CN100489488C - Thermal analysis method for determining silicane mixture content - Google Patents
Thermal analysis method for determining silicane mixture content Download PDFInfo
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- CN100489488C CN100489488C CNB2006100403313A CN200610040331A CN100489488C CN 100489488 C CN100489488 C CN 100489488C CN B2006100403313 A CNB2006100403313 A CN B2006100403313A CN 200610040331 A CN200610040331 A CN 200610040331A CN 100489488 C CN100489488 C CN 100489488C
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Abstract
The thermal analysis method for content of silicane mixture comprises: in inertial gas, heating as 10Deg/min till 550Deg and holding for 60min; then, changing into oxygen at 650Deg and holding 60min; obtaining the initial mass M0 and M1 at 105Deg, calculating the content for the low-boil as (M1-M0)/M0*100%, the silicane coupling agent as (M2-M1)/M0*100%, with the final mass M3, the carbon black content as (M3-M2)/M0*100%, and final residual content as M3/M0*100%. This invention has well accuracy and sensitivity.
Description
Technical field
The present invention relates to a kind of hot analyzing detecting method, be specifically related to a kind of heat analysis method of measuring silicane mixture content with thermogravimetry.
Background technology
Silane mixture is a kind of novel silane coupling agent and the potpourri of carbon black, is a kind of very important starting material during rubber industry is produced, and it is widely used as vulcanizing agent and activator.Owing to exist (the R-S of functional group of two kinds of character in the special molecular structure of silane coupling agent
iX
3), inorganic filler and rubber are combined with chemical force, thereby the usability of physical property such as wear-resistingly, anti-tearing of making rubber, flexible resistance and finished product is significantly improved, and energy consumption only is like product half.But, method with routine is difficult to the content of low-boiling point materials such as moisture content, ethanol, silane coupling agent, carbon black and final residue thing in the sample silane mixture is measured accurately, and each components contents is very necessary in the silane mixture and accurately measure.At first, the quality that how much directly has influence on rubber finished products such as tire of moisture content, ethanol content if content is more, then can makes and contain a lot of pores in the finished product, and rubber product is ruptured easily, reduces its serviceable life etc.Secondly, final residue thing major part comes from silane coupling agent, and residue is many more, shows that the quality of silane coupling agent is just poor more, and its production technology is bad more.At last, the blending ratio of carbon black and silane coupling agent is different, also can influence the capability and performance and the energy consumption of product.The existing dependence on import of silane mixture is converted to production domesticization gradually at present, everything is all had higher requirement to accuracy and simplicity that silicane mixture content is measured, and chemical analysis of wasting time and energy such as burning, titration, extraction etc. can not have been satisfied and produced and the needs of development, its accuracy is lower, and the human factor influence is bigger.
Heat analysis method is a kind of under programed temperature, a kind of technology of the physical property of measurement of species and temperature relation.In the process of heating or cooling, along with the variation of structure, phase and the chemical property of material all can be with the variation of corresponding physical property.But also do not use heat analysis method to measure the report of silicane mixture content at present.
Summary of the invention
Starting material silane compound as a kind of rubber industry, it is used more and more widely, in order to improve accuracy and the convenience that its component concentration is measured, improve the quality of finished product, adapt to need of industrial production, shortcoming at general chemical analysis method, the present invention will provide a kind of detection new method of quick, easy, accurate, highly sensitive silane mixture quality: gravitational thermal analysis method is used for measuring each component concentration of silane mixture, is specially content of low boilers, silane coupling agent, carbon black and final residue amounts such as moisture content, ethanol.
Used thermogravimetry (TG) is that it is under programed temperature among the present invention, a kind of technology of measurement of species quality and temperature relation.Its ultimate principle is: pyrolysis macromolecular compound fully in nitrogen, then in air with the carbon black after-flame, remaining residue is a residue.
A kind of heat analysis method of measuring silicane mixture content, under programed temperature, measurement of species quality and temperature relation may further comprise the steps:
Sample is positioned in the inert gas atmosphere (for example nitrogen) speed program heating with 10 ℃/min;
Continue to be heated to 550 ℃, isothermal 60min;
Be warming up to 650 ℃;
Gas is replaced with oxygen, isothermal 60min;
Calculate by thermogravimetric curve:
From thermogravimetric curve, read the initial mass M of sample
0, the mass M when reading 105 ℃
1, the content of low-boiling point material (as moisture content and ethanol) is: (M
1-M
0)/M
0* 100%;
Read the mass M of sample
2, the content of the silane coupling agent in the silane mixture is: (M
2-M
1)/M
0* 100%;
Read in the silane mixture final mass M under the oxygen atmosphere
3, the percentage composition of carbon black is in the silane mixture: (M
3-M
2)/M
0* 100%;
The content of final residue thing is: M
3/ M
0* 100%.
More optimize and more particularly, step of the present invention is as follows:
1, choosing of amount of samples: get 5～10mg sample, be positioned in the alundum (Al planchet;
2, the design of program: in nitrogen atmosphere, be heated to 550 ℃ with the speed of 10 ℃/min from room temperature; Isothermal 60min under 550 ℃ of temperature; Speed with 10 ℃/min is warming up to 650 ℃; Change gas, change oxygen into by nitrogen; At 650 ℃ of isothermal 60min again.
3, choosing of atmosphere: the flow of nitrogen and oxygen is: 40ml/min.
4, calculate by thermogravimetric curve: curve as shown in Figure 1, from thermogravimetric curve,
A. can directly read the initial mass M when beginning to heat
0With the mass M 105 ℃ the time
1, the content of low-boiling point material such as moisture content and ethanol is so
(M
1-M
0)/M
0*100％；
Mass M when b. reading in following 650 ℃ of nitrogen atmosphere
2, (M so
2-M
1)/M
0* 100% is the content of the silane coupling agent in the silane mixture just;
C. read in silane mixture final mass M under the oxygen atmosphere from thermogravimetric curve
3, so, the percentage composition of carbon black is in the silane mixture: (M
3-M
2)/M
0* 100%;
D. the content of final residue thing is: M
3/ M
0* 100%.
In above scheme:
1, the basic structure of thermogravimetric analyzer is made up of the heating furnace of precision balance and linear program temperature control.Thermobalance is to measure according to the relation of the inclination of balance beam and weight change, and sensitivity can reach 0.1 μ g; Programed temperature is controlled by near two thermopairs in the burner hearth and the heating furnace silk, can provide accurately and sensitive temperature program(me), and temperature accuracy can reach ± and 2 ℃.
2, thermogravimetry (TG) measurement sample dosage is 5-10mg only among the present invention, and consumption is few.To the test of can repeatedly sampling of a certain batch of sample.
3, whole experiment is about two hours, and method is fast convenient, can detect each components contents of sample silane mixture quickly and accurately.
4, all processes is automatically performed by instrument, has reduced the influence of the sum of errors surrounding environment of manual operation.
Alundum (Al planchet described in the step 1 also can be used the Pt planchet instead.
The present invention has done a large amount of comparative experiments inventor aspect the speed of the flow of isothermal time, the atmosphere of test, programming rate, the sample dosage, grasped best experiment condition with this, technical progress of the present invention is: measure accurately, consumption is few, highly sensitive, method is simple, quick.Quality control to the industrialization of silane mixture has practical significance.
Description of drawings
Fig. 1 is the thermogravimetric curve of silane mixture standard items;
Fig. 2 is the thermogravimetric curve of sample silane mixture.
Embodiment
Embodiment 1, measures the heat analysis method of silicane mixture content,
The 7 serial thermogravimetric analyzers that instrument adopts U.S. PE company to produce are got import silane mixture material samples 8.539mg and homemade sample 8.417mg, and the flow of nitrogen and oxygen is: 40ml/min.
Choosing of amount of samples: get 5～10mg sample, be positioned in the alundum (Al planchet;
The design of program: in nitrogen atmosphere, be heated to 550 ℃ with the speed of 10 ℃/min from room temperature; Isothermal 60min under 550 ℃ of temperature; Speed with 10 ℃/min is warming up to 650 ℃; Change gas, change oxygen into by nitrogen; At 650 ℃ of isothermal 60min again.
Choosing of atmosphere: the flow of nitrogen and oxygen is: 40ml/min.
Calculate by thermogravimetric curve: curve from thermogravimetric curve, is heated to 550 ℃ from room temperature with the speed of 10 ℃/min as shown in Figure 1 in nitrogen atmosphere; Isothermal 60min under 550 ℃ of temperature; Speed with 10 ℃/min is warming up to 650 ℃; Change gas, change oxygen into by nitrogen; At 650 ℃ of isothermal 60min again; Obtain thermogravimetric curve, its synoptic diagram such as Fig. 2; From thermogravimetric curve, can directly read the initial mass M when beginning to heat
0With the mass M 105 ℃ the time
1, the content of low-boiling point material such as moisture content and ethanol is (M so
1-M
0)/M
0* 100%; Mass M when reading in following 650 ℃ of nitrogen atmosphere
2, (M so
2-M
1)/M
0* 100% is the content of the silane coupling agent in the silane mixture just; Read in silane mixture final mass M under the oxygen atmosphere from thermogravimetric curve
3, so, the percentage composition of carbon black is in the silane mixture:
(M
3-M
2)/M
0*100％；
The content of final residue thing is:
M
3/M
0*100％。
Claims (7)
1, a kind of heat analysis method of measuring silicane mixture content, under programed temperature, measurement of species quality and temperature relation may further comprise the steps:
Sample is positioned in the inert gas atmosphere, with the speed program heating of 10 ℃/min;
Continue to be heated to 550 ℃, isothermal 60min;
Be warming up to 650 ℃;
Gas is replaced with oxygen, isothermal 60min;
Calculate by thermogravimetric curve:
From thermogravimetric curve, read the initial mass M of sample
0, the mass M when reading 105 ℃
1, the content of low-boiling point material is: (M
1-M
0)/M
0* 100%;
The mass M of sample when reading in following 650 ℃ of nitrogen atmosphere
2, the content of the silane coupling agent in the silane mixture is: (M
2-M
1)/M
0* 100%;
Read in the silane mixture final mass M under the oxygen atmosphere
3, the percentage composition of carbon black is in the silane mixture: (M
3-M
2)/M
0* 100%;
The content of final residue thing is: M
3/ M
0* 100%.
According to the heat analysis method of the described mensuration silicane mixture content of claim 1, it is characterized in that 2, concrete steps are as follows:
Choosing of amount of samples: get 5～10mg sample, be positioned in the planchet;
The design of program: in nitrogen atmosphere, be heated to 550 ℃ with the speed of 10 ℃/min from room temperature; Isothermal 60min under 550 ℃ of temperature; Speed with 10 ℃/min is warming up to 650 ℃; Change gas, change oxygen into by nitrogen; At 650 ℃ of isothermal 60min again;
Choosing of atmosphere: the flow of nitrogen and oxygen is: 40ml/min;
Calculate by thermogravimetric curve, from thermogravimetric curve:
A. directly read the initial mass M when beginning to heat
0With the mass M 105 ℃ the time
1, the content of low-boiling point material moisture content and ethanol is (M
1-M
0)/M
0* 100%;
Mass M when b. reading in following 650 ℃ of nitrogen atmosphere
2, (M
2-M
1)/M
0* 100% is the content of the silane coupling agent in the silane mixture;
C. read in silane mixture final mass M under the oxygen atmosphere from thermogravimetric curve
3, the percentage composition of carbon black is in the silane mixture: (M
3-M
2)/M
0* 100%;
D. the content of final residue thing is: M
3/ M
0* 100%.
3, according to the heat analysis method of the described mensuration silicane mixture content of claim 2, it is characterized in that,
Described inert gas is a nitrogen;
Described planchet is the alundum (Al planchet.
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| CN101067594B (en) * | 2007-06-18 | 2010-12-15 | 登封电厂集团铝合金有限公司 | Method for guiding smelting process by determining relative carbon-content in solid sample of Electro-thermal method smelting aluminum silicon alloy |
| CN102288514B (en) * | 2011-07-01 | 2013-01-23 | 攀枝花学院 | Method for analyzing free carbon |
| CN103954528B (en) * | 2014-05-26 | 2016-03-09 | 国网山东省电力公司菏泽供电公司 | Electric wire and cable jacket material oxidation induction period and content of carbon black proving installation |
| CN106644812B (en) * | 2016-12-02 | 2019-10-15 | 山东圣泉新材料股份有限公司 | The quantitative detecting method of graphene in a kind of solution |
| CN106644804A (en) * | 2016-12-02 | 2017-05-10 | 山东圣泉新材料股份有限公司 | Quantitative detection method for graphene in composite masterbatch |
| CN107290243A (en) * | 2017-05-25 | 2017-10-24 | 常州第六元素材料科技股份有限公司 | A kind of accurate measurement method of graphene content in graphene slurry |
| CN107421843B (en) * | 2017-08-22 | 2020-06-19 | 中交四航工程研究院有限公司 | Moisture detection method of silane paste |
| CN109297853A (en) * | 2018-08-22 | 2019-02-01 | 深圳信测标准技术服务股份有限公司 | A method of for automatically detecting content of carbon black in rubber |
| CN110987711B (en) * | 2019-11-26 | 2022-11-25 | 国联汽车动力电池研究院有限责任公司 | Component testing and analyzing method for lithium ion battery anode material |
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