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A kind of high-efficiency and controllable method for preparing polyisoprene

A technology for polyisoprene and isoprene, which is applied in the field of efficient and controllable preparation of polyisoprene, can solve the problems of low activity of iron-based catalysts, uncontrollable selectivity, easy deactivation of catalysts, etc. Good industrial application prospect, easy operation, high activity effect

Active Publication Date: 2022-07-05
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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Problems solved by technology

[0005] The present invention provides an efficient and controllable method for preparing polyisoprene in order to solve the technical problems of low activity, uncontrollable selectivity and sensitive and easy deactivation of the existing iron-based catalysts

Method used

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  • A kind of high-efficiency and controllable method for preparing polyisoprene
  • A kind of high-efficiency and controllable method for preparing polyisoprene
  • A kind of high-efficiency and controllable method for preparing polyisoprene

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Experimental program
Comparison scheme
Effect test

specific Embodiment approach 1

[0029] Embodiment 1: The structural formula of the rigid framework iron complex 1a of this embodiment is:

[0030]

[0031] Its specific synthesis method is as follows: add FeCl to a 100mL single-necked flask 2 (146.4mg, 1.2mmol, 1.0equiv), then dissolved in 2mL of glacial acetic acid, and then added 6,7-dihydro-5H-quinolin-8-one (170.0mg, 1.2mmol, 1.0equiv) and aniline (107.6 mg, 1.2 mmol, 1.0 equiv) solution in glacial acetic acid (8 mL), refluxed at 130 ° C for 12 hours, cooled to room temperature, added ether (50 mL), and a purple solid was precipitated; filtered, and washed with 30 mL of ether three times to obtain a purple Solid, rigid framework iron complex 1a.

[0032] Result: Yield 53.9%.

[0033] Infrared analysis: FT-IR (KBr, disk, cm -1 ): 3060, 2948, 1623, 1585 (ν, C=N), 1486, 1450, 1335, 1202, 1130, 790, 698.

[0034] Elemental Analysis: Anal.Calcd for C 30 H 28 Cl 4 Fe 2 N 4 : C, 51.62%; H, 4.04%; N, 8.03%. Found: C, 51.24%; H, 3.65%; N, 7.83%.

[0...

specific Embodiment approach 2

[0036] Embodiment 2: The structural formula of the rigid framework iron complex 2a of this embodiment is:

[0037]

[0038] Its specific synthesis method is as follows: add FeCl to a 100mL single-necked flask 2 (86.1 mg, 0.7 mmol, 1.0 equiv), then dissolved in 2 mL of glacial acetic acid; then added 6,7-dihydro-5H-quinolin-8-one (100.0 mg, 0.7 mmol, 1.0 equiv) and p-toluidine respectively (72.8 mg, 0.7 mmol, 1.0 equiv) in glacial acetic acid (8 mL), refluxed at 130°C for 12 hours, cooled to room temperature, and a large amount of ether (50 mL) was added to precipitate a dark brown solid; filter, and wash with 30 mL of ether for 3 Next, a dark brown solid, the rigid framework iron complex 2a, was obtained.

[0039] Result: Yield 60.6%.

[0040] Infrared analysis: FT-IR (KBr, disk, cm -1 ): 2943, 1578 (ν, C=N), 1505, 1455, 1357, 1337, 1219, 1110, 837, 791, 770.

[0041] Elemental Analysis: Anal.Calcd for [C 32 H 32 Cl 4 Fe 2 N 4 ][CH 3 COOH][H 2 O]: C, 50.78%; H, 4...

specific Embodiment approach 3

[0043] Embodiment 3: The structural formula of the rigid framework iron complex 3a of this embodiment is:

[0044]

[0045] Its specific synthesis method is as follows: add FeCl to a 100mL single-necked flask 2(99.0 mg, 0.8 mmol, 1.0 equiv), then dissolved in 2 mL of glacial acetic acid; 6,7-dihydro-5H-quinolin-8-one (115.0 mg, 0.8 mmol, 1.0 equiv) and 1-naphthalene were added respectively A solution of amine (111.9 mg, 0.8 mmol, 1.0 equiv) in glacial acetic acid (8 mL) was refluxed at 130 °C for 12 hours, cooled to room temperature, a large amount of ether (50 mL) was added, and a gray-brown solid was precipitated; filtered, and washed with 30 mL of ether 3 times to obtain a gray-brown solid, the rigid framework iron complex 3a.

[0046] Result: Yield 51.6%.

[0047] Infrared analysis: FT-IR (KBr, disk, cm -1 ): 3054, 2942, 1626, 1583 (ν, C=N), 1452, 1390, 1333, 1285, 1216, 1130, 781.

[0048] Elemental Analysis: Anal.Calcd for [C 38 H 32 Cl 4 Fe 2 N 4 ][3H 2 O]:...

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Abstract

An efficient and controllable method for preparing polyisoprene. The invention belongs to the field of conjugated diene catalytic polymerization. The invention solves the technical problems of low activity of the existing iron-based catalyst, uncontrollable selectivity and sensitive and easy deactivation of the catalyst. The method of the present invention is as follows: under an inert gas atmosphere, the isoprene monomer, the rigid framework iron complex, the co-catalyst and the solvent are added to the reactor, and the reaction is stirred at ‑40 to 100 ° C for 12s to 120min, and the reaction is completed. After quenching by adding hydrochloric acid methanol solution, filtering, washing and vacuum drying in turn, polyisoprene is obtained; the reactivity can reach up to 10 8 g / mol(Fe) / h, the selectivity of cis-1,4 / trans-1,4 is (99:1)~(1:99). The method of the invention can be suitable for the preparation of rubber materials with different properties; the method and application are constructed for the development of high-performance and special-performance polymer materials. In addition, the catalytic system provided by the invention has strong heat resistance, and can maintain high activity even at a high temperature of 100° C., so that the industrial application prospect of this type of catalyst is better.

Description

technical field [0001] The invention belongs to the field of conjugated diene catalytic polymerization, in particular to a method for efficiently and controllably preparing polyisoprene. Background technique [0002] Polyisoprene, which is formed by the polymerization of isoprene monomer under the action of a catalyst, is an important synthetic rubber. According to different unit structures, polyisoprene can be divided into polyisoprene with cis-1,4 structure, polyisoprene with trans-1,4 structure, 1,2- and 3,4- Polyisoprene, the specific structure is as follows: [0003] [0004] Polymers with different selectivity have different applications. In isoprene polymerization, titanium-based catalysis and rare-earth catalysis systems have been studied most deeply. However, titanium-based catalysts have wide molecular weight distribution and complex active species; rare earth metals are expensive, and catalyst costs are high. This series of factors limit its further applicat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/08C08F4/70
CPCC08F136/08C08F4/7006Y02P20/584
Inventor 王庆刚王亮朱广乾张献辉荆楚杨
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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