CN100365202C - Instantaneously heating and fast cooling set for cellulose - Google Patents
Instantaneously heating and fast cooling set for cellulose Download PDFInfo
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- CN100365202C CN100365202C CNB2006100491028A CN200610049102A CN100365202C CN 100365202 C CN100365202 C CN 100365202C CN B2006100491028 A CNB2006100491028 A CN B2006100491028A CN 200610049102 A CN200610049102 A CN 200610049102A CN 100365202 C CN100365202 C CN 100365202C
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 28
- 239000001913 cellulose Substances 0.000 title claims abstract description 28
- 238000010438 heat treatment Methods 0.000 title claims abstract description 27
- 238000001816 cooling Methods 0.000 title claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 73
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 16
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 241000282693 Cercopithecidae Species 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 17
- 238000012360 testing method Methods 0.000 description 8
- 238000004227 thermal cracking Methods 0.000 description 8
- 239000000571 coke Substances 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 5
- 230000005855 radiation Effects 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001722 flash pyrolysis Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009834 vaporization Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012075 bio-oil Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007416 differential thermogravimetric analysis Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- TWNIBLMWSKIRAT-VFUOTHLCSA-N levoglucosan Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@H]2CO[C@@H]1O2 TWNIBLMWSKIRAT-VFUOTHLCSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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Abstract
The present invention discloses an instantaneous heating and fast cooling device for cellulose. A xenon lamp is placed at the focal point of an ellipsoidal reflective mirror, and light rays are converged on a plane mirror with an angle of 45 DEG. The plane mirror is sequentially connected with a light diaphragm, a shutter and a quartz glass tube which is placed on a photocell, and cellulose samples are filled in the quartz glass tube. A programmable controller is respectively in circuit connection with valves V1, V2, V3, V4, V5; one end of the valve V1 is connected with a nitrogen bottle, and one end of the valve V2 is connected with a liquid nitrogen groove; the output ends of the valves V1, V2 are connected with the input ends of the valves V3, V4; the output end of the valve V4 is connected with one end of the quartz glass tube, and the other end of the quartz glass tube is connected with the input end of the valve V5 after passing through a filter; the output end of the valve V5 is connected with a gas chromatograph. The heating time of the samples of the present invention is controlled by the shutter. In order to measure the heating time of the focal point, the photocell is arranged at the focal point; the conversion of nitrogen gas and liquid nitrogen are controlled by an electromagnetic valve. The opening and the closure of the shutter and the electromagnetic valve are controlled by the PLC programmable controller.
Description
Technical field
The present invention relates to a kind of instantaneously heating and fast cooling set for cellulose.
Background technology
Energy and environment are two principal themes of current social development.The development of economic society is important motivity with the energy, and the exhaustive exploitation of fossil fuel and use have brought huge pressure to environmental protection.Living beings are as a kind of important renewable and clean energy resource resource, to help to alleviate the pressure of national economy fast development to its reasonable development and efficient utilization to energy demand, can overcome simultaneously the environmental pollution that traditional fossil fuel utilizes in the process to be caused, thereby the emphasis paid close attention to of the persons that become the working energy beyond suspicion.
As the important component part of biomass thermal chemical conversion technology, the biomass through pyrolysis technology can be high-grade liquid fuel with Wood Adhesives from Biomass---bio oil and important chemical product are subjected to extensive concern to its research and application.Cellulose has occupied almost half content as the key component of living beings in biomass material, its thermal cracking behavior embodies the thermal cracking rule of living beings integral body to a great extent, and is therefore significant to the research of cellulose thermal cracking mechanism.
The researcher has carried out a large amount of research to cellulosic thermal cracking mechanism both at home and abroad, and " Broido-Shafizadeh " model is widely accepted.At a lower temperature, the process of a degree of polymerization reduction fast of cellulose thermal cracking experience, the intermediate state material of formation low polymerization degree; This material is extremely unstable under higher temperature, and life period is less than 1s, under the free radical effect further degraded can take place, and makes cellulose macromolecule enter into the Main Stage of pyrolysis, generates tar, coke and micromolecular light gas then.Wherein coke is two parallel competitive reactions with the generation of tar, and low temperature helps the generation of coke, and it is the coercibility fugitive constituent of feature product that higher temperatures then is partial to generate with the levoglucosan.
