Tung oil polyol and synthesis method thereof

Abstract

The invention discloses tung oil polyol and a synthesis method thereof. The synthesis method comprises the following steps: mixing tung oil, carboxylic acid, a metal ion supported cation exchange resin catalyst, a hydroxylation reagent, and deionized water according to a certain ratio, heating the mixture to a temperature of 35 to 45 DEG C; dropwise adding a hydrogen peroxide solution under violent stirring, controlling the addition speed to maintain the temperature in a range of 40 to 65 DEG C, after addition, maintaining the reaction temperature for 3 to 5 hours, stopping the reactions; filtering the reaction system to separate out the solid catalyst, allowing the reaction system to stand still to carry out layering, separating water phase from the reaction system, neutralizing the oil phase, washing the oil phase by water, and subjecting the oil phase to reduced pressure distillation to obtain tung oil polyol. The yield of the prepared tung oil polyol is more than 92%, the hydroxyl value of the product is 120 to 270 mgKOH / g, the acid value is less than 1.0 mgKOH / g, the water content is less than 0.1 wt%, and the tung oil polyol can be used to prepare a polyurethane material.

Description

technical field

[0001] The invention belongs to the field of polyurethane materials, and in particular relates to a tung oil polyol and a synthesis method. Background technique

[0002] Polyurethane materials have been widely used in industry and people's daily life due to their good mechanical properties and easy molding. The main raw materials used to produce polyurethane include isocyanates, polyols and other additives, of which polyols account for more than 50%. In the process of industrial production, polyols are mainly used in the field of polyurethane, so the factors affecting the polyurethane industry are also the main factors affecting the polyol market. Polyols can be divided into polyether polyols and polyester polyols according to their molecular structure. Among them, polyether polyols dominate the market, accounting for more than 70% of the entire polyol demand.

[0003] Typically, polyols are prepared from petroleum. As a non-renewable resource, the scarcit...

Examples

Embodiment 1

[0022] Add 500g tung oil, 115g formic acid (85wt% solution), 50gAl 3+ Supported cation exchange resin catalyst (wherein Al 3+ The loading amount accounts for 2% of the mass of the catalyst, the same below), 300g of butanol, 50g of deionized water, heated up to 40°C and stirred evenly. Then slowly add 450g of 30wt% hydrogen peroxide aqueous solution dropwise under vigorous stirring conditions, and control the dropping rate to keep the reaction temperature at about 50°C. After the reaction system was separated into layers, the water phase was removed, and the oil phase was washed with 10 wt% sodium bicarbonate aqueous solution until neutral, and then the product was washed with hot water at 70°C for 3 times. The washed product was distilled at 2000Pa and 80°C for 2 hours to obtain the tung oil polyol product with a yield of 93.8%, a hydroxyl value of 250mgKOH / g, a viscosity of 8200mPa·s, an acid value of 0.80mgKOH / g, and low water content. At 0.1wt%, it can be used to prepare ...

Embodiment 2

[0024] Add 500g tung oil, 115g formic acid (85wt% solution), 50gAl 3+ Loaded cation exchange resin catalyst, 300g butanol, 50g deionized water, heated up to 45°C and stirred evenly. Then slowly add 450g of 30wt% hydrogen peroxide solution dropwise under vigorous stirring conditions, and control the dropping rate to keep the reaction temperature at about 65°C. After the reaction system was separated into layers, the water phase was removed, and the oil phase was washed with 10 wt% sodium bicarbonate aqueous solution until neutral, and then the product was washed with hot water at 70°C for 3 times. The washed product was distilled at 2000Pa and 80°C for 2 hours to obtain the tung oil polyol product with a yield of 93.5%, a hydroxyl value of 232mgKOH / g, a viscosity of 10400mPa·s, an acid value of 0.92mgKOH / g, and low water content. At 0.1wt%, it can be used to prepare polyurethane rigid foam products.

Embodiment 3

[0026] Add 500g tung oil, 115g formic acid (85wt% solution), 50gAl 3+ Loaded cation exchange resin catalyst, 300g butanol, 50g deionized water, heated up to 35°C and stirred evenly. Then slowly add 450g of 30wt% hydrogen peroxide solution dropwise under vigorous stirring conditions, and control the dropping rate to keep the reaction temperature at about 40°C. After the reaction system was separated into layers, the water phase was removed, and the oil phase was washed with 10 wt% sodium bicarbonate aqueous solution until neutral, and then the product was washed with hot water at 70°C for 3 times. The washed product was distilled at 2000Pa and 80°C for 2 hours to obtain the tung oil polyol product with a yield of 92.6%, a hydroxyl value of 172mgKOH / g, a viscosity of 3290mPa·s, an acid value of 0.68mgKOH / g, and low water content. At 0.1wt%, it can be used to prepare polyurethane products.

technical field

[0001] The invention belongs to the field of polyurethane materials, and in particular relates to a tung oil polyol and a synthesis method. Background technique

[0002] Polyurethane materials have been widely used in industry and people's daily life due to their good mechanical properties and easy molding. The main raw materials used to produce polyurethane include isocyanates, polyols and other additives, of which polyols account for more than 50%. In the process of industrial production, polyols are mainly used in the field of polyurethane, so the factors affecting the polyurethane industry are also the main factors affecting the polyol market. Polyols can be divided into polyether polyols and polyester polyols according to their molecular structure. Among them, polyether polyols dominate the market, accounting for more than 70% of the entire polyol demand.

[0003] Typically, polyols are prepared from petroleum. As a non-renewable resource, the scarcit...

Examples

Embodiment 1

[0022] Add 500g tung oil, 115g formic acid (85wt% solution), 50gAl 3+ Supported cation exchange resin catalyst (wherein Al 3+ The loading amount accounts for 2% of the mass of the catalyst, the same below), 300g of butanol, 50g of deionized water, heated up to 40°C and stirred evenly. Then slowly add 450g of 30wt% hydrogen peroxide aqueous solution dropwise under vigorous stirring conditions, and control the dropping rate to keep the reaction temperature at about 50°C. After the reaction system was separated into layers, the water phase was removed, and the oil phase was washed with 10 wt% sodium bicarbonate aqueous solution until neutral, and then the product was washed with hot water at 70°C for 3 times. The washed product was distilled at 2000Pa and 80°C for 2 hours to obtain the tung oil polyol product with a yield of 93.8%, a hydroxyl value of 250mgKOH / g, a viscosity of 8200mPa·s, an acid value of 0.80mgKOH / g, and low water content. At 0.1wt%, it can be used to prepare ...

Embodiment 2

[0024] Add 500g tung oil, 115g formic acid (85wt% solution), 50gAl 3+ Loaded cation exchange resin catalyst, 300g butanol, 50g deionized water, heated up to 45°C and stirred evenly. Then slowly add 450g of 30wt% hydrogen peroxide solution dropwise under vigorous stirring conditions, and control the dropping rate to keep the reaction temperature at about 65°C. After the reaction system was separated into layers, the water phase was removed, and the oil phase was washed with 10 wt% sodium bicarbonate aqueous solution until neutral, and then the product was washed with hot water at 70°C for 3 times. The washed product was distilled at 2000Pa and 80°C for 2 hours to obtain the tung oil polyol product with a yield of 93.5%, a hydroxyl value of 232mgKOH / g, a viscosity of 10400mPa·s, an acid value of 0.92mgKOH / g, and low water content. At 0.1wt%, it can be used to prepare polyurethane rigid foam products.

Embodiment 3

[0026] Add 500g tung oil, 115g formic acid (85wt% solution), 50gAl 3+ Loaded cation exchange resin catalyst, 300g butanol, 50g deionized water, heated up to 35°C and stirred evenly. Then slowly add 450g of 30wt% hydrogen peroxide solution dropwise under vigorous stirring conditions, and control the dropping rate to keep the reaction temperature at about 40°C. After the reaction system was separated into layers, the water phase was removed, and the oil phase was washed with 10 wt% sodium bicarbonate aqueous solution until neutral, and then the product was washed with hot water at 70°C for 3 times. The washed product was distilled at 2000Pa and 80°C for 2 hours to obtain the tung oil polyol product with a yield of 92.6%, a hydroxyl value of 172mgKOH / g, a viscosity of 3290mPa·s, an acid value of 0.68mgKOH / g, and low water content. At 0.1wt%, it can be used to prepare polyurethane products.