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A method for the determination of hydroxyl content in methyl vinyl raw rubber

A technology of methyl vinyl raw and hydroxyl groups in glue, applied in the field of detection, can solve the problems of increasing the number of remelting, increasing the damage rate of products, and relatively accurate testing, achieving high detection sensitivity, simple pre-treatment, and small relative deviation Effect

Active Publication Date: 2018-10-09
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The content of hydroxyl groups in raw rubber is not yet one of the indicators that must be tested for raw rubber, but it has a great impact on the rubber compound and products. Excessive hydroxyl content in raw rubber will cause the structure of the compound rubber and shorten the storage time. , increase the number of re-smelting during use, waste energy and manpower, in addition, it will cause difficulty in demoulding the product and increase the damage rate of the product
[0003] There are three methods for testing the content of silicon hydroxyl groups: lithium aluminum hydride method, Karl Fischer method and infrared spectroscopy. The hydroxyl content is relatively high, and the test can be relatively accurate. Infrared spectroscopy requires a standard sample with known hydroxyl content, and the determination of trace hydroxyl content requires harsh conditions to eliminate the influence of trace moisture in the environment. For this trace of silanol The content test has not been reported yet

Method used

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  • A method for the determination of hydroxyl content in methyl vinyl raw rubber
  • A method for the determination of hydroxyl content in methyl vinyl raw rubber
  • A method for the determination of hydroxyl content in methyl vinyl raw rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Raw rubber treatment:

[0047] Weigh 50g of vinyl-terminated methylvinyl raw rubber sample, put it into a flask, add 100g of toluene, after it is completely dissolved, add 4.0g of hexamethyldisilazane, stir at 80°C for 4 hours, and then release the volatile components , get sample X1;

[0048] Weigh 50g of vinyl-terminated methyl vinyl raw rubber sample, put it into a flask, add 100g of toluene, after it is completely dissolved, add 5.0g of hexamethyldisilazane, stir at 100°C for 3h, and then release the volatile components , get sample X2;

[0049] Weigh 50g of vinyl-terminated methylvinyl raw rubber sample, put it into a flask, add 100g of toluene, after it is completely dissolved, add 7.5g of hexamethyldisilazane, stir at 110°C for 2 hours, and then remove volatile components , to obtain sample X3.

Embodiment 2

[0051] Standard sample configuration:

[0052] The known O-SiMe 3 10.0345 g of methyl silicone oil with a content of 0.684% was dissolved in 100.96 g of octamethylcyclotetrasiloxane to make a standard sample Z1, and the content of trimethoxysilyl in the standard sample was 0.062%;

[0053] The known O-SiMe 3 10.5482g of methyl silicone oil with a content of 0.684% was dissolved in 80.94g of octamethylcyclotetrasiloxane to make standard sample Z2, and the content of trimethoxysilyl in the standard sample was 0.079%;

[0054] The known O-SiMe 3 10.8350 g of methyl silicone oil with a content of 0.684% was dissolved in 151.32 g of octamethylcyclotetrasiloxane to prepare standard sample Z3, and the content of trimethoxysilyl in the standard sample was 0.046%.

Embodiment 3

[0056] Weigh 0.1181g of standard sample Z1 into a 20mL headspace bottle and then add 3mL of 2g / L ethoxylation reagent. Weigh the sample in Example 1, take 0.1025g sample X1, 0.1183g sample X1, 0.1075g sample X1, add respectively in three 20mL headspace vials, then add 3mL 2g / L of Ethoxylation reagent. Weigh 0.1224g of raw rubber sample C into a 20mL headspace bottle, and then add 3mL of 2g / L ethoxylation reagent. After the above headspace bottle is sealed, shake it until the sample is completely dissolved.

[0057] Sample analysis:

[0058] Place the above headspace vial into the headspace sampler:

[0059] The operating conditions of the gas chromatograph with a hydrogen flame detector are: inlet temperature: 200°C; split ratio: 10:1; septum purge rate: 3mL / min; initial temperature: 45°C; 5°C / min; final temperature: 200°C; hydrogen flow rate: 30mL / min; gas supply: 20mL / min.

[0060] Headspace sampler operating procedures: furnace temperature: 60°C; transfer line temperat...

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Abstract

The invention relates to a detection method, and concretely relates to a method for detecting the content of hydroxyl groups in methyl vinyl raw rubber. The method comprises the following steps: 1, processing a vinyl-terminated methyl vinyl raw rubber sample C by adopting hexamethyldisilazane to convert Si-OH in the raw rubber into Si-O-SiMe3, and removing excessive hexamethyldisilazane to obtain a silazane processed raw rubber sample X; and 2, dissolving potassium hydroxide in ethyl orthosilicate to prepare an ethoxylation reagent Y, reacting the ethoxylation reagent Y with the sample X to form volatile Me3SiOEt, adopting headspace injection gas chromatogram to carry out quantitative analysis, correcting through an external standard technology, and calculating to obtain the content of hydroxyl groups in the raw rubber. The method has the advantages of simplicity in pretreatment, no strict detection environment, high sensitivity, small relative deviation and good repeatability.

Description

technical field [0001] The invention relates to a detection method, in particular to a method for determining the hydroxyl content in methyl vinyl raw rubber. Background technique [0002] The content of hydroxyl groups in raw rubber is not yet one of the indicators that must be tested for raw rubber, but it has a great impact on the rubber compound and products. Excessive hydroxyl content in raw rubber will cause the structure of the compound rubber and shorten the storage time. , Increase the number of re-smelting during use, waste energy and manpower, in addition to cause difficulty in demoulding the product, and increase the damage rate of the product. [0003] There are three methods for testing the content of silicon hydroxyl groups: lithium aluminum hydride method, Karl Fischer method and infrared spectroscopy. The hydroxyl content is relatively high, and the test can be relatively accurate. Infrared spectroscopy requires a standard sample with known hydroxyl content...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 刘海龙许栋石科飞
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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