Rapid quantitative analysis method for antioxidant in rubber

A quantitative analysis and anti-aging agent technology, which is applied in the field of rubber and rubber formula analysis, can solve the problems of low quantitative results and self-loss, etc., and achieve the effect of convenient sample processing, good effect and good reproducibility

Active Publication Date: 2016-05-04
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under long-term high-temperature extraction conditions, the anti-aging agent will degrade in the thermal oxygen environment, and at the same time, it will also react with other compounding agents in the extract to cause its own loss, resulting in low quantitative results

Method used

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  • Rapid quantitative analysis method for antioxidant in rubber
  • Rapid quantitative analysis method for antioxidant in rubber
  • Rapid quantitative analysis method for antioxidant in rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Quantitative analysis of anti-aging agent in laboratory self-made 1# compound rubber and vulcanized rubber

[0030] The basic formula of the rubber compound is (parts by mass):

[0031] Component 1: natural rubber NR100; carbon black N33045, white carbon black 7000GR40, stearic acid (industrial grade) 2.0, zinc oxide 3.5, silane coupling agent X50S8.0, zinc stearate (laboratory self-made) 2.5, hard Pentaerythritol fatty acid ester 1.0,

[0032] Component 2: Antiaging agent 6PPD1.5, Antiaging agent A2.0,

[0033] Component 3: sulfur 1.8, vulcanization accelerator NS1.5,

[0034] Preparation process: In a 1.6-liter Banbury mixer (manufactured by FARREL), add natural rubber NR and knead for 60s, then add stearic acid and zinc oxide and continue kneading for 40s, and finally add carbon black, white carbon black, silane coupling agent, zinc stearate, pentaerythritol stearate, knead to a temperature of 160°C, discharge the glue and take out the sheet, cool for l...

Embodiment 2

[0066] Example 2: Quantitative analysis of anti-aging agent in laboratory self-made 2# compound rubber and vulcanized rubber

[0067] The basic formula of the rubber compound is (parts by mass):

[0068] Component 1: natural rubber NR100; carbon black N33045, white carbon black 7000GR40, stearic acid (industrial grade) 2.0, zinc oxide 3.5, silane coupling agent X50S8.0, zinc stearate (laboratory self-made) 2.5, hard Pentaerythritol fatty acid ester 1.0,

[0069] Component 2: Antiaging agent 4010NA2.5, Antiaging agent D1.5,

[0070] Component 3: sulfur 1.8, vulcanization accelerator NS1.5,

[0071] Preparation process: In a 1.6-liter Banbury mixer (manufactured by FARREL), add natural rubber NR and knead for 60s, then add stearic acid and zinc oxide and continue kneading for 40s, and finally add carbon black, white carbon black, silane coupling agent, zinc stearate, pentaerythritol stearate, knead to a temperature of 160°C, discharge the glue and take out the sheet, cool for...

Embodiment 3

[0091] Example 3: Quantitative analysis of anti-aging agent in the sidewall rubber of German Continental snow tire (205 / 55R16) (it has been determined that the rubber contains anti-aging agent 6PPD and anti-aging agent 4030 by other analysis means)

[0092] 3.1 Preparation of internal standard stock solution: Weigh 150.21 mg of methyl n-octanoate into a 50 mL volumetric flask, and dilute to volume with acetone.

[0093] 3.2 Preparation of mixed standard sample stock solution: Weigh 254.65mg of antiaging agent 6PPD and 246.59mg of antiaging agent 4030 into a 50mL volumetric flask, dissolve in acetone to volume.

[0094] 3.3 Preparation of standard series solutions: pipette 0.5mL, 1.0mL, 1.5mL, 2.5mL, and 3.5mL of standard sample stock solution into five 10mL volumetric flasks in sequence, add 1.0mL internal standard stock solution respectively, and dilute with acetone.

[0095] 3.4 Preparation of rubber extract: use MM400 mixed freeze grinder (manufactured by Retsch, Germany) t...

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Abstract

The invention aims at to provide a method for rapid quantification of the content of an organic antioxidant in vulcanized and mixed rubber, which belongs to the fields of rubber and analysis of rubber formulas, wherein the vulcanized and mixed rubber comprises, but not limited to, natural or synthetic raw material rubber and compounds thereof, a variety of aid products with rubber as a carrier, a vulcanized and mixed rubber complex and the like. According to a technical scheme in the invention, the method comprises the following concrete steps: preparing particles with a size of less than 2 mm<3> from a rubber compound; subjecting the particles to ultrasonic extraction with a solvent; accurately adding an internal-standard substance into extract; subjecting the extract to separation and testing by using capillary column gas chromatography; and quantitatively determining the content of the antioxidant in the vulcanized and mixed rubber through comparison with a standard antioxidant solution. The method is simple in treatment steps and fast in an analysis speed, uses consistent chromatographic conditions and can quantify a plurality of antioxidants in the rubber compound at the same time.

Description

technical field [0001] The invention belongs to the field of rubber and rubber formula analysis, in particular to a rapid quantitative analysis method for various organic antioxidants in all types of vulcanized and mixed rubber. Described vulcanization and mixing rubber include but not limited to natural or synthetic raw rubber (including but not limited to NR, BR, SBR, IIR, CIIR, BIIR, EPDM, CR, silica gel, etc.) and their compound; Various auxiliary products for the carrier; rubber compounds for vulcanization and mixing, etc. Background technique [0002] With the development of the rubber industry, the research on rubber and rubber formula has attracted more and more attention. Accurate quantification of the anti-aging agent content in the rubber compound is of great significance to the analysis of rubber and rubber formulations. [0003] At present, the analysis of components in rubber compounds, especially in rubber compounds, usually uses the Soxhlet extraction metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/025
Inventor 王璨高剑琴房彩琴刘哲胡小娜董栋
Owner BEIJING RED AVENUE INNOVA
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