The proposition of intermediate state material in cellulose thermal cracking mechanism model is the focus that research workers dispute on owing to do not provide compellent experiment support always.But Donald is by differential thermogravimetric analysis, about 180 ℃, find a little endothermic peak, and, show certain reaction has taken place under the low temperature really by the detection of infrared spectrum to the cellulosic structure in the pyrolytic process, cellulosic structure is changed, thereby obtain a kind of intermediateness compound.And the strongest proof will give the credit to the early 21st century, and Boutin has observed directly a kind of material of molten state in his experiment, and just the existence for the intermediate state material provides true foundation.Detect and find that this material at room temperature is a kind of water miscible solid, but be different from flash pyrolysis oil (being in a liquid state under the room temperature), by the chromaticness on-line analysis, its component is simple relatively, and kind also obviously is less than the flash pyrolysis oil.This result of the test has proved no matter the generation of this intermediate state material is to be presented as uncontrollable process in the flash cracker of high heating intensity, still these become the important step of controlling whole pyrolytic process in firing equipment at a slow speed at thermobalance, cellulosic thermal cracking all must have been passed through this important physicochemical change process, thereby make cellulose macromolecule enter into the Main Stage of pyrolysis, generate tar, coke and micromolecular light gas then.
Result of study for many years shows, directly obtaining in thermobalance of this intermediate state material is impossible realize, and the flash thermal cracker be if can effectively control its further decomposition, just its certain existence of susceptible of proof, and its generation and evolution process furtherd investigate.
Summary of the invention
After a large amount of tests and theoretical research to cellulose thermal cracking mechanism, the object of the present invention is to provide a kind of instantaneously heating and fast cooling set for cellulose.
The technical solution used in the present invention is to comprise heating system and cooling, control system, wherein:
1) heating system: the focus place that xenon lamp is placed on ellipsoidal mirror, light converges at 45 ° plane mirror after reflection, plane mirror is connected to diaphragm, shutter straight down successively, is placed on photronic quartz glass tube, the cellulose sample is placed in the monkey, and places on the quartz glass plate of airtight quartz glass tube;
2) cooling, control system: the PLC Programmable Logic Controller is connected with the first valve V1, the second valve V2, the 3rd valve V3, the 4th valve V4 and the 5th valve V5 circuit respectively, the termination nitrogen cylinder of the first valve V1, the termination liquid nitrogen tank of the second valve V2, the output of the first valve V1 and the second valve V2 is connected with the input of the 3rd valve V3 and the 4th valve V4, one end of the output termination quartz glass tube of the 4th valve V4, the other end of quartz glass tube is through connecing the input of the 5th valve V5, the output termination gas chromatograph of the 5th valve V5 behind the filter.
The beneficial effect that the present invention has is:
1) the high pressure xenon short-act lamp is as a kind of comparatively desirable spot light, by obtaining the high focus point of heat flow rate per unit area after the ellipsoidal mirror reflection, main body reactor adopting quartz glass pipe, to infrared almost transparent, a large amount of radiations heat energies sees through quartz ampoule and is radiated on the material, satisfies the requirement of obtaining the needed flash intensification of intermediate state material pyrolysis;
2) because the intermediate state material is at high temperature extremely unstable, in the moment that heating finishes, utilize the principle of liquid nitrogen vaporization heat absorption that it is cooled to room temperature, obtain the intermediate state material of stable existence;
3) control by the rotary shutter of steel the heat time heating time of sample, its high-temperature capability height, response are soon.For accurately measuring the heat time heating time at focus place, at the focus place photocell is set, can accurately measure between the logical light time at focus place;
4) the switch control of the switching of nitrogen and liquid nitrogen by electromagnetic valve in the course of reaction, the switch of each valve and shutter is by a PLC Controlled by Programmable Controller, and is easy to use, reliability is high, response is fast;
5) input power of adjusting xenon lamp can change the heat flow rate per unit area at focus place, adjusts the heat time heating time that can change sample switch time of shutter, thus the degree that the control reaction is carried out;
6) escaping gas that adopts high pure nitrogen that reaction is emitted carries out reactor, and is through directly entering the gas chromatographic detection composition behind a small amount of tar of filter elimination, convenient and swift.
Description of drawings
Fig. 1 is the structural principle schematic diagram of instantaneously heating and fast cooling set for cellulose;
Fig. 2 is that the A of Fig. 1 is to view;
Fig. 3 is the enlarged drawing of cooling system.
Among the figure: 1, xenon lamp, 2, ellipsoidal mirror, 3, fan, 4, plane mirror, 5, quartz glass tube, 6, the cellulose sample, 7, nitrogen cylinder, 8, liquid nitrogen tank, 9, filter, 10, PLC Programmable Logic Controller, 11, gas chromatograph, 12, workbench, 13, diaphragm, 14, shutter, 15, photocell, 16, rubber stopper.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
As Fig. 1, Fig. 2, shown in Figure 3, the present invention includes heating system and cooling, control system, wherein:
1) heating system: the focus place that xenon lamp 1 is placed on ellipsoidal mirror 2, light converges at 45 ° plane mirror 4 after reflection, plane mirror 4 is connected to diaphragm 13, shutter 14 straight down successively, is placed on the quartz glass tube 5 of photocell 15, the cellulose sample is placed in the monkey, and place on the quartz glass plate of airtight quartz glass tube 5, photocell 15 is placed on the workbench 12;
2) cooling, control system: PLC Programmable Logic Controller 10 respectively with the first valve V1, the second valve V2, the 3rd valve V3, the 4th valve V4 is connected with the 5th valve V5 circuit, the termination nitrogen cylinder 7 of the first valve V1, the termination liquid nitrogen tank 8 of the second valve V2, the output of the first valve V1 and the second valve V2 is connected with the input of the 3rd valve V3 and the 4th valve V4, one end of the output termination quartz glass tube 5 of the 4th valve V4, the other end of quartz glass tube 5 is through connecing the input of the 5th valve V5, the output termination gas chromatograph 11 of the 5th valve V5 behind the filter 9.
The high pressure xenon short-act lamp 1 that it is 3kW that this experimental rig adopts a power is as radiation source, and its luminous point brightness is higher, is a kind of comparatively desirable spot light.Its luminous point is placed on the first focus place of ellipsoidal mirror 2, and light converges at second focus of reflective mirror after reflection.A fan 3 is set, to the outside heat radiation, to guarantee xenon lamp 1 and ellipsoidal mirror 2 trouble free services at the ellipsoidal mirror back.A light beam steering device is set in the light path, i.e. the plane mirror 4 of 45 ° of placements of one side, light beam converges at a border circular areas after reflection straight down.Cellulose sample 6 is placed in the monkey, and places on the quartz glass plate of airtight quartz glass tube 5.Adjust whole optical path, make sample be positioned at the high focal spot of heat flow rate per unit area just.The shutter 14 that be 0.01s by a response time heat time heating time of sample is controlled.For accurately measuring the heat time heating time at focus place, a photocell 15 is set at the focus place, determine that accurately its sensitivity is 0.01s between the logical light time at focus place.The cellulose sample 6 that takes a morsel is tiled in the crucible bottom surface, is placed on the focus place in the quartz glass tube 5, and rubber stopper 16 makes reaction system be in closed state beyond the Great Wall, and connects whole system.Open xenon lamp 1 and press the test arrangement input power, open PLC Programmable Logic Controller 10 then, whole system brings into operation by setup program.At first, the electrically heated rod energising in the liquid nitrogen tank 8, liquid nitrogen is heated to vaporize to make and produces certain pressure in the liquid nitrogen tank, opens valve V2, V3 liquid nitrogen is discharged smoothly; Valve-off V2, V3 open valve V1, V4, V5 then, make nitrogen be full of the entire reaction system, keep inert atmosphere; Valve-off V1, V4, V5, and moment open shutter 14, make the 6 flash pyrolysis of cellulose sample, when shutter 14 is closed by setting-up time, open valve V2, V4, V5, liquid nitrogen is sprayed onto sample surfaces rapidly it is cooled off; Valve-off V2 opens V1 subsequently, and nitrogen enters reaction system and the gaseous product purging is entered gas chromatograph 11 (as Agilent 6810 type gas chromatographs) and carries out analyzing and testing.Owing to may contain uncooled tar in the gaseous product, a filter 9 is set, before entering gas chromatograph 11 in order to avoid damage instrument.
The most critical part:
1) the flash heating system of sample
The high pressure xenon short-act lamp that it is 3kW that this experimental rig adopts a power is as radiation source, and its luminous point brightness is higher, is a kind of comparatively desirable spot light.Xenon lamp spectrum is the mixed light of wavelength 0.2～2.0 μ m, and the content of 0.8～1.0 μ m near-infrared radiation is higher, accounts for 78%, and visible light accounts for 12%, and ultraviolet ray accounts for 10%.Its luminous point is placed on the first focus place of ellipsoidal mirror, and light converges at second focus of reflective mirror after reflection.A light beam steering device is set in the light path, i.e. the plane mirror of 45 ° of placements of one side, light beam converges at a border circular areas after reflection straight down.Ellipsoidal mirror and plane mirror surface plating total reflection film aluminium film.The cellulose sample is placed in the monkey, and places airtight quartz glass tube, is convenient to picking and placeing of sample.Adjust whole optical path, make sample be positioned at the high focal spot of heat flow rate per unit area just.The heat flow rate per unit area at focus place can be regulated by the input power that changes xenon lamp.
2) accelerate cooling system of sample
Because the intermediate state material is at high temperature extremely unstable,, need it is cooled to room temperature in the moment that heating finishes.This experimental rig utilizes the principle of liquid nitrogen vaporization heat absorption that it is cooled off.The vaporization of being heated of the electrically heated rod that in the liquid nitrogen storage tank three power to be set be 1kW, liquid nitrogen makes and produces certain pressure in the liquid nitrogen tank, and when valve opening, liquid nitrogen just can spray and be used to cool off sample.
