阅读说明：本技术 微波热解油页岩装置 (Microwave pyrolysis oil shale device ) 是由 李术元 何璐 马跃 岳长涛 于 2019-11-05 设计创作，主要内容包括：本申请公开一种微波热解油页岩装置,该装置包括：用于容纳微波的谐振腔；至少部分伸入所述谐振腔内的反应容器,所述反应容器用于放置油页岩；与所述反应容器相连的进气部,所述进气部用于向所述反应容器内输入惰性气体；与所述反应容器相连的油气收集部,所述油气收集部用于收集所述油页岩热解后生成的油气。该微波热解油页岩装置能有效利用油页岩,提高热解后页岩油的收率、页岩热解气的收率及热值,并且能实现页岩油脱硫脱氮脱氧。(The application discloses microwave pyrolysis oil shale device, the device includes: a resonant cavity for containing microwaves; a reaction vessel extending at least partially into the resonant cavity, the reaction vessel being adapted to receive oil shale; the gas inlet part is connected with the reaction vessel and is used for inputting inert gas into the reaction vessel; and the oil gas collecting part is connected with the reaction container and is used for collecting oil gas generated after the oil shale is pyrolyzed. The microwave oil shale pyrolysis device can effectively utilize oil shale, improve the yield of the pyrolyzed shale oil and the yield and the heat value of the shale pyrolysis gas, and realize desulfurization, denitrification and deoxidation of the shale oil.)

1. A microwave pyrolysis oil shale device, characterized by includes:

a resonant cavity for containing microwaves;

a reaction vessel extending at least partially into the resonant cavity, the reaction vessel being adapted to receive oil shale;

the gas inlet part is connected with the reaction vessel and is used for inputting inert gas into the reaction vessel;

and the oil gas collecting part is connected with the reaction container and is used for collecting oil gas generated after the oil shale is pyrolyzed.

2. The microwave oil shale pyrolysis apparatus of claim 1, further comprising a microwave emitting portion for emitting microwaves to the resonant cavity, wherein the microwave emitting portion comprises a magnetron and a waveguide connected to each other, the waveguide is disposed between the magnetron and the resonant cavity, the waveguide is connected to the resonant cavity, the magnetron is used for emitting microwaves, and the waveguide is used for transmitting the microwaves emitted by the magnetron into the resonant cavity.

3. The apparatus according to claim 2, wherein there are two microwave emitting portions, and the two microwave emitting portions are disposed at different heights on different sides of the resonant cavity.

4. The apparatus according to claim 1, wherein a container for holding the oil shale is disposed in the reaction container, a sealing cover is disposed on a top of the reaction container, and the sealing cover is provided with a first opening connected to the gas inlet portion and a second opening connected to the oil and gas collecting portion.

5. The apparatus according to claim 4, wherein the reaction vessel and the holding vessel are made of quartz; the reaction vessel is arranged on the central axis of the resonant cavity.

6. The apparatus according to claim 4, wherein the sealing cover further has a third opening, and the third opening has a thermocouple extending into the container, and the thermocouple is in contact with the oil shale but not in contact with the container; the microwave pyrolysis oil shale device further comprises:

the infrared thermometer is extended into the resonant cavity and used for measuring the internal temperature of the resonant cavity;

and the control part is electrically connected with the thermocouple and the infrared thermometer.

7. The microwave pyrolysis oil shale apparatus of claim 1, further comprising a housing, the housing being disposed outside the resonant cavity, the housing being made of metal.

8. The microwave pyrolysis oil shale apparatus of claim 1, wherein the air inlet portion comprises:

a gas cylinder for storing the inert gas;

an air inlet line connecting the cylinder to the reaction vessel;

the valve is arranged at one end of the air inlet pipeline close to the air bottle;

the first gas flowmeter is arranged on the gas inlet pipeline and positioned between the valve and the reaction container;

and the carrier gas guide pipe is connected with the gas inlet pipeline and extends into the reaction container to be close to the bottom of the reaction container.

9. The microwave pyrolysis oil shale apparatus of claim 1, wherein the oil and gas collection portion comprises:

an oil gas output pipe connected with the reaction vessel;

the insulating heating belt is arranged outside the oil-gas output pipe and used for heating oil gas in the oil-gas output pipe;

the condenser is connected with the oil-gas output pipe and is positioned at the downstream of the oil-gas output pipe and used for cooling oil gas generated after the oil shale is pyrolyzed;

the liquid collecting container is connected with the condenser and is used for collecting the liquid passing through the condenser;

and the air bag is connected with the condenser and is used for collecting the gas passing through the condenser.

10. The apparatus according to claim 9, wherein there are five condensers, and the oil and gas collecting portion further comprises a thermostat connected to the condensers for providing circulating condensate to the condensers; and a second gas flow meter is arranged at the upstream of the gas bag.

Technical Field

The application relates to the technical field of oil shale pyrolysis, in particular to a microwave oil shale pyrolysis device.

