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Efficient preparation method of high molecular weight polymyrcene with high 3, 4-structure content

A technology of high molecular weight and myrcene, which is applied in the field of high-efficiency preparation of high molecular weight polymyrcene, can solve the problems of low catalytic activity, high polymerization cost, and large amount of catalyst, and achieve high catalytic activity, high molecular weight, and easy operation.

Active Publication Date: 2021-01-26
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the technical problems of low catalytic activity, large amount of catalyst and high polymerization cost in the existing polymyrcene system with high 3,4 structure content, the present invention provides an efficient and cheap preparation method with high Method for high molecular weight polymyrcene with 3,4-structure content

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  • Efficient preparation method of high molecular weight polymyrcene with high 3, 4-structure content
  • Efficient preparation method of high molecular weight polymyrcene with high 3, 4-structure content
  • Efficient preparation method of high molecular weight polymyrcene with high 3, 4-structure content

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specific Embodiment approach 1

[0034] Specific embodiment one: the efficient preparation method of a kind of polymyrcene of the present 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 bipyridyl iron complex in sequence under anhydrous and oxygen-free argon gas conditions 1 (10μmol, 1equiv, 2.82mg), under the condition of stirring, polymerize 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 liquid, and polymerize The mixture 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 this embodiment is >99%, and the microstructural selec...

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 95%, and the microstructural selectivity of the polymer is: 44% of 1,4-polymyrcene and 56% of 3,4-polymyrcene, M n (Number average molecular weight, g / mol) was 800,000, and PDI (molecular weight distribution) was 2.9.

specific Embodiment approach 3

[0039] Embodiment 3: The difference between this embodiment and Embodiment 1 is that the co-catalyst is MAO and the dosage is (1.0 mmol, 100 equiv, 0.67 mL). Other steps and parameters are the same as those in the first embodiment.

[0040] The yield of this embodiment is 68%, and the microstructural selectivity of the polymer is: 45% 1,4-polymyrcene and 55% 3,4-polymyrcene, M n (Number average molecular weight, g / mol) was 300,000, and PDI (molecular weight distribution) was 2.4.

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Abstract

The invention relates to an efficient preparation method of high molecular weight polymyrcene with high 3, 4-structure content, which belongs to the field of iron catalyzed myrcene polymerization. Inorder to solve the technical problems of low catalytic activity, large catalyst dosage and high polymerization cost in the existing technology for preparing polymyrcene with high 3, 4-structure content, the invention provides an efficient and cheap method for preparing high molecular weight polymyrcene with high 3, 4-structure content. The method comprises the following steps of 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 1.4*10<6> g / mol, the molecular weight distribution ranges from 1.5 to 5.0, the molar content of the 3, 4- polymyrcene ranges from 50% to 70%, and the molar content of the 1, 4-polymyrcene ranges from 30% to 50%.

Description

technical field [0001] The invention belongs to the field of iron-catalyzed myrcene polymerization, and in particular relates to a high-efficiency preparation method of high-molecular-weight polymyrcene with high 3,4-structure content. Background technique [0002] At present, due to the unsustainable regeneration of petroleum resources and the energy crisis, it is of great significance to prepare bio-based green rubber materials using bio-based monomers with similar structures as raw materials to alleviate the current severe energy crisis and environmental problems. Myrcene (β-Myrcene) is a linear monoterpene-conjugated diene compound derived from plants and similar in structure to isoprene. The content of myrcene in cork oil in Jilin Province, which is rich in conifer resources in my country, can be as high as 80%, which can provide a sufficient source of bio-based myrcene. Polymyrcene, as a bio-based green rubber, has excellent elasticity and low temperature resistance, ...

Claims

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Application Information

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IPC IPC(8): C08F136/22C08F4/70
CPCC08F136/22C08F4/7006
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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