Gallate base cyclic carbonate, non-isocyanate polyurethane and preparation method thereof

An acid-based non-isocyanate and non-isocyanate technology is applied in the field of preparation of biomass-based cyclic carbonates and non-isocyanate polyurethanes, which can solve problems such as human health and environmental hazards, and achieve safe preparation process, high product conversion rate, and high reaction efficiency. mild effects

Inactive Publication Date: 2015-11-18
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional polyurethane production uses highly toxic and volatile polyisocyanate

Method used

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  • Gallate base cyclic carbonate, non-isocyanate polyurethane and preparation method thereof
  • Gallate base cyclic carbonate, non-isocyanate polyurethane and preparation method thereof
  • Gallate base cyclic carbonate, non-isocyanate polyurethane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In a 1L autoclave, add 200g of gallic acid-based epoxy resin, 2g of lithium bromide, 1g of ethylene glycol and 100mL of N-methylpyrrolidone (NMP), raise the temperature to 110°C, and introduce CO 2 To a certain pressure, vent after leak detection. Repeat the operation three times, completely remove the air in the kettle, and introduce CO 2 Keeping the pressure at 2MPa, the reaction was stirred for 9h. After the reaction was completed, the remaining CO in the kettle was evacuated. 2 , The product was poured out while it was hot, the catalyst and NMP were removed by washing with hot water, and the water was distilled off under reduced pressure to obtain a brown solid, namely gallic acid-based cyclocarbonate. The epoxy value of the product was analyzed, and the conversion rate of the epoxy group was 98.9%.

[0034] Product gallic acid base cyclocarbonate in embodiment 1 1 HNMR (500MHz, DMSO-d 6 ,δ):7.01-7.34(m,hydrogensofaromatic); 5.03-5.19(m,methinehydrogensofcyclic...

Embodiment 2

[0038] In a 1L autoclave, add 200g of gallic acid-based epoxy resin, 2g of lithium bromide, 2g of ethylene glycol and 100mL of N,N-dimethylformamide, raise the temperature to 80°C, and introduce CO 2 To a certain pressure, vent after leak detection. Repeat the operation three times, completely remove the air in the kettle, and introduce CO 2 Keep the pressure at 5MPa, and stir the reaction for 15h. After the reaction was completed, the remaining CO in the kettle was evacuated. 2, The product was poured out while it was hot, the catalyst and solvent were removed by washing with hot water, and the water was distilled off under reduced pressure to obtain a brown solid, namely gallic acid-based cyclocarbonate.

Embodiment 3

[0040] In a 1L autoclave, add 200g of gallic acid-based epoxy resin, 2g of lithium bromide, 4g of ethylene glycol and 100mL of N-methylpyrrolidone (NMP), raise the temperature to 130°C, and introduce CO 2 To a certain pressure, vent after leak detection. Repeat the operation three times, completely remove the air in the kettle, and introduce CO 2 Keep the pressure at 0.5MPa, and stir the reaction for 24h. After the reaction was completed, the remaining CO in the kettle was evacuated. 2 , The product was poured out while it was hot, the catalyst and NMP were removed by washing with hot water, and the water was distilled off under reduced pressure to obtain a brown solid, namely gallic acid-based cyclocarbonate.

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Abstract

The present invention discloses gallate base cyclic carbonate, non-isocyanate polyurethane and a preparation method thereof. The method employs reaction of gallate base epoxy resin and CO2 in the presence of a catalyst to prepare the gallate base cyclic carbonate, which then reacts with an amine compound to prepare the non-isocyanate polyurethane. The preparation method of the gallate base cyclic carbonate has the advantages of simpleness, mild reaction conditions, and safe and nontoxic preparation process. The prepared polyurethane material does not use highly toxic isocyanate as raw material; the manufacturing process is safe and environment-friendly; and the gallate base cyclic carbonate and non-isocyanate polyurethane have the advantages of biodegradability and environment compatibility.

Description

technical field [0001] The present invention relates to a kind of preparation method of biomass-based cyclocarbonate and its non-isocyanate polyurethane, especially a kind of gallic acid-based epoxy resin and CO 2 A method for preparing gallic acid-based cyclocarbonate and its non-isocyanate polyurethane by reaction. Background technique [0002] Polyurethane materials are widely used in foams, elastomers, coatings and adhesives due to their excellent durability, impact resistance, adhesion, tear resistance, abrasion resistance and stress relaxation properties. The traditional polyurethane production uses highly toxic and volatile polyisocyanate as the main raw material, causing great harm to human health and the environment. As a new type of environmentally friendly polyurethane material, non-isocyanate polyurethane does not use polyisocyanate during preparation and use, so it has the advantages of less toxic and side effects, safe and environmentally friendly preparation ...

Claims

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Application Information

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IPC IPC(8): C07D317/36C08G71/04
CPCC07D317/36C08G71/04
Inventor 刘贵锋孔振武吴国民陈健霍淑平金灿
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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