Background

The oil shale has huge reserves and feasibility of development and utilization, and is an important petroleum supplementary energy source. Oil shale is a sedimentary rock with a framework of inorganic mineral matter and contains solid organic matter, mainly kerogen and a small amount of asphaltenes. Oil shale is a solid fossil fuel, and is heated to 450-. The shale oil can be directly used as liquid fuel for marine turbines, or used for producing products such as gasoline, kerosene, diesel oil, paraffin and the like through a rectification process, and the shale pyrolysis gas can be used as fuel gas, coal gas or chemical gas through benzene removal and acid gas removal.

At present, the most effective and perfect oil shale pyrolysis technology is the aboveground dry distillation technology, namely, the oil shale is exploited out of the ground and then is subjected to dry distillation by a production device to obtain a product. The more important oil shale pyrolysis process in the world comprises a Chinese pacific process, a Brazilian peterol jack process, a Esania Kulotte process and the like. However, these conventional oil shale pyrolysis processes have the following disadvantages:

(1) the oil shale material is heated by adopting heat conduction and heat convection, namely, heat is firstly transferred to the surface of the oil shale, and then the central temperature is gradually increased by heat conduction. The external heating mode has the advantages of low speed, low efficiency, uneven heating of the oil shale and high energy consumption, increases the production cost for enterprises, has no economic advantages, and does not accord with the environmental protection concept;

(2) shale oil yield is not high. Taking the smoothing process of China as an example, the shale oil yield of the smoothing furnace is about 65% of that of an aluminum retort (standard method for measuring the oil content of oil shale) for low-grade oil shale, and can only reach 80% for high-grade oil shale, so that resource waste is caused;

(3) the shale oil produced by pyrolysis contains a large amount of non-hydrocarbon organic compounds such as sulfur, nitrogen, oxygen and the like. If shale oil is used directly as fuel oil, the large amounts of sulfur, nitrogen, and oxygen compounds can cause difficulties in its storage, transportation, and utilization, such as fuel instability, increased viscosity, gum formation and discoloration, pollutant emissions, and the like. If the shale oil is used for producing oil products, the shale oil needs to be subjected to deep processing treatment. However, the downstream processing of shale oil is more complex than petroleum processing, its reaction conditions are severe, hydrodenitrogenation efficiency is low, nitrogen compounds inhibit hydrodesulfurization/oxygen, catalysts are easily deactivated, equipment is easily corroded, etc.;

(4) the shale pyrolysis gas generated by pyrolysis has low yield and low calorific value, and the shale pyrolysis gas with low calorific value can not be used as gas for coal gas and chemical industry, can only be used as gas for fuel, and is not beneficial to the comprehensive utilization of the oil shale.

In summary, the existing oil shale pyrolysis technology has the problems of low comprehensive utilization efficiency of oil shale, environmental pollution and the like.

Disclosure of Invention

In view of the defects of the prior art, one of the purposes of the present application is to provide a microwave oil shale pyrolysis device, which can effectively utilize oil shale, improve the yield of the pyrolyzed shale oil and the yield and calorific value of the shale pyrolysis gas, and realize desulfurization, denitrification and deoxidation of the shale oil.

In order to achieve the purpose, the technical scheme is as follows:

an apparatus for microwave pyrolysis of oil shale, comprising:

a resonant cavity for containing microwaves;

a reaction vessel extending at least partially into the resonant cavity, the reaction vessel being adapted to receive oil shale;

the gas inlet part is connected with the reaction vessel and is used for inputting inert gas into the reaction vessel;

and the oil gas collecting part is connected with the reaction container and is used for collecting oil gas generated after the oil shale is pyrolyzed.

As a preferred embodiment, the microwave oil shale pyrolysis apparatus further includes a microwave emitting portion that emits microwaves to the resonant cavity, the microwave emitting portion includes a magnetron and a waveguide that are connected to each other, the waveguide is disposed between the magnetron and the resonant cavity, the waveguide is connected to the resonant cavity, the magnetron is configured to emit microwaves, and the waveguide is configured to transmit the microwaves emitted by the magnetron into the resonant cavity.

In a preferred embodiment, there are two microwave emitting portions, and the two microwave emitting portions are disposed at different heights on different sides of the resonant cavity.

As a preferred embodiment, a container for placing the oil shale is arranged in the reaction container, a sealing cover is arranged at the top of the reaction container, and a first opening connected with the air inlet part and a second opening connected with the oil gas collecting part are arranged on the sealing cover.

In a preferred embodiment, the reaction vessel and the holding vessel are made of quartz; the reaction vessel is arranged on the central axis of the resonant cavity.

As a preferred embodiment, a third opening is further formed in the sealing cover, a thermocouple extending into the holding container is arranged in the third opening, and the thermocouple is in contact with the oil shale but not in contact with the holding container; the microwave pyrolysis oil shale device further comprises:

the infrared thermometer is extended into the resonant cavity and used for measuring the internal temperature of the resonant cavity;

and the control part is electrically connected with the thermocouple and the infrared thermometer.

As a preferred embodiment, the microwave oil shale pyrolysis device further comprises a housing, the housing is arranged outside the resonant cavity, and the housing is made of metal.

As a preferred embodiment, the air intake portion includes:

a gas cylinder for storing the inert gas;

an air inlet line connecting the cylinder to the reaction vessel;

the valve is arranged at one end of the air inlet pipeline close to the air bottle;

the first gas flowmeter is arranged on the gas inlet pipeline and positioned between the valve and the reaction container;

and the carrier gas guide pipe is connected with the gas inlet pipeline and extends into the reaction container to be close to the bottom of the reaction container.

