CN113908771B - Low-pressure flash pyrolysis flow tube reaction device based on continuous molecular beam source - Google Patents
Low-pressure flash pyrolysis flow tube reaction device based on continuous molecular beam source Download PDFInfo
- Publication number
- CN113908771B CN113908771B CN202111203066.7A CN202111203066A CN113908771B CN 113908771 B CN113908771 B CN 113908771B CN 202111203066 A CN202111203066 A CN 202111203066A CN 113908771 B CN113908771 B CN 113908771B
- Authority
- CN
- China
- Prior art keywords
- pair
- inlet pipe
- supporting plate
- sample inlet
- pipe
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/006—Processes utilising sub-atmospheric pressure; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/02—Feed or outlet devices therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of pyrolysis instruments, and particularly relates to a low-pressure flash pyrolysis flow tube reaction device based on a continuous molecular beam source. The device comprises a test bed, an installation mechanism, a flash pyrolysis mechanism and a vacuum box; the flash pyrolysis mechanism comprises a cylindrical cavity horizontally arranged in the vacuum box, and a sample inlet pipe, a water inlet pipe and a water outlet pipe which are arranged in the cylindrical cavity, the water cooling cavity is arranged in the cavity at the other end of the cylindrical cavity in a sliding manner, the other end of the sample inlet pipe penetrates through the water cooling cavity, the extending end of the sample inlet pipe is connected with a silicon carbide pipe, and a pair of graphite electrodes is sleeved on the silicon carbide pipe; a sliding table is arranged in the corresponding cylindrical cavity at the push rod extending end of the linear introducer, the push rod extending end is fixedly connected with the sliding block, and the upper end of the sliding block is fixedly connected with the corresponding sample injection pipe. The silicon carbide tube is used as a reactor, the graphite electrode is used for heating, rapid temperature rise is realized, secondary reaction is reduced, annihilation of active important reaction intermediates such as free radicals and the like can be reduced under low pressure, continuous sampling can be realized, and reaction kinetics research of pyrolysis samples is perfected.
Description
Technical Field
The invention belongs to the technical field of pyrolysis reactors, and particularly relates to a low-pressure flash pyrolysis flow tube reaction device based on a continuous molecular beam source.
Background
In current various scientific research experiments, various reaction devices and equipment are in endlessly, and a large number of experiments provide a wide data base for the development and verification of reaction kinetics. The pyrolysis reaction is the first stage of high-temperature combustion and is a key process for exploring the decomposition path of a sample such as fuel in the initial stage.
The existing pyrolysis reaction device mainly has the following problems:
(1) the pyrolysis reaction can not be carried out in a higher vacuum environment, most of active intermediate products such as free radicals and the like are easy to annihilate under normal pressure or high pressure, and can not be observed;
(2) the slow pyrolysis reaction device is slow in pyrolysis reaction, is easy to generate secondary reaction, cannot accurately capture reaction intermediates, and cannot accurately provide a reaction network;
(3) discontinuous sampling, continuous sampling research cannot be carried out through a coupling molecular beam sampling system and a photoionization mass spectrum, and the experimental period and errors are greatly increased;
(4) the material of the reactor can not reach a higher temperature range, the boiling point of more species is higher, the starting pyrolysis temperature of the parent substance of the species and the complete decomposition temperature of the parent substance of the species are also higher, and the material of the general reactor can not reach the requirement of the complete decomposition temperature of the parent substance of the species.
Therefore, there is an urgent need for a low-pressure flash pyrolysis apparatus using a silicon carbide tube as a reactor and heating with a graphite electrode in order to reduce secondary reactions and continuously sample important reaction intermediates such as radicals under pyrolysis conditions in a low-pressure environment and in a higher temperature range.
Disclosure of Invention
Aiming at the problems, the invention designs a low-pressure flash pyrolysis flow tube reaction device based on a continuous molecular beam source, flash pyrolysis is carried out under a low-pressure environment, and the key reaction can be better understood, so that the reaction kinetics of flash pyrolysis of multiple species can be perfected.
