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Method for identifying sulfonamide accelerant in rubber

A technology of sulfenamides and an identification method, which is applied in the identification field of sulfenamide accelerators in rubber mixing, can solve the problems that there are no literatures and methods for the identification method of sulfenamides accelerators, and the method is simple. Effect

Active Publication Date: 2016-12-07
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there is no literature and methods published on the identification method of sulfenamide accelerators in compounded rubber

Method used

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  • Method for identifying sulfonamide accelerant in rubber
  • Method for identifying sulfonamide accelerant in rubber
  • Method for identifying sulfonamide accelerant in rubber

Examples

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Comparison scheme
Effect test

Embodiment 1

[0042] Example 1: Analysis of sulfenamide accelerators in laboratory prepared mixed rubber

[0043] The basic formula of compounded rubber is (parts by mass): 40 parts of natural rubber NR, 60 parts of butadiene rubber BR; 75 parts of carbon black N37575, 4.0 parts of process oil, 2.0 parts of stearic acid, 1.5 parts of zinc oxide, and 4.0 parts of tackifying resin , 2.0 parts of anti-aging agent 4020, 1.5 parts of anti-aging agent RD, 1.5 parts of sulfur, and 1.6 parts of vulcanization accelerator DZ. The total amount of rubber samples is 193.1 parts.

[0044] Preparation process: use a 1.6-liter Banbury internal mixer (produced by FARREL Company), mix rubber, carbon black and other compounds except sulfur and vulcanization accelerator DZ for 6 minutes and heat up to 160 ° C to obtain a master batch, and Cool the masterbatch to below 90°C; then use an open rubber mixer to mix vulcanization accelerator and sulfur into the masterbatch, and knead the above mixture for 10 minutes ...

Embodiment 2

[0049] Embodiment 2: Qualitative analysis of sulfenamide accelerator in unknown mixed rubber sample

[0050] Sample source: provided by a tire factory.

[0051] The sample was prepared with a liquid nitrogen cryo-grinder to be less than 1.0mm 3 Take 1025.3 mg of colloidal particles, according to the GB / T3516-2006 method, methanol is used as a solvent to prepare a sample extract, and the extract is analyzed by a GC / MS system. The chromatographic conditions are the same as in Example 1.

[0052] The total ion chromatogram (see Image 6 C). The chromatogram when finding extraction ion m / z=98, 167 in sample total ion flow chart (see Image 6 D) The mass spectrogram and accelerator CZ mass spectrogram ( figure 2 ) are the same, and the substance peak at the retention time t=22.91min is the accelerator CZ, so it is determined that the accelerator CZ is added in the mixed rubber sample.

[0053] In order to determine whether the sample contains high-boiling sulfenamide accelera...

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Abstract

The invention provides a method for identifying a sulfonamide accelerant in a rubber. The method is used for detecting a mixing rubber and mainly comprises the following steps: 1) cutting a rubber sample into pieces and extracting; 2) using a gas chromatograph-mass spectrometer to extract a characteristic ion of the sulfonamide accelerant in a total ion current spectrogram of the sample; 3) in order to judge whether a high boiling point accelerant not detected by the gas chromatograph-mass spectrometer is added in a rubber material, adding a scorch retarder CTP in an extraction solution to continue detection, extracting a characteristic ion of benzothiazole in the total ion current spectrogram of the sample, if no characteristic ion of benzothiazole is detected, then determining that no sulfonamide accelerant is added in the mixing rubber sample, if benzothiazole is detected, then extracting the characteristic ion of the corresponding amine substance one by one, and if the corresponding amine substance is found, then determining that the corresponding accelerant is added in the rubber. The method uses a gas chromatograph-mass spectrometer (GC-MS) method to identify the sulfonamide accelerant in the rubber, and the sensitivity and the accuracy are both very high.

Description

technical field [0001] The invention belongs to the field of testing and analysis, in particular to a qualitative analysis method for sulfenamide accelerators in rubber, in particular to an identification method for sulfenamide accelerators in rubber compound. Background technique [0002] With the development of the rubber industry, the research on rubber and rubber formula has attracted more and more attention. It is of great significance to accurately distinguish the type of accelerator in the mixed rubber for the analysis of rubber and rubber formula. [0003] The sulfenamide accelerator is a kind of slow-acting accelerator derived from 2-mercaptobenzothiazole (accelerator M) as the parent. The structure is as follows: [0004] [0005] R=N-R', wherein R' is linear or branched alkanes, cycloalkanes or dicycloalkanes, heterocycloalkanes, alkanes and cycloalkanes substituted by one or more N / S / O / halogen atoms. [0006] Sulphenamide accelerators have a long scorch time...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/08
CPCG01N30/08G01N30/88
Inventor 王璨高剑琴房彩琴董栋
Owner BEIJING RED AVENUE INNOVA
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