As a preferred embodiment, the oil and gas collecting portion includes:

an oil gas output pipe connected with the reaction vessel;

the insulating heating belt is arranged outside the oil-gas output pipe and used for heating oil gas in the oil-gas output pipe;

the condenser is connected with the oil-gas output pipe and is positioned at the downstream of the oil-gas output pipe and used for cooling oil gas generated after the oil shale is pyrolyzed;

the liquid collecting container is connected with the condenser and is used for collecting the liquid passing through the condenser;

and the air bag is connected with the condenser and is used for collecting the gas passing through the condenser.

In a preferred embodiment, the number of the condensers is five, and the oil gas collecting part further comprises a thermostat, wherein the thermostat is connected with the condenser and is used for providing circulating condensate for the condenser; and a second gas flow meter is arranged at the upstream of the gas bag.

Has the advantages that:

the microwave pyrolysis oil shale device that this application embodiment provided adopts microwave pyrolysis oil shale through setting up the resonant cavity, can effectively utilize oil shale, improves the yield of pyrolysis back shale oil, the yield and the calorific value of shale pyrolysis gas to can realize shale oil desulfurization denitrogenation deoxidation. The inert gas is purged into the reaction vessel through the gas inlet portion, and the air in the reaction vessel can be discharged before the pyrolysis starts. The inert gas that the high temperature oil gas that produces will get into the reaction vessel in the pyrolysis process heats through the heat transfer, and the condensable steam that the pyrolysis produced can get into oil gas collection portion under high temperature inert gas's the carrying, avoids the internal wall of reaction vessel to glue shale oil. The device is beneficial to collecting more shale oil into the oil-gas collecting part, improves the oil collecting efficiency and the accuracy of measuring the shale oil yield, fully utilizes the heat of the pyrolysis process to heat the inert gas, and improves the comprehensive utilization efficiency of the heat.

Specifically, the yield of shale oil obtained by using the device for microwave pyrolysis of oil shale provided by the embodiment of the application is 5.95%. The oil content of the oil shale used in this embodiment was 6.62% as determined by the standard aluminum retort method, and since 5.95%/6.62% ═ 89.88%, the shale oil produced herein was 90.00% of the standard aluminum retort method. Namely the shale oil production efficiency of the device is about 90 percent. This shows that the microwave pyrolysis oil shale device that this application embodiment provided can obtain higher shale oil yield.

By using the device for microwave pyrolysis of oil shale, the sulfur content in the prepared shale oil is 2.21%, the sulfur content in the shale oil prepared by pyrolysis of oil shale in the traditional method is 9.26%, and because (9.26% -2.21%)/9.26% ═ 76.13%, the sulfur content in the shale oil prepared by pyrolysis in the device is reduced by 76.13% compared with the sulfur content in the shale oil prepared by pyrolysis of oil shale in the traditional method. This shows that the microwave pyrolysis oil shale device that this application embodiment provided has good desulfurization effect.

By using the device for microwave pyrolysis of oil shale, the nitrogen content in the prepared shale oil is 1.05%, the nitrogen content in the shale oil prepared by pyrolysis of oil shale in the traditional method is 1.21%, and because (1.21% -1.05%)/1.21% ═ 13.22%, the nitrogen content in the shale oil prepared by pyrolysis in the device is reduced by 13.22% compared with the nitrogen content in the shale oil prepared by pyrolysis of oil shale in the traditional method. This shows that the microwave pyrolysis oil shale device provided by the embodiment of the application has a good denitrification effect.

By using the device for microwave pyrolysis of oil shale, the oxygen content in the prepared shale oil is 2.67%, the oxygen content in the shale oil prepared by pyrolysis of oil shale by the traditional method is 3.59%, and because (3.59% -2.67%)/3.59% ═ 25.63%, the oxygen content in the shale oil prepared by pyrolysis by using the device is reduced by 25.63% compared with the oxygen content in the shale oil prepared by pyrolysis of oil shale by the traditional method. This shows that the microwave pyrolysis oil shale device provided by the embodiment of the application has a good deoxidation effect.

By using the device for microwave pyrolysis of oil shale, the yield of the prepared shale gas is 5.78%, the yield of the shale gas prepared by pyrolysis of oil shale in the traditional method is 4.12%, and because (5.78% -4.12%)/4.12% ═ 40.29%, the yield of the shale gas prepared by pyrolysis in the device is improved by 40.29% compared with the yield of the shale gas prepared by pyrolysis of oil shale in the traditional method. This shows that the microwave pyrolysis oil shale device that this application embodiment provided can obtain higher shale gas yield.

By utilizing the device for microwave pyrolysis of the oil shale, the calorific value of the prepared shale gas is 38528.97kJ/m³(kilojoules per cubic meter), the calorific value of the shale gas prepared by pyrolyzing the oil shale by the traditional method is 27404.16kJ/m3, and because (38528.97-27404.16)/27404.16 is 40.60%, the calorific value of the shale gas prepared by pyrolyzing the oil shale by the device is improved by 40.60% compared with the calorific value of the shale gas prepared by pyrolyzing the oil shale by the traditional method. This shows that the microwave pyrolysis oil shale device provided by the embodiment of the application can obtain higher shale gas calorific value.

