CN103558323B - Micro fluidized bed cracking reaction analysis device and method by utilizing analysis device for carrying out cracking reaction analysis upon coal tar - Google Patents
Micro fluidized bed cracking reaction analysis device and method by utilizing analysis device for carrying out cracking reaction analysis upon coal tar Download PDFInfo
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Abstract
The invention provides a micro fluidized bed cracking reaction analysis device and a method for utilizing the analysis device for carrying out cracking reaction analysis upon coal tar. With the device, liquid raw material feeding, cracking, and qualitative and quantitative analysis can be carried out, and reaction kinetic parameters and reaction mechanism can be calculated. The micro fluidized bed cracking reaction analysis device comprises: a gas cylinder, a sample bottle, a fluidizing medium arranged in the reactor, a switch valve assembly with a six-way valve with a quantitation ring, a feeding pump, a return pipeline, a mass spectrometer, and a computer. The method for carrying out cracking reaction analysis upon coal tar comprises the steps that: the gas cylinder is opened; heating furnace temperature is set; the coal tar raw material is subjected to a preheating viscosity-reducing treatment; the pass way of the quantitation ring is connected; the quantitation ring is connected with a first gas outlet branch; coal tar drops are torn into liquid particles, and the liquid particles enter the reactor; the mass spectrometer carries out inspection and analysis; and different heating furnace temperatures are set, and obtained data are analyzed.
Description
Technical field
The present invention relates to a kind of miniature fluidized bed cracking reaction analytical equipment and utilize it coal tar to be carried out to the method for cracking reaction analysis.
Background technology
The cracking reaction of liquid phase feed is extensively present in various material conversion process, and the research of asking calculation and reaction mechanism of its reaction power mathematic(al) parameter is the basis of the area research developments such as chemical industry, the energy, environment, metallurgy, material.Traditional power science study method is to carry out under certain heating rate prerequisite, adopt thermogravimetric analyzer to the quality of sample in time and the variation of temperature measure in real time, thereby the kinetic parameter of the reaction of deriving, but be subject to the restriction of thermogravimetric analyzer measuring principle and structure, reaction can not be carried out under steady temperature, has relatively large deviation with intrinsic course of reaction.
Summary of the invention
One of the object of the invention is to provide a kind of miniature fluidized bed cracking reaction analytical equipment, can realize sample introduction, cracking to liquid charging stock, and crucial other components are carried out to qualitative and quantitative analysis, change to ask according to gas concentration and calculate reaction power mathematic(al) parameter and reaction mechanism thereof.
Two of the object of the invention is to provide a kind ofly utilizes above-mentioned miniature fluidized bed cracking reaction analytical equipment coal tar to be carried out to the method for cracking reaction analysis.
The present invention adopts technical scheme as follows:
A kind of miniature fluidized bed cracking reaction analytical equipment, comprising:
Gas cylinder, gas cylinder outlet nozzle place is provided with reduction valve;
Sample bottle, treats the liquid charging stock of cracking reaction for splendid attire;
Reactor, outside is provided with heating furnace, has liquid charging stock entrance, fluidizing gas entrance and pyrolysis product outlet, and inside is placed with fluidizing agent;
Transfer valve assembly, comprises the six-way valve encircling with quantitatively;
Feeding engine, is communicated with sample bottle and six-way valve by feeding pipe, for liquid charging stock being transported to quantitative ring;
Feed back pipeline, between sample bottle and six-way valve, for unnecessary liquid charging stock is transmitted back to sample bottle;
Mass spectrometer, connects pyrolysis product outlet, for the product of analytical review cracking reaction; With
Computer, connects mass spectrometer, and the data that mass spectrometer analysis is obtained are preserved and can be read and show;
The branch road of giving vent to anger of gas cylinder is divided into two, the Article 1 branch road liquid charging stock entrance of coupled reaction device after the first switch valve, six-way valve successively of giving vent to anger, the Article 2 fluidizing gas entrance of branch road through second switch valve coupled reaction device of giving vent to anger.