3) control system
Control by shutter the heat time heating time of sample.The shutter that this device adopts is the rotary shutter of steel, and its response time is 0.01s.For accurately measuring the heat time heating time at focus place, at the focus place photocell is set, its sensitivity is 0.01s.The switching of nitrogen and liquid nitrogen is controlled by the electromagnetic valve in the light path.And the switch of shutter and electromagnetic valve is by a PLC Controlled by Programmable Controller.
At first take by weighing a certain amount of cellulose substances in the process of the test and be tiled in the crucible bottom surface, be placed on the focus place in the quartz glass tube, stopper makes reaction system be in closed state beyond the Great Wall, and connects pipe-line system.Open xenon lamp and press the test arrangement input power, open the PLC Programmable Logic Controller then, whole system brings into operation by setup program.At first, the electrically heated rod energising in the liquid nitrogen tank, liquid nitrogen is heated to vaporize to make and produces certain pressure in the liquid nitrogen tank, opens valve V2, V3 liquid nitrogen is discharged smoothly; Valve-off V2, V3 open valve V1, V4, V5 then, make nitrogen be full of the entire reaction system, keep inert atmosphere; Valve-off V1, V4, V5, and moment open shutter, make the pyrolysis of cellulose sample flash, when shutter is closed by setting-up time, open valve V2, V4, V5, liquid nitrogen is sprayed onto sample surfaces rapidly it is cooled off; Valve-off V2 opens V1 subsequently, and nitrogen enters reaction system and the gaseous product purging is entered gas-chromatography and carries out analyzing and testing.Owing to may contain uncooled tar in the gaseous product, a filter is set, before entering gas-chromatography in order to avoid damage instrument.After the off-test, cellulosic crucible will be housed take out, sample wherein is water-soluble.Utilize the intermediate state material water-soluble and the water-fast character of cellulose is separated with unreacted cellulose this intermediate state material by filtering solution with coke produced.The aqueous solution is dried under 45 ℃ of temperature, can obtain the solid intermediate state material of stable existence.
Claims (2)
1. an instantaneously heating and fast cooling set for cellulose is characterized in that comprising heating system and cooling, control system, wherein:
1) heating system: the focus place that xenon lamp (1) is placed on ellipsoidal mirror (2), light converges at 45 ° plane mirror (4) after reflection, plane mirror (4) is connected to diaphragm (13), shutter (14) straight down successively, is placed on the quartz glass tube (5) on the photocell (15), the cellulose sample is placed in the monkey, and places on the quartz glass plate of airtight quartz glass tube (5);
2) cooling, control system: PLC Programmable Logic Controller (10) respectively with the first valve V1, the second valve V2, the 3rd valve V3, the 4th valve V4 is connected with the 5th valve V5 circuit, the termination nitrogen cylinder (7) of the first valve V1, the termination liquid nitrogen tank (8) of the second valve V2, the output of the first valve V1 and the second valve V2 is connected with the input of the 3rd valve V3 and the 4th valve V4, one end of the output termination quartz glass tube (5) of the 4th valve V4, connect the input of the 5th valve V5 behind the other end process filter (9) of quartz glass tube (5), the output termination gas chromatograph (11) of the 5th valve V5.
2. a kind of instantaneously heating and fast cooling set for cellulose according to claim 1 is characterized in that: described xenon lamp (1) is the high pressure xenon short-act lamp of 3kW, and spectrum is the mixed light of wavelength 0.2～2.0 μ m.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100491028A CN100365202C (en) | 2006-01-16 | 2006-01-16 | Instantaneously heating and fast cooling set for cellulose |
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| CNB2006100491028A CN100365202C (en) | 2006-01-16 | 2006-01-16 | Instantaneously heating and fast cooling set for cellulose |
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| CN1811057A CN1811057A (en) | 2006-08-02 |
| CN100365202C true CN100365202C (en) | 2008-01-30 |
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| CN106221848B (en) * | 2016-09-29 | 2019-02-19 | 太原理工大学 | The fixed bed reactors baked for biomass |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2898028Y (en) * | 2006-01-16 | 2007-05-09 | 浙江大学 | Device for thermal cracking intermediate substance by cellulose |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN2898028Y (en) * | 2006-01-16 | 2007-05-09 | 浙江大学 | Device for thermal cracking intermediate substance by cellulose |
Non-Patent Citations (2)
| Title |
|---|
| radiant flash pyrolysis of cellulose- evidence for theformationof short life time intermediate liquid species. Boutin O, et al.J ANAL APPL PYROL,Vol.47 No.1. 1998 * |
| 纤维素快速热裂解机理试验研究 Ⅰ.试验研究. 廖艳芬等.燃料化学学报，第31卷第2期. 2003 * |
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