The data show that the device for microwave pyrolysis of the oil shale effectively reduces the content of non-hydrocarbon organic compounds such as sulfur, nitrogen and oxygen in the prepared shale oil and improves the yield and the heat value of the shale gas under the condition of ensuring the yield of the prepared shale oil.

Specific embodiments of the present application are disclosed in detail with reference to the following description and drawings, indicating the manner in which the principles of the application may be employed. It should be understood that the embodiments of the present application are not so limited in scope.

Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments, in combination with or instead of the features of the other embodiments.

It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps or components.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without inventive exercise.

Fig. 1 is a schematic structural diagram of an apparatus for microwave pyrolysis of oil shale according to an embodiment of the present disclosure.

Description of reference numerals:

1. a housing; 2. a magnetron; 3. a waveguide; 4. a resonant cavity; 5. a holding container; 6. a reaction vessel; 7. a sealing cover; 8. a carrier gas conduit; 9. a gas cylinder; 10. a first gas flow meter; 11. a thermocouple; 12. an infrared thermometer; 13. a control unit; 14. a digital display; 15. an oil gas output pipe; 16. an insulating heating tape; 17. a flask; 18. a thermostat; 19. a second gas flow meter; 20. an air bag; 21. a spherical condenser tube.

Detailed Description

In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

It will be understood that when an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

In the oil shale industry, no energy-saving device or method is available for realizing desulfurization, denitrification and deoxidation of shale oil and simultaneously preparing shale pyrolysis gas with high yield and high calorific value in the process of pyrolyzing oil shale by using microwaves.

Microwaves are non-ionizing electromagnetic energy with a wavelength of 1cm-1m and a corresponding frequency of 300MHz-300 GHz. The microwave pyrolysis is to generate internal friction heat through the high-frequency reciprocating motion of dipole molecules in a heated body so as to increase the temperature of the heated material, namely, electromagnetic energy directly acts on medium molecules to be converted into heat without heat conduction. The transmission performance of microwave pyrolysis enables the inner medium and the outer medium of the material to be heated and heated simultaneously, and the microwave pyrolysis device has the advantages of high heating speed, uniform heating, energy conservation, high efficiency, sensitive reaction, convenience in operation and the like, and can shorten the process time, improve the productivity and reduce the cost. In order to improve the utilization ratio of oil shale, overcome prior art's not enough, this application has proposed a microwave pyrolysis oil shale device.

For convenience of explanation, the left-hand direction of the reader facing fig. 1 is defined as "up" and the right-hand direction of the reader facing fig. 1 is defined as "down" in this specification.

Please refer to fig. 1. The utility model provides a microwave pyrolysis oil shale device in the embodiment of this application, the device includes: a resonant cavity 4, a reaction vessel 6, an air inlet part and an oil gas collecting part.

Wherein the resonant cavity 4 is used for accommodating microwaves. The reaction vessel 6 is used for placing oil shale. The reaction vessel 6 extends at least partially into the resonant cavity 4 for microwave pyrolysis of oil shale therein. The gas inlet is connected to the reaction vessel 6. The gas inlet is used for inputting inert gas into the reaction container 6. The oil gas collecting part is connected with the reaction vessel 6. The oil gas collecting part is used for collecting oil gas generated after the oil shale is pyrolyzed.

The microwave pyrolysis oil shale device that this application embodiment provided adopts microwave pyrolysis oil shale through setting up resonant cavity 4, can effectively utilize oil shale, improves the yield of pyrolysis back shale oil and shale pyrolysis gas to can realize shale oil desulfurization denitrogenation deoxidation. The reaction vessel 6 is purged with an inert gas through the gas inlet portion, and the air in the reaction vessel 6 can be discharged before the pyrolysis starts. The inert gas that will get into reaction vessel 6 is heated to the high temperature oil gas that produces among the pyrolysis process through the heat transfer, and the condensable steam that the pyrolysis produced can get into oil gas collection portion under high temperature inert gas's the carrying, avoids reaction vessel 6's internal wall to glue shale oil. The device is beneficial to collecting more shale oil into the oil-gas collecting part, improves the oil collecting efficiency and the accuracy of measuring the shale oil yield, fully utilizes the heat of the pyrolysis process to heat the inert gas, and improves the comprehensive utilization efficiency of the heat.

Specifically, the yield of shale oil obtained by using the device for microwave pyrolysis of oil shale provided by the embodiment of the application is 5.95%. The oil content of the oil shale used in this embodiment was 6.62% as determined by the standard aluminum retort method, and since 5.95%/6.62% ═ 89.88%, the shale oil produced herein was 90.00% of the standard aluminum retort method. Namely the shale oil production efficiency of the device is about 90 percent. This shows that the microwave pyrolysis oil shale device that this application embodiment provided can obtain higher shale oil yield.

By using the device for microwave pyrolysis of oil shale, the sulfur content in the prepared shale oil is 2.21%, the sulfur content in the shale oil prepared by pyrolysis of oil shale in the traditional method is 9.26%, and because (9.26% -2.21%)/9.26% ═ 76.13%, the sulfur content in the shale oil prepared by pyrolysis in the device is reduced by 76.13% compared with the sulfur content in the shale oil prepared by pyrolysis of oil shale in the traditional method. This shows that the microwave pyrolysis oil shale device that this application embodiment provided has good desulfurization effect.