The invention specifically comprises the following steps:
a low-pressure flash pyrolysis flow tube reaction device based on a continuous molecular beam source comprises a cube-shaped test bed 1, an installation mechanism, a flash pyrolysis mechanism and a vacuum box 2, wherein the vacuum box 2 is arranged at the upper end of the test bed 1 in a sliding mode through the matching of a sliding frame 11 and a pair of sliding rails 12;
the mounting mechanism comprises a first supporting plate 31, a second supporting plate 32 and an adjusting mechanism, the first supporting plate 31 is adjustably mounted on one side of the second supporting plate 32 through the adjusting mechanism, the other side of the second supporting plate 32 is fixedly mounted on the front end surface of the vacuum box 2 through a vacuum flange 21,
a first mounting hole and a second mounting hole are correspondingly formed in the first supporting plate 31 and the second supporting plate 32 respectively, the first mounting hole is sealed through a mounting flange 33, and the second mounting hole is communicated with the vacuum box 2;
the flash pyrolysis mechanism comprises a cylindrical cavity 41 horizontally arranged in the vacuum box 2, and a sample inlet pipe 42, a water inlet pipe 43 and a water outlet pipe 44 which are arranged in the cylindrical cavity 41, wherein one end of the cylindrical cavity 41 is fixedly connected with the mounting flange 33, a water cooling cavity 45 is arranged in a cavity at the other end of the cylindrical cavity 41 in a sliding manner,
one end of the water inlet pipe 43, one end of the water outlet pipe 44 and one end of the sample inlet pipe 42 penetrate through the mounting flange 33 respectively, the other end of the water inlet pipe 43 and the other end of the water outlet pipe 44 are communicated with the water-cooling cavity 45 respectively, the other end of the sample inlet pipe 42 penetrates through the water-cooling cavity 45, the extending end of the sample inlet pipe is connected with a silicon carbide pipe 46, and a pair of graphite electrodes 47 are sleeved on the silicon carbide pipe 46;
the mounting flange 33 is inserted with a linear introducer 48, a sliding table 49 is arranged in the cylindrical cavity 41 corresponding to the push rod extension end of the linear introducer 48, a sliding block 491 is arranged on the sliding table 49 in a matching manner, the push rod extension end is fixedly connected with the sliding block 491 through threads, and the upper end of the sliding block 491 is fixedly connected with the corresponding sample injection tube 42 through a connecting convex block 492, so that the silicon carbide tube 46 can horizontally move through the linear introducer 48.
Further, the adjusting mechanism comprises a pair of connecting blocks 34 and a pair of limiting blocks 35, a pair of grooves are vertically formed in the upper end and the lower end of the first supporting plate 31, the pair of limiting blocks 35 are arranged in the pair of grooves and fixedly connected with the second supporting plate 32 through adjusting the vertically arranged kidney-shaped holes in a threaded manner, so that the vertical installation position of the first supporting plate 31 can be adjusted;
the pair of connecting blocks 34 are fixedly mounted on the second supporting plates 32 corresponding to the left and right sides of the first supporting plate 31, and a pair of adjusting bolts are horizontally inserted, and the threaded ends of the pair of adjusting bolts correspondingly abut against the left and right sides of the first supporting plate 31, and adjust the horizontal mounting position of the first supporting plate 31.
Further, a pair of connecting groove has been seted up respectively on the vertical of a pair of stopper 35, is equipped with a pair of stopper 351 of connecting in a pair of connecting groove, and a pair of stopper 351 of connecting and corresponding second backup pad 32 fixed connection for the vertical fixed position of spacing a pair of connecting block 35.
Further, the carriage 11 includes a connection plate 111 arranged parallel to the width direction of the test stand, and the lower end of the second support plate 32 is fixedly connected to the connection plate 111;
a pair of groove sliding blocks 112 is correspondingly arranged at two ends of the connecting plate 111, and the pair of groove sliding blocks 112 is matched with a pair of slide rails 12 arranged in the length direction of the test bed 1; the middle parts of the pair of groove sliding blocks 112 are correspondingly provided with a pair of gaps 113, and the bottom end of the vacuum box 2 is correspondingly inserted in the pair of gaps 113 through the pair of insertion blocks 22.
Further, a pair of mounting cylinders 221 is correspondingly arranged at the second mounting hole and the vacuum flange 21, and a pair of mounting bosses is correspondingly arranged on the pair of mounting cylinders 221, and the pair of mounting bosses is locked and fixed by more than four hook-shaped calipers 222, so that the second support plate 32 is fixedly connected with the vacuum flange 21.
Further, the flash pyrolysis mechanism further comprises a bubbling tank 5, wherein the bubbling tank 5 comprises a cross-shaped communicating pipe and is fixedly arranged in the cylindrical cavity 41 through a pair of L-shaped supporting plates 51;
the sample inlet pipe 42 comprises a first sample inlet pipe and a second sample inlet pipe which are connected in an inserting manner, the inlet end of the first sample inlet pipe penetrates through the connecting flange 33, the outlet end of the first sample inlet pipe axially penetrates through the bubbling tank 5 and is connected with the inlet end of the second sample inlet pipe in an inserting manner, the outlet end of the second sample inlet pipe penetrates through the water-cooling cavity 45 and is connected with a silicon carbide pipe 46, and a pair of graphite electrodes 47 are sleeved on the silicon carbide pipe 46;
the vertical axis of the bubbling tank 5 is connected with the carrier gas.
Further, the cylindrical cavity 41 comprises a support sleeve 411 and a copper screen 412, the support sleeve 411 and the copper screen 412 are coaxially and fixedly connected through a flange, a sliding table support plate 413 is coaxially arranged at the lower end of the connecting end of the support sleeve 411 in an extending mode, the sliding table support plate 413 is inserted into the copper screen 412, and the sliding table 49 is horizontally arranged on the sliding table support plate 413.
Further, the mounting flange 33 is provided with three flange interfaces 331, and a thermocouple or a heating wire is inserted in a matching manner.
The beneficial technical effects of the invention are as follows:
(1) the invention relates to a low-pressure flash pyrolysis flow tube reaction device based on a continuous molecular beam source, which comprises a cube-shaped test bed, an installation mechanism, a flash pyrolysis mechanism and a vacuum box, wherein the flash pyrolysis mechanism comprises a cylindrical cavity horizontally arranged in the vacuum box, and a sample inlet tube, a water inlet tube and a water outlet tube which are arranged in the cylindrical cavity, one end of the cylindrical cavity is fixedly connected with an installation flange, a water cooling cavity is slidably arranged in the cavity at the other end of the cylindrical cavity, the extending end of the sample inlet tube is connected with a silicon carbide tube, and a pair of graphite electrodes is sleeved on the silicon carbide tube; therefore, the invention uses the silicon carbide tube as a reactor and uses the graphite electrode to resistively heat the silicon carbide tube, so that the reactant (sample) enters the silicon carbide tube after being mixed with the carrier gas and has very fast temperature rise rate (about 10)3K/s), so that reactants are heated up rapidly for pyrolysis in an ultrashort time (usually 50-200 microseconds), the gradient of the temperature and the product concentration in the radial direction can be reduced by a smaller inner diameter, a relatively uniform reaction environment is favorably created, the pyrolysis reaction at the temperature up to 2000K can be realized, the flash pyrolysis reaction is performed in a low-pressure environment by a vacuum box, the residence time of the reactants in a silicon carbide tube is shorter, the gas density is lower, the initial decomposition temperature is higher, the collision among molecules in the reaction process can be effectively reduced, the secondary reaction of a sample in the reaction tube can be greatly reduced, high-activity free radical species can be generated, the number density of the free radical species is considerable, no pollution is caused, early reaction products are favorably captured, the free radicals are not easy to annihilate under the low pressure, the graphite electrode is heated and extinguished rapidly, the secondary reaction is reduced, the continuous sampling can be realized, and the reaction kinetics research of the pyrolysis sample can be perfected in a larger temperature interval.
(2) The first supporting plate is adjustably arranged on one side of the second supporting plate through the adjusting mechanism, the other side of the second supporting plate is fixedly arranged on the front end face of the vacuum box through the vacuum flange, and the position of the flash pyrolysis mechanism in the vacuum box can be adjusted by adjusting the mounting position of the first supporting plate on the second supporting plate; meanwhile, a sliding table is arranged in the corresponding cylindrical cavity at the extension end of the push rod of the linear introducer, a sliding block is arranged on the sliding table in a matching mode, the extension end of the push rod is fixedly connected with the sliding block through threads, and the upper end of the sliding block is fixedly connected with the corresponding sample inlet pipe through a connecting lug, so that the silicon carbide pipe can horizontally move through the linear introducer; the position of the silicon carbide tube can be adjusted in a three-dimensional space through the position adjustment, so that the aim of controlling the signal intensity is fulfilled.
(3) The invention also comprises a bubbling tank, wherein carrier gas is introduced into the bubbling tank, the carrier gas and the sample are fully mixed in the bubbling tank and then introduced into the silicon carbide tube for pyrolysis, and when the invention is combined with a molecular beam sampling system and a flight time mass spectrum, a set of complete pyrolysis and mass spectrum device can be formed.
Drawings
FIG. 1 is a schematic view of the construction of a low pressure flash pyrolysis flow tube reactor apparatus of the present invention.
Fig. 2 is a schematic structural diagram of the test carrier of the present invention.
