CN114088629B - High-temperature high-pressure gas-solid two-phase dynamic absorption tank device for spectrum analysis - Google Patents
High-temperature high-pressure gas-solid two-phase dynamic absorption tank device for spectrum analysis Download PDFInfo
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- CN114088629B CN114088629B CN202111400327.4A CN202111400327A CN114088629B CN 114088629 B CN114088629 B CN 114088629B CN 202111400327 A CN202111400327 A CN 202111400327A CN 114088629 B CN114088629 B CN 114088629B
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/39—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using tunable lasers
-
- G01N15/075—
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N2021/0106—General arrangement of respective parts
- G01N2021/0112—Apparatus in one mechanical, optical or electronic block
Abstract
The high-temperature high-pressure gas-solid two-phase dynamic absorption tank device for spectrum analysis comprises a furnace body consisting of two half furnace bodies, wherein a gas-solid sample pipeline is connected with a gas-solid sample inlet pipeline on a reaction tank; the discharge port of the solid storage device is connected with a gas-solid sample pipeline through a sample pipe branch; the feeding mechanism is arranged in the storage cavity, and the upper end of the feeding thimble penetrates out to the upper part of the storage cavity cover through the through hole; the ejection head is longitudinally and slidably arranged in the storage cavity and is arranged at the lower end of the feeding ejector pin; the second sealing ring and the first sealing ring are fixedly sleeved on the outer side of the lower portion of the feeding thimble at intervals up and down, and the outer ring surfaces are matched with the inner surface of the storage cavity in a sliding sealing mode. The device can provide stable high-temperature high-pressure environment, and is favorable for accurately analyzing molecular spectrums. The device can provide the gas environment of the mixed particulate matters with high temperature and high pressure, can be used for simulating the flame environment of the mixed carbon smoke particles in the combustion state, and is favorable for simultaneously detecting gas spectrum and extinction parameters of the particulate matters.
Description
Technical Field
The invention belongs to the technical field of laser spectrum detection, and particularly relates to a high-temperature high-pressure gas-solid two-phase dynamic absorption tank device for spectrum analysis.
Background
In industry, the burning phenomenon is accompanied in the production process of engineering raw materials such as steel, iron, nonferrous metals, quartz mud, ceramics, glass and the like, and the processing processes such as coking production, fertilizer production, petroleum refining and the like. Heating of living sites and daily food production, in most cases the preferred heat source is still combustion of fuel. However, fossil fuel combustion is also a main aspect of pollution, and various harmful gases such as sulfur oxides, nitrogen dioxide, nitric oxide, ozone, carbon monoxide and the like are generated in a partial combustion process, so that ecological environment is worsened and human health is endangered. In such a large environment, combustion efficiency is improved, and studies on reduction of greenhouse gas emissions have been increasingly conducted in recent years. Flame temperature, combustion gas product concentration, soot concentration and size have a significant impact on the combustion of the flame, and these parameters can accurately characterize the flame combustion state, so detection of these parameters is a primary detection target for current stage combustion diagnostics.
In recent years, due to the rapid development of laser technology, spectroscopic technology and electronic information technology, the gas diagnosis technology based on optical measurement has been rapidly developed, wherein the tunable semiconductor laser absorption spectroscopic technology is a trace gas detection technology with excellent sensitivity and accuracy, and the rapid development of the technology in recent years has good maturity and stability in the gas diagnosis field, and has the advantages of rapid response speed, large dynamic range, strong selectivity, low cost, simple and compact instrument structure and the like, and has been widely applied to the aspects of trace gas detection, greenhouse gas flux detection and the like. In order to eliminate the influence of various factors such as flow field stability, consistency, high temperature heat radiation and the like in high temperature and high pressure flame on optical detection, a high temperature and high pressure environment with only detection objects needs to be simulated, and the spectral detection technology is applied to gas and soot analysis under the environment of high temperature and high pressure, so that certain difficulty is brought to the application of the spectral detection technology, and the main difficulty is to maintain the tightness of the high temperature and high pressure gas environment and how to mix gas and particulate matters under the high pressure sealing, so that the simultaneous analysis of gas spectrum and particulate matter extinction signals cannot be realized by the existing analysis device, and the research progress of the gas spectrum and particulate matter extinction signals is limited.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a high-temperature high-pressure gas-solid two-phase dynamic absorption tank device for spectrum analysis, which can provide a gas environment of high-temperature high-pressure mixed particulate matters, can be used for simulating a flame environment of mixed soot particles in a combustion state, and is beneficial to simultaneous detection of gas spectrum and particulate matter extinction parameters.
The invention provides a high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis, which comprises a heating furnace, a gas cell, a first water-cooling pipe, a second water-cooling pipe, a first glass column, a second glass column, a first gas outlet pipeline, a gas-solid sample pipeline, a solid storage device and a feeding mechanism, wherein the first gas outlet pipeline is connected with the heating furnace;
the heating furnace consists of a first half furnace body and a second half furnace body, the first half furnace body and the second half furnace body are connected in a buckled mode, furnace grooves which are concave inwards are formed in the middle of the opposite surfaces, and left communicating grooves and right communicating grooves are formed in the left end and the right end of the buckling surfaces; heating resistance wires are arranged in the two hearth grooves; two hearth grooves in the buckled state form a heating cavity of the heating furnace, two left communication grooves in the buckled state form a left communication hole, and two right communication grooves in the buckled state form a right communication hole;
The upper end and the lower end of the hearth groove in the first half furnace body extend to the upper end face and the lower end face of the hearth groove respectively, and the upper end and the lower end of the hearth groove in the second half furnace body extend to the upper end face and the lower end face of the hearth groove respectively; upper communicating holes are formed at the upper ends of the two hearth grooves in the buckled state, and lower communicating holes are formed at the lower ends of the two hearth grooves in the buckled state;
the gas tank is internally provided with a reaction cavity, the upper ends of the gas tank are of cone structures, the centers of the upper ends and the centers of the lower ends of the gas tank are respectively and fixedly connected with a vertical gas-solid sample inlet pipeline and a solid sample outlet pipeline which are communicated with the reaction cavity, and the left ends and the right ends of the gas tank are respectively and fixedly connected with a first window pipeline and a second window pipeline which are communicated with the reaction cavity; the gas tank is arranged in the heating cavity, the upper end and the lower end of the gas tank are respectively communicated with the outside of the heating furnace through an upper communication hole and a lower communication hole, and the first window pipeline and the second window pipeline respectively penetrate out of the heating furnace through a left communication hole and a right communication hole; the first air outlet pipeline is fixedly connected to the upper end of the air tank, and the inner cavity of the first air outlet pipeline is communicated with the reaction cavity;
the first water cooling pipe and the second water cooling pipe are respectively arranged on the left side and the right side of the outside of the heating furnace, and are respectively spirally attached and wound on the outside of the left end of the first window pipeline and the outside of the right end of the second window pipeline;
The first glass column and the second glass column are respectively inserted into the first window pipeline and the second window pipeline, the first glass column and the first window pipeline are connected in a sealing way through vacuum silicone rubber, and the first glass column is communicated with a left axial straight-through light path of the reaction cavity; the second glass column is connected with the second window pipeline in a sealing way through vacuum silicone rubber, and the second glass column is communicated with a right axial straight-through light path of the reaction cavity;
the gas-solid sample pipeline is horizontally arranged above the heating furnace, the left end of the gas-solid sample pipeline is fixedly connected with the large-diameter end of the reducing straight-through clamping sleeve joint, and the right end of the gas-solid sample pipeline is connected with the upper end of the gas-solid sample inlet pipeline in a penetrating way through the right-angle clamping sleeve joint;
the solid storage device is vertically arranged above the gas-solid sample pipeline, a cylindrical storage cavity is formed in the solid storage device, a storage cavity cover is assembled at the upper end of the solid storage device, and a discharge hole at the lower end of the solid storage device is connected with the middle part of the gas-solid sample pipeline in a penetrating manner through a vertically arranged sample pipe branch; a through hole is formed in the center of the storage cavity cover; the middle part of the sample tube branch is connected with a spherical valve in series;
the feeding mechanism is arranged in the storage cavity and consists of a feeding thimble, a jacking head, a second sealing ring and a first sealing ring, and the upper end of the feeding thimble penetrates out to the upper side of the storage cavity cover through a through hole; the ejection head is longitudinally and slidably arranged in the storage cavity and is arranged at the lower end of the feeding thimble; the second sealing ring and the first sealing ring are fixedly sleeved on the outer side of the lower portion of the feeding thimble at intervals up and down, and the outer ring faces are matched with the inner surface of the storage cavity in a sliding sealing mode.
Furthermore, in order to ensure better sealing effect at two ends of the window pipeline, simultaneously, the straightness of an optical path can be ensured, and the window pipeline further comprises a first inner flange, a second inner flange, a first light-passing pipeline and a second light-passing pipeline;
the first inner flange is fixedly connected to the outside of the left end of the first window pipeline, a first groove is formed in the center of the joint surface of the first inner flange, a first sealing ring is assembled in the first groove, and the inner ring surface of the first sealing ring is in sealing connection with the outer circular surface of the left end of the first glass column; the second inner flange is fixedly connected to the outer part of the right end of the second window pipeline, a second groove is formed in the center of the joint surface of the second inner flange, a second sealing ring is assembled in the second groove, and the inner ring surface of the second sealing ring is in sealing connection with the outer circular surface of the right end of the second glass column;
the outer part of the right end of the first light transmission pipeline is fixedly connected with a first outer side flange, the center of the joint surface of the first outer side flange is provided with a first annular groove, the inner circular surface of the first outer side flange is provided with a second annular groove, and a first sealing ring and a second sealing ring are respectively assembled in the first annular groove and the second annular groove; the first light passage pipe is coaxially arranged at the left side of the first window pipeline, the first outer side flange is fixedly connected with the first inner side flange, the first sealing ring is connected with the first sealing ring in a fitting way, and the second sealing ring is connected with the outer circular surface of the left end of the first glass column extending into the first outer side flange in a sealing way;
The outer part of the left end of the second light-passing pipeline is fixedly connected with a second outer flange, the center of the joint surface of the second outer flange is provided with a third annular groove, the inner circular surface of the second outer flange is provided with a fourth annular groove, and a third sealing ring and a fourth sealing ring are respectively assembled in the third annular groove and the fourth annular groove; the second light-passing pipe is coaxially arranged on the right side of the second window pipeline, the second outer side flange is fixedly connected with the second inner side flange, the third sealing ring is connected with the second sealing ring in a fitting mode, and the fourth sealing ring is connected with the outer circular surface of the right end of the second glass column extending into the second outer side flange in a sealing mode.
The device further comprises a third inner flange, a second air outlet pipeline, a fourth inner flange and a fourth blind flange, wherein the third inner flange is fixedly connected to the outer part of the upper end of the first air outlet pipeline, a third groove is formed in the center of the joint surface of the first inner flange, and a third sealing ring is assembled in the third groove; a third outer flange is fixedly sleeved outside one end of the second air outlet pipeline, and the other end of the second air outlet pipeline is connected with a through valve; the third outer flange is fixedly connected with the third inner flange, and the third sealing ring is in sealing connection with the joint surface of the third outer flange; the fourth inner flange is fixedly sleeved outside the lower end of the solid sample discharge pipeline, a fourth groove is formed in the center of the joint surface of the fourth inner flange, and a fourth sealing ring is assembled in the fourth groove; the joint surface of the fourth blind plate flange is provided with a fifth annular groove, and a fifth sealing ring is assembled in the fifth annular groove; the fourth blind flange is fixedly connected with the fourth inner side flange, and the joint surface of the fourth blind flange and the fifth sealing ring are in sealing connection with the fourth sealing ring. The end part of the first air outlet pipeline is fixedly connected with the third inner flange, so that the first air outlet pipeline and the second air outlet pipeline with the third outer flange can be conveniently and reliably connected, and the first air outlet pipeline and the external pipeline can be conveniently and reliably connected; through the cooperation of fourth inboard flange and fourth blind flange, can carry out effectual closure to solid sample discharge line at mutual fixed connection, simultaneously, can also make solid sample discharge line and outside intercommunication at mutual separation.
Further, in order to facilitate stable and reliable connection of the two half furnace bodies, and simultaneously, in order to facilitate separation of the two half furnace bodies, the first half furnace body and the second half furnace body are fixedly connected together through a stainless steel clamp sleeved outside.
Further, in order to conveniently realize the operation of exhausting and supplying air to the gas absorption pipeline, the reducing straight-through clamping sleeve joint is connected with one interface of the three-way valve through a pipeline, the other two interfaces of the three-way valve are respectively connected with the vacuum pump and the high-pressure gas cylinder through the pipeline, a digital display pressure gauge and a flow control valve are connected in series on the pipeline between the reducing straight-through clamping sleeve joint and the three-way valve, the digital display pressure gauge is used for controlling the flow rate passing through the inside of the gas-solid sample pipeline, and the flow control valve is used for controlling the pressure change of the inside of the gas-solid sample pipeline.
Further, in order to make the diffusion of the particulate matters more uniform and to minimize the heat loss of the part exposed outside the heating furnace, the lower ends of the gas tanks are cone structures.
Furthermore, in order to ensure that the heat conductivity coefficient of the furnace body is lower, the cracking can not occur in the long-term heating process, and meanwhile, the energy-saving effect can be achieved, the first half furnace body and the second half furnace body are both made of high-temperature resistant fiber materials, and the heat insulation effect can be effectively ensured by adopting the high-temperature fiber materials; in order to have good high temperature resistance, oxidation resistance and heat conduction effects, the solid storage device, the gas-solid sample pipeline and the gas tank are all made of stainless steel materials; in order to ensure that the water-cooled tube has good extensibility and tensile property, thereby being capable of better manufacturing a threaded pipeline which is attached to a gas absorption pipeline, the first water-cooled tube and the second water-cooled tube are manufactured by processing copper tubes; in order to bear higher atmospheric pressure, ensure the consistency of temperature and have good near infrared light transmission performance, the first glass column and the second glass column are both made of JGS3 optical quartz glass.
Further, in order to effectively reduce interference effects in the light transmission process, two end faces of the first glass column and the second glass column form an inclined angle of 1.5 degrees with the vertical direction.
Further, in order to conveniently control the feeding action of the feeding thimble, a tail hole is formed in the upper end of the feeding thimble in a penetrating way in the radial direction, and a metal rod is arranged in the tail hole in a penetrating way; in order to conveniently control the temperature control process of the heating furnace, the heating resistance wire is connected with an external temperature control system; in order to effectively cool the sealing parts at two ends of the window pipeline, so that the situation that the sealing parts are damaged due to overhigh temperature of the end parts is prevented, and the high tightness of the two ends of the gas absorption pipeline is ensured, one end of the first water cooling pipe is connected with a cold water supply source, the other end of the first water cooling pipe is connected with a cooling water recovery tank, one end of the second water cooling pipe is connected with the cold water supply source, and the other end of the second water cooling pipe is connected with the cooling water recovery tank.
Further, in order to effectively monitor the temperature change condition of different positions in the reaction process, the surface of the gas tank is provided with a first temperature sensor, a second temperature sensor is arranged on the inner side of the first water cooling pipe on the first window pipeline, a third temperature sensor is arranged on the inner side of the second water cooling pipe on the second window pipeline, and the first temperature sensor, the second temperature sensor and the third temperature sensor are respectively used for collecting temperature signals of the gas tank, the end part of the first window pipeline and the end part of the second window pipeline.
According to the invention, the gas-solid sample pipeline is horizontally arranged above the gas tank, the left end of the gas-solid sample pipeline is connected with the large-diameter end of the reducing straight-through clamping sleeve joint, the right end of the gas-solid sample pipeline is connected with the upper end of the gas-solid sample inlet pipeline in a penetrating way through the right-angle clamping sleeve joint, and gas, solid or a gas-solid mixture can be conveniently supplied into the gas tank through the gas-solid sample pipeline, so that the reaction process of the solid-containing sample in the gas tank is realized; the first gas outlet pipeline is connected to the upper end of the gas tank, so that the gas in the reaction process or after the reaction is discharged can be conveniently. By connecting the solid sample discharge line to the lower end of the gas cell, it is possible to easily discharge the solid sample after the completion of the reaction to the outside. Through setting up vertical solid storage device in the top of gas-solid sample pipeline, can be convenient for add the solid reactant in the gas-solid sample pipeline, and then can be when letting in the gas reactant that has certain velocity of flow in the gas-solid sample pipeline, utilize the gaseous reactant of flow to take into the gas pond with the even, simultaneously, can also make the reactant realize the mixing each other in the in-process through the gas-solid sample pipeline to can be convenient for realize the abundant mixing between gaseous reactant and the solid reactant. The filled reaction gas can be pressurized through the arrangement of the reducing straight-through clamping sleeve connector, so that solid reaction particles can be more effectively driven to be fed into the reaction cavity of the reaction tank; through the arrangement of the right-angle clamping sleeve connector, the connection and the separation between the gas-solid sample pipeline and the gas-solid sample inlet pipeline can be conveniently realized, and the air flow can be effectively buffered, so that the supplied air flow can be prevented from disturbing the sample in the internal space of the reaction cavity, the reliable performance of the experimental process is effectively ensured, and more accurate experimental results can be obtained; in addition, the upper end of the gas tank is in a cone structure, so that mixed materials entering from a gas-solid sample entering pipeline can be uniformly scattered in the reaction cavity, and meanwhile, the gas flow filled in the reaction cavity can be further buffered by being matched with a right-angle clamping sleeve joint, so that the stability of the environment of the reaction cavity can be further ensured, the reliable performance of an experimental process is further ensured, and more accurate experimental results can be obtained; through the mutual cooperation of the solid storage device and the gas-solid sample pipeline, the gas tank can not only react gas reaction materials, but also react gas-solid mixture materials, thereby being beneficial to realizing the simultaneous analysis of gas spectrum and particle extinction signals and effectively increasing the universality of the device. First glass post and second glass post of cartridge respectively in first window pipeline and the second window pipeline at both ends about the gas pond through connecting to fill between window pipeline and glass post through vacuum silica gel, can effectively prolong the length of sealing portion, and then can effectually increase the sealed effect of gas pond, can avoid making sealing portion damage because of the influence of high temperature in the gas pond heating process, simultaneously, the setting of glass post can also guarantee to have outstanding spectral transmittance. Through being equipped with first water-cooled tube and second water-cooled tube around the tip at first window pipeline and second window pipeline respectively, can utilize the water-cooling to realize the continuous cooling to tip sealing portion to can make the temperature of the sealing portion of tip can not rise to too high, in order to avoid the tip sealing portion sealing member to take place the condition of damaging because of the high temperature to appear, like this, effectively guaranteed the inside gas tightness of gas pool at high temperature in-process, thereby can ensure the experimental environment that possess high temperature high pressure. The device has excellent spectral transmittance, high temperature resistance, oxidation resistance and acid and alkali corrosion resistance, has good heat conduction effect, can be used for simulating the flame environment of the mixed carbon smoke particles in a combustion state, and is favorable for simultaneously detecting gas spectrum and particulate matter extinction parameters.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention;
FIG. 2 is a schematic view of the structure of the first half furnace body or the second half furnace body in the invention;
FIG. 3 is a schematic view of the structure of a gas cell in the present invention;
FIG. 4 is a schematic view of the construction of a first inboard flange of the present invention;
FIG. 5 is a schematic view of the construction of a first outboard flange of the present invention;
FIG. 6 is a schematic view of a second inboard flange according to the present invention;
FIG. 7 is a schematic view of the construction of a second outboard flange of the present invention;
FIG. 8 is a schematic view of a third inboard flange according to the present invention;
FIG. 9 is a schematic view of a third outboard flange according to the present invention;
FIG. 10 is a schematic view of a fourth inboard flange according to the present invention;
FIG. 11 is a schematic view of a fourth blind flange according to the present invention;
fig. 12 is a schematic structural view of the feeding mechanism in the present invention.
In the figure: 1. a reducing straight-through clamping sleeve joint, 2, a spherical valve, 3, a right-angle clamping sleeve joint, 4, a gas-solid sample pipeline, 5, a solid storage device, 6, a storage cavity cover, 7, a feeding thimble, 8, a third inner flange, 9, a third outer flange, 10, a second water cooling pipe, 11, a second outer flange, 12, a second inner flange, 13, a second half furnace body, 14, a fourth inner flange, 15, a fourth blind flange, 16, a gas tank, 17, a first water cooling pipe, 18, a first inner flange, 19, a first outer flange, 20, a first half furnace body, 21, a first glass column, 22, a second glass column, 23 and a first groove, 24, annular grooves one, 25, annular grooves two, 26, second grooves 27, annular grooves three, 28, annular grooves four, 29, a first light-passing pipeline, 30, a second light-passing pipeline, 31, an air outlet pipeline two, 32, a third groove 33, annular grooves five, 34, a fourth groove, 35, a plug, 36, a first sealing ring, 37, a second sealing ring, 38, a tail hole, 39, a left communicating groove, 40, a right communicating groove, 41, a hearth groove, 42, a gas-solid sample inlet pipeline, 43, a solid sample discharge pipeline, 44, a storage cavity, 45, a sample pipe branch, 46, a first window pipeline, 47, a second window pipeline, 48 and an air outlet pipeline one.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
As shown in fig. 1 to 12, a high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis comprises a heating furnace, a gas cell 16, a first water-cooling pipe 17, a second water-cooling pipe 10, a first glass column 21, a second glass column 22, a first gas outlet pipeline 48, a gas-solid sample pipeline 4, a solid storage device 5 and a feeding mechanism;
the heating furnace consists of a first half furnace body 20 and a second half furnace body 13, the first half furnace body 20 and the second half furnace body 13 are connected in a buckled mode, a furnace tank 41 which is concave inwards is formed in the middle of the opposite surface, and a left communicating groove 39 and a right communicating groove 40 are formed in the left end and the right end of the buckled surface; heating resistance wires are uniformly distributed in the two hearth grooves 41; the two hearth grooves 41 in the buckled state form a heating cavity of the heating furnace, the two left communicating grooves 39 in the buckled state form a left communicating hole, and the two right communicating grooves 40 in the buckled state form a right communicating hole;
the upper end and the lower end of the hearth groove 41 in the first half furnace body 20 extend to the upper end face and the lower end face respectively, and the upper end and the lower end of the hearth groove 41 in the second half furnace body 13 extend to the upper end face and the lower end face respectively; upper communication holes are formed at the upper ends of the two hearth grooves 41 in the buckled state, and lower communication holes are formed at the lower ends of the two hearth grooves 41 in the buckled state;
The gas tank 16 is provided with a reaction cavity, the upper ends of the reaction cavity are of cone structures, the centers of the upper ends and the centers of the lower ends of the reaction cavity are respectively and fixedly connected with a vertical gas-solid sample inlet pipeline 42 and a solid sample outlet pipeline 43 which are communicated with the reaction cavity, the left ends and the right ends of the reaction cavity are respectively and fixedly connected with a first window pipeline 46 and a second window pipeline 47 which are communicated with the reaction cavity, and the first window pipeline 46 and the second window pipeline 47 are arranged oppositely left and right and coaxially; the gas tank 16 is installed in the heating chamber, and the upper and lower ends thereof are respectively communicated with the outside of the heating furnace through an upper communication hole and a lower communication hole, and the first and second window pipes 46 and 47 are respectively penetrated out of the outside of the heating furnace through a left communication hole and a right communication hole; the first air outlet pipeline 48 is fixedly connected to the upper end of the air tank 16, and the inner cavity of the first air outlet pipeline is communicated with the reaction cavity;
in order to effectively cool the sealing parts at the two ends of the gas tank and prevent the sealing parts from being damaged due to overhigh temperature at the end parts, so as to ensure high tightness at the two ends of the gas absorption pipeline, the first water-cooling pipe 17 and the second water-cooling pipe 10 are respectively arranged at the left side and the right side of the outside of the heating furnace and respectively spirally attached and wound at the left end of the first window pipeline 46 and the right end of the second window pipeline 47;
The first glass column 21 and the second glass column 22 are respectively inserted into the first window pipeline 46 and the second window pipeline 47, the first glass column 21 and the first window pipeline 46 are connected through vacuum silicone rubber in a sealing way, and the first glass column 21 forms a left axial straight-through light path communicated to the reaction cavity; as one preference, the right end of the first glass column 21 is flush with the right end of the first window line 46, the left end of the first glass column 21 extends to the left of the left end of the first window line 46, and the vacuum silicone rubber fills the space between the first glass column 21 and the first window line 46; the second glass column 22 and the second window pipeline 47 are connected in a sealing way through vacuum silicone rubber, and the second glass column 22 forms a right axial straight-through light path communicated with the reaction cavity, preferably, the left end of the second glass column 22 is flush with the left end of the second window pipeline 47, the right end of the second glass column 22 extends to the right side of the right end of the second window pipeline 47, and the vacuum silicone rubber is distributed in the space between the second glass column 22 and the second window pipeline 47; the left axial straight-through light path and the right axial straight-through light path are coaxially arranged;
the gas-solid sample pipeline 4 is horizontally arranged above the heating furnace, the left end of the gas-solid sample pipeline is fixedly connected with the large-diameter end of the reducing straight-through clamping sleeve joint 1, and the right end of the gas-solid sample pipeline is connected with the upper end of the gas-solid sample inlet pipeline 42 in a penetrating way through the right-angle clamping sleeve joint 3;
The solid storage device 5 is vertically arranged above the gas-solid sample pipeline 4, a cylindrical storage cavity 44 is formed in the solid storage device, a storage cavity cover 6 is assembled at the upper end of the solid storage device, and a discharge hole at the lower end of the solid storage device is connected with the middle part of the gas-solid sample pipeline 4 in a penetrating manner through a vertically arranged sample pipe branch 45; a through hole is formed in the center of the storage cavity cover 6; the middle part of the sample tube branch 45 is connected in series with a spherical valve 2, and the spherical valve 2 is a stainless steel clamping sleeve spherical valve as one preferable choice; as a further preferred aspect, the solid storage device 5 is disposed near the left end of the gas-solid sample line 4, so that the gas and the solid have a longer mixing time in the gas-solid sample line 4, and can be introduced into the reaction cavity of the reaction tank 6 after being uniformly mixed.
The feeding mechanism is arranged in the storage cavity 44 and consists of a feeding thimble 7, a top head 35, a second sealing ring 37 and a first sealing ring 36, wherein the upper end of the feeding thimble 7 passes through a through hole to penetrate out of the upper part of the storage cavity cover 6, and a tail hole 38 radially penetrates through the upper end of the feeding thimble; the ejector head 35 is longitudinally and slidably arranged in the storage cavity 44 and is arranged at the lower end of the feeding ejector pin 7; the second sealing ring 37 and the first sealing ring 36 are fixedly sleeved at the outer side of the lower part of the feeding thimble 7 at intervals up and down, and the outer annular surfaces are matched with the inner surface of the storage cavity 44 in a sliding sealing manner.
In order to make the sealing effect of the two ends of the window pipeline better, and at the same time, the straightness of the optical path can be ensured, the window pipeline further comprises a first inner flange 18, a second inner flange 12, a first light-passing pipeline 29 and a second light-passing pipeline 30;
the first inner flange 18 is fixedly connected to the outside of the left end of the first window pipeline 46, a first groove 23 is formed in the center of the joint surface of the first inner flange, a first sealing ring is assembled in the first groove 23, and the inner ring surface of the first sealing ring is in sealing connection with the outer circular surface of the left end of the first glass column 21; the second inner flange 12 is fixedly connected to the outside of the right end of the second window pipeline 47, the center of the joint surface of the second inner flange is provided with a second groove 26, a second sealing ring is assembled in the second groove 26, and the inner ring surface of the second sealing ring is in sealing connection with the outer ring surface of the right end of the second glass column 22; as a preferable mode, the sealing ring is a fluororubber sealing ring, the highest bearable temperature of the fluororubber sealing ring and high-temperature silicone rubber is 500K, and the sealing structure of the optical window part can be guaranteed not to be damaged in high temperature by matching with a water cooling system, so that the air tightness of the gas tank 16 is effectively maintained.
The outer part of the right end of the first light transmission pipeline 29 is fixedly connected with a first outer side flange 19, the center of the joint surface of the first outer side flange 19 is provided with a first annular groove 24, the inner circular surface of the first outer side flange is provided with a second annular groove 25, and a first sealing ring and a second sealing ring are respectively assembled in the first annular groove 24 and the second annular groove 25; the first light-passing pipeline 29 is coaxially arranged at the left side of the first window pipeline 46, the first outer side flange 19 is fixedly connected with the first inner side flange 18, the first sealing ring is connected with the first sealing ring in a fitting way, and the second sealing ring is connected with the outer circular surface extending to the left end of the first glass column 21 in the first outer side flange 19 in a sealing way; through making sealing washer two and the left end sealing connection of first glass post, can cooperate vacuum silicone rubber to realize dual sealed effect.
The outer part of the left end of the second light-passing pipeline 30 is fixedly connected with a second outer side flange 11, the center of the joint surface of the second outer side flange 11 is provided with a third annular groove 27, the inner circular surface of the second outer side flange is provided with a fourth annular groove 28, and a third sealing ring and a fourth sealing ring are respectively assembled in the third annular groove 27 and the fourth annular groove 28; the second light-passing pipeline 30 is coaxially arranged on the right side of the second window pipeline 47, the second outer side flange 11 is fixedly connected with the second inner side flange 12, the third sealing ring is connected with the second sealing ring in a fitting mode, and the fourth sealing ring is in sealing connection with the outer circular surface extending to the right end of the second glass column 22 in the second outer side flange 11. Through making sealing washer four and the right-hand member sealing connection of second glass post, can cooperate vacuum silicone rubber to realize dual sealed effect. As a preferable mode, the sealing ring is a fluororubber sealing ring, the highest bearable temperature of the fluororubber sealing ring and high-temperature silicone rubber is 500K, and the sealing structure of the optical window part can be guaranteed not to be damaged in high temperature by matching with a water cooling system, so that the air tightness of the gas tank 16 is effectively maintained.
As a preferable mode, the first light-transmitting tube 29 and the second light-transmitting tube 30 are cylindrical stainless steel tubes, which are mainly used for detecting specific gases, when the content of the detected object in the air is high, the accuracy of detection can be affected by the exposure of an external light path in the air, and nitrogen is continuously introduced into the tubes during spectrum detection, so that the air in the external light path of the gas pool 16 can be removed, and the influence of components in the air on the detection result can be eliminated.
As a preferable mode, the device further comprises a third inner flange 8, a second air outlet pipeline 31, a fourth inner flange 14 and a fourth blind flange 15, wherein the third inner flange 8 is fixedly connected to the outer part of the upper end of the first air outlet pipeline 48, a third groove 32 is formed in the center of the joint surface of the third inner flange, and a third sealing ring is assembled in the third groove 32; the third outer flange 9 is fixedly sleeved outside one end of the second air outlet pipeline 31, and the other end of the second air outlet pipeline is connected with a through valve, so that the second air outlet pipeline 31 is preferably a stainless steel capillary, and a stainless steel clamping sleeve needle valve is arranged in the middle of the second air outlet pipeline to control the flow rate and the on-off of air conveniently; the third outer flange 9 is fixedly connected with the third inner flange 8, and the third sealing ring is in sealing connection with the joint surface of the third outer flange 9; the fourth inner flange 14 is fixedly sleeved outside the lower end of the solid sample discharge pipeline 43, a fourth groove 34 is formed in the center of the joint surface of the fourth inner flange, and a fourth sealing ring is assembled in the fourth groove 34; an annular groove five 33 is formed in the joint surface of the fourth blind flange 15, and a sealing ring five is assembled in the annular groove five 33; the fourth blind flange 15 is fixedly connected with the fourth inner side flange 14, and the joint surface of the fourth blind flange 15 and the fifth sealing ring are in sealing connection with the fourth sealing ring. The end part of the first air outlet pipeline is fixedly connected with the third inner flange, so that the first air outlet pipeline and the second air outlet pipeline with the third outer flange can be conveniently and reliably connected, and the first air outlet pipeline and the external pipeline can be conveniently and reliably connected; through the cooperation of fourth inboard flange and fourth blind flange, can carry out effectual closure to solid sample discharge line at mutual fixed connection, simultaneously, can also make solid sample discharge line and outside intercommunication at mutual separation.
In order to facilitate the stable and reliable connection of the two half-furnace bodies, and simultaneously, in order to facilitate the separation of the two half-furnace bodies, the first half-furnace body 20 and the second half-furnace body 13 are fixedly connected together through stainless steel hoops sleeved outside. Preferably, the reducing straight-through clamping sleeve joint 1 is a stainless steel reducing straight-through clamping sleeve joint, and the right-angle clamping sleeve joint 3 is a stainless steel right-angle clamping sleeve joint.
In order to conveniently realize the operation of exhausting and supplying air to the gas absorption pipeline, the reducing straight-through clamping sleeve joint 1 is connected with one interface of the three-way valve through a pipeline, the other two interfaces of the three-way valve are respectively connected with a vacuum pump and a high-pressure gas cylinder through the pipeline, a digital display pressure gauge and a flow control valve are connected in series on the pipeline between the reducing straight-through clamping sleeve joint 1 and the three-way valve, the digital display pressure gauge is used for real-time pressure change inside the gas-solid sample pipeline 4, and the flow control valve is used for controlling flow inside the gas-solid sample pipeline 4. The whole gas pool can be pumped to vacuum by the vacuum pump, so that the accuracy of adding the gas sample is ensured. The high-pressure gas cylinder is filled with gas to be measured and diluent gas, so that the gas samples with different concentrations can be mixed. The flow control system controls the air flow rate of each bottle of air, helps to mix a gas sample of a specified concentration and controls the concentration of solid particulate matter. The digital display pressure gauge is used for detecting the 16 pressure in the gas tank, and the measuring range is-0.1 atm to 10atm.
The lower ends of the gas cells 16 are tapered in order to provide a more uniform diffusion of particulate matter and minimal loss of heat from the portion exposed to the exterior of the furnace.
In order to enable the heat conductivity coefficient of the furnace body to be low, the cracking can not occur in the long-term heating process, and meanwhile, the energy-saving effect can be achieved, the first half furnace body 20 and the second half furnace body 13 are made of high-temperature resistant fiber materials, and the heat insulation effect can be effectively guaranteed by adopting the high-temperature fiber materials; in order to have good high temperature resistance, oxidation resistance and heat conduction effects, the solid storage device 5, the gas-solid sample pipeline 4 and the gas tank 16 are all made of 316 stainless steel materials, and as the tested gas sample possibly carries high corrosive components, the pollution and corrosion of the tested gas sample to instrument parts are the most main reasons for causing equipment faults, the contact gas parts are made of corrosion resistant materials, so that the damage of the corrosive components to the equipment can be avoided; in order to make the water-cooled tube have good extensibility and stretching performance, so that the water-cooled tube can be better manufactured into a threaded pipeline which is attached to a gas absorption pipeline, the first water-cooled tube 17 and the second water-cooled tube 10 are manufactured by processing copper tubes; in order to withstand higher atmospheric pressure, ensure temperature uniformity and have good light transmission performance, the first glass column 21 and the second glass column 22 are made of JGS3 optical quartz glass.
In order to effectively reduce interference effects during light transmission, both end surfaces of the first glass column 21 and the second glass column 22 form an inclined angle of 1.5 degrees with respect to the vertical direction.
In order to control the feeding action of the feeding thimble conveniently, a metal rod is arranged in the tail hole 38 in a penetrating way; in order to conveniently control the temperature control process of the heating furnace and control the internal temperature in the hearth, the heating resistance wire is connected with an external temperature control system, and as a preference, the outer ends of the heating resistance wire extend out from the side edges of the first half furnace body 20 and the second half furnace body 13 and are wrapped by the insulating porcelain posts so as to avoid conditions such as high-temperature scalding, electric shock and the like. The end of the resistance wire is connected with a voltage controller through a ceramic wiring terminal, and the power of the heating furnace is controlled through the voltage controller, so that the effect of temperature regulation is achieved; in order to effectively cool the sealing parts at two ends of the window pipeline, so as to prevent the damage of the sealing parts caused by overhigh temperature of the end parts and ensure high tightness of the two ends of the gas absorption pipeline, one end of the first water cooling pipe 17 is connected with a cold water supply source, the other end of the first water cooling pipe is connected with a cooling water recovery tank, one end of the second water cooling pipe 10 is connected with the cold water supply source, and the other end of the second water cooling pipe is connected with the cooling water recovery tank. As a preference, the water flow rate is controlled to be higher than 1L/min during the cooling process to ensure the cooling effect
In order to effectively monitor the temperature change conditions of different positions in the reaction process, a first temperature sensor is arranged on the surface of the gas tank 16, a second temperature sensor is arranged on the inner side of the first water cooling pipe 17 on the first window pipeline 46, a third temperature sensor is arranged on the inner side of the second water cooling pipe 10 on the second window pipeline 47, and the first temperature sensor, the second temperature sensor and the third temperature sensor are respectively used for collecting temperature signals of the gas tank 16, the end part of the first window pipeline 46 and the end part of the second window pipeline 47.
As a preferable mode, the temperature sensor adopts a high-temperature-resistant K-type thermocouple, and a high-temperature ceramic fiber temperature measuring wire is selected to prevent temperature accuracy from being reduced due to the fact that the outer skin of the thermocouple wire is damaged at high temperature. The temperature consistency between two sides and the middle of the direction of the light path of the furnace body can be detected by arranging a plurality of thermocouples, and the device can improve the spatial resolution of the temperature of the direction of the light path by increasing the number of the thermocouples.
According to the invention, the gas-solid sample pipeline is horizontally arranged above the gas tank, the left end of the gas-solid sample pipeline is connected with the large-diameter end of the reducing straight-through clamping sleeve joint, the right end of the gas-solid sample pipeline is connected with the upper end of the gas-solid sample inlet pipeline in a penetrating way through the right-angle clamping sleeve joint, and gas, solid or a gas-solid mixture can be conveniently supplied into the gas tank through the gas-solid sample pipeline, so that the reaction process of the solid-containing sample in the gas tank is realized; the first gas outlet pipeline is connected to the upper end of the gas tank, so that the gas in the reaction process or after the reaction is discharged can be conveniently. By connecting the solid sample discharge line to the lower end of the gas cell, it is possible to easily discharge the solid sample after the completion of the reaction to the outside. Through setting up vertical solid storage device in the top of gas-solid sample pipeline, can be convenient for add the solid reactant in the gas-solid sample pipeline, and then can be when letting in the gas reactant that has certain velocity of flow in the gas-solid sample pipeline, utilize the gaseous reactant of flow to take into the gas pond with the even, simultaneously, can also make the reactant realize the mixing each other in the in-process through the gas-solid sample pipeline to can be convenient for realize the abundant mixing between gaseous reactant and the solid reactant. The filled reaction gas can be pressurized through the arrangement of the reducing straight-through clamping sleeve connector, so that solid reaction particles can be more effectively driven to be fed into the reaction cavity of the reaction tank; through the arrangement of the right-angle clamping sleeve connector, the connection and the separation between the gas-solid sample pipeline and the gas-solid sample inlet pipeline can be conveniently realized, and the air flow can be effectively buffered, so that the supplied air flow can be prevented from disturbing the sample in the internal space of the reaction cavity, the reliable performance of the experimental process is effectively ensured, and more accurate experimental results can be obtained; in addition, the upper end of the gas tank is in a cone structure, so that mixed materials entering from a gas-solid sample entering pipeline can be uniformly scattered in the reaction cavity, and meanwhile, the gas flow filled in the reaction cavity can be further buffered by being matched with a right-angle clamping sleeve joint, so that the stability of the environment of the reaction cavity can be further ensured, the reliable performance of an experimental process is further ensured, and more accurate experimental results can be obtained; through the mutual cooperation of the solid storage device and the gas-solid sample pipeline, the gas tank can not only react gas reaction materials, but also react gas-solid mixture materials, thereby being beneficial to realizing the simultaneous analysis of gas spectrum and particle extinction signals and effectively increasing the universality of the device. First glass post and second glass post of cartridge respectively in first window pipeline and the second window pipeline at both ends about the gas pond through connecting to fill between window pipeline and glass post through vacuum silica gel, can effectively prolong the length of sealing portion, and then can effectually increase the sealed effect of gas pond, can avoid making sealing portion damage because of the influence of high temperature in the gas pond heating process, simultaneously, the setting of glass post can also guarantee to have outstanding spectral transmittance. Through being equipped with first water-cooled tube and second water-cooled tube around the tip at first window pipeline and second window pipeline respectively, can utilize the water-cooling to realize the continuous cooling to tip sealing portion to can make the temperature of the sealing portion of tip can not rise to too high, in order to avoid the tip sealing portion sealing member to take place the condition of damaging because of the high temperature to appear, like this, effectively guaranteed the inside gas tightness of gas pool at high temperature in-process, thereby can ensure the experimental environment that possess high temperature high pressure. The device has excellent spectral transmittance, high temperature resistance, oxidation resistance and acid and alkali corrosion resistance, has good heat conduction effect, can be used for simulating the flame environment of the mixed carbon smoke particles in a combustion state, and is favorable for simultaneously detecting gas spectrum and particulate matter extinction parameters.
As a preferred embodiment:
the diameter of the reducing straight-through clamping sleeve joint 1 is 26mm to 6mm, the diameters of interfaces at two sides of the spherical valve 2 are 19mm, and the diameters of interfaces at two ends of the right-angle clamping sleeve joint 3 are 19mm.
The length of the gas-solid sample pipeline 4 with the outer diameter of 26mm and the inner diameter of 22mm is 700mm, and the length of the sample pipe branch 45 with the outer diameter of 19mm and the inner diameter of 17mm is 60mm.
The upper part of the solid storage device 5 has an outer diameter of 26mm, an inner diameter of 22mm and a length of 100mm, and the lower part has an outer diameter of 19mm and an inner diameter of 17mm and a length of 40mm. The outer diameter of the storage cavity cover 6 is 26mm and the height is 20mm. The total length of the feeding thimble 7 is 150mm, the middle interval of the diameter of the feeding thimble first sealing ring 36 and the diameter of the feeding thimble second sealing ring 37 are 19mm, the feeding thimble head 35 is a column table, the radius of the top end is 12mm, the radius of the low end is 19mm, the height is 15mm, and the interval between the feeding thimble head and the feeding thimble first sealing ring 36 is 5mm.
The gas-solid sample inlet 42, the solid sample outlet 43 and the gas outlet pipe 48 have the inner diameter of 22mm, the outer diameter of 26mm and the lengths of 30mm, 20mm and 30mm respectively, the outer diameter of 56mm, the inner diameter of 52mm and the length of 85mm of the first window pipe 46 and the second window pipe 47, and the outer diameter of 54mm, the inner diameter of 45mm and the length of 50mm of the first light-transmitting pipe 29 and the second light-transmitting pipe 30.
The first glass column 21 and the second glass column 22 are made of JGS3 materials, the transmittance of the near infrared spectrum is more than 90% under the length of 10mm, the diameter of the glass column is 50mm, the length of the glass column is 85mm, the round surfaces on two sides are polished, the radian of the round surfaces on two sides is 1.5 degrees, the light interference effect is prevented, and the side column surfaces are frosted to prevent stray light reflection.
The total height of the gas tank 16 is 220mm, the inner diameter 116 is 120mm, the outer diameter of the gas tank is 120mm, the height of the upper cone is 50mm, and the height of the lower cone is 20mm.
The first water cooling pipe 17 and the second water cooling pipe 10 are made of copper pipes, have good ductility and heat conductivity, are wound on the outer sides of the first window pipe 46 and the second window pipe 47, are connected in series with an external water tank water pump, and jointly form a water cooling system. The system can ensure that the high-temperature silicon rubber used for adhering the first glass column 21 and the second glass column 22 on the two sides of the optical window is not melted due to the over-high temperature, and the sealing ring is protected at a proper temperature. The sealing rings used by the device are fluororubber sealing rings, and the temperature resistance is higher than 500K.
For the multiple tests of the above embodiment example, the device has good working performance in the temperature range of 300K-1100K, the maximum average temperature deviation of the center and the two sides of the furnace body is 12.1K at the temperature of 500K, the maximum average temperature deviation of the center and the two sides of the furnace body is 21.4K at the temperature of 800K, the maximum average temperature deviation of the center and the two sides of the furnace body is 36.9K at the temperature of 1100K, and the allowable deviation range is reached. At 300K, the vacuum degree of the device can reach 15pa. Under vacuum conditions, the average gas leakage rate at 500K was 5Pa/min, the average gas leakage rate at 800K was 5Pa/min, and the average gas leakage rate at 1100K was 7Pa/min. At a maximum use pressure of 9atm, the average gas leakage rate at 500K is 20Pa/min, the average gas leakage rate at 800K is 24Pa/min, and the average gas leakage rate at 1100K is 37Pa/min. The highest use temperature of the device can reach 1300K, and the long-term use temperature is 1100K.
Working principle:
before use, the interior of the heating furnace should be cleaned, and the mirror surfaces at the two ends of the glass column should be wiped by alcohol.
Firstly, a water cooling system is started, the pressure of a water pump is regulated, and the water flow rate in the first water cooling pipe 17 and the second water cooling pipe 10 is ensured to be more than 1L/min. And (3) starting the mass flowmeter to preheat for 15 minutes to reach an optimal use state, closing the gas valves at two sides of the flowmeter to ensure zero setting operation on the flowmeter after no gas flows, and ensuring the accuracy of flowmeter indication. And opening the digital display pressure gauge. The temperature sensor and the temperature display are set and turned on. The high power voltage regulator is turned on and the input voltage is set. And after the temperature in the furnace reaches the temperature to be detected, starting gas detection.
Gas detection at normal pressure: at first, all valves in the whole system are closed, the gas pool 16 is closed by closing the valve communicated with the gas outlet pipeline II 31, the vacuum pump is opened, the valve connected with the vacuum pump and Chi Nalian is opened, the gas pool 16 is vacuumized, the digital display pressure gauge degree is observed, when the vacuum degree is lower than 30pa, the valve connected with the vacuum pump and Chi Nalian is firstly closed, and the vacuum pump can be closed after the valve is closed. At this time, the gas pool is in a vacuum state. The high-pressure gas cylinder is opened to press gas into the gas cylinder pressure reducing valve, the outlet pressure is controlled to be lower than 4atm, and the gas leakage caused by overlarge pressure difference on the two sides of ventilation of the flowmeter is prevented. According to the concentration of the target gas, the flow rate ratio of the flow meters of the diluent gas and the gas to be measured is regulated, the flow rate of the flow meters is regulated according to the concentration of the target particles, the falling speed of the particles is fixed, the concentration of the particles is lower when the flow rate of the gas is faster, and after the regulation is finished, the flow meters and the valves behind the flow meters are opened, so that the gas is flushed into a gas tank. When the degree of the display pressure gauge is observed and the air pressure in the air pool is higher than one atmosphere, the valve communicated with the flange air pipeline 31 is opened to enable the air pool to be communicated with the outside, so that the outside air can be prevented from flowing backwards, and a pure and flowing target air environment is obtained. In this case, the target gas with a fixed concentration and flow rate is in the gas pool at one atmosphere. After the pressure gauge and the flowmeter show stable numbers, the spherical valve 2 can be opened, the feeding thimble 7 is manually pressed to enable the materials to slowly fall into the gas-solid sample pipeline 4, and flowing target gas uniformly brings the particles into the gas pool to obtain a high-temperature gas environment of mixed particles.
Gas detection at high pressure: at first, all valves in the whole system are closed, the valve connected with the flange gas pipeline 31 is closed to seal the gas tank, the vacuum pump is opened, the valve connected with the vacuum pump and Chi Nalian is opened, the gas tank is vacuumized, the digital display pressure gauge degree is observed, when the vacuum degree is lower than 30pa, the valve connected with the vacuum pump and Chi Nalian is firstly closed, and the vacuum pump can be closed after the valve is closed. At this time, the gas pool is in a vacuum state. The high-pressure gas cylinder is opened to press gas into the gas cylinder pressure reducing valve, the outlet pressure is controlled to be lower than 4atm, and the gas leakage caused by overlarge pressure difference on the two sides of ventilation of the flowmeter is prevented. According to the concentration of the target gas, the flow rate ratio of the flow meters of the diluent gas and the gas to be measured is regulated, the flow rate of the flow meters is regulated according to the concentration of the target particles, the falling speed of the particles is fixed, the concentration of the particles is lower when the flow rate of the gas is faster, and after the regulation is finished, the flow meters and the valves behind the flow meters are opened, so that the gas is flushed into a gas tank. When the degree of the display pressure gauge is observed and the air pressure in the air tank is higher than one atmosphere, the valve communicated with the flange air pipeline 31 is opened to enable the air tank to be communicated with the outside, the opening size of the valve is regulated to enable the air pressure in the air tank to continuously rise, the pressure of the outlet of the pressure reducing valve of the air bottle is required to be regulated in the air pressure rising process, the pressure of the air inlet end of the flowmeter is enabled to be higher than the pressure of the air outlet end, and the air outlet valve is regulated to be stable in pressure after the pressure rises to the target pressure. At this time, the gas pool is filled with a target gas with a fixed concentration and flow rate of the target gas pressure. After the pressure gauge and the flowmeter show stable numbers, the spherical valve 2 can be opened, the feeding thimble 7 is manually pressed to enable the materials to slowly fall into the gas-solid sample pipeline 4, and the flowing target gas uniformly brings the particles into the gas pool to obtain a high-temperature and high-pressure gas environment for mixing the particles.
Claims (10)
1. The utility model provides a high temperature high pressure gas-solid two-phase dynamic absorption cell device for spectral analysis, includes heating furnace, gas tank (16), first water-cooled tube (17), second water-cooled tube (10), first glass post (21) and second glass post (22), the heating furnace comprises first half furnace body (20) and second half furnace body (13), and first half furnace body (20) and second half furnace body (13) looks buckled are connected to furnace tank (41) that inwards caves in are seted up at the middle part of opposite face all, left intercommunication groove (39) and right intercommunication groove (40) have all been seted up at the left and right sides of buckling face; heating resistance wires are uniformly distributed in the two hearth grooves (41); two hearth grooves (41) in the buckled state form a heating cavity of the heating furnace, two left communication grooves (39) in the buckled state form a left communication hole, and two right communication grooves (40) in the buckled state form a right communication hole;
the device is characterized by further comprising an air outlet pipeline I (48), an air-solid sample pipeline (4), a solid storage device (5) and a feeding mechanism;
the upper end and the lower end of a hearth groove (41) in the first half furnace body (20) respectively extend to the upper end face and the lower end face of the hearth groove, and the upper end and the lower end of the hearth groove (41) in the second half furnace body (13) respectively extend to the upper end face and the lower end face of the hearth groove; upper communication holes are formed at the upper ends of the two hearth grooves (41) in the buckled state, and lower communication holes are formed at the lower ends of the two hearth grooves (41) in the buckled state;
The inside of the gas tank (16) is provided with a reaction cavity, the upper end of the gas tank is of a cone structure, the center of the upper end and the center of the lower end of the gas tank are respectively and fixedly connected with a vertical gas-solid sample inlet pipeline (42) and a solid sample outlet pipeline (43) which are communicated with the reaction cavity, and the left end and the right end of the gas tank are respectively and fixedly connected with a first window pipeline (46) and a second window pipeline (47) which are communicated with the reaction cavity; the gas tank (16) is arranged in the heating cavity, the upper end and the lower end of the gas tank are respectively communicated with the outside of the heating furnace through an upper communication hole and a lower communication hole, and a first window pipeline (46) and a second window pipeline (47) respectively penetrate out of the outside of the heating furnace through a left communication hole and a right communication hole; the first air outlet pipeline (48) is fixedly connected to the upper end of the air tank (16), and the inner cavity of the first air outlet pipeline is communicated with the reaction cavity;
the first water cooling pipe (17) and the second water cooling pipe (10) are respectively arranged on the left side and the right side of the outside of the heating furnace, and are respectively spirally attached and wound on the outside of the left end of the first window pipeline (46) and the outside of the right end of the second window pipeline (47);
the first glass column (21) and the second glass column (22) are respectively inserted into the first window pipeline (46) and the second window pipeline (47), the first glass column (21) and the first window pipeline (46) are connected in a sealing manner through vacuum silicone rubber, and the first glass column (21) forms a left axial straight-through light path communicated to the reaction cavity; the second glass column (22) and the second window pipeline (47) are connected in a sealing way through vacuum silicone rubber, and the second glass column (22) forms a right axial straight-through light path communicated to the reaction cavity;
The gas-solid sample pipeline (4) is horizontally arranged above the heating furnace, the left end of the gas-solid sample pipeline is fixedly connected with the large diameter end of the reducing straight-through clamping sleeve joint (1), and the right end of the gas-solid sample pipeline is connected with the upper end of the gas-solid sample inlet pipeline (42) in a penetrating way through the right-angle clamping sleeve joint (3);
the solid storage device (5) is vertically arranged above the gas-solid sample pipeline (4), a cylindrical storage cavity (44) is formed in the solid storage device, a storage cavity cover (6) is assembled at the upper end of the solid storage device, and a discharge hole at the lower end of the solid storage device is connected with the middle part of the gas-solid sample pipeline (4) in a penetrating manner through a vertically arranged sample pipe branch (45); a through hole is formed in the center of the storage cavity cover (6); the middle part of the sample tube branch (45) is connected in series with a spherical valve (2);
the feeding mechanism is arranged in the storage cavity (44) and consists of a feeding thimble (7), a jacking head (35), a second sealing ring (37) and a first sealing ring (36), and the upper end of the feeding thimble (7) penetrates out to the upper part of the storage cavity cover (6) through a through hole; the ejection head (35) is longitudinally and slidably arranged in the storage cavity (44) and is arranged at the lower end of the feeding thimble (7); the second sealing ring (37) and the first sealing ring (36) are fixedly sleeved on the outer side of the lower portion of the feeding thimble (7) at intervals up and down, and the outer ring surfaces are matched with the inner surface of the storage cavity (44) in a sliding sealing mode.
2. The high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis according to claim 1, further comprising a first inner flange (18), a second inner flange (12), a first light-passing pipeline (29) and a second light-passing pipeline (30);
the first inner flange (18) is fixedly connected to the outer part of the left end of the first window pipeline (46), a first groove (23) is formed in the center of the joint surface of the first inner flange, a first sealing ring is assembled in the first groove (23), and the inner ring surface of the first sealing ring is in sealing connection with the outer circular surface of the left end of the first glass column (21); the second inner flange (12) is fixedly connected to the outer part of the right end of the second window pipeline (47), a second groove (26) is formed in the center of the joint surface of the second inner flange, a second sealing ring is assembled in the second groove (26), and the inner ring surface of the second sealing ring is in sealing connection with the outer circular surface of the right end of the second glass column (22);
the outside of the right end of the first light transmission pipeline (29) is fixedly connected with a first outer flange (19), the center of the joint surface of the first outer flange (19) is provided with a first annular groove (24), the inner circular surface of the first outer flange is provided with a second annular groove (25), and a first sealing ring and a second sealing ring are respectively assembled in the first annular groove (24) and the second annular groove (25); the first light transmission pipeline (29) is coaxially arranged at the left side of the first window pipeline (46), the first outer side flange (19) is fixedly connected with the first inner side flange (18), the first sealing ring is connected with the first sealing ring in a fitting way, and the second sealing ring is in sealing connection with the outer circular surface of the left end of the first glass column (21) extending into the first outer side flange (19);
The outside of the left end of the second light-passing pipeline (30) is fixedly connected with a second outside flange (11), the center of the joint surface of the second outside flange (11) is provided with a third annular groove (27), the inner circular surface of the second outside flange is provided with a fourth annular groove (28), and a third sealing ring and a fourth sealing ring are respectively assembled in the third annular groove (27) and the fourth annular groove (28); the second light-passing pipeline (30) is coaxially arranged on the right side of the second window pipeline (47), the second outer side flange (11) is fixedly connected with the second inner side flange (12), the sealing ring III is connected with the second sealing ring in a fitting mode, and the sealing ring IV is in sealing connection with the outer circular surface extending to the right end of the second glass column (22) in the second outer side flange (11).
3. The high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis according to claim 1 or 2, further comprising a third inner flange (8), a second air outlet pipeline (31), a fourth inner flange (14) and a fourth blind flange (15), wherein the third inner flange (8) is fixedly connected to the outer part of the upper end of the first air outlet pipeline (48), a third groove (32) is formed in the center of the joint surface of the third inner flange, and a third sealing ring is assembled in the third groove (32); a third outer flange (9) is fixedly sleeved outside one end of the second air outlet pipeline (31), and the other end of the second air outlet pipeline is connected with a through valve; the third outer flange (9) is fixedly connected with the third inner flange (8), and the third sealing ring is in sealing connection with the joint surface of the third outer flange (9); the fourth inner flange (14) is fixedly sleeved outside the lower end of the solid sample discharge pipeline (43), a fourth groove (34) is formed in the center of the joint surface of the fourth inner flange, and a fourth sealing ring is assembled in the fourth groove (34); an annular groove five (33) is formed in the joint surface of the fourth blind flange (15), and a sealing ring five is assembled in the annular groove five (33); the fourth blind flange (15) is fixedly connected with the fourth inner side flange (14), and the joint surface of the fourth blind flange (15) and the fifth sealing ring are both in sealing connection with the fourth sealing ring.
4. A high temperature high pressure gas-solid two phase dynamic absorption cell apparatus for spectrum analysis according to claim 3, wherein the first half furnace body (20) and the second half furnace body (13) are fixedly connected together by stainless steel hoops sleeved outside.
5. The high-temperature high-pressure gas-solid two-phase dynamic absorption tank device for spectrum analysis according to claim 4, wherein the variable-diameter straight-through clamping sleeve joint (1) is connected with one interface of a three-way valve through a pipeline, the other two interfaces of the three-way valve are respectively connected with a vacuum pump and a high-pressure gas cylinder through pipelines, a digital display pressure gauge and a flow control valve are connected in series on the pipeline between the variable-diameter straight-through clamping sleeve joint (1) and the three-way valve, the digital display pressure gauge is used for real-time pressure change inside a gas-solid sample pipeline (4), and the flow control valve is used for controlling flow inside the gas-solid sample pipeline (4).
6. The high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis according to claim 5, wherein the lower ends of the gas cells (16) are cone structures.
7. The high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis according to claim 6, wherein the first half-furnace body (20) and the second half-furnace body (13) are both made of high-temperature resistant fiber materials; the solid storage device (5), the gas-solid sample pipeline (4) and the gas tank (16) are all made of 316 stainless steel materials; the first water cooling pipe (17) and the second water cooling pipe (10) are manufactured by copper pipe processing; the first glass column (21) and the second glass column (22) are made of JGS3 optical quartz glass.
8. The high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis according to claim 7, wherein both end surfaces of the first glass column (21) and the second glass column (22) are inclined at an angle of 1.5 ° to the vertical direction.
9. The high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis according to claim 8, wherein a tail hole (38) is radially formed at the upper end of the feeding thimble (7) in a penetrating way, and a metal rod is arranged in the tail hole (38) in a penetrating way; the heating resistance wire is connected with an external temperature control system; one end of the first water cooling pipe (17) is connected with a cold water supply source, the other end of the first water cooling pipe is connected with a cooling water recovery tank, one end of the second water cooling pipe (10) is connected with the cold water supply source, and the other end of the second water cooling pipe is connected with the cooling water recovery tank.
10. The high-temperature high-pressure gas-solid two-phase dynamic absorption cell device for spectrum analysis according to claim 9, wherein a first temperature sensor is arranged on the surface of the gas cell (16), a second temperature sensor is arranged on the inner side of the first water cooling tube (17) on the first window pipeline (46), a third temperature sensor is arranged on the inner side of the second water cooling tube (10) on the second window pipeline (47), and the first temperature sensor, the second temperature sensor and the third temperature sensor are respectively used for collecting temperature signals of the gas cell (16), the end part of the first window pipeline (46) and the end part of the second window pipeline (47).
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