By using the device for microwave pyrolysis of oil shale, the nitrogen content in the prepared shale oil is 1.05%, the nitrogen content in the shale oil prepared by pyrolysis of oil shale in the traditional method is 1.21%, and because (1.21% -1.05%)/1.21% ═ 13.22%, the nitrogen content in the shale oil prepared by pyrolysis in the device is reduced by 13.22% compared with the nitrogen content in the shale oil prepared by pyrolysis of oil shale in the traditional method. This shows that the microwave pyrolysis oil shale device provided by the embodiment of the application has a good denitrification effect.

By using the device for microwave pyrolysis of oil shale, the oxygen content in the prepared shale oil is 2.67%, the oxygen content in the shale oil prepared by pyrolysis of oil shale by the traditional method is 3.59%, and because (3.59% -2.67%)/3.59% ═ 25.63%, the oxygen content in the shale oil prepared by pyrolysis by using the device is reduced by 25.63% compared with the oxygen content in the shale oil prepared by pyrolysis of oil shale by the traditional method. This shows that the microwave pyrolysis oil shale device provided by the embodiment of the application has a good deoxidation effect.

By using the device for microwave pyrolysis of oil shale, the yield of the prepared shale gas is 5.78%, the yield of the shale gas prepared by pyrolysis of oil shale in the traditional method is 4.12%, and because (5.78% -4.12%)/4.12% ═ 40.29%, the yield of the shale gas prepared by pyrolysis in the device is improved by 40.29% compared with the yield of the shale gas prepared by pyrolysis of oil shale in the traditional method. This shows that the microwave pyrolysis oil shale device that this application embodiment provided can obtain higher shale gas yield.

By utilizing the device for microwave pyrolysis of the oil shale, the calorific value of the prepared shale gas is 38528.97kJ/m³(kilojoules per cubic meter), the calorific value of the shale gas prepared by pyrolyzing the oil shale by the traditional method is 27404.16kJ/m3, and because (38528.97-27404.16)/27404.16 is 40.60%, the calorific value of the shale gas prepared by pyrolyzing the oil shale by the device is improved by 40.60% compared with the calorific value of the shale gas prepared by pyrolyzing the oil shale by the traditional method. This shows that the microwave pyrolysis oil shale device provided by the embodiment of the application can obtain higher shale gas calorific value.

The data show that the device for microwave pyrolysis of the oil shale effectively reduces the content of non-hydrocarbon organic compounds such as sulfur, nitrogen and oxygen in the prepared shale oil and improves the yield and the heat value of the shale gas under the condition of ensuring the yield of the prepared shale oil.

In a microwave field, substances with stronger polarity are easier to absorb microwaves so as to vibrate and break bonds, and carbon-sulfur bonds, carbon-nitrogen bonds and carbon-oxygen bonds have polarity and are easy to break under the action of microwaves. Due to the particularity of the microwave action mechanism, the size, shape, internal cavity volume and material volume ratio of the resonant cavity 4 and the like influence the material wave-absorbing efficiency, thereby influencing the action of the microwave and the atoms such as sulfur, nitrogen, oxygen and the like. Therefore, the effects of desulfurization, nitrogen and oxygen of different resonant cavities 4 and the microwave oil shale pyrolysis device are different.

In the embodiment of the present application, the resonant cavity 4 may be a metal cavity. Since the metal does not absorb the microwaves but reflects them. The shape of the resonant cavity 4 is not limited in the present application, and may be, for example, a rectangular parallelepiped, a cylinder, or another shape. In a preferred embodiment, the resonant cavity 4 has a rectangular parallelepiped shape, which allows the volume of the resonant cavity 4 to be larger. The microwaves are transmitted into the interior of the resonant cavity 4 and reflected therein until they are absorbed by the oil shale. The cavity 4 may be a multi-mode cavity 4, i.e. the microwaves are stable within the cavity 4. Because the microwave is continuously reflected inside the resonant cavity 4, a plurality of "modes" are formed in the resonant cavity 4, and the more modes in the resonant cavity 4, the more the distribution structure of the electromagnetic field is, and the more uniform the distribution of the microwave energy in the resonant cavity 4 is.

In the embodiment of the present application, the microwave oil shale pyrolysis apparatus further includes a microwave emitting portion that emits microwaves to the resonant cavity 4. The microwave emitting part may include a magnetron 2 and a waveguide 3 connected thereto. The waveguide 3 is arranged between the magnetron 2 and the resonant cavity 4. The waveguide 3 is connected to the resonant cavity 4. The magnetron 2 is used for emitting microwaves, and the waveguide 3 is used for transmitting the microwaves emitted by the magnetron 2 into the resonant cavity 4.

Specifically, the microwave emitting portion has two, that is, two magnetrons 2 and two waveguides 3. The two microwave emitting parts are arranged at different heights on different sides of the resonant cavity 4, so that the microwave field can be more completely and uniformly covered in the resonant cavity 4. Different height values can be calculated and selected by integrating multiple factors such as the angle (the incident angle and the reflection angle) of the microwave entering the resonant cavity 4, the size of the resonant cavity 4, the position of the material (oil shale), the installation of other devices and the like, and the height value is not limited in the application.

