CN101613617A - A kind of method of preparing biological oil through vacuum pyrolysis of biomasses - Google Patents
A kind of method of preparing biological oil through vacuum pyrolysis of biomasses Download PDFInfo
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Abstract
The method of preparing biological oil through vacuum pyrolysis of biomasses comprises following flow process: (1) vacuum cracking: add in the reactor through pretreated raw material, and the cracking that under the heating of peripheral tube formula stove, heats up, reactor is built-in with heat-transfer device.(2) condensation: the fugitive constituent under the low temperature (being mainly water vapor) is imported into drying tower, and the fugitive constituent under the high temperature is imported into condensation in the coil condenser, can be implemented in the line sampling in the cracking process.(3) absorb: can not coagulate water vapor in the gas tower that is dried and absorb, nitride and sulfide are absorbed by the bubbling absorption bottle, effectively reduce the pollution of vacuum pump oil.The inventive method has partly solved the problem that lags behind because of the low intensification that brings of biomass heat transfer efficiency in the temperature-rise period and condensation efficiency is low and the problem of online sampling, has tentatively reduced the water content in the bio oil simultaneously.
Description
Technical field
The invention discloses a kind of recovery method of biomass solid waste, particularly a kind of under the certain vacuum degree pyrolysis produce the method for bio oil.
Background technology
Along with the scarcity day by day of fossil energy, biomass energy is enriched with its hypotoxicity, low pollution and reserves and is begun to receive publicity.
Biomass thermal chemical transformation technology is a kind of of Biomass Energy Utilization technology, wherein vacuum cracking is to be the technology of major objective product with the liquid phase bio oil, this technology makes biomass material be converted under certain vacuum degree and temperature can not coagulate combustion gas, three kinds of energy forms of bio oil and coke.Biomass at high temperature at first change into fugitive constituent, and this fugitive constituent is converted into bio oil and can not coagulates combustion gas by behind the condensing works.The composition of fugitive constituent is similar to flue gas, and condensation method commonly used at present is that chilling coagulates.Patent CN101343547A discloses the method that bio oil is produced in a kind of vacuum cracking classification, but the condensing works limitation of design has restricted the productive rate of bio oil, and because whole system is in negative pressure condition, is difficult to realize the online sampling of sample.The condensation of the disclosed cracked oil condensation method of CN1030252A takes time one-level phlegma to the previous stage condensation, may cause the polymerization even the coking of lower boiling heat-sensitive substance.Contain a large amount of moisture in the bio oil of condensation, and miscible with the polar compound height among the bio oil, be difficult to separate.Conventional separation method is owing to the poor heat stability of bio oil is difficult to reach ideal effect, as underpressure distillation.Though method such as column chromatography and molecular distillation can well be isolated moisture, its cost is too high, only is applicable to the separation of produced of high added value product.Moisture in the bio oil is from two portions, a part comes from the free-water of biomass absorption itself, a part comes from the water that cracking produces, and biomass material can be removed free-water through after the drying treatment, but the moisture in still can absorbed air in the process of its transfer and sealing.In addition, in the cracked starting stage, owing to be in low-pressure state in the still, gas content is few, and biomass itself are the poor conductors of heat, so there is hysteresis quality in its heat transfer, thereby has increased the heating-up time of biomass.
Summary of the invention
Technical problem: the purpose of the method for the present invention is that provides a kind of method of preparing biological oil through vacuum pyrolysis of biomasses, improve the condensation effect of fugitive constituent and realize the online sampling of sample, can increase simultaneously the heat transfer efficiency in the reactor, suitably reduce the content of moisture in the oil phase, partly solve the problem of cracked oil later separation difficulty.
Technical scheme: the method for preparing biological oil through vacuum pyrolysis of biomasses of the present invention is specific as follows:
1) earlier the enhancement of heat transfer device is positioned in the reactor, add the biomass samples of handling well again, the good seal flange face, start vacuum pump, check the system resistance to air loss, determine that resistance to air loss is good after, close first T-valve, open nitrogen valve and charge into nitrogen, question response still internal pressure rises to normal pressure, closes nitrogen valve;
2) close second stopping valve, open first T-valve and switch to the 3rd branch road, emptying reaction gas reactor;
3) treat that system vacuum tightness reaches about 5-10kpa, start temperature controller, the control furnace temperature is warming up to 105-140 ℃ in the fs, stops 15-35 minute under this temperature, removes free-water residual in the biomass;
4) first T-valve is cut to the 4th branch road, and second T-valve switches to first collector, opens the 4th stopping valve, regulates the 5th stopping valve on the absorption bottle, obtains suitable bubbling rate by the regulated valve switch size; Regulate temperature controller, the control furnace temperature rises to warm 400-600 ℃ eventually in subordinate phase with 10-30 ℃/min speed, and condensed product is collected in first collector, second collector, the 3rd collector, and condensable gases is not compressed to be pumped in the collection and confinement of gases jar and collects;
5) during online sampling, close the 4th stopping valve, second T-valve switches to the 5th branch road, collection liquid sample from collector; Open the 7th stopping valve and from the collection and confinement of gases jar, gather gaseous sample;
6) after question response finishes, close first T-valve, open the 6th stopping valve and prevent pump oil suck-back, close vacuum pump, close the 7th stopping valve, open nitrogen valve and charge into nitrogen, treat that the still internal pressure rises to normal pressure, closes nitrogen valve;
7) open first stopping valve, the 3rd stopping valve collection of biological oil, question response still temperature is reduced to room temperature, collects coke, the cleaning reactor.
Beneficial effect:
1, the inventive method can increase the heat transfer efficiency of reaction system, reduces the reaction times, reduces energy consumption, alleviates energy shortage to a certain extent;
2, the inventive method feeds nitrogen before and after reaction, effectively reduces the oxygen content of whole reaction system, has reduced the oxygen level of cracking component, has increased the product calorific value;
3, the inventive method adopts stainless steel elbow to immerse cooling medium, has increased contact area, has improved condensation effect, has increased the productive rate of pyrolysis oil;
4, the inventive method is provided with branch road L3 and L4 behind reactor lead line L2, reduces the mixed volume of water vapor in bio oil under the low temperature in the switching by branch road under low temperature and the high temperature;
5, the inventive method can realize the online sampling of sample and not influence the vacuum tightness of whole reaction system;
6, the inventive method is equipped with absorption bottle before vacuum pump, can regulate the bubbling degree and improve assimilated efficiency by regulating intake valve, effectively reduces the pollution to pump oil of nitride in the uncooled gas and sulfide simultaneously.
Description of drawings
Fig. 1 is the inventive method apparatus structure synoptic diagram;
Fig. 2 is the bottom schematic view of enhancement of heat transfer device in the inventive method device;
Fig. 3 is an enhancement of heat transfer device sectional view in the inventive method device;
Fig. 4 is a heating curve.
Have among the above figure: 1, nitrogengas cylinder, 2, nitrogen valve, 3, reactor, 4, tube furnace, 5, blind pipe, 6, thermopair, 7, vacuum meter, 8, first T-valve, 9, coil condenser, 10, second T-valve, 11, first stopping valve, 12, second stopping valve, 13, the 3rd stopping valve, 14, the 4th stopping valve, 15, the 3rd collector, 16, the 5th stopping valve, 17, resorber, 18, drying tower, 19, the 6th stopping valve, 20, vacuum pump, 21, surge flask, 22, compression pump, 23, the 7th stopping valve, 24, the collection and confinement of gases jar, 25, the 7th stopping valve, 26, temperature controller, 27, first collector, 28, second collector, L1, first branch road, L2, second branch road, L3, the 3rd branch road, L4, the 4th branch road, L5, the 5th branch road.
Embodiment
Below in conjunction with accompanying drawing the inventive method is further described.
Embodiment:
As shown in Figure 1, the setting drawing of this inventive method comprises interconnective reactive system, condenser system and pump system.Reactive system comprises stainless steel cauldron 3, tube furnace 4 and temperature controller 26, the reactor upper flange surface has interface, connect vacuum meter 7, blind pipe 5, the first branch road L1 and the second branch road L2 respectively, the reactor condenser system comprises three grades of condensations, be equipped with water and mixture of ice and water respectively in the preceding condensed in two stages groove, condensate trap and stainless steel elbow are welded as a whole 9, and the stainless steel elbow exit is connected to collector, are salt ice in the third stage condensate trap.Pump system comprises resorber 17, drying tower 18, surge flask 21, vacuum pump 20, compression pump 22.The pipe fitting junction is respectively equipped with T-valve and stopping valve.
Comprehensive said apparatus, the step that bio oil is produced in the pyrolysis of this example biomass vacuum is as follows:
With the wheat straw stalk is raw material, is crushed to particle size range 3-5mm, dries by the fire 12h down at 80-105 ℃.With heat-transfer device---be welded with the circular steel plate (shown in accompanying drawing 2,3) of heat conductive rod, place in the reactor, then add raw material, the good seal flange face.Start vacuum pump 20, check the system resistance to air loss, determine that resistance to air loss is good after, close first T-valve 8, open nitrogen valve 2 and charge into nitrogen, question response still internal pressure rises to normal pressure, closes nitrogen valve 2.Close second stopping valve 12, open first T-valve 8 and switch to the 3rd branch road L3, emptying reaction gas reactor.The system vacuum tightness for the treatment of reaches 5-10kpa, starts temperature controller 26, and the control furnace temperature is warming up to 105-140 ℃ in the fs, stops 10-30 minute under this temperature, removes free-water residual in the biomass.First T-valve 8 is cut to the 4th branch road L4, and second T-valve 10 switches to first collector 27, opens the 4th stopping valve 14, regulates the 5th stopping valve 16 on the absorption bottle 17, obtains suitable bubbling rate by the regulated valve switch size.Regulate temperature controller 26, the control furnace temperature rises to warm 400-600 ℃ eventually in subordinate phase with 10-30 ℃/min speed, condensed product is collected in first collector 27, second collector 28, the 3rd collector 15, and condensable gases is not compressed pump 22 and is pressed into collection in the collection and confinement of gases jar 24.During online sampling, close the 4th stopping valve 14, the second T-valve 10 and switch to the 5th branch road L5, collection liquid sample from collector 11.Open the 7th stopping valve 23 and from collection and confinement of gases jar 24, gather gaseous sample; Question response is closed first T-valve 8 after finishing, and opens the 6th stopping valve 19 and prevents pump oil suck-back, closes vacuum pump 20, closes the 7th stopping valve 25, opens nitrogen valve 2 and charges into nitrogen, treats that the still internal pressure rises to normal pressure, closes nitrogen valve 2.Open first stopping valve, 11, the three stopping valve, 13 collection of biological oil, question response still temperature is reduced to room temperature, collects coke, the cleaning reactor.
Figure 4 shows that heating curve figure, furnace temperature is risen to 500 ℃ by room temperature, curve 1,2,3 is respectively body of heater, adds heat-transfer device and does not add the interior heating curve of heat-transfer device reactor.Heat-transfer device has improved the hysteresis quality that biomass heat up, thereby can reduce the heating-up time, save energy.
Table 1 is the experiment correlation data, and data 1 be the normal straight tube condensation, and splitting gas directly enters condenser system, passes through that step 3 low temperature does not dewater described in the inventive method; Data 2 are the described coil pipe condensation of the inventive method, through the low temperature step that dewaters.
Table 1 bio oil yield and water content
Claims (1)
1. the method for a preparing biological oil through vacuum pyrolysis of biomasses is characterized in that this method comprises the steps:
1) earlier the enhancement of heat transfer device is positioned in the reactor (3), add the biomass samples of handling well again, the good seal flange face, start vacuum pump (20), check the system resistance to air loss, determine that resistance to air loss is good after, close first T-valve (8), open nitrogen valve (2) and charge into nitrogen, question response still internal pressure rises to normal pressure, closes nitrogen valve (2);
2) close second stopping valve (12), open first T-valve (8) and switch to the 3rd branch road (L3), emptying reaction gas reactor;
3) treat that system vacuum tightness reaches about 5-10kpa, start temperature controller (26), the control furnace temperature is warming up to 105-140 ℃ in the fs, stops 15-35 minute under this temperature, removes free-water residual in the biomass;
4) first T-valve (8) is cut to the 4th branch road (L4), second T-valve (10) switches to first collector (27), open the 4th stopping valve (14), regulate the 5th stopping valve (16) on the absorption bottle (17), obtain suitable bubbling rate by the regulated valve switch size; Regulate temperature controller (26), the control furnace temperature rises to warm 400-600 ℃ eventually in subordinate phase with 10-30 ℃/min speed, condensed product is collected in first collector (27), second collector (28), the 3rd collector (15), and condensable gases is not compressed pump (22) and is pressed into collection in the collection and confinement of gases jar (24);
5) during online sampling, close the 4th stopping valve (14), second T-valve (10) switches to the 5th branch road (L5), collection liquid sample from collector (11); Open the 7th stopping valve (23) and from collection and confinement of gases jar (24), gather gaseous sample;
6) after question response finishes, close first T-valve (8), open the 6th stopping valve (19) and prevent pump oil suck-back, close vacuum pump (20), close the 7th stopping valve (25), open nitrogen valve (2) and charge into nitrogen, treat that the still internal pressure rises to normal pressure, close nitrogen valve (2);
7) open first stopping valve (11), the 3rd stopping valve (13) collection of biological oil, question response still temperature is reduced to room temperature, collects coke, the cleaning reactor.
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| CN2009101832292A CN101613617B (en) | 2009-07-23 | 2009-07-23 | Method for preparing biological oil through vacuum pyrolysis of biomasses |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805647A (en) * | 2010-04-23 | 2010-08-18 | 倪建辉 | Method for preparing natural gas by biomass material thermal cracking and thermal cracking furnace used by same |
| CN102226095A (en) * | 2011-05-27 | 2011-10-26 | 中国科学院过程工程研究所 | Device and method for preparing fuel and chemicals by gradient pyrolysis of biomass and step-by-step collection |
| CN103215054A (en) * | 2013-03-15 | 2013-07-24 | 上海交通大学 | Batch type nitrogen gas filling single-phase pressure release low cost biological charcoal preparation apparatus and method thereof |
| CN103316647A (en) * | 2013-07-04 | 2013-09-25 | 东南大学 | Method for preparing supported solid-base catalyst and bio-oil |
| CN105176550A (en) * | 2015-10-28 | 2015-12-23 | 湖南炭道新能源科技有限公司 | Continuous carbonizing device and method |
| CN110312832A (en) * | 2016-12-22 | 2019-10-08 | 再制浆技术股份有限公司 | Method for changing fiber individually |
| CN110662820A (en) * | 2017-03-27 | 2020-01-07 | 扫描船有限公司 | Microwave pyrolysis reactor |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3721450C1 (en) * | 1987-06-30 | 1988-12-08 | Asea Brown Boveri | Process for cooling hot pyrolysis gas |
| CN100387367C (en) * | 2005-08-10 | 2008-05-14 | 重庆大学 | Biomass pyrolysis liquefied technique and apparatus system thereof |
| US7834226B2 (en) * | 2007-12-12 | 2010-11-16 | Chevron U.S.A. Inc. | System and method for producing transportation fuels from waste plastic and biomass |
| CN101343547A (en) * | 2008-09-02 | 2009-01-14 | 中国科学院广州能源研究所 | Apparatus and method for preparing biological oil with biomass vacuum thermal cracking and classification |
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2009
- 2009-07-23 CN CN2009101832292A patent/CN101613617B/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805647A (en) * | 2010-04-23 | 2010-08-18 | 倪建辉 | Method for preparing natural gas by biomass material thermal cracking and thermal cracking furnace used by same |
| CN102226095A (en) * | 2011-05-27 | 2011-10-26 | 中国科学院过程工程研究所 | Device and method for preparing fuel and chemicals by gradient pyrolysis of biomass and step-by-step collection |
| CN102226095B (en) * | 2011-05-27 | 2014-01-15 | 中国科学院过程工程研究所 | Device and method for preparing fuel and chemicals by gradient pyrolysis of biomass and step-by-step collection |
| CN103215054A (en) * | 2013-03-15 | 2013-07-24 | 上海交通大学 | Batch type nitrogen gas filling single-phase pressure release low cost biological charcoal preparation apparatus and method thereof |
| CN103215054B (en) * | 2013-03-15 | 2014-10-15 | 上海交通大学 | Batch type nitrogen gas filling single-phase pressure release low cost biological charcoal preparation apparatus and method thereof |
| CN103316647A (en) * | 2013-07-04 | 2013-09-25 | 东南大学 | Method for preparing supported solid-base catalyst and bio-oil |
| CN105176550A (en) * | 2015-10-28 | 2015-12-23 | 湖南炭道新能源科技有限公司 | Continuous carbonizing device and method |
| CN110312832A (en) * | 2016-12-22 | 2019-10-08 | 再制浆技术股份有限公司 | Method for changing fiber individually |
| CN110312832B (en) * | 2016-12-22 | 2021-05-07 | 再制浆技术股份有限公司 | Method for individualizing fibers |
| CN110662820A (en) * | 2017-03-27 | 2020-01-07 | 扫描船有限公司 | Microwave pyrolysis reactor |
| CN110662820B (en) * | 2017-03-27 | 2021-05-25 | 扫描船有限公司 | Microwave pyrolysis reactor |
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