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Cobalt complex conjugated microporous polymer catalyst, and preparation and application thereof

A technology of conjugated microporous and metallic cobalt, applied in the field of cyclic carbonate, can solve problems such as harsh conditions, and achieve the effects of increasing solubility, improving reaction yield and shortening reaction time.

Active Publication Date: 2015-02-11
ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the main use of CO 2 The CO 2 into commercially useful organic chemicals, but the catalysts used in these reactions catalyze the conversion of CO 2 The conditions are relatively harsh, and its catalytic activity is limited by high temperature and high pressure. Therefore, it is necessary to find a catalyst that can achieve CO2 under relatively mild conditions. 2 Catalytic conversion is an urgent problem to be solved

Method used

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  • Cobalt complex conjugated microporous polymer catalyst, and preparation and application thereof
  • Cobalt complex conjugated microporous polymer catalyst, and preparation and application thereof
  • Cobalt complex conjugated microporous polymer catalyst, and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1), the synthesis method of Salen-Co: dissolve 0.75mmol Salen in 10ml dry anhydrous toluene, add the methanol solution of cobalt acetate (1mmolCo(OAc) 2 dissolved in 10ml of methanol), and refluxed at 80°C for 5h to obtain the desired Salen-Co compound;

[0037] 2), the synthetic method of Salen-Co-OAc: dissolve 0.65mmol Salen-Co in 6ml toluene and 18mlCH 2 Cl 2 In the mixed solvent, inject 6.5mmol of CH3 COOH, under the protection of argon, stirred at 25°C for 5h to obtain the desired Salen-Co-OAc compound; figure 2 shown;

[0038] 3), the synthetic method of CMP-1: 0.45mmol Salen-Co-OAc, 1.35mmol 1,3,5-triethynylbenzene, 40mg CuI, 80mg tetrakis(triphenylphosphopalladium), use 15ml toluene and 5ml three Ethylamine was used as a solvent, refluxed at 85°C for 72h, and post-treated to obtain the desired CMP[Salen-Co-OAc] compound; the NMR of the compound was as follows Figure 5 shown;

[0039] 4), catalytic CO 2 Reaction with alkylene oxides:

[0040] ①, 100mg CM...

Embodiment 2

[0044] 1), the synthesis method of Salen-Co: dissolve 0.6mmol Salen in 10ml dry anhydrous toluene, add the methanol solution of cobalt acetate (1mmolCo(OAc) 2 dissolved in 10ml of methanol), and refluxed at 80°C for 5h to obtain the desired Salen-Co compound;

[0045] 2), the synthetic method of Salen-Co-OAc: 0.5mmol Salen-Co is dissolved in 5ml toluene and 15mlCH 2 Cl 2 In the mixed solvent, add 5.0mmol of CH by syringe 3 COOH, under the protection of argon, stirred at 25°C for 5h to obtain the desired Salen-Co-OAc compound; figure 2 shown;

[0046] 3), the synthetic method of CMP-1: 0.6mmol Salen-Co-OAc, 2.4mmol 1,3,5-triethynylbenzene, 60mg CuI, 100mg tetrakis(triphenylphosphopalladium), use 16ml toluene and 6ml tris Ethylamine was used as a solvent, refluxed at 85°C for 72h, and post-treated to obtain the desired CMP[Salen-Co-OAc] compound; the NMR of the compound was as follows Figure 5 shown;

[0047] 4), catalytic CO 2 Reaction with alkylene oxides:

[0048] ①...

Embodiment 3

[0052] 1), the synthesis method of Salen-Co: dissolve 0.5mmol Salen in 8ml dry anhydrous toluene, add the methanol solution of cobalt acetate (1mmolCo(OAc) 2 Dissolved in 8ml of methanol), refluxed at 80°C for 5h to obtain the desired Salen-Co compound;

[0053] 2), the synthetic method of Salen-Co-OAc: dissolve 0.65mmol Salen-Co in 5ml toluene and 15mlCH 2 Cl 2 In the mixed solvent, add 9.0mmol of CH by syringe 3 COOH, under the protection of argon, stirred at 25°C for 6h to obtain the desired Salen-Co-OAc compound; figure 2 shown;

[0054] 3), the synthetic method of CMP-1: 0.6mmol Salen-Co-OAc, 2.0mmol 1,3,5-triethynylbenzene, 50mg CuI, 100mg tetrakis(triphenylphosphopalladium), use 16ml toluene and 5ml tris Ethylamine was used as a solvent, refluxed at 85°C for 72h, and post-treated to obtain the desired CMP[Salen-Co-OAc] compound; the NMR of the compound was as follows Figure 5 shown;

[0055] 4), catalytic CO 2 Reaction with alkylene oxides:

[0056] ①, 100mg C...

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Abstract

The invention researches and develops a novel catalyst capable of catalyzing the reaction of CO2 with epoxyalkane to produce cyclic carbonate at a temperature of 0 to 160 DEG C and a pressure of 0.1 to 6 MPa and a preparation and application thereof. The catalyst is a cobalt complex conjugated microporous polymer CMP[Salen-Co-R1] and has structural formulas of CMP-1, CMP-2 and CMP-3 as described in the specification; in the formulas, R1 is -OAc, -Cl, -Br or -I, and R2 is -H, -tBu, -iBu, -NO2, -Cl, -CH2NEt2 or -CH2N(Bn)Et2Br. The polymer catalyst is used to catalyze the reaction of CO2 and epoxyalkane at normal temperatures and pressures, yield of obtained cyclic carbonate is 35 to 90%, and repeated usage of the catalyst almost poses no influence to the yield; the yield is more than 90% when the reaction is carried out at a high temperature of 50 to 120 DEG C and a high pressure of 2 to 6 MPa for 1 to 3 h. According to the invention, catalysis of the reaction of CO2 with epoxyalkane is realized under mild reaction conditions, so restriction of high temperatures and pressures on the reaction is overcome; and the catalyst can be repeatedly used, so the problem of a low utilization rate of the catalyst in the prior art is overcome.

Description

technical field [0001] The present invention has synthesized metal cobalt complexed conjugated microporous polymer CMP[Salen-Co-R 1 ], and used it as a catalyst to catalyze CO under mild conditions 2 The cyclic carbonate is synthesized by reacting with alkylene oxide, and the repeated use of the polymer catalyst has almost no influence on the yield of the cyclic carbonate. Background technique [0002] CO 2 It is one of the most abundant carbon sources on the earth, and has many advantages such as large reserves, safety, non-toxicity, and cheapness. However, CO 2 It is also one of the main greenhouse gases. In recent years, due to the CO in the atmosphere 2 The concentration of CO2 is constantly rising, the greenhouse effect is constantly increasing, leading to global warming, and at the same time, disastrous weather is becoming more frequent. Therefore, how to process and utilize CO more conveniently 2 has become more important. It is of great significance to the devel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C08G61/12C07D317/36
Inventor 邓伟侨谢勇刘晓焕
Owner ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI
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