CN100523798C - Method and device for on-line monitoring biomass coke conductive characteristic during pyrogenation - Google Patents

Method and device for on-line monitoring biomass coke conductive characteristic during pyrogenation Download PDF

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Publication number
CN100523798C
CN100523798C CNB2007100223669A CN200710022366A CN100523798C CN 100523798 C CN100523798 C CN 100523798C CN B2007100223669 A CNB2007100223669 A CN B2007100223669A CN 200710022366 A CN200710022366 A CN 200710022366A CN 100523798 C CN100523798 C CN 100523798C
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solid phase
phase column
line monitoring
signal
heating
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CN101059461A (en
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肖刚
金保升
肖睿
仲兆平
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Southeast University
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Southeast University
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Abstract

The invention discloses a method for online detecting the conductivity of biomass coke in pyrolysis process, and a relative device. The method comprises that first adding constant pressure on two ends of a solid post made from 50-200 deals of biomass, then heating the solid post and collecting the temperature signal, adding voltages on two ends of the solid post, collecting the voltage and current signals of the wires at two ends of the solid post, connecting a displacement sensor with at least one end of the solid post, collecting the displacement signal of the length change of the solid post, converting and storing the information data of collected voltage, current signals, displacement signal and temperature signal. The invention can realize online measurement of conductive character, to obtain overall conductivity data with high accuracy, with improved working efficiency.

