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Method for measuring content of carbonyl oxygen-containing functional groups on surface of carbon black

A functional group and carbon black technology, applied in the field of determination of carbonyl oxygen-containing functional group content, can solve problems such as large-scale equipment and complex calculations

Inactive Publication Date: 2015-11-18
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the problem that the prior art method for measuring the content of carbonyl oxygen-containing functional groups on the surface of carbon black requires large-scale equipment and complicated calculations, and provides a method for measuring the content of carbonyl oxygen-containing functional groups on the surface of carbon black by chemical titration

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  • Method for measuring content of carbonyl oxygen-containing functional groups on surface of carbon black
  • Method for measuring content of carbonyl oxygen-containing functional groups on surface of carbon black
  • Method for measuring content of carbonyl oxygen-containing functional groups on surface of carbon black

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specific Embodiment approach 1

[0074] Specific embodiment one: the method for measuring the carbonyl oxygen-containing functional group content on the surface of carbon black in this embodiment is implemented according to the following steps:

[0075] Step 1. Configuration and calibration of standard solution

[0076] Prepare and calibrate 0.1mol / L HCl standard solution, 0.1mol / L NaOH standard solution and 0.1mol / L NaOCH 2 CH 3 standard solution;

[0077] Step 2. Sample determination

[0078] ①. Take carbon black with a particle size of ≤75 μm, dry it in a vacuum oven at 120°C for 36 hours, and store it in a desiccator;

[0079] ②. Weigh 2 carbon black samples with an electronic balance and place them in No. 1 flask and No. 2 flask respectively; add excess 0.1mol / L NaOCH to No. 1 flask 2 CH 3 Standard solution, add excess 0.1mol / L NaOH standard solution to the No. 2 flask, ultrasonically disperse the solutions in the two flasks for 20 minutes, and reflux for 1.5h to 3h;

[0080] ③. Then add 0.1mol / L H...

specific Embodiment approach 2

[0107] Specific embodiment two: the difference between this embodiment and specific embodiment one is: the configuration and calibration of the HCl standard solution described in step one are carried out according to the following steps:

[0108] 1. Measure 8.4 mL of concentrated hydrochloric acid with a mass fraction of 37% and add it to 1000 mL of distilled water, shake well to obtain a hydrochloric acid solution;

[0109] 2. Burn anhydrous sodium carbonate at 270°C to constant weight, weigh 0.2g, accurate to 0.0001g, dissolve in 50mL of distilled water, add 10 drops of bromocresol green-methyl red mixed indicator;

[0110] 3. Titrate with the prepared hydrochloric acid solution until the solution changes from green to dark red, boil for 2 minutes, continue titrating after cooling to make the solution dark red again;

[0111] 4. Blank test: add 50mL distilled water to the Erlenmeyer flask, drop 10 drops of bromocresol green-methyl red mixed indicator, titrate with the prepar...

specific Embodiment approach 3

[0120] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: the configuration and calibration of the NaOH standard solution described in step one are carried out according to the following steps:

[0121] 1. Weigh 4.0g of sodium hydroxide, accurate to 0.0001g, put it in a plastic beaker, pour it into 1000mL of carbon dioxide-free water, shake it well and dissolve it to get NaOH solution;

[0122] 2. Dry the benchmark potassium hydrogen phthalate at 110°C to constant weight, weigh 0.6g, accurate to 0.0001g, dissolve it in 50mL of carbon dioxide-free water, add 2 drops of phenolphthalein indicator solution, and use step 1 Titrate the NaOH solution prepared in , until the solution is pink and keeps 30s without fading;

[0123] 3. Blank test: Add 50mL of carbon dioxide-free water to the Erlenmeyer flask, add 2 drops of phenolphthalein indicator solution, and titrate with the NaOH solution prepared in step 1 until the solution is ...

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Abstract

The invention relates to a method for measuring the content of carbonyl oxygen-containing functional groups on the surface of carbon black. The method aims at solving the problems that in the prior art, when an existing method for measuring the content of carbonyl oxygen-containing functional groups on the surface of carbon black is used, large devices are needed and calculation is complex. The method includes the steps of firstly, configuring and calibrating a standard solution; secondly, measuring a carbon black sample; thirdly, calculating the content of carbonyl oxygen-containing functional groups on the surface of unit carbon black according to the result. The method is completed through a chemical tritration method, experiment steps and calculation steps are simple, no large devices need to be used, the method is easy to implement, and the measurement result is accurate. The method is suitable for measuring the content of carbonyl oxygen-containing functional groups on the surface of carbon black.

Description

technical field [0001] The invention relates to a method for measuring the content of carbonyl oxygen-containing functional groups. Background technique [0002] The surface chemical properties of carbon black usually refer to hydrogen content, oxygen content, volatile matter, pH value, and the type and content of surface functional groups, etc., while the oxygen-containing functional groups on the surface of carbon black have the most significant impact on the properties of carbon black. It can be seen from the Fourier transform infrared spectrogram that the main surface oxygen-containing functional groups such as carbonyl, phenolic hydroxyl, carboxyl and lactone groups are combined around the huge aromatic condensed ring of carbon black. These oxygen-containing groups are hydrophilic and readily form hydrogen bonds in aqueous systems. The increase of the content of these groups is beneficial to the stable dispersion of carbon black in the aqueous system. [0003] At pres...

Claims

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Application Information

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IPC IPC(8): G01N31/16
Inventor 黎德育代洋洋田相军李宁
Owner HARBIN INST OF TECH
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