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Insoluble sulfur and its preparation method and oil-extended insoluble sulfur and its application and ionic liquid as a stabilizer

A technology of ionic liquid and sulfur, which is applied in the preparation/purification of sulfur, can solve the problem of unsatisfactory stabilization effect of stabilizers for insoluble sulfur, and achieve the effect of avoiding inaccurate measurement and high stability

Active Publication Date: 2016-08-31
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the invention is to overcome the technical problem that the stabilizing effect of the existing insoluble sulfur stabilizer is still unsatisfactory

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0035] The present invention also provides a preparation method of insoluble sulfur, which comprises heating and melting the raw material sulfur and performing polymerization, and rapidly cooling the mixture obtained by the polymerization, wherein the polymerization is carried out in the presence of ionic liquid. The preparation method of the present invention can improve the stability of the prepared insoluble sulfur by polymerizing the raw material sulfur in the presence of the ionic liquid. The types of anions and cations of the ionic liquid have been described in detail above, and will not be described in detail here.

[0036] The amount of the ionic liquid used depends on the amount of raw sulfur, and is not particularly limited. Generally, relative to 100 parts by weight of raw sulfur, the amount of the ionic liquid can be 0.01-1 part by weight, preferably 0.01-0.5 part by weight, more preferably 0.01-0.1 part by weight, and even more preferably 0.02-0.05 part by weight ...

Embodiment 1

[0054] (1) Melt polymerization reaction

[0055] Add 2.0kg of industrial sulfur with a purity of >99.9% to a 2L reaction kettle, pass through nitrogen protection, raise the temperature to 135°C, keep it for 10 minutes, and then add [EMIM]Cl (i.e., 1-ethyl-chloride 3-methylimidazole) and white carbon black (volume average particle size of 100nm). Wherein, relative to 100 parts by weight of industrial sulfur, the amount of [EMIM]Cl is 0.04 parts by weight, and the amount of white carbon black is 0.03 parts by weight. After stirring evenly, the temperature was raised to 240° C. and kept for 15 minutes to carry out the polymerization reaction.

[0056] (2) Quenching

[0057] After the reaction was finished, the liquid mixture in the reactor was sprayed into a 10kg ice-water bath with high-pressure nitrogen as the carrier gas.

[0058] (3) dry

[0059] The solid mixture was separated from the ice-water bath, and placed in a blast drying oven at a temperature of 60° C. for 4 hou...

Embodiment 2

[0066] The same method as in Example 1 was used to prepare insoluble sulfur and extend it with oil, except that in step (1), white carbon black was not used.

[0067] After testing, the obtained oil-extended insoluble sulfur has a stability of 78% at 105°C / 15min and a stability of 40% at 120°C / 15min.

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Abstract

The invention relates to insoluble sulfur, a preparation method thereof, oil-charged insoluble sulfur and application of oil-charged insoluble sulfur. According to the application, ionic liquid is taken as a stabilizer of the insoluble sulfur and is particularly taken as the stabilizer of raw material sulfur melt polymerization reaction, so that the heat stability of the prepared insoluble sulfur can be obviously improved. Particularly, when ionic liquid is taken as the stabilizer for use in the raw material sulfur melt polymerization reaction, the stability of the final prepared insoluble sulfur at 105 DEGC / 15min can reach above 75%, and the stability of the final prepared insoluble sulfur at 120 DEGC / 15min can reach above 40%.

Description

technical field [0001] The present invention relates to the application of ionic liquid as insoluble sulfur stabilizer. The invention also relates to an insoluble sulfur and its preparation method and oil-extended insoluble sulfur. The present invention further relates to the use of the insoluble sulfur and the oil-extended insoluble sulfur as vulcanizing agents. Background technique [0002] Insoluble sulfur, also known as polymeric sulfur, is a long-chain polymer formed by ring-opening polymerization of ordinary sulfur (ie, raw material sulfur), and is named for its insolubility in carbon disulfide. Different from ordinary sulfur, insoluble sulfur has little solubility in rubber. Therefore, insoluble sulfur is mainly used as a rubber vulcanizing agent and is widely used in the production of high-grade tires and other rubber products without worrying about blooming. The preparation methods of insoluble sulfur mainly include high-temperature gas-phase method and low-temper...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/12C08K3/06
Inventor 吴立报胡伟庆刘清华严俊黄婉利罗望群李大念姚思涵王晨栋
Owner CHINA PETROLEUM & CHEM CORP
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