Preferably, in described miniature fluidized bed cracking reaction analytical equipment, reactor is tubular structure, and fluidizing gas entrance and pyrolysis product outlet arrange along reactor axis direction, fluidizing gas entrance is arranged on reactor lower end, and pyrolysis product outlet is arranged on reactor upper end.
Preferably, in described miniature fluidized bed cracking reaction analytical equipment, sample bottle is arranged in water-bath.
Preferably, in described miniature fluidized bed cracking reaction analytical equipment, the first switch valve is electromagnetic impulse valve.
Preferably, in described miniature fluidized bed cracking reaction analytical equipment, feeding engine is peristaltic pump.
Preferably, in described miniature fluidized bed cracking reaction analytical equipment, give vent to anger branch road and Article 2 of Article 1 given vent to anger on branch road mass-flow gas meter is all installed.
Utilize above-mentioned miniature fluidized bed cracking reaction analytical equipment coal tar to be carried out to a method for cracking reaction analysis, comprise the following steps:
1) open gas cylinder, the pressure that utilizes reduction valve adjustment to give vent to anger, opens second switch valve while the first switch valve in closed condition, and gas is entered by the fluidizing gas entrance of reactor, adjusts gas admission velocity;
2) furnace temp is set;
3) coal tar raw material is carried out the processing of preheating viscosity reduction;
4) switch six-way valve knob to connecting the quantitatively path of ring, by feeding engine, coal tar raw material after treatment preheating viscosity reduction is pumped to six-way valve and is full of quantitative ring;
5) again switch six-way valve knob, make quantitatively ring and the Article 1 branch road of giving vent to anger be connected, complete and carry out sample introduction preliminary work;
6) in question response device, fluidizing gas admission velocity is stable, and heating furnace reaches after set temperature, press the first switch valve and produce one pulse gas, under the effect of pulse gas, the coal tar drop spraying from quantitative ring is torn as drop particle, and drop particle enters cracking reaction occurs in reactor through liquid charging stock entrance;
7) gaseous product that cracking produces is led to mass spectrometer through pyrolysis product outlet and is checked analysis;
8) set different furnace temp repeating steps 1) to 7), analyze the data obtained, can draw the cracking reaction kinetic parameter of coal tar raw material, infer its reaction mechanism.
Preferably, coal tar is carried out in the method for cracking reaction analysis, coal tar raw material preheat temperature is 95 DEG C, and furnace temp is 300 ~ 900 DEG C.
Preferably, coal tar is carried out in the method for cracking reaction analysis, Article 2 is given vent to anger, and to enter fluidizing gas inlet velocity be 0.25L/min for the gas of branch road.
Preferably, coal tar is carried out in the method for cracking reaction analysis, coal tar raw material residence time in reactor is 1.1 ~ 2.3s.
Principle of work of the present invention:
In the time carrying out liquid charging stock cracking reaction, liquid charging stock sprays in reactor by gas cylinder gas percussive action; Liquid charging stock enters after reactor, and cracking reaction occurs rapidly, and the product that reaction generates is entered in mass spectrometer and detected by pyrolysis product outlet, detects data by computer reading displayed and preserves.By the processing to data, can obtain the product kind of liquid charging stock cracking, each cracking reaction order of occurrence with and the kinetic parameter such as energy of activation, pre-exponential factor, for the cracking reaction mechanism of study of various liquid charging stock provides guidance.
Beneficial effect of the present invention: the quick cracking reaction analytic system of liquid charging stock can realize instantaneous sample introduction, the cracking of liquid charging stock under arbitrary temp, and by follow-up on-line mass spectroscopy, crucial gas composition is carried out to qualitative and quantitative analysis, change to ask according to gas concentration and calculate reaction power mathematic(al) parameter and reaction mechanism thereof.This device, compared with traditional thermogravimetric analyzer, has reduced the impact of external diffusion on reaction to greatest extent, can also infer reaction mechanism according to the release sequence of key component and burst size characteristic simultaneously.Be with a wide range of applications.
Brief description of the drawings
Fig. 1 is the structural representation of the selected embodiment of the present invention.
In figure 1, gas cylinder, 2, reduction valve, 3, T-valve, 4, the first switch valve, 5, feeding engine, 6, mass flowmeter, 7, quantitative ring, 8, six-way valve, 9, mass spectrometer, 10, liquid charging stock entrance, 11, computer, 12, fluidizing agent, 13, reactor, 14, heating furnace, 15, sample bottle, 16, water-bath, 17, second switch valve, 18, feed back pipeline, 19, the Article 1 branch road of giving vent to anger, 20, the Article 2 branch road of giving vent to anger, 21, feeding pipe, 22, fluidizing gas entrance, 23, pyrolysis product outlet.
Embodiment
Better understand the present invention for the ease of those skilled in the art, below in conjunction with the drawings and specific embodiments, the present invention is described in further details, following is only the exemplary protection scope of the present invention that do not limit.
With reference to accompanying drawing 1, a kind of miniature fluidized bed cracking reaction analytical equipment, comprises gas cylinder 1, sample bottle 15, reactor 13, mass spectrometer 9 and computer 11.Sample bottle 15 is treated the liquid charging stock of cracking reaction for splendid attire, be arranged in water-bath 16; Reactor 13 outsides are provided with heating furnace 14, and have liquid charging stock entrance 10, fluidizing gas entrance 22 and pyrolysis product outlet 23, and inside is placed with fluidizing agent 12; Transfer valve assembly comprises with the six-way valve 8 that quantitatively encircles 7; The gas cylinder outlet nozzle place of gas cylinder 1 is provided with reduction valve 2, the branch road of giving vent to anger of gas cylinder 1 is divided into two, Article 1, the branch road 19 liquid charging stock entrance 10 of coupled reaction device 13 after the first switch valve 4, six-way valve 8 successively of giving vent to anger, Article 2 is given vent to anger branch road 20 through the fluidizing gas entrance 22 of second switch valve 17 coupled reaction devices 13, and Article 1 branch road 19 and the Article 2 branch road 20 of giving vent to anger of giving vent to anger connects the pipeline at the outlet nozzle place of gas cylinder 1 through T-valve 3; Feeding engine 5 is communicated with sample bottle 15 and six-way valve 8 by feeding pipe 21, for liquid charging stock being transported to quantitative ring 7; Feed back pipeline 18 is between sample bottle 15 and six-way valve 8, for unnecessary liquid charging stock is transmitted back to sample bottle 15; Mass spectrometer 9, for the product of analytical review cracking reaction, connects pyrolysis product outlet 23; Computer 11 connects mass spectrometer 9, mass spectrometer 9 is analyzed to the data that obtain and preserve and can read and show.
In the present embodiment, reactor 13 is quartzy sandpipe, and fluidizing gas entrance 22 and pyrolysis product outlet 23 are along reactor 13 axis direction settings, and fluidizing gas entrance 22 is arranged on reactor 13 lower ends, and pyrolysis product outlet 23 is arranged on reactor 13 upper ends.
In the present embodiment, the first switch valve 4 is electromagnetic impulse valve, can complete the instantaneous accurate Pulsed Sampling of liquid charging stock, due to the effect of pulse gas, liquid charging stock is torn as fine particle produces atomizing effect, realizes the cracking reaction of liquid charging stock under arbitrary temp.
In the present embodiment, feeding engine 5 is peristaltic pump.
In the present embodiment, give vent to anger branch road 19 and Article 2 of Article 1 given vent to anger on branch road 20 and mass-flow gas meter 6 is all installed, convenient speed of observing gas.