In the embodiment of the application, a holding container 5 for holding the oil shale is arranged in the reaction container 6, so that the mass of the oil shale and the mass of the solid product can be conveniently weighed before and after the reaction. As quartz is transparent to microwaves, microwaves are not absorbed in the reaction process, and the reaction vessel 6 and the containing vessel 5 are resistant to high temperature, and can be made of quartz. The shape of the reaction vessel 6 is not limited in the present embodiment, and preferably, the reaction vessel 6 is a cylindrical tube.

The holding container 5 may be a quartz crucible. Because the microwaves are repeatedly reflected within the confined cavity 4, the microwave distribution within the cavity 4 is uniform. In a preferred embodiment, the reaction vessel 6 is located on the central axis of the resonant cavity 4 to ensure that the oil shale absorbs microwaves uniformly. The oil shale is heated uniformly, so that the pyrolysis speed is high, the time required by the oil shale pyrolysis can be shortened, and the energy consumption is reduced. As shown in fig. 1, the reaction vessel 6 and the resonant cavity 4 are both arranged along a vertical direction, and the reaction vessel 6 is located on a central axis of the resonant cavity 4.

And a sealing cover 7 is arranged at the top of the reaction container 6, so that the pyrolysis reaction is conveniently carried out. The sealing cover 7 is firm, pressure-resistant, high-temperature resistant, non-reactive with high-temperature oil gas and corrosion resistant. The sealing cover 7 may be made of stainless steel material. The sealing cover 7 and the reaction vessel 6 can be connected through double flanges, so that the sealing performance is ensured. The sealing cover 7 is provided with a first opening connected with the air inlet part and a second opening connected with the oil-gas collecting part. The junction of first opening and air inlet portion, the junction of second opening and oil gas collection portion all are equipped with seal assembly, make reaction vessel 6 leakproofness good. The inert gas is continuously blown and air cannot enter, so that the oil shale is pyrolyzed under the inert gas atmosphere.

In the present embodiment, the sealing cover 7 may further have a third opening. A thermocouple 11 extending into the holding container 5 is arranged in the third opening. And a sealing fitting is arranged at the joint of the thermocouple 11 and the third opening, so that the reaction container 6 has good sealing property. The height of the thermocouple 11 is adjusted before the pyrolysis reaction starts, so that the thermocouple 11 is in contact with the oil shale and is not in contact with the holding container 5, and is used for measuring the real-time temperature in the pyrolysis process of the oil shale and the central temperature of the oil shale. The thermocouple 11 may be a type K thermocouple 11.

Specifically, the microwave oil shale pyrolysis device may further include an infrared thermometer 12 extending into the resonant cavity 4, and configured to measure the internal temperature of the resonant cavity 4, that is, the surface temperature of the oil shale. The infrared thermometer 12 may be embedded in the lower end of the side wall of the resonant cavity 4, and the temperature measuring end thereof is communicated with the cavity of the resonant cavity 4.

The apparatus for microwave pyrolysis of oil shale may further include a control part 13. The control unit 13 is electrically connected to the thermocouple 11, and the control unit 13 is electrically connected to the infrared thermometer 12. The control unit 13 can select a temperature measurement method: the temperature is measured by the thermocouple 11 or by the infrared thermometer 12 or by both.

In addition, the control part 13 may also be electrically connected with the magnetron 2 of the microwave emitting part to switch different microwave heating modes, such as a continuous heating mode, a final temperature-keeping heating mode, and the like. A continuous heating mode, i.e. heating for a certain time at a certain microwave power, can be realized by setting the microwave power and the heating time before pyrolysis; the final temperature-heat preservation heating mode, namely, heating to the set final temperature under certain microwave power and then preserving heat at the temperature for a certain time, can be realized by setting the microwave power, the final temperature and the heat preservation time before pyrolysis. The control unit 13 may also set reaction parameters, control the magnetron 2 to start or stop, and store reaction data. Provides favorable conditions for deep research of microwave pyrolysis oil shale in laboratories.

The control section 13 may also be provided with a digital display 14 for displaying the data collected by the control section 13. As a visual window of the control unit 13, an operator can set reaction parameters, observe real-time data during a reaction process, start or stop the operation of the apparatus, copy data, and the like through an operation panel of the digital display 14.

In the embodiment of the present application, the microwave oil shale pyrolysis device further comprises a housing 1. The housing 1 is arranged outside the resonant cavity 4. The housing 1 is made of metal. The metal is firm, can play supporting, fixed action to its inside device is protected. The metal has good heat resistance, and when heat generated by heating the inside of the resonant cavity 4 is transferred outwards, the metal shell 1 is not easy to be damaged by heat. The connection of the reaction vessel 6 and the sealing cap 7 may be located outside the metal casing 1.

In the present embodiment, the gas inlet portion includes a gas cylinder 9, a gas inlet line, a valve, a first gas flow meter 10, and a carrier gas conduit 8. The gas cylinder 9 is used for storing inert gas, such as nitrogen, argon, helium, etc., which is also referred to as carrier gas, hereinafter, supplied to the entire apparatus. In this embodiment, nitrogen gas is selected as an example. The gas inlet line connects the gas cylinder 9 to the reaction vessel 6 and is secured by means of a securing fitting. The gas inlet line may be connected to the reaction vessel 6 via a first opening in the sealing lid 7. The valve is arranged at one end of the air inlet pipeline close to the air bottle 9 and used for controlling the opening and closing of the air bottle 9. The first gas flowmeter 10 is arranged on the gas inlet pipeline and positioned between the valve and the reaction container 6, and is used for measuring the gas flow rate. The first gas flow meter 10 may be a rotameter. The carrier gas conduit 8 is connected to the gas inlet line and extends into the reaction vessel 6 near the bottom of the reaction vessel 6.

In the intake line, the flow rate of the carrier gas measured by the first gas flow meter 10 is preferably in the range of 50 to 300 mL/min. The carrier gas plays a role in purging oil gas generated by pyrolysis to the oil gas collecting part in the pyrolysis process. When oil gas stays in the reaction vessel 6, microwave is further absorbed for secondary reaction. The carrier gas flow rate determines the residence time of the oil gas in the quartz reactor. Thus, the carrier gas flow rate may affect the product composition of microwave pyrolysis oil shale.

Preferably, the carrier gas conduit 8 is a cylindrical quartz tube with a diameter of 1cm, although it may be of a different shape in other embodiments. The inlet line may be a rubber tube through which the inlet of the carrier gas conduit 8 communicates with the gas cylinder 9. The outlet of the carrier gas conduit 8 is disposed at the bottom end of the reaction vessel 6. In addition, the outlet of the carrier gas conduit 8 may be located outside the holding container 5. The carrier gas conduit 8 is used for conveying inert gas into the reaction container 6, and meanwhile, the oil shale material is prevented from being blown out of the containing container 5 by the gas flow, so that the accuracy of the experiment is enhanced. And the high-temperature oil gas generated in the pyrolysis process can heat the inert gas, condensable steam generated by microwave pyrolysis enters the oil gas collecting part under the carrying of high-temperature carrier gas, shale oil is prevented from being adhered to the inner wall surfaces of the reaction container 6 and the sealing cover 7, the shale oil is favorably collected into the oil gas collecting part as much as possible, the oil collecting efficiency and the accuracy of determining the yield of the shale oil are improved, meanwhile, the heat generated in the pyrolysis process is fully utilized for heating the carrier gas, and the comprehensive utilization efficiency of the heat is improved.

In the present embodiment, the oil and gas collecting portion includes an oil and gas output pipe 15, an insulating heating belt 16, a condenser, a liquid collecting container, and an air bag 20. Wherein the oil gas output pipe 15 is connected with the reaction vessel 6. The oil gas output pipe 15 can be connected with the reaction vessel 6 through a second opening on the sealing cover 7 and is fixed through a fixing fitting. The insulating heating belt 16 is arranged outside the oil gas output pipe 15 and used for heating oil gas in the oil gas output pipe 15. The insulating heating belt 16 may be provided with a temperature controller for maintaining the temperature of the insulating heating belt 16 at a certain appropriate value, for example, 200 ℃. The winding of insulating heating area 16 is in the outside of oil gas output tube 15, avoids inside and outside difference in temperature too big to cause to glue shale oil and then block up oil gas output tube 15 in the oil gas output tube 15, is favorable to the collection and the separation of oil gas result, has improved the accuracy of collection oil efficiency and survey shale oil output, has strengthened the security simultaneously.

The outlet of the oil gas output pipe 15 is connected with a condenser, and oil gas generated by the oil shale pyrolysis enters the condenser through the oil gas output pipe 15. The oil gas output pipe 15 is a linkage junction of the oil shale microwave pyrolysis part and the oil gas condensation part. The condenser can cool the oil gas generated after the oil shale is pyrolyzed. And high-temperature oil gas generated by pyrolysis is divided into a condensable part and a non-condensable part after being condensed. The liquid collecting container is connected with the condenser and is used for collecting liquid passing through the condenser, namely a condensable part. The gas bag 20 is connected to the condenser for collecting the gas after passing through the condenser, i.e., the non-condensable portion. A second gas flow meter 19 may be provided upstream of the gas pocket 20 for metering the volume of shale pyrolysis gas. The second gas flow meter 19 may be a wet gas flow meter. By using the container 5, the liquid collecting container and the air bag 20, the device can separate and collect solid, liquid and gas products generated by pyrolysis and perform quantitative analysis.

In a preferred embodiment, there are five condensers, i.e., five condensers. The five-stage condenser can be connected by five spherical condenser pipes 21 and three flasks 17 through rubber conduits. Three of the flasks 17 served as liquid collection vessels. The oil and gas collecting part is also provided with a thermostat 18. The thermostat 18 is connected to the condenser for providing circulating condensate to the condenser. The thermostat 18 may be provided with a circulation pump to provide power. The thermostat 18 regulates the temperature of the circulating condensate. In particular, the recycle condensate may be ethanol, which may be at a temperature of-10 ℃.

In a specific application scenario, when the microwave oil shale pyrolysis device provided by the embodiment of the present application is used for oil shale pyrolysis, the microwave oil shale pyrolysis device may include the following steps:

step 1: placing oil shale (oil content is 6.62%, diameter is less than or equal to 3mm) in a containing container 5, placing the containing container 5 in a reaction container 6, inserting a K-type thermocouple 11 into the oil shale without touching the containing container 5, covering a stainless steel sealing cover 7 on the reaction container 6, sealing by two flanges, hermetically connecting the whole set of device according to the figure 1, setting the temperature of an insulating heating belt 16 to be 200 ℃, and starting to heat;

step 2: conveying nitrogen to the reaction container 6 from a gas bottle 9, measuring the flow rate of the nitrogen by a first gas flowmeter 10, wherein the constant speed is 150mL/min, recording the initial volume displayed by a second gas flowmeter 19, introducing the nitrogen into the reaction container 6 through a carrier gas conduit 8, and continuously purging by carrier gas until the whole reaction is finished;

and step 3: the heating mode is switched to a final temperature-heat preservation mode through a digital display 14, the temperature measurement mode of a K-type thermocouple 11 is selected, and reaction parameters are set as follows: microwave power is 600W, reaction final temperature is 520 ℃, temperature difference is 5 ℃, and heat preservation time is 20min, ethanol is pumped to a five-stage condenser through a thermostat 18 to be used as circulating condensate, and the temperature of the ethanol is set to be-10 ℃;

and 4, step 4: after nitrogen is introduced for 20min, a microwave emission source is started, the magnetron 2 emits microwaves to the resonant cavity 4, the temperature of the microwaves absorbed by oil shale in the reaction container 6 is increased, the temperature of the oil shale is monitored in real time by the K-type thermocouple 11 and stored, when the temperature reaches 525 ℃, the control part 13 sends a stop signal to the magnetron 2, the magnetron 2 stops emitting the microwaves at the moment, the temperature of the oil shale is reduced along with the temperature, when the temperature is reduced to 515 ℃, the control part 13 sends a start signal to the magnetron 2, the magnetron 2 starts emitting the microwaves at the moment, the temperature of the oil shale is increased along with the temperature, and the reaction is finished when the temperature is maintained for 20min repeatedly;

and 5: due to nitrogen purging, oil gas products generated in the oil shale pyrolysis process enter the five-stage condenser through an oil gas output pipe 15, a condensable part is shale oil and is stored in a flask 17, and a non-condensable part is shale pyrolysis gas and is stored in an air bag 20;

step 6: when no more white oil gas enters at the inlet of the five-stage condenser, the cylinder 9 valve is closed and the end volume indicated by the second gas flow meter 19 is recorded.

It should be noted that, in the description of the present application, the terms "first", "second", and the like are used for descriptive purposes only and for distinguishing similar objects, and no precedence between the two is intended or should be construed to indicate or imply relative importance. In addition, in the description of the present application, "a plurality" means two or more unless otherwise specified.

Any numerical value recited herein includes all values from the lower value to the upper value, in increments of one unit, provided that there is a separation of at least two units between any lower value and any higher value. For example, if it is stated that the number of a component or a value of a process variable (e.g., temperature, pressure, time, etc.) is from 1 to 90, preferably from 20 to 80, and more preferably from 30 to 70, it is intended that equivalents such as 15 to 85, 22 to 68, 43 to 51, 30 to 32 are also expressly enumerated in this specification. For values less than 1, one unit is suitably considered to be 0.0001, 0.001, 0.01, 0.1. These are only examples of what is intended to be explicitly recited, and all possible combinations of numerical values between the lowest value and the highest value that are explicitly recited in the specification in a similar manner are to be considered.

Unless otherwise indicated, all ranges include the endpoints and all numbers between the endpoints. The use of "about" or "approximately" with a range applies to both endpoints of the range. Thus, "about 20 to about 30" is intended to cover "about 20 to about 30", including at least the endpoints specified.

All articles and references disclosed, including patent applications and publications, are hereby incorporated by reference for all purposes. The term "consisting essentially of …" describing a combination shall include the identified element, ingredient, component or step as well as other elements, ingredients, components or steps that do not materially affect the basic novel characteristics of the combination. The use of the terms "comprising" or "including" to describe combinations of elements, components, or steps herein also contemplates embodiments that consist essentially of such elements, components, or steps. By using the term "may" herein, it is intended to indicate that any of the described attributes that "may" include are optional.

A plurality of elements, components, parts or steps can be provided by a single integrated element, component, part or step. Alternatively, a single integrated element, component, part or step may be divided into separate plural elements, components, parts or steps. The disclosure of "a" or "an" to describe an element, ingredient, component or step is not intended to foreclose other elements, ingredients, components or steps.

It is to be understood that the above description is intended to be illustrative, and not restrictive. Many embodiments and many applications other than the examples provided will be apparent to those of skill in the art upon reading the above description. The scope of the present teachings should, therefore, be determined not with reference to the above description, but should instead be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are hereby incorporated by reference for all purposes. The omission in the foregoing claims of any aspect of subject matter that is disclosed herein is not intended to forego such subject matter, nor should the inventors be construed as having contemplated such subject matter as being part of the disclosed subject matter.