Fig. 3 is a schematic view of the structure of the carriage and the second support plate of the present invention.
FIG. 4 is a schematic structural view of a vacuum box and mounting mechanism of the present invention.
FIG. 5 is a schematic view of the structure of the installation mechanism and the flash pyrolysis mechanism of the present invention.
Fig. 6 is a cross-sectional view of fig. 5.
Fig. 7 is a schematic view of the structure of fig. 5 with the copper screen removed.
Fig. 8 is a schematic view of the structure of the flash pyrolysis mechanism and the bubbling tank of the present invention.
FIG. 9 is a schematic structural diagram of the water cooling section and the pyrolysis section of the present invention.
Wherein: the test bed comprises a test bed frame 1, a sliding frame 11, a 111 connecting plate, a pair of groove sliding blocks 112, a pair of sliding rails 12, a pair of gaps 121, a vacuum box 2, a vacuum flange 21, a pair of inserting blocks 22, a pair of installing cylinders 221, a pair of hook-shaped calipers 222, a first supporting plate 31, a second supporting plate 32, a mounting flange 33, a flange interface 331, a pair of connecting blocks 34, a pair of connecting limiting blocks 351, a pair of limiting blocks 35, a cylindrical cavity 41, a supporting sleeve 411, a copper screen 412, a sliding table supporting plate 413, a sample inlet pipe 42, a water inlet pipe 43, a water outlet pipe 44, a water cooling cavity 45, a silicon carbide pipe 46, a pair of graphite electrodes 47, a linear introducer 48, a sliding table 49, a sliding block 491, a 492 connecting convex block 492, a 5 bubbling tanks and a pair of L-shaped supporting plates 51.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Examples
Referring to fig. 1, 2 and 3, the low-pressure flash pyrolysis flow tube reaction device based on a continuous molecular beam source comprises a cubic test bench 1, a mounting mechanism, a flash pyrolysis mechanism and a vacuum box 2, wherein the vacuum box 2 is arranged at the upper end of the test bench 1 in a sliding manner through the matching of a sliding frame 11 and a pair of sliding rails 12; the test bed 1 is quite convenient for moving the instrument, and the pair of slide rails 12 can reduce a large amount of disassembly and assembly workload and reduce time wasted by disassembling and assembling the instrument.
Referring to fig. 4 and 5, the mounting mechanism includes a first support plate 31, a second support plate 32 and an adjusting mechanism, the first support plate 31 is adjustably mounted on one side of the second support plate 32 via the adjusting mechanism, the other side of the second support plate 32 is fixedly mounted on the front end surface of the vacuum chamber 2 via the vacuum flange 21,
a first mounting hole and a second mounting hole are correspondingly formed in the first support plate 31 and the second support plate 32 respectively, the first mounting hole is sealed through a mounting flange 33, and the second mounting hole is communicated with the vacuum box 2;
the adjusting mechanism comprises a pair of connecting blocks 34 and a pair of limiting blocks 35, a pair of grooves are vertically formed in the upper end and the lower end of the first supporting plate 31, the pair of limiting blocks 35 are arranged in the pair of grooves, and the vertical installation position of the first supporting plate 31 can be adjusted by adjusting the threaded fixed connection of the vertically arranged waist-shaped holes and the second supporting plate 32;
the pair of connecting blocks 34 are fixedly mounted on the second supporting plates 32 corresponding to the left and right sides of the first supporting plate 31, and a pair of adjusting bolts are horizontally inserted, and the threaded ends of the pair of adjusting bolts correspondingly abut against the left and right sides of the first supporting plate 31, and adjust the horizontal mounting position of the first supporting plate 31.
A pair of connecting grooves is respectively seted up in the vertical of a pair of connecting block 34, is equipped with a pair of stopper 341 of connecting in a pair of connecting groove, and a pair of stopper 341 of connecting and corresponding second backup pad 32 fixed connection for the horizontal fixed position of a spacing pair of connecting block 34. The position of the flash pyrolysis mechanism within the vacuum chamber 2 can be adjusted by adjusting the mounting position of the first support plate 31 on the second support plate 32.
