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Method for measuring content of iron ions in organic silicon products

A measurement method and technology of iron ions, applied in the direction of color/spectral property measurement, etc., can solve the problems of low total iron content, difficult biochemical degradation, affecting the application range, etc., to achieve accurate detection results, avoid digestion process, and high detection accuracy. Effect

Active Publication Date: 2018-11-13
YICHANG COLLIN SILICON MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of industrial production, due to equipment corrosion and the quality of raw and auxiliary materials, the content of impurities in methylchlorosilane hydrolyzate is relatively high, which has a great impact on product quality, especially iron impurities, which directly affect the apparent color of the product , thus affecting its scope of application
[0003] At present, there is no national standard or industry standard for the detection of iron substances in methylchlorosilane hydrolyzate at home and abroad, and because methylchlorosilane hydrolyzate has low total iron content (generally less than 2ppm), high organic content, physical and chemical properties Stable, difficult to biochemical degradation and other characteristics, ordinary detection methods can not be accurately detected

Method used

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  • Method for measuring content of iron ions in organic silicon products
  • Method for measuring content of iron ions in organic silicon products
  • Method for measuring content of iron ions in organic silicon products

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Sample pretreatment: Weigh 100ml of hydrolyzate (specifically, the product after hydrolysis of dimethyldichlorosilane, including HO-[Si(CH 3 ) 2 ] n -OH and other linear siloxanes and [-O-Si(CH 3 ) 2 -] n Cyclic siloxane), 70ml of deionized water, 2ml of nitric acid, and 28ml of hydrogen peroxide were placed in a high-pressure storage tank made of steel-lined tetrafluoroethylene, and then placed in an ultrasonic cleaner at 90°C for 40 minutes of shaking and mixing; , put it into a separating funnel and let it stand for stratification; take 50ml of the lower layer liquid and transfer it to a 100ml volumetric flask, use deionized water to make up the volume, shake it up, and let it stand until the solution is clear, use a pipette to draw 50ml of the supernatant liquid for the next step One-step detection, while making a sample blank.

[0026] (2) Determination of iron standard curve: take 0.001mg / ml Fe respectively 2+ Put standard solution 0, 5, 10, 15, 20, 25ml...

Embodiment 2

[0034] (1) Sample pretreatment: Weigh 100ml of hydroxyl silicone oil, 80ml of deionized water, 2ml of nitric acid, and 18ml of hydrogen peroxide into a steel-lined PTFE high-pressure storage tank, and then put them into an ultrasonic cleaning machine and shake and mix at 40°C 80min; After the pressure is released, put it into a separatory funnel and let it stand for stratification; transfer 50ml of the lower layer liquid to a 100ml volumetric flask, use deionized water to make up the volume, shake well, and let it stand until the solution is clear, use a pipette to absorb the upper layer. 50ml of solution was used for the next step of detection, and a sample blank was made at the same time.

[0035] (2) Determination of iron standard curve: take 0.001mg / ml Fe respectively 2+ Put standard solution 0, 5, 10, 15, 20, 25ml into six 50ml colorimetric tubes, respectively add 1ml 10% hydroxylamine hydrochloride solution, 2ml 0.15% phenanthroline solution and 5ml acetic acid-sodium ac...

Embodiment 3

[0042] (1) Sample pretreatment: Weigh 100ml of DMC, 70ml of deionized water, 3ml of nitric acid, and 27ml of hydrogen peroxide, place them in a steel-lined PTFE high-pressure storage tank, then put them into an ultrasonic cleaner and shake and mix at 65°C for 60min; After the pressure is released, put it into a separatory funnel and let it stand for stratification; take 50ml of the lower layer liquid and transfer it to a 100ml volumetric flask, use deionized water to make up the volume, shake well, and let it stand until the solution is clear, use a pipette to draw 50ml of the supernatant liquid For the next step of detection, while making a sample blank.

[0043](2) Determination of iron standard curve: take 0.001mg / ml Fe respectively 2+ Put standard solutions 0, 5, 10, 15, 20, 25ml into six 50ml colorimetric tubes, respectively add 1ml 10% hydroxylamine hydrochloride solution, 2ml 0.15% phenanthroline solution and 5ml acetic acid-sodium acetate buffer solution, add water Di...

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Abstract

The invention relates to a method for measuring the content of iron ions in organic silicon products. The method includes: contrasting to an iron standard curve to pretreat an organic silicon sample,adding phenanthroline solution, and calculating the concentration of iron ions in the sample according to light absorption coefficients of a spectrophotometer. According to an ultrasonic cleaning principle, complete mixed reaction of the sample with deionized water, acidic materials and an oxidant can be realized while solution emulsification is avoided. In an acidic environment, hydrogen peroxideserves as the oxidant, main structures of products of organic silicon are unaffected while impurities in the products of organic silicon can be effectively oxidized and form ions dissolved in water,and accuracy of detection results is guaranteed. The method is simple and convenient, a long-time organic matter digestion process is avoided, high detection precision is realized, and expensive ICP detection is avoided.

Description

technical field [0001] The invention belongs to the technical field of organosilicon production, in particular to a method for measuring total iron content in organosilicon products. Background technique [0002] Organosilicon products are a class of organic materials that combine the performance of inorganic materials and organic materials. They have basic properties such as low surface tension and small viscosity-temperature coefficient, and have excellent characteristics such as high and low temperature resistance, electrical insulation, and oxidation resistance. They are widely used in aerospace , electronics, construction and other industries. There are many kinds of organic silicon products, according to incomplete statistics, there are more than 10,000 kinds, and more than 90% of them are synthesized from methyl chlorosilane hydrolyzate. In the process of industrial production, due to equipment corrosion and the quality of raw and auxiliary materials, the content of ...

Claims

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Application Information

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IPC IPC(8): G01N21/31
CPCG01N21/31
Inventor 王文金杜宏伟李聪
Owner YICHANG COLLIN SILICON MATERIAL CO LTD