Quantitative determination method for carbon-carbon double bonds on surface of powder

A technology for quantitative determination and carbon-carbon double bond, which is applied in the direction of chemical analysis by titration, and can solve the problems of lack of quantitative determination methods

Inactive Publication Date: 2021-06-11
ZHEJIANG THIRD AGE MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problem of lack of quantitative determination method in the above-mentioned prior art, th

Method used

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  • Quantitative determination method for carbon-carbon double bonds on surface of powder
  • Quantitative determination method for carbon-carbon double bonds on surface of powder

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Weigh 50 g of spherical polymethylsilsesquioxane micropowder (3.0 μm in particle size) sample 1 with an analytical balance, add it to an iodine measuring bottle, add 150 mL of carbon tetrachloride and stir for later use.

[0019] Use a pipette to add 10 mL of iodine bromide solution (concentration: 0.1 mol / L) into the iodine flask, stir and place in the dark for 2 hours, then add 100 mL of distilled water and 5 mL of potassium iodide solution (concentration: 10 wt%) and shake well for later use .

[0020] Titrate with 0.1mol / L sodium thiosulfate solution and shake the iodine measuring bottle until the solution turns light yellow, add 2mL starch indicator, continue titration until the blue color disappears, repeat three groups of experiments, consume sodium thiosulfate solution The average volume is 14.5mL.

[0021] Use the same method to determine the blank control group, and consume 20.4 mL of sodium thiosulfate solution. The mass fraction (ie, content) of the vinyl ...

Embodiment 2

[0023] Use an analytical balance to weigh 50 g of angular polymethylsilsesquioxane micropowder (2.0 microns in particle size) sample 2, add it to an iodine bottle, add 150 mL of carbon tetrachloride, and stir for later use.

[0024] Use a pipette to add 10 mL of iodine bromide solution (concentration: 0.1 mol / L) into the iodine flask, stir and place in the dark for 2 hours, then add 100 mL of distilled water and 5 mL of potassium iodide solution (concentration: 10 wt%) and shake well for later use .

[0025] Titrate with 0.1mol / L sodium thiosulfate solution and shake the iodine measuring bottle until the solution turns light yellow, add 2mL starch indicator, continue titration until the blue color disappears, repeat three groups of experiments, consume sodium thiosulfate solution The average volume of 14.1mL.

[0026] Use the same method to determine the blank control group, and consume 20.4 mL of sodium thiosulfate solution. Calculated by the formula, the vinyl mass fractio...

Embodiment 3

[0028] Use an analytical balance to weigh 20 g of spherical polymethylsilsesquioxane micropowder (particle size: 1.0 μm) sample three, add it to an iodine bottle, add 30 mL of carbon tetrachloride and stir for later use.

[0029] Use a pipette to add 10 mL of iodine bromide solution (concentration: 0.1 mol / L) into the iodine flask, stir and place in a dark place for 2 hours, then add 40 mL of distilled water and 5 mL of potassium iodide solution (concentration: 10 wt%) and shake well for later use .

[0030] Titrate with 0.05mol / L sodium thiosulfate solution and shake the iodine measuring bottle until the solution turns light yellow, add 2mL starch indicator, continue titration until the blue color disappears, repeat three groups of experiments, consume sodium thiosulfate solution The average volume is 14.3mL.

[0031] Use the same method to determine the blank control group, and consume 20.3 mL of sodium thiosulfate solution. Calculated by the formula, the vinyl mass fracti...

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Abstract

The invention relates to a quantitative determination method for carbon-carbon double bonds on the surface of powder, which comprises the steps of weighing Wg of powder, adding into an iodine flask, adding an organic dispersant, and stirring; adding an excessive iodine bromide solution into the iodine flask, stirring, placing in a dark place, adding distilled water and a potassium iodide solution, and uniformly shaking; using a sodium thiosulfate solution with the molar concentration of c mol/L for titration, shaking the iodine flask till the solution becomes light yellow, adding a starch indicator, continuing the titrationtill blue disappears, repeating the experimental group for multiple times, and taking the average volume of the sodium thiosulfate solution consumed each time to be V1 mL; and taking the volume of the sodium thiosulfate solution consumed by the blank control group to be V2mL. The calculation formula of the content X% of the carbon-carbon double bonds is shown in the description. The quantitative determination method for the carbon-carbon double bonds on the surface of the powder is low in cost, high in accuracy, simple and convenient to operate, good in repeatability and suitable for determination of the content of the carbon-carbon double bonds in the polyalkyl silsesquioxane micro powder.

Description

technical field [0001] The invention relates to the content of carbon-carbon double bonds, in particular to a method for quantitatively determining the carbon-carbon double bonds on the surface of powder. Background technique [0002] Polymethylsilsesquioxane micropowder is one of the research hotspots in the downstream of organic silicon in recent years. It is a polymer microsphere with both organic and inorganic properties. It has the advantages of high wear resistance, high hardness, high melting point, smoothness, non-toxicity, and tasteless. It is widely used in rubber plastics, cosmetics, coatings, pigments, and optical products. middle. At present, there is no report on the determination of carbon-carbon double bond content on the surface of polyhydrocarbylsilsesquioxane powder. Contents of the invention [0003] In order to solve the above-mentioned problem of lack of quantitative determination method in the prior art, the present invention provides a quantitativ...

Claims

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Application Information

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IPC IPC(8): G01N31/16
CPCG01N31/16
Inventor 蒋攀张磊磊陈晨张大伟莫忆凡
Owner ZHEJIANG THIRD AGE MATERIAL TECH CO LTD
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