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Efficient preparation method of high-molecular-weight polymyrcene with high 1,4-structure content

A high-molecular-weight, myrcene technology is applied in the field of efficient preparation of high-molecular-weight polymyrcene, can solve the problems of low catalytic activity, large amount of catalyst and high polymerization cost, and achieves the effects of high catalytic activity, high molecular weight and low price

Active Publication Date: 2021-01-05
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the technical problems of the existing 1,4-polymyrcene with low catalytic activity, large amount of catalyst and high polymerization cost, the present invention provides an efficient and cheap method for preparing polymyrcene with high 1,4-structure content. Molecular weight polymyrcene method

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  • Efficient preparation method of high-molecular-weight polymyrcene with high 1,4-structure content
  • Efficient preparation method of high-molecular-weight polymyrcene with high 1,4-structure content
  • Efficient preparation method of high-molecular-weight polymyrcene with high 1,4-structure content

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specific Embodiment approach 1

[0034] Specific embodiment 1: A high-efficiency preparation method of high-molecular-weight polymyrcene with high 1,4-structure content in this embodiment is carried out according to the following steps:

[0035] Take a Schlenk bottle, add 45mL of toluene, cocatalyst MAO (5mmol, 500equiv, 3.33mL), myrcene monomer (50mmol, 5000equiv, 8.6mL), and pyridinimine iron complex in sequence under the condition of anhydrous and oxygen-free argon. Material 1 (10μmol, 1equiv, 4.0mg), under the condition of stirring, polymerized at 25°C for 30min, then added 20mL of a mixed solution of hydrochloric acid and methanol and 5mL of anti-aging agent to quench the reaction, and poured off the clear liquid. The polymer was washed with ethanol three times, and the obtained polymer was vacuum-dried at 40° C. to constant weight to obtain polymyrcene; the volume ratio of methanol to concentrated hydrochloric acid in the mixed solution of hydrochloric acid and methanol was 50:1.

[0036] The yield of t...

specific Embodiment approach 2

[0037] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the amount of co-catalyst MAO is (2.5 mmol, 250 equiv, 1.67 mL). Other steps and parameters are the same as those in the first embodiment.

[0038] The yield of this embodiment is 98%, and the microstructural selectivity of the polymer is: 62% 1,4-polymyrcene and 38% 3,4-polymyrcene, M n (Number average molecular weight, g / mol) was 1.57 million, and PDI (molecular weight distribution) was 1.8.

specific Embodiment approach 3

[0039] Embodiment 3: This embodiment is different from Embodiment 1 in that the amount of toluene is 90 mL, and the amount of myrcene monomer is (100 mmol, 10000 equiv, 17.2 mL). Other steps and parameters are the same as those in the first embodiment.

[0040] The yield of this embodiment is >99%, and the microstructural selectivity of the polymer is: 65% 1,4-polymyrcene and 35% 3,4-polymyrcene, M n (Number average molecular weight, g / mol) was 1.38 million, and PDI (molecular weight distribution) was 2.1.

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Abstract

The invention relates to an efficient preparation method of high molecular weight polymyrcene with high 1,4-structure content, and belongs to the field of iron catalyzed myrcene polymerization. In order to solve the problems of low activity, large catalyst dosage, high polymerization cost and the like of the existing high 1,4-polymyrcene catalytic technology, the invention provides an efficient and cheap method for preparing high-molecular-weight polymyrcene with high 1,4-structure content. The method comprises the following steps: adding a solvent, a main catalyst, a cocatalyst and myrcene monomers into a reactor in any sequence under the protection of inert gas, carrying out polymerization reaction while stirring, adding a quenching agent and an anti-aging agent, carrying out quenching reaction, repeatedly washing with ethanol, and carrying out vacuum drying to obtain polymyrcene; the number-average molecular weight of the obtained polymyrcene ranges from 2.0*10<5> g / mol to 1.7*10<6>g / mol, the molecular weight distribution ranges from 1.5 to 5.5, the molar content of the 1,4-polymyrcene ranges from 50% to 70%, and the molar content of the 3,4-polymyrcene ranges from 30% to 50%.The method is high in catalytic activity and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of iron-catalyzed myrcene polymerization, in particular to a high-efficiency preparation method of high-molecular-weight polymyrcene with high 1,4-structure content. 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. Myrcene (β-Myrcene) is a linear monoterpene-conjugated diene compound. Its structure is similar to myrcene. It is widely present in plants and can be obtained from various plants, especially conifers. For example: myrcen...

Claims

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Application Information

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