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Liquid chromatography method for purity of rubber vulcanization accelerator MBT

A liquid chromatography analysis and rubber vulcanization technology is applied in the field of liquid chromatography analysis of the purity of 2-mercaptobenzothiazole, a rubber vulcanization accelerator, and can solve the problems of high analysis results and large errors.

Inactive Publication Date: 2009-12-02
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the analysis method of MBT purity is mainly the acid-base titration method. Since this method detects all the acidic substances in the sample, the analysis results obtained are generally high and the error is large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] Weigh 10 mg of MBT sample with a high-angle weighing bottle, add 20 ml of 95% ethanol solution to it, put it in an ultrasonic cleaner and vibrate for 5 minutes, transfer it to a 100 ml volumetric flask after taking it out, and use 95% ethanol solution Dilute to the mark, shake well and filter; keep the room temperature at 20°C, the liquid chromatography is a VWD detector, the column model is EXTEND-C18, the liquid chromatography uses water and methanol as the mobile phase, the flow rate is 0.5ml / min, VWD detection The wavelength of the detector is 100nm, inject 10 μl of sample into the liquid chromatography with a micro injector, and the gradient program is: when the injection time is 0 to 10 minutes, the proportion of water in the mobile phase is 90%, and the proportion of methanol is 10%; At 10 to 20 minutes, the proportion of water in the mobile phase is 0%, and the proportion of methanol is 100%; at 20 to 25 minutes, the proportion of water in the mobile phase is 0%,...

example 2

[0010] Weigh 50 mg of MBT sample with a high-angle weighing bottle, add 80 ml of 96% ethanol solution into it, put it in an ultrasonic cleaner and vibrate for 10 minutes, transfer it to a 250 ml volumetric flask after taking it out, and use 96% ethanol solution Dilute to the mark, shake well, and filter; keep the room temperature at 23°C, use water and methanol as the mobile phase in liquid chromatography, the flow rate is 2.5ml / min, the wavelength of the VWD detector is 254nm, inject samples into the liquid chromatography with a micro injector 25 μl, the gradient program is: when the injection time is 0 to 10 minutes, the proportion of water in the mobile phase is 95%, and the proportion of methanol is 5%; The proportion of methyl alcohol is 95%; 20~25 minutes, the proportion of water in the mobile phase is 5%, the proportion of methanol is 95%; 25~30 minutes, the proportion of water in the mobile phase is 95%, the proportion of methanol is 5%. In this way, the purity of the...

example 3

[0012] Weigh 70 mg of MBT sample with a high-angle weighing bottle, add 100 ml of 99% ethanol solution to it, put it in an ultrasonic cleaner and vibrate for 20 minutes, transfer it to a 500 ml volumetric flask after taking it out, and use 99% ethanol solution Dilute to the mark, shake well, and filter; keep the room temperature at 27°C, use water and methanol as the mobile phase in liquid chromatography, the flow rate is 5.0ml / min, the wavelength of the VWD detector is 392nm, inject samples into the liquid chromatography with a micro injector 50 μl, the gradient program is: when the injection time is 0-10 minutes, the proportion of water in the mobile phase is 100%, and the proportion of methanol is 0%; when the injection time is 0-20 minutes, the proportion of water in the mobile phase is 10%, The proportion of methanol is 90%; 20-25 minutes, the proportion of water in the mobile phase is 10%, the proportion of methanol is 90%; 25-30 minutes, the proportion of water in the mo...

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Abstract

The invention discloses a liquid chromatography method for purity of a rubber vulcanization accelerator MBT. The method comprises the following processes: using a high-angle weighing bottle to weigh 10 to 100 milligrams of an MBT sample, adding 5 to 200 milliliters of 95 to 99 percent alcohol solution into the MBT sample, putting the mixture into an ultrasound cleaner and oscillating the mixture for 2 to 20 minutes, then taking the mixture out and transferring the mixture to a volumetric flask of 100 to 1,000 milliliters, using 95 to 99 percent alcohol to dilute the mixture to the scale, and shaking up and filtering the mixture; and keeping the mixture for 20 to 30 DEG C at room temperature, then injecting 10 to 50 mu l of sample into liquid chromatography by using a trace sample injector, and obtaining the purity of the sample MBT after 30 minutes, wherein the liquid chromatography is a VWD detector, the model of a chromatographic column is EXTEND-C18, the liquid chromatography uses water and methanol as flow phases, the flow rate is 0.5 to 5.0 milliliters per minute, the wavelength of the VWD detector is 100 to 400 nanometers, and the precision is + / -0.2 percent. The method has the advantages of simple process, high analysis result accuracy and small error.

Description

technical field [0001] The invention relates to a liquid chromatography analysis method for the purity of a rubber vulcanization accelerator 2-mercaptobenzothiazole (MBT), belonging to the technical field of rubber vulcanization accelerator MBT analysis. Background technique [0002] With the development of the rubber industry, people pay more and more attention to the research and production of vulcanization accelerators. Vulcanization accelerator plays a very important role in the rubber vulcanization process. It can greatly accelerate the reaction between rubber and vulcanizing agent, improve productivity, and at the same time improve the physical and mechanical properties of vulcanized rubber. MBT is an indispensable one in the rubber industry. main accelerator. The purity of vulcanization accelerator MBT has a great influence on the quality of downstream products. Therefore, accurate analysis of the purity of MBT is of decisive significance for the production of downst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34
Inventor 孙桂英王树华洪学斌王树领王树恒
Owner KEMAI CHEM
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