Referring to fig. 6, the flash pyrolysis mechanism comprises a cylindrical cavity 41 horizontally arranged in the vacuum box 2, and a sample inlet pipe 42, a water inlet pipe 43 and a water outlet pipe 44 arranged in the cylindrical cavity 41, wherein one end of the cylindrical cavity 41 is fixedly connected with the mounting flange 33, a water cooling cavity 45 is slidably arranged in the cavity at the other end of the cylindrical cavity 41,
one end of each of the water inlet pipe 43, the water outlet pipe 44 and the sample inlet pipe 42 respectively penetrates through the mounting flange 33, the other end of each of the water inlet pipe 43 and the water outlet pipe 44 is respectively communicated with the water-cooling cavity 45, the other end of the sample inlet pipe 42 penetrates through the water-cooling cavity 45, the extending end of the sample inlet pipe is connected with a silicon carbide pipe 46, and a pair of graphite electrodes 47 are sleeved on the silicon carbide pipe 46; the silicon carbide tube 46 has an inner diameter of 1mm, an outer diameter of 2mm, and a length of 40mm, and the silicon carbide tube 46 having a small inner diameter, which is fitted with a pair of graphite electrodes 47, has a very fast temperature rise rate (about 10 a)3K/s) to quickly heat the reactants for pyrolysis in an ultrashort time (usually 50-200 microseconds), wherein the quick heating can greatly reduce the secondary reaction of the sample in the silicon carbide tube 46 reaction tube, can generate high-activity radical species, has considerable number density and no pollution, and is beneficial to capturing reaction products of early reaction such as unstable reaction intermediates and short-lived easily quenched intermediates.
And under the low pressure environment that this device realized, low pressure pyrolysis makes reactant dwell time shorter in carborundum pipe 46, and gas density is lower and initial decomposition temperature is higher, can effectively reduce the collision between the molecule in the reaction process, can be better the free radical in the detection reaction, and to the capture of these unstable midbodies for follow-up analysis perfects the sample reaction mechanism and has very big advantage.
Referring to fig. 7, a linear introducer 48 is inserted into the mounting flange 33, a sliding table 49 is arranged in the cylindrical cavity 41 corresponding to the push rod extension end of the linear introducer 48, a sliding block 491 is arranged on the sliding table 49 in a matching manner, the push rod extension end is fixedly connected with the sliding block 491 through threads, and the upper end of the sliding block 491 is fixedly connected with the corresponding sample injection tube 42 through a connecting bump 492, so that the silicon carbide tube 46 can horizontally move through the linear introducer 48, which is very convenient.
The carriage 11 comprises a connecting plate 111 arranged in parallel with the width direction of the test bench, and the lower end of the second supporting plate 32 is fixedly connected with the connecting plate 111;
a pair of groove sliding blocks 112 is correspondingly arranged at two ends of the connecting plate 111, and the pair of groove sliding blocks 112 is matched with a pair of slide rails 12 arranged in the length direction of the test bed 1; a pair of gaps 113 are correspondingly formed in the middle of the pair of groove sliding blocks 112, and the bottom end of the vacuum box 2 is correspondingly inserted into the pair of gaps 113 through a pair of insertion blocks 22.
The second mounting hole opening and the opening of the vacuum flange 21 are correspondingly provided with a pair of mounting cylinders 221, and the pair of mounting cylinders 221 are correspondingly provided with a pair of mounting bosses, and the pair of mounting bosses are locked and fixed by more than four hook-shaped calipers 222, so that the second support plate 32 is fixedly connected with the vacuum flange 21.
Referring to fig. 8 and 9, the flash pyrolysis mechanism further comprises a bubbling tank 5, wherein the bubbling tank 5 comprises a cross-shaped communicating pipe and is fixedly arranged in the cylindrical cavity 41 through a pair of L-shaped supporting plates 51;
the sample inlet pipe 42 comprises a first sample inlet pipe and a second sample inlet pipe which are connected in an inserting manner, the inlet end of the first sample inlet pipe penetrates through the connecting flange 33, the outlet end of the first sample inlet pipe axially penetrates through the bubbling tank 5 and is connected with the inlet end of the second sample inlet pipe in an inserting manner, the outlet end of the second sample inlet pipe penetrates through the water-cooling cavity 45 and is connected with a silicon carbide pipe 46, and a pair of graphite electrodes 47 are sleeved on the silicon carbide pipe 46;
the vertical axial direction of the bubbling tank 5 is communicated with carrier gas, and when the device is combined with a molecular beam sampling system and a flight time mass spectrum, a set of complete pyrolysis and mass spectrum device can be formed.
The cylindrical cavity 41 comprises a supporting sleeve 411 and a copper screen 412, the supporting sleeve 411 and the copper screen 412 are coaxially and fixedly connected through flanges, a sliding table supporting plate 413 is coaxially arranged at the lower end port of the connecting end of the supporting sleeve 411 in an extending mode, the sliding table supporting plate 413 is inserted into the copper screen 412, and the sliding table 49 is horizontally arranged on the sliding table supporting plate 413. An observation window is arranged in the axial direction of the supporting sleeve 411, so that the reaction condition can be observed conveniently.
The mounting flange 33 is provided with three flange interfaces 331, and thermocouples or heating wires are inserted in a matching manner to monitor the reaction temperature in real time.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A low-pressure flash pyrolysis flow tube reaction device based on a continuous molecular beam source is characterized in that: the device comprises a cube-shaped test bench (1), an installation mechanism, a flash pyrolysis mechanism and a vacuum box (2), wherein the vacuum box (2) is arranged at the upper end of the test bench (1) in a sliding manner through the matching of a sliding frame (11) and a pair of sliding rails (12);
the mounting mechanism comprises a first supporting plate (31), a second supporting plate (32) and an adjusting mechanism, the first supporting plate (31) is adjustably mounted on one side of the second supporting plate (32) through the adjusting mechanism, the other side of the second supporting plate (32) is fixedly mounted on the front end surface of the vacuum box (2) through a vacuum flange (21),
a first mounting hole and a second mounting hole are correspondingly formed in the first supporting plate (31) and the second supporting plate (32) respectively, the first mounting hole is sealed through a mounting flange (33), and the second mounting hole is communicated with the vacuum box (2);
the flash pyrolysis mechanism comprises a cylindrical cavity (41) horizontally arranged in the vacuum box (2), and a sample inlet pipe (42), a water inlet pipe (43) and a water outlet pipe (44) which are arranged in the cylindrical cavity (41), one end of the cylindrical cavity (41) is fixedly connected with the mounting flange (33), a water cooling cavity (45) is slidably arranged in the cavity at the other end of the cylindrical cavity (41), one ends of the water inlet pipe (43), the water outlet pipe (44) and the sample inlet pipe (42) respectively penetrate through the mounting flange (33), the other ends of the water inlet pipe (43) and the water outlet pipe (44) are respectively communicated with the water cooling cavity (45), the other end of the sample inlet pipe (42) penetrates through the water cooling cavity (45), the extending end of the sample inlet pipe is connected with a silicon carbide pipe (46), and a pair of graphite electrodes (47) is sleeved on the silicon carbide pipe (46);
a linear introducer (48) is inserted into the mounting flange (33), a sliding table (49) is arranged in a cylindrical cavity (41) corresponding to a push rod extending end of the linear introducer (48), a sliding block (491) is arranged on the sliding table (49) in a matching manner, the push rod extending end is fixedly connected with the sliding block (491) in a threaded manner, and the upper end of the sliding block (491) is fixedly connected with a corresponding sample inlet pipe (42) through a connecting lug (492), so that the silicon carbide pipe (46) can horizontally move through the linear introducer (48);
the adjusting mechanism comprises a pair of connecting blocks (34) and a pair of limiting blocks (35), a pair of grooves are vertically formed in the upper end and the lower end of the first supporting plate (31), the pair of limiting blocks (35) are arranged in the pair of grooves and fixedly connected with the second supporting plate (32) through adjusting the vertically arranged waist-shaped holes in a threaded manner, and the vertical mounting position of the first supporting plate (31) can be adjusted;
the pair of connecting blocks (34) are fixedly installed on the second supporting plates (32) corresponding to the left side and the right side of the first supporting plate (31) and are horizontally inserted with a pair of adjusting bolts, and the threaded ends of the pair of adjusting bolts correspondingly abut against the left side and the right side of the first supporting plate (31) and adjust the horizontal installation position of the first supporting plate (31).
2. The continuous molecular beam source based low pressure flash pyrolysis flow tube reactor of claim 1, wherein: a pair of connecting grooves are respectively formed in the vertical direction of the pair of limiting blocks (35), a pair of connecting limiting blocks (351) are arranged in the pair of connecting grooves, and the pair of connecting limiting blocks (351) are fixedly connected with the corresponding second supporting plate (32) and used for limiting the vertical fixing positions of the pair of limiting blocks (35).
3. The continuous molecular beam source-based low pressure flash pyrolysis flow tube reactor device of claim 1, wherein: the sliding frame (11) comprises a connecting plate (111) arranged in parallel to the width direction of the test bench, and the lower end of the second supporting plate (32) is fixedly connected with the connecting plate (111);
a pair of groove sliding blocks (112) is correspondingly arranged at two ends of the connecting plate (111), and the pair of groove sliding blocks (112) is matched with a pair of sliding rails (12) arranged in the length direction of the test bench (1); a pair of gaps (121) are correspondingly formed in the middle of the pair of sliding rails (12), and the bottom end of the vacuum box (2) is correspondingly inserted into the pair of gaps (121) through a pair of insertion blocks (22).
4. The continuous molecular beam source based low pressure flash pyrolysis flow tube reactor of claim 1, wherein: the second mounting hole orifice and the orifice of the vacuum flange (21) are correspondingly provided with a pair of mounting cylinders (221), a pair of mounting bosses are correspondingly arranged on the pair of mounting cylinders (221), and the pair of mounting bosses are locked and fixed through more than four hook-shaped calipers (222), so that the second support plate (32) is fixedly connected with the vacuum flange (21).
5. The continuous molecular beam source-based low pressure flash pyrolysis flow tube reactor device of claim 1, wherein: the flash pyrolysis mechanism further comprises a bubbling tank (5), wherein the bubbling tank (5) comprises a cross communicating pipe and is fixedly arranged in the cylindrical cavity (41) through a pair of L-shaped supporting plates (51);
the sample inlet pipe (42) comprises a first sample inlet pipe and a second sample inlet pipe which are connected in an inserting mode, the inlet end of the first sample inlet pipe penetrates through the mounting flange (33), the outlet end of the first sample inlet pipe axially penetrates through the bubbling tank (5) and is connected with the inlet end of the second sample inlet pipe in an inserting mode, the outlet end of the second sample inlet pipe penetrates through the water-cooling cavity (45) and is connected with a silicon carbide pipe (46), and a pair of graphite electrodes (47) is sleeved on the silicon carbide pipe (46);
the vertical axial direction of the bubbling tank (5) is communicated with carrier gas.
6. The continuous molecular beam source-based low pressure flash pyrolysis flow tube reactor device of claim 1, wherein: cylinder chamber (41) are including supporting sleeve (411) and copper screen (412), and supporting sleeve (411) and copper screen (412) pass through the coaxial fixed connection of flange, and the coaxial extension of port has arranged slip table backup pad (413) under the link of supporting sleeve (411), and slip table backup pad (413) are inserted and are located in copper screen (412), slip table (49) horizontal arrangement is on slip table backup pad (413).
7. The continuous molecular beam source based low pressure flash pyrolysis flow tube reactor of claim 1, wherein: the mounting flange (33) is provided with three flange interfaces (331) which are inserted with thermocouples or heating wires in a matching way.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111203066.7A CN113908771B (en) | 2021-10-15 | 2021-10-15 | Low-pressure flash pyrolysis flow tube reaction device based on continuous molecular beam source |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111203066.7A CN113908771B (en) | 2021-10-15 | 2021-10-15 | Low-pressure flash pyrolysis flow tube reaction device based on continuous molecular beam source |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113908771A CN113908771A (en) | 2022-01-11 |
| CN113908771B true CN113908771B (en) | 2022-07-15 |
Family
ID=79240789
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111203066.7A Active CN113908771B (en) | 2021-10-15 | 2021-10-15 | Low-pressure flash pyrolysis flow tube reaction device based on continuous molecular beam source |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113908771B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101301600A (en) * | 2008-06-30 | 2008-11-12 | 浙江理工大学 | Reciprocating type high-temperature synthesizing device |
| CN104495746A (en) * | 2014-12-12 | 2015-04-08 | 中山大学 | Device for producing synthetic gas by pyrolysis of biomass from plasma |
| CN105157416A (en) * | 2015-09-16 | 2015-12-16 | 苏州汇科机电设备有限公司 | High-temperature vacuum sintering furnace |
| CN107576717A (en) * | 2017-10-24 | 2018-01-12 | 中国科学技术大学 | A kind of in-situ detector for different diffusion length catalytic reaction gas phase intermediate products |
| CN108686609A (en) * | 2018-07-18 | 2018-10-23 | 中国工程物理研究院核物理与化学研究所 | A kind of fast cooling type Na131I destructive distillation process units |
| CN110618097A (en) * | 2019-09-04 | 2019-12-27 | 广东省测试分析研究所（中国广州分析测试中心） | Mercury morphological analysis pyrolysis device with adjustable and controllable temperature and flow rate and use method |
| WO2021184713A1 (en) * | 2020-03-17 | 2021-09-23 | 烽火通信科技股份有限公司 | Sintering device and sintering method for optical fiber preform soot body |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5700323B2 (en) * | 2009-06-08 | 2015-04-15 | 独立行政法人物質・材料研究機構 | Metal heat treatment furnace |
-
2021
- 2021-10-15 CN CN202111203066.7A patent/CN113908771B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101301600A (en) * | 2008-06-30 | 2008-11-12 | 浙江理工大学 | Reciprocating type high-temperature synthesizing device |
| CN104495746A (en) * | 2014-12-12 | 2015-04-08 | 中山大学 | Device for producing synthetic gas by pyrolysis of biomass from plasma |
| CN105157416A (en) * | 2015-09-16 | 2015-12-16 | 苏州汇科机电设备有限公司 | High-temperature vacuum sintering furnace |
| CN107576717A (en) * | 2017-10-24 | 2018-01-12 | 中国科学技术大学 | A kind of in-situ detector for different diffusion length catalytic reaction gas phase intermediate products |
| CN108686609A (en) * | 2018-07-18 | 2018-10-23 | 中国工程物理研究院核物理与化学研究所 | A kind of fast cooling type Na131I destructive distillation process units |
| CN110618097A (en) * | 2019-09-04 | 2019-12-27 | 广东省测试分析研究所（中国广州分析测试中心） | Mercury morphological analysis pyrolysis device with adjustable and controllable temperature and flow rate and use method |
| WO2021184713A1 (en) * | 2020-03-17 | 2021-09-23 | 烽火通信科技股份有限公司 | Sintering device and sintering method for optical fiber preform soot body |
Non-Patent Citations (2)
| Title |
|---|
| "Experimental and Kinetic Modeling Study of n Butanol Pyrolysis and Combustion";Jianghuai Cai et al.;《energy&fuels》;20120827;第26卷;全文 * |
| 油气生成过程实验研究的思考与展望;邹艳荣等;《石油实验地质》;20040830;第26卷(第04期);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113908771A (en) | 2022-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113908771B (en) | Low-pressure flash pyrolysis flow tube reaction device based on continuous molecular beam source | |
| JP2014524024A (en) | Sample presentation device for radiation-based analyzers | |
| CN104515824A (en) | Gas-phase substance analysis device and gas-phase introduction device | |
| Zolghadr et al. | On the Method of Pulse‐Heated Analysis of Solid Reactions (PHASR) for Polyolefin Pyrolysis | |
| CN104241074A (en) | Photo ionization mass spectrum device used for detecting products of laser heating reactor in situ | |
| Gibbins et al. | Experimental study of coal pyrolysis and hydropyrolysis at elevated pressures using a variable heating rate wire-mesh apparatus | |
| Teschmit et al. | Characterizing and optimizing a laser-desorption molecular beam source | |
| CN110632165B (en) | Biomass combustion aerosol preparation and detection integrated device and method thereof | |
| Gumerov et al. | Regeneration of the catalysts by supercritical fluid extraction | |
| Sargazi et al. | Modern Sample Preparation Techniques: A Brief Introduction | |
| Di Sanzo | Determination of oxygenates in gasoline range hydrocarbons by capillary column gas chromatography: a user's experience with an oxygen-specific detector (OFID) | |
| Zhang et al. | Determination of antimony, arsenic, bismuth, selenium, tellurium and tin by low pressure atomic absorption spectrometry with a quartz tube furnace atomizer and hydride generation with air addition | |
| Duangkaew et al. | In situ mass spectrometry of glucose decomposition under hydrothermal reactions | |
| CN115188516A (en) | Block sample irradiation device based on ion implanter and temperature control method | |
| Li et al. | Insight into the pyrolysis of benzene via a novel ultra-high temperature pyrolysis photoionization mass spectrometry | |
| Zhou et al. | Thermal-assisted gasification injector for analyzing high-salt solution samples: a novel device developed for online coupling of liquid chromatography with direct analysis in real time mass spectrometry | |
| CN111175806B (en) | Beam scattering target device and beam energy dissipation analyzer | |
| CN103675089B (en) | A kind of method analyzing coal tar pyrolysis low molecule product | |
| CN204155900U (en) | A kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product | |
| CN102226793B (en) | Portable fast detector for foaming agent of foam plastics | |
| CN105784855A (en) | Application of carbon nanotube-grafted carbon fiber composite filiform filler in vaporizing chamber of gas chromatograph | |
| CN204389459U (en) | Gaseous substance analytical equipment and gas phase gatherer | |
| Juvet et al. | Polymer identification and quantitative determination of additives by photolysis-gas chromatography | |
| CN208155947U (en) | A kind of analytical equipment for drug line detection | |
| Kojima et al. | Thermal decomposition of poly (γ-methyl-L-glutamate) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |