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Detection method for vulcanization accelerator diphenylguanidine terminal point

A technology of vulcanization accelerator and detection method, which is applied in the direction of analyzing the material through chemical reaction and analyzing the material through observing the influence of the chemical indicator. The effect of simple steps and simple steps

Inactive Publication Date: 2016-02-24
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the oxygen oxidation method, the determination of the end point of the diphenylguanidine product is confirmed by the absence of diphenylthiourea in the reaction system. According to the solubility of diphenylguanidine and diphenylthiourea, the materials in the oxidation kettle are generally washed with water, Ethanol is dissolved, and if it is clear and transparent, it is judged as the end point. However, because diphenylthiourea has a certain solubility in ethanol, in the actual production process, although the end point material is clear and transparent after being dissolved in ethanol, the actual reaction may not reach the end point.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Take the diphenylguanidine product with an initial melting point of 144°C as a standard sample, take the reaction material from the oxidation kettle and wash it with water, take two medicine spoons of the washed material, put it into a colorimetric tube, and add 1.0mol / L of 25ml of hydrochloric acid, fully shake to dissolve it, after standing for 20min, compared with the standard sample, there are obviously insoluble flocs in the colorimetric tube, and it is relatively turbid, and the washed material is dried according to GB / T11409-2008: 3.1 It is stipulated that the initial melting point for testing is 142.1°C.

Embodiment 2

[0013] Take the diphenylguanidine product with an initial melting point of 144°C as a standard sample, take the reaction material from the oxidation kettle and wash it with water, take two medicine spoons of the washed material, put it into a colorimetric tube, and add 1.0mol / L of 25ml of hydrochloric acid, fully shake to dissolve, after standing for 20min, compared with the standard sample, there is no obvious insoluble floc in the colorimetric tube, and the dissolution is clear, and the washed material is dried according to GB / T11409-2008: 3.1 It is stipulated that the initial melting point for testing is 144.4°C.

Embodiment 2

[0015] Take the diphenylguanidine product with an initial melting point of 144°C as a standard sample, take the reaction material from the oxidation kettle and wash it with water, take two medicine spoons of the washed material, put it into a colorimetric tube, and add 1.0mol / L of 25ml of hydrochloric acid, fully oscillate to make it dissolve, after standing for 20min, compared with the standard sample, there is no insoluble floc in the colorimetric tube, it dissolves and clarifies, and the washed material is dried according to GB / T11409-2008: 3.1. The detected initial melting point was 145.2°C.

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Abstract

The invention relates to the technical field of production of diphenylguanidine, and in particular discloses a detection method for a vulcanization accelerator diphenylguanidine terminal point. The detection method takes a washed material in an oxidation pot in the production of diphenylguanidine as a detection object, and is characterized by comprising the steps of taking two medicine spoons of the material and putting into a colorimetric tube, adding 25ml of hydrochloric acid of 0.5 to 1.0mol / L into the colorimetric tube, vibrating adequately, enabling the material to dissolve, standing for 20 minutes, and comparing with a standard sample, wherein if the phenomena are consistent, the material is considered to be in a state of reaching the terminal point, if insoluble floccules exist or the material is relatively turbid compared with the standard sample, the material is considered to be in a state of not reaching the terminal point, and the reaction is continued. The detection method is simple in step, easy to operate, accurate in terminal point phenomenon judgement, is suitable for being widely promoted and applied, and the yield of acceptable products is facilitated.

Description

(1) Technical field [0001] The invention relates to the technical field of diphenylguanidine production, in particular to a method for detecting the endpoint of a vulcanization accelerator diphenylguanidine. (2) Background technology [0002] At present, the commonly used method for producing vulcanization accelerator diphenylguanidine products in the industry is the oxygen oxidation method. The production process is to put diphenylthiourea, ammonia water, and catalysts into the beating kettle. Oxidation is carried out under pressure conditions. During the oxidation process, the surface molecules of diphenylthiourea are in full contact with ammonia water and oxygen, and the reaction is first performed to produce DPG molecules that fall off from the surface of CA. During the reaction, the sheet-like CA is separated layer by layer. After the reaction, the reaction reaches the end point. In the oxygen oxidation method, the determination of the end point of the diphenylguanidin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/82
CPCG01N21/82
Inventor 薛香菊吴艳萍沙德昌冯秀兰谢耿柱董玉伟
Owner SHANDONG SUNSINE CHEM