CN104237299A - Thermal analysis method for measuring contents of polydimethylsiloxane (PDMS), SiO2 and aluminum hydroxide (ATH) in silicone rubber composite insulator - Google Patents
Thermal analysis method for measuring contents of polydimethylsiloxane (PDMS), SiO2 and aluminum hydroxide (ATH) in silicone rubber composite insulator Download PDFInfo
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Abstract
The invention relates to a thermal analysis method for measuring the contents of polydimethylsiloxane (PDMS), SiO2 and aluminum hydroxide (ATH) in a silicone rubber composite insulator. The method comprises the steps of S1, respectively measuring the thermal gravity loss (TG) curves of the PDMS, the ATH and the SiO2 for three times by a thermal gravity loss-differential thermal analysis combination comprehensive thermal analyzer, and averaging; S2, cutting three parts from the silicone rubber insulator randomly, wherein the cut parts have the sizes of 1cm*1cm and the masses within the range of 5-50mg; pretreating, then measuring the TG curves of the silicone rubber insulator for three times, and averaging; S3, calculating the thermal weight loss rates of the PDMS, the ATH, the SiO2 and the silicone rubber insulator in the ranges of 20-360 DEG C and 360-700 DEG C according to the TG curves; S4, substituting the obtained numerical values into the formula delta M=(m(ATH)*deltam(ATH)+m(PDMS)*delta m(PDMS)+m(SiO2)*delta m(SiO2))/(m(ATH)+m(PDMS)+m(SiO2)); and S5, working out the equation in the S4, and calculating the contents of the ATH and the SiO2 relative to the PDMS. According to the method, the contents of the three components of the silicone rubber composite insulator can be worked out by utilizing the thermal weight loss rates of the three components in the respective specific thermal decomposition temperature ranges, and a concrete calculation method is provided.
Description
Technical field
The present invention relates to dimethyl silicone polymer, white carbon powder, aluminium-hydroxide powder (PDMS, SiO in a kind of mensuration silicon rubber compound insulator
2, ATH) heat analysis method of content.
Background technology
In ultra-high-tension power transmission line, decide the operation life of whole piece transmission line of electricity the serviceable life of composite insulator string, therefore, how to filter out good quality, composite insulator of good performance drop into application and seem most important.
But for power industry relevant departments, the detection of each component concentration in composite insulator at present, the detection particularly to white carbon, content of aluminium powder also exists certain technical barrier.For the composite insulator that white carbon, content of aluminium powder are slightly on the high side, its price occupies very large advantage relative to the insulator of other kinds, and can up to standardly pass through in Performance Detection in every respect, such composite insulator is on short terms without any problem, but in long-term hanging net operation, just likely there is situation about terminating in advance serviceable life, not in time, so will cause irremediable economic loss to country if find.Therefore, in numerous competitive bidding companies, select the composite insulator production firm that cheap, quality again can be up to standard, need undoubtedly to set up a set of industry examination criteria to pass judgment on the quality of each vendor product quality.
At present, power industry also lacks the effective characterization method of system to the detection of silicon rubber insulator component concentration.
Summary of the invention
Technical matters to be solved by this invention, is just to provide PDMS, SiO in a kind of mensuration silicon rubber compound insulator
2, ATH content thermal analysis system,
Solve the problems of the technologies described above, the technical solution used in the present invention is:
PDMS, SiO in a kind of mensuration silicon rubber compound insulator
2, ATH content thermal analysis system, it is characterized in that comprising the following steps:
The Thermal Synthetic Analysis instrument of S1 TG-DTA coupling measures three PDMS, ATH, SiO respectively
2thermal weight loss (TG) curve, to three times measure data average;
S2 cuts three positions at random to silicon rubber insulator, and each position size is 1cm × 1cm, and quality, in 5 ~ 50mg, after pretreatment, records three silicon rubber insulator thermal weight loss (TG) curves, averages to the data that three times are measured;
S3 calculates PDMS, ATH, SiO within the scope of 20 ~ 360 DEG C and 360 ~ 700 DEG C according to thermal weight loss (TG) curve analysis software
2, silicon rubber insulator thermal weight loss rate;
S4 substitutes into thermal weight loss rate △ M formula (1) of silicon rubber insulator according to step S3 institute value:
△M＝(m
ATH×△m
ATH+m
PDMS×△m
PDMS+m
SiO2×△m
SiO2)/(m
ATH+m
PDMS+m
SiO2)--------------(1)；
Wherein: △ M is the thermal weight loss rate of silicon rubber insulator, be given value;
△ m
aTH, △ m
pDMS, △ m
siO2be respectively ATH, PDMS and SiO
2in the thermal weight loss rate of relevant temperature scope, it is also given value;
M
aTH, m
pDMS, m
siO2be respectively ATH, PDMS and SiO in silicon rubber insulator
2quality, be unknown number;
The equation of S5 solution procedure S4, calculates ATH, SiO
2relative to the relative content of PDMS.
The heating rate of the Thermal Synthetic Analysis instrument of described step S1 is 10k/min, and work atmosphere is air, and working temperature is at 20 ~ 700 DEG C.
Pre-service in described step S2 refers to: sample 3 parts clean up after, be placed in electrically heated drying cabinet, at 50 ~ 100 DEG C dry 10 ~ 14 hours, transfer in drying cupboard after taking-up and place; During test, sample is taken out, be trimmed to granularity and be less than 2mm
Beneficial effect: the principle of physical change and chemical change can occur when heating or cool according to material in the present invention, adopt thermogravimetry (TG) and differential thermal analysis coupling technique, determine the component concentration of various known component silicon rubber insulator, and give concrete operating process and computing method.
Thermogravimetry (TG) (TG) is under programed temperature, the quality of measurement of species and a kind of technology of temperature relation; Differential thermal analysis (DTA) is under programed temperature, and the temperature difference of measurement of species and reference substance in time or a kind of technology of temperature variation.Thermogravimetry (TG) and differential thermal analysis coupling can measure the thermal weight loss rate variation with temperature relation of each component in silicon rubber insulator accurately, different according to the behavior of different material thermal weight loss, derive PDMS, SiO in silicon rubber insulator
2, ATH content.
Experimental data shows, same sample, and measure TG curve three times, the thermal weight loss rate error under same temperature is no more than 2%, and reproducibility is good, and result of calculation accurately and reliably.
ATH, SiO of comparative example
2, PDMS TG curve, wherein, SiO
2in Range of measuring temp, do not have thermal decomposition, without obvious mass loss, there is the temperature range non-overlapping copies of thermal decomposition weightlessness in ATH and PDMS, therefore, content mutual interference in solution procedure of three kinds of components is few, and the resultant error calculated is little.
Accompanying drawing explanation
Fig. 1 is that reappearance TG curve is measured in three times of aluminium-hydroxide powder (ATH);
Fig. 2 is that reappearance TG curve is measured in three times of white carbon powder (SiO2);
Fig. 3 is that reappearance TG curve is measured in three times of dimethyl silicone polymer (PDMS);
Fig. 4 is SiO
2content is that the silicon rubber insulator of 20 parts measures reappearance TG curve three times;
To be ATH content be Fig. 5 that the silicon rubber insulator of 160 parts measures reappearance TG curves three times;
Fig. 6 is the TG curve of the silicon rubber insulator of different ATH content;
Fig. 7 is different SiO
2the TG curve of the silicon rubber insulator of content;
Fig. 8 is ATH, SiO of being combined
2, PDMS TG curve map.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is further elaborated.
PDMS, SiO in mensuration silicon rubber compound insulator of the present invention
2, ATH content thermal analysis system, comprise the following steps:
The Germany's resistance to STA449 of speeding Thermal Synthetic Analysis instrument of S1 TG-DTA coupling measures three PDMS, ATH, SiO respectively
2thermal weight loss (TG) curve, to three times measure data average; During measurement, the heating rate of Thermal Synthetic Analysis instrument is 10k/min, and work atmosphere is air, and working temperature is at 20 ~ 700 DEG C.
S2 specifically comprises following sub-step
S2-1 appoints sampling 3 parts (cutting middle clean part) from the full skirt of insulator or sheath position, and specification is 1cm × 1cm, and quality is in 5 ~ 50mg, after cleaning up, be placed in electrically heated drying cabinet, dry 10 ~ 14 hours at 50 ~ 100 DEG C, transfer in drying cupboard after taking-up and place.During test, sample is taken out, cut into granularity and be less than 2mm;
S2-2 opens computer, opens Thermal Synthetic Analysis instrument, opens the switch of each part of detecting successively;
Open the resistance to STA449 Survey Software of speeding of Germany, the gas outlet of putting on body of heater is Open;
Open nitrogen cylinder, pressure regulation is by force 5 ~ 50kpa, and observation flowmeter is Protective is 5 ~ 30mL/min;
Purge2 (on the left of body of heater) is adjusted to 5 ~ 30mL/min;
Click " opening " on " file " hurdle, choose the baseline under a corresponding heating rate, click " continuation ", in " measurement pattern ", select " sample+correction ", fill in sample number into spectrum, material category and title;
Accept hurdle, selecting " temperature correction ", " sensitivity correction ", keep interface;
S2-3 rises the right high-temperature furnace body, puts into sky crucible, falls high-temperature furnace body, lid is restored, after stable, and zero setting;
Rise high-temperature furnace body, take out crucible, setting-out product, are placed on crucible on support, fall body of heater, show sample quality, after digital radix point to be shown 3rd stable after, write down sample quality, in the interface of opening above, input these data;
S2-4 point " continuation ", insert sweep gas, protection gas information, in " continuation ", click " temperature program(me) ", confirm or revise the final temperature needing to measure, select sweep gas 2, protection gas, point " continuation ", inserts file, preservation;
Successively click determine, Initializing operating condition, clearing, beginning, measure run;
The analysis software that S3 carries according to thermal weight loss (TG) curve Thermal Synthetic Analysis instrument, measures PDMS, ATH, SiO within the scope of 20 ~ 360 DEG C and 360 ~ 700 DEG C
2, silicon rubber insulator thermal weight loss rate;
S4 substitutes in thermal weight loss rate △ M formula (1) of silicon rubber insulator according to step S3 institute value and calculates;
△M＝(m
ATH×△m
ATH+m
PDMS×△m
PDMS+m
SiO2×△m
SiO2)/(m
ATH+m
PDMS+m
SiO2)--------------(1)；
In formula, △ M is the weight-loss ratio of silicon rubber insulator,
△ m
aTH, △ m
pDMS, △ m
siO2be respectively ATH, PDMS and SiO
2in the thermal weight loss rate of relevant temperature scope,
M
aTH, m
pDMS, m
siO2be respectively ATH, PDMS and SiO in silicon rubber insulator
2quality;
S5 chooses two groups of different △ M, △ m
aTH, △ m
pDMS, △ m
siO2, can ATH, SiO be calculated
2relative to the quality of PDMS.
Following embodiment is see Fig. 1 to Fig. 7.
The silicon rubber insulator of certain component of embodiment 1 (PDMS is 120 parts, and ATH is 80 parts, and white carbon is 25 parts), the computing method of its component concentration, comprise the following steps:
(1), to measure silicon rubber thermal weight loss rate in 20 ~ 360 DEG C with analysis software be 12.63%, and in 360 ~ 700 DEG C, silicon rubber thermal weight loss rate is 43.65%.
(2), measure at 20 ~ 360 DEG C of PDMS, ATH, SiO with analysis software
2thermal weight loss rate be respectively 2.85%, 30.49%, 1.81%, equation can be obtained 1.: 12.63%=(m
aTH× 30.49%+100 × 2.85%+m
siO2× 1.81%)/(m
aTH+ 100+m
siO2).
(3), measure at 360 ~ 700 DEG C of PDMS, ATH, SiO with analysis software
2thermal weight loss rate be respectively 77.22%, 5.17%, 0.67%, equation can be obtained 2.: 43.65%=(m
aTH× 5.17%+100 × 77.22%+m
siO2× 0.67%)/(m
aTH+ 100+m
siO2).
(4), 2. 1. solving equation group obtain: m
aTH=66.18, m
siO2=18.87.
(5), each constituent mass mark is calculated:
m
ATH(％)＝66.18÷(66.18+100+18.87)＝35.8％，m
SiO2(％)＝18.87÷(66.18+100+18.87)＝10.2％，m
PDMS＝100÷(66.18+100+18.87)＝54.0％；
(6), each component Theoretical Mass mark: m
aTH(%)=80 ÷ (80+120+25)=35.6%, m
siO2(%)=25 ÷ (80+120+25)=11.1%, m
pDMS(%)=120 ÷ (80+120+25)=53.3%.
The silicon rubber insulator of certain component of embodiment 2 (PDMS is 120 parts, and ATH is 110 parts, and white carbon is 25 parts), the computing method of its component concentration, comprise the following steps:
(1), to measure silicon rubber thermal weight loss rate in 20 ~ 360 DEG C with analysis software be 15%, and in 360 ~ 700 DEG C, silicon rubber thermal weight loss rate is 38.68%.
(2), measure at 20 ~ 360 DEG C of PDMS, ATH, SiO with analysis software
2thermal weight loss rate be respectively 2.85%, 30.49%, 1.81%, equation can be obtained 1.: 12.63%=(m
aTH× 30.49%+100 × 2.85%+m
siO2× 1.81%)/(m
aTH+ 100+m
siO2).
(3), measure at 360 ~ 700 DEG C of PDMS, ATH, SiO with analysis software
2thermal weight loss rate be respectively 77.22%, 5.17%, 0.67%, equation can be obtained 2.: 43.65%=(m
aTH× 5.17%+100 × 77.22%+m
siO2× 0.67%)/(m
aTH+ 100+m
siO2).
(4), 2. 1. solving equation group obtain: m
aTH=94.11, m
siO2=18.43.
(5), each constituent mass mark is calculated: m
aTH(%)=94.11 ÷ (94.11+100+18.43)=44.3%, m
siO2(%)=18.43 ÷ (94.11+100+18.43)=8.7%, m
pDMS=100 ÷ (94.11+100+18.43)=47.0%.
(6), each component Theoretical Mass mark: m
aTH(%)=110 ÷ (110+120+25)=43.2%, m
siO2(%)=25 ÷ (110+120+25)=9.7%, m
pDMS(%)=120 ÷ (110+120+25)=47.1%.
The silicon rubber insulator of certain component of embodiment 3 (PDMS is 120 parts, and ATH is 160 parts, and white carbon is 25 parts), the computing method of its component, comprise the following steps:
(1), to measure silicon rubber thermal weight loss rate in 20 ~ 360 DEG C with analysis software be 17.35%, and in 360 ~ 700 DEG C, silicon rubber thermal weight loss rate is 32.81%.
(2), measure at 20 ~ 360 DEG C of PDMS, ATH, SiO with analysis software
2thermal weight loss rate be respectively 2.85%, 30.49%, 1.81%, equation can be obtained 1.: 17.35%=(m
aTH× 30.49%+100 × 2.85%+m
siO2× 1.81%)/(m
aTH+ 100+m
siO2).
(3), measure at 360 ~ 700 DEG C of PDMS, ATH, SiO with analysis software
2thermal weight loss rate be respectively 77.22%, 5.17%, 0.67%, equation can be obtained 2.: 32.81%=(m
aTH× 5.17%+100 × 77.22%+m
siO2× 0.67%)/(m
aTH+ 100+m
siO2).
(4), 2. 1. solving equation group obtain: m
aTH=135.71, m
siO2=21.47.
(5), each constituent mass mark is calculated: m
aTH(%)=135.71 ÷ (135.71+100+21.47)=52.7%, m
siO2(%)=18.87 ÷ (135.71+100+21.47)=8.4%, m
pDMS=100 ÷ (135.71+100+21.47)=38.9%.
(6), each component Theoretical Mass mark: m
aTH(%)=160 ÷ (160+120+25)=52.4%, m
siO2(%)=25 ÷ (160+120+25)=8.3%, m
pDMS(%)=120 ÷ (160+120+25)=39.3%.
Table 1 different component silicon rubber insulator component concentration calculated value.
In embodiment, at 20 ~ 360 DEG C, △ m
aTHvalue is 30.49% ± 0.33%, △ m
pDMSvalue is 2.85% ± 0.2%, △ m
siO2value is 1.81% ± 0.31%; At 360 ~ 700 DEG C, △ m
aTHvalue is 5.17% ± 0.48%, △ m
pDMSvalue is 77.22% ± 1.07%, △ m
siO2value is 0.67 ± 0.48%; Calculate gained ATH, SiO
2, PDMS massfraction effective error is ± 1%.
The invention provides one utilizes thermogravimetry (TG) and differential thermal analysis coupling (TG-DTA) to measure the method for Main Components content in silicon rubber compound insulator.Ultra-high-tension power transmission line silicon rubber compound insulator component comprises: methyl vinyl silicone rubber (PDMS), white carbon (SiO
2), aluminium hydroxide (ATH), three's quality raises with temperature linearity and the curve (TG curve) of change has marked difference in different temperatures scope, see Fig. 8, white carbon is weightless hardly in 20 ~ 700 DEG C, the thermal decomposition weightlessness of ATH occurs in 220 ~ 320 DEG C, and the thermal decomposition weightlessness of PDMS occurs in 350 ~ 600 DEG C.The present invention utilizes the thermal weight loss rate of three kinds of components in respective particular thermal decomposition temperature interval, calculates the content of silicon rubber compound insulator three kinds of components, and gives concrete computing method.
Meanwhile, the present invention has following several defect to have to be solved: 1, thermal analyzer built-in electronic accuracy of balance is high, load-carrying is low, and the quality that sample is put in single measurement is few, and locality is obvious; 2, thermal analysis system is highly sensitive, requires to be no more than 2% to three measurement errors of same sample, otherwise, calculate acquired results under-represented.
Claims (3)
1. one kind measures PDMS, SiO in silicon rubber compound insulator
2, ATH content thermal analysis system, it is characterized in that comprising the following steps:
The Thermal Synthetic Analysis instrument of S1 TG-DTA coupling measures three PDMS, ATH, SiO respectively
2thermal weight loss (TG) curve, to three times measure data average;
S2 cuts three positions at random to silicon rubber insulator, and each position size is 1cm × 1cm, and quality, in 5 ~ 50mg, after pretreatment, records three silicon rubber insulator thermal weight loss (TG) curves, averages to the data that three times are measured;
S3 calculates PDMS, ATH, SiO within the scope of 20 ~ 360 DEG C and 360 ~ 700 DEG C according to thermal weight loss (TG) curve analysis software
2, silicon rubber insulator thermal weight loss rate;
S4 substitutes into thermal weight loss rate △ M formula (1) of silicon rubber insulator according to step S3 institute value:
△M＝(m
ATH×△m
ATH+m
PDMS×△m
PDMS+m
SiO2×△m
SiO2)/(m
ATH+m
PDMS+m
SiO2)--------------(1)；
Wherein: △ M is the thermal weight loss rate of silicon rubber insulator, be given value;
△ m
aTH, △ m
pDMS, △ m
siO2be respectively ATH, PDMS and SiO
2in the thermal weight loss rate of relevant temperature scope, it is also given value;
M
aTH, m
pDMS, m
siO2be respectively ATH, PDMS and SiO in silicon rubber insulator
2quality, be unknown number;
The equation of S5 solution procedure S4, calculates ATH, SiO
2relative to the relative content of PDMS.
2. PDMS, SiO in mensuration silicon rubber compound insulator according to claim 1
2, ATH content thermal analysis system, it is characterized in that: the heating rate of the Thermal Synthetic Analysis instrument of described step S1 is 10k/min, and work atmosphere is air, and working temperature is at 20 ~ 700 DEG C.
3. PDMS, SiO in mensuration silicon rubber compound insulator according to claim 1 and 2
2, ATH content thermal analysis system, it is characterized in that:
Pre-service in described step S2 refers to: sample 3 parts clean up after, be placed in electrically heated drying cabinet, at 50 ~ 100 DEG C dry 10 ~ 14 hours, transfer in drying cupboard after taking-up and place; During test, sample is taken out, be trimmed to granularity and be less than 2mm.
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| CN113030168A (en) * | 2021-03-18 | 2021-06-25 | 国网河北省电力有限公司电力科学研究院 | Silicon rubber material quality evaluation method based on TGA-FTIR |
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