CN112525763A - Method for detecting residual quantity of crosslinking by-products - Google Patents
Method for detecting residual quantity of crosslinking by-products Download PDFInfo
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- CN112525763A CN112525763A CN201910887879.9A CN201910887879A CN112525763A CN 112525763 A CN112525763 A CN 112525763A CN 201910887879 A CN201910887879 A CN 201910887879A CN 112525763 A CN112525763 A CN 112525763A
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- 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
Abstract
A method for detecting residual amounts of crosslinking byproducts, the method comprising the steps of: degassing the crosslinked cable insulation wire core to obtain a degassed insulation wire core; intercepting a section of degassed insulated wire core as a sample, performing annular slicing along the circumference of the sample, then sampling along the radial direction of the insulating layer to obtain sample wafers at different positions of the insulating layer, and placing the sample wafers in a constant temperature and humidity environment; putting the sample into a thermal weight loss analyzer for detection, setting the detection time, quickly raising the detection temperature to the set temperature, and obtaining a time-dependent change curve of the mass of the sample at the set temperature through the thermal weight loss analyzer; and calculating the loss quality of the sample wafer through the change curve to detect the residual quantity of the crosslinking by-products at different positions of the insulating layer, and further verifying the degassing effect. The method for detecting the residual quantity of the crosslinking by-products has the advantages of accurate detection result and capability of detecting the degassing effect at different positions in the insulating layer.
Description
Technical Field
The invention relates to the field of cable manufacturing, in particular to a method for detecting residual quantity of a crosslinking byproduct.
Background
The insulating material of the high-voltage cross-linked polyethylene insulated cable is subjected to cross-linking reaction in the production process, so that the insulating material is converted from a thermoplastic material with a linear structure into a thermosetting material with a net structure, and the operating temperature of the cable is increased. However, during the crosslinking reaction, various crosslinking byproducts such as methane, water, cumyl alcohol, acetophenone and the like are generated, and the crosslinking byproducts are volatile substances and seriously affect the insulation quality of the cable. In order to reduce the influence of the crosslinking by-products on the insulation performance of the cable, degassing after the insulation production of the high-voltage cable is an essential process. The insulated wire core is typically placed in an oven for several days or even tens of days to eliminate by-products of the crosslinking reaction.
As the voltage level increases, the thickness of the insulation gradually increases and the time required for de-gassing increases. If the degassing time is too long, unnecessary energy consumption waste is caused, and the production efficiency is reduced. Too short degassing time can lead to insufficient removal of the crosslinked product and affect the quality of the cable, so an effective method for detecting the removal effect of the crosslinked product is urgently needed to verify the degassing effect, guide the degassing process and guarantee the quality of the cable. At present, a scientific and effective test method is lacked for detecting the degassing effect, and quantitative analysis cannot be carried out. The degassing time is usually prolonged to ensure the sufficient removal of the crosslinking by-products, and although the cable quality is ensured, the disadvantages of increasing energy consumption, prolonging delivery cycle and the like exist.
Disclosure of Invention
In view of the above, it is desirable to provide a method for detecting the residual amount of crosslinking byproducts, which can detect the outgassing effect at different positions in the insulating layer with accurate detection results.
One embodiment of the present invention provides a method for detecting a residual amount of a crosslinking byproduct, which is used for detecting a residual amount of a crosslinking byproduct in a crosslinked electrical-crosslinked insulated wire core, wherein the insulated wire core comprises an insulating layer, and the method comprises the following steps:
step 1, degassing a crosslinked cable insulating wire core to obtain a degassed insulating wire core;
step 3, putting the sample wafer into a thermal weight loss analyzer for detection, setting detection time, quickly raising the detection temperature to the set temperature, and obtaining a time-dependent change curve of the sample wafer quality at the set temperature through the thermal weight loss analyzer;
and 4, calculating the loss quality of the sample wafer through the change curve to detect the residual quantity of the crosslinking by-products at different positions of the insulating layer, and further verifying the degassing effect.
Further, the sampling in step 2 comprises the following steps: intercepting one section the insulating core, along the circumference of insulating core carries out the hoop and cuts into slices and obtains first sample piece, then along first sample piece radially will the insulating layer divides into a plurality of sample layers in proper order to sample along each sample layer circumferencial direction and obtain the second sample piece.
Further, the number of the sampling layers is at least 3.
Further, the thickness of the first sample wafer ranges from 1mm to 2 mm.
Furthermore, the number of the second sample slices obtained by sampling each sampling layer is at least 3.
Further, the mass of the second sample is in the range of 15mg to 25 mg.
Further, the set temperature range in the step 4 is 170 ℃ to 180 ℃.
Further, the set time duration in the step 4 ranges from 20min to 40 min.
Further, the temperature range of the constant temperature and humidity environment in the step 2 is 15 ℃ to 25 ℃, and the humidity range is 45% to 60%.
Further, the calculation in step 4 includes the following steps: the number of the second sample wafers obtained by sampling each sampling layer is n, the initial mass of each second sample wafer is W1, the mass after thermal weight loss analysis and heating stabilization is W2, and the average value A of the residual quantity of the crosslinking reaction byproducts of the crosslinking cables of each sampling layer is calculated by the following formula: a ═ [ (W1-W2)/W1 × 100% ]/n.
In the method for detecting the residual quantity of the crosslinking by-products, the precision of the detection result obtained by the thermal weight loss analyzer is high, the small change of the quality of the sample can be accurately recorded, and the detection accuracy is improved. In the detection process, the quality change condition of the sample can be continuously and automatically read and recorded, and the influence of manual operation on the detection result is reduced, so that the detection accuracy is improved. By means of circumferential slicing along the circumference of the sample and then sampling along the radial position of the insulating layer, the residual quantity of the cross-linking by-products at different positions of the insulating layer is accurately detected, and the degassing effect of the cable is comprehensively reflected.
Drawings
FIG. 1 is a schematic flow chart of a method for detecting a residual amount of a crosslinking byproduct according to an embodiment of the present invention.
Fig. 2 is a structural diagram of an insulated wire core in an embodiment of the present invention.
Fig. 3 is a graph illustrating a variation in mass of the second sampling layer pattern 2 according to an embodiment of the present invention.
Fig. 4 is a graph showing a mass change of the third sampling layer pattern 2 according to another embodiment of the present invention.
Description of the main elements
| Insulated wire core | 100 |
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10 |
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20 |
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30 |
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31 |
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32 |
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33 |
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40 |
The following detailed description will further illustrate the invention in conjunction with the above-described figures.
Detailed Description
So that the manner in which the above recited objects, features and advantages of embodiments of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to the embodiments thereof which are illustrated in the appended drawings. In addition, the features of the embodiments of the present application may be combined with each other without conflict.
In the following description, numerous specific details are set forth to provide a thorough understanding of embodiments of the invention, some, but not all embodiments of the invention. All other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort belong to the protection scope of the embodiments of the present invention.
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 embodiments of the present invention belong. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of embodiments of the invention.
Referring to fig. 1 and fig. 2, a method for detecting a residual amount of a crosslinking byproduct is used to detect residual amounts of crosslinking byproducts at different positions in a crosslinked cable, so as to analyze a degassing effect of the crosslinked cable, and the method for detecting a residual amount of a crosslinking byproduct specifically includes the following steps:
s1, degassing the crosslinked cable insulated wire core to obtain a degassed insulated wire core 100;
specifically, the crosslinked cable is placed in a drying room for degassing treatment to obtain the degassed insulated wire core 100. The degassed insulated wire core 100 comprises a conductor 10, a conductor shielding layer 20, an insulating layer 30 and an insulated shielding layer 40 which are sequentially arranged from inside to outside.
S2, sampling the degassed insulated wire core 100, and placing the sample wafer in a constant temperature and humidity environment;
specifically, a section of the insulated wire core 100 is cut, and a circumferential slice is performed along the circumference of the insulated wire core 100 sample to obtain a first sample. Preferably, the thickness of the first sample ranges from 1mm to 2 mm. Then along the first sample piece radially will insulating layer 30 divides into a plurality of sample layers to evenly sample along each sample layer circumferencial direction and obtain a plurality of second sample pieces, in order to avoid because the cross-linking accessory substance is in the error that insulating layer 30 maldistribution leads to, and then the accurate detection the residual amount of the different positions cross-linking accessory substance of insulating core 100. Preferably, the number of sampling layers is at least 3; the number of the second sample wafers obtained by sampling of each sampling layer is at least 3; the mass of each of the second sample pieces ranges from 15mg to 25 mg. The environment of constant temperature and constant humidity includes constant temperature and constant humidity, the constant temperature scope is 15 ℃ to 25 ℃, the constant humidity scope is 45% to 60%. The environment of constant temperature and humidity is used for preventing insulating sinle silk 100 from weing and excessively drying, improves the accuracy of testing result.
In one embodiment, the insulating layer 30 is divided into a first sampling layer 31, a second sampling layer 32 and a third sampling layer 33 from inside to outside. And respectively sampling the first sampling layer 31, the second sampling layer 32 and the third sampling layer 33 to obtain second sample wafers, wherein the number of the second sample wafers obtained by sampling each sampling layer is 3.
And S3, sequentially placing the second sample wafers into a thermal weight loss analyzer for detection, rapidly increasing the detection temperature to a set temperature, setting the detection time, and obtaining the change curve of the mass of each second sample wafer along with the time at the set temperature through the thermal weight loss analyzer.
Specifically, after the second sample is prepared, the second sample is rapidly placed into a thermal weight loss analyzer for detection, so that the placing time is shortened, and the measurement error caused by volatilization of the crosslinking by-products is prevented. The set temperature range is 170 ℃ to 180 ℃ to accelerate the volatilization speed of the crosslinking by-products in the second sample wafer, thereby reducing the detection time. The set time range is 20min to 40 min. The thermal weight loss analyzer is an instrument for detecting the mass change relation of substances by using a thermogravimetric method. Thermogravimetry is the measurement of the mass of a substance as a function of time at a programmed temperature. The precision of the detection result obtained by the thermal weight loss analyzer is high, the small change of the sample quality can be accurately recorded, and the detection accuracy is improved. In the detection process, the quality change condition of the sample can be continuously and automatically read and recorded, and the influence of manual operation on the detection result is reduced.
And S4, calculating the lost quality of the second sample through the change curve to detect the residual quantity of the crosslinking by-products at different positions of the insulating layer.
Specifically, in the detection process, the crosslinking by-product in the second sample wafer gradually volatilizes at the set temperature until the quality is gradually stable, and the mass lost by the second sample wafer is the residual amount of the crosslinking by-product. And calculating the percentage of the residual quantity of the cross-linking by-products of each second sample wafer, and calculating the average value of the percentage of the residual quantity of the cross-linking by-products of the second sample wafer of each sampling layer, wherein the average value can reflect the residual quantity of the cross-linking by-products at different positions in the insulating layer 30. The calculation specifically comprises the following steps that the number of second sample wafers obtained by sampling each sampling layer is n, the initial mass of each second sample wafer is W1, the mass after the thermal weight loss analysis and the heating stabilization is W2, and the average value A of the residual quantity of the crosslinking reaction byproducts of the crosslinking cables of each sampling layer is calculated through the following formula: a ═ [ (W1-W2)/W1 × 100% ]/n. The smaller the average value A, the better the degassing effect, and on the contrary, the larger the average value A, the worse the degassing effect. And then the degassing effect of the cable is comprehensively reflected through the average value, and the optimization of the degassing process is guided.
The technical solution of the present invention will be further described in detail with reference to the following specific examples.
Example 1
Selecting 110kV high-voltage crosslinked polyethylene insulated cable cores, and placing the 110kV high-voltage crosslinked polyethylene insulated cable cores into a drying room for degassing treatment, wherein the degassing treatment time is 4 days. Intercepting one section 110kV high pressure crosslinked polyethylene insulated cable sinle silk, along the circumference of 110kV high pressure crosslinked polyethylene insulated cable sinle silk carries out the hoop and cuts into slices and obtains first sample wafer, the thickness of first sample wafer is 1 mm. Then, the insulating layer is divided into 3 sampling layers along the radial direction of the first sample wafer, the 3 sampling layers are respectively sampled to obtain second sample wafers, the number of the second sample wafers obtained by sampling each sampling layer is 3, and the second sample wafers are respectively a sample 1, a sample 2 and a sample 3. And the sample 1, the sample 2 and the sample 3 were placed in a constant temperature and humidity environment. And sequentially placing each sample into a thermal weight loss analyzer for detection, rapidly increasing the detection temperature to 175 ℃, wherein the detection time is 30min, and obtaining a time-dependent change curve of the mass of each sample at a set temperature through the thermal weight loss analyzer.
Referring to fig. 3, fig. 3 is a continuous variation curve of the mass of the second sampling layer sample 2 with time, the crosslinking by-product gradually volatilizes during the testing process, the mass of the sample 2 gradually becomes stable in about 15min, the initial mass W1 of the second sampling layer sample 2 is 18.8107578mg, the residual mass W2 is 18.7548mg, and the mass lost by the second sampling layer sample 2 in the testing time is 0.0559578mg, so that the percentage of the mass lost by the second sampling layer sample 2 in the testing time is 0.3001% by calculation, and the residual amount of the volatilized crosslinking by-product is 0.3001%. The change rule of the quality of other samples along with time is similar to that of the sample 2 of the second sampling layer, and the description is omitted.
Table 1 shows the crosslinking by-product test results. From Table 1, the percent by-product residual cross-linking over the test time for all second coupons can be seen. Specifically, the average value of the first sampling layer is 0.4691%, the average value of the second sampling layer is 0.3079%, and the average value of the third sampling layer is 0.2833%. Therefore, the degassing effect of different positions of the insulating layer of the 110kV high-voltage crosslinked polyethylene insulated cable core is better than that of the second sampling layer, and the degassing effect of the second sampling layer is better than that of the first sampling layer.
TABLE 1
Example 2
Selecting 110kV high-voltage crosslinked polyethylene insulated cable cores, and placing the 110kV high-voltage crosslinked polyethylene insulated cable cores into a drying room for degassing treatment, wherein the degassing treatment time is 7 days. Intercepting one section 110kV high pressure crosslinked polyethylene insulated cable sinle silk, along the circumference of 110kV high pressure crosslinked polyethylene insulated cable sinle silk carries out the hoop and cuts into slices and obtains first sample wafer, the thickness of first sample wafer is 1 mm. Then, the insulating layer is divided into 3 sampling layers along the radial direction of the first sample wafer, the 3 sampling layers are respectively sampled to obtain second sample wafers, the number of the second sample wafers obtained by sampling each sampling layer is 3, and the second sample wafers are respectively a sample 1, a sample 2 and a sample 3. And the sample 1, the sample 2 and the sample 3 were placed in a constant temperature and humidity environment. And sequentially placing each sample into a thermal weight loss analyzer for detection, rapidly increasing the detection temperature to 175 ℃, wherein the detection time is 30min, and obtaining a time-dependent change curve of the mass of each sample at a set temperature through the thermal weight loss analyzer.
Referring to fig. 4, fig. 4 is a continuous variation curve of the mass of the third sampling layer sample 2 with time, the crosslinking by-product gradually volatilizes during the testing process, the mass of the sample 2 gradually stabilizes at about 16min, the initial mass W1 of the third sampling layer sample 2 is 20.5618486mg, the mass lost by the third sampling layer sample 2 during the testing time is 0.0379486mg, and the residual mass W2 is 20.5239mg, so that the percentage of the mass lost by the third sampling layer sample 2 during the testing time is 0.1846% by calculation, and the residual amount of the volatilized crosslinking by-product is 0.1846%. The change rule of the quality of the rest second sample wafers along with the time is similar to that of the sample wafer 2 of the third sampling layer, and the description is omitted.
