A kind of preparation method of alicyclic polycarbonate

A technology for cyclic carbonate and aliphatic aldehyde, which is applied in the field of catalytic synthesis of chemical industry, can solve the problems of difficulty in obtaining and high price, and achieves the effects of cheap and easy-to-obtain process raw materials, simple operation, and efficient and simple process.

Active Publication Date: 2022-05-27
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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  • A kind of preparation method of alicyclic polycarbonate
  • A kind of preparation method of alicyclic polycarbonate
  • A kind of preparation method of alicyclic polycarbonate

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preparation example Construction

[0055] The preparation method of the catalyst according to the preparation method of aliphatic cyclic polycarbonate of the present invention can be carried out as follows: hydrogen-type molecular sieves such as H-β, 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 to constant weight at 200°C, then drop to room temperature, add silica sol with a concentration of 20%-40% to the above carrier powder, and then add Ni, Pd, Rh, Ru, Sn, Cu, Co in an inert atmosphere , metal salts of Mn, Fe, Cr, or halide salts of transition metals such as porphyrin, bis(butanedione oxime, bisacetylacetone, Salen, etc. and Ni, Pd, Rh, Ru, Sn, Cu, Co, Mn, Fe, etc.) The formed complex precursor is hydrothermally or alcoholic heat-treated at 40-95°C for 2-48h, and the solid obtained by suction filtratio...

Embodiment 1

[0064] The H-ZSM-5 (Si / Al=38) was dewatered and degassed under vacuum at 200°C for 6h, then put into a flask, and the required amount of toluene solution of 3-aminopropyltriethoxysilane was added under nitrogen protection. added, and stirred at room temperature for 24 h, evaporated the solvent, and vacuum-dried at 150 °C to obtain a carrier precursor modified with surface ammonia. The amino group in the prepared precursor accounted for the SiO in ZSM-5. 2 The quality fraction of 20%. The synthesis of Co-Salen was carried out according to the reported route (L.E.Martínez, J.L.Leighton, D.H.Carsten, E.N.Jacobsen, J.Am.Chem.Soc.117(1997) 5897.), the Salen ligand was via tert-butylsalicylic Aldehyde and ethylenediamine structure amines through the condensed Schiff base. Add 20 g of carrier precursor to the flask, under N 2 Dichloromethane was added under the protection, fully stirred to form a suspension, 50 g of Co-Salen solution in dichloromethane was added, stirred at room te...

Embodiment 2

[0066] The SBA-15 was dewatered and degassed under vacuum at 200°C for 6h, then put into a flask, and the required amount of toluene solution of 3-aminopropyltriethoxysilane was added under nitrogen protection, and stirred at room temperature for 24h, Evaporate the solvent to dryness and vacuum dry at 150°C to obtain a carrier precursor modified with surface ammonia. The amino group in the prepared precursor is the same as the SiO in SBA-15. 2 The mass ratio is 1:5. The synthesis of Co-Salen was carried out according to the reported route (L.E.Martínez, J.L.Leighton, D.H.Carsten, E.N.Jacobsen, J.Am.Chem.Soc.117(1997) 5897.), the Salen ligand was via tert-butyl water The amines of sylaldehyde and ethylenediamine structure pass through the condensed Schiff base. Add 20 g of carrier precursor to the flask, under N 2 Dichloromethane was added under the protection, fully stirred to form a suspension, 50 g of Co-Salen solution in dichloromethane was added, stirred at room temperat...

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Abstract

The invention discloses a method for preparing cyclic carbonates. The method uses olefins, aldehydes, and carbon dioxide to co-convert into more valuable cyclic carbonate chemicals, wherein carbon dioxide is in a supercritical state, which is used as a reactant and simultaneously As a solvent, the method also uses a new composite heterogeneous nano-catalyst material that simultaneously activates carbon dioxide and olefins, and it is used to activate carbon dioxide and olefins together to achieve high-yield conversion under mild conditions to prepare cyclic carbonates. . The process raw material of the invention is cheap and easy to obtain, the catalyst is non-corrosive, the process is simple to operate, no other reaction steps are required, the process is efficient, simple and easy to operate, economical and pollution-free, and is beneficial to large-scale industrial production of cyclic carbonates.

Description

[0001] Relevant earlier application [0002] This application claims the priority of the Chinese invention patent application filed on October 23, 2020 with the title of a preparation method of aliphatic cyclic polycarbonate, the application number is 202011143857.0, and the entire content of the prior application is cited by reference The manner 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 catalytic co-transformation of coupled olefins. Background technique [0004] Carbon dioxide is a greenhouse gas and an inexhaustible "renewable" carbon resource. Considering factors such as comprehensive utilization of resources and environmental governance, the utilization of carbon dioxide as a resource has high application value and environmental protection significance. . The ...

Claims

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Application Information

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Patent Type & Authority Patents(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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