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Preparation method of aliphatic cyclic polycarbonate

A technology of cyclic carbonate and aliphatic aldehyde, which is applied in the field of catalytic synthesis of chemical industry, can solve the problems of high price and difficult acquisition, and achieve the effects of simple operation, cheap and easy-to-obtain process raw materials, and simplified product separation

Active Publication Date: 2021-08-20
源创核新(北京)新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, Dai Yongbo et al. found that 1-methyltrimethylene cyclocarbonate can be polymerized by ring-opening to produce polycarbonate materials with excellent performance (Dai Yongbo, "Rare Earth Compounds Initiate 1-Methyltrimethylene Cyclocarbonate Ring-opening Polymerization") and Mechanism Research", Master Thesis of Zhejiang University, 2011), however, its synthetic raw material 1-methyltrimethylene cyclocarbonate is relatively special, and it is relatively difficult and expensive to obtain

Method used

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  • Preparation method of aliphatic cyclic polycarbonate
  • Preparation method of aliphatic cyclic polycarbonate
  • Preparation method of aliphatic cyclic polycarbonate

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preparation example Construction

[0055] According to the preparation mode of the catalyst of the preparation method of alicyclic polycarbonate of the present invention can be carried out as follows: hydrogen type molecular sieve such as H-beta, SBA-15, H-Y, ZSM-5 (silicon-aluminum ratio 12-300), composite Oxide superacids such as SiO 2 -Al 2 o 3 , SiO 2 -TiO 2 , SiO 2 -ZrO 2 , SiO 2 -WO 3 , SiO 2 -MoO 3 , SiO 2 -SnO 2 、TiO 2 -ZrO 2 、TiO 2 -WO 3 、TiO 2 -Al 2 o 3 Vacuum dry at 200°C to constant weight, then drop to room temperature, add 20%-40% concentration of silica sol to the above carrier powder, and then add Ni, Pd, Rh, Ru, Sn, Cu, Co under an inert atmosphere , Mn, Fe, Cr metal salts, or porphyrin, bis-butyledionoxime, diacetylacetone, Salen, etc. and Ni, Pd, Rh, Ru, Sn, Cu, Co, Mn, Fe and other transition metal halide salts The formed complex precursor is treated with hydrothermal or alcohol heat at 40-95°C for 2-48h, and the solid obtained by suction filtration is in N 2 Dry the prep...

Embodiment 1

[0064] H-ZSM-5 (Si / Al=38) was vacuum dewatered and degassed at 200°C for 6h, then put into a flask, and under the protection of nitrogen, the required amount of 3-aminopropyltriethoxysilane in toluene solution Added and stirred at room temperature for 24h, evaporated to dryness, and vacuum dried at 150°C to obtain a surface ammonia-modified carrier precursor, the amino group in the prepared precursor accounted for the SiO in ZSM-5 2 The mass fraction is 20%. The synthesis of Co-Salen is carried out (L.E.Martínez, J.L.Leighton, D.H.Carsten, E.N.Jacobsen, J.Am.Chem.Soc.117 (1997) 5897.) Aldehydes and amines of ethylenediamine structure are condensed by Schiff bases. Add 20 g of carrier precursor into the flask, under N 2 Add dichloromethane under protection, stir well to form a suspension, add 50g of Co-Salen in dichloromethane solution, stir at room temperature for 24h, then filter, wash thoroughly with diethyl ether and dry in vacuum at 60°C to obtain the catalyst Co-Salen / Z...

Embodiment 2

[0066] Dehydrate and degas SBA-15 at 200°C for 6 hours in vacuum, then put it into a flask, add the required amount of 3-aminopropyltriethoxysilane toluene solution under nitrogen protection, and stir at room temperature for 24 hours, Evaporate the solvent to dryness, and dry in vacuum at 150°C to obtain the surface ammonia-modified carrier precursor. The amino group in the prepared precursor and the SiO in SBA-15 2 The mass ratio is 1:5. The synthesis of Co-Salen is carried out synthetically (L.E.Martínez, J.L.Leighton, D.H.Carsten, E.N.Jacobsen, J.Am.Chem.Soc.117 (1997) 5897.) The amines of the structure of valylaldehyde and ethylenediamine are condensed by the Schiff base. Add 20 g of carrier precursor into the flask, under N 2 Add dichloromethane under protection, stir well to form a suspension, add 50g of Co-Salen in dichloromethane solution, stir at room temperature for 24h, then filter, wash thoroughly with diethyl ether and dry in vacuum at 60°C to obtain the catalys...

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Abstract

The invention discloses a preparation method of cyclic carbonate. According to the method, olefin, aldehydes and carbon dioxide are co-converted into a more valuable cyclic carbonate chemical, and carbon dioxide is in a supercritical state and is used as a reactant and a solvent at the same time. According to the method, a novel composite heterogeneous nano catalyst material for simultaneously activating carbon dioxide and olefin is also adopted, and is used for jointly activating carbon dioxide and olefin, so that the aim of preparing cyclic carbonate through high-yield conversion under mild conditions is fulfilled. The process raw materials are cheap and easy to obtain, the catalyst is non-corrosive, the process is simple to operate, other reaction steps are not needed, the process is efficient, simple and feasible, economic and pollution-free, and large-scale industrial production of the cyclic carbonate is facilitated.

Description

[0001] related earlier application [0002] This application claims the priority of the Chinese invention patent application filed on October 23, 2020, the title of which is a preparation method of aliphatic cyclic polycarbonate, and the application number is 202011143857.0. The entire content of this earlier application is cited method is incorporated herein by reference. technical field [0003] The invention belongs to the field of catalytic synthesis chemical industry, and in particular relates to a method for preparing cyclic carbonate by high-value catalysis of carbon dioxide and co-transformation of coupled olefins. Background technique [0004] Carbon dioxide is a kind of greenhouse gas, and at the same time it is an inexhaustible "renewable" carbon resource. Considering factors such as comprehensive utilization of resources and environmental governance, the resource utilization of carbon dioxide has high application value and environmental protection significance ....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/36B01J31/22
CPCC07D317/36B01J31/2217B01J2531/845B01J2231/328B01J2531/847Y02P20/54
Inventor 牟新东张新志王文久尹斌石健刘涛
Owner 源创核新(北京)新材料科技有限公司
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