CN113945479A - Thermogravimetric analysis test method based on high-temperature furnace - Google Patents

Thermogravimetric analysis test method based on high-temperature furnace Download PDF

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CN113945479A
CN113945479A CN202111121869.8A CN202111121869A CN113945479A CN 113945479 A CN113945479 A CN 113945479A CN 202111121869 A CN202111121869 A CN 202111121869A CN 113945479 A CN113945479 A CN 113945479A
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CN113945479B (en
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惠昆
闫宁
边城
关轶文
栾涛
杨燕京
李宏岩
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Xian Modern Chemistry Research Institute
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Abstract

The invention provides a thermogravimetric analysis test method based on a high-temperature furnace, which comprises the steps of mixing and preparing initial reactants, carrying out a control group test, carrying out a test group test and carrying out error correction to obtain the actual mass residual rate M of the thermogravimetric analysis test of the high-temperature furnaceRFour steps in total; the thermogravimetric analysis test method based on the high-temperature furnace calculates the actual mass residual rate M of the thermogravimetric analysis test of the high-temperature furnaceRIntroducing error correction value E by setting contrast groupCMass remaining ratio before correction M for test groupR0Error correction is carried out, so that finally obtained test data are closer to a true value, the defect that the high-temperature furnace cannot weigh reactants in real time is overcome, and the accuracy of the thermogravimetric analysis test based on the high-temperature furnace is improved.

Description

Thermogravimetric analysis test method based on high-temperature furnace
Technical Field
The invention belongs to the field of chemical reactions, relates to a chemical reaction characteristic test, and particularly relates to a thermogravimetric analysis test method based on a high-temperature furnace.
Background
In the study of the characteristics of chemical reactions, including reaction rates, kinetic parameters, etc., experimental studies are generally conducted based on a thermogravimetric analyzer. The thermogravimetric analyzer is characterized in that reactants can be weighed in real time during the chemical reaction, and the mass change conditions of the reactants at different temperatures can be obtained in one test. However, there are many limitations to the use of thermogravimetric analyzers in practical scientific research work. For example, many reactions are carried out at high temperatures exceeding the temperature at which the thermogravimetric analyzer is used, or an atmosphere containing a reducing component corrodes the thermocouple of the thermogravimetric analyzer in a high temperature environment, under which the thermogravimetric analyzer cannot be used, or at a high cost. Therefore, it is often necessary to conduct experimental studies on chemical reactions with the aid of a high-temperature furnace instead of a thermogravimetric analyzer.
The high-temperature furnace has the advantages that the equipment can reach higher temperature, the equipment cost is low, the test system has a simple structure, the operation is convenient, and the high-temperature furnace can be used in a complex atmosphere containing oxidizing components and reducing components. However, compared with the thermogravimetric analyzer, the thermogravimetric analysis test using the high temperature furnace has the following defects: firstly, when a high-temperature furnace is adopted for thermogravimetric analysis testing, because reactants cannot be weighed in real time, the error of a test result is often larger, and the accuracy of test data is reduced; secondly, when studying the chemical reaction characteristics under high temperature conditions, it is often necessary to perform experiments under a plurality of different temperature conditions to obtain the mass change of the reactants under different temperature conditions, and then describe the relationship between the temperature and the reaction characteristics. When a high-temperature furnace is used for thermogravimetric analysis testing, errors of test results are different at different reaction temperatures, so that a test method suitable for different temperatures needs to be provided.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a thermogravimetric analysis test method based on a high-temperature furnace, and solve the technical problem that the result accuracy of the thermogravimetric analysis test based on the high-temperature furnace in the prior art is low.
In order to solve the technical problems, the invention adopts the following technical scheme:
a thermogravimetric analysis test method based on a high-temperature furnace comprises the following steps:
step one, mixing to prepare an initial reactant;
step two, carrying out a control group test:
step 2.1, weighing the initial reactant in the step one to obtain the initial reactant mass M of the control group1-0Placing the weighed initial reactant of the control group in a high-temperature furnace, and raising the temperature to a preset reaction temperature T at a temperature raising rate of 5-10 ℃/min;
step 2.2, after the reaction temperature rises to the preset reaction temperature T, cooling, and weighing and obtaining the residual reaction mass M of the control group after the reaction temperature is reduced to the room temperature1；
Step three, carrying out test group tests:
step 3.1, weighing the initial reactant in the step one to obtain the initial reactant mass M of the test group2-0Placing the weighed initial reactants of the test group in a high-temperature furnace, and adopting a heating rate of 5-10 ℃/min to raise the temperature to a preset reaction temperature T;
step 3.2, after the reaction temperature is increased to the preset reaction temperature T, carrying out constant temperature thermogravimetric reaction;
and 3.3, after the constant-temperature thermogravimetric reaction is finished, cooling, and weighing and obtaining the mass M of the residual reaction mass of the test group after the reaction temperature is reduced to room temperature2；
Step four, correcting errors and obtaining the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testR：
According to formula EC＝100％－M1/M1-0Calculating the correction value of the acquisition error EC(ii) a Wherein M is1The residual reaction mass of the control group in the second step,M1-0the initial reaction mass of the control group in the second step;
according to formula MR0＝M2/M2-0Calculating and obtaining the mass residual rate M before correction of the test groupR0(ii) a Wherein M is2The remaining reaction mass, M, of the test group described in step three2-0The initial reaction mass of the test group in the second step;
obtaining an error correction value ECAnd the pre-correction mass remaining rate M of the test groupR0Then, according to the formula MR＝MR0+ECAnd calculating and obtaining the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testR。
The invention also comprises the following technical characteristics:
specifically, the initial reactant is composed of graphite and silicon dioxide, and the mass ratio of the graphite to the silicon dioxide is 1: 1.7.
Specifically, in step 2.1 and step 3.1, the preset reaction temperature T is 1400 ℃ to 1700 ℃.
Preferably, in step 2.1 and step 3.1, the temperature rise rate is 5 ℃/min.
Specifically, in step 3.2, the reaction time of the isothermal thermogravimetric reaction is tcPreferably 0.5min to 10min, in the step 3.2, the reaction time of the constant temperature thermogravimetric reaction is tcIt is 10 min.
In the thermogravimetric analysis test method based on the high-temperature furnace, the specific method for correcting the error is as follows: calculating the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testRIntroducing error correction value ECMass remaining ratio before correction M for test groupR0Error correction is carried out, and finally the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis test is obtainedR。
Specifically, in step 2.1 and step 3.1, the temperature rise process is completely the same.
Specifically, in step 2.2 and step 3.3, the cooling process is completely the same.
Compared with the prior art, the invention has the following technical effects:
the thermogravimetric analysis test method based on the high-temperature furnace calculates the actual mass residual rate M of the thermogravimetric analysis test of the high-temperature furnaceRIntroducing error correction value E by setting contrast groupCMass remaining ratio before correction M for test groupR0Error correction is carried out, so that finally obtained test data are closer to a true value, the defect that the high-temperature furnace cannot weigh reactants in real time is overcome, and the accuracy of the thermogravimetric analysis test based on the high-temperature furnace is improved.
The thermogravimetric analysis test method based on the high-temperature furnace can be suitable for different reaction temperatures, and therefore, the method has wide application prospects in chemical reaction characteristic tests.
Drawings
FIG. 1 is a schematic representation of the reaction kinetics based on thermogravimetric analysis experiments in a high temperature furnace.
FIG. 2 is a graph showing reaction kinetics curves of thermogravimetric analysis tests based on a high temperature furnace in examples 1 to 3.
The present invention will be explained in further detail with reference to examples.
Detailed Description
In the invention, when a high-temperature furnace is used for thermogravimetric analysis, the difference between the test results of a thermogravimetric analyzer and a thermogravimetric analysis test of the high-temperature furnace is found, and the specific process is as follows:
and setting a control group and a test group, wherein the control group adopts a thermogravimetric analyzer, and the test group adopts a high-temperature furnace. Reactants consisting of graphite and silica in a mass ratio of 1:1.7 were weighed and mixed.
After mixing the reactants, 50mg of the reactant was taken as a control group, 5g of the reactant was taken as a test group, and the reaction conditions were as follows: the temperature rise rate is 5 ℃/min, and the temperature is kept at 1200 ℃ for 2 minutes. After the completion of the reaction, the data were analyzed by the normalization method, and the initial reaction substance amount was defined as 100%, and the test results are shown in table 1.
TABLE 1 test results of thermogravimetric analyzer and high temperature furnace
Inter-group setup/error Mass residual rate/%)
Control group 99.50
Test group 99.20
As can be seen from table 1, there was a difference of 0.3% between the mass residual rate of the test group and the mass residual rate of the thermogravimetric analyzer of the control group, and the mass residual rate of the high temperature furnace was larger than the mass residual rate of the thermogravimetric analyzer.
After the above problems are found, we have made the following three assumptions for the reason that the test results of the high temperature furnace and the thermogravimetric analyzer are different: firstly, as the reactant layer in the high-temperature furnace is stacked too thickly, more reactant gas cannot be released in time, so that test errors are caused; second, the temperature rise rate during the test is too slow, which causes test errors.
In view of the first hypothesis mentioned above, we have performed the following analysis, based on the prior literature, in combination with the knowledge of the skilled person: in the high-temperature furnace, reactants are uniformly spread on the bottom surface of the crucible, the thickness of a reactant layer is smaller, and inert gas flows through the upper part of the reactants along the horizontal direction; in the thermogravimetric analyzer, the reactants are deposited in a crucible with a certain thickness. That is, the thickness of the reactant layer in the high temperature furnace is less than the thickness of the reactant layer in the thermogravimetric analyzer. From the above analysis, it is found that the mass loss rate of the high temperature furnace is greater than that of the thermogravimetric analyzer, and the reason for this is unlikely that the reaction gas cannot be released in time due to the excessively thick deposition of the reactant layer in the high temperature furnace, so the first assumption can be eliminated.
In view of the second hypothesis, we developed experiments to study, and the specific experimental procedures are as follows:
a control group, a test group 1 and a test group 2 were set, and reactants consisting of graphite and silica in a mass ratio of 1:1.7 were weighed and mixed.
The test conditions for the control group were as follows: 50mg of the reaction product was taken out and subjected to thermogravimetric reaction using a thermogravimetric analyzer. The thermogravimetric reaction conditions are that the heating rate is 5 ℃/min, and the constant temperature thermogravimetric reaction is carried out for 2min at 1200 ℃.
The test conditions of test group 1 were as follows: 5g of reactant is taken, and thermogravimetric reaction is carried out by adopting a high-temperature furnace. The conditions for the thermogravimetric reaction were the same as those of the control group.
Test group 2 differs from test group 1 in that the temperature increase rate was 10 ℃/min.
After the completion of the reaction, the data were analyzed by the normalization method, and the initial reaction substance amount was defined as 100%, and the test results are shown in table 2.
TABLE 2 influence of the heating rate on the Mass fraction
Setting between groups Mass residual rate/%)
Control group 99.50
Test group 1 99.20
Test group 2 99.28
As can be seen from table 2, the mass remaining rate of the test group 1 was 0.22% different from the mass loss rate of the control group, and the mass remaining rate of the test group 2 was 0.30% different from the mass loss rate of the control group. From the above analysis, it is understood that the temperature increase rate has an influence on the mass residual rate, and the larger the temperature increase rate is, the smaller the difference between the mass residual rate and the actual value is, and the closer the test result is to the actual condition.
Therefore, the experimental error of the thermogravimetric analysis of the high-temperature furnace can be reduced by increasing the temperature rise rate theoretically. In fact, however, it is difficult to reduce the experimental error of the thermogravimetric analysis of the high temperature furnace by increasing the temperature rise rate, because the temperature rise rate of the high temperature furnace is limited, generally not exceeding 10 ℃/min, and the temperature rise rate must be kept at a low level as the temperature rises.
Based on the above experimental results, we performed the following analysis, as shown in fig. 1:
when the temperature exceeds 1200 ℃, graphite and SiO2The carbothermic reduction reaction of the mixed reactants was started, and the temperature at which the carbothermic reduction reaction started to proceed was defined as the actual reaction temperature T1The time point at which the carbothermic reduction reaction starts is recorded as the actual reaction start time t1(ii) a In the process of constant-temperature thermogravimetric reaction, the target reaction temperature T0Often more than 1200 deg.C, the point in time when the temperature begins to rise is recorded as the time-starting time t0The time point at which the temperature starts to decrease is referred to as the timer end time t0-1The time point at which the carbothermic reduction reaction was completed is recorded as the actual reaction completion time t1-1。
At about 1200 deg.C, graphite and SiO2Already starting to generate carbothermic reduction reaction, raising the temperature to the target reaction temperature T at 1200 DEG C0In the time period of (2), graphite and SiO2The mass loss rate due to carbothermic reduction will be calculated in the mass residual rate, similarly from the target reaction temperature T0Reducing the temperature to 1200 ℃ in a cooling time period, and carrying out a carbothermic reduction reactionThe resulting mass loss rate will also be calculated in the mass residual rate. Therefore, the quality residual rate obtained by the final calculation is reduced compared with the actual value.
Based on the above tests and analysis, as shown in fig. 2, the invention provides a thermogravimetric analysis test method based on a high temperature furnace, which comprises the steps of mixing and preparing initial reactants, carrying out a control group test, carrying out a test group test and error correction, and obtaining the actual mass residual rate M of the thermogravimetric analysis test of the high temperature furnaceRFour steps in total; calculating the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testRThen, error correction value E is introduced by setting a comparison groupCMass remaining ratio before correction M for test groupR0Error correction is carried out, and finally the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis test is obtainedRAnd the accuracy of the experimental result of the thermogravimetric analysis test based on the high-temperature furnace is improved.
In the invention:
error correction value ECAt the temperature rise time tU1And a cooling time tD1In the time period of (1), i.e. at the temperature rise time tU2And a cooling time tD2The rate of mass loss due to carbothermic reduction reaction during the period of time (2).
The high temperature furnace is a high temperature furnace known in the art.
The thermogravimetric analyzer employs a thermogravimetric analyzer known in the art.
The present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention fall within the protection scope of the present invention.
Example 1:
the embodiment provides a thermogravimetric analysis test method based on a high-temperature furnace, which comprises the following steps:
step one, mixing to prepare an initial reactant; the initial reactants consisted of graphite and silica in a mass ratio of 1: 1.7.
Step two, carrying out a control group test:
step 2.1, weighing the initial reactant in the step one to obtain the initial reactant mass M of the control group1-0，M1-05g, the initial reactant of the control group weighed out was placed in a high temperature furnace, and the temperature was raised to 1400 ℃ at a rate of 10 ℃/min. In this example, the time required for the reaction temperature to rise was referred to as the temperature rise time tU1。
Step 2.2, after the reaction temperature rises to 1400 ℃, cooling, and weighing and obtaining the residual reaction mass M of the control group after the reaction temperature is reduced to room temperature1，M14.945 g. In this example, the time required for the reaction temperature to decrease is recorded as the temperature decrease time tD1。
Step three, carrying out test group tests:
step 3.1, weighing the initial reactant in the step one to obtain the initial reactant mass M of the test group2-0，M2-0The initial reactants of the test group weighed to be 5g are placed in a high temperature furnace, and the reaction temperature is increased to 1400 ℃ by adopting the temperature rising rate of 5 ℃/min. In this example, the time required for the reaction temperature to rise was referred to as the temperature rise time tU2。
Step 3.2, carrying out constant temperature thermogravimetric reaction at the reaction temperature of 1400 ℃, wherein the reaction time of the constant temperature thermogravimetric reaction is tcIt is 10 min. In this embodiment, the protective atmosphere for the isothermal thermogravimetric reaction is an argon atmosphere.
And 3.3, after the constant-temperature thermogravimetric reaction is finished, cooling, and weighing and obtaining the mass M of the residual reaction mass of the test group after the reaction temperature is reduced to room temperature2，M24.835 g; in this example, the time required for the reaction temperature to decrease is recorded as the temperature decrease time tD2。
In this embodiment, the temperature raising process in step 2.1 is completely the same as that in step 3.1, and the temperature lowering process in step 2.2 is completely the same as that in step 3.3, so that the test error caused by the difference in the temperature raising and lowering processes between the control group and the test group can be eliminated.
Step four, obtaining the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testR：
According to formula EC＝100％－M1/M1-0Calculating the correction value of the acquisition error EC(ii) a The calculation results are shown in table 3. According to formula MR0＝M2/M2-0Calculating and obtaining the mass residual rate M before correction of the test groupR0The calculation results are shown in table 3. Obtaining the mass residual rate M before correction of the test groupR0And error correction value ECThen, according to the formula MR＝MR0+ECAnd calculating and obtaining the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testRThe calculation results are shown in table 3.
Example 2:
the embodiment provides a thermogravimetric analysis test method based on a high-temperature furnace, which comprises the following steps:
in this embodiment, the first step is the same as the first step of embodiment 1.
In this example, step two was substantially the same as step two of example 1, except that the reaction temperature was 1600 ℃ and the residual reactant mass M in the control group was1It was 4.825 g.
In this example, step three was substantially the same as step three of example 1, except that the reaction temperature was 1600 ℃ and the remaining reactant mass M in the test group was23.730 g.
In this example, step four was the same as step four in example 1, and the calculation results are shown in table 3.
Example 3:
the embodiment provides a thermogravimetric analysis test method based on a high-temperature furnace, which comprises the following steps:
in this embodiment, the first step is the same as the first step of embodiment 1.
In this example, step two was substantially the same as step two of example 1, except that the reaction temperature was 1700 ℃ and the residual reactant mass M in the control group was1It was 4.740 g.
In this example, step three was substantially the same as step three of example 1, except that the reaction temperature was 1700 ℃, and the remaining reaction mass of the test groupM2It was 2.475 g.
In this example, step four was the same as step four in example 1, and the calculation results are shown in table 3.
TABLE 3 actual mass residual ratio M of the high-temperature furnace thermogravimetric analysis test of examples 1 to 3R
Data type/embodiment Example 1 Example 2 Example 3
Mass remaining rate M before correctionR0/％ 96.7 74.6 49.5
Error correction value EC/％ 1.1 3.5 5.2
Actual mass remaining rate MR/％ 97.8 78.1 54.7
From examples 1 to 3, it is clear that in examples 1, 2 and 3, the isothermal thermogravimetric reaction is performedThe reaction temperature is 1400 ℃, 1600 ℃ and 1600 ℃ respectively, and the error correction value EC1.1%, 3.5% and 5.2%, respectively. From the above data, it can be seen that the higher the reaction temperature is, the error correction value ECThe larger the test error, i.e., the greater the thermogravimetric analysis test performed by the high temperature furnace.
The method calculates the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testRThen, error correction value E is introduced by setting a comparison groupCMass remaining ratio before correction M for test groupR0Error correction is carried out, and finally the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis test is obtainedRThe method is closer to an actual value, improves the accuracy of the thermogravimetric analysis test of the high-temperature furnace, is suitable for different reaction temperatures, and has wide application prospect in the chemical reaction characteristic test.

Claims (7)

1. A thermogravimetric analysis test method based on a high-temperature furnace comprises the following steps:
step one, mixing to prepare an initial reactant;
the method is characterized in that:
step two, carrying out a control group test:
step 2.1, weighing the initial reactant in the step one to obtain the initial reactant mass M of the control group1-0Placing the weighed initial reactant of the control group in a high-temperature furnace, and raising the temperature to a preset reaction temperature T at a temperature raising rate of 5-10 ℃/min;
step 2.2, after the reaction temperature rises to the preset reaction temperature T, cooling, and weighing and obtaining the residual reaction mass M of the control group after the reaction temperature is reduced to the room temperature1；
Step three, carrying out test group tests:
step 3.1, weighing the initial reactant in the step one to obtain the initial reactant mass M of the test group2-0Placing the weighed initial reactants of the test group in a high-temperature furnace, and adopting a heating rate of 5-10 ℃/min to raise the temperature to a preset reaction temperature T;
step 3.2, after the reaction temperature is increased to the preset reaction temperature T, carrying out constant temperature thermogravimetric reaction;
and 3.3, after the constant-temperature thermogravimetric reaction is finished, cooling, and weighing and obtaining the mass M of the residual reaction mass of the test group after the reaction temperature is reduced to room temperature2；
Step four, correcting errors and obtaining the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testR：
According to formula EC＝100％－M1/M1-0Calculating the correction value of the acquisition error EC(ii) a Wherein M is1The residual reaction mass of the control group, M, described in step two1-0The initial reaction mass of the control group in the second step;
according to formula MR0＝M2/M2-0Calculating and obtaining the mass residual rate M before correction of the test groupR0(ii) a Wherein M is2The remaining reaction mass, M, of the test group described in step three2-0The initial reaction mass of the test group in the second step;
obtaining an error correction value ECAnd the pre-correction mass remaining rate M of the test groupR0Then, according to the formula MR＝MR0+ECAnd calculating and obtaining the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testR。
2. The thermogravimetric analysis test method based on a high temperature furnace as claimed in claim 1, wherein in step one, the initial reactants are composed of graphite and silica in a mass ratio of 1: 1.7.
3. The thermogravimetric analysis test method based on a high temperature furnace as claimed in claim 1, characterized in that in step 2.1 and step 3.1, the predetermined reaction temperature T is between 1400 ℃ and 1700 ℃.
4. The thermogravimetric analysis test method based on a high temperature furnace as claimed in claim 1, characterized in that in step 2.1 and step 3.1, the temperature rise rate is 5 ℃/min.
5. The thermogravimetric analysis test method based on a high temperature furnace as claimed in claim 1, wherein in step 3.2, the reaction time of the isothermal thermogravimetric reaction is tcIs 0.5min to 10 min.
6. The thermogravimetric analysis test method based on a high temperature furnace as claimed in claim 1, wherein in step 3.2, the reaction time of the isothermal thermogravimetric reaction is tcIt is 10 min.
7. The thermogravimetric analysis test method based on a high-temperature furnace as claimed in claim 1, wherein the specific method of error correction is as follows: calculating the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis testRIntroducing error correction value ECFor the mass remaining rate M before correctionR0Error correction is carried out, and finally the actual mass residual rate M of the high-temperature furnace thermogravimetric analysis test is obtainedR。
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