CN103816850A - A pyrolysis method and device with controllable microwave output energy per unit mass reactant - Google Patents
A pyrolysis method and device with controllable microwave output energy per unit mass reactant Download PDFInfo
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- 239000000376 reactant Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000197 pyrolysis Methods 0.000 title abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- 238000005336 cracking Methods 0.000 claims description 62
- 238000003860 storage Methods 0.000 claims description 22
- 239000010453 quartz Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 16
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 14
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 14
- 239000000498 cooling water Substances 0.000 claims description 11
- 241001269238 Data Species 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910000323 aluminium silicate Inorganic materials 0.000 claims description 5
- 230000007797 corrosion Effects 0.000 claims description 5
- 238000005260 corrosion Methods 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- 239000011094 fiberboard Substances 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- 238000003776 cleavage reaction Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 230000007017 scission Effects 0.000 claims description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 238000004891 communication Methods 0.000 claims description 2
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- 238000005259 measurement Methods 0.000 abstract description 2
- 239000004215 Carbon black (E152) Substances 0.000 abstract 1
- 238000009529 body temperature measurement Methods 0.000 abstract 1
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- 238000009833 condensation Methods 0.000 abstract 1
- 230000007423 decrease Effects 0.000 abstract 1
- 229930195733 hydrocarbon Natural products 0.000 abstract 1
- 150000002430 hydrocarbons Chemical class 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 24
- 230000001105 regulatory effect Effects 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 11
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Natural products CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 4
- 230000000740 bleeding effect Effects 0.000 description 4
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical group O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 238000004260 weight control Methods 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 241000609240 Ambelania acida Species 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 2
- 235000017491 Bambusa tulda Nutrition 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 244000082204 Phyllostachys viridis Species 0.000 description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000010905 bagasse Substances 0.000 description 2
- 239000011425 bamboo Substances 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 240000006766 Cornus mas Species 0.000 description 1
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- 239000010696 ester oil Substances 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
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- 238000005303 weighing Methods 0.000 description 1
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Abstract
一种单位质量反应物微波输出能量可控的裂解方法及装置，所述的方法是随反应物质量减小或反应时间的延长，通过自动控制降低微波功率，保证反应物在整个裂解过程中单位质量微波输出能量保持恒定。装置包括微波腔体、微波发生器、质量测定系统，温度测定的系统、PLC实时数据采集控制系统、实时显示腔体内物料图像系统、后台计算机组态软件采集与控制系统、冷凝系统、负压系统。本发明提供的装置自动化程度高，操作简便，采用本发明可以获得多种反应物在最佳的微波条件下裂解得到高品质的烃类燃料和绿色化学品等，反应物具有工业化应用前景。
A pyrolysis method and device with controllable microwave output energy per unit mass of reactant. The method is to reduce the microwave power through automatic control as the mass of the reactant decreases or the reaction time prolongs, so as to ensure that the reactant is in the whole pyrolysis process. The mass microwave output energy remains constant. The device includes a microwave cavity, a microwave generator, a quality measurement system, a temperature measurement system, a PLC real-time data acquisition control system, a real-time display system for material images in the cavity, a background computer configuration software acquisition and control system, a condensation system, and a negative pressure system. . The device provided by the invention has a high degree of automation and is easy to operate. By adopting the invention, various reactants can be cracked under optimal microwave conditions to obtain high-quality hydrocarbon fuels and green chemicals. The reactants have industrial application prospects.
Description
Technical field
The invention belongs to biomass energy and oil and fat chemical energy field.
Background technology
The temperature difference in tradition cracking oil plant crop reaction system between the each position of material is very big, in hot biography process, more there is not the material base to the preferential heat supply of polar functional group, therefore in traditional cracking process, the fracture order of chemical bond shows as randomness and uncontrollability, cause pyrolysis product very complicated, particularly auxiliary cracking (the Microwave Assisted Pyrolysis of the high microwave of oxygenatedchemicals quantity, MAP) can significantly improve the catalysis directionality of biomass cracking, thereby it is good selective that pyrolysis product is shown.
