KR20160139615A - Vacuum distillation/condensation recovery type thermal behavior analysis device and method - Google Patents

Abstract

The present invention relates to a thermal behavior analysis device and a method thereof, which are capable of concurrently performing a quantitative analysis and a thermal behavior analysis on an inorganic or organic compound sample in a selective condition such as a decompression volatilization/condensation collection. The thermal behavior analysis device comprises: an upper cover flange module which includes a load cell, a pressure sensor, an insulator, an electric heater, and an atmosphere creation gas supply device; a reactor module which is divided into a volatilization region at a low portion thereof and a condensation region at an upper portion thereof, which each control a temperature; a lower cover flange module which performs a volatile material collection, a pressure adjustment, and a gas discharge; and a data collection module which senses a change in a weight of a sample and changes in a temperature and a pressure in a reactor, transfers the sensed change as an electric signal, and stores the sensed changes as data.

Description

FIELD OF THE INVENTION [0001] The present invention relates to an apparatus for analyzing volatile / condensate recovery type thermal behavior,

The present invention relates to an apparatus and a method for analyzing thermal behavior of a sample in a reactor by physical volatilization, chemical reaction, and decomposition reaction, and more particularly, to an apparatus for analyzing thermal behavior of a sample in an open system and a closed system, And the apparatus and method for analyzing the sample.

The distillation method is considered to be one of methods for obtaining a very high efficiency while purifying or separating a compound containing an organic or inorganic substance which can be volatilized. In order to purify or separate high-purity compounds by distillation, it is necessary to analyze the thermal behavior of the material. Thermo-Gravimetric Analyzer (TGA) is widely used to analyze the thermal behavior have.

Generally, thermogravimetric analyzer is a device that measures the change in mass of a sample as a function of time or temperature by applying a temperature program to the analysis sample. The change in mass is a volatile or chemical reaction that generates a volatile substance or a gaseous substance of the sample, It is generated by decomposition reaction. Considering the characteristics of the material and the operating conditions of the TGA, an acid gas atmosphere such as oxygen or air or an inert gas atmosphere such as nitrogen or argon may be formed to realize the volatilization or chemical reaction conditions of the sample.

Recently, the use of thermogravimetric analyzer which can observe thermogravimetry under various pressure conditions has been increasing. Particularly, in the case of a sample sensitive to moisture or oxygen, development of analyzer capable of measuring thermogravimetry under vacuum (decompression) condition Is also increasing.

For example, Korean Patent No. 10-1116364 discloses a method of loading a sample into a reactor body having a uniform temperature distribution so that condensation of the sample does not occur under a reduced pressure operating condition of the closed system, A device designed to enable precise weight analysis by minimizing weight error has been disclosed.

However, since most thermogravimetric analyzers currently in use are designed to operate only in a closed system, there are limitations in providing various analysis conditions and methods depending on the samples. From the analysis results of the samples, operating conditions Is difficult to secure.

In addition, commercial thermogravimetric analyzers are optimized only for the mass change detection of vapor phase materials generated by volatilization, chemical reaction or pyrolysis, and provide data for analyzing changes in temperature and pressure due to volatilization and condensation in the reactor There is a problem that can not be done. Therefore, it is required to develop an analyzer capable of simultaneously establishing process conditions for high purity purification and separation of organic or inorganic compounds and analyzing the condensation behavior of gaseous substances.

Korean Patent Publication No. 10-2010-0121937 Korean Patent Publication No. 10-2011-0018511

"Recovery of Residual LiCl-KCl Eutetic Salts in Radioactive Rare Earth Precipitates", J. of The Korean Radioactive Waste Society, Vol 8 (4). P. 303-309, Dec. 2010

It is an object of the present invention to improve the limited analysis method of the thermogravimetric analyzer as described above to enable the analysis of the condensation characteristics of the gaseous material discharged from the volatilization of the sample and to purify the compound containing the volatile organic or inorganic substance Or separation or separation of a selective component in separation.

It is a further object of the present invention to provide a method and apparatus for reducing the volatility of a substance that is volatilized under atmospheric pressure or reduced pressure by setting the reduced pressure volatilization step and the condensation recovery step in an selective recovery method based on the volatilization rate and recovery state of the sample, And a method of connecting the peripheral devices.

It is still another object of the present invention to provide a process for purifying and separating high purity inorganic or organic compounds, which enables to purify and separate the samples in high purity, thereby improving industrial processes and reducing industrial wastes And to provide a method of analyzing a sample that can be imported.

The thermal behavior analysis apparatus capable of simultaneously analyzing the thermal behavior of the reduced pressure volatilization and the condensation recovery of the present invention includes an upper cover flange module composed of a load cell, a pressure sensor, a heat insulating material, an electric heater, A lower cover flange module for performing a volumetric recovery, a pressure regulating and a gas discharge, and a temperature sensor for detecting temperature, pressure and weight change of the sample from the reactor main body, And then stores the data as data.

The thermal behavior analysis method of the present invention can accurately measure volatilization, pyrolysis rate and thermal behavior by measuring the weight loss due to volatilization or thermal decomposition of an inorganic or organic sample material according to pressure and temperature in real time, Provides condensation behavior data for the volatilized material.

The present invention relates to a method for analyzing the volatility and condensation characteristics of a sample by integrating the step of analyzing the volatilization and condensation characteristics of the sample and the collecting step of the recovered sample by providing a decompression volatilization / condensation recovery type thermal behavior analyzing apparatus, thereby complicating the multistage purification and separation / recovery process of organic or inorganic compounds having similar chemical characteristics Can be simplified. In addition, by analyzing the real-time thermal behavior of the sample, it is possible to reduce the test cost and time required for the design / manufacture of the process equipment by establishing optimized purification and separation / recovery process conditions and increasing the purity and recovery rate of the sample.

The above-described thermal behavior analyzer and analysis method facilitates remote control and monitoring of the high-temperature type reactor, thereby enhancing the productivity of the process using the high-temperature type reactor. More specifically, in a spent nuclear fuel pyrolysis process for recovering a nuclear fuel material for a fourth generation reactor, separation and recovery of the radioactive rare-earth precipitate and the eutectic salt are facilitated. In addition, electrolytic eutectic salts discharged from dyestrate carbonate fuel cells and direct carbon fuel cells can be easily reused through purification and component separation, thereby reducing the amount of industrial waste and increasing the recovery rate. Thus, it is expected that the environment-friendly industrial environment can be established and the energy production cost can be lowered .

On the other hand, in the conventional molten salt recovery method, there is a problem that the sample residue and the container are difficult to be desorbed, and the cooling manifold is placed at the bottom of the recovery vessel in consideration of the difficulty of reusing the vessel. Thus, the quenched recovered sample provides an economical advantage in that it is easy to remove from the recovery container and the container can be reused.

FIG. 1 is a schematic view of an apparatus for recovering chloride in a eutectic salt according to a first embodiment of the present invention
2 to 4 are process charts sequentially showing a process for decompression / condensation recovery of one or its chlorides from a eutectic salt sample according to the present invention
5 is a graph showing the relationship between temperature and pressure data when operating without a eutectic salt as a sample in the LiCl-KCl waste eutectic salt recovery system according to the present invention
6 is a graph showing the relationship between temperature and pressure data (about 2 kg of sample) during operation of the sample in the LiCl-KCl waste eutectic salt recovery system according to the present invention,
FIG. 7 is a graph showing the morphology of NdCl ₃ separated in LiCl-KCl-NdCl ₃ eutectic salt samples according to the present invention by X-ray diffraction analysis

Hereinafter, the present invention will be described with reference to the accompanying drawings.

The present invention relates to an upper cover flange module composed of a load cell, a pressure sensor, a heat insulating material, an electric heater, an atmospheric composition or a reaction gas device, and a reactor capable of temperature control by being divided into a volatile region and a condensation region, Module including a lower cover flange module for performing volumetric recovery, pressure regulation and gas discharge, and a data collection module capable of real time monitoring and data storage after detecting temperature, pressure, weight change of sample, The present invention relates to a thermal behavior analyzing apparatus, and provides an apparatus and a method capable of simultaneously analyzing the thermal behavior of volatilization and condensation / recovery.

1, the load cell 104 and the pressure sensor 103 connected to the reaction sample vessel inside the reactor body are connected to the gas injection section 101 through the atmosphere injection device 101, And is connected through a flow meter 102 for injecting a gas. The upper cover flange module 100 is configured such that the load cell 104 and the reaction sample container are connected to each other through a lead wire and charged into the reactor body.

The upper cover flange module 100 includes an O-ring 105 which is a sealing member for securing the airtightness between the reactor body and the cover flange. To protect the O-ring 105, And is configured to circulate through the embedded top cooling manifold 110.

The cover heater 109 of the upper cover flange module 100 is configured to be located in the center of the lower surface of the upper cover flange manifold 110 and to be loaded inside the reactor module. At this time, the cover heater 109 secures the heat insulation with the outer wall of the reactor by the outer heat insulating material 108, and is installed in the hollow shape together with the inner heat insulating material 107, And a function of heating the volatile component of the reaction gas so as to prevent the volatile component from entering the reactor. The cover heater 109 is configured to have a function of heating to maintain a temperature higher than the set temperature of the reactor main body lower heater 205 by 100 ^° C or more.

  The reactor main body 207 of the reactor module 200 which proceeds with the volatilization or decomposition reaction of the sample is charged into the reactor main body 207 through the upper cover flange and the lead wire and caused by volatilization or decomposition reaction And a ramp 208 to assist in the recovery of the sample by condensation of the gaseous material. At this time, the reactor body 207 is heated by the upper heater 204 and the lower heater 205, and the first temperature sensor 201 and the lower heater 205 at the position of the upper heater 204 for detecting the temperature of the main body, And a function of adjusting the temperature in the volatilization zone and the temperature in the condensation zone of the sample by the third temperature sensor 203 at the lower position of the lower heater 205. [

The reactor main body 207 is made of quartz having high heat resistance and corrosion resistance, and a heat-resistant ceramic or nickel-based alloy such as alumina, magnesia, or zirconia. The reactor body 207 is thermally and chemically stable during the volatilization and condensation of the sample. .

The reactor module 200 is divided into the reactor main body upper heater 204 and the lower heater 205 so as to individually control the temperature according to the test temperature set value in the reactor. By the volatilization and condensation, And is configured to form a vertical temperature gradient to provide a temperature differential to such an extent that separation is possible. More specifically, to separate NdCl ₃ and LiCl-KCl from eutectic mixed salts such as LiCl-KCl-NdCl ₃ , at a pressure of 0.5 Torr, the temperature of the upper heater region is 750 ^° C to 850 ^° C And the temperature of the lower heater region is set at 610 ^° C to 700 ^° C. At this time, the temperature of the condensed sample in the upper part of the recovery vessel is set to 500 ^° C to 590 ^° C, and the refrigerant of the cooling manifold is circulated so that the temperature of the bottom of the recovery vessel is 50 ° C or less. At this time, the thermal behavior of the sample is accurately detected through the first temperature sensor 201, the second temperature sensor 201, and the third temperature sensor 203.

The volatile material recovery container 301 according to the volatilization and condensation of the sample in the reactor module 200 is configured to be positioned on the upper surface of the buried cooling manifold 302 in the lower cover flange for rapid cooling of the condensate recovery type sample And the recovered sample is a gas, a gas collector 310 used is connected to the first valve 308 and the third valve 308 of the valves 306, 307 and 308 of FIG. 1 connected to perform the gas discharge and the reduced pressure in the reactor body 207. [ (307). At this time, the pressure inside the reactor main body 207 is easily controlled by positioning the minute flow rate control valve 311 at the upper end of the decompressor 312 for controlling the pressure of the reactor main body 207. The sample collection container 301 is made of heat-resistant and corrosion-resistant quartz, heat-resistant ceramics such as alumina or zirconia, or a metal container made of SUS or nickel alloy.

The gas collection vessel 310 naejineun metal oxides _{(SiO 2, Al 2 O 3} , CaO, Fe 2 O 3, MgO, Na 2 O) as a column, the adsorbent according to the physical / chemical properties of the volatile substance for trapping the zeolite or And activated carbon.

The data acquisition module 400 of FIG. 1 includes a fourth temperature sensor 304 for detecting the temperature inside the reactor body and the bottom surface of the recovery vessel 301, a first temperature sensor 201 for each position of the reactor body, The PLC control device 401 including the second temperature sensor 202 and the third temperature sensor 203 for measuring the temperature and converting it into an electric signal, and the data collecting device 402, . Here, the programmable logic controller (PLC) is composed of a CPU module, a programmable software and a communication module to automatically control the device.

As described above, the decompression volatilization / condensation recovery type thermal behavior analyzing apparatus of the present invention can set the operation conditions inside the reactor main body 207 through the PLC control device 401, and can control the weight of the sample Change and change of temperature and pressure value in real time.

The thermal behavior analyzing apparatus of the present invention is a method for analyzing volatilization and condensation behavior, which maximizes the sample recovery rate depending on the operating conditions (volatile region atmosphere in the reactor module) and the state immediately before the volatilization of the material (solid and liquid or gas) The temperature inside the reactor body is set.

The test analysis process through the reactor includes a first step of setting the operating conditions of the sample and a second step of charging the sample and observing the volatilization and condensation characteristics of the sample under the operating conditions and the second step of monitoring the volatile residue and the collected sample And a third step of retrieving the data.

In the first step, the temperature program and the operation gas atmosphere are set in the same manner as in the conventional thermal behavior analyzer. In the present invention, not only the temperature control setting of the upper heater 204 in the volatile region, 205 were set separately so that a temperature gradient could be artificially applied to the reactor. It is set so that the recovery method according to the state of the separated and purified sample immediately before the collection can be easily set using the process of FIG. Also, in order to prevent the gaseous material from flowing back into the upper portion where the load cell 104 is located according to the temperature gradient in the reactor during the sample analysis, the temperature of the electric heater provided in the upper cover is set to 100 ^° C High. When the temperature setting step is completed, the operating pressure for setting the decompression condition is set, and the valve is adjusted to have the flow of the selected sample according to the state just before the volatilized material is collected.

In the second step, the sensitivity of detection of changes in weight when the sample is loaded can be varied depending on the capacity of the reactor and the load cell, and the material of the reaction sample container 206 in the sample mounting part is selected depending on the chemical characteristics of the sample. The resolution of the load cell 104 has a value of ± 0.02 to 0.05% which can be set to a value between 0.02 and 2 mV / kgf as the output voltage for the drive voltage applied to the load cell, Therefore, the load cell which can measure the weight of various sections between ^10-4 mg and several kg is selected and replaced.

After charging the sample in the second step, the composition of the reaction gas in the reactor is set by injecting an oxidizing gas or an inert gas, and the valve is adjusted according to the temperature control process, the reaction of the recovered sample, and the sampling method .

The cooling water is circulated in the upper / lower cover flange after completing the pressure regulation in the second step and performing the temperature regulation process, or the air cooling type cooling method using the refrigerant gas circulation. The purpose of circulating the refrigerant in the upper cover flange is to protect the O-ring 105 to maintain airtightness. The reason for circulating the refrigerant in the lower cover flange is to protect the O-ring, So that it can be easily separated from the water.

In the second step, the volatilization and condensation behavior of the sample are observed by observing the changes in pressure and temperature during the reaction as the inside of the reactor reaches the set temperature condition. At this time, observation of the temperature change in the lower region of the reactor module is performed in the data collection module 400 and is performed through the PLC control device 401 and the data collection device 402 which are devices for controlling various kinds of machines or programs. When the condensation of the volatilized material proceeds, the temperature of the condensation region is increased by radiating heat to the surrounding region. When the condensation and the thermal termination are terminated, the temperature of the condensation region is recovered to a certain temperature, The condensation or the emission of the temperature is terminated.

The data on temperature and pressure changes in the second stage can be monitored or stored through a computer-based program like the existing thermal behavior analyzer. At this time, the volatilization and condensation behavior of the sample according to the pressure are analyzed using the temperature data for the volatile region and the condensation region.

After the end of the experiment in the third step, the remaining samples in the sample container are recovered as in the existing thermal behavior analyzer, and at the same time, the volatiles collected in the condensation region are recovered.

In the third step, the recovery of volatiles is performed in a recovery vessel placed above the lower cover flange in the case of recovering liquid or solid phase. When the type immediately before the capture is in the gas phase, the pipeline is connected to the side of the lower region of the reactor module, The volatiles are recovered from the gas collecting container 310 that collects the material. At this time, the recovery container 301 positioned above the lower cover flange 303 has high temperature heat resistance and corrosion resistance according to the physical / chemical characteristics of the condensed material. Specifically, it is made of a heat-resistant ceramic material such as quartz or alumina or zirconia designed to meet the sample weight and volume, or is a metal material having high temperature corrosion resistance such as a nickel-based metal.

The recovery vessel for collecting the gaseous material in the third step can be selected variously according to the physical / chemical characteristics of the volatile substance. Column the adsorbent for gas collection are to be capable of use in a variety of physical / chemical adsorption conditions, as an adsorbent, such as a metal oxide and a zeolite or activated carbon, such as _{SiO 2, Al 2 O 3,} CaO, Fe 2 O 3, MgO, Na 2 O Charge.

2A and 2B are process diagrams for understanding the method of analyzing the thermal behavior of the sample according to the number of reduced-pressure volatilization / condensation of the present invention. First, as shown in FIGS. 2A to 2C, analysis is possible through three sample analysis methods. That is, it is possible to obtain a liquid or solid recovery sample by two methods in a closed system and an open system, and a method for obtaining a gas recovery sample.

The closed test method and the open test method for liquid / solid recovery sampling are described below with reference to FIG. 2B as follows.

The closed test method of the liquid / solid recovery sample is as follows. First, after the load cell 104 is adjusted to zero, the sample is connected to the reaction sample container 206 by a lead wire having a high temperature resistant resistance such as a load cell and a nickel wire or a platinum wire or a molybdenum wire I will. Then, the process of charging the upper cover flange module 100 into the reactor main body is performed in P1 and P2 of FIG. 2A.

The second valve 306 of the lower cover flange module 300 is opened and the first valve 308 and the third valve 307 are closed. The process P3 is a process of setting the gas composition, pressure, and temperature in advance in the PLC control device 401 and the data collection device 402. Thereafter, the analysis process includes a step P4 'in which the heaters 109, 204, and 205 in the reactor and the decompression device 312 are operated, and a step in which the reaction gas is introduced into the reactor body 207 connected to the upper cover flange To the P5 process. At this time, in order to protect the decompression device 312, the filter 305 is disposed at the upper end of the decompression device 312. In the next step, the sample is subjected to a P5 'process to confirm that the temperature condition before the reaction is initiated or volatilized has been reached.

P6 'In the process below, the second valve 306 is closed to form a closed system after reducing the pressure to the minimum set pressure while injecting the atmospheric composition gas. Next, the P8 process of observing the change in weight and thermal behavior of the sample and collecting the data and the P9 process of cooling the temperature of the reactor main body to room temperature after confirming the completion of the test are opened to open the upper and lower cover flanges at P10, do. At this time, the heater used is controlled by a constant temperature raising rate of 1500 ^o It is preferable to manufacture the heater according to the density and the capacity of the heating element so that the heating can be performed at C or lower.

Meanwhile, the open test method of the liquid / solid recovery sample is the same as the closed test method of the process before P5 'of FIG. 2B. The P6 process and the P6 process of forming the open system by operating at the set pressure and temperature by injecting gas into the reactor main body The process proceeds to P9 where the weight change and the thermal behavior of the sample are observed and the data is collected. After confirming the end of the test from the output of the data collection device 402, the gas injection is stopped and the temperature of the reactor body 207 is cooled to room temperature. In step P10, the upper and lower cover flanges are opened to remove the sample. At this time, the recovery container 301 positioned above the lower cover flange 303 has high temperature heat resistance and corrosion resistance according to the physical / chemical characteristics of the condensed material. Specifically, it is made of a heat-resistant ceramic material such as quartz, alumina or zirconia designed to meet the sample weight and volume, or a metallic container made of SUS or nickel alloy.

In Fig. 2c, an open test procedure for recovering a gaseous sample is described. The second valve 306 of the lower cover flange module 300 is closed and the first valve 308 and the third valve 307 are opened to regulate the valve so as to pass the adsorption column material filled in the gas collecting container 310 do. In step P3, the composition, pressure, and temperature of the gas are preset in the PLC control device 401 and the data collection device 402. Next, in a process P4, the cover heater 109, the upper heater 204 and the lower heater 205 are operated. At P5, the reaction gas is supplied into the reactor body 207 connected to the upper cover flange 106 in a predetermined gas composition Lt; / RTI > Thereafter, the operating pressure is set. At P7 in FIG. 2C, the gas collecting container and the operating conditions are set, and at P8, the data is collected at the same time as the change in the weight of the sample and the observation of the change in the thermal behavior. After confirming the end of the experiment, gas injection is stopped, and the temperature of the reactor main body is cooled to room temperature in the process of P9. Thereafter, the test is terminated at P10, which is a process of opening the upper and lower cover flanges and taking out the collected sample in the gas collecting container 310. [

EXAMPLES Reactor operating condition confirmation test by analysis of thermal behavior of the eutectic salt of LiCl-KCl according to the present invention

For the analysis of 2 kg of LiCl-KCl waste eutectic salt, blank test without specimen was carried out using a reduced pressure volatilization / condensation recovery type thermal behavior analyzer and set at the volatilization temperature and pressure of the component to be separated in the reactor main body Fig. 3 shows the result of observing the post-change. In FIG. 3 (a), the result of the operation of the upper heater can be confirmed so that the volatilization temperature occurring around the upper heater in the reactor body is maintained at a constant temperature of about 900 ^° C or less. This is the volatilization temperature of the component to be separated in the eutectic salt in the reactor body before measurement of the analytical sample, and (b) is the measurement of the pressure inside the reactor body at this time. In contrast, in FIG. 4, about 2 kg of the eutectic salt sample is actually mounted, and the temperature of the first temperature sensor 201, which is a volatilization region where volatilization of the sample mainly occurs in the reactor main body, is maintained at a constant temperature of about 900 ^° C So that the temperature and the output value of the upper heater were set and operated. At this time, the temperature of the cover heater 109 charged in the reactor main body was maintained at 900 ^o C or higher. 4 (a) is a measured value of the heater temperature at the position of the first temperature sensor 201 where the sample is volatilized in the reactor body, and the data measured value of the first temperature sensor 201 in the volatile region is (B) of Fig. The temperature of the lower heater is set to a predetermined temperature of 800 ^° C or more so that the volatilized sample is condensed after the volatilization by pyrolysis of the sample, and then the output value of the second temperature sensor 202 in the condensing region is shown in (c ). At this time, the measured pressure change inside the reactor body is shown in (d) of FIG.

4, the pressure in the reactor increases as the salt as the sample evaporates in the volatile region from the point (e) at which the valve is closed after the depressurization to the point (f) until the set temperature of the upper and lower heaters, And (g) region where the condensation starts, the temperature and pressure gradually increase due to the endothermic reaction. The volatilized salt in the volatilization region decreases and the volatilized salt in the condensation region begins to condense, and the pressure gradually decreases and the temperature again shows a behavior increasing. As a final step, it was confirmed that the temperature and pressure were kept constant after the evaporation of the salt was terminated in the region (g). The results showed that the time required for volatilizing and separating the 2 kg LiCl-KCl waste eutectic salt was about 2 hours in the (g) region of 2.7 hours, It was possible to secure an optimum operating condition for maximizing the recovery rate of the treated sample according to the change in temperature and pressure behavior inside the reactor body.

<Example> separation of my NdCl ₃ LiCl-KCl-NdCl ₃ eutectic salt LiCl-KCl according to the invention and restoration test

FIG. 5 shows the XRD results of the residual samples recovered after analysis of the reduced pressure volatilization / condensation recovery type of LiCl-KCl-NdCl ₃ eutectic salt samples. As shown in the XRD analysis results, the residual eutectic salt in the sample vessel was confirmed to have NdCl ₃ crystals in both the 750 ^o C and 850 ^o C volatilization zone temperature setting tests. In the test of the sample as described above, the pressure of the reactor main body was fixed at 0.5 Torr and the temperature of the volatilization zone of the reactor main body was varied to quantitatively analyze the recovered sample. As a result, the NdCl ₃ separation rate was measured. Respectively. As shown in Table 1 below, 750 The high separation efficiency of NdCl ₃ of 96.1 ~ 99.5% at the temperature of ^o C or higher was obtained. It can be confirmed that the operating conditions for increasing the recovery rate according to the condensation characteristics of the volatilized LiCl-KCl eutectic salt can be set in FIG.

Recovery embodiment according to at reduced pressure (0.5 Torr) from a LiCl-KCl-NdCl ₃ molten salt at a temperature of NdCl ₃ Temperature ( ^o C) 750 800 850 Separation rate (%) 99.5 99.2 96.1

It will be understood by those skilled in the art that the foregoing description of the present invention is for illustrative purposes only and that those of ordinary skill in the art can readily understand that various changes and modifications may be made without departing from the spirit or essential characteristics of the present invention. will be. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.

100: upper cover flange module 300: lower cover flange module
101: gas injection part 301: recovery container
102: Flow meter 302: Lower cooling manifold
103: Pressure sensor 303: Lower cover flange
104: load cell 304: fourth temperature sensor
105: Top O-ring 305: Filter
106: upper cover flange 306: second valve
107, 108: Insulating material 307: Third valve
109: Cover heater 308: First valve
110: upper cooling manifold 309: lower O-ring
200: reactor module 310: gas collection container
201: first temperature sensor 311: micro flow rate control valve
202: second temperature sensor 312: decompression device
203: third temperature sensor 400: data acquisition module
204: upper heater 401: PLC control device
205: lower heater 402: data collecting device
206: Reaction sample vessel
207: reactor body
208: ramp

Claims (10)

In the thermal behavior analysis method,
A first step of setting an operation condition of the sample;
A second step of observing the volatilization and condensation characteristics of the sample; And
A third step of recovering the volatile residue and the collected sample after completion of the reaction;
/ RTI &gt; The method according to claim 1,
In the first step,
Opening the second valve (306) of the lower cover flange module (300);
Closing the first valve (308) and the third valve (307) to operate the decompression device (312); And
Stopping the gas injection and closing the second valve (306) to form a closed system; A foil
And a method of recovering a sample in a liquid state and a solid state
Wherein the thermal behavior analysis method comprises: The method according to claim 1,
The first step includes opening a second valve 306 of the lower cover flange module 300;
Closing the first valve (308) and the third valve (307) to operate the decompression device (312); And
Gas is injected into the reactor body and controlled to have a set pressure,
;
And a method of recovering liquid and solid samples containing
A method of analyzing thermal behavior as a gating.
The method according to claim 1,
In the first step, the second valve (306) of the lower cover flange module (300) is closed and the first
Opening the valve 308 and the third valve 307;
And setting a gas collecting container operating condition.
Wherein the method comprises the steps of:
A thermal behavior analyzer comprising an upper cover flange module (100), a reactor module (200), a lower cover flange module (300), and a data acquisition module (400)
The upper cover flange module 100 includes a load cell 104 capable of internal pressure measurement of the reactor body 207 and gas injection and replaceable,
The reactor module 200 includes an upper heater 204 and a lower heater 205 forming a vertical warm tool boat inside the reactor body 207 charging the sample and a ramp 208 formed to allow recovery of the condensed sample, Lt; / RTI &gt;
The lower cover flange module 300 includes a recovery vessel 301 of a condensed sample and a decompression device 312 connected to a valve that controls opening and closing so as to form a closed or open system of the reactor body,
Characterized in that the data acquisition module (400) comprises a PLC control device (401) for controlling the reactor body (207) and a data acquisition device (402).
The upper cover flange module (100) according to claim 5, further comprising a gas injection part (101), a pressure sensor (103) and a flow meter (102) Is connected to the thermal analyzer.
6. The apparatus according to claim 5, wherein the lower cover flange module (300) is configured to cool the sample collection container (301) by circulating a coolant through the lower cooling manifold (302) .
6. The method of claim 5, wherein the reactor module (200) ^o C or less and a constant heating rate.
6. The thermal behavior analyzing apparatus according to claim 5, wherein the gas is supplied as an inert gas or an oxidizing gas.
6. The thermal behavior analyzer of claim 5, wherein the load cell (104) is replaceable.

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