Novel trans-1,4-polyisoprene synthesis method with high monomer conversion rate

A technology of polyisoprene and isoprene, applied in the field of polymer synthesis, can solve the problems of affecting product quality, large stirring power, long reaction time and the like

Inactive Publication Date: 2018-10-23
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The catalyst efficiency of vanadium or vanadium/titanium catalytic system is low, the polymerization process is complicated, the viscosity of the reaction system is extremely high, the energy consumption and material consumption are high, and its cost and price are comparable to Eucommia gum, so it is difficult to obtain popularization and application; Catalyst bulk method polymerization has higher catalyst efficiency, but the stirring power is large, and low-temperature polymerization is required, the reaction time is long, and the late stage of the reaction is basically in the form of solid parti...

Method used

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  • Novel trans-1,4-polyisoprene synthesis method with high monomer conversion rate
  • Novel trans-1,4-polyisoprene synthesis method with high monomer conversion rate
  • Novel trans-1,4-polyisoprene synthesis method with high monomer conversion rate

Examples

Experimental program
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Effect test

Embodiment 1

[0027]Bake a clean 30ml polymerization tube at 100°C for 2 hours and replace it with high-purity nitrogen several times. After cooling, add isoprene monomer, n-hexane, triisobutylaluminum and The supported titanium catalyst was pre-polymerized in an ice bath at 0°C with stirring for 30 minutes, then transferred to a water bath at 30°C to continue polymerization for 6 hours, and finally injected an ethanol solution containing anti-aging agent 264 into the polymerization tube to terminate the reaction. The mixture was taken out and washed repeatedly with the above-mentioned ethanol solution to obtain a non-adhesive powdery granular polymer, which was dried in a vacuum oven at 40°C to constant weight. According to the quality of product, calculate catalyst efficiency to be 2824.1g / gTi, monomer conversion rate is 59.7%; According to 1 According to the H-NMR spectrum, the calculated trans-1,4-configuration content of the product is 98.2%, the cis-1,4-configuration content is 1.3%, ...

Embodiment 2

[0029] Bake a clean 1000ml three-neck flask at 100°C for 2 hours and replace it with high-purity nitrogen several times. After cooling, in a dry nitrogen atmosphere, first add n-hexane, triisobutylaluminum and supported titanium catalyst in sequence, and then inject A small amount of isoprene, inject the remaining isoprene after a period of time, pre-polymerize for 30 minutes under ice bath and stirring conditions at 0°C, then transfer to a water bath at 30°C to continue polymerization for 6 hours, and finally inject into a three-necked flask containing Ethanol solution of anti-aging agent 264 to terminate the reaction. The mixture was taken out and washed repeatedly with the above-mentioned ethanol solution to obtain a non-adhesive powdery granular polymer, which was dried in a vacuum oven at 40°C to constant weight. According to the quality of product, calculate catalyst efficiency to be 3094.4g / gTi, monomer conversion rate is 65.3%; According to 1 According to the H-NMR sp...

Embodiment 3

[0031] The polymerization method is the same as that of Example 1, except that the polymer is polymerized in a water bath at 60° C., and after post-treatment, a block polymer is obtained. According to the quality of product, calculate catalyst efficiency to be 2851.1g / gTi, monomer conversion rate is 60.2%; According to 1 According to the H-NMR spectrum, the calculated trans-1,4-configuration content of the product is 98.3%, the cis-1,4-configuration content is 1.0%, and the 3,4-configuration content is 0.7%.

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Abstract

The invention relates to a preparation method of trans-1,4-polyisoprene (TPI). A supported titanium catalyst is used to catalyze polyisoprene polymerization, and a solution-slurry method is adopted tosynthesize powdery or block shaped trans-1,4-polyisoprene (TPI). The catalysis efficiency and monomer conversion rate are high, and the method has reached the industrialization standards. The synthesized TPI has the advantages of high hardness and excellent dynamic properties and can be easily crystallized at a room temperature. TPI has a wide application range. In a zero crosslinking phase, TPIis a thermoplastic material and is used as a medical material; in a low crosslinking phase, TPI is a thermo-elastic material and is used as a shape memory material; and when the crosslinking density exceeds a certain value, TPI becomes a rubber type high elasticity material. At present, TPI has great advantages in fields of green tires and medium-high temperature damping materials, and has a greatapplication value.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, in particular to a preparation method of trans-1,4-polyisoprene and trans-1,4-polyisoprene prepared by the method. Background technique [0002] Trans-1,4-polyisoprene (Trans-1,4-polyisoprene), referred to as TPI, also known as synthetic Eucommia gum, has the same trans -1,4-configuration, the only difference is that natural Eucommia gum is end-capped with ester groups, while TPI, gutta-percha and balata gum are end-capped with hydroxyl groups. The chemical composition of TPI is exactly the same as that of natural rubber (NR), but the structure of the double bond in the molecular chain is opposite. The two methine groups of TPI are on both sides of the double bond axis, while the two methine groups of NR are on the double bond On the same side of the connecting axis, this leads to a large difference in performance between the two. The main performance is that NR is an amorphous polymer...

Claims

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Application Information

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IPC IPC(8): C08F136/08C08F4/642C08F2/06C08K5/13
CPCC08F136/08C08F2/06C08K5/13C08F4/642
Inventor 贺继东魏萌萌张伟
Owner QINGDAO UNIV OF SCI & TECH
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