Microwave cracking reactor is the key that biomass cracking is prepared green chemical technology, although microwave cracking technology makes great progress, the research of this one side of microwave cracking stove not enough.Microwave cracking stove has merged the advantages such as heating is rapid, good uniformity, convenient operation control through the development of several generations, but do not realize all the time unit mass reactant and absorb the controlled cracking technology of microwave, generally, in microwave cracking process, reactant constantly reduces along with the carrying out quality of cracking reaction, but microwave output power does not but change, therefore cause the reactant absorption microwave of reaction later stage unit mass too much, temperature sharply rises, and then generation pyrogenetic reaction, affect the quality of green chemical; In addition, the unnecessary microwave not absorbed by reactant may affect magnetron, causes reduce service life.
In addition, the heating mechanism that microwave is special and traditional heat conduction heating has very large difference, therefore studies that reactant react under the condition of heating using microwave and weightless rule is necessary, particularly larger for size, the reactant of difficult pulverizing.
Summary of the invention
The object of the invention is to make up existing microwave cracking stove and can not realize the controlled deficiency of unit mass reactant absorption microwave, propose a kind of controlled microwave cracking method of unit mass reactant microwave output energy, the present invention also provides a kind of for realizing said method microwave cracking device in addition.
The present invention is achieved by the following technical solutions.
The controlled cleavage method of a kind of unit mass reactant microwave output energy of the present invention, it is characterized in that reducing or the prolongation in reaction time with reactant quality, reduce microwave power by automatic control, guarantee that reactant unit mass microwave output energy reserving in whole cracking process is constant.
The controlled cracker of a kind of unit mass reactant microwave output energy of the present invention comprises lower margin balancing (1), seal box (2), precision balance (3), polytetrafluoroethylene (PTFE) mass sensor (4), microwave generator (5), quartz reactor (6), corrosion resistant plate (7), aluminosilicate fiberboard (8), air inlet (9), gas outlet (10), microwave cracking instrument switch (11), LED shows touch control screen (12), cracking cavity (13), non-contact infrared thermometer (14), camera (15), gas storage cylinder (16), flowmeter (17), computer (18), cooling water recirculation system (19), condenser (20), liquid collection tank (21), aspiration pump (22).
Lower margin balancing (1) is arranged on four inferior horns of furnace body chassis, and the cracking cavity (13) that is positioned at upper of furnace body is divided into inside and outside two-layer, and internal layer is aluminosilicate fiberboard (8), and skin is corrosion resistant plate (7); Cracking cavity (13) left and right sides is provided with microwave generator (5), and the positive upper right corner is provided with microwave cracking instrument switch (11) and LED shows touch control screen (12); Camera (15) is equipped with in its inside; Precision balance (3) is arranged in the seal box (2) of lower portion of furnace body, and is connected with the scale pan that is positioned at cracking cavity (13) by polytetrafluoroethylene (PTFE) mass sensor (4); Quartz reactor (6) is placed on the scale pan, and reactant is positioned in quartz reactor (6); Non-contact infrared thermometer (14) is positioned at quartz reactor (6) top; The both sides of cracking cavity (13) are respectively equipped with air inlet (9) and gas outlet (10), quartz reactor (6) passes air inlet (9) by silicone tube and is connected to gas storage cylinder (16), is connected to condenser (20) by another silicone tube through gas outlet (10); The other end of condenser (20) is connected with liquid collection tank (21), aspiration pump (22) successively, and condenser (20) is connected to cooling water recirculation system (19) simultaneously; Gas storage cylinder (16) is equipped with flowmeter (17) and valve.Computer (18) is connected to LED by DOL Data Output Line and shows touch control screen (12).
The scale pan of the present invention is the circular polytetrafluoroethylmaterial material that scribbles alumina silicate.
Pressure type in polytetrafluoroethylene (PTFE) mass sensor of the present invention (4) employing, the degree of accuracy is 0.01g, range of weighing 0-1000g can place quartz reactor (6).Microwave along with test mass reduce automatically reduce microwave power (reduce microwave power must not be less than 0.1W).Time controlled system scope 1s-99h, along with the prolongation of equipment task time reduces microwave power (reduce microwave power and must not be less than 0.1W) automatically.
Microwave generator of the present invention (5), its microwave power 0-3K continuous stepless is adjustable, can placing glass reactor in microwave cavity, non-contact infrared thermometer (14) Real-Time Monitoring microwave cavity temperature 0-1200 ℃, when heating material arrives the condition of high temperature, the difference of temperature controlling range upper and lower limit is not less than 50 ℃.
Condenser (20) temperature is by adjustable between cooling water recirculation system (20)-5 ℃-5 ℃.
Negative pressure system can pass through aspiration pump (22) and regulate.
LED shows that touch control screen (12) adopts PLC to carry out time, weight, Temperature Setting control and microwave power and regulates, and touch-screen also shows as man machine operation interface; Camera (15) is equipped with in cracking cavity (13) inside, shows in real time material image in cavity, by digital hard disc video recorder, real-time material image is carried out to digital processing and hard-disc storage, and output image memory is greater than 1500 hours; Background computer (18) is controlled data communication system collection and is recorded the real time datas such as temperature, microwave power, time, weight, image.Possess data list, visual picture shows, real time data demonstration, and historical data shows, hard-disc storage function.
The object of the invention is to make up existing microwave cracking stove and can not realize the controlled deficiency of unit mass reactant absorption microwave, provide and can, along with in course of reaction, programmable reduces microwave power automatically for examination reactant quality reduces with the prolongation of time, guarantee that reactant unit mass microwave output energy exposure in whole cracking process keeps constant.Reduce traditional microwave cracking equipment in the pyrogenetic reaction but occurring that diminishes of cracking late phase reaction amount under high power microwave radiation, guaranteed the high-quality of reactant cracking liquid.Microwave output power can setting and quality, time, temperature measuring system interlink.Quality measurement system is implemented the variation of monitoring reactant; Temperature measuring system is used non-contact infrared thermometer Real-Time Monitoring microwave cavity temperature.Microwave cracking atmosphere can be inert atmosphere or reducing atmosphere, background computer collection and record the real time datas such as temperature, microwave power, time, weight, image.Adopt the present invention can obtain the cracking under best microwave condition of multiple reactant and obtain HC fuel and the green chemical etc. of high-quality.Plant automation degree provided by the invention is high, easy and simple to handle, can further be adapted as the continuous production equipment of industrial applications.
Accompanying drawing explanation
Accompanying drawing is the structural representation of cracker of the present invention.In accompanying drawing, 1 is lower margin balancing, and 2 is seal box, 3 is precision balance, 4 polytetrafluoroethylene (PTFE) mass sensors, and 5 is microwave generator, 6 is quartz reactor, and 7 is aluminosilicate fiberboard, and 8 is corrosion resistant plate, 9 is air inlet, 10 is gas outlet, and 11 is microwave cracking instrument switch, and 12 shield for LED shows touch control, 13 is cracking cavity, 14 is non-contact infrared thermometer, and 15 is camera, and 16 is gas storage cylinder, 17 is flowmeter, 18 is computer, and 19 is cooling water recirculation system, and 20 is condenser, 21 is liquid collection tank, and 22 is aspiration pump.
The specific embodiment
The present invention will be described further by following examples.
Embodiment 1.
By the saponified quartz reactor (6) that adds of wilson dogwood oil dry 500g, quartz reactor (6) is connected respectively to gas storage cylinder (16) and condenser (20), regulate the flowmeter (17) of gas storage (inert gas or reducibility gas) steel cylinder (16) to maximum opening, open the switch of gas storage cylinder (16), control valve, to suitable aperture, washes away reaction system 2 minutes.Regulating the temperature of cooling water recirculation system (20) is 0 ℃, and bleeding regulating pump (22) negative pressure system is adjusted to 0.2bar.Close cracking fire door, open microwave cracking instrument switch (11), show touch control screen (12) selection Weight control pattern by LED, regulating power is 1500W, it is that the every minimizing of 3W/g(reactant quality 1g microwave output power reduces 3W that power-weight automatic control program is set), reaction time 15min, opens starting switch, cracking starts, and background computer (19) gathers and record the real time datas such as temperature, microwave power, time, weight, image.Cracking finishes, and liquid collection tank (21) is collected cracking liquid 420g, and product liquid obtains gasoline 140 g, diesel oil 200g, kerosene 80g through rectifying.
