Modified sulfur, method for preparing same, apparatus for preparing same, and use thereof

Patent metadata

Field	Value
Publication number	US-2016137500-A1
Application number	US-201314900102-A
Country	US
Kind code	A1
Filing date	Jun 21, 2013
Priority date	Jun 22, 2012
Publication date	May 19, 2016
Grant date	—

Abstract

Disclosure relates to modified sulfur, preparation method thereof, preparation equipment thereof. The modified sulfur has spinnability or includes micro-structures such as fiber-, film- and network-like structure. The modified sulfur can be prepared by inducing polymerization with ultrasonic or ageing. The modified sulfur has various excellent features such as anticorrosiveness, waterproofing, strength, and fast drying and can control the features depending on its viscosity or polymerization degree. In addition due to the above features, the modified sulfur can be applied to anticorrosive or waterproofing material and can prepare anticorrosive or waterproofing material which has good workability, hardening, salt spray resistance, and weldability exceeding a certain level, and specially improved adhesiveness. Furthermore, when applying the modified sulfur to asphalt composition, gelation and depression are reduced, properties such as bending strength and tensile strength are improved, and it is possible to obtain asphalt composition with good working stability at RT.

First claim

What is claimed is:

1 . Modified sulfur comprising 100 parts by weight of sulfur and 1˜300 parts by weight of dicyclopentadiene-based modifier and having 3,000˜2,000,000 cP of viscosity at 135° C., which comprises micro-structures such as fiber, film, or network structure, or has spinnability.

2 . The modified sulfur of claim 1 which comprises 1˜200 parts by weight of initiator, based on 100 parts by weight of the sulfur.

3 . The modified sulfur of claim 2 , wherein the initiator comprises at least one selected from the group consisting of sulfur, modified sulfur, asphalt, sulfide, polysulfide, hydrocarbon compound, and their combinations.

4 . The modified sulfur of claim 2 , wherein the initiator comprises at least one selected from the group consisting of trans cinnamaldehyde, dimethylaniline, dibuthylphthalate, diiodomethane, isobutylaldehyde, methacylamide, diethylaniline, rongalite, nitroethane, formaldehyde hydrate, phenylacetamide, benzyl acetate, dodecyl benzene sulfonic acid, trioctyl amine, methylmorpholine, morpholine, dimethylaniline, napthalene and their combinations.

5 . The modified sulfur of claim 1 which comprises at least one additive selected from the group consisting of surfactant, coupling agent, catalyst, cross-linker, dispersant and their combinations.

6 . The modified sulfur of claim 5 which is mixed with the additive under solvent, and
wherein the solvent comprises at least one selected from the group consisting of water, amine-based solvent, ester-based solvent, ketone-based solvent, aliphatic or aromatic hydrocarbon-based solvent, ether-based solvent, alcohol-based solvent, polyol solvent, amide solvent, sulfone or sulfoxide solvent, acetate-based solvent, anhydrous inorganic solvent, and their combinations.

7 . The modified sulfur of claim 6 which is hydrophilic or hydrophobic.

8 . A method for preparing modified sulfur comprising:
mixing 100 parts by weight of sulfur with 1˜300 parts by weight of dicyclopentadiene-based modifier and melting them at 120° C. or higher to prepare the first mixture; polymerizing the first mixture at 120° C. or higher to prepare the first reactant; and terminating the polymerization of the first reactant at the end point of the reaction to prepare modified sulfur, wherein the end point of the reaction is between the time when the first reactant obtains spinnability and the time when rubberization of the first reactant occurs, and wherein the modified sulfur prepared after the terminating has 3,000˜2,000,000 cP of viscosity at 135° C. and comprises micro-structures such as fiber, film, or network structure, or has spinnability.

9 . The method of claim 8 , wherein the first mixture, the first reactant, and their combinations may further comprise an initiator, and
wherein the initiator is 0.1˜200 parts by weight, based on 100 parts by weight of the sulfur.

10 . The method of claim 8 which further comprises ageing the first reactant between the said polymerizing and terminating,
wherein the ageing is performed by leaving it at 40° C. or higher.

