Test method for rubber oil causing non-photo-thermal yellowing of calcium carbonate filled rubber oil extended compounds

By mixing SBS, rubber oil, and high-whiteness calcium powder in a specific ratio, storing the mixture in the dark, and then testing it with a colorimeter, the problem of accuracy and efficiency in detecting active substances in naphthenic rubber oil was solved, thus improving the quality control of naphthenic rubber oil.

CN116481977BActive Publication Date: 2025-11-18PETROCHINA CO LTD
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Patent Information

Application Number
CN202210037225.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-01-13
Publication Date
2025-11-18
Estimated Expiration
2042-01-13

AI Technical Summary

Technical Problem

Existing technologies cannot effectively detect whether naphthenic rubber oils contain specific active substances that cause yellowing of oil-extended rubber composites, resulting in low detection accuracy and efficiency.

Method used

By mixing SBS, rubber oil, and high-whiteness calcium powder in a specific ratio and storing them in the dark for a certain period of time, the yellowing index of the mixed material is tested using a colorimeter to determine whether the rubber oil contains trace amounts of active substances.

Benefits of technology

This improved the accuracy and efficiency of detecting active substances in rubber oils, reduced workload, and ensured the accuracy of product quality control.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a test method for rubber oil causing non-photothermal yellowing of oil-extended rubber calcium powder formula particles, and according to a certain proportion, a specific brand of SBS, rubber oil and calcium powder with a specific whiteness are weighed, the mixed materials are stored in the dark for a specific time at a specific temperature, and a color difference instrument is used to test the yellowing index of the mixed materials. The application relates to the technical field of naphthenic base rubber oil application. The test method for rubber oil causing non-photothermal yellowing of oil-extended rubber calcium powder formula particles can realize the following steps: at a specific temperature, rubber oil, rubber and calcium powder are mixed in a specific proportion, the mixture is stored in the dark for a specific time, the synergistic effect of the three materials is utilized, a color difference instrument is used to test the yellowing index, and whether trace active substances that are difficult to be detected by large-scale instruments and equipment are contained in high-pressure hydrogenated rubber oil is determined. The active substances will produce bad results for actual application.
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Description

Technical Field

[0001] This invention relates to the field of cycloalkyl rubber oil application technology, and specifically to a test method for determining whether high-pressure hydrogenated rubber oil can cause non-photothermal yellowing of oil-extended calcium carbonate powder particles. Background Technology

[0002] In production practice, the yellowing phenomenon of rubber oils and oil-extended rubber composites is of great concern in the application of naphthenic rubber oils. It is generally believed that the yellowing of oil-extended rubber composites is directly related to the photothermal aging resistance of individual materials and the severity of the light and heat conditions applied to the composite. That is, it is considered that the photothermal yellowing resistance of each monomer material (including rubber oil, rubber, and resin), or the intensity and duration of photothermal exposure, are the causes of yellowing. However, there is no relevant literature or data regarding whether interactions between the materials lead to yellowing. This innovative achievement is based on research into the interactions between materials, discovering a type of oil-extended rubber composite that yellows quickly due to interactions between materials even without direct photothermal exposure. The essence of this phenomenon is due to a special active substance in the rubber oil, present in extremely small amounts that cannot be directly detected by large-scale equipment. Rubber oils containing this active substance can be specifically judged by observing the interaction between multiple materials to determine whether yellowing occurs.

[0003] This invention represents the first definition and study of a novel phenomenon, as there are currently no similar technologies in the field, either domestically or internationally. Originating from a new discovery in production practice, this invention describes a synergistic yellowing process under conditions of light and heat avoidance. Theoretically, it completely overturns the traditional understanding of yellowing in this field, namely, that the yellowing of oil-extended materials is an appearance manifestation based on light and heat aging. It expands upon the traditional theory of yellowing of oil-extended rubber materials, first proposing a material yellowing phenomenon not based on light and heat conditions, and discovering a new yellowing mechanism caused by rubber oil. A testing method for detecting this new yellowing has also been established.

[0004] This invention represents a leading technology in the industry, and currently there are no related technologies applied domestically or internationally. It will promote the development of the entire naphthenic rubber oil industry. It facilitates quality control during product upgrades and iterations, and lays a solid theoretical foundation for next-generation naphthenic rubber oil products. Summary of the Invention

[0005] (a) Technical problems to be solved

[0006] To address the shortcomings of existing technologies, this invention provides a test method for non-photothermal yellowing of oil-extended calcium carbonate powder formulation particles caused by rubber oil. This method is used to determine whether high-pressure hydrogenated rubber oil contains a specific active substance that is the root cause of yellowing due to the interaction of multiple materials. This enables quality control of high-pressure hydrogenated naphthenic rubber oil.

