CN117705529A - Preparation method of rubber self-adhesion detection standard sample - Google Patents
Preparation method of rubber self-adhesion detection standard sample Download PDFInfo
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- CN117705529A CN117705529A CN202311728576.5A CN202311728576A CN117705529A CN 117705529 A CN117705529 A CN 117705529A CN 202311728576 A CN202311728576 A CN 202311728576A CN 117705529 A CN117705529 A CN 117705529A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 56
- 238000001514 detection method Methods 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 238000003825 pressing Methods 0.000 claims description 18
- 238000004073 vulcanization Methods 0.000 claims description 18
- 238000005520 cutting process Methods 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 13
- 229920005989 resin Polymers 0.000 claims description 13
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 12
- 239000003292 glue Substances 0.000 claims description 12
- 239000004744 fabric Substances 0.000 claims description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- -1 polypropylene Polymers 0.000 claims description 10
- 230000003014 reinforcing effect Effects 0.000 claims description 10
- 244000043261 Hevea brasiliensis Species 0.000 claims description 9
- 229920003052 natural elastomer Polymers 0.000 claims description 9
- 229920001194 natural rubber Polymers 0.000 claims description 9
- 230000003712 anti-aging effect Effects 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000004743 Polypropylene Substances 0.000 claims description 6
- 239000004927 clay Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 5
- 239000012190 activator Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 5
- 239000008117 stearic acid Substances 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- 229920000298 Cellophane Polymers 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 description 25
- 239000000463 material Substances 0.000 description 12
- 239000000853 adhesive Substances 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000003490 calendering Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000019808 microcrystalline wax Nutrition 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L7/00—Compositions of natural rubber
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Investigating Strength Of Materials By Application Of Mechanical Stress (AREA)
Abstract
The invention relates to the technical field of rubber detection, and discloses a preparation method of a rubber self-viscosity detection standard sample. The preparation method is convenient and quick, and the prepared standard sample is stable and durable.
Description
Technical Field
The invention relates to the technical field of rubber detection, in particular to a preparation method of a rubber self-adhesion detection standard sample.
Background
In the process of manufacturing and shaping a tire, one layer of extrusion or calendaring rubber material is paved on the other layer of extrusion or calendaring rubber material, before vulcanization, the rubber materials are bonded together according to part layers, the formula of the tire rubber material contains a plurality of components with different solubilities, when the temperature changes, some formula components can be separated from the rubber material, frost is formed on the surface of the rubber material, the self-adhesion of the rubber material in the shaping process can be destroyed, the manufacturing and processing of the tire is influenced, a rubber self-adhesion tester adopts a butt adhesion test method to test the adhesion formed after two rubber sheets are contacted and pressed for a certain time, the self-adhesion of unvulcanized rubber is used for representing, in order to judge the adhesion of the rubber materials with different formulas, the test wheel of equipment in the test uses the same standard sample to test the different rubber materials, the self-adhesion of the formula rubber materials is evaluated through experiments, the quality of rubber products is ensured, and the adhesion and the reliability in the use of the rubber materials is ensured.
Chinese patent (publication No. CN116793949A, publication No. 2023.09.22) discloses an apparatus and method for evaluating quality of a tire wirecord fabric. The apparatus includes: stripping the test piece; the thickness gauge is used for measuring the total thickness of the stripping test piece; the vulcanizing mould is used for vulcanizing the stripping test piece, and the thickness of the vulcanizing mould is 80% -95% of the total thickness of the test piece; the tensile machine is used for carrying out peeling test on the vulcanized peeling test piece on the tensile machine and drawing a load curve; the camera shooting assembly is arranged on the tension machine and used for shooting the adhesion condition of the rubber on the surface of the stripped test piece steel wire after stripping. The equipment adopts the stripping test piece with a specific structure, the stripping test piece is vulcanized, then the pulling machine and the camera assembly obtain the pictures of the adhesion force of the curtain cloth and the adhesion condition of the rubber material on the surface of the stripped stripping test piece steel wire, and the quality of the steel wire curtain cloth is evaluated through the judgment standard of the adhesion force of the curtain cloth and the pictures of the standard scoring sample piece, so that the quality of the steel wire curtain cloth of the tire can be comprehensively reflected. In order to further optimize the evaluation criteria, a standard sample of uniform specification and stability is required as a reference, but no method for preparing such standard sample is currently available.
Disclosure of Invention
The invention provides a preparation method of a rubber self-viscosity detection standard sample, aiming at the defects of the prior art.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the rubber self-adhesion detection standard sample comprises the following specific steps:
1) Wrapping the mixed standard rubber on a roll mill to ensure smooth surface, controlling the thickness of a piece discharged from the roll mill within 0.6mm plus or minus 0.1mm, and cutting a 200mm multiplied by 200mm sample;
2) Cutting a piece of 250mm multiplied by 250mm polypropylene palm fiber cloth, and cutting a piece of 250mm multiplied by 250mm high temperature resistant glass paper;
3) The 200mm multiplied by 200mm sample is clamped between polypropylene palm fiber cloth and cellophane, and is placed on a flat vulcanizing machine for vulcanization, and the vulcanization conditions are as follows: vulcanizing at 100 ℃ for 1min;
4) And cutting the vulcanized sample into strips with the width of 12mm plus or minus 0.5mm and the length of 170mm plus or minus 10mm, and obtaining a standard sample.
Preferably, the standard rubber is prepared by mixing the following raw materials in parts by weight based on 100 parts by weight of rubber component: 100 parts of natural rubber, 55.0 parts of carbon black, 75.0 parts of rubber oil, 12.0 parts of high styrene resin, 6.0 parts of clay, 5.5 parts of an activating agent, 14 parts of phenolic reinforcing resin, 1.0 part of an anti-aging agent, 3.5 parts of a vulcanizing agent, 2.51 parts of a vulcanization accelerator and 0.15 part of a scorch retarder.
Preferably, the activator is zinc oxide and stearic acid, wherein 3.5 parts by weight of zinc oxide and 2 parts by weight of stearic acid are used;
the accelerator adopts NS and HEXA-65, wherein, 0.36 weight parts of vulcanization accelerator NS and 2.15 weight parts of vulcanization accelerator HEXA-65.
Preferably, the carbon black adopts N375, the rubber oil adopts naphthenic oil, the phenolic aldehyde reinforcing resin adopts 205 phenolic aldehyde reinforcing resin, the anti-aging agent adopts RD, the vulcanizing agent adopts 7020, and the scorch retarder adopts CTP.
The invention further discloses a preparation method of the standard rubber, and the mixing method of the standard rubber comprises the following specific steps:
1) And (3) mixing: adding a part of natural rubber, carbon black, high styrene, clay, activator, phenolic reinforcing resin and anti-aging agent, setting the rotation speed at 53rpm and the pressure at 5.5kg/cm 2 Pressing a top bolt to 105 ℃; lifting the top bolt, adding rubber oil, setting the rotation speed to 58rpm and the pressure to 5.5kg/cm 2 Pressing a top bolt to 138 ℃, lifting the top bolt in place, pressing the top bolt to 150 ℃ and discharging glue;
2) The vulcanizing section is used for adding the vulcanizing agent, the rest natural rubber, the vulcanization accelerator and the scorch retarder, pressing for 25 seconds, and setting the rotating speed to 30rpm and the pressure to 4.5kg/cm 2 Lifting the top bolt in place, setting the rotation speed to 25rpm and the pressure to 4.5kg/cm 2 Pressing for 20 seconds; lifting the top bolt in place, setting the rotating speed to 30rpm and the pressure to 4.5kg/cm 2 Pressing for 15 seconds to 105 ℃ for discharging glue.
Furthermore, the invention also discloses a standard sample prepared by the method.
Furthermore, the invention also discloses application of the standard sample in rubber self-viscosity detection synthesis.
The beneficial effects of the invention are as follows: the standard sample of the invention has good stability and stable performance in the use process, and the formula is not added with microcrystalline wax, so that the gum stock can be prevented from being separated out in the use process.
Detailed Description
The technical solutions in the embodiments are clearly and completely described below in connection with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a preparation method of a rubber self-viscosity detection standard sample.
Standard glue formulation: 100 parts of natural rubber, 55.0 parts of N375 carbon black, 75.0 parts of naphthenic oil, 12.0 parts of high styrene resin, 6.0 parts of clay, 3.5 parts of zinc oxide, 2 parts of stearic acid, 14 parts of 205 phenolic aldehyde reinforcing resin, 1.0 parts of anti-aging agent RD, 3.5 parts of 7020 vulcanizing agent, 0.36 parts of vulcanization accelerator NS, 2.15 parts of vulcanization accelerator HEXA-65 and 0.15 parts of scorch retarder CTP.
