Analysis method of organic acid content in rubber steel wire adhesive organic acid cobalt salt

A technology of organic acid cobalt salt and analysis method, which is applied in the direction of analysis materials, measurement devices, material separation, etc., and can solve the problems that no literature and methods have been published in the analysis

Active Publication Date: 2014-10-29
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current international / national testing standards for cobalt salts of organic acids only stipulate a few test items of cobalt content, ash content, softening point, and boron content. There are no documents and methods for the analysis of various organic acids in cobalt salts of organic acids. is blank

Method used

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  • Analysis method of organic acid content in rubber steel wire adhesive organic acid cobalt salt
  • Analysis method of organic acid content in rubber steel wire adhesive organic acid cobalt salt
  • Analysis method of organic acid content in rubber steel wire adhesive organic acid cobalt salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: Quantitative analysis of organic acid in certain cobalt decanoate

[0030] 1. Quantitative analysis of organic acids with C2-C8 carbon atoms in cobalt decanoate

[0031] 1.1 Preparation of internal standard solution: Weigh 191.5mg of n-butyric acid into a 25ml volumetric flask, and dilute to volume with n-heptane.

[0032] 1.2 Sample preparation: Grind cobalt decanoate fully, weigh 15.2mg (without internal standard sample), 14.2mg, 15.6mg, 15.4mg (parallel sample) powder samples into four 10ml volumetric flasks, and use a pipette gun to accurately Pipette 500μl of internal standard solution into three parallel samples, then add 2ml of boron trifluoride-n-pentanol solution, place in 85°C water bath for 1h, add 3mL of n-heptane and shake vigorously for at least 15s, continue to add 5mL Shake the saturated sodium chloride solution well, let it stand for stratification, and take the upper layer solution for gas chromatography analysis.

[0033] 1.3 Calculati...

Embodiment 2

[0052] Embodiment 2: Quantitative analysis of organic acid in certain cobalt stearate

[0053] 1. Quantitative analysis of organic acids with C8-C22 carbon atoms in cobalt stearate

[0054] 1.1 Preparation of internal standard solution: Weigh 103.8mg capric acid into a 25ml volumetric flask, and dilute to volume with n-heptane.

[0055] 1.2 Sample preparation: Grind cobalt stearate thoroughly, weigh 15.3mg (without internal standard sample), 17.3mg, 17.8mg, 15.0mg (parallel sample) powder samples into four 10ml volumetric flasks. Use a pipette gun to accurately pipette 500 μl of internal standard solution into three parallel samples. After adding 3mL of boron trifluoride-methanol solution, place it in a water bath at 75°C for 1h, then add 5mL of n-heptane to fully shake for extraction, continue to add 10ml of saturated sodium chloride solution, shake fully and let it stand for stratification. analyze.

[0056] 1.3 Calculation results are listed in the table below:

[0057]...

Embodiment 3

[0061] Embodiment 3: Quantitative analysis of organic acid in certain cobalt boroacylate

[0062] 1. Quantitative analysis of C2-C8 organic acids in cobalt boroacylate

[0063] 1.1 Preparation of internal standard solution: Weigh 70.4mg of n-butyric acid into a 25ml volumetric flask, and dilute to volume with n-heptane.

[0064] 1.2 Sample preparation: Grind cobalt boroacylate fully, weigh 16.2mg (without internal standard sample), 16.3mg, 17.3mg, 15.6mg (parallel sample) powder samples into four 10ml volumetric flasks, and use a pipette gun Accurately pipette 300μl of internal standard solution into three parallel samples, then add 2ml of boron trifluoride-n-pentanol solution, place it in a water bath at 85°C for 1h, add 3mL of n-heptane and shake vigorously for at least 15s, continue to add Shake 5mL saturated sodium chloride solution well, let it stand for stratification, and take the upper layer solution for gas chromatography analysis.

[0065] 1.3 Calculation of results ...

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Abstract

The invention aims at providing an analytical method for the total content of free organic acid and organic acid radical ions in a rubber and steel wire bonding agent, which is simple to operate, high in accuracy of analysis result and small in error. The chemical properties of the organic acid in the cobalt salt are greatly different due to the different lengths and branching degrees of the carbon chains, so that the organic acid is difficult to quantitatively test through a single process. The analytical method is realized by the following technical scheme: when the carbon number of the organic acid is C2-C8, selecting an organic acid with the carbon number of C2-C8 as an internal standard substance, and selecting monohydric alcohol with the carbon number of C3-C8 for esterification, preferably monohydric alcohol with the carbon number of C3-C5; when the organic acid is the organic acid with the carbon number of C8-C22, selecting monohydric alcohol with the carbon number of C8-C22 as an internal standard substance, and selecting monohydric alcohol with the carbon number of C1-C8 for esterification, preferably monohydric alcohol with the carbon number of C1-C4; and when the organic acid is isocaprylic acid and neodecanoic acid, selecting the organic acid with the carbon number of C6-C18 as an internal standard substance to realize the aim of using a gas chromatography to perform compartment analysis.

Description

technical field [0001] The invention belongs to the field of steel wire adhesive materials for rubber industry, and in particular relates to an analysis method for organic acid content in rubber steel wire adhesive organic acid cobalt salts. Background technique [0002] With the development of the rubber industry, the research and production of rubber additives have attracted more and more attention. Organic acid cobalt salt plays a very important role in the bonding process of radial tire steel wire and rubber. Organic acid cobalt salt products are divided into cobalt decanoate, cobalt boroacylate, cobalt stearate and cobalt oleate. The basic structural formula is as follows: [0003] [0004] The composition and content of organic acids in cobalt organic acid salt products from different manufacturers are different. Accurate analysis of the differences in various components in cobalt organic acid salt products of the same kind has great impact on tire factory raw mate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 高剑琴王璨阮振刚刘慧娜李秋荣关云歌房彩琴赵丽丽董栋
Owner BEIJING RED AVENUE INNOVA
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