CN111896419A - Thermal weight loss detection method and system for mixture of TESPT and carbon black and application - Google Patents
Thermal weight loss detection method and system for mixture of TESPT and carbon black and application Download PDFInfo
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- CN111896419A CN111896419A CN202010768343.8A CN202010768343A CN111896419A CN 111896419 A CN111896419 A CN 111896419A CN 202010768343 A CN202010768343 A CN 202010768343A CN 111896419 A CN111896419 A CN 111896419A
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- 239000006229 carbon black Substances 0.000 title claims abstract description 33
- 239000000203 mixture Substances 0.000 title claims abstract description 26
- 230000004580 weight loss Effects 0.000 title claims abstract description 25
- 238000001514 detection method Methods 0.000 title claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- 229920001971 elastomer Polymers 0.000 claims description 8
- 230000001360 synchronised effect Effects 0.000 claims description 8
- 238000002411 thermogravimetry Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- NELNNGOFUZQQGL-UHFFFAOYSA-N triethoxy-[1-(1-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)C(CC)SSSSC(CC)[Si](OCC)(OCC)OCC NELNNGOFUZQQGL-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- 238000004442 gravimetric analysis Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention relates to a thermal weight loss detection method, a system and application of a mixture of TESPT and carbon black, wherein the method comprises the following steps: heating a known amount of sample in nitrogen flow, wherein the lost weight is the weight of volatile substances at 350-360 ℃; heating a known amount of sample to 900-950 ℃ by using air or oxygen instead of nitrogen flow, wherein the weight loss is the weight of the carbon black; the remaining content is the percentage of ash. The method is simple to operate, high in accuracy, good in repeatability and easy to popularize.
Description
Technical Field
The invention belongs to the field of chemistry, and discloses a method for detecting the component content of a mixture of TESPT and carbon black by TGA analysis.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
Thermogravimetric analysis (TGA) is a technique for measuring the relationship between the mass of a sample and the temperature or time of the sample under the control of program temperature and in different atmospheres, and is widely applied to the quantitative determination of components of an industrial elastomer system, and can accurately analyze volatile substances in the elastomer system, such as water, a plasticizer and the like; carbon black can also be analyzed as well as inorganic fillers and ash.
The combined use of TESPT (bis (triethoxysilylpropyl) tetrasulfide) and carbon black has an important role in the rubber process, so that the accurate and rapid determination of the content of each component in industrial production is very important, but the inventor finds that: at present, no more effective method for solving the problem exists in the aspects of rubber industry and the like.
Disclosure of Invention
In order to overcome the problems, the invention provides a detection method for analyzing the content of components of a mixture of TESPT and carbon black by using TGA. The method is simple to operate, high in accuracy, good in repeatability and easy to popularize.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, a method for detecting a thermal weight loss of a mixture of TESPT and carbon black is provided, which includes:
heating a known amount of sample in a nitrogen flow, wherein the weight lost at 350-360 ℃ is the weight of volatile substances;
heating a known amount of sample to 900-950 ℃ by using air or oxygen instead of nitrogen flow, wherein the weight loss is the weight of the carbon black; the remaining content is the percentage of ash.
Therefore, the invention provides a simple, quick and efficient method for detecting the component content of the mixture of TESPT and carbon black. A known amount of sample is heated in nitrogen flow by using a synchronous thermal analyzer, and the lost sample at 350-360 ℃ is the weight of the volatile substance. And (3) replacing nitrogen flow with air or oxygen, and heating to 900-950 ℃, wherein the weight lost is the weight of the carbon black. The weight which is not lost in the air or oxygen flow at 900-950 ℃ is the weight of the ash.
In a second aspect of the present invention, a system for detecting the thermal weight loss of a mixture of TESPT and carbon black is provided, which includes: thermogravimetric analyzer, weighing device.
The device provided by the invention has a simple structure, replaces the traditional gravimetric analysis, namely, the scheme of detection through heating equipment such as a drying oven and a muffle furnace, can accurately control the experimental conditions through the synchronous thermal analyzer, and has good repeatability and high accuracy.
In a third aspect of the invention, there is provided the use of the system described above in the rubber industry.
The invention can realize accurate and rapid determination of the rubber sample containing TESPT (bis (triethoxysilylpropyl) tetrasulfide) and carbon black in industrial production, so the invention is expected to be widely applied to the rubber industry.
The invention has the beneficial effects that:
(1) the invention replaces the traditional gravimetric analysis, namely the scheme of detection by heating equipment such as a drying oven, a muffle furnace and the like, can accurately control the experimental conditions by the synchronous thermal analyzer, has good repeatability and high accuracy, and greatly changes the traditional scheme.
(2) The method is simple, low in cost, strong in practicability and easy to popularize.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a temperature/weight chart of example 1 of the present invention.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
Interpretation of terms
In the present application, TESPT means: (bis (triethoxysilylpropyl) tetrasulfide).
A thermal weight loss detection method of a mixture of TESPT and carbon black comprises the following steps:
heating a known amount of sample in a nitrogen flow, wherein the weight lost at 350-360 ℃ is the weight of volatile substances;
heating a known amount of sample to 900-950 ℃ by using air or oxygen instead of nitrogen flow, wherein the weight loss is the weight of the carbon black; the remaining content is the percentage of ash.
The general thermogravimetric detection method is characterized in that the measurement is carried out by a gravimetric method, the number of key points needing to be controlled during measurement is particularly large, and the requirements on operator operation and experimental environment are high. For this reason, the system of the application researches the thermal weight loss change rule of the mixture of TESPT and carbon black, and finds that: the high temperature is set to 900-950 ℃, so that sufficient combustion is ensured, ash content is more thoroughly remained, the accuracy of results is improved, the detection time is shortened, and the accurate and rapid determination of the content of each component is realized.
In some embodiments, the sample is a mixture of TESPT and carbon black.
In some embodiments, the detecting employs a thermogravimetric analyzer.
In some embodiments, the thermogravimetric analyzer is a synchronous thermal analyzer.
In some embodiments, the initial temperature is set to 30 to 40 ℃ and the nitrogen flow rate is set to 20 to 30 ml/min.
In some embodiments, the temperature is raised from 30-40 ℃ to 350-360 ℃ at a temperature raising rate of 20-30 ℃/min in a nitrogen atmosphere.
In some embodiments, the nitrogen flow is switched to oxygen flow or air flow at a constant temperature of 350-360 ℃ for 3-5 min in a nitrogen atmosphere.
In some embodiments, the temperature is raised to 900-950 ℃ in 20-30 ml/min oxygen flow or air flow at a temperature raising rate of 20-30 ℃/min.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1:
experimental equipment:
synchronous thermal analyzer: TGA-DSC2, mettler-toledo;
the method comprises the following operation steps:
program setting: the initial temperature was set at 30 ℃ and the nitrogen flow rate was set at 20 ml/min; heating from 30 ℃ to 350 ℃ at a heating rate of 20 ℃/min in a nitrogen atmosphere; keeping the temperature of the mixture constant at 350 ℃ for 3min in the nitrogen atmosphere, switching the nitrogen flow into oxygen flow, and heating the mixture to 900 ℃ in the oxygen flow of 20ml/min at the heating rate of 20 ℃/min.
Sample detection: 12mg of sample was weighed to the nearest 0.1mg in the instrument sample pan. Note that the sample weight should be consistent with the scale of the instrument. Calling out a temperature-raising program, inputting the mass of the sample, prompting the operation equipment according to the equipment, adjusting a recorder to enable the instrument to directly read the weight loss percentage of the sample, and waiting for the equipment to finish the automatic operation.
And (4) analyzing results: directly reading the weight loss in the nitrogen flow at 30-350 ℃ in a temperature/weight chart, namely the percentage content of the volatile components; reading the mass loss in air or oxygen at 350-900 ℃ in a chart, namely the percentage content of the carbon black; and finally, obtaining the residual content which is the percentage content of the ash content by differentiating.
And (3) testing results:
a total of 10 sets of tests were performed, with the results shown in table 1,
TABLE 1 results of thermogravimetric testing of different samples
| Serial number | Volatile matter% | Carbon black, content of | Ash content% |
| 1 | 33.5968 | 65.4122 | 0.9910 |
| 2 | 33.5724 | 65.4324 | 0.9952 |
| 3 | 33.5815 | 65.4126 | 1.0059 |
| 4 | 33.5904 | 65.4296 | 0.9800 |
| 5 | 33.5865 | 65.4326 | 0.9809 |
| 6 | 33.5902 | 65.4014 | 1.0084 |
| 7 | 33.6025 | 65.4031 | 0.9944 |
| 8 | 33.5914 | 65.4125 | 0.9961 |
| 9 | 33.5984 | 65.4099 | 0.9917 |
| 10 | 33.5768 | 65.5314 | 0.8918 |
| Mean value of | 33.5887 | 65.4278 | 0.9835 |
| Standard deviation of | 0.009583 | 0.038176 | 0.033479 |
Wherein the test results of the first group are: 33.5968% of volatile matters; carbon black 65.4142%, ash 0.9910%, as shown in figure 1.
Example 2:
experimental equipment:
synchronous thermal analyzer: TGA-DSC2, mettler-toledo;
the method comprises the following operation steps:
program setting: the initial temperature was set at 40 ℃ and the nitrogen flow rate was set at 30 ml/min; heating from 40 ℃ to 360 ℃ at a heating rate of 30 ℃/min in a nitrogen atmosphere; keeping the temperature of the mixture constant in the nitrogen atmosphere at the temperature of 360 ℃ for 5min, switching the nitrogen flow into oxygen flow, and heating the mixture to 950 ℃ in the oxygen flow of 30ml/min at the heating rate of 30 ℃/min.
Sample detection: weigh 5mg of sample to the nearest 0.1mg in the instrument sample pan. Note that the sample weight should be consistent with the scale of the instrument. Calling out a temperature-raising program, inputting the mass of the sample, prompting the operation equipment according to the equipment, adjusting a recorder to enable the instrument to directly read the weight loss percentage of the sample, and waiting for the equipment to finish the automatic operation.
And (4) analyzing results: directly reading the weight loss in the nitrogen flow from 40 ℃ to 360 ℃ in a temperature/weight chart, wherein the weight loss is the percentage content of the volatile components; reading the mass loss in air or oxygen at 360-950 ℃ in a chart, namely the percentage content of the carbon black; and finally, obtaining the residual content which is the percentage content of the ash content by differentiating.
Example 3:
experimental equipment:
synchronous thermal analyzer: TGA-DSC2, mettler-toledo;
the method comprises the following operation steps:
program setting: the initial temperature was set at 35 ℃ and the nitrogen flow rate was set at 25 ml/min; heating from 35 deg.C to 355 deg.C at a heating rate of 25 deg.C/min in nitrogen atmosphere; keeping the temperature of the mixture constant at 355 ℃ for 4min in a nitrogen atmosphere, switching the nitrogen flow into an oxygen flow, and heating the mixture to 925 ℃ in the oxygen flow at a heating rate of 25 ℃/min.
Sample detection: weigh 20mg of sample to the nearest 0.1mg in the instrument sample pan. Note that the sample weight should be consistent with the scale of the instrument. Calling out a temperature-raising program, inputting the mass of the sample, prompting the operation equipment according to the equipment, adjusting a recorder to enable the instrument to directly read the weight loss percentage of the sample, and waiting for the equipment to finish the automatic operation.
And (4) analyzing results: directly reading the weight loss in the nitrogen flow from 35 ℃ to 355 ℃ in a temperature/weight chart, namely the percentage content of the volatile components; reading the mass loss in air or oxygen at 355 ℃ to 925 ℃ in a graph, namely the percentage of carbon black; and finally, obtaining the residual content which is the percentage content of the ash content by differentiating.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the present invention has been described with reference to the specific embodiments, it should be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A thermal weight loss detection method of a mixture of TESPT and carbon black is characterized by comprising the following steps:
heating a known amount of sample in nitrogen flow, wherein the lost weight is the weight of volatile substances at 350-360 ℃;
heating a known amount of sample to 900-950 ℃ by using air or oxygen instead of nitrogen flow, wherein the weight loss is the weight of the carbon black; the remaining content is the percentage of ash.
2. The method for detecting the thermal weight loss of a mixture of TESPT and carbon black of claim 1, wherein said sample is a mixture of TESPT and carbon black.
3. The method for the thermogravimetric analysis of TESPT with carbon black mixture according to claim 1, characterized in that the thermogravimetric analyzer is used for the detection.
4. The method of claim 3, wherein the thermogravimetric analyzer is a synchronous thermal analyzer.
5. The method for detecting the thermal weight loss of a mixture of TESPT and carbon black of claim 1, wherein the initial temperature is set to 30 to 40 ℃ and the nitrogen flow rate is set to 20 to 30 ml/min.
6. The method for detecting the thermal weight loss of a mixture of TESPT and carbon black of claim 1, wherein the temperature is raised from 30-40 ℃ to 350-360 ℃ at a rate of 20-30 ℃/min in a nitrogen atmosphere.
7. The method for detecting the thermal weight loss of a mixture of TESPT and carbon black according to claim 1, characterized in that the temperature is kept constant for 3-5 min in a nitrogen flow at 350-360 ℃, and the nitrogen flow is switched to an oxygen flow or an air flow.
8. The method for detecting the thermal weight loss of a mixture of TESPT and carbon black of claim 1, wherein the temperature is raised to 900 to 950 ℃ at a rate of 20 to 30 ℃/min in an oxygen flow or an air flow of 20 to 30 ml/min.
9. A system for detecting the thermal weight loss of a mixture of TESPT and carbon black comprises: thermogravimetric analyzer, weighing device.
10. Use of the system of claim 9 in the rubber industry.
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| CN113567293A (en) * | 2021-07-21 | 2021-10-29 | 湖北亿纬动力有限公司 | Method for testing content of carbon nanotubes in carbon nanotube conductive slurry |
| CN114734387A (en) * | 2022-04-06 | 2022-07-12 | 奇瑞汽车股份有限公司 | Fixture and method for measuring volatilization loss of plasticizer of PVC (polyvinyl chloride) planar material for vehicle |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113567293A (en) * | 2021-07-21 | 2021-10-29 | 湖北亿纬动力有限公司 | Method for testing content of carbon nanotubes in carbon nanotube conductive slurry |
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Application publication date: 20201106 |