The standard rubber is mixed, and the specific steps are as follows:
1) And (3) mixing: adding a part of natural rubber, carbon black, high styrene, clay, activator, phenolic reinforcing resin and anti-aging agent, setting the rotation speed at 53rpm and the pressure at 5.5kg/cm 2 Pressing a top bolt to 105 ℃; lifting the top bolt, adding rubber oil, setting the rotation speed to 58rpm and the pressure to 5.5kg/cm 2 Pressing a top bolt to 138 ℃, lifting the top bolt in place, pressing the top bolt to 150 ℃ and discharging glue;
2) The vulcanizing section is used for adding the vulcanizing agent, the rest natural rubber, the vulcanization accelerator and the scorch retarder, pressing for 25 seconds, and setting the rotating speed to 30rpm and the pressure to 4.5kg/cm 2 Lifting the top bolt in place, setting the rotation speed to 25rpm and the pressure to 4.5kg/cm 2 Pressing for 20 seconds; lifting the top bolt in place, setting the rotating speed to 30rpm and the pressure to 4.5kg/cm 2 Pressing for 15 seconds to 105 ℃ for discharging glue.
The preparation method of the standard sample comprises the following specific steps:
1) Wrapping the mixed standard rubber on a roll mill to ensure smooth surface, controlling the thickness of a piece discharged from the roll mill within 0.6mm plus or minus 0.1mm, and cutting a 200mm multiplied by 200mm sample;
2) Cutting a piece of 250mm multiplied by 250mm polypropylene palm fiber cloth, and cutting a piece of 250mm multiplied by 250mm high temperature resistant glass paper;
3) The 200mm multiplied by 200mm sample is clamped between polypropylene palm fiber cloth and cellophane, and is placed on a flat vulcanizing machine for vulcanization, and the vulcanization conditions are as follows: vulcanizing at 100 ℃ for 1min;
4) And cutting the vulcanized sample into strips with the width of 12mm plus or minus 0.5mm and the length of 170mm plus or minus 10mm, and obtaining a standard sample.
The obtained standard samples were subjected to stability test, and the test results are shown in table 1.
The standard sample stability detection method comprises the following steps: and (3) carrying out press-fit pull-off detection (test conditions of 20 press-fit speed, 20 pull-off speed and 1 press-fit time) by adopting a rubber self-adhesive tester, winding the cut standard sample in a test groove of a test wheel, cutting off redundant parts, tearing off glass paper, loading the test wheel back onto detection equipment, and detecting the standard adhesive force (N) without placing the sample to be detected on a lower clamping plate.
TABLE 1
As can be seen from Table 1, the standard test adhesive force prepared by the invention is stable and can be used for detecting the self-adhesiveness of rubber.
Application example 1
The obtained standard sample is applied to rubber self-adhesion detection.
The rubber self-adhesion detection method comprises the following steps: and (3) performing press-fit pull-off detection (test conditions of press-fit speed 20, pull-off speed 20 and press-fit time 1) by adopting a rubber self-adhesive tester, winding the cut standard sample in a test groove of a test wheel, cutting off redundant parts, tearing off glass paper, loading the test wheel back to detection equipment, putting the rubber to be detected on a lower clamping plate, and detecting the adhesive force (N) of the rubber to be detected. The rubber to be tested takes 5 component compounds of the tire, 20 batches of each component compound. The test results are shown in Table 2.
Tack criterion (N): the upper triangular glue is more than or equal to 8N, the lower triangular glue is more than or equal to 6, the cushion glue is more than or equal to 15, the transition layer glue is more than or equal to 12, and the film glue is more than or equal to 15.