Description

The method and apparatus of biomass coke conductive characteristic in a kind of on-line monitoring pyrolytic process
Technical field
The present invention relates to the method and apparatus of biomass coke conductive characteristic in a kind of on-line monitoring pyrolytic process, belong to the technical field of biomass pyrolytic and coke feature measurement.
Background technology
Living beings are a kind of typical renewable resources, and the annual carbon of fixing by photosynthesis of plant just reaches 2 * 10 on the earth 11T.Coke is one of main target product of biomass pyrolytic, has the coke of good conductive characteristic, generally is referred to as to conduct electricity charcoal, is a kind of electromagnetic shielding material of cheap environmental protection.Along with the widespread use of electronic equipment, the demand of electromagnetic shielding material also sharply increases, and utilizing biomass pyrolytic to produce electromagnetic shielding material is the effective way of meeting the need of market.But, the upgrading and the optimization of this technology have been restricted because the restriction of measurement means is difficult to further investigate biomass conductive carbon forming process and mechanism.
At present, the means of postgraduate's material pyrolysis mechanism mainly are gravitational thermal analysis methods, and it investigates in the biomass pyrolysis process solid product quality emphatically with the Changing Pattern in temperature of reaction or reaction time.This method can only reflect the reaction kinetics process of biomass pyrolytic, and can't learn the development law of solid product conductive characteristic in the pyrolytic process.For the process that biomass pyrolytic is produced the conduction charcoal, after temperature of reaction was elevated to more than 600~700 ℃, the solid product quality was very little with the variation of temperature of reaction, and this moment, the variation of its conductive characteristic is but extremely violent, and (resistivity can be from 1 * 10 7~1 * 10 8Ohmcm is reduced to 0.1~1 ohmcm).The method of specializing in the solid product conductive characteristic at present can only obtain off-line data, be difficult to reflect the dynamic process of conductive characteristic differentiation comprehensively, in addition, also have two serious defectives: (a) solid product of pyrolysis must be through after the cooling procedure, ability its resistance of energy measurement or resistivity, the cumulative errors of measurement is big; (b) preparation process of testing sample is loaded down with trivial details, so, be necessary very much to design special On-line Measuring Method and measurement mechanism, biomass pyrolytic solid product conductive characteristic is carried out particular study with the Changing Pattern in temperature of reaction or reaction time, provide basic data and theoretical foundation for utilizing living beings to produce the High Performance Shielding material.
Summary of the invention
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, the method and apparatus of biomass coke conductive characteristic in the little on-line monitoring pyrolytic process of a kind of measuring error is provided.
For achieving the above object, measuring method of the present invention adopts following technical scheme, at first applies constant pressure at the solid phase column two ends that are made of 50-200 purpose living beings; Then this solid phase column is heated and gathers the temperature signal of heating, simultaneously apply voltage at solid phase column two ends, collection is connected the voltage and current signal on the lead of solid phase column two ends, and at least one end connection of solid phase column displacement transducer, gather the displacement signal that solid phase column body length changes, and voltage and current signal, displacement signal, the temperature signal of gathering carried out the conversion and the storage of information data.
The described thermal recovery program controlled mode that adds, promptly in electrothermal furnace, arrange thermopair, gather the temperature signal in the electrothermal furnace, the temperature signal that collects is input to the intelligent industrial adjustment control, on this controller, set heating schedule, by the output power that this controller is regulated electrothermal furnace, the control electrothermal furnace heats up according to preset program.
Described solid phase column is the inner negative pressure that keeps in heating process, its vacuum tightness is 0Pa-30000Pa, the fugitive constituent that biomass pyrolytic is produced is in time discharged, and prevents from because of the instability of fugitive constituent the second pyrolysis reaction to take place, and influences the conductive characteristic of coke and the accuracy of resistance measurement.
Realize the device of above-mentioned measuring method, comprise heating furnace with temperature control equipment, displacement transducer, electric resistance measuring apparatus, data acquisition, conversion and memory storage and the pyrolysis reactor that is arranged on inside heating furnace, described temperature control equipment and data acquisition, conversion links to each other with memory storage, described pyrolysis reactor comprises that two ends are connected with the column hollow shell of electrode, be provided with the feeding port of filled biomass matter at least one end of housing, the feeding port place is provided with a piston, a described wherein termination electrode is arranged on the piston, described electrode links to each other with described electric resistance measuring apparatus by lead, be connected to data acquisition then, conversion and memory storage, also be provided with a constant pressure bringing device and described displacement transducer on described piston, displacement transducer is connected to data acquisition by lead, conversion and memory storage.
Described heating furnace is the programmed control heating furnace.
Described piston is provided with and is used to make enclosure interior to be in the bleeding point of negative pressure, and described electrode is provided with the venthole that makes column hollow shell inside be in negative pressure accordingly.
Described constant pressure bringing device is a mass.
Described feeding port is two, is separately positioned on the two ends of housing.
The internal diameter of described housing is 0.5-3mm.
Compared with prior art, the present invention has following effect:
1, biological particles requires 50-200 orders, it is more even that it is distributed in the solid phase column, simultaneously apply constant pressure at the cylindrical body two ends that constitute by it, solid phase column compaction rate is stable in the maintenance pyrolytic process, the solid product of living beings and pyrolysis thereof is fluffy attitude material, in heating process, can be more and more looser under the situation that does not have the external force effect, contact resistance is also just increasing, make each stage institute's measuring resistance not possess comparability, be difficult to characterize the Changing Pattern of solid product conductive characteristic, so, need in pyrolytic process, to apply constant pressure, keep the stability of solid phase column compaction rate, make the resistance measurement data that obtain in the pyrolytic process have comparability; By applying voltage, and the electric signal that flows through lead is carried out data acquisition and processing (DAP), gather the temperature signal of displacement letter that solid phase column body length changes and heating simultaneously and handle, realize the purpose of on-line measurement at solid phase column two ends.
2, the present invention adopts the solid phase column that is made of living beings or pyrolysis product is applied constant pressure, guaranteed the consistance of measuring object compaction rate in the conductive characteristic measuring process, prevent because of the inner contact resistance of solid phase column increases, and the measuring-signal that causes is irregular; Make the conductive characteristic measurement data in the whole pyrolytic process have comparability, the degree of accuracy height;