[0007] (II) Technical Solution

[0008] To achieve the above objectives, the present invention provides the following technical solution: a test method for non-photothermal yellowing of oil-extended calcium carbonate powder formulation particles caused by rubber oil, specifically including the following steps:

[0009] S1. Accurately weigh SBS of a specific manufacturer's grade into a 250ml beaker and record the mass.

[0010] S2. Add a certain amount of rubber oil to the oven at 50℃±2℃, stir thoroughly, and let it absorb the oil for 45 minutes.

[0011] S3. After the SBS particles have fully absorbed the oil, add a certain amount of calcium powder (600 mesh, whiteness greater than 95%) and stir thoroughly to ensure that the calcium powder evenly covers the surface of the oil-extended adhesive particles.

[0012] S4. Oil-filled granules are kept in the dark at a certain temperature for a specific period of time for later use.

[0013] S5. A flat container with a cylindrical recess, the recess is covered with a layer of aluminum foil to avoid ambient light interfering with the test results;

[0014] S6. After storing the granules in the dark, fill them into a flat container with cylindrical depressions, making sure it is even and flat without large pores. Then cover the granules with a quartz glass plate, ensuring that the quartz glass plate and the flat container are on the same flat surface.

[0015] S7. Place the flat container covered with a quartz glass plate close to the test hole of the colorimeter, ensuring that the particles completely cover the test hole and do not move. After deducting the influence of the quartz glass, use the instrument to calculate the yellowing index of the particles.

[0016] Preferably, in step S1, the mass of SBS from a specific manufacturer is accurately weighed to be 3.9g.

[0017] Preferably, the mass of rubber oil added in step S2 is 9.5-11.1g, and the specific amount added is determined according to the solubility characteristics of the rubber oil.

[0018] Preferably, the mass of calcium powder added in step S3 is 13.9g.

[0019] Preferably, the storage temperature of the oil-filled particles in step S4 is 30℃±5℃.

[0020] Preferably, the retention time of the oil-filled particles in step S4 is 72 hours.

[0021] Preferably, in step S5, the flat container has a cylindrical stepped groove with a depth of 1 cm.

[0022] Preferably, in step S5, the flat container has a length of 6.8cm, a width of 5.2cm, and a thickness of 2.2cm.

[0023] Preferably, in step S6, the quartz glass plate has a length of 5cm, a width of 5.2cm, and a thickness of 0.2cm.

[0024] (III) Beneficial Effects

[0025] This invention provides a test method for non-photothermal yellowing of oil-extended calcium powder formulation particles caused by rubber oil. Compared with existing technologies, it has the following advantages: This test method for non-photothermal yellowing of oil-extended calcium powder formulation particles caused by rubber oil involves weighing a specific grade of SBS, rubber oil, and calcium powder of a specific whiteness according to a certain ratio, mixing them thoroughly, storing them in the dark at a certain temperature for a specific period of time, and then testing the yellowing index of the mixture using a colorimeter. The key feature is that: at a certain temperature, a fixed proportion of SBS and rubber oil are accurately weighed, thoroughly stirred and absorbed, and then a specified weight of calcium powder is added, ensuring the whiteness of the calcium powder meets the requirements. This allows the calcium powder to fully and uniformly coat the oil-extended rubber particles, forming oil-extended calcium powder formulation particles. By storing the mixture of rubber oil, rubber, and calcium powder in a specific ratio at a controlled temperature for a limited time, and then storing it in the dark for a specified period, a colorimeter can be used to test the yellowing index. This allows for the determination of whether the high-pressure hydrogenated rubber oil contains trace amounts of active substances that are difficult to detect by large instruments. These active substances can produce adverse results in practical applications. This method is highly beneficial for improving detection accuracy, efficiency, and reducing workload, and it closely matches actual application scenarios, accurately identifying rubber oil products that may have potential application problems. Attached Figure Description

[0026] Figure 1 This is a flowchart of the testing method of the present invention;

[0027] Figure 2 This is a front view of the flat-plate container structure of the present invention;

[0028] Figure 3 This is a top view of the flat-plate container structure of the present invention;

[0029] Figure 4This is a front view of the quartz glass plate structure of the present invention;

[0030] Figure 5 This is a top view of the quartz glass plate structure of the present invention;

[0031] Figure 6 This is a schematic diagram illustrating the stacking order of samples and materials in an embodiment of the present invention. Detailed Implementation

[0032] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0033] Please see Figure 1-6 The present invention provides three technical solutions: a test method for non-photothermal yellowing of oil-extended calcium powder formulation particles caused by rubber oil, specifically including the following embodiments:

[0034] Example 1

[0035] S1. Accurately weigh a specific brand of SBS in a 250ml beaker and record the mass. The mass of the specific brand of SBS is 3.9g.

[0036] S2. At 50°C in an oven, add a certain amount of rubber oil, stir thoroughly, and let it absorb the oil for 45 minutes. The mass of the rubber oil added is 10.5g. The specific amount added depends on the solubility characteristics of the rubber oil.

[0037] S3. After the SBS particles have fully absorbed the oil, add a certain amount of calcium powder (600 mesh, whiteness greater than 95%), stir thoroughly to ensure that the calcium powder evenly covers the surface of the oil-filled adhesive particles. The mass of calcium powder added is 13.9g.

[0038] S4. The oil-filled particles are kept at a certain temperature under light-protected conditions for a specific period of time for later use. The storage temperature of the oil-filled particles is 30℃ and the storage time is 72h.

[0039] S5. A flat container with a cylindrical recess, the recess is covered with a layer of aluminum foil to avoid ambient light interference with the test results. The flat container has a cylindrical stepped groove with a depth of 1cm. The flat container is 6.8cm long, 5.2cm wide and 2.2cm thick.

[0040] S6. After storing the granules in the dark, fill them into a flat container with cylindrical depressions, making sure it is even and flat without large gaps. Then cover the granules with a quartz glass plate, ensuring that the quartz glass plate and the flat container are on the same flat surface. The quartz glass plate is 5cm long, 5.2cm wide, and 0.2cm thick.

[0041] S7. Place the flat container covered with a quartz glass plate close to the test hole of the colorimeter, ensuring that the particles completely cover the test hole and do not move. After deducting the influence of the quartz glass, use the instrument to calculate the yellowing index of the particles.

[0042] Example 2

[0043] S1. Accurately weigh a specific brand of SBS in a 250ml beaker and record the mass. The mass of the specific brand of SBS is 3.9g.

[0044] S2. At 48℃ in the oven, add a certain amount of rubber oil, stir thoroughly, and let it absorb the oil for 45 minutes. The mass of the rubber oil added is 9.5g. The specific amount added depends on the solubility characteristics of the rubber oil.

[0045] S3. After the SBS particles have fully absorbed the oil, add a certain amount of calcium powder (600 mesh, whiteness greater than 95%), stir thoroughly to ensure that the calcium powder evenly covers the surface of the oil-filled adhesive particles. The mass of calcium powder added is 13.9g.

[0046] S4. The oil-filled particles are kept at a certain temperature under light-protected conditions for a specific period of time for later use. The storage temperature of the oil-filled particles is 25℃ and the storage time is 72h.

[0047] S5. A flat container with a cylindrical recess, the recess is covered with a layer of aluminum foil to avoid ambient light interference with the test results. The flat container has a cylindrical stepped groove with a depth of 1cm. The flat container is 6.8cm long, 5.2cm wide and 2.2cm thick.

[0048] S6. After storing the granules in the dark, fill them into a flat container with cylindrical depressions, making sure it is even and flat without large gaps. Then cover the granules with a quartz glass plate, ensuring that the quartz glass plate and the flat container are on the same flat surface. The quartz glass plate is 5cm long, 5.2cm wide, and 0.2cm thick.

[0049] S7. Place the flat container covered with a quartz glass plate close to the test hole of the colorimeter, ensuring that the particles completely cover the test hole and do not move. After deducting the influence of the quartz glass, use the instrument to calculate the yellowing index of the particles.

[0050] Example 3

[0051] S1. Accurately weigh a specific brand of SBS in a 250ml beaker and record the mass. The mass of the specific brand of SBS is 3.9g.

[0052] S2. At 52℃ in the oven, add a certain amount of rubber oil, stir thoroughly, and let it absorb the oil for 45 minutes. The mass of rubber oil added is 11.1g. The specific amount added is determined according to the solubility characteristics of the rubber oil.

