Analysis method of organic additives in rubber and plastic auxiliaries with rubber as carriers

An organic additive and analysis method technology, applied in the rubber and plastic industry, can solve the problems of difficult extraction and discrimination, low content, etc., and achieve the effects of fast and convenient method, high sensitivity and accuracy, and short extraction time

Active Publication Date: 2016-03-23
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In rubber and plastic additives, compared with the active ingredients and raw rubber carrier, there are more types of organic additives but less content, so it is not easy to extract and distinguish

Method used

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  • Analysis method of organic additives in rubber and plastic auxiliaries with rubber as carriers
  • Analysis method of organic additives in rubber and plastic auxiliaries with rubber as carriers
  • Analysis method of organic additives in rubber and plastic auxiliaries with rubber as carriers

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1: Analysis of organic additives in a certain rubber adhesive resorcinol 80 (R80) (product resorcinol effective content is 80%, rubber carrier content 20%)

[0026] 1.1 Take about 300mg of R80 sample, cut it into pieces, and make it smaller than 5mm 3 For the granules, put the granules in a 50mL pear-shaped bottle, add 10mL of chloroform, ultrasonic at 50°C for 15min, and let stand;

[0027] 1.2 After the sample is completely dissolved, continue to add 20mL of acetone, and conduct ultrasonic extraction at room temperature for 30min, gel blocks appear in the pear-shaped bottle, and phase separation occurs;

[0028] 1.3 Take 1 μL of the extract for detection by gas chromatography-mass spectrometry, where the detection conditions are:

[0029] The chromatographic conditions are: TR-5MS chromatographic column, column length: 30m; inner diameter: 0.25mm; film thickness: 0.25μm. The control program of the column temperature is: the initial temperature is 50°C, keep ...

Embodiment 2

[0033] Example 2: Analysis of organic additives in the rubber adhesive resorcinol 80 (R80) produced by Sanshui Taixin (the effective content of resorcinol in the product is 80%, and the rubber carrier content is 20%)

[0034] 2.1 Take about 500mg of R80 sample and cut it into pieces to make the size less than 5mm 3 granules, put the granules in a 50mL pear-shaped bottle, add 10mL tetrahydrofuran (THF), and let stand after ultrasonication for 20min at room temperature;

[0035]2.2 After the sample is completely dissolved, continue to add 20mL of ethanol, and conduct ultrasonic extraction at room temperature for 30 minutes, gel blocks appear in the pear-shaped bottle, and phase separation occurs;

[0036] 2.3 Take 1 μL of the extract for detection by gas chromatography-mass spectrometry, where the detection conditions are:

[0037] The chromatographic conditions are: HP-5MS chromatographic column, column length: 30m; inner diameter: 0.32mm; film thickness: 0.25μm. The control ...

Embodiment 3

[0041] Example 3: Analysis of organic additives in a zinc oxide 80 (ZnO80) product on the market (the effective content of zinc oxide in the product is 80%, and the rubber carrier content is 20%)

[0042] 3.1 Take 10 columnar Zn80 masterbatches and cut them into pieces to make them smaller than 5mm 3 granules, put the granules in a 100mL pear-shaped bottle, add 20mL tetrahydrofuran (THF), and put them under ultrasonication for 30min at 60°C and let them stand still;

[0043] 3.2 The sample is completely dissolved, and the upper and lower layers are layered. The white powdery insoluble matter in the lower layer is ZnO, and the viscous solution in the upper layer is a mixed solution of masterbatch, organic additives and THF; continue to add 40mL of methanol, ultrasonically extract at room temperature for 30min, and place in a pear-shaped bottle Gel blocks appear and phase separation occurs; at this time, a white ZnO solid in the lower layer appears in the pear-shaped bottle, a c...

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Abstract

An analysis method of organic additives in rubber and plastic auxiliaries with rubber as carriers specifically includes the steps of firstly, taking, 1 part by weight of sizing material master batch carrying auxiliaries, cutting the master batch into pieces, adding solvent A, and conducting ultrasonic dissolution; secondly, continuing to add solvent B for ultrasonic extraction after dissolution is completed till gel blocks appear and phase separation happens; thirdly, taking a liquid phase and gas inlet phase gas chromatograph-mass spectrometer (GC-MS) to detect the mass spectrum of liquid, and recognizing the types of the organic additives through mass spectrums of all the components. The method is rapid and convenient, qualitative analysis is conducted on the organic additives by using the GC-MS and the mass spectrums, and sensitivity and accuracy are high.

Description

technical field [0001] The invention belongs to the field of rubber and plastic industries, and in particular relates to the identification of organic additive components in rubber and plastic additives with rubber as a carrier. Background technique [0002] Rubber and plastic additives are one of the main raw materials in the rubber industry. Its history runs through the entire process of the development of the rubber / plastic industry and is inseparable from the development of the rubber / plastic industry. According to their functions, rubber and plastic additives can be roughly divided into six categories: vulcanization additives, protective additives, reinforcing additives, adhesive additives, process operation additives, and special additives. Each category contains many subcategories, involving thousands of products. For example, vulcanization aids include vulcanization agents (crosslinking agents), accelerators, activators, anti-scorch agents, etc., and accelerators ca...

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 高剑琴王璨房彩琴刘慧娜阮振刚董栋
Owner BEIJING RED AVENUE INNOVA
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