Table 2 shows the crosslinking by-product test results. From Table 2, the percent by-product residual cross-linking over the test time for all second coupons can be seen. Specifically, the average value of the first sampling layer is 0.2481%, the average value of the second sampling layer is 0.2231%, and the first average value of the third sampling layer is 0.1980%. Therefore, the degassing effect of different positions of the insulating layer of the 110kV high-voltage crosslinked polyethylene insulated cable core is better than that of the second sampling layer, and the degassing effect of the second sampling layer is better than that of the first sampling layer.
TABLE 2
In the method for detecting the residual quantity of the crosslinking byproducts, a section of the insulating wire core 100 is intercepted in a constant-temperature and constant-humidity environment, a circumferential slice is carried out along the circumference of the insulating wire core 100 to obtain a first sample wafer and samples are taken along the circumferential direction of each sampling layer, so that the residual quantity of the crosslinking byproducts at different positions of the insulating layer 30 is accurately detected, and the degassing effect of the cable is comprehensively reflected. The precision of the detection result obtained by the thermal weight loss analyzer is high, the small change of the sample quality can be accurately recorded, and the detection accuracy is improved. In the detection process, the quality change condition of the sample can be continuously and automatically read and recorded, and the influence of manual operation on the detection result is reduced.
Although the embodiments of the present invention have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the embodiments of the present invention.
Claims (10)
1. A method for detecting the residual quantity of a crosslinking byproduct is used for detecting the residual quantity of the crosslinking byproduct in a crosslinking electric-linked insulated wire core, wherein the insulated wire core comprises an insulating layer, and the method is characterized by comprising the following steps:
step 1, degassing a crosslinked cable insulating wire core to obtain a degassed insulating wire core;
step 2, intercepting a section of degassed insulated wire core as a sample, performing annular slicing along the circumference of the sample, then sampling along the radial direction of the insulating layer to obtain sample wafers at different positions of the insulating layer, and placing the sample wafers in a constant temperature and humidity environment;
step 3, putting the sample wafer into a thermal weight loss analyzer for detection, setting detection time, quickly raising the detection temperature to the set temperature, and obtaining a time-dependent change curve of the sample wafer quality at the set temperature through the thermal weight loss analyzer;
and 4, calculating the loss quality of the sample wafer through the change curve to detect the residual quantity of the crosslinking by-products at different positions of the insulating layer, and further verifying the degassing effect.
2. The method for detecting the residual amount of the crosslinking by-products according to claim 1, wherein the sampling in the step 2 comprises the steps of: intercepting one section the insulating core, along the circumference of insulating core carries out the hoop and cuts into slices and obtains first sample piece, then along first sample piece radially will the insulating layer divides into a plurality of sample layers in proper order to sample along each sample layer circumferencial direction and obtain the second sample piece.
3. The method according to claim 2, wherein the number of the sampling layers is at least 3.
4. The method of claim 3, wherein the thickness of the first sample is in the range of 1mm to 2 mm.
5. The method according to claim 2, wherein the number of the second samples obtained by sampling each sampling layer is at least 3.
6. The method of claim 5, wherein the mass of the second sample is in a range of 15mg to 25 mg.
7. The method according to claim 1, wherein the temperature set in step 4 is in the range of 170 ℃ to 180 ℃.
8. The method for detecting the residual amount of the crosslinking by-products according to claim 1, wherein the set time period in the step 4 is in a range of 20min to 40 min.
9. The method for detecting the residual amount of the crosslinking by-products according to claim 1, wherein the temperature of the constant temperature and humidity environment in the step 2 is in a range of 15 ℃ to 25 ℃, and the humidity is in a range of 45% to 60%.
10. The method for detecting the residual amount of the crosslinking by-products according to claim 2, wherein the calculation in the step 4 comprises the steps of: the number of the second sample wafers obtained by sampling in each sampling layer is n, and the initial mass of each second sample wafer is W1The mass after the thermal weight loss analysis and the heating stabilization is W2Calculating the cross-linking of the cross-linked cable of each sampling layer by the following formulaAverage value of residual amount of co-reaction by-products a: a ═ W [ [ (W)1-W2)/W1×100％]/n。
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