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Method for detecting low hydroxyl content in low-moisture-interference modified white carbon black

A detection method and technology of white carbon black, applied in the field of chemical analysis, can solve the problem of inability to accurately detect the hydroxyl content of low hydroxyl content

Active Publication Date: 2021-02-05
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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Problems solved by technology

[0006] Aiming at the deficiencies of the existing technology, especially the problem that the hydroxyl content in modified silica with low hydroxyl content cannot be accurately detected, the present invention provides a method for detecting low hydroxyl content in modified silica with low moisture interference

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  • Method for detecting low hydroxyl content in low-moisture-interference modified white carbon black
  • Method for detecting low hydroxyl content in low-moisture-interference modified white carbon black
  • Method for detecting low hydroxyl content in low-moisture-interference modified white carbon black

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Embodiment Construction

[0010] The present invention is achieved through the following technical solutions:

[0011] A method for detecting low-hydroxyl content in low-moisture interference modified white carbon black, comprising the steps of:

[0012] a. Preparation of standard samples:

[0013] Using diphenylsilanediol as the standard substance, take different quality standard substances and dilute them with dry tetrahydrofuran to obtain standard solutions with different concentrations. Put the headspace bottle at 110-130 Heat in a heating bath at ℃ for 2 hours, seal the cap while it is hot, and after cooling, inject standard solutions and reaction solutions of different concentrations into the headspace vials to obtain standard samples;

[0014] b. Preparation of blank sample

[0015] Heat the headspace bottle in a heating bath at 110-130°C for 2 hours at a humidity of ≤20% under nitrogen protection, seal the cap while it is hot, and inject the reaction solution into the headspace bottle after c...

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Abstract

The invention relates to a method for detecting the content of low hydroxyl in low-moisture-interference modified white carbon black. The method comprises the following steps: selecting diphenyl silanediol as a standard sample, heating a standard sample and modified silicon dioxide in a dry nitrogen (less than or equal to 5ppm moisture) environment respectively, carrying out closed reaction, carrying out quantitative analysis by headspace-gas chromatography, and performing correcting by an external standard method, and carrying out comparing with the standard sample to obtain the content of hydroxyl in the modified silicon dioxide. The instrument detection method for the hydroxyl content in the modified silicon dioxide is established by optimizing chromatographic conditions of a headspacesample injector and a gas chromatograph and manufacturing a diluted Grignard reagent and a closed reaction system; methodology verification experiments show that the established method is high in accuracy, resistant to environmental moisture interference and good in reproducibility (relative standard deviation being smaller than 5%), and the quality of hydroxyl in the modified silicon dioxide canbe effectively detected.

Description

technical field [0001] The invention relates to a method for detecting low hydroxyl content in low-moisture interference modified white carbon black, and belongs to the technical field of chemical analysis. Background technique [0002] Fumed silica is nano-silica with surface hydroxyl groups and adsorbed water generated after high-temperature hydrolysis of silicon halides. Since fumed silica is obtained by hydrolysis and polycondensation of halosilanes, there are still residual There are many silanols (Si-OH) on the surface of silica and inside the aggregates. The remaining silanols in the aggregates need to be removed at a higher temperature and are difficult to detect, but they have little effect on the performance of the product. The activity of silicon hydroxyl groups on the surface is relatively high, which has a great impact on the performance of the product. Therefore, the content of hydroxyl groups in silica is a very important technical indicator. It is used in dif...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/16G01N30/86
CPCG01N30/02G01N30/06G01N30/16G01N30/8675G01N2030/047G01N2030/067
Inventor 伊港石科飞孙江刘海龙张学迪肖月玲
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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