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Synthesis method of five-membered cyclic carbonate

A technology of cyclic carbonate and synthesis method, which is applied in the field of synthesizing five-membered cyclic carbonate with urea and diol, can solve the problems of high requirements on equipment material and operating conditions, explosion of epoxy compounds, complicated process conditions, etc. Indirect utilization, easy recycling, good stability

Inactive Publication Date: 2012-05-23
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Ethyl (propyl) carbonate was first synthesized by phosgene. Although the product yield and purity of this route are high, the process conditions are complicated, and phosgene is eliminated due to potential safety hazards.
Ethyl (propyl) carbonate can also be synthesized by corresponding epoxy compounds and carbon dioxide. This method has the risk of explosion of epoxy compounds, and has higher requirements on equipment materials and operating conditions. In industry, quaternary ammonium salts are mainly used as catalysts, and the preparation cost is relatively high. higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Titrate zinc nitrate and yttrium nitrate with 1mol / L sodium carbonate precipitant until the precipitation is complete, age the precipitate at 70°C for 12 hours, wash the obtained precipitate with distilled water several times until neutral, dry at 120°C, and roast at 300-600°C to obtain a powdery solid , marked as Zn a Y, where the value of a ranges from 0.1 to 5.

[0028] 500g urea, 1033g ethylene glycol, 15g above catalyst Zn a Y was added to a 2L stainless steel reaction kettle with a reflux device. After the reactor was sealed, it was reacted at 120°C for 4 hours under reduced pressure (2-3KPa). The reaction mixture was cooled to room temperature, the catalyst was recovered by filtration, the mixture was added to the internal standard of biphenyl, and the selectivity of the main by-product 2-hydroxyurethane was 2%, and urea was decomposed to produce CO 2 Selectivity<3%, the analysis results are as follows:

[0029] Ethylene glycol / urea

Embodiment 2

[0031] 500g of urea, 1033g of ethylene glycol, 15g of the catalyst ZnaY of Example 1, which was reused 10 times, were added to a 2L stainless steel reactor with a reflux device, and after the reactor was sealed, under reduced pressure (2 to 3KPa), the reaction was carried out at 120°C 4h. The reaction mixture was cooled to room temperature, the catalyst was recovered by filtration, the mixture was added to the internal standard of biphenyl, and the selectivity of the main by-product 2-hydroxyurethane was 2%, and urea was decomposed to produce CO 2 Selectivity<3%, the analysis results are as follows:

[0032] Ethylene glycol / urea

Embodiment 3

[0034] 2500g urea, 5165g ethylene glycol, 75g embodiment 1 catalyst Zn a Y, put into a 10L stainless steel reaction kettle with a reflux device, seal the reactor, and react under reduced pressure (2-3KPa) at 120°C for 4h. The reaction mixture was cooled to room temperature, the catalyst was recovered by filtration, the mixture was added to the internal standard of biphenyl, and the selectivity of the main by-product 2-hydroxyurethane was 2%, and urea was decomposed to produce CO 2 Selectivity 2%, analysis result is as follows:

[0035] Ethylene glycol / urea

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Abstract

The invention discloses a synthesis method of five-membered cyclic carbonate. Urea and diol are used as raw materials and are reacted to prepare the cyclic carbonate in the presence of a catalyst under reduced pressure conditions. The synthesis method has the advantages of low cost of raw materials, milder reaction conditions and good stability, and the catalyst is easy to separate.

Description

technical field [0001] The invention relates to a method for synthesizing five-membered cyclic carbonate from urea and diol. Background technique [0002] Five-membered cyclic carbonates, including ethylene carbonate, propylene carbonate, etc., are not only high-boiling and high-polarity solvents with excellent performance, but also important organic chemical products. The main uses are as follows: [0003] Ethylene carbonate is a strong polar solvent, which has a large solubility for carbon dioxide, hydrogen sulfide and organic sulfur, but has a small solubility for nitrogen, CO, methane, oxygen, etc. It is widely used in the fields of natural gas, hydrogen production and synthesis gas Used as a decarburizer. Using ethylene carbonate as raw material, it can be further transesterified with alcohol to prepare dialkyl carbonate. Ethylene carbonate is also a good solvent for polyamide, polyacrylonitrile, bisphenol resin and other polymers. The mixed solution of ethylene carb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D317/38C07D317/36
Inventor 邓友全王利国李健田雄王瀛刘士民马祥元何昱德卢六斤
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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