TABLE 2
| Sequence number | Upper triangle | Lower triangle | Cushion rubber | Transition layer | Film sheet |
| 1 | 9.76 | 7.4 | 15.79 | 12.17 | 15.38 |
| 2 | 9.84 | 6.1 | 15.44 | 13.88 | 15.32 |
| 3 | 8.94 | 6.32 | 16.03 | 11.91 | 15.79 |
| 4 | 8.29 | 7.88 | 16.51 | 12.99 | 15.93 |
| 5 | 8.26 | 8.07 | 15.78 | 12.67 | 16.26 |
| 6 | 8.62 | 6.68 | 15.93 | 12.83 | 16.26 |
| 7 | 8.47 | 6.68 | 16.52 | 12.46 | 16.62 |
| 8 | 9.67 | 6.22 | 16.64 | 12.43 | 16.42 |
| 9 | 9.06 | 6.61 | 16.03 | 13.85 | 15.24 |
| 10 | 8.54 | 6.87 | 15.92 | 12.35 | 15.94 |
| 11 | 9.03 | 6.64 | 16.12 | 12.56 | 15.77 |
| 12 | 9.05 | 6.23 | 15.24 | 13.21 | 16.02 |
| 13 | 9.02 | 6.89 | 16.39 | 12.41 | 15.96 |
| 14 | 8.03 | 6.57 | 15.44 | 12.58 | 15.46 |
| 15 | 8.56 | 7.21 | 15.02 | 13.11 | 16.01 |
| 16 | 9.12 | 6.98 | 16.36 | 13.24 | 16.14 |
| 17 | 8.67 | 6.51 | 16.82 | 12.16 | 15.68 |
| 18 | 9.08 | 7.19 | 15.35 | 12.64 | 15.24 |
| 19 | 9.89 | 8.02 | 16.61 | 13.21 | 16.45 |
| 20 | 8.46 | 6.87 | 16.84 | 12.83 | 16.24 |
| Maximum value | 9.89 | 8.07 | 16.82 | 13.88 | 16.62 |
| Minimum value | 8.03 | 6.10 | 15.02 | 11.91 | 15.24 |
| Extremely poor | 1.86 | 1.97 | 1.8 | 1.97 | 1.38 |
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art. The generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. The preparation method of the rubber self-adhesion detection standard sample is characterized by comprising the following specific steps:
1) Wrapping the mixed standard rubber on a roll mill to ensure smooth surface, controlling the thickness of a piece discharged from the roll mill within 0.6mm plus or minus 0.1mm, and cutting a 200mm multiplied by 200mm sample;
2) Cutting a piece of 250mm multiplied by 250mm polypropylene palm fiber cloth, and cutting a piece of 250mm multiplied by 250mm high temperature resistant glass paper;
3) The 200mm multiplied by 200mm sample is clamped between polypropylene palm fiber cloth and cellophane, and is placed on a flat vulcanizing machine for vulcanization, and the vulcanization conditions are as follows: vulcanizing at 100 ℃ for 1min;
4) And cutting the vulcanized sample into strips with the width of 12mm plus or minus 0.5mm and the length of 170mm plus or minus 10mm, and obtaining a standard sample.
2. The method for preparing a standard sample according to claim 1, wherein the standard rubber is prepared by mixing the following raw materials in parts by weight based on 100 parts by weight of the rubber component:
100 parts of natural rubber, 55.0 parts of carbon black, 75.0 parts of rubber oil, 12.0 parts of high styrene resin, 6.0 parts of clay, 5.5 parts of an activating agent, 14 parts of phenolic reinforcing resin, 1.0 part of an anti-aging agent, 3.5 parts of a vulcanizing agent, 2.51 parts of a vulcanization accelerator and 0.15 part of a scorch retarder.
3. The method for preparing a standard sample according to claim 2, wherein the activator is zinc oxide and stearic acid, wherein the zinc oxide is 3.5 parts by weight and the stearic acid is 2 parts by weight;
the accelerator adopts NS and HEXA-65, wherein, 0.36 weight parts of vulcanization accelerator NS and 2.15 weight parts of vulcanization accelerator HEXA-65.
4. The method for preparing the standard sample according to claim 2, wherein the carbon black is N375, the rubber oil is naphthenic oil, the phenolic reinforcing resin is 205 phenolic reinforcing resin, the anti-aging agent is RD, the vulcanizing agent is 7020, and the scorch retarder is CTP.
5. The method for preparing the standard sample according to any one of claims 1 to 4, wherein the method for mixing the standard rubber comprises the following specific steps:
1) And (3) mixing: adding a part of natural rubber, carbon black, high styrene,Clay, activator, phenolic aldehyde reinforcing resin and anti-aging agent, the rotating speed is 53rpm, the pressure is 5.5kg/cm 2 Pressing a top bolt to 105 ℃; lifting the top bolt, adding rubber oil, setting the rotation speed to 58rpm and the pressure to 5.5kg/cm 2 Pressing a top bolt to 138 ℃, lifting the top bolt in place, pressing the top bolt to 150 ℃ and discharging glue;
2) The vulcanizing section is used for adding the vulcanizing agent, the rest natural rubber, the vulcanization accelerator and the scorch retarder, pressing for 25 seconds, and setting the rotating speed to 30rpm and the pressure to 4.5kg/cm 2 Lifting the top bolt in place, setting the rotation speed to 25rpm and the pressure to 4.5kg/cm 2 Pressing for 20 seconds; lifting the top bolt in place, setting the rotating speed to 30rpm and the pressure to 4.5kg/cm 2 Pressing for 15 seconds to 105 ℃ for discharging glue.
6. A standard sample prepared according to the method of any one of claims 1-5.
7. The use of the standard sample of claim 6 in the integrated detection of rubber self-tackiness.
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| CN202311728576.5A CN117705529A (en) | 2023-12-15 | 2023-12-15 | Preparation method of rubber self-adhesion detection standard sample |
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