Preparation method of oil-filled insoluble sulphur

A sulfur and soluble technology, applied in the direction of sulfur preparation/purification, chemical instruments and methods, sulfur compounds, etc., can solve problems such as darkening of product color, high energy consumption of extraction agent recovery, and weak operation continuity, etc., to reduce Solvent loss, elimination of corrosion and waste water discharge, high volatility effect

Inactive Publication Date: 2007-09-19
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a preparation method of oil-extended insoluble sulfur in order to overcome the shortcomings of the prior art, such as poor continuity of process operation, high energy consumption for extractant recovery, and darkening of product color.

Method used

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  • Preparation method of oil-filled insoluble sulphur
  • Preparation method of oil-filled insoluble sulphur
  • Preparation method of oil-filled insoluble sulphur

Examples

Experimental program
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Effect test

Embodiment 1

[0031] 1000g of sulfur with a content of 99% and 1g of composite stabilizer (KI0.5g, styrene 0.5g) were placed in a 3L reactor, and nitrogen gas was repeatedly charged 4 times to get rid of the air in the kettle. Start the program to heat up, and after the temperature in the kettle reaches 120°C and all the raw materials are melted, turn on the stirring device on the kettle. Continue to heat up to 300°C and keep the temperature for 25 minutes. Stop stirring after the reaction, open the valve at the bottom of the kettle, and the reaction raw materials directly flow into the quenching pool from the outlet of the valve. The quenching liquid is circulating water, and the on-site water temperature is 25°C. The product is a plastic mixture of soluble sulfur and insoluble sulfur, which is transferred to a blast dryer for curing treatment, controlled at a temperature of 80°C, and dried for 6 hours. The air-dried product that loses moisture is then transferred to a ball mill for crushi...

Embodiment 2

[0034] 1000g content is the sulfur of 99% and 3g composite stabilizer (wherein MgI0.6g, 2-methylstyrene 2.4g) is placed in 3L reactor, repeatedly fills with nitrogen 4 times to get rid of the air in the still. Start the program to heat up, and after the temperature in the kettle reaches 120°C and all the raw materials are melted, turn on the stirring device on the kettle. Continue to heat up to 240°C, and keep the temperature for 60 minutes. Stop stirring after the reaction, open the valve at the bottom of the kettle, and the reaction raw materials directly flow into the quenching pool from the outlet of the valve. The quenching liquid is circulating water, and the on-site water temperature is 15°C. The product is a plastic mixture of soluble sulfur and insoluble sulfur, which is transferred to a blast dryer for curing treatment, controlled at a temperature of 60°C, dried for 10 hours, and then moved to a ball mill to grind the product after air-drying and losing moisture, and...

experiment example 3

[0037] 1000g of sulfur with a content of 99% and 5g of composite stabilizer (KI0.36g, MgI0.36g, thiazole 4.28g) were placed in a 3L reactor, and nitrogen was repeatedly charged 4 times to get rid of the air in the kettle. Start the program to heat up, and after the temperature in the kettle reaches 120°C and all the raw materials are melted, turn on the stirring device on the kettle. Continue to heat up to 270°C, and keep the temperature for 40 minutes. Stop stirring after the reaction, open the valve at the bottom of the kettle, the reaction raw materials directly flow into the quench tank from the outlet of the valve, the quench liquid is circulating water, and the on-site water temperature is 100°C (adding ice cubes to the quench tank is used to reduce the water temperature). The product is a plastic mixture of soluble sulfur and insoluble sulfur, which is transferred to a blast dryer for curing treatment, controlled at a temperature of 50°C, and dried for 15 hours. Sievin...

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Abstract

The present invention relates to a preparation method of insoluble sulfur of special vulcanizing agent used for rubber, in particular to a preparation method of oil charge type insoluble sulfur, which comprises the steps of: using ordinary sulfur as raw material which is added with composite stabilizer; putting into a reaction kettle which is provided with a heating controller and a stirring device; nitrogen blanketting; melt polymerization at 200~300 DEG C; thermal insulation for 25~120 min; quenching, curing, drying, size reduction and sieving; extracting by using a mixed solvent as extractant, centrifugal separation of the liquid after extraction, fluidized drying of the residue, and then obtaining insoluble sulfur; and then executing oil charge to obtain oil charge type insoluble sulfur with high stability. The operation has a strong continuity, the recovery energy consumption of the extractant is low and the product has high thermal stability.

Description

technical field [0001] The invention relates to the preparation of special vulcanizing agent insoluble sulfur used in rubber, in particular to a preparation method of oil-extended insoluble sulfur. Background technique [0002] Insoluble sulfur (IS) is a non-toxic polymer modified variety that is soluble in carbon disulfide and has an eight-membered ring structure and is polymerized through special processing. Insoluble sulfur is chemically inert and physically inert. It has good distribution stability in the rubber compound, uniform vulcanization and cross-linking points of the product, overcomes the "blooming" phenomenon on the surface of the rubber compound, and can prevent early scorching of the rubber compound during processing. . It is widely used in tire carcass compound, buffer compound, white sidewall compound and bonding compound of skeleton material. [0003] The preparation methods of insoluble sulfur mainly include gasification method, melting method, contact ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/12C01B17/027
Inventor 武文良王勇
Owner NANJING UNIV OF TECH
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