Embodiment 2.
By the saponified Chinese tallow tree ester oil dry 500g quartz reactor (6) that adds, quartz reactor (6) is connected respectively to gas storage cylinder (16) and condenser (20), regulate the flowmeter (17) of gas storage (inert gas or reducibility gas) steel cylinder (16) to maximum opening, open the switch of gas storage cylinder (16), control valve, to suitable aperture, washes away reaction system 2 minutes.Regulating the temperature of cooling water recirculation system (20) is 0 ℃, and bleeding regulating pump (22) negative pressure system is adjusted to 0.2bar.Close cracking fire door, open microwave cracking instrument switch (11), show touch control screen (12) selection Weight control pattern by LED, regulating power is 1500W, it is 4W/g (the every minimizing of reactant quality 1g microwave output power reduces 4W) that power-weight automatic control program is set, and reaction time 15min, opens starting switch, cracking starts, and background computer (19) gathers and record the real time datas such as temperature, microwave power, time, weight, image.Cracking finishes, and liquid collection tank (21) is collected cracking liquid 400g, and product liquid obtains gasoline 60 g, diesel oil 180g, kerosene 160g through rectifying.
Embodiment 3.
200g drying bagasse (10% phosphoric acid is processed rear) is added to quartz reactor (6), quartz reactor (6) is connected respectively to gas storage cylinder (16) and condenser (20), regulate the flowmeter (17) of gas storage (inert gas or reducibility gas) steel cylinder (16) to maximum opening, open the switch of gas storage cylinder (16), control valve, to suitable aperture, washes away reaction system 2 minutes.Regulating the temperature of cooling water recirculation system (20) is 0 ℃, and bleeding regulating pump (22) negative pressure system is adjusted to 0.2bar.Close cracking fire door, open microwave cracking instrument switch (11), show touch control screen (12) selection Weight control pattern by LED, regulating power is 2000W, it is 10W/g (the every minimizing of reactant quality 1g microwave output power reduces 10W) that power-weight automatic control program is set, and reaction time 20min, opens starting switch, cracking starts, and background computer (19) gathers and record the real time datas such as temperature, microwave power, time, weight, image.Cracking finishes, and collects cracking liquid 95g, and bagasse coke 70g, it is acetic acid that product liquid obtains water 55g(main component through rectifying), oil phase 40g(main component is furfural).
Embodiment 4.
By dry 200g bamboo waste (4% phosphoric acid, 8%MgCl
2after processing) add quartz reactor (6), quartz reactor (6) is connected respectively to gas storage cylinder (16) and condenser (20), regulate the flowmeter (17) of gas storage (inert gas or reducibility gas) steel cylinder (16) to maximum opening, open the switch of gas storage cylinder (16), control valve, to suitable aperture, washes away reaction system 2 minutes.Regulating the temperature of cooling water recirculation system (20) is 0 ℃, and bleeding regulating pump (22) negative pressure system is adjusted to 0.2bar.Close cracking fire door, open microwave cracking instrument switch (11), show touch control screen (12) selection Weight control pattern by LED, regulating power is 1800W, and it is 9W/g (the every minimizing of reactant quality 1g, microwave output power reduces 9W) that power-weight automatic control program is set, reaction time 25min, open starting switch, cracking starts, and background computer (19) gathers and record the real time datas such as temperature, microwave power, time, weight, image.Cracking finishes, and collects cracking liquid 85g, and bamboo coke 80g, it is acetic acid that product liquid obtains water 40g(main component through rectifying), oil phase 45g(main component is furfural).
