A kind of high-efficiency preparation method and application of ultra-high molecular weight poly-β-farnesene

A technology of ultra-high molecular weight and farnesene, which is applied in the direction of chemical recovery, etc., can solve the problems of low molecular weight of poly-β-farnesene and high cost of rare earth metal reactants, and achieve high polymerization activity, low price, and high-efficiency preparation method Effect

Active Publication Date: 2022-06-03
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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Problems solved by technology

[0004] The present invention provides a high-efficiency preparation method and application of ultra-high molecular weight poly-β-farnesene in order to solve the technical problems of low molecular weight of poly-β-farnesene obtained by the existing method and high cost of using rare earth metal reactants

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  • A kind of high-efficiency preparation method and application of ultra-high molecular weight poly-β-farnesene
  • A kind of high-efficiency preparation method and application of ultra-high molecular weight poly-β-farnesene
  • A kind of high-efficiency preparation method and application of ultra-high molecular weight poly-β-farnesene

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specific Embodiment approach 1

[0036] Embodiment 1: A kind of efficient preparation method of poly-β-farnesene of the present embodiment is carried out according to the following steps:

[0037] Take a Schlenk bottle, add 30 mL of toluene, cocatalyst MAO (2.5 mmol, 500 equiv, 1.67 mL), β-farnesene monomer (25 mmol, 5000 equiv, 6.3 mL), Pyridine iron complex 1 (5μmol, 1equiv, 2.1mg), under stirring conditions, after polymerization at 25 ° C for 30min, add 20mL of a mixed solution of hydrochloric acid and methanol and 5mL of anti-aging agent to quench the reaction, pour off the clear After the solution, the polymer was washed three times with ethanol, and the obtained polymer was vacuum-dried at 40°C to constant weight to obtain poly-β-farnesene; the volume ratio of methanol to concentrated hydrochloric acid in the mixed solution of hydrochloric acid and methanol was 50 :1.

[0038] The yield of this embodiment is >99%. The microstructural selectivity of the polymer was: 45% 1,4-polyβ-farnesene and 55% 3,4-...

specific Embodiment approach 2

[0046] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the amount of co-catalyst MAO is (1.25 mmol, 250 equiv, 0.83 mL). Other steps and parameters are the same as in the first embodiment.

[0047] The yield of this embodiment was 97%. The microstructural selectivity of the polymer was: 45% 1,4-polyβ-farnesene and 55% 3,4-polyβ-farnesene, M n (number average molecular weight, g / mol) was 1.47 million, and PDI (molecular weight distribution) was 2.6.

specific Embodiment approach 3

[0048] Embodiment 3: The difference between this embodiment and Embodiment 1 is that the co-catalyst is MMAO, and the dosage is (2.5 mmol, 500 equiv, 1.25 mL). Other steps and parameters are the same as in the first embodiment.

[0049] The yield of this embodiment is >99%. The microstructural selectivity of the polymer was: 46% 1,4-polyβ-farnesene and 54% 3,4-polyβ-farnesene, M n (number average molecular weight, g / mol) was 1.3 million, and PDI (molecular weight distribution) was 1.9.

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Abstract

A high-efficiency preparation method and application of ultra-high molecular weight poly-β-farnesene. The invention belongs to the field of polymer synthesis. The invention aims to solve the technical problems that the molecular weight of the polyβ-farnesene obtained by the existing method is low and the cost of the rare earth metal reactant used is relatively high. The method of the present invention: under the protection condition of inert gas, the solvent, the main catalyst, the co-catalyst, and β-farnesene monomer are added into the reactor in any order, and under the condition of stirring, at 0°C to 100°C Polymerize for 10 minutes to 240 minutes, then add a quencher and anti-aging agent to the reaction system to quench the reaction, wash repeatedly with ethanol, and vacuum dry to obtain polyβ-farnesene; the main catalyst is a bipyridyl iron complex. The microstructure of the poly-β-farnesene obtained in the present invention consists of 3,4-poly-β-farnesene with a molar fraction of 50% to 70% and 1,4-poly-β-farnesene with a molar fraction of 30% to 50%. Composition of farnesene, the number average molecular weight scope of gained polyβ-farnesene is 8.0 * 10 5 g / mol~1.7×10 6 g / mol, molecular weight distribution 1.5~3.5.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and in particular relates to an efficient preparation method and application of ultra-high molecular weight poly-β-farnesene. Background technique [0002] At present, the monomers for the synthesis of polyconjugated diene rubber materials are mainly derived from petrochemical resources. However, due to the unsustainable regeneration of petroleum resources and the energy crisis, it is necessary to find bio-based monomers to replace petroleum-based monomers and prepare bio-based monomers. It is of great significance to study green rubber materials, promote the sustainable development of the tire rubber industry, and alleviate the current serious energy crisis and environmental problems. [0003] As a bio-based green rubber, poly-β-farnesene has excellent elasticity and low temperature resistance, and has received extensive attention in the development of new bio-based green rubber materials. At p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/22C08F4/70C08L47/00
CPCC08F136/22C08L47/00C08F4/7006Y02P20/584
Inventor 王庆刚王亮朱瑞周丽匡佳
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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