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Preparation and application of styrene-conjugated diene copolymer containing active combined sulfur

A technology of conjugated dienes and conjugated dienes, which is applied in the preparation and application field of styrene-conjugated diene copolymers containing active bound sulfur, can solve the difficult-to-control sulfur reversion phenomenon, which has not been reported, and guarantees It can achieve the effect of improving physical and mechanical properties, easy to use, and easy to control the reaction without solving problems such as the optimal strength of vulcanized materials and products.

Active Publication Date: 2013-10-30
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This vulcanization method with the addition of elemental sulfur is a heterogeneous vulcanization reaction, and it is difficult to control the reversion of sulfur during the vulcanization process, which cannot guarantee the best strength of vulcanized materials and products.
[0007] So far, the use of active polysulfide-containing organosilicon compounds to couple styrene-conjugated diene copolymers has not been reported.

Method used

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  • Preparation and application of styrene-conjugated diene copolymer containing active combined sulfur
  • Preparation and application of styrene-conjugated diene copolymer containing active combined sulfur
  • Preparation and application of styrene-conjugated diene copolymer containing active combined sulfur

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Under nitrogen protection, add the mixture of the hexane-hexanaphthene mixed solvent of 2.2L and the styrene (S)-butadiene (B) of 360g in the polymerization reactor of 5 liters at 60-120 ℃, wherein Mass S / B=75 / 25, start stirring and add 12ml of 0.4mol / L butyllithium, after 30min of polymerization, then add 1.6mmol of bis-[γ-(triethoxysilyl)propyl]tetrasulfide The coupling reaction was carried out for 20 minutes, and then 1.2 g of 2,6-di-tert-butyl-p-methylphenol was added. Finally, after the polymer is condensed with water vapor to remove the solution and moisture, and then dried, the number average molecular weight of the product is measured to be 8.3×10 4 , the degree of coupling is 2.47, the molecular weight distribution index is 2.38, the melt index of the resin is 8.5g / 10min, and the combined active sulfur mass content is 0.056%. Table 1 is the physical properties of the prepared styrene-butadiene resin.

[0062] Table 1 combines the physical properties of thiobu...

Embodiment 2

[0065] Under the protection of nitrogen, at 50-90 ° C, add 2.5 L of hexane-cyclohexane and 70 g of styrene (S) to a 5-liter polymerization reactor, then start stirring and add 0.4 mol / L butyl Lithium 11mol, after 30min of polymerization reaction, add 163.3g of butadiene (S / B=3 / 7) to continue the reaction for 25min, then add 0.678mmol of bis-[γ-(trimethoxysilyl)propyl]trisulfide The coupling reaction was carried out for 20 minutes, and 1.5 g of 2,6-di-tert-butyl-p-cresol was added after discharging. Finally, after the polymer is condensed and dried with water vapor, the number average molecular weight of the product is measured to be 32×10 4 , the degree of coupling is 5.63, the molecular weight distribution index is 1.06, and the mass content of sulfur bound in the synthesized star-shaped SBS is 0.032%. Table 2 is the physical property of preparing SBS.

[0066] Table 2 Physical properties of SBS containing bound sulfur

[0067]

Embodiment 3

[0069] Under nitrogen protection, at 50-90°C, add 3.5L of cyclohexane / hexane mixed solvent and 30g of styrene (S) to a 5-liter polymerization reactor, then add 0.4mol / L 8ml of butyllithium, after 30min of polymerization reaction, add 146.4g of isoprene (S / Ip=17 / 83) to continue the reaction for 25min, then add 1.60mmol of bis-[γ-(trichlorosilyl)propyl] Tetrasulfide was subjected to coupling reaction for 20 minutes, and 0.8 g of 2,6-di-tert-butyl-p-cresol was added after discharging. Finally, after the polymer is condensed and dried with water vapor, the number average molecular weight of the product is measured to be 10.3×10 4 , the degree of coupling is 1.82, the molecular weight distribution index is 1.08, and the mass content of sulfur combined in the synthesized coupled-line SIS is 0.062%. Table 3 shows the physical properties of the prepared active sulfur-containing wire-coupled SIS.

[0070] Table 3 Physical properties of SIS containing bound sulfur

[0071]

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Abstract

The invention discloses preparation and application of styrene-conjugated diene copolymer containing active combined sulfur. A sulfur-containing silicane molecular structure is necessarily characterized in that A) the tail end of the sulfur atom is connected with the carbon atom; B) the polymerized sulfur appears in the molecule in the form of -Sn-, wherein n is in a range from 2 to 5; C) the molecule contains silicon bonds, such as -Si-R3, wherein R is alkoxy or halogen. The molecular ratio of the polymer tail end active lithium to the sulfur-containing silicane is (1-6):1, the average molecular weight of the polymer is 0.08-0.4 million, molecular weight distribution is in the form of unimodal distribution, molecular weight distribution index is 1-2.8, the mass content of the combined sulfur of the copolymer is 0.030-0.062%, the copolymer resin or the elastomer is high in strength, the copolymer crude rubber is low in cold fluidity and excellent in processability, and the vulcanized rubber is not reversed.

Description

technical field [0001] The present invention relates to the preparation and application method of styrene-conjugated diene copolymer containing active combined sulfur. Background technique [0002] Styrene and conjugated diene can be directionally polymerized into random or block copolymers under the trigger of butyllithium in a solvent, and the molecular chain can be linear or star-shaped. This material is especially suitable for thermoplastic elastomers or for manufacturing Tires or other plastic materials. In particular, it should be pointed out that some oligomers will inevitably be produced in the preparation of linear styrene-conjugated diene polymers. Mixed in granular SBS and SIS, it will stick together and agglomerate during storage, which will bring troubles to subsequent processing; if it is synthesized solution polystyrene butadiene rubber, it will produce unnecessary cold flow phenomenon during storage, showing cold flow Large (that is, the stiffness is not go...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/24C08L9/06C08K5/548B60C1/00
Inventor 张建国宁朝晖李尚英梁红文胡朝阳
Owner CHINA PETROLEUM & CHEM CORP
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