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Tung oil polyhydric alcohol with high hydroxyl value and preparation method thereof

A technology of tung oil polyol and high hydroxyl value, which is applied in the field of polyurethane materials, can solve problems such as increased viscosity and ineffective reaction, and achieve the effects of improving reactivity, avoiding cross-linking side reactions, and avoiding cross-linking

Active Publication Date: 2017-07-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the influence of the conjugated double bond of tung oil, cross-linking occurs during the amine methylation reaction with hydroxyl-containing amines, resulting in increased viscosity and ineffective reaction

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 500g of tung oil, 125g of formic acid (85wt% solution), 0