Method for preparing 4-vinylpyridine using single component rare earth organic compound as catalyst

A technology for vinyl pyridine and organic compounds, which is applied in the field of preparation of polymers by coordination polymerization, can solve the problems of low reaction conversion rate, affect actual use, easy to burn, etc., and achieve the effects of clear structure, cost reduction and efficiency improvement.

Inactive Publication Date: 2004-03-03
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above-mentioned coordination polymerization reports all need to use a binary catalyst, and the aluminum alkyl is expensive, and has a lively performance and is prone to combustion, which affects the actual use; at the same time, the reaction conversion rate is low, generally not more than 40%.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: After the polymerization bottle with stirring bar is deoxidized and dewatered, a certain amount of 4-vinylpyridine and the required amount of toluene are added under the protection of argon, and the polymerization bottle is placed in an oil bath at 25°C In, add [(i-PrN) with a syringe 2 CN(SiMe 3 ) 2 ] 2 Nd(μ-Me) 2 Li(TMEDA). After the polymerization reaction was carried out for 15 minutes, the reaction was terminated with methanol, and the polymer was precipitated with methanol, dried in vacuum, and the conversion rate was calculated. The results are listed in Table 1.

[0029] Table 1 [(i-PrN) 2 CN(SiMe 3 ) 2 ] 2 Nd(μ-Me) 2 Dosage of Li(TMEDA)

[0030] Effects on 4-VP aggregation

[0031] No. [Monomer] / [Catalyst] Yield (%) M η (10 -4 )

[0032] 1 700 99 1.53

[0033] 2 1000 100 1.01

[0034] 3 1500 100 3.01

[0035] 4 2500 100 3.58

[0036] 5 4000 80 5.33

[0037] [Monomer] = 20%

Embodiment 2

[0038] Example 2: This example illustrates the influence of the central metal on the guanidino rare earth methyl compound when catalyzing the polymerization of 4-VP. Other conditions and operations are the same as in Embodiment 1.

[0039] Table 2 The influence of the central metal on the guanidinium rare earth methyl compound in catalyzing 4-VP polymerization

[0040] No. Catalyst [Monomer] / [Catalyst] Yield (%) M η (10 -4 )

[0041] 1 1 1000 100 1.01

[0042] 2 1 1500 100 3.01

[0043] 3 1 2000 97 4.42

[0044] 4 1 4000 80 5.33

[0045] 5 2 1000 100 7.23

[0046] 6 2 1500 82 7.29

[0047] 7 2 2000 54 10.49

[0048] 8 MeLi 700 0 -

[0049] Catalyst: [(i-PrN) 2 CN(SiMe 3 ) 2 ] 2 Ln(μ-Me) 2 Li(TMEDA)(Ln=Nd(1), Yb(2))

Embodiment 3

[0050] Example 3: This example illustrates the effect of the catalyst structure on the catalytic activity of trivalent rare earth organic compounds to catalyze 4-VP polymerization. Unless otherwise specified, other conditions and operations are the same as in Example 1.

[0051] Table 3 The results of 4-VP polymerization catalyzed by different trivalent rare earth organic compounds

[0052] No. Catalyst [Monomer] / [Catalyst Temperature Yield

[0053] chemical agent] (°C) (%)

[0054] 1 [(i-PrN) 2 CN(SiMe 3 ) 2 ] 2 Yb(μ- 1000 25 100

[0055] Me) 2 Li(TMEDA)

[0056] 2 [(iPrN) 2 CN(SiMe 3 ) 2 ] 2 YN(iPr) 2 500 40 79.2

[0057] [N(C 6 h 3 iP 2 -

[0058] 3 2, 6) (SiMe 3 )] 2 YbMe(μ-Me)Li(THF) 3 700 15 46.2

[0059] 4 [(Bu t Cp) 2 Nd(μ-Me)] 2 200 15 100

[0060] 5* [(MeCp) 2 Yb(THF) 2 ][BPh 4 ] 200 90 90.2

[0061] 6* [(Bu t Cp) 2 Yb(THF)...

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Abstract

A process using organic RE compound as catalyst for preparing poly(4-vinylpyridine) features that the 4-vinylpyridine monomer, said catalyst and solvent take part in polymerizing reaction in inertial gas. Its advantages are high catalytic activity of catalyst, high output rate, and high molecular weight of resultant polymer.

Description

technical field [0001] The invention relates to a method for preparing poly(4-vinylpyridine), in particular to a method for preparing poly(4-vinylpyridine) by using a rare earth organic complex as a catalyst for coordination polymerization. Background technique [0002] Poly(4-vinylpyridine) is a water-soluble polymer after being salified by quaternary ammonium, which can be used as polyelectrolyte; the nitrogen atom on the pyridine ring has strong coordination ability, and can coordinate with a series of metals to form metal Polymers, thus poly(4-vinylpyridine) can also be used as a catalyst carrier for organic and polymer reactions. Therefore, poly(4-vinylpyridine) is a functional polymer material with a wide range of applications. [0003] In the prior art, the methods for synthesizing poly(4-vinylpyridine) mainly include free radical initiated polymerization, anion initiated polymerization and coordination polymerization. [0004] Wherein, anio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/00C08F126/06
Inventor 姚英明沈琪罗云杰张振琴邓明宇薛明强
Owner SUZHOU UNIV
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