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Method for producing insoluble sulfur by using liquid phase method

A liquid phase method, sulfur technology, applied in the preparation/purification of sulfur, etc., can solve the problems of poor thermal stability and dispersion, high production cost, high polymerization conversion rate, etc., to improve melting point and dispersion, and ensure high thermal stability , the effect of high insoluble sulfur content

Active Publication Date: 2013-02-06
朝阳明宇化工有限公司
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Problems solved by technology

This method has a high conversion rate of insoluble sulfur, but the reaction temperature is high, the consumption of raw materials is large, and the cost is high; it is flammable and explosive, the operation under pressure is dangerous, and the dust in the crushing process is high; and the thermal stability and dispersibility of the product All are poor; American Flex Company adopts the vaporization one-step method, which has high polymerization conversion rate, low sulfur consumption rate, high insoluble sulfur content, thermal stability and dispersibility in the product, but the melting temperature in the production process is as high as 550 ~600℃, high risk; moreover, the process is complex, the efficiency is low, and the production cost is high

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  • Method for producing insoluble sulfur by using liquid phase method

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Effect test

Embodiment 1

[0018] 1) Melting aging: Add industrial sulfur with a purity ≥ 99.9% to a melting kettle with a capacity of 8T and melt it. When the temperature in the kettle reaches 340-350°C, keep it at a constant temperature for 30 minutes, and then spray FeCl 3 +HNO 3 +H 2 O quenching liquid for quenching treatment, FeCl 3 with HNO 3 The weight percentages in the quenching liquid are 2% and 0.4% respectively, and then dried at 70-75°C for 8-9 hours to obtain 60 pieces with a weight percentage of insoluble sulfur of 40% and a weight content of soluble sulfur of 60%;

[0019] 2) Extraction: put 60 aged strips in the extraction tank with pure CS 2 Solvent extraction 3 times, each time 50min, so that the weight percentage of insoluble sulfur after extraction is ≥ 95%, that is, 90 strips with insoluble sulfur content of more than 90% and soluble sulfur content of about 10% are obtained. The used CS2 solvent can be recycling through distillation;

[0020] 3) Stabilization treatment: 0.75 k...

Embodiment 2

[0025] 1) Melting aging: Add industrial sulfur with a purity ≥ 99.9% to a melting kettle with a capacity of 8T and melt it. When the temperature in the kettle reaches 340-350°C, keep it at a constant temperature for 30 minutes, and then spray FeCl 3 +HNO 3 +H 2 O quenching liquid for quenching treatment, FeCl 3 with HNO 3 The weight percentages in the quenching liquid are 2% and 0.4% respectively, and then dried at 70-75°C for 8-9 hours to obtain 60 pieces with a weight percentage of insoluble sulfur of 40% and a weight content of soluble sulfur of 60%;

[0026] 2) Extraction: put 60 aged strips in the extraction tank with pure CS 2 Solvent extraction 3 times, each time 40min, so that the weight percentage of insoluble sulfur after extraction is ≥ 95%, that is, 90 strips with an insoluble sulfur content of more than 90% and a soluble sulfur content of about 10% are obtained. The used CS2 solvent can be recycling through distillation;

[0027] 3) Stabilization treatment: 0...

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Abstract

The invention discloses a method for producing insoluble sulfur by using a liquid phase method, which comprises the following steps of: adding sulfur into a melting kettle, keeping for 30-40 min at a temperature of 340-350 DEG C, then spraying FeCl3, HNO3 and H2O quenching liquid for quenching; extracting aged 60 strip with a CS2 solvent for 3-4 times to ensure that the content of insoluble sulphur is not less than 95 percent, wherein the aged 60 strip is extracted for 40-50min each time; stabilizing an extractant for 20-40min by using a composite stabilizing agent prepared from KCl, KClO3 and acid water solution; drying for 30-40 min at a temperature of 70-80 DEG C to ensure that the water content is controlled below 0.5 percent; charging oil for absorbing by respectively using naphthenic oil and liquid rubber after drying; and crushing oil charged adsorbate to 100-180mu to obtain the insoluble sulfur. The insoluble sulfur prepared by using the method of the invention has the characteristics of high thermal stability, high content of insoluble sulphur, high dispersibility and high thinness. The method has the advantages of simple operation, high efficiency, low cost and high safety, and is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing sulfur, in particular to a method for producing insoluble sulfur by a liquid phase method with high temperature stability. Background technique [0002] Insoluble sulfur (insoluble means insoluble in carbon disulfide, referred to as IS) is a macromolecule polymerized by hundreds of thousands or even millions of sulfur atoms. It belongs to inorganic polymers. It is a rubber vulcanizing agent with excellent performance. The surface of the finished product or semi-finished product does not spray frost and increases the adhesion, which is conducive to improving the operating environment. At the same time, it is also a good rubber vulcanization accelerator, which can accelerate the vulcanization speed and make the vulcanization even. At present, insoluble sulfur has been widely used in tire carcass rubber, buffer rubber, white sidewall rubber and the bonding rubber of skeleton materials, which can improve the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/12
Inventor 时宝成吴丽红
Owner 朝阳明宇化工有限公司
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