Method for preparing beta-pinene polymer using alpha-diimine nickel complex as catalyst

A technology for nickel complexes and polymers is applied in the field of preparing high-molecular-weight beta-pinene polymers, and can solve the problems of complex post-processing process, low molecular weight of poly-beta-pinene, and large dosage, etc.

Inactive Publication Date: 2006-12-27
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, there are following disadvantages in the cationic polymerization of β-pinene under Lewis acid catalysis: (1) in order to obtain the polymkeric substance with practical use molecular weight, polymerization must be carried out under lower temperature (n In the range of 1000 to 4000), this limits the application of β-pinene resin as a tackifier or filler in materials with high heat resistance requirements (such as high temperature hot melt adhesives, etc.)

Method used

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  • Method for preparing beta-pinene polymer using alpha-diimine nickel complex as catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Example 1: β-pinene polymerization catalyzed by α-diimine nickel complex 1 / MAO system

[0019] Firstly, the a-diimine nickel complex 1 and MAO were made into concentrations of 3.46×10 -3 mol / L and 80.4g / L toluene solution, wherein a-diimine nickel complex 1 needs to add a small amount of dichloroethane (20%) to help dissolve. Then, 1.0 mL of the above-mentioned α-diimine nickel complex 1 solution, 1.0 mL of MAO solution, 8.0 mL of toluene, and 5.0 mL of β-pinene were sequentially added into the 50 mL ground-mouth reaction vial with a syringe. Seal the reaction bottle and react at 40°C for 1.5 h, then pour the reaction solution into 400 mL of 5% methanolic hydrochloric acid solution to obtain a white precipitate. The monomer conversion rate is 90.5%, and the activity of the catalyst system is 1.14×10 6 [g(polymer) / mol(N i )]. The number average molecular weight of the β-pinene polymer measured by GPC was 4200, and the PDI=1.73.

Embodiment 2

[0020] Example 2: β-pinene polymerization catalyzed by a-diimine nickel complex 2 / MAO system

[0021] The same polymerization method as in Example 1, but with a-diimine nickel complex 2 instead of a-diimine nickel complex 1. Reaction at 40°C for 1.5h, conversion rate 90.7%, catalyst system activity is 1.14×10 6 [g(polymer) / mol(N i )]. The number average molecular weight of the β-pinene polymer measured by GPC was 4400, and the PDI=1.92.

Embodiment 3

[0022] Example 3: β-pinene polymerization catalyzed by a-diimine nickel complex 3 / MAO system

[0023] The same polymerization method as in Example 1 was used, but the feeding was changed to 0.5 mL of α-diimine nickel complex 3 solution, 0.5 mL of MAO solution, 9.0 mL of toluene, and 5.0 mL of β-pinene. Reacted at 40°C for 1.5h, the conversion rate was 94.1%, and the activity of the catalyst system was 1.59×10 6 [g(polymer) / mol(N i )]. The number-average molecular weight of the β-pinene polymer measured by GPC was 7450, and the PDI=2.02.

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Abstract

The invention relates to terpene resin, which in detail relates to a method for preparing high molecular weight beta- firpene polymer. The invention employs catalyst comprising alpha- biimines nickel compounds (main catalyst) and methyl aluminoxanes (adjuvant catalyst) to catalyze beta- firpene monomer for polymerization. The method can prepare beta- firpene polymer with higher molecular weight at temperature 40 Deg. C and lower catalyst concentration (6.92 * 10-4 -3.47 *10-5 mol / l), and number average molecular weight is larger than 4000, with maximum being 7450.

Description

technical field [0001] The invention relates to terpene resins, in particular to a method for preparing high molecular weight β-pinene polymers. Background technique [0002] Natural terpene monomer β-pinene ( ) is the main component of turpentine, and its polymerization product, terpene resin, has good viscosity-increasing properties, anti-aging and thermal stability, and is widely used in industries such as pressure-sensitive adhesives, hot-melt adhesives, and elastomer fillers. At the same time, due to its non-toxic, odorless and chemical corrosion resistance, it can also be used in food and medical industries. [0003] β-pinene in Lewis acid such as AlCl 3 etc. The industrial production of terpene resin has been realized through cationic polymerization. But, there are following disadvantages in the cationic polymerization of β-pinene under Lewis acid catalysis: (1) in order to obtain the polymkeric substance with practical use molecular weight, polymerization must be...

Claims

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Application Information

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IPC IPC(8): C08F132/08C08F4/70
Inventor 卢江陈永汉余鹏梁晖
Owner SUN YAT SEN UNIV
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