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Method for identifying organic sulfide in rubber

An identification method and sulfide technology, applied in the field of analysis, can solve the problems of inability to directly extract and detect, difficult to identify organic small molecules, and long sample processing time, and achieve the effects of protecting environmental health, shortening extraction time, and shortening soaking time.

Active Publication Date: 2019-04-02
BEIJING RED AVENUE INNOVA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since organic sulfides such as HTS and KA9188 will break, decompose and react with rubber molecules during the rubber vulcanization process, they will be cross-linked in the rubber network and cannot be directly extracted and detected
Usually chemical methods are used to destroy the cross-linked network of rubber to obtain fragments of sulfur-containing compounds, and then solvents are used to extract the structure of small organic molecules. However, this method takes a long time to process samples, and the regenerated small organic molecules are far from the original sulfur-containing substances. , the characteristic small organic molecules are difficult to identify and are easily affected by other sulfur-containing compounds

Method used

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  • Method for identifying organic sulfide in rubber
  • Method for identifying organic sulfide in rubber
  • Method for identifying organic sulfide in rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1: Analysis of HTS in known vulcanized rubber

[0052] Laboratory preparation of vulcanizates:

[0053] The formula of vulcanized rubber is (parts by mass): 40 parts of natural rubber NR, 60 parts of butadiene rubber BR; 75 parts of carbon black N375, 4.0 parts of operating oil, 2.0 parts of stearic acid, 1.5 parts of zinc oxide, 4.0 parts of tackifying resin, anti-aging 2.0 parts of agent 4020, 1.5 parts of anti-aging agent RD, 1.5 parts of sulfur, 1.6 parts of vulcanization accelerator DZ, 1.5 parts of HTS, and 0.2 parts of anti-scorch agent CTP.

[0054] Preparation process: use a 1.6-liter Banbury internal mixer (produced by FARREL company), mix rubber, carbon black and other compounds except sulfur, vulcanization accelerator and anti-scorch agent CTP for 6 minutes and heat up to 160 ° C to obtain the mother Mix the rubber, and cool the masterbatch to below 90°C; then use an open rubber mixer to mix the vulcanization accelerator, sulfur and anti-scorch agen...

Embodiment 2

[0075] Embodiment 2: the analysis of the vulcanized rubber containing accelerator TBzTD, not containing organic S-alkyl thiosulfate or its derivatives prepared in laboratory

[0076] Vulcanizate sample preparation:

[0077] The basic formula of vulcanized rubber is (parts by mass): 100 parts of styrene-butadiene rubber ESBR, 30 parts of white carbon black, 40 parts of carbon black N375, 5 parts of silane coupling agent X50S, 4.0 parts of process oil, 2.0 parts of stearic acid, 1.5 parts of zinc oxide 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, 1.5 parts of vulcanization accelerator DZ, and 1.0 parts of vulcanization accelerator TBzTD.

[0078] Preparation process: use 1.6 liters of Banbury internal mixer (produced by FARREL company), mix rubber, carbon black and other compounds except sulfur and vulcanization accelerator for 6 minutes and heat up to 160 ° C to obtain masterbatch, and The masterbatch...

Embodiment 3

[0091] Embodiment 3: the analysis of certain unknown vulcanized rubber

[0092] Step 1. Sample preparation

[0093] Prepare the sample with a liquid nitrogen cryo-grinder to be less than 0.2mm 3 For small particles, take about 500mg of colloidal particles in the extraction tube, add 10mL of chloroform and 10 drops of potassium iodide, and place the extraction tube in a microwave extractor for 10 minutes; turn on the microwave extractor and perform microwave extraction for 15 minutes at 500W and 40°C; Turn off the extractor, wait for about 30 minutes, take out the extraction tube, and pipette 1 μL of the extract into the GC / MS system for analysis.

[0094] Step 2. GC-MS test

[0095] The chromatographic conditions are: TR-5MS (30m*0.25mm*0.25μm) chromatographic column; the control program of the column temperature is: the initial temperature is 50°C, rises to 310°C at 10°C / min, and maintains for 10min. Carrier gas: He; carrier gas flow rate: 1mL / min. Chromatography mass spe...

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Abstract

The invention provides a method for identifying organic sulfides in rubber. The method comprises the following steps of: step 1, sample preparation: making a rubber or rubber additive sample into particles of less than 2 mm 3, and dissolving or extracting the sample with an organic solvent; step 2, GC-MS test: using a gas chromatography-mass spectrometer to detect the mass spectrum of the solution; step 3, characteristic ion extraction and extraction substance judgment; step 4, metal element determination; and step 5, organic sulfide structure judgment. The method has simple processing steps,fast analysis speed and consistent chromatographic conditions, and can simultaneously identify various components in the product, and is especially suitable for identification and detection of unknownsamples.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to an identification method of organic sulfides in rubber, especially an identification method of organic sulfides in vulcanized rubber, where the organic sulfides are mainly alkylene disulfides. Background technique [0002] Since the beginning of the 21st century, my country's rubber additives industry has vigorously strengthened the adjustment of product structure, replacing toxic and harmful products with green and environmentally friendly products has become the primary task of the rubber additives industry, and a large number of applications of various new additives have emerged. [0003] Rubber is a chain-like polymer material, adding a vulcanizing agent can cause a cross-linking reaction with it to form a three-dimensional network structure, making the rubber change from a plastic material to an elastic material, making the rubber highly elastic and flexible in a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/7206G01N2030/067G01N2030/062G01N2030/025Y02W30/62
Inventor 房彩琴高剑琴王璨刘慧娜李秋荣胡小娜艾相豪董栋张宁
Owner BEIJING RED AVENUE INNOVA
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