Utilize described miniature fluidized bed cracking reaction analytical equipment coal tar to be carried out to a method for cracking reaction analysis, comprise the following steps:
1) open gas cylinder 1, utilize reduction valve 2 to adjust the pressure of giving vent to anger and open 17 while of second switch valve the first switch valve 4 in closed condition, gas is entered by the fluidizing gas entrance 22 of reactor 13, adjust gas admission velocity to 0.25L/min, make the fluidizing agent 12 of reactor 13 in best fluidized state;
2) heating furnace 14 temperature being set is 750 DEG C, and reactor 13 is heated to assigned temperature, and heating furnace 14 temperature can be selected as required between 300 ~ 900 DEG C;
3) coal tar raw material is heated to 95 DEG C and carries out the processing of preheating viscosity reduction, 6mPas when 1100mPas is reduced to 95 DEG C while making coal tar raw material viscosity from 25 DEG C through water-bath 16;
4) switch six-way valve 8 knobs to connecting the quantitatively path of ring 7, by feeding engine 5, coal tar raw material after treatment preheating viscosity reduction is pumped to six-way valve 8 and is full of quantitative ring 7;
5) again switch six-way valve 8 knobs, make quantitatively ring 7 and the Article 1 branch road 19 of giving vent to anger be connected, complete and carry out sample introduction preliminary work;
6) the interior fluidization gas velocity of question response device 13 is stable, and heating furnace 14 reaches after set temperature, press the first switch valve 4 and produce one pulse gas, under the effect of pulse gas, it is 35 μ m left and right drop particles that the coal tar drop spraying from quantitative ring 7 is torn, drop particle enters in reactor 13 cracking reaction occurs through liquid charging stock entrance 10, coal tar raw material in reactor 13 residence time between 1.1 ~ 2.3s, owing to being subject to the effect of pulse gas and fluidizing gas, now temperature of reactor slightly reduces, and substantially maintains between 740 ~ 750 DEG C;
7) the gaseous product pyrolysis product outlet 23 that cracking produces is led to mass spectrometer 9 and is checked analysis;
8) set different furnace temps as 650 DEG C, 700 DEG C, 800 DEG C repeating steps 1) to 7), analyze the data obtained, can draw the cracking reaction kinetic parameter of coal tar raw material, infer its reaction mechanism.
The Conversion Rate Methods In The Decompositions such as employing are processed data, show that the energy of activation of coal tar cracking and pre-exponential factor are respectively 20.35KJ/mol and 12.5s
-1, be all less than the measured value of traditional gravitational thermal analysis method: 76.7KJ/mol ~ 162KJ/mol and 2 ' 10
4s
-1.
This shows: the heat and mass transfer performance that this device tool is higher, the reaction power mathematic(al) parameter of its mensuration more approaches the intrinsic process of chemical reaction than conventional test methodologies, the test and the analysis that can be the reaction power mathematic(al) parameter of complex fluid raw material provide effective apparatus and method.
Below only described ultimate principle of the present invention and preferred implementation, those skilled in the art can make many changes and improvements according to foregoing description, and these changes and improvements should belong to protection scope of the present invention.