[0053] S3. After the SBS particles have fully absorbed the oil, add a certain amount of calcium powder (600 mesh, whiteness greater than 95%), stir thoroughly to ensure that the calcium powder evenly covers the surface of the oil-filled adhesive particles. The mass of calcium powder added is 13.9g.

[0054] S4. The oil-filled particles are kept at a certain temperature under light-protected conditions for a specific period of time for later use. The storage temperature of the oil-filled particles is 35℃ and the storage time is 72h.

[0055] S5. A flat container with a cylindrical recess, the recess is covered with a layer of aluminum foil to avoid ambient light interference with the test results. The flat container has a cylindrical stepped groove with a depth of 1cm. The flat container is 6.8cm long, 5.2cm wide and 2.2cm thick.

[0056] S6. After storing the granules in the dark, fill them into a flat container with cylindrical depressions, making sure it is even and flat without large gaps. Then cover the granules with a quartz glass plate, ensuring that the quartz glass plate and the flat container are on the same flat surface. The quartz glass plate is 5cm long, 5.2cm wide, and 0.2cm thick.

[0057] S7. Place the flat container covered with a quartz glass plate close to the test hole of the colorimeter, ensuring that the particles completely cover the test hole and do not move. After deducting the influence of the quartz glass, use the instrument to calculate the yellowing index of the particles.

[0058] In summary, this invention enables the determination of whether high-pressure hydrogenated rubber oil contains trace amounts of active substances that are difficult to detect by large instruments by mixing rubber oil, rubber, and calcium powder in a specific ratio at a certain temperature, storing the mixture in the dark for a certain period of time, and utilizing the synergistic effect of the three materials. The yellowing index is then measured using a colorimeter. These active substances can produce adverse results in practical applications. This invention is highly beneficial for improving detection accuracy, efficiency, and reducing workload, and it closely aligns with real-world application scenarios, accurately identifying rubber oil products that may pose potential application risks.

[0059] Furthermore, any content not described in detail in this specification is existing technology known to those skilled in the art.

[0060] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0061] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A test method for non-photothermal yellowing of oil-extended calcium carbonate powder formulation particles caused by rubber oil, used to determine whether high-pressure hydrogenated rubber oil contains a special active substance that causes synergistic yellowing due to the interaction of multiple materials, characterized by: Specifically, the following steps are included: S1. Accurately weigh SBS of a specific manufacturer's grade into a 250ml beaker and record the mass. In step S1, the mass of SBS from a specific manufacturer and brand is accurately weighed to be 3.9g. S2. Add a certain amount of rubber oil to the oven at 50℃±2℃, stir thoroughly, and let it absorb the oil for 45 minutes; the mass of rubber oil added in step S2 is 9.5-11.1g. S3. After the SBS particles have fully absorbed the oil, add a certain amount of calcium powder (600 mesh, whiteness greater than 95%) and stir thoroughly to ensure that the calcium powder evenly covers the surface of the oil-filled adhesive particles. The mass of calcium powder added in step S3 is 13.9g. S4. Oil-filled granules are kept in the dark at a certain temperature for a specific period of time for later use. The storage temperature of the oil-filled particles in step S4 is 30℃±5℃. The oil-filled particles are held for 72 hours in step S4. S5. A flat container with a cylindrical indentation, the indentation being covered with a layer of aluminum foil; S6. After storing the granules in the dark, fill them into a flat container with cylindrical depressions, making sure it is even and flat without large pores. Then cover the granules with a quartz glass plate, ensuring that the quartz glass plate and the flat container are on the same flat surface. S7. Place the flat container covered with a quartz glass plate close to the test hole of the colorimeter, ensuring that the particles completely cover the test hole and do not move. After deducting the influence of the quartz glass, use the instrument to calculate the yellowing index of the particles.

2. The test method for non-photothermal yellowing of oil-extended calcium powder formulation particles caused by rubber oil according to claim 1, characterized in that: In step S5, a cylindrical stepped groove with a depth of 1 cm is provided on the flat container.

3. The test method for non-photothermal yellowing of oil-extended calcium powder formulation particles caused by rubber oil according to claim 1, characterized in that: In step S5, the flat container has a length of 6.8cm, a width of 5.2cm, and a thickness of 2.2cm.

4. The test method for non-photothermal yellowing of oil-extended calcium powder formulation particles caused by rubber oil according to claim 1, characterized in that: In step S6, the quartz glass plate has a length of 5cm, a width of 5.2cm, and a thickness of 0.2cm.

Citation Information

Patent Citations

  • Maleimide-modified ABS resin composition

    JP1997216981A