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Catalyst and its preparation method and application, cyclic carbon dioxide-based polycarbonate and its preparation method

A technology based on polycarbonate and carbon dioxide, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of unstable polyanhydride structures and pending development

Active Publication Date: 2021-02-09
JILIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In epoxy monomer and CO 2 In the reaction, there are two problems of product selectivity and regioselectivity: product selectivity refers to the reaction between epoxy monomer and CO 2 Two reactions occur: one is cycloaddition, which generates small molecule cyclic carbonate products, and the other is epoxy monomer and CO 2 Copolymerization to obtain polycarbonate products; regioselectivity means that in the copolymerization reaction, there are three different processes: one is epoxy monomer and CO 2 complete alternating copolymerization, is CO 2 The goal of polycarbonate synthesis, the second is the continuous ring opening of epoxy monomers during the polymerization process to form polyether doped in polycarbonate, and the third is CO 2 Continuous insertion forms polyanhydrides, but because the reaction cannot occur thermodynamically and the structure of polyanhydrides is unstable, the epoxy monomer and CO 2 CO in the copolymerization reaction 2 The process of continuous insertion has not been reported
Cyclic CO 2 The synthesis of polycarbonate-based polycarbonate is still a blank, for the synthesis of cyclic CO 2 New catalytic systems based on polycarbonate have yet to be developed

Method used

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  • Catalyst and its preparation method and application, cyclic carbon dioxide-based polycarbonate and its preparation method
  • Catalyst and its preparation method and application, cyclic carbon dioxide-based polycarbonate and its preparation method
  • Catalyst and its preparation method and application, cyclic carbon dioxide-based polycarbonate and its preparation method

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preparation example Construction

[0056] The present invention provides the preparation method of the catalyst for synthesizing cyclic carbon dioxide-based polycarbonate described in the above technical scheme, comprising the following steps:

[0057] Mixing 4,4-diaminodiphenylmethane, acetylacetone, p-toluenesulfonic acid and toluene, and performing the first hydroxylamine condensation reaction to obtain the first ligand;

[0058] mixing the ethanol solution of the first ligand, the hydrochloric acid solution of 1,4-dioxane, and 4,4-diaminodiphenylmethane to perform a second hydroxylamine condensation reaction to obtain the second ligand;

[0059] Mixing the solution of the second ligand and the solution of the zinc compound to perform a substitution reaction to obtain a catalyst for synthesizing cyclic carbon dioxide-based polycarbonate;

[0060] The zinc compound in the zinc compound solution includes zinc compounds of alkyl zinc or alkyl derivatives.

[0061] In the present invention, unless otherwise spe...

Embodiment 1

[0085] 4,4-Diaminodiphenylmethane (11.6g, 58.4mmol, 1.0eq), acetylacetone (12mL, 117mmol, 2.0eq) and p-toluenesulfonic acid (1.0g, 5.8mmol, 0.01eq) were dissolved in 1L of toluene Reflux at 130°C for 2h, carry out the first hydroxylamine condensation reaction, use saturated NaHCO 3 The resulting mixture was washed with an aqueous solution, and the solvent was removed by rotary evaporation, and 19 g of a khaki solid was obtained after washing with hexane, which was the first ligand with a yield of 90%; the H NMR spectrum of the first ligand (500 MHz 1 H NMR benzene-d 6 )See figure 1 ; NMR data: δ13.07(s, 2H, -OH), δ6.77-6.79(d, J=10.0Hz, 4H, C-H), δ6.67-6.69(d, J=10.0Hz, 4H, C-H), δ5.00(s, 2H, C-H), δ3.55(s, 2H, CH 2 ),δ2.05(s,6H,CH 3 ), δ1.55(s,6H,CH 3 ), according to the nuclear magnetic spectrum information, the structure of the compound is the above-mentioned target first ligand structure;

[0086] The first ligand (3g, 8.3mmol, 1.0eq) was dissolved in 120mL ethanol, ...

Embodiment 2

[0089] 4,4-Diaminodiphenylmethane (24.0g, 117.0mmol, 2.0eq), acetylacetone (12mL, 117mmol, 2.0eq) and p-toluenesulfonic acid (100.0g, 580.0mmol, 1.0eq) were dissolved in 1L of toluene Reflux at 100°C for 2 hours to carry out the first hydroxylamine condensation reaction, using saturated NaHCO 3The resulting mixture was washed with an aqueous solution, and the solvent was removed by rotary evaporation, and 20.1 g of a khaki solid was obtained after washing with hexane, which was the first ligand with a yield of 95%; the H NMR spectrum of the first ligand (500 MHz 1 H NMR benzene-d 6 )see picture 1;

[0090] The first ligand (3g, 8.3mmol, 1.0eq) was dissolved in 250mL ethanol, and the HCl solution of dioxane (the concentration of hydrochloric acid was 4.0M, 8.4mL, 33.6mmol, 4.0eq) was added dropwise, and then 4,4-Diaminodiphenylmethane (1.65g, 8.3mmol, 1.0eq), reflux overnight at 90°C for the second hydroxylamine condensation reaction, disperse the resulting solid in water, ad...

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Abstract

The invention provides a catalyst, its preparation method and application, cyclic carbon dioxide-based polycarbonate and its preparation method, and belongs to the technical field of carbon dioxide-based polycarbonate. Catalyst provided by the invention can realize epoxy monomer (meso-CHO) and CO 2 Alternating copolymerization of (regioselective polycarbonate>99%) and exhibited high activity (TOF>3200h ‑1 ), the catalyst of the present invention can be used to prepare cyclic CO for the first time 2 based polycarbonate, and for the first time synthesized antithermodynamically conventional containing continuous CO 2 unit of CO 2 based polycarbonate (PCHC).

Description

technical field [0001] The invention relates to the technical field of carbon dioxide-based polycarbonate, in particular to a catalyst and its preparation method and application, cyclic carbon dioxide-based polycarbonate and its preparation method. Background technique [0002] Development CO 2 Polycarbonate-based polycarbonate is a practical and efficient means of mitigating the greenhouse effect and mitigating the fossil energy crisis. Since Inoue et al used ZnEt in 1969 2 / H 2 O system realizes epoxy and CO for the first time 2 Since the aggregation of CO 2 Synthesis of polycarbonate based on polycarbonate has received extensive attention. Epoxy monomers include but not limited to propylene oxide (PO), cyclohexene oxide (CHO), cyclopentene oxide (CPO) and limonene oxide (LO). Among them, PO and CHO epoxy monomers are the most widely studied due to the advantages of wide sources and cheap prices, and are particularly eye-catching. In epoxy monomer and CO 2 In the rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/34C07F3/06B01J31/22
CPCB01J31/1815B01J2531/0241B01J2531/26C07F3/06C08G64/34
Inventor 张越涛廖曦何江华
Owner JILIN UNIV
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