11 . The method of claim 9 , wherein the initiator comprises at least one selected from the group consisting of trans cinnamaldehyde, dimethylaniline, dibuthylphthalate, diiodomethane, isobutylaldehyde, methacylamide, diethylaniline, rongalite, nitroethane, formaldehyde hydrate, phenylacetamide, benzyl acetate, dodecyl benzene sulfonic acid, trioctyl amine, methylmorpholine, morpholine, dimethylaniline, napthalene and their combinations.

12 . A method for preparing modified sulfur comprising:
preparing a mixture comprising 100 parts by weight of sulfur, 1˜300 parts by weight of dicyclopentadiene-based modifier, and 0.1˜200 parts by weight of initiator; sonicating the mixture with ultrasonic to prepare a reactant; and ageing the reactant at 40° C. or higher to prepare the modified sulfur, wherein the modified sulfur has 3000˜2000,000 cP of viscosity and comprises micro-structures such as fiber, film, or network structure, or has spinnability.

13 . The method of claim 12 , wherein the initiator comprises at least one selected from the group consisting of trans cinnamaldehyde, dimethylaniline, dibuthylphthalate, diiodomethane, isobutylaldehyde, methacylamide, diethylaniline, rongalite, nitroethane, formaldehyde hydrate, phenylacetamide, benzyl acetate, dodecyl benzene sulfonic acid, trioctyl amine, methylmorpholine, morpholine, dimethylaniline, napthalene and their combinations.

14 . The method of claim 12 , wherein the sonicating is performed at 120° C. or lower.

15 . The method of claim 12 , wherein the sulfur is powder or melted at 120° C. or higher.

16 . The method of claim 12 , wherein the modified sulfur is prepared in continuous manner using continuous type equipment for preparing modified sulfur comprising a reaction part where the sonicating is performed and an ageing part into which the reactant discharged from the reaction part is flown.

17 . The method of claim 12 , wherein the preparing is performed by putting materials comprising 100 parts by weight of sulfur, 1˜300 parts by weight of dicyclopentadiene-based modifier, and 0.1˜200 parts by weight of initiator into a material inlet of the equipment for preparing modified sulfur;
wherein the sonicating is performed by putting a mixture comprising the said materials into the reaction part connected with the material inlet and then treating the mixture with ultrasonic generated in an ultrasonic irradiator installed in the reaction part so that a reactant is formed by reacting solid sulfur included in the mixture with the dicyclopentadiene-based modifier by cavitation that minute bubbles are formed and destructed again; and
wherein the ageing is performed by ageing the reactant flown into the ageing part from a reactant inlet connected with the reaction part to prepare the modified sulfur, and obtaining the modified sulfur prepared in continuous manner using at least one outlet part located sequentially from the reactant inlet.

18 . Equipment for preparing modified sulfur comprising:
a reaction part comprising the first housing having a material inlet and a reactant outlet, and an ultrasonic generator for sonication in the first housing; and an ageing part comprising the second housing having a reactant inlet connected with the reactant outlet and a modified sulfur outlet, an ageing container for storing the reactant in the second housing, and a temperature maintenance device for maintaining temperature in the ageing container.

19 . The equipment of claim 18 , wherein the modified sulfur outlet is formed on at least one side of the ageing container, and comprises more than 2 outlets located on different distances from the reactant inlet.

20 . The equipment of claim 18 , wherein the modified sulfur outlet comprises a low viscosity outlet, medium viscosity outlet, and high viscosity outlet formed on at least one side of the ageing container sequentially, and
wherein distance between the low viscosity outlet and the modified sulfur outlet is shorter than that between the high viscosity outlet and the modified sulfur outlet.

21 . The equipment of claim 18 which further comprises a flux controlling part for controlling flux of reactant flown into the ageing part.

22 . The equipment of claim 20 which further comprises:
a low viscosity modified sulfur storing part connected to the low viscosity outlet; a medium viscosity modified sulfur storing part connected to the mediu

Assignees

• Korea Inst Sci & Tech

Inventors

• Kim Goo Dae
• Park No Gyung
• Kwon Hyok
• Seo Young Sik
• Yu Seung Gun
• Noh Hyuk Rae

Classifications

• C04B14/36

  Inorganic materials not provided for in groups {C04B14/022 and} C04B14/04 - C04B14/34 · CPC title

• B01J2219/00168

  controlling the viscosity · CPC title

• C09D7/61

  inorganic · CPC title

• B01J2208/00575

  Controlling the viscosity · CPC title

• B01J2219/00051

  Controlling the temperature · CPC title