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Environment-friendly preparation method of high-dispersity insoluble sulfur

A high-dispersion and sulfur technology, applied in the preparation/purification of sulfur, can solve the problems of affecting the wear resistance of rubber products, poor dispersion of insoluble sulfur, corrosion of carbon steel equipment, etc., to achieve a unique and novel method, high heat resistance Sexuality, low toxicity effect

Inactive Publication Date: 2016-06-22
CHANGZHOU DAAO NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem that the present invention mainly solves: for the poor dispersibility of insoluble sulfur in rubber at present, has directly influenced the wear resistance of rubber product, and although the commonly used carbon disulfide extraction agent is big to the solubility of soluble sulfur, separation efficiency is high, but Still there is easy to generate static electricity, corrosive to carbon steel equipment, flammable and explosive, toxic to human body, expensive, and the current situation that solvent recovery is also very difficult. A kind of self-made chlorinated polystyrene is provided as an initiator first, It is compounded with sulfur and melted at high temperature, after being cooled by extracting refrigerant and extracted by compound extractant, the surface is sprayed and modified with stearic acid and polyethylene glycol, and finally oil-extended to obtain highly dispersed and insoluble sulfur. The environmentally friendly preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0027]First add 10g of cuprous chloride, 20mL of styrene, 5mL of diethylene glycol dimethyl ether and 40mL of carbon tetrachloride successively in a 500mL three-necked flask. After the addition is complete, feed nitrogen into the bottle at a rate of 10mL / min until After exhausting the air in the bottle, seal it; then put the sealed three-neck flask into an incubator, set the temperature at 65°C, keep it warm for 10 hours, add 20mL of absolute ethanol to the reaction solution, let it settle overnight, and precipitate a light yellow Chlorinated polystyrene, filter and collect the filtrate, put it in an oven and dry it to constant weight at 105°C; then weigh 500g of sulfur and 5g of the above-mentioned dried chlorinated polystyrene, mix them evenly, put them in a high-temperature reaction kettle, and stir Stir with a rod, add 3g of composite stabilizer during the stirring process, heat up to 200°C, keep the temperature for 2 hours, and make the material in a molten state, wherein ...

example 2

[0030] First add 15g of cuprous chloride, 25mL of styrene, 8mL of diethylene glycol dimethyl ether and 45mL of carbon tetrachloride successively in a 500mL three-necked flask, and feed nitrogen into the bottle at a rate of 10mL / min after the addition, until After exhausting the air in the bottle, seal it; then put the sealed three-neck flask into an incubator, set the temperature at 60°C, and keep it warm for 11 hours, then add 25mL of absolute ethanol to the reaction solution, let it stand for precipitation overnight, and precipitate a light yellow color Chlorinated polystyrene, filter and collect the filtrate, put it in an oven and dry it to constant weight at 108°C; then weigh 550g of sulfur and 8g of the above-mentioned dried chlorinated polystyrene, mix them evenly, put them in a high-temperature reaction kettle, and stir Stir with a rod, add 4g of composite stabilizer during the stirring process, heat up to 250°C, keep the temperature for 2.5h, and make the material in a ...

example 3

[0033] First add 20g of cuprous chloride, 30mL of styrene, 10mL of diethylene glycol dimethyl ether and 50mL of carbon tetrachloride successively in a 500mL three-necked flask. After the addition is complete, feed nitrogen into the bottle at a rate of 10mL / min until After exhausting the air in the bottle, seal it; then put the sealed three-neck flask into an incubator, set the temperature at 75°C, keep it warm for 12 hours, add 30mL of absolute ethanol to the reaction solution, let it settle overnight, and precipitate a light yellow Chlorinated polystyrene, filter and collect the filtrate, put it in an oven and dry it to constant weight at 110°C; then weigh 600g of sulfur and 10g of the above-mentioned dried chlorinated polystyrene, mix them evenly, put them in a high-temperature reaction kettle, and stir Rod is stirred, and 5g composite stabilizer is added in the stirring process, is heated up to 300 ℃, heat preservation reaction 3h, makes material be molten state, and wherein...

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Abstract

The invention discloses an environment-friendly preparation method of high-dispersity insoluble sulfur, belonging to the technical field of sulfur preparation. The preparation method comprises the following steps: preparing chlorinated polystyrene as an initiator, compounding the chlorinated polystyrene with sulfur, melting at high temperature, cooling by a cooling agent, extracting by a composite extractant, carrying out surface spray modification on stearic acid and polyethyleneglycol, and finally, extending oil, thereby obtaining the high-dispersity insoluble sulfur. The example proves that the method is simple to operate and lowers the production cost; the mixed solvent is used instead of carbon bisulfide as the extractant, so that the method has the advantages of low operation risks, low toxicity and recoverable solvent and is not corrosive for carbon steel equipment; and the dispersity of the insoluble sulfur in rubber is obviously enhanced, and the wear resistance of the rubber product is enhanced.

Description

technical field [0001] The invention discloses an environment-friendly preparation method of highly dispersed insoluble sulfur, which belongs to the technical field of sulfur preparation. Background technique [0002] Insoluble sulfur (abbreviated as IS) molecular formula: Su, is a non-toxic, flammable yellow powder, named for its insolubility in carbon disulfide. It has the viscoelasticity and molecular weight distribution of polymers, so it is also called elastic sulfur or polymeric sulfur. Its relative molecular weight is 3200-40000, and it belongs to inorganic polymer chemical raw materials. [0003] Insoluble sulfur, which is mainly used as a high-grade accelerator and vulcanizing agent in the rubber industry, is widely used in the production of tires and other rubber composite products, such as tire carcass rubber, buffer rubber, white sidewall rubber and turnover rubber. It can also be used in rubber materials such as tires, hoses, tapes and other rubber and skeleton...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K3/06C08L21/00C01B17/12
CPCC08K3/06C01B17/12C01P2004/60C01P2006/32C01P2006/80C08L2201/08
Inventor 王力威张帆林大伟
Owner CHANGZHOU DAAO NEW MATERIAL TECH CO LTD
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