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A kind of quantitative analysis method of binding styrene content

A technology combining styrene and a certain amount, applied in the quantitative analysis combined with styrene content, combined with the quantitative analysis of styrene content determination, can solve the problems of difficulty, poor stability, and high human injury.

Active Publication Date: 2016-05-25
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the methods for detecting the content of bound styrene in rubber and rubber additives mainly include: refractive index method, ozonolysis method, spectrophotometry, infrared spectroscopy, cracking gas phase method and thermogravimetric analysis method, among which GB is the most commonly used method. / T13646-1992 "Spectrophotometric Method for the Determination of Bound Styrene Content in Rubber", but this method has the following disadvantages: (1) The sample needs to be extracted and nitrated before the determination of the Bound Styrene content, and the sample is pre-treated The treatment usually takes 22 to 26 hours, which is not only time-consuming and poor in stability, but also the nitrification treatment method used has great environmental pollution and high harm to the human body; (2) GB / T13646-1992 is used for the determination of the combined styrene content In order to ensure that the absorbance value of the test solution is between 0.3-0.8, the mass of the sample (in grams) multiplied by the estimated percentage of bound styrene is equal to 4.5
This brings difficulty or inconvenience to the actual experimental operation, and has certain limitations.

Method used

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  • A kind of quantitative analysis method of binding styrene content
  • A kind of quantitative analysis method of binding styrene content
  • A kind of quantitative analysis method of binding styrene content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Embodiment 1 (directly styrene-butadiene rubber is carried out microwave digestion treatment, then test)

[0076] Set the microwave digestion conditions as follows: power 400W, temperature 150°C, heat up to the digestion temperature in 45 minutes and keep at this temperature for 30 minutes. (1), sample pretreatment

[0077] Step 1, take styrene-butadiene rubber (manufacturer: Yanshan Petrochemical, row number: 1502, no oil-extended, combined with a theoretical value of styrene mass content of 23.5%), and cut it into a size of 2mm 3 particle. Weigh sample 1 (0.0590g) and sample 1' (0.0741g) respectively and place them in microwave digestion tanks, add 8mL of concentrated nitric acid each, and put them into microwave digestion apparatus for microwave digestion. After the digestion was completed, the solution was naturally cooled to room temperature 25° C. to obtain a reaction solution. (2) Test of bound styrene content in styrene-butadiene rubber

[0078] Sample 1 and...

Embodiment 2

[0096] Embodiment 2 (the styrene-butadiene rubber is carried out microwave extraction and microwave digestion process, then test)

[0097] Set the microwave digestion conditions as follows: power 400W, temperature 150°C, heat up to the digestion temperature in 45 minutes and keep at this temperature for 30 minutes. (1), sample pretreatment

[0098] Step 1, take styrene-butadiene rubber (manufacturer: Yanshan Petrochemical, row number: 1502, no oil-extended, combined with a theoretical value of styrene mass content of 23.5%), and cut it into a size of 2mm 3 particle. Weigh 2.0017g of sample and place it in a microwave extraction tank, add 12mL of acetone, and put it into a microwave extraction-digestion apparatus for microwave extraction (set the microwave extraction conditions as: power 400W, extraction temperature 90°C, heat up to the extraction temperature in 40min and temperature for 20 minutes). After filtering the extracted sample, dry it in a GZX-9070MBE oven at 70°C ...

Embodiment 3-4

[0106] In addition to replacing the microwave digestion conditions with a power of 800W, a digestion temperature of 180°C, raising the temperature to the digestion temperature for 45 minutes and keeping it at this temperature for 30 minutes and power of 1200W, a digestion temperature of 200°C, raising the temperature to the digestion temperature for 45 minutes and keeping it at this temperature for 30 minutes, Adopt the method identical with embodiment 1 to test, and carry out parallel sample test, and specific data is shown in Table 3.

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Abstract

The invention provides a method which comprises the following steps: firstly, adopting microwave-assisted extraction and microwave digestion to perform pretreatment on a sample containing bound styrene, and then measuring the content of bound styrene. Compared with the sample pretreatment method in GB / T13646-1992, the sample pretreatment method disclosed by the invention greatly shortens the pretreatment time, avoids environmental pollution and harms to the body of an experimenter, caused by a large amount of harmful gas generated due to the utilization of a large amount of a reagent in the traditional pretreatment method, improves the working efficiency, reduces the dosage of the reagent, decreases baseline value and improves the accuracy of the detection result.

Description

technical field [0001] The present invention relates to the technical field of analysis of rubber processing aids, in particular to a quantitative analysis method for combining styrene content, and in particular to a quantitative analysis using microwave extraction and microwave digestion methods to pretreat a sample to be tested, and then performing a quantitative analysis for determining the content of combined styrene method. Background technique [0002] In the future, the automobile industry will develop rapidly, and the consumption of tires will increase by leaps and bounds. At the same time, it will also drive the vigorous development of the rubber and rubber additives industry. Therefore, the pretreatment and quantitative analysis of rubber and rubber additives become very important. [0003] At present, the methods for detecting the content of bound styrene in rubber and rubber additives mainly include: refractive index method, ozonolysis method, spectrophotometry,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/33G01N1/44
Inventor 李秋荣胡小娜房彩琴宋传全董栋
Owner BEIJING RED AVENUE INNOVA