3, in the pyrolytic process, apply constant voltage at solid phase column two ends, with the conductive characteristic of solid phase column in time or the variation of temperature rule, in time be converted into the electric signal that flows through lead, and carry out collection, conversion and the storage of signal data, obtain the Changing Pattern of solid phase column conductive characteristic in the whole pyrolytic process; Compare with traditional off-line type measuring method, reduced the error that causes because of cooling procedure, realized the on-line measurement of conductive characteristic, obtained more comprehensive conductive characteristic data, improved work efficiency greatly.
4, adopting the material internal diameter of good heat conductivity and insulation is the thin-walled hollow cylindrical shell of 0.5-3mm, make the uniformity of temperature profile in the solid phase column in the pyrolytic process, reduce the error that the Yin Wendu inequality is brought, guarantee the accuracy of solid phase column conductive characteristic DATA REASONING; Adopt high temperature resistant, thermal expansivity is little, stable chemical performance, the material open column shape housing that rigidity is strong guarantee that the solid phase column is kept constant cross section column in the pyrolytic process, reduce the error of conductive characteristic data acquisition and conversion; Make the solid phase column conductive characteristic data of measuring in the pyrolytic process have higher accuracy.
5, the present invention not only can carry out on-line measurement at the conductive characteristic of coke in the biomass pyrolysis process, also can be used for gasifying, the on-line measurement of coke conductive characteristic in other courses of reaction such as burning applied range.
Description of drawings
Fig. 1 is the structural representation of measurement mechanism of the present invention
Fig. 2 is the structural representation of pyrolysis reactor 12
Fig. 3 is the structural representation of piston 4
Fig. 4 is arranged on the floor map of the electrode 8 on the piston 4
Fig. 5 is the change curve of the inventive method gained measurement data
Embodiment
Below in conjunction with accompanying drawing, the present invention is elaborated:
At first apply constant pressure at the solid phase column two ends that constitute by 50-200 purpose living beings; Then this solid phase column is heated and gathers the temperature signal of heating, simultaneously apply voltage at solid phase column two ends, collection is connected the voltage and current signal on the lead of solid phase column two ends, and at least one end connection of solid phase column displacement transducer, gather the displacement signal that solid phase column body length changes, and voltage and current signal, displacement signal, the temperature signal of gathering carried out the conversion and the storage of information data.
The described thermal recovery program controlled mode that adds, described solid phase column be the inner negative pressure that keeps in heating process, and its vacuum tightness is 0Pa-30000Pa.
Embodiment: as shown in Figure 1 and Figure 2, at first with after living beings 10 fragmentations, particle diameter 50-200 purpose living beings 20~100mg is obtained in screening, it is joined in the insulation thin-wall housing cylinder 9 of pyrolysis reactor 12, pyrolysis reactor 12 is arranged on the inside base body 14 of heating furnace 3; internal diameter of thin cylinder 9 is 2mm, made by the rigid insulation material with good heat conductive performance, reduced solid phase column internal temperature gradient in the pyrolytic process and and the temperature of heating furnace 3 burner hearths between difference.About 50~the 100mm of cylinder 9 length, open feeding port at cylinder 9 at least one ends, also can open feeding port to make things convenient for the cleaning of cylinder 9 in two ends, opening part connects piston 4, the sounding rod of one displacement transducer 13 is connected with piston 4, and is connected to data acquisition, conversion and memory storage 1 by lead.Act on piston 4 with living beings boil down to column with constant pressure bringing device 5, pressure is P, P=0.5~3.0bar, and constant pressure bringing device 5 is selected mass for use.Measure the column of biomass body length, write down applied pressure size on the piston 4, i.e. the weight of mass, mass also can be selected counterweight for use.End of being close to the solid phase column at piston 4 is provided with electrode 8, as shown in Figure 3, piston 4 is provided with and is used to make housing 9 inside to be in the bleeding point 6 of negative pressure, and electrode 8 is provided with the venthole that makes column hollow shell 9 inside be in negative pressure accordingly, as shown in Figure 4.Pyrolysis reactor 12 is put into programmed control heating furnace 3, lead 7 is connected with electric resistance measuring apparatus 2, the temperature signal of heating furnace 3 is input to data acquisition, conversion and the memory storage 1 from the temperature control equipment 15 of heating furnace 3, bleeding point 6 is inserted vacuum pump 11, make pyrolysis reactor 12 inner sustain negative pressure state, its vacuum tightness is 0Pa-30000Pa, in time discharges to guarantee pyrolysis devolatilization part.
Heating furnace 3 also can adopt the programmed control heating furnace, after configuring heating schedule, open heating furnace 3 and electric resistance measuring apparatus 2, gather electric current and voltage signal, gather the temperature signal of the temperature control equipment 15 of heating furnace 3 simultaneously, pyrolytic reaction takes place in the solid phase column when heating, inner living beings reduce, under the effect of constant pressure bringing device 5, by piston 4 compression solid phase columns its length is reduced, and the displacement signal of its length variations is measured by the displacement transducer 14 that links to each other with piston 4, at last with the voltage and current signal that collects, displacement signal, temperature signal is input to data acquisition, in conversion and the memory storage 1, according to the resistivity law, with obtaining data conversion is change in resistance data under the constant voltage, store and draw the change curve of resistivity with temperature of reaction or reaction time, the resistivity formula is: (wherein R is a resistance to ρ=R/ (L/S), L is a cylinder length, S is the cylinder cross-sectional area), as define relative resistance rate=log (biomass coke resistivity/1 Ω cm), can obtain similar result shown in Figure 5.
The programmed control heating can be adopted the intelligent industrial adjustment control, and controller can be selected the AI-708P type for use.
Data acquisition, conversion and memory storage 1 comprise data collecting instrument and computer, and data collecting instrument can be selected the HP34970A type for use.Utilize data collecting instrument to gather voltage and current signal, displacement signal, temperature signal, and convert it into digital signal and be transferred in the computer, time data is provided by computer self.Calculate the resistance value of solid phase column according to formula R=U/I (wherein R is that resistance, U are that solid phase column both end voltage, I are the electric current by the solid phase column), utilize resistivity formula ρ=R/ (L/S) (wherein ρ is that resistivity, R are that resistance, L are that cylinder length, S are the cylinder cross-sectional area) again, be translated into the resistivity of measuring object, and be stored in the computer, also above-mentioned two formula can be merged into a total resistivity and calculate formula ρ=(U/I)/(L/S)).
The KTF series displacement transducer that displacement transducer can select for use U.S. BEI DUNCAN company to produce, its range is 75-1000mm.

Claims (9)

1, the method for biomass coke conductive characteristic in a kind of on-line monitoring pyrolytic process is characterized in that: at first apply constant pressure at the solid phase column two ends that are made of 50-200 purpose living beings; Then this solid phase column is heated and gathers the temperature signal of heating, simultaneously apply voltage at solid phase column two ends, collection is connected the voltage and current signal on the lead of solid phase column two ends, and at least one end connection of solid phase column displacement transducer, gather the displacement signal that solid phase column body length changes, and the change in resistance data that voltage and current signal, displacement signal, the temperature signal of gathering is converted under the constant voltage store also.
2, on-line monitoring method according to claim 1 is characterized in that described type of heating adopts the programmed control type of heating.
3, on-line monitoring method according to claim 1 is characterized in that described solid phase column inner negative pressure that keeps in heating process.
4, on-line monitoring method according to claim 3 is characterized in that described negative pressure, and its vacuum tightness is 0Pa-30000Pa.
5, a kind of device of realizing the described on-line monitoring method of claim 1, comprise the have temperature control equipment heating furnace (3) of (15), displacement transducer (13), electric resistance measuring apparatus (2), data acquisition, conversion and memory storage (1) and the pyrolysis reactor (12) that is arranged on heating furnace (3) inside, described temperature control equipment (15) and data acquisition, conversion links to each other with memory storage (1), it is characterized in that described pyrolysis reactor (12) comprises that two ends are connected with the column hollow shell (9) of electrode (8), be provided with the feeding port of filled biomass matter at least one end of housing (9), the feeding port place is provided with a piston (4), a described wherein termination electrode (8) is arranged on the piston (4), described electrode (8) links to each other with described electric resistance measuring apparatus (2) by lead (6), be connected to data acquisition then, conversion and memory storage (1), also be provided with a constant pressure bringing device (5) and described displacement transducer (13) on described piston (4), displacement transducer (13) is connected to data acquisition by lead, conversion and memory storage (1).
6, device according to claim 5, it is characterized in that described piston (4) is provided with is used to make housing (9) inside to be in the bleeding point (6) of negative pressure, and described electrode (8) is provided with the venthole that makes column hollow shell (9) inside be in negative pressure accordingly.
7,, it is characterized in that described constant pressure bringing device (5) is a mass according to claim 5 or 6 described devices.
8, device according to claim 5 is characterized in that described feeding port is two, is separately positioned on the two ends of housing (9).
9, device according to claim 5, the internal diameter that it is characterized in that described housing (9) is 0.5-3mm.
CNB2007100223669A 2007-05-15 2007-05-15 Method and device for on-line monitoring biomass coke conductive characteristic during pyrogenation Expired - Fee Related CN100523798C (en)

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CN104914130B (en) * 2014-03-10 2017-08-15 河北联合大学 A kind of assay method and device of little particle coke gasification
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