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Terminal carboxyl group SBS, preparation and application thereof in asphalt modification

A carboxyl-terminated, asphalt technology, applied in the field of preparation of carboxyl-terminated functionalized styrene/butadiene block polymers, can solve the problems of unfavorable industrial production, cumbersome operation, and many side reactions, and achieve easy industrial production and operation The effect of simple process and low production cost

Active Publication Date: 2019-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method directly uses high-purity carbon dioxide to react with the end of the active polymer to obtain a carboxyl-terminated compound. This method has more side reactions and produces a large number of diploid ketone structures and triploid alcohol structures at room temperature. In order to obtain carboxyl-terminated compounds The product is often added with a large amount of polar additives to react at -78°C, the cost is high, and the operation is cumbersome, which is not conducive to industrial production

Method used

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  • Terminal carboxyl group SBS, preparation and application thereof in asphalt modification
  • Terminal carboxyl group SBS, preparation and application thereof in asphalt modification
  • Terminal carboxyl group SBS, preparation and application thereof in asphalt modification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] 2800mL cyclohexane with N 2 Press into a 5L stainless steel polymerization kettle, add 50mL styrene, preheat to 60-65°C, use 9.1mL (0.3mol / L) n-BuLi to initiate the reaction for 30min, and use N 2 Press in 339mL of butadiene to carry out the second-stage reaction, stay at high temperature for 30min, add 50mL styrene to carry out the three-stage reaction, add 1.7mL (2mol / L) of epoxycyclohexane (the molar ratio of the added amount to the active lithium is 1.2 : 1) reacted for 30min, then added 5.4mL (2.5g / 50mL) maleic anhydride (the molar ratio of added amount to active lithium was 1:1) for capping reaction, after 30min the reaction was basically completed, and terminated with ethanol. The polymer glue was released from the kettle, and samples were taken for GPC analysis of molecular weight and distribution. Add 0.25% (accounting for dry glue mass fraction) of antioxidants 1076 and 168, stir evenly, carry out water precipitation coagulation, and dry. The prepared SBS ru...

Embodiment 2

[0081] Same as example 1, the difference is that after the three-stage reaction, add 1.4mL (2mol / L) epoxycyclohexane (the molar ratio of the added amount to active lithium is 1:1) to react for 30min, then add 5.4mL (2.5g / L) 50 mL) of maleic anhydride (the molar ratio of the added amount to the active lithium is 1:1) was subjected to a capping reaction, and the reaction was basically completed after 30 min, and terminated with ethanol. The polymer glue was released from the kettle, and samples were taken for GPC analysis of molecular weight and distribution. Add 0.25% (accounting for dry glue mass fraction) of antioxidants 1076 and 168, stir evenly, carry out water precipitation coagulation, and dry. The prepared SBS rubber block was used for the application test of asphalt modification. The number average molecular weight of SBS obtained by GPC test is 11.0×10 4 g / mol, the molecular weight distribution is 1.04.

Embodiment 3

[0085] zoom in verification

[0086]Add 1600L of preheated cyclohexane into the polymerization kettle, and control the temperature at 60-70°C. After adding 18Kg of styrene and stirring evenly, first use 0.6L (0.3mol / L) of butyllithium to break impurities. , and then add 2.18L (0.3mol / L) butyllithium to initiate a first-stage reaction. After the first-stage reaction for 30 minutes, add 84Kg butadiene for the second-stage reaction. After staying at high temperature for 30 minutes, add 18Kg styrene for the third-stage reaction, and add 110.7mL The epoxy cyclohexane (the mol ratio of addition and active lithium is 1: 1) reacts 30min, then adds 107g maleic anhydride (the mol ratio of addition and active lithium is 1: 1) carries out capping reaction, After 30 minutes, the reaction was basically completed and terminated with water. Samples were taken for GPC analysis of molecular weight and distribution. Press into the glue tank, add 0.25% (accounting for the mass fraction of dry g...

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Abstract

The invention discloses a terminal carboxyl group SBS, which has an epoxy ring opening flexible bond, an ester bond and a terminal carboxyl group and other structures. The preparation method of the terminal carboxyl group SBS is also disclosed, and active anionic SBS block polymer is prepared by using an anionic polymerization method; ring opening reaction is carried out on the anionic SBS block polymer and an epoxy hydrocarbon compound to obtain active oxygen anion SBS block polymer; terminal capping reaction is carried out on the active oxygen anion SBS block polymer and an acid anhydride compound; after the terminal capping reaction is finished, the terminal carboxyl group SBS is obtained after termination and post-treatment. Besides, the invention also discloses the application of theterminal carboxyl group SBS to asphalt modification. The terminal carboxyl group SBS can obviously improve the comprehensive performance of the asphalt and reduce a segregation value, thereby improving the transportation storage stability of modified asphalt. Besides, the preparation method of the terminal carboxyl group SBS is simple and is easy in industrialized implementation.

Description

Technical field: [0001] The invention belongs to the technical field of polymer modified asphalt, and relates to a preparation method of a carboxyl-terminated functionalized styrene / butadiene block polymer and its use in modifying asphalt to improve storage stability. technical background: [0002] Styrene-butadiene-styrene block polymer (SBS) is a thermoplastic elastomer with good elasticity, deformation self-recovery and crack self-healing properties, low-temperature plasticity, high-temperature stability and aging resistance of asphalt , Adhesion, wear resistance and service life have been significantly improved, and it has become the most commonly used road asphalt modifier in the world. However, the composition and structure of SBS and asphalt are quite different, it is difficult to form a stable system during blending, and the phase separation of polymer and asphalt is prone to occur during thermal storage. Therefore, the main disadvantage of SBS modified asphalt is th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F8/00C08L95/00C08L53/02
CPCC08F8/00C08L95/00C08L2201/08C08F293/00C08L53/025
Inventor 宋丽莉梁红文严绍敏
Owner CHINA PETROLEUM & CHEM CORP
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