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Iron-based catalyst for pentadiene polymerization and method for preparing polypentadiene

A piperylene and catalyst technology, which is applied in the field of preparation of iron-based catalysts and polypiperylene, which can solve the problems of low catalyst activity, uncontrollable polypiperylene configuration, and increased synthesis costs, etc.

Inactive Publication Date: 2011-09-21
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The catalysts provided in the prior art all have disadvantages, such as uncontrollable configuration of the prepared polypiperylene, low catalyst activity at high temperature, etc., seriously affecting the polymerization of polypiperylene, causing waste of raw materials, increasing synthetic cost

Method used

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  • Iron-based catalyst for pentadiene polymerization and method for preparing polypentadiene
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  • Iron-based catalyst for pentadiene polymerization and method for preparing polypentadiene

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preparation example Construction

[0037] The present invention also provides a preparation method of polypiperylene, a) dissolving piperylene monomer in an organic solvent to obtain piperylene solution; b) dissolving iron isooctanoate, alkylaluminum compound, The electron donor is mixed with the piperylene solution at a molar ratio of 1:5 to 20:1 to 5 to obtain a reaction solution; the electron donor is a phosphite compound; c) the reaction solution is mixed at 0 to Heating at 70°C, the piperylene monomer undergoes a polymerization reaction, and after the reaction is terminated, the product is condensed, and polypiperylene is obtained after drying.

[0038] The polypiperylene provided by the present invention, that is, polypiperylene, uses the iron-based catalyst provided by the present invention, preferably in anhydrous and oxygen-free, under nitrogen protection, mixes the organic solvent with the piperylene monomer, and configures The concentration of the monomer is preferably 0.08-0.2 g / mL of the piperylene...

Embodiment 1

[0042] Add 7mL of hexane, 3mL of piperylene monomer, and hexane solution of iron isooctanoate to the catalyst reaction flask protected by anhydrous and oxygen-free nitrogen. The molar ratio of piperylene to Fe is 1500, diethyl phosphite Hexane solution of ester, [P] / [Fe]=2 and hexane solution of triisobutylaluminum, [Al] / [Fe]=10, at 50°C, after 4 hours of polymerization reaction, containing 1% 2,6-di-tert-butyl-p-cresol in ethanol to terminate. Polyisoprene was coagulated with excess ethanol. The yield of polymer was 96.4 wt%.

[0043] Polymer 400M prepared by embodiment 1 1 H spectrum characterizes the microstructure, such as figure 1 As shown, the 1,4-structure content in the polymer molecule is 35.9%, the 1,2-structure content is 61.0%, and the 3,4-structure content is 3.1%. The model for molecular weight and molecular weight distribution is Waters 515 Gel Permeation Chromatography instrument, THF was used as the mobile phase, and polystyrene was used as the standard sa...

Embodiment 2

[0045] As described in Example 1, other conditions are exactly the same, only the molar ratio of triisobutylaluminum to Fe is changed to 5, the yield of the polymer is 3.2wt%, the polymer 1,4-structure content is 32.6%, 1 , 2-structure content is 61.4%, 3,4-structure content is 6.0%, number average molecular weight (Mn) is 2.15×10 5 , The molecular weight distribution index is 3.2.

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Abstract

The invention provides an iron-based catalyst for pentadiene polymerization, which comprises iron iso-octoate, an alkyl aluminum compound and an electron donor in the mole ratio of 1: (5-20): (1-5), wherein the electron donor is an orthophosphorous acid ester compound. The iron-based catalyst provided by the invention still has high activity at over 50DEG C; in addition, the content of the configuration of a repetitive unit of the polypentadiene can be controlled by controlling the content of the alkyl aluminum compound. The invention also provides a method for preparing the polypentadiene.

Description

technical field [0001] The invention relates to the field of polymer synthesis, in particular to an iron-based catalyst for the polymerization of piperylene and a preparation method for polypiperylene. Background technique [0002] Piperylene, also known as 1,3-pentadiene, is one of the main components of petroleum carbon five fractions, with a content of about 11.0%. It is a chemical raw material second only to cyclopentadiene and isoprene. However, after the polymerization of piperylene, there are 11 kinds of geometric isomers containing double bonds and stereoisomerism of asymmetric carbon atoms, of which only a part of the polymer is rubber, so the polymerization of piperylene and the polymerization can be obtained The configuration of polymers has become a research hotspot in recent years. [0003] US Patent No. 4,048,418 discloses a method for the polymerization of piperylene catalyzed by an iron-based catalyst to obtain polypiperylene with a cis-1,4 structure content...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F36/04C08F136/04C08F4/70
Inventor 张学全贾翔宇蔡洪光代全权毕吉福张春雨那丽华姜连升齐晓梅石路颖张志强林曙光
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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