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Preparation method of ultrahigh cis-polybutadiene rubber

A technology of cis-polybutadiene and rubber, which is applied in the field of preparation of ultra-high cis-polybutadiene rubber, and can solve problems such as poor fluidity, heterogeneity, and disadvantages

Inactive Publication Date: 2017-05-31
SHAANXI JUJIEHAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This kind of rare earth catalyst is often unfavorable for transportation and continuous industrial production due to its high viscosity, heterogeneity and poor fluidity during aging.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Preparation of catalyst

[0019] The baked and dried ampoule was replaced with nitrogen several times and filled with nitrogen, and 2 mL of 0.1 mol / L Nd hexane solution and 0.1 mol / L Bd hexane solution were quantitatively injected into the ampoule respectively with a disposable syringe. and 1.0 mol / L diisobutylaluminum hydride hexane solution; binary aging the mixture in the above ampoule; measure 2 mL of 0.3 mol / L diisobutylaluminum chloride with a disposable syringe The hexane solution is injected into the above-mentioned binary aging solution, and three-way aging is carried out to obtain the Nd-based catalyst;

[0020] (2) Synthesis of BR

[0021] Into a 50 mL ampoule that was vacuum-dried and replaced with nitrogen, 30 mL of Bd hexane solution with a mass concentration of 0.1 g / mL and an aged Nd-based catalyst were added in sequence, and reacted for 20 min, and then mixed with ethanol / The hexane solution terminates the polymerization reaction, and the obtaine...

Embodiment 2

[0024] (1) Preparation of catalyst

[0025] The baked and dried ampoule was replaced with nitrogen several times and filled with nitrogen, and 2 mL of 0.1 mol / L Nd hexane solution and 0.1 mol / L Bd hexane solution were quantitatively injected into the ampoule respectively with a disposable syringe. and 1.0 mol / L diisobutylaluminum hydride hexane solution; binary aging the mixture in the above ampoule; measure 2 mL of 0.3 mol / L diisobutylaluminum chloride with a disposable syringe The hexane solution is injected into the above-mentioned binary aging solution, and three-way aging is carried out to obtain the Nd-based catalyst;

[0026] (2) Synthesis of BR

[0027] Into a 50 mL ampoule that was vacuum-dried and replaced with nitrogen, 30 mL of Bd hexane solution with a mass concentration of 0.1 g / mL and an aged Nd-based catalyst were added in sequence, and reacted for 28 minutes, and then mixed with ethanol / The hexane solution terminates the polymerization reaction, and the obt...

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Abstract

The invention relates to the technical field of functional materials and particularly relates to a preparation method of ultrahigh cis-polybutadiene rubber. The preparation method of the ultrahigh cis-polybutadiene rubber comprises the following steps: (1) carrying out nitrogen displacement on a baked and dried ampoule bottle for several times, filling the ampoule bottle with nitrogen, quantitatively injecting an Nd hexane solution, a Bd hexane solution and a diisobutylaluminium hydride hexane solution into the ampoule bottle respectively by virtue of a disposable syringe, carrying out binary ageing on mixed liquid in the ampoule bottle, measuring out a diisobutyl aluminum chloride hexane solution by virtue of the disposable syringe, injecting the diisobutyl aluminum chloride hexane solution into binary ageing liquid, and carrying out ternary ageing; and (2) sequentially adding the Bd hexane solution and an Nd-series catalyst into a 50mL ampoule bottle which is subjected to vacuum drying and nitrogen displacement, and terminating polymerization reaction, so as to prepare the ultrahigh cis-polybutadiene rubber. The cis-1,4-structural molar fraction of polybutadiene rubber prepared by virtue of the preparation method exceeds 99%, and the maximum can reach 100%. The method is simple in operation and can be easily promoted in a large scale.

Description

technical field [0001] The invention relates to the technical field of functional materials, in particular to a preparation method of ultra-high cis-polybutadiene rubber. Background technique [0002] Cis-l,4-polybutadiene rubber (BR) is one of the general-purpose synthetic rubbers. It has good elasticity, wear resistance and low temperature resistance, low heat generation, low hysteresis loss, flex resistance and crack resistance. Good performance and dynamic performance, widely used in tires, tapes, hoses, rubber shoes and other manufacturing industries. The catalysts used to synthesize BR include cobalt series, titanium series, nickel series and rare earth series. Among them, the cis-1,4-structure mole fraction of BR synthesized by rare earth catalysts can reach 98% to 99%, which is the general titanium, cobalt , Nickel catalyst can not be achieved, so it has higher stereoregularity than traditional BR, and has better green rubber strength and vulcanized rubber performan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/06C08F4/54
CPCC08F136/06C08F4/545
Inventor 李长英
Owner SHAANXI JUJIEHAN CHEM CO LTD
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