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Preparation method of 3,4-polybeta-myrcene

A kind of technology of myrcene and isoprene, applied in the field of preparation of 3,4-poly-β-myrcene

Active Publication Date: 2015-05-27
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, 3,4-poly-β-myrcene with high 3,4-structure content has not been reported so far.

Method used

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  • Preparation method of 3,4-polybeta-myrcene

Examples

Experimental program
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Effect test

preparation example Construction

[0068] Preparation of catalyst combination:

[0069] Preparation of Catalyst Combination 1: At 25°C, add 10 μmol of the rare earth complex shown in formula 1, 10 μmol of [Ph 3 C][B(C 6 f 5 ) 4 ], 100 μmol triisobutylaluminum and chlorobenzene solvent, the concentration of the rare earth complex in the catalyst combination is 2.0mmol L –1 , and reacted for 2 minutes to obtain catalyst combination 1.

[0070] Preparation of catalyst combination 2: at 25°C, add 10 μmol of the rare earth complex shown in formula 2, 10 μmol of [Ph 3 C][B(C 6 f 5 ) 4 ], 100 μmol triisobutylaluminum and chlorobenzene solvent, the concentration of the rare earth complex in the catalyst combination is 0.67mmol L –1 , and reacted for 2 minutes to obtain catalyst combination 2.

[0071] Preparation of Catalyst Combination 3: At 0°C, add 10 μmol of the rare earth complex shown in formula 2, 10 μmol of [Ph 3 C][B(C 6 f 5 ) 4 ], 100 μmol triisobutylaluminum and toluene solvent, the concentratio...

Embodiment 1

[0091] Take 5ml of the toluene solution of catalyst combination 1, place it in an anhydrous and anaerobic-treated polymerization bottle, add 5.0mmol β-myrcene, carry out the polymerization reaction at 25°C for 0.5 hours, add 2ml of ethanol with a volume concentration of 10% hydrochloric acid The solution terminates the polymerization reaction, and the reaction solution is poured into 100ml of methanol to settle to obtain 3,4-poly-β-myrcene; the obtained polymer is then dried in a vacuum oven for 48 hours to obtain a dry constant weight, with a net weight of 0.68 g. Overall conversion 100%. With NMR spectrum ( 1 H NMR) and carbon nuclear magnetic spectrum ( 13 CNMR) analysis obtains poly-β-myrcene 3, and the content of 4 structural units is 98%; Use GPC analysis to obtain the number-average molecular weight (M) of 3,4-poly-β-myrcene n ) is 134,000, the molecular weight distribution (M w / M n ) is 1.71, and the 3,4-poly-β-myrcene glass transition temperature (T g ) is -42°...

Embodiment 8

[0094] The solvent used in embodiment 8 is chlorobenzene, figure 1 It is the carbon nuclear magnetic spectrum of the 3,4-poly-β-myrcene prepared in Example 8, and the obtained 3,4-poly-β-myrcene has an isotactic structure mmmm>99%.

[0095] Table 1: 3,4-poly-β-myrcene synthesized in Examples 1-40

[0096]

[0097]

[0098] From the polymerization data of Examples 1 to 40 of the polymerization of 3,4-poly-β-myrcene, it can be concluded that the rare earth catalyst provided by the present invention catalyzes the 3,4 selective polymerization of β-myrcene by means of coordination polymerization , β-myrcene monomer can obtain 100% conversion. The number average molecular weight of 3,4-poly-β-myrcene is 0.1×10 4 ~150×10 4 Within the range, the molecular weight distribution is 1.1-3.0. The rare earth catalyst has high adaptability to temperature, and in the polymerization temperature range of -30-80°C, the 3,4-structure content of poly-β-myrcene can be no less than 90%.

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Abstract

The invention relates to a preparation method of 3,4-polybeta-myrcene and belongs to the field of polymer preparation. The preparation method comprises the following steps: (a), under the protection of inert gas nitrogen gas or argon gas, dissolving a rare earth catalyst in an organic solvent to obtain a rare earth catalyst solution; (b), with beta-myrcene as a monomer raw material, performing a catalytic polymerization reaction on the rare earth catalyst solution to obtain 3,4-polybeta-myrcene. According to the preparation method of 3,4-polybeta-myrcene, the content of a 3,4 structural unit of 3,4-polybeta-myrcene, which is prepared by performing the catalytic polymerization reaction through the rare earth catalyst solution, is not less than 90%; the preparation method has great innovativeness.

Description

technical field [0001] The invention relates to the field of polymer preparation, in particular to a preparation method of 3,4-poly-β-myrcene. Background technique [0002] Rubber is a highly elastic polymer material with reversible deformation. It has excellent resilience, insulation, water resistance and plasticity. It also has oil resistance, acid resistance, alkali resistance, heat resistance, cold resistance and Excellent properties such as pressure and wear resistance. Therefore, rubber has a wide range of uses in industrial production, medical and health care, agricultural production and daily life. However, due to the limited production of natural rubber, and in order to meet the different needs of various industries and fields, various synthetic rubbers with different properties have been widely concerned by the industry. [0003] Myrcene, a dimer of isoprene, exists in the volatile oils of Umbelliferae cress, Cupressaceae juniper and Rosaceae plants, including tw...

Claims

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Application Information

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IPC IPC(8): C08F136/22C08F4/52C08F236/22C08F236/08
Inventor 崔冬梅刘博李世辉
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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