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Method for analyzing absolute content of polysulfide silane coupling agent monomer

A technology of silane coupling agent and absolute content, which is applied in the direction of analyzing materials, using nuclear magnetic resonance for analysis, and measuring devices, etc., which can solve the problem of high requirements for equipment environment, lack of equipment for nuclear magnetic resonance instruments, and inability to completely feed back polysulfides Silane coupling agent quality and other issues

Active Publication Date: 2020-03-06
南京曙光精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Consider simultaneously the volatile impurity content in the polysulfide silane coupling agent, polymer content, the effective content of the component polysulfide silane coupling agent monomer expected in the polysulfide silane coupling agent product (hereinafter referred to as the absolute content ) analysis method has not been published
[0006] At present, although the relative content of monomers and polymers in silane coupling agents can be tested by the method of silicon nuclear magnetic resonance spectroscopy, general enterprises are not equipped with nuclear magnetic resonance instruments. In addition to the complicated and cumbersome daily maintenance of nuclear magnetic resonance instruments, the main reason is It is expensive, has high requirements for the equipment environment, high maintenance costs, and high testing costs, and has high requirements for the professional knowledge and skills of operators, which is not suitable for the daily production and testing needs of enterprises.
Moreover, this test method obtains the relative content of the monomer, not the absolute content, and cannot fully feedback the quality of the polysulfide silane coupling agent.

Method used

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  • Method for analyzing absolute content of polysulfide silane coupling agent monomer
  • Method for analyzing absolute content of polysulfide silane coupling agent monomer
  • Method for analyzing absolute content of polysulfide silane coupling agent monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0095] Take a "bis(3-propyltriethoxysilane) disulfide sample A" sample as a standard sample, carry out gas chromatography internal standard method, nuclear magnetic resonance silicon spectrum detection, and then carry out liquid chromatography detection. Then take a "bis(3-propyltriethoxysilane) disulfide sample B" and carry out gas chromatography internal standard method and liquid chromatography detection, and the specific detection data are shown in Table (1) and Table (2).

Embodiment 2

[0097] Similarly, with the "bis(3-propyltriethoxysilane) disulfide sample A" sample of Example 1 as a standard sample, the "bis(3-propyltriethoxysilane) disulfide sample Sample C" is detected by gas chromatography internal standard method and liquid chromatography, and the specific detection data are shown in Table (3)

Embodiment 3

[0099] Take a "bis(3-propyltriethoxysilane) tetrasulfide sample D" sample as a standard sample, carry out gas chromatography internal standard method, nuclear magnetic resonance silicon spectrum detection, and then carry out liquid chromatography detection. Then take a "bis(3-propyltriethoxysilane) tetrasulfide sample E" for gas chromatography internal standard method and liquid chromatography detection, and the specific detection data are shown in Table (4) and Table (5).

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Abstract

The invention discloses a method for analyzing the absolute content of a polysulfide silane coupling agent monomer. The analysis method comprises the steps of testing a polysulfide silane coupling agent by adopting a gas chromatography internal standard method and a nuclear magnetic resonance silicon spectrum method; and correcting the data of the nuclear magnetic resonance silicon spectrum methodby using the data of the gas chromatography internal standard method to obtain the absolute content of the total monomer of the polysulfide silane coupling agent. The method disclosed by the invention is suitable for a detection method required by daily production monitoring, is simple and convenient to operate, low in detection cost and easy to popularize and apply, can truly feed back the effective content of the monomer in the polysulfide silane coupling agent product, and solves the problem of an analysis method which puzzles polysulfide silane coupling agent production enterprises and users for a long time at present.

Description

technical field [0001] The invention relates to an analysis method for the absolute content of a polysulfide silane coupling agent monomer, which belongs to the technical field of chemical industry. Background technique [0002] Polysulfide silane coupling agent, the general formula is [(RO) n R' 3-n SiC m h 2m ] 2 S x , wherein, x=2~10, it has a hydrolyzable group, which is easily hydrolyzed to produce Si-OH, and then undergoes condensation reaction with inorganic substances to form Si-O-Si chemical bonds or hydrogen bonds (covalent bonds). It can build a bridge between chemical bonds or covalent bonds, thus acting as a coupling agent. [0003] Because the polysulfide silane coupling agent has easily hydrolyzed groups, it will inevitably encounter water or humid air during its raw material source, production and storage process, resulting in the hydrolysis of the hydrolyzable groups to form Si- Monomers with OH groups, monomers containing Si-OH groups have a tendency...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N24/08
CPCG01N30/88G01N24/08G01N2030/884
Inventor 陶再山李春华
Owner 南京曙光精细化工有限公司