, and the laser welding apparatus of the present invention is not limited in any way, and all simple modifications, equivalent changes and modifications made according to the technical spirit of the present invention are still within the technical solutions of the present invention.
Claims (13)
1. An autoclave, comprising:
the high-pressure reaction kettle cavity is used for accommodating biomass, solvent and water;
the ultrasonic generating device is used for generating cavitation bubbles in the aqueous solution in the cavity of the high-pressure reaction kettle;
the high-voltage electrode assembly is used for discharging in the high-voltage reaction kettle cavity to generate plasma;
the ultrasonic generating device and the high-voltage electrode assembly act cooperatively, the cavitation bubbles are provided by the ultrasonic generating device, and the high-voltage electrode assembly discharges and loads on the cavitation bubbles to realize discharge and generate plasma, so that the cavitation bubble volume is increased, the solution heating efficiency is improved, and the liquefaction effect of the content of free radicals in the cavitation bubbles is improved.
2. The autoclave of claim 1, wherein the high-voltage electrode assembly comprises a high-voltage electrode and an insulating ceramic plate, the insulating ceramic plate is provided with a circular groove, and the high-voltage electrode is embedded in the insulating ceramic plate.
3. The autoclave of claim 2, wherein the high-voltage electrode assembly protrudes from the autoclave through an electrode lead assembly comprising a high-voltage electrode lead and an insulating ceramic bushing.
4. The autoclave of claim 1, further comprising a pressure sensor assembly including a pressure sensor for measuring pressure within the autoclave and an insulating ceramic sleeve of the pressure sensor for isolating the autoclave from the pressure sensor.
5. The autoclave of claim 1, further comprising a temperature sensor assembly including a temperature sensor for measuring the temperature of the autoclave and an insulating ceramic bushing for the temperature sensor for isolating the autoclave from the temperature sensor.
6. The autoclave of claim 1, wherein the ultrasonic generating assembly comprises a high-pressure resistant ultrasonic generator, a cylindrical insulating ceramic layer, a cylindrical ground electrode, and a high-pressure resistant insulating ceramic bushing.
7. The autoclave of claim 1, further comprising a high pressure relief valve.
8. The autoclave of claim 1, further comprising a plasma power supply, wherein the plasma power supply is loaded on the cavitation bubbles through a high voltage electrode assembly to generate a plasma by discharging.
9. The autoclave of claim 1, further comprising an ultrasonic generator power supply connected to the ultrasonic generator for driving the ultrasonic generator to output ultrasonic waves.
10. The autoclave of claim 1, wherein the biomass is one or more of straw, vegetable oil, fat, and animal liver, the solvent is one or more of methanol, ethanol, formaldehyde, and acetaldehyde, and the water is one of purified water and distilled water.
11. A method of controlling an autoclave as claimed in any one of the preceding claims 1 to 10, comprising the steps of:
(1) preparing solution according to the proportion, and filling the solution into a cavity of a high-pressure reaction kettle;
(2) applying voltage 600-800V to the high-voltage electrode through the plasma power supply;
(3) after the solution reaches the first state, regulating the voltage output of the plasma power supply to 1200-1500V;
(4) after the solution reaches the second state, continuing for a certain time, completing the liquefaction of the biomass, and gradually reducing the voltage to be closed;
(5) and cooling the solution, and finishing liquefaction.
12. The control method as described in claim 11, wherein the solution reaches the first state where the solution temperature is 284-505 ℃, the pressure is less than 2.4MPa, and the corresponding loop current is decreased to 0.05-0.1A.
13. The control method as described in claim 11, wherein the solution reaching the second state is a solution temperature of 364-.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010951594.XA CN112090371B (en) | 2020-09-11 | 2020-09-11 | High-pressure reaction kettle and control method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010951594.XA CN112090371B (en) | 2020-09-11 | 2020-09-11 | High-pressure reaction kettle and control method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112090371A true CN112090371A (en) | 2020-12-18 |
| CN112090371B CN112090371B (en) | 2021-06-22 |
Family
ID=73751342
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010951594.XA Expired - Fee Related CN112090371B (en) | 2020-09-11 | 2020-09-11 | High-pressure reaction kettle and control method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112090371B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115818918A (en) * | 2023-02-06 | 2023-03-21 | 杨思泽 | Method for treating excrement by plasma electrolytic liquefaction |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015181180A1 (en) * | 2014-05-26 | 2015-12-03 | MWK Bionik GmbH | Production method and apparatus for microbiologically converting gases |
| CN108636310A (en) * | 2018-05-31 | 2018-10-12 | 厦门大学 | Plasma electrolysis liquefying plant |
| CN109689198A (en) * | 2016-01-25 | 2019-04-26 | 明尼苏达大学董事会 | Liqu id plasmas tapping equipment and the method for synthesizing biologic diesel oil for using it |
| CN109692637A (en) * | 2019-01-22 | 2019-04-30 | 华中科技大学 | A kind of integral type electric discharge device and liquid discharge system |
| WO2019132693A1 (en) * | 2017-12-27 | 2019-07-04 | Сергей Сергеевич КАЦУБА | Technological complex for ultrasonic hydrothermal cleaning of ceramic material from cast turbine blades |
| CN110237799A (en) * | 2019-07-15 | 2019-09-17 | 诸暨市瀚海环保科技有限公司 | A kind of biomass cellulose hydrothermal liquefaction high pressure reaction assembly |
| CN110713853A (en) * | 2019-10-24 | 2020-01-21 | 江苏大学 | Method for utilizing oily wastewater by combining electro-catalysis with algae |
-
2020
- 2020-09-11 CN CN202010951594.XA patent/CN112090371B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015181180A1 (en) * | 2014-05-26 | 2015-12-03 | MWK Bionik GmbH | Production method and apparatus for microbiologically converting gases |
| CN109689198A (en) * | 2016-01-25 | 2019-04-26 | 明尼苏达大学董事会 | Liqu id plasmas tapping equipment and the method for synthesizing biologic diesel oil for using it |
| WO2019132693A1 (en) * | 2017-12-27 | 2019-07-04 | Сергей Сергеевич КАЦУБА | Technological complex for ultrasonic hydrothermal cleaning of ceramic material from cast turbine blades |
| CN108636310A (en) * | 2018-05-31 | 2018-10-12 | 厦门大学 | Plasma electrolysis liquefying plant |
| CN109692637A (en) * | 2019-01-22 | 2019-04-30 | 华中科技大学 | A kind of integral type electric discharge device and liquid discharge system |
| CN110237799A (en) * | 2019-07-15 | 2019-09-17 | 诸暨市瀚海环保科技有限公司 | A kind of biomass cellulose hydrothermal liquefaction high pressure reaction assembly |
| CN110713853A (en) * | 2019-10-24 | 2020-01-21 | 江苏大学 | Method for utilizing oily wastewater by combining electro-catalysis with algae |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115818918A (en) * | 2023-02-06 | 2023-03-21 | 杨思泽 | Method for treating excrement by plasma electrolytic liquefaction |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112090371B (en) | 2021-06-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112090371B (en) | High-pressure reaction kettle and control method thereof | |
| Zhang et al. | Changes of gallic acid mediated by ultrasound in a model extraction solution | |
| Loow et al. | Role of energy irradiation in aiding pretreatment of lignocellulosic biomass for improving reducing sugar recovery | |
| Li et al. | Pyrolysis behavior of hydrochar from hydrothermal carbonization of pinewood sawdust | |
| CA2722879C (en) | Processing biomass and petroleum containing materials | |
| US9988651B2 (en) | Processes for increasing bioalcohol yield from biomass | |
| JP2018061960A (en) | Processing for material | |
| US10745776B2 (en) | Method and device for increasing laser-induced shock wave pressure | |
| Sharma et al. | A comprehensive review of renewable energy production from biomass-derived bio-oil | |
| EP2647716A1 (en) | Processing biomass | |
| US20130274527A1 (en) | Method For The Dissolving And Rapid Hydrolyzing Of Lignocellulose Biomass, Device Thereof And Use Of the Same | |
| US20220010216A1 (en) | Continuous Operation Method for Microwave High-Temperature Pyrolysis of Solid Material Comprising Organic Matter | |
| IL225700A (en) | Method comprising treating a biomass feedstock to produce sugars | |
| JP2010512998A5 (en) | ||
| Bundhoo et al. | Promising unconventional pretreatments for lignocellulosic biomass | |
| Brahim et al. | Impact of ultrasounds and high voltage electrical discharges on physico-chemical properties of rapeseed straw’s lignin and pulps | |
| Gallego-García et al. | Recent advances on physical technologies for the pretreatment of food waste and lignocellulosic residues | |
| BR112018015196B1 (en) | PLASMA REACTOR AND PROCESS FOR FEEDING THE FLOW OF REAGENT COMPOUNDS TO A PLASMA REACTOR AND DISCHARGE | |
| WO2011103180A2 (en) | Process for hydrolysis of wet fiber and method for producing fermentation products from wet fiber | |
| Zhang et al. | A review of aviation oil production from organic wastes through thermochemical technologies | |
| Ling et al. | Roles of physical fields in the extraction of pectin from plant food wastes and byproducts: A systematic review | |
| US20080311637A1 (en) | Apparatus and methods for ethanol production | |
| Mudassir et al. | Plasma-assisted hydrodeoxygenation of bio-oils | |
| CN101224407A (en) | Ultrasound microwave chemical reactor | |
| CN106006621A (en) | Preparing method for multilayer graphene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20210622 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |