CN114062189B - Method for measuring content of rubber in silicon rubber - Google Patents
Method for measuring content of rubber in silicon rubber Download PDFInfo
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- CN114062189B CN114062189B CN202111360824.6A CN202111360824A CN114062189B CN 114062189 B CN114062189 B CN 114062189B CN 202111360824 A CN202111360824 A CN 202111360824A CN 114062189 B CN114062189 B CN 114062189B
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 155
- 238000000034 method Methods 0.000 title claims abstract description 50
- 229920001971 elastomer Polymers 0.000 title claims abstract description 49
- 239000005060 rubber Substances 0.000 title claims abstract description 49
- 239000004945 silicone rubber Substances 0.000 claims abstract description 118
- 238000006243 chemical reaction Methods 0.000 claims abstract description 69
- 238000005336 cracking Methods 0.000 claims abstract description 45
- 238000002411 thermogravimetry Methods 0.000 claims abstract description 43
- 239000003054 catalyst Substances 0.000 claims abstract description 33
- 239000003292 glue Substances 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 42
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 17
- 239000000919 ceramic Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 11
- 238000003776 cleavage reaction Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 9
- 238000006297 dehydration reaction Methods 0.000 claims description 9
- 230000002378 acidificating effect Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 230000007017 scission Effects 0.000 claims description 2
- 239000002253 acid Substances 0.000 description 12
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 9
- 239000012212 insulator Substances 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 7
- 239000004570 mortar (masonry) Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- 238000010008 shearing Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 230000004580 weight loss Effects 0.000 description 6
- -1 dimethyl siloxane Chemical class 0.000 description 5
- 239000011256 inorganic filler Substances 0.000 description 5
- 229910003475 inorganic filler Inorganic materials 0.000 description 5
- 239000011241 protective layer Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004200 deflagration Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Abstract
The invention provides a method for measuring the content of rubber in silicon rubber, which comprises the following steps: mixing silicone rubber with the mass of M 0 with a cracking catalyst, and carrying out a cracking reaction to prepare a silicone rubber prefabricated member, wherein the mass of the silicone rubber prefabricated member is M 1; the temperature of the cracking reaction is 160-200 ℃; performing thermogravimetric analysis on the silicone rubber prefabricated part with the mass of m 0, wherein the mass of the silicone rubber prefabricated part after the thermogravimetric analysis is finished is m 1; substituting M 0、M1、m0 and M 1 into an equation to calculate the glue content A; equation isThe measuring method can accurately measure the rubber content in the silicon rubber.
Description
Technical Field
The invention relates to the technical field of electrical materials, in particular to a method for measuring the content of rubber in silicone rubber.
Background
The silicone rubber is a common organic silicon material and is widely applied to various fields of daily necessities, medical treatment, electronics, electricity and the like. In the electric power system, most of umbrella skirt sheaths of composite insulators, insulating layers in cable joints and the like are made of silicon rubber. The silicon rubber applied in the power system comprises high-temperature vulcanized silicon rubber, room-temperature vulcanized silicon rubber, liquid silicon rubber and the like, wherein the liquid silicon rubber is vulcanized by adopting a platinum catalyst, so that the ceramic phenomenon can occur under the high-temperature effect, and the flame retardant effect is effectively achieved.
For some silicone rubber materials used on equipment, the rubber content has a critical effect on performance. For example, in the silicone rubber used in the composite insulator, a large amount of inorganic filler such as aluminum hydroxide is generally added to achieve good tracking resistance and electrical erosion resistance, and these non-reinforced fillers have great influence on the mechanical properties and aging resistance of the silicone rubber, so that after a long period of operation, the silicone rubber body is liable to undergo serious aging phenomena such as cracking and chalking. Aiming at the ageing problem of the silicone rubber material, the rubber content can be used as one of indexes for judging the comprehensive performance of the silicone rubber.
The traditional technology adopts Fourier transform infrared spectrum, density, thermogravimetric analysis and other methods to measure the rubber content, wherein the thermogravimetric analysis method mainly carries out high-temperature pyrolysis on the silicon rubber, and calculates the rubber content according to the weight loss of different decomposition stages. However, the conventional thermogravimetric analysis method is only aimed at a large amount of high-temperature vulcanized silicone rubber using a composite insulator, and the accuracy of the measurement result of the gel content of the ceramic silicone rubber by the thermogravimetric analysis method is low, so that the application of the method is limited.
Disclosure of Invention
Based on the above, the invention provides a method for measuring the rubber content in the silicone rubber, which can accurately measure the rubber content in the silicone rubber.
The invention is realized by the following technical scheme.
A method for measuring the content of rubber in silicon rubber comprises the following steps:
Mixing silicone rubber with the mass of M 0 with a cracking catalyst, and carrying out a cracking reaction to prepare a silicone rubber prefabricated member, wherein the mass of the silicone rubber prefabricated member is M 1; the temperature of the cracking reaction is 160-200 ℃;
performing thermogravimetric analysis on the silicone rubber prefabricated part with the mass of m 0, wherein the mass of the silicone rubber prefabricated part after the thermogravimetric analysis is finished is m 1;
Substituting M 0、M1、m0 and M 1 into an equation to calculate the glue content A;
the equation is
In one embodiment, the silicone rubber is selected from the group consisting of ceramic silicone rubbers.
In one embodiment, the cracking catalyst is an acidic catalyst or a basic catalyst.
In one embodiment, the acid is selected from at least one of sulfonic acid and sulfuric acid.
In one embodiment, the base is selected from potassium hydroxide.
In one embodiment, the method further comprises the following steps before mixing the silicone rubber with mass M 0 with the cracking catalyst: the silicone rubber with mass M 0 was dehydrated.
In one embodiment, the temperature of dehydration is 80 ℃ to 110 ℃; the dehydration time is 0.3 h-0.8 h.
In one embodiment, the thermogravimetric analysis conditions are: the atmosphere is nitrogen; the gas flow is 20 mL/min-50 mL/min; the heating rate is 5 ℃/min to 20 ℃/min; the heating temperature is 25-1100 deg.c.
In one embodiment, the time for the cleavage reaction is from 0.5h to 1h.
In one embodiment, the temperature of the cleavage reaction is 150℃to 250 ℃.
Compared with the prior art, the method for measuring the rubber content in the silicone rubber has the following beneficial effects:
According to the method for measuring the rubber content in the silicone rubber, disclosed by the invention, the silicone rubber is subjected to cracking reaction before thermogravimetric analysis, the cracking reaction temperature is limited to 160-200 ℃, and the silicone rubber prefabricated member with the main body of inorganic filler is obtained, so that a compact protective layer does not appear in the silicone rubber prefabricated member in the thermogravimetric analysis process, the silicone rubber prefabricated member is decomposed relatively thoroughly in the thermogravimetric analysis process, and a relatively accurate rubber content result is finally obtained.
Drawings
Fig. 1 is a silicone rubber preform provided by an embodiment of the present invention.
Detailed Description
In order that the invention may be readily understood, a more particular description of the invention will be rendered by reference to specific embodiments that are illustrated in the appended drawings. Preferred embodiments of the present invention are shown in the examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise. In the description of the present invention, the meaning of "several" means at least one, such as one, two, etc., unless specifically defined otherwise.
The words "preferably," "more preferably," and the like in the present invention refer to embodiments of the invention that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values for the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
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. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The invention provides a method for measuring the content of rubber in silicon rubber, which comprises the following steps:
Mixing silicone rubber with the mass of M 0 with a cracking catalyst, and carrying out a cracking reaction to prepare a silicone rubber prefabricated member, wherein the mass of the silicone rubber prefabricated member is M 1; the temperature of the cracking reaction is 160-200 ℃;
Performing thermogravimetric analysis on the silicone rubber prefabricated part with the mass of m 0, wherein the mass of the silicone rubber prefabricated part after the thermogravimetric analysis is finished is m 1;
substituting M 0、M1、m0 and M 1 into an equation to calculate the glue content A;
Equation is
In one specific example, the temperature of the cleavage reaction includes, but is not limited to 160℃、161℃、162℃、 163℃、164℃、165℃、166℃、167℃、168℃、169℃、170℃、171℃、172℃、173℃、174℃、175℃、176℃、177℃、178℃、179℃、180℃、181℃、182℃、 183℃、184℃、185℃、186℃、187℃、188℃、189℃、190℃、191℃、192℃、 193℃、194℃、195℃、196℃、197℃、198℃、199℃ and 200 ℃.
Thermogravimetric analysis, also known as thermogravimetric analysis, refers to a method of measuring the mass of a substance at a programmed temperature in relation to temperature or time, by analyzing the thermogravimetric curve, it is possible to know the information associated with the mass, such as composition of the sample and possibly of the intermediate product produced, thermal stability, thermal decomposition conditions, and the product produced. The thermal gravimetric analysis is carried out on the silicon rubber by carrying out thermal pyrolysis, the content of the rubber contained in the silicon rubber is calculated according to the weight loss of different decomposition stages, and the method is accurate relative to an infrared spectrum, density and other analysis methods, however, the accuracy has a certain limitation, and for the silicon rubber which can be ceramic in a high-temperature environment and form a compact protective layer, the silicon rubber is not completely decomposed due to the fact that a large amount of cross links are integrally formed in the thermal gravimetric analysis process, so that the accuracy of the rubber content calculation result is obviously reduced.
The inventor finds that the silicon rubber prefabricated member with the main body of inorganic filler can be obtained by carrying out cracking reaction on the silicon rubber and limiting the cracking reaction temperature to 160-200 ℃, and the silicon rubber prefabricated member can not be ceramic or have a compact protective layer in the thermogravimetric analysis process, so that the decomposition is relatively thorough, and the accurate rubber content result is finally obtained.
It will be appreciated that in the present invention, the higher the measured gum content, the more accurate, since the ceramic silicone rubber of the inner layer is protected by the ceramic layer in thermogravimetric experiments, and is not easily decomposed completely. The cracking effect is to decompose part of the siloxane in advance by using a chemical means, so that the residual silicone rubber can be fully decomposed by heating in a thermogravimetric experiment. According to the method for measuring the rubber content in the silicone rubber, disclosed by the invention, the silicone rubber is subjected to cracking reaction before thermogravimetric analysis, the cracking reaction temperature is limited to 160-200 ℃, and the silicone rubber prefabricated member with the main body of inorganic filler is obtained, so that a compact protective layer does not appear in the silicone rubber prefabricated member in the thermogravimetric analysis process, the silicone rubber prefabricated member is decomposed relatively thoroughly in the thermogravimetric analysis process, and a relatively accurate rubber content result is finally obtained.
In a specific example, the temperature of the cleavage reaction is 150℃to 250 ℃. It is understood that in the present invention, the temperature of the cleavage reaction includes, but is not limited to 150℃、155℃、160℃、165℃、170℃、 171℃、172℃、173℃、174℃、175℃、176℃、177℃、178℃、179℃、180℃、 181℃、182℃、183℃、184℃、185℃、186℃、187℃、188℃、189℃、190℃、 195℃、200℃、205℃、210℃、215℃、220℃、225℃、230℃、235℃、240℃、 245℃ and 250 ℃.
Too low a cracking reaction temperature can lead to too slow reaction, too high a cracking reaction temperature can increase unnecessary energy consumption, and reach the flash point of a decomposed product DMC, so that deflagration is easy to occur, and safety accidents are caused.
In a specific example, the time of the cleavage reaction is 0.5h to 1h. It is understood that in the present invention, the time of the cleavage reaction includes, but is not limited to, 0.5h, 0.6h, 0.7h, 0.8h, 0.9h, 1.0h.
In a specific example, the silicone rubber is selected from ceramic silicone rubbers.
In a specific example, the cleavage catalyst is an acidic catalyst or a basic catalyst.
It will be appreciated that in the present invention, the components of the silicone rubber material include a filler that reacts with the acidic catalyst, and the cracking catalyst is an alkaline wash catalyst. More specifically, the filler capable of reacting with the acidic catalyst includes at least one of a hydroxide and a carbonate.
In a specific example, the acid is selected from at least one of sulfonic acid and sulfuric acid.
In a specific example, the acid is a sulfonic acid.
In one specific example, the acid is sulfuric acid. More specifically, the acid is concentrated sulfuric acid.
In a more specific example, the acid is a mixture of sulfonic acid and concentrated sulfuric acid.
In a specific example, the base is selected from potassium hydroxide.
In a specific example, the method further comprises the following steps before mixing the silicone rubber with mass M 0 with the cracking catalyst: the silicone rubber with mass M 0 was dehydrated.
The purpose of dehydrating the silicone rubber is to remove trace moisture absorbed by the silicone rubber in natural environment, and the dehydration link is required to ensure that the catalytic effect of the concentrated sulfuric acid is not affected because the water absorption of the adopted acid (the concentrated sulfuric acid) is very strong.
In one specific example, the temperature of dehydration is from 80 ℃ to 110 ℃.
It is understood that in the present invention, the temperature of dehydration includes, but is not limited to 80℃、81℃、82℃、 83℃、84℃、85℃、86℃、87℃、88℃、89℃、90℃、91℃、92℃、93℃、94℃、 95℃、96℃、97℃、98℃、99℃、100℃、101℃、102℃、103℃、104℃、105℃、 106℃、107℃、108℃、109℃ and 110 ℃.
In a specific example, the time for dehydration is from 0.3h to 0.8h.
It is understood that the time for dehydration includes, but is not limited to 0.3h、0.35h、0.4h、0.45h、0.46h、 0.47h、0.48h、0.49h、0.5h、0.51h、0.52h、0.53h、0.54h、0.55h、0.6h、0.65h、0.7h、0.75h and 0.8 hours.
In one specific example, the conditions for thermogravimetric analysis are: the atmosphere is nitrogen; the gas flow is 20 mL/min-50 mL/min; the heating rate is 5 ℃/min to 20 ℃/min; the heating temperature is 25-1100 deg.c.
It is understood that in the present invention, the conditions of thermogravimetric analysis include, but are not limited to, 20 mL/min、21mL/min、22mL/min、23mL/min、24mL/min、25mL/min、26mL/min、 27mL/min、28mL/min、29mL/min、30mL/min、31mL/min、32mL/min、33 mL/min、34mL/min、35mL/min、36mL/min、37mL/min、38mL/min、39mL/min、 40mL/min、41mL/min、42mL/min、43mL/min、44mL/min、45mL/min、46 mL/min、47mL/min、48mL/min、49mL/min and 50mL/min.
It is understood that in the present invention, the temperature rise rate includes, but is not limited to 5℃ /min、6℃/min、7℃/min、8℃/min、9℃/min、10℃/min、11℃/min、12℃/min、 13℃/min、14℃/min、15℃/min、16℃/min、17℃/min、18℃/min、19℃/min and 20 ℃/min in the conditions of thermogravimetric analysis.
In a more specific example, the method for measuring the rubber content in the silicone rubber comprises the following steps:
After shearing the silicone rubber umbrella skirt, weighing mass M 0, placing into a reaction container, heating to 80-110 ℃, and dehydrating for 0.3-0.8 h;
Adding a cracking catalyst into the reaction vessel, wherein the cracking catalyst is an acid catalyst or a basic catalyst, more specifically, the cracking catalyst is at least one of sulfonic acid and concentrated sulfuric acid, or potassium hydroxide; heating to 160-200 ℃, continuously stirring to react, and pumping volatile components generated by the reaction by a vacuum pump;
stopping heating after the reaction is almost completed, naturally cooling the reaction vessel, taking out the silicone rubber prefabricated part from the reaction vessel, and weighing the mass M 1 of the silicone rubber prefabricated part to remove most of inorganic matters of siloxane;
grinding the silicone rubber prefabricated part into uniform fine powder by using a mortar, and then placing the mass m 0 into a thermal weight loss analyzer, wherein the reaction atmosphere is set to be nitrogen, and the gas flow is 20-50 mL/min; the heating rate is 5 ℃/min to 20 ℃/min; the heating temperature interval is 25-1100 ℃, and the final stable mass m 1 is recorded.
Substituting M 0、M1、m0 and M 1 into the equationThe gum content in the silicone rubber was calculated.
The method for measuring the rubber content in the silicone rubber of the present invention is described in further detail below with reference to specific examples. The raw materials used in the following examples are all commercially available products unless otherwise specified.
Example 1
The embodiment provides a method for measuring the content of rubber in silicone rubber, which comprises the following steps:
step one, cracking the silicon rubber:
(1) Cutting the silicon rubber umbrella skirt of a terminal insulator of a certain cable (samples are provided by manufacturers for recycling waste silicon rubber), weighing the mass M 0 to be 120g, placing the cable into a reaction container, heating to 95 ℃, and dehydrating for 0.5h;
(2) Adding 3g of sulfonic acid and 3g of concentrated sulfuric acid into a reaction vessel as an acid cracking catalyst, heating to 170 ℃, continuously stirring for reaction, and pumping volatile components such as DMC (dimethyl siloxane mixed ring) generated by the reaction by a vacuum pump;
(3) After 1 hour of reaction, the heating was stopped, the reaction vessel was allowed to cool naturally, and the silicone rubber preform, which was an inorganic substance from which most of the siloxane had been removed, was taken out of the reaction vessel, and as shown in FIG. 1, the mass M 1 was 81.6g.
Performing thermogravimetric analysis on the silicone rubber prefabricated part:
Grinding the silicone rubber prefabricated member prepared in the step (I) into uniform fine powder by using a mortar, putting 5.12mg of m 0 mg into a thermal weight loss analyzer, setting the reaction atmosphere to be nitrogen, the gas flow to be 20mL/min, the heating rate to be 10 ℃/min, the heating temperature range to be 25-1100 ℃, and recording the final stable mass m 1 to be 4.83mg.
Step three, calculating the glue content:
Substituting M 0、M1、m0 and M 1 into the equation The rubber content in the silicone rubber provided in this example was calculated to be 35.9%.
Regarding the method for measuring the content of the rubber in the silicone rubber, the higher the content of the rubber is, the more accurate the content of the rubber is generally measured, because the silicone rubber of the inner layer of the ceramic silicone rubber is protected by the ceramic layer in a thermogravimetric experiment, and is not easy to be decomposed completely. The cracking effect is to decompose part of the siloxane in advance by using a chemical means, so that the residual silicone rubber can be fully decomposed by heating in a thermogravimetric experiment.
Example 2
The embodiment provides a method for measuring the content of rubber in silicone rubber, which comprises the following steps:
step one, cracking the silicon rubber:
(1) Selecting a silicone rubber umbrella skirt of the cable terminal insulator as in example 1, shearing, weighing mass M 0 to be 120g, placing into a reaction container, adding 3g of sulfonic acid and 3g of sulfuric acid into the reaction container as acid cracking catalysts, heating to 170 ℃, continuously stirring for reaction, and pumping volatile components such as DMC (dimethyl siloxane mixed ring) generated by the reaction by a vacuum pump;
(2) After 1 hour of reaction, the heating was stopped, the reaction vessel was allowed to cool naturally, and the silicone rubber preform, which was an inorganic substance from which most of the siloxane had been removed, was taken out of the reaction vessel, and the mass M 1 was 83.2g.
Performing thermogravimetric analysis on the silicone rubber prefabricated part:
Grinding the silicone rubber prefabricated member prepared in the step (I) into uniform fine powder by using a mortar, putting 7.30mg of the mass m 0 into a thermal weightless analyzer, setting the reaction atmosphere to be nitrogen, the gas flow to be 20mL/min, the heating rate to be 10 ℃/min, the heating temperature range to be 25-1100 ℃, and recording the final stable mass m 1 to be 6.92mg.
Step three, calculating the glue content:
Substituting M 0、M1、m0 and M 1 into the equation The rubber content in the silicone rubber provided in this example was calculated to be 34.3%.
Example 3
The embodiment provides a method for measuring the content of rubber in silicone rubber, which comprises the following steps:
step one, cracking the silicon rubber:
(1) Selecting a silicon rubber umbrella skirt of the cable terminal insulator which is the same as that of the embodiment 1, shearing, weighing the mass M 0 to be 120g, placing the silicon rubber umbrella skirt into a reaction container, heating to 95 ℃, and dehydrating for 0.5h;
(2) Adding 3g of sulfonic acid serving as an acid cracking catalyst into a reaction container, heating to 170 ℃, continuously stirring for reaction, and pumping volatile components such as DMC (dimethyl siloxane mixed ring) generated by the reaction by using a vacuum pump;
(3) After 1 hour of reaction, the heating was stopped and the reaction vessel was allowed to cool naturally, and the silicone rubber preform, which was an inorganic substance from which most of the siloxane had been removed, was taken out of the reaction vessel, and its mass M 1 was 95.9g.
Performing thermogravimetric analysis on the silicone rubber prefabricated part:
Grinding the silicone rubber prefabricated member prepared in the step (I) into uniform fine powder by using a mortar, putting 5.73g of m 0 g into a thermal weightless analyzer, setting the reaction atmosphere to be nitrogen, the gas flow to be 20mL/min, the heating rate to be 10 ℃/min, the heating temperature range to be 25-1100 ℃, and recording the final stable mass m 1 to be 4.76g.
