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POSS modified rosin nonisocyanate polyurethane and preparation method of nonisocyanate polyurethane

A non-isocyanate, rosin-based technology, applied in the field of preparation of POSS modified rosin-based non-isocyanate polyurethane, can solve the problems of poor water resistance, low glass transition temperature, etc., and achieves low raw material cost, simple method and mild reaction conditions. Effect

Inactive Publication Date: 2016-04-20
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

[0004] Aiming at the shortcomings of rosin-based NIPU materials such as poor water resistance and low glass transition temperature, the invention provides a POSS modified rosin-based non-isocyanate polyurethane and a preparation method thereof

Method used

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  • POSS modified rosin nonisocyanate polyurethane and preparation method of nonisocyanate polyurethane
  • POSS modified rosin nonisocyanate polyurethane and preparation method of nonisocyanate polyurethane
  • POSS modified rosin nonisocyanate polyurethane and preparation method of nonisocyanate polyurethane

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Experimental program
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Embodiment 1

[0030] In a 1L autoclave, add 100g of epoxy-based POSS, 1g of lithium bromide, 0.5g of ethylene glycol and 30mL of N-methylpyrrolidone (NMP), raise the temperature to 100°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 2MPa, and stir the reaction for 10h. Evacuate the remaining CO in the kettle 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 light yellow viscous liquid, namely cyclocarbonate-based POSS. The epoxy value of the product was analyzed, and the epoxy group conversion rate was 98.9%.

[0031] Product cyclocarbonate group POSS in embodiment 1 1 HNMR (500MHz, CDCl 3 ,δ): 4.79-4.95(m, 1H, cyclocarbonate group methylene); 4.52(t, 1H, cyclocarbonate group methylene); 4.41(t, 1H, cyclocarbonate group met...

Embodiment 2

[0035]Dissolve 3.0g of rosin-based cyclocarbonate in DMF to prepare a solution with a solid content of 35%, then add 0.48g of hexamethylenediamine curing agent, stir evenly, coat a film on a tinplate sheet or tetrafluoroethylene board, and cure at 100°C for 8 hours , Measuring the properties of the coating film (GB / T1732-93, GB / T1731-93, GB / T1720-89, GB / T6739-2006). Coating film NIPU performance: T g 34.81°C, T d (50%) 384.97 ℃, impact strength ≥ 50cm, adhesion level 1, flexibility 0.5mm, pencil hardness 2H, 24h water absorption 37.45%.

Embodiment 3

[0037] Dissolve 3.0g of rosin-based cyclocarbonate and 1.0g of cyclocarbonate-based POSS in DMF to prepare a solution with a solid content of 35%, then add 0.74g of hexamethylenediamine curing agent, stir evenly, and place on a tinplate sheet or tetrafluoroethylene plate Put on the coating film, cure at 100°C for 8 hours, and measure the properties of the coating film (GB / T1732-93, GB / T1731-93, GB / T1720-89, GB / T6739-2006). Coating film NIPU / POSS (1) performance: T g 65.26°C, T d (50%) 397.15 ℃, impact strength ≥ 50cm, adhesion level 1, flexibility 0.5mm, pencil hardness 2H, 24h water absorption 16.59%.

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Abstract

The invention discloses POSS modified rosin nonisocyanate polyurethane and a preparation method of the nonisocyanate polyurethane. According to the method, epoxy group POSS and CO2 react under the action of a catalyst to synthesize cyclic carbonate-based POSS, then the cyclic carbonate-based POSS is copolymerized with rosin-based cyclic carbonate and an amino compound, and the POSS modified nonisocyanate polyurethane is prepared. The method for preparing the cyclic carbonate-based POSS is simple and convenient, and reaction conditions are mild; the prepared polyurethane material has a good thermodynamic property, no isocyanate with hypertoxicity is adopted in the preparation process, and the preparation process is safe and environmentally friendly.

Description

technical field [0001] The invention discloses a preparation method of POSS-modified rosin-based non-isocyanate polyurethane, in particular to a preparation method of rosin-based non-isocyanate polyurethane modified by cyclocarbonate-based POSS. Background technique [0002] As a new type of environmentally friendly polyurethane material, non-isocyanate polyurethane (NIPU) not only has good processing performance, chemical corrosion resistance and low permeability, but also discards highly toxic and moisture-sensitive polyisocyanates during preparation and use. Therefore, it has the advantages of less toxic and side effects, safe and environmentally friendly preparation and use processes, and is a new generation of polyurethane materials with broader application prospects. However, NIPU materials have shortcomings such as poor water resistance and low glass transition temperature, which seriously restrict the promotion and application of its related products. [0003] Polyh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G71/04
CPCC08G71/04
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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