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Efficient preparation method and application of poly beta-farnesene with ultra-high molecular weight

A technology of ultra-high molecular weight and farnesene, which is applied in chemical recycling and other fields, and can solve the problems of low molecular weight of poly-β-farnesene and high cost of rare earth metal reactants

Active Publication Date: 2021-03-19
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Efficient preparation method and application of poly beta-farnesene with ultra-high molecular weight
  • Efficient preparation method and application of poly beta-farnesene with ultra-high molecular weight
  • Efficient preparation method and application of poly beta-farnesene with ultra-high molecular weight

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specific Embodiment approach 1

[0036] Specific embodiment one: the efficient preparation method of a kind of poly-beta-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) and Pyridine iron complex 1 (5μmol, 1equiv, 2.1mg), after polymerization at 25°C for 30min under stirring, 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 3 times with ethanol, and the obtained polymer was vacuum-dried to constant weight at 40°C 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-poly-β-farnesene and 55% ...

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 those in the first embodiment.

[0047] The yield of this embodiment was 97%. The microstructural selectivity of the polymer was: 45% 1,4-poly-β-farnesene and 55% 3,4-poly-β-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 cocatalyst is MMAO, and the dosage is (2.5 mmol, 500 equiv, 1.25 mL). Other steps and parameters are the same as those in the first embodiment.

[0049] The yield of this embodiment is >99%. The microstructural selectivity of the polymers was: 46% 1,4-poly-β-farnesene and 54% 3,4-poly-β-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

The invention discloses an efficient preparation method and application of poly beta farnesene with ultra-high molecular weight. The invention belongs to the field of polymer synthesis. The inventionaims to solve the technical problems of low molecular weight of poly beta farnesene obtained by existing methods and higher cost of adopted rare earth metal reactants. The method comprises the following steps: adding a solvent, a main catalyst, a cocatalyst and a beta-farnesene monomer into a reactor according to any sequence under the protection of inert gas, performing polymerizing for 10-240 minutes at 0-100 DEG C while stirring, adding a quenching agent and an anti-aging agent into the reaction system for quenching reaction, repeatedly performing washing with ethanol, and carrying out vacuum drying to obtain the poly beta-farnesene . The main catalyst is a bipyridine iron complex. The microstructure of the obtained poly beta-farnesene is composed of 3,4-poly beta-farnesene with the molar fraction of 50%-70% and 1,4-poly beta-farnesene with the molar fraction of 30%-50%, the number-average molecular weight of the obtained poly beta-farnesene ranges from 8.0 x 10<5> g / mol to 1.7 x 10<6> g / mol, and the molecular weight distribution ranges from 1.5 to 3.5.

Description

technical field [0001] The invention belongs to the field of polymer synthesis, and in particular relates to a high-efficiency 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 mainly come from petrochemical resources, but due to the unsustainable regeneration of petroleum resources and the energy crisis, it is necessary to look for bio-based monomers to replace petroleum-based monomers, and to prepare bio-based Green rubber materials are of great significance to promote the sustainable development of the tire rubber industry and alleviate the current serious energy crisis and environmental problems. [0003] As a kind of 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 present, peo...

Claims

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Application Information

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Patent Type & Authority Applications(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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