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Ageing progress testing method in insoluble sulfur preparing process

A preparation process and detection method technology, which is applied in the field of aging progress detection in the preparation process of insoluble sulfur using differential thermal analysis technology, can solve the problems of undiscovered detection method, reduced product yield, low product thermal stability rate, etc., and achieve accurate determination Aging degree, high thermal stability, good practical effect

Inactive Publication Date: 2004-12-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of insoluble sulfur generally includes processes such as polymerization and aging, pulverization and extraction, additive treatment and oil extension; aging is an important intermediate link in the entire production of insoluble sulfur; in the production process of insoluble sulfur, the viscous Elastic intermediate products, after aging heat treatment, the product becomes hard and brittle in shape, and the three-dimensional structure of polymerized sulfur molecules changes microscopically; only after proper aging treatment, the final product of insoluble sulfur can have better thermal stability; If the aging treatment is incomplete, the thermal stability of the final product will be low, and if the aging treatment is excessive, the product yield will be reduced
[0004] At present, in the relevant literature on the preparation and production of insoluble sulfur at home and abroad, there is no report on the detection method in the aging treatment

Method used

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  • Ageing progress testing method in insoluble sulfur preparing process
  • Ageing progress testing method in insoluble sulfur preparing process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a box-type aging processor with a processing capacity of 100 kg / batch, a batch of samples has been aged at a certain temperature for 3 hours; 5 grams of samples were respectively sampled from 5 different parts of this batch of samples, and a total of 25 grams of samples were taken; Finally, weigh 25 milligrams of the sample and put it into the sample cell of the differential thermal analyzer, use air as the detection atmosphere, start from 50 ° C, increase the temperature to 160 ° C at a rate of 5 ° C per minute, and detect the differential thermal analysis spectrum at the same time. Only one strong endothermic peak and one exothermic peak were detected in the differential thermal spectrum of this sample, in which the peak value of the exothermic peak was around 115°C, and the peak value of the endothermic peak was around 125°C; between 60°C and 90°C No exothermic peak appears, indicating that this batch of aged samples has been aged completely.

[0020] Using this b...

Embodiment 2

[0022] In the same manner as in Example 1, another batch of samples aged in the aging device for 1 hour was subjected to differential thermal analysis; it was found that there was an obvious exothermic double peak between 60°C and 90°C in the differential thermal spectrum, indicating that this batch The product is not aged completely, and the insoluble sulfur product obtained after further processing in the same way as in Example 1 with this intermediate product is through between 110 ℃, under the condition of 15 minutes, the thermal stability test is carried out, and its thermal stability rate is 71.3%. The analytical spectrum of this batch of aging samples is shown in differential thermal analysis figure 2 .

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Abstract

A detection method utilizes differential thermal analysis method to judge whether ageing is completed or not based on whether obvious thermal releasing peak is occured or not at temperature of 30 degree (to 160 degreeC through determination of differential thermal analysis curve of ageing sample under the condition of using air as detection atomshere at detection temperature of 20 deg.C to 200 deg.C.

Description

technical field [0001] The invention relates to an intermediate product inspection technology for detecting whether the aging is complete in the preparation process of insoluble sulfur, in particular to a method for detecting the aging progress in the preparation process of insoluble sulfur using differential thermal analysis technology. Background technique [0002] Insoluble sulfur is a high molecular polymer of sulfur. It is named because it is insoluble in carbon disulfide. Insoluble sulfur is mainly used in rubber products such as tires, rubber shoes, hoses, and tapes. [0003] There are two methods of producing insoluble sulfur from sulfur: melting method and vaporization method. The preparation of insoluble sulfur generally includes processes such as polymerization and aging, pulverization and extraction, additive treatment and oil extension; aging is an important intermediate link in the entire production of insoluble sulfur; in the production process of insoluble su...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N25/20
Inventor 孙志强徐杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI