Method for preparing insoluble sulfur

A technology of sulfur and solubility, which is applied in the field of preparation of insoluble sulfur as a vulcanizing agent, can solve the problems of volatile, high toxicity, and unexplained recovery, and achieve the effects of accelerating cooling, preventing high temperature reduction, and avoiding flammability

Inactive Publication Date: 2013-03-20
TAIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent CN1769162A discloses a method for preparing high-quality insoluble sulfur. The 7020 type product filled with white oil can still reach 92% of thermal stability within 15 minutes, which is better than the samples of the same type provided by domestic and foreign manufacturers. , but the extraction agent used in the example provided is carbon disulfide, and the stabilizer and carbon disulfide are added to the extractant in a certain proportion to extract the sulfur strips, but the process of recovering carbon disulfide is not described, and carbon disulfide itself is also prone to Volatile and highly toxic
Chinese patent CN1462721 also provides a preparation method of high-quality insoluble sulfur, the preparation process is also carried out at low temperature, the extraction process is to add composite stabilizer A and composite stabilizer B to carbon disulfide at the same time, at 50-80 ° C Under heating 0.5-3.0 hour, reaction product is extracted, but because mentioned composite stabilizer A comprises metal-organic salt, composite stabilizer B comprises the olefinic organic compound with carbon-carbon double bond, may be in the final product that makes like this Metal impurities are brought into the product insoluble sulfur

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 500g of sulfur into the reactor and raise the temperature. After the temperature in the reactor reaches 160°C, turn on the stirring device on the kettle. After keeping the temperature for 10 minutes, add 4g of beeswax into the reactor from the feed port of the reactor and continue to raise the temperature. To 270°C, keep warm for 60min. After the reaction was over, the stirring was stopped, and the fan beside the reactor was turned on, and nitrogen was continuously flushed into the reactor simultaneously. A sieve plate with a thickness of 5mm, a diameter of 7cm, and a sieve plate with a hole diameter of 2mm is installed directly below the bottom valve of the reactor. When the bottom valve is opened, the reaction product flows directly into the quenching pool through the sieve hole. The quenching liquid is an ice-water mixed bath. The water temperature was measured at 3°C.

[0020] The product is a plastic mixture, which is solidified and dried in a blast drying ove...

Embodiment 2

[0022] Add 500g of sulfur into the reactor and raise the temperature. After the temperature in the reactor reaches 160°C, turn on the stirring device on the kettle. After keeping the temperature for 15 minutes, add 2.5g of acetanilide into the reactor from the feed port of the reactor, and continue The temperature was raised to 240°C, and the reaction was kept for 120 minutes. After the reaction was over, the stirring was stopped, and the fan beside the reactor was turned on, and nitrogen was continuously flushed into the reactor simultaneously. A sieve plate with a thickness of 5mm, a diameter of 8cm, and a sieve plate with a hole diameter of 3mm is installed directly below the bottom valve of the reactor. When the bottom valve is opened, the reaction product flows directly into the quenching pool through the sieve hole. The quenching liquid is an ice-water mixed bath. The water temperature was measured at 1°C.

[0023] The product is a plastic mixture, which is solidified a...

experiment example 3

[0025] Add 500g of sulfur into the reactor and raise the temperature. After the temperature in the reactor reaches 160°C, turn on the stirring device on the kettle. After keeping the temperature for 15 minutes, add 2g of acetanilide and 2g of Thiazole, continue to heat up to 260°C, and keep warm for 90min. After the reaction was over, the stirring was stopped, and the fan beside the reactor was turned on, and nitrogen was continuously flushed into the reactor simultaneously. A sieve plate with a thickness of 5mm, a diameter of 10cm, and a sieve plate with a hole diameter of 4mm is installed directly below the bottom valve of the reactor. When the bottom valve is opened, the reaction product flows directly into the quenching pool through the sieve hole. The quenching liquid is an ice-water mixed bath. The water temperature was measured at 1°C.

[0026] The product is a plastic mixture, which is solidified and dried in a blast drying oven. After the product is completely dry, i...

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Abstract

The present invention discloses a method for preparing insoluble sulfur, and the method comprises the following steps of: adding sulfur into a reactor, when the temperature in the reactor rises to 160 degrees centigrade, starting stirring, and adding a stabilizer after keeping the temperature for 10-15min; continuing to heat to a reaction temperature, actuating a fan after the reaction is terminated, simultaneously feeding nitrogen gas into the reactor, and rapidly cooling the reaction product which enters an ice water bath from sieve pores; placing the cooled product into an drying oven for curing and drying, then ball milling for crushing, adding the crushed product together with an extractant into an extraction tank to perform extraction, for residue after suction filtration, repeatedly performing the above-mentioned extraction and filtration until the final residue is substantially constant in weight, and vacuum drying the residue to obtain insoluble sulfur powder. The insoluble sulfur obtained by using the present method is not mixed with metal ions; the improvement of the reactor apparatus can accelerate the cooling of the product; and the organic solvent used is non-toxic and non-volatile.

Description

technical field [0001] The invention relates to the preparation of vulcanizing agent insoluble sulfur used in tire rubber, in particular to a method for preparing insoluble sulfur by melting at low temperature. Background technique [0002] Insoluble sulfur, also known as μ-type sulfur. The product is a light yellow powder with an amorphous structure, insoluble in organic solvents such as carbon disulfide and toluene, and is a non-toxic polymer modified by special processing and polymerization of ordinary sulfur with an eight-membered ring structure that is soluble in carbon disulfide Variety. 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 can be widely used in tire carcass rubber, buffer rub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/12
Inventor 沈敏王勇李呈宏郑紫微马丹汇王鹏朱晓琴
Owner TAIZHOU UNIV
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