Step three, calculating the glue content:
Substituting M 0、M1、m0 and M 1 into the equation The rubber content in the silicone rubber provided in this example was calculated to be 33.6%.
Example 4
The embodiment provides a method for measuring the content of rubber in silicone rubber, which comprises the following steps:
step one, cracking the silicon rubber:
(1) Selecting a silicon rubber umbrella skirt of the cable terminal insulator which is the same as that of the embodiment 1, shearing, weighing the mass M 0 to be 120g, placing the silicon rubber umbrella skirt into a reaction container, heating to 95 ℃, and dehydrating for 0.5h;
(2) Adding 3g of sulfuric acid serving as an acid cracking catalyst into a reaction container, heating to 170 ℃, continuously stirring for reaction, and pumping volatile components such as DMC (dimethyl siloxane mixed ring) generated by the reaction by using a vacuum pump;
(3) After 1 hour of reaction, the heating was stopped, the reaction vessel was allowed to cool naturally, and the silicone rubber preform, which was an inorganic substance from which most of the siloxane had been removed, was taken out of the reaction vessel, and its mass M 1 was 87.2g.
Performing thermogravimetric analysis on the silicone rubber prefabricated part:
grinding the silicone rubber prefabricated member prepared in the step (one) into uniform fine powder by using a mortar, putting 5.29g of m 0 g into a thermal weightless analyzer, setting the reaction atmosphere to be nitrogen, the gas flow to be 20mL/min, the heating rate to be 10 ℃/min, the heating temperature range to be 25-1100 ℃, and recording the final stable mass m 1 to be 4.99g.
Step three, calculating the glue content:
Substituting M 0、M1、m0 and M 1 into the equation The rubber content in the silicone rubber provided in this example was calculated to be 31.5%.
Comparative example 1
The comparative example provides a method for measuring the content of rubber in silicone rubber, which comprises the following steps:
Step one, performing thermogravimetric analysis on a silicone rubber prefabricated part:
(1) Selecting a silicon rubber umbrella skirt of the cable terminal insulator which is the same as that of the embodiment 1, shearing, weighing the mass M 0 to be 120g, placing the silicon rubber umbrella skirt into a reaction container, heating to 95 ℃, dehydrating for 0.5h, and weighing the mass M 1 to be 119.4g;
(2) Grinding into uniform fine powder by using a mortar, putting 4.95g of m 0 mass into a thermal weight loss analyzer, setting the reaction atmosphere to be nitrogen, setting the gas flow to be 20mL/min, heating at a heating rate of 10 ℃/min, heating at a temperature interval of 25-1100 ℃, and recording that the final stable mass m 1 is 3.75g.
Step two, calculating the glue content:
Substituting m 0 and m 1 into the equation The rubber content in the silicone rubber provided in this example was calculated to be 24.6%.
Comparative example 2
The comparative example provides a method for measuring the content of rubber in silicone rubber, which comprises the following steps:
step one, cracking the silicon rubber:
(1) Selecting a silicon rubber umbrella skirt of the cable terminal insulator which is the same as that of the embodiment 1, shearing, weighing the mass M 0 to be 120g, placing the silicon rubber umbrella skirt into a reaction container, heating to 95 ℃, and dehydrating for 0.5h;
(2) Adding 3g of sulfonic acid and sulfuric acid into a reaction vessel as acid cracking catalysts, heating to 120 ℃, continuously stirring for reaction, and pumping volatile components such as DMC (dimethyl siloxane mixed ring) generated by the reaction by a vacuum pump;
(3) After 1 hour of reaction, the heating was stopped, the reaction vessel was allowed to cool naturally, and the silicone rubber preform was taken out of the reaction vessel, which was inorganic matters from which most of the siloxane had been removed, and the mass M 1 was weighed to be 101.4g.
Performing thermogravimetric analysis on the silicone rubber prefabricated part:
Grinding the silicone rubber prefabricated member prepared in the step (one) into uniform fine powder by using a mortar, putting 5.92mg of m 0 mg into a thermal weight loss analyzer, setting the reaction atmosphere to be nitrogen, the gas flow to be 20mL/min, the heating rate to be 10 ℃/min, the heating temperature range to be 25-1100 ℃, and recording the final stable mass m 1 to be 4.85g.
Step three, calculating the glue content:
Substituting M 0、M1、m0 and M 1 into the equation The rubber content in the silicone rubber provided in this example was calculated to be 30.8%.
In the invention, the higher the measured rubber content is, the more accurate the ceramic silicone rubber is, because the inner silicone rubber is protected by the ceramic layer in the thermogravimetric experiment, and is not easy to decompose completely. The cracking effect is to decompose part of the siloxane in advance by using a chemical means, so that the residual silicone rubber can be fully decomposed by heating in a thermogravimetric experiment. Comparison of the results of examples 1 to 4 with those of comparative examples 1 to 2 shows that the accuracy of the results of the method for measuring the content of the rubber in the silicone rubber provided in examples 1 to 4 is higher than that of the method for measuring the content of the rubber in the silicone rubber provided in comparative examples 1 to 2. According to the method for measuring the rubber content in the silicone rubber, disclosed by the invention, the silicone rubber is subjected to cracking reaction before thermogravimetric analysis, the cracking reaction temperature is limited to 160-200 ℃, and the silicone rubber prefabricated member with the main body of inorganic filler is obtained, so that a compact protective layer does not appear in the silicone rubber prefabricated member in the thermogravimetric analysis process, the silicone rubber prefabricated member is decomposed relatively thoroughly in the thermogravimetric analysis process, and a relatively accurate rubber content result is finally obtained.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples merely represent a few embodiments of the present invention, which facilitate a specific and detailed understanding of the technical solutions of the present invention, but are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. It should be understood that, based on the technical solutions provided by the present invention, those skilled in the art may obtain technical solutions through logical analysis, reasoning or limited experiments, which are all within the scope of protection of the appended claims. The scope of the patent is therefore intended to be covered by the appended claims, and the description and drawings may be interpreted as illustrative of the contents of the claims.
Claims (10)
1. The method for measuring the rubber content in the silicone rubber is characterized by comprising the following steps of:
Mixing silicone rubber with the mass of M 0 with a cracking catalyst, and carrying out a cracking reaction to prepare a silicone rubber prefabricated member, wherein the mass of the silicone rubber prefabricated member is M 1; the temperature of the cracking reaction is 160-200 ℃;
performing thermogravimetric analysis on the silicone rubber prefabricated part with the mass of m 0, wherein the mass of the silicone rubber prefabricated part after the thermogravimetric analysis is finished is m 1;
Substituting M 0、M1、m0 and M 1 into an equation to calculate the glue content A;
the equation is ；
The silicone rubber is selected from ceramic silicone rubber; the step of dehydrating the silicone rubber is also included before mixing the mass of M 0 with the cleavage catalyst.
2. The method for measuring the gum content in the silicone rubber according to claim 1, wherein the cracking catalyst is an acidic catalyst or a basic catalyst.
3. The method for measuring the gum content in silicone rubber according to claim 2, wherein the acidic catalyst is at least one selected from the group consisting of sulfonic acid and sulfuric acid.
4. A method for measuring the gum content in silicone rubber according to claim 3, wherein the acidic catalyst is a mixture of sulfonic acid and concentrated sulfuric acid.
5. The method for measuring the gum content in silicone rubber according to claim 2, wherein the basic catalyst is potassium hydroxide.
6. The method for measuring the content of rubber in silicone rubber according to claim 1, wherein the dehydration temperature is 80-110 ℃.
7. The method for measuring the rubber content in the silicone rubber according to claim 1, wherein the time for dehydration is 0.3h to 0.8h.
8. The method for measuring the content of rubber in silicone rubber according to any one of claims 1 to 7, wherein the conditions for thermogravimetric analysis are: the atmosphere is nitrogen; the gas flow is 20 mL/min-50 mL/min; the heating rate is 5-20 ℃/min; the heating temperature is 25-1100 deg.c.
9. The method for measuring the rubber content in the silicone rubber according to any one of claims 1 to 7, wherein the time for the cleavage reaction is 0.5h to 1h.
10. The method for measuring the rubber content in the silicone rubber according to any one of claims 1 to 7, wherein the temperature of the cracking reaction is 170 ℃.
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