Claims (9)
1. a method of utilizing miniature fluidized bed cracking reaction analytical equipment coal tar to be carried out to cracking reaction analysis, miniature fluidized bed cracking reaction analytical equipment, comprising: gas cylinder (1), gas cylinder outlet nozzle place is provided with reduction valve (2);
Sample bottle (15), treats the liquid charging stock of cracking reaction for splendid attire; Reactor (13), outside is provided with heating furnace (14), has liquid charging stock entrance (10), fluidizing gas entrance (22) and pyrolysis product outlet (23), and inside is placed with fluidizing agent (12); Transfer valve assembly, comprises with the six-way valve (8) that quantitatively encircles (7);
Feeding engine (5), is communicated with sample bottle (15) and six-way valve (8) by feeding pipe (21), for liquid charging stock being transported to quantitative ring (7); Feed back pipeline (18), is positioned between sample bottle (15) and six-way valve (8), for unnecessary liquid charging stock being transmitted back to sample bottle (15); Mass spectrometer (9), connects pyrolysis product outlet (23), for the product of analytical review cracking reaction; And computer (11), connecting mass spectrometer (9), the data that mass spectrometer (9) analysis is obtained are preserved and can be read and show; The branch road of giving vent to anger of gas cylinder (1) is divided into two, Article 1, branch road (19) the liquid charging stock entrance (10) of coupled reaction device (13) after the first switch valve (4), six-way valve (8) successively of giving vent to anger, Article 2 is given vent to anger branch road (20) through the fluidizing gas entrance (22) of second switch valve (17) coupled reaction device (13), it is characterized in that comprising the following steps:
1) open gas cylinder (1), the pressure that utilizes reduction valve (2) adjustment to give vent to anger, open second switch valve (17) while the first switch valve (4) in closed condition, gas is entered by the fluidizing gas entrance (22) of reactor (13), adjust gas admission velocity;
2) heating furnace (14) temperature is set;
3) coal tar raw material is carried out the processing of preheating viscosity reduction;
4) switch six-way valve (8) knob to connecting the quantitatively path of ring (7), by feeding engine (5), coal tar raw material after treatment preheating viscosity reduction is pumped to six-way valve (8) and is full of quantitative ring (7);
5) again switch six-way valve (8) knob, quantitative ring (7) and the Article 1 branch road (19) of giving vent to anger is connected, complete and carry out sample introduction preliminary work;
6) the interior fluidization gas velocity of question response device (13) is stable, and heating furnace (14) reaches after set temperature, press the first switch valve (4) and produce one pulse gas, under the effect of pulse gas, from quantitative ring (7), the coal tar drop of ejection is torn as drop particle, and drop particle enters generation cracking reaction in reactor (13) through liquid charging stock entrance (10);
7) gaseous product that cracking produces is led to mass spectrometer (9) through pyrolysis product outlet (23) and is checked analysis;
8) set different furnace temp repeating steps 1) to 7), analyze the data obtained, can draw the cracking reaction kinetic parameter of coal tar raw material, infer its reaction mechanism.
2. method of coal tar being carried out to cracking reaction analysis according to claim 1, is characterized in that: coal tar raw material preheat temperature is 95 DEG C, and heating furnace (14) temperature is 300 ~ 900 DEG C.
3. method of coal tar being carried out to cracking reaction analysis according to claim 1, is characterized in that: Article 2 is given vent to anger, and to enter fluidizing gas entrance (22) speed be 0.25L/min for the gas of branch road (20).
4. method of coal tar being carried out to cracking reaction analysis according to claim 1, is characterized in that: coal tar raw material residence time in reactor (13) is 1.1 ~ 2.3s.
5. according to the method that coal tar is carried out to cracking reaction analysis described in claim 1 to 4 any one, it is characterized in that: reactor (13) is tubular structure, fluidizing gas entrance (22) and pyrolysis product outlet (23) are along reactor (13) axis direction setting, fluidizing gas entrance (22) is arranged on reactor (13) lower end, and pyrolysis product outlet (23) is arranged on reactor (13) upper end.
6. according to the method that coal tar is carried out to cracking reaction analysis described in claim 1 to 4 any one, it is characterized in that: sample bottle (15) is arranged in water-bath (16).
7. according to the method that coal tar is carried out to cracking reaction analysis described in claim 1 to 4 any one, it is characterized in that: the first switch valve (4) is electromagnetic impulse valve.
8. according to the method that coal tar is carried out to cracking reaction analysis described in claim 1 to 4 any one, it is characterized in that: feeding engine (5) is peristaltic pump.
9. according to the method that coal tar is carried out to cracking reaction analysis described in claim 1 to 4 any one, it is characterized in that: give vent to anger branch road (19) and Article 2 of Article 1 given vent to anger on branch road (20) mass-flow gas meter (6) is all installed.
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