Claims (7)
1. the controlled cleavage method of unit mass reactant microwave output energy, it is characterized in that reducing or the prolongation in reaction time with reactant quality, reduce microwave power by automatic control, guarantee that reactant unit mass microwave output energy reserving in whole cracking process is constant.
2. realize the device of method described in claim 1, it is characterized in that comprising lower margin balancing (1), seal box (2), precision balance (3), polytetrafluoroethylene (PTFE) mass sensor (4), microwave generator (5), quartz reactor (6), corrosion resistant plate (7), aluminosilicate fiberboard (8), air inlet (9), gas outlet (10), microwave cracking instrument switch (11), LED shows touch control screen (12), cracking cavity (13), non-contact infrared thermometer (14), camera (15), gas storage cylinder (16), flowmeter (17), computer (18), cooling water recirculation system (19), condenser (20), liquid collection tank (21), aspiration pump (22), lower margin balancing (1) is arranged on four inferior horns of furnace body chassis, and the cracking cavity (13) that is positioned at upper of furnace body is divided into inside and outside two-layer, and internal layer is aluminosilicate fiberboard (8), and skin is corrosion resistant plate (7), cracking cavity (13) left and right sides is provided with microwave generator (5), and the positive upper right corner is provided with microwave cracking instrument switch (11) and LED shows touch control screen (12), camera (15) is equipped with in its inside, precision balance (3) is arranged in the seal box (2) of lower portion of furnace body, and is connected with the scale pan that is positioned at cracking cavity (13) by polytetrafluoroethylene (PTFE) mass sensor (4), quartz reactor (6) is placed on the scale pan, and reactant is positioned in quartz reactor (6), non-contact infrared thermometer (14) is positioned at quartz reactor (6) top, the both sides of cracking cavity (13) are respectively equipped with air inlet (9) and gas outlet (10), quartz reactor (6) passes air inlet (9) by silicone tube and is connected to gas storage cylinder (16), is connected to condenser (20) by another silicone tube through gas outlet (10), the other end of condenser (20) is connected with liquid collection tank (21), aspiration pump (22) successively, and condenser (20) is connected to cooling water recirculation system (19) simultaneously, gas storage cylinder (16) is equipped with flowmeter (17) and valve, computer (18) is connected to LED by DOL Data Output Line and shows touch control screen (12).
3. device according to claim 2, is characterized in that the described scale pan is the circular polytetrafluoroethylmaterial material that scribbles alumina silicate.
4. device according to claim 2, is characterized in that pressure type in described polytetrafluoroethylene (PTFE) mass sensor (4) employing.
5. device according to claim 2, is characterized in that described microwave generator (5), and its microwave power 0-3K continuous stepless is adjustable; Non-contact infrared thermometer (14) Real-Time Monitoring microwave cavity temperature 0-1200 ℃, when heating material arrives the condition of high temperature, the difference of temperature controlling range upper and lower limit is not less than 50 ℃.
6. device according to claim 2, is characterized in that described condenser (20) temperature is by adjustable between cooling water recirculation system (20)-5 ℃-5 ℃.
7. device according to claim 2, is characterized in that described LED demonstration touch control screen (12) adopts PLC to carry out time, weight, Temperature Setting control and microwave power and regulates, and touch-screen is as man machine operation interface demonstration; Camera (15) is equipped with in cracking cavity (13) inside, shows in real time material image in cavity, by digital hard disc video recorder, real-time material image is carried out to digital processing and hard-disc storage, and output image memory is greater than 1500 hours; Background computer (18) is controlled data communication system collection and is recorded the real time datas such as temperature, microwave power, time, weight, image.
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| CN107051350A (en) * | 2017-05-18 | 2017-08-18 | 华南理工大学 | A kind of double source thermal coupling chemical chain gasification method and its device based on microwave |
| CN112774593A (en) * | 2020-12-31 | 2021-05-11 | 南通瀚蓝机械科技有限公司 | Lysate sealing box |
| CN114309023A (en) * | 2021-11-22 | 2022-04-12 | 中国科学院理化技术研究所 | Low-temperature and low-power carbon-containing material microwave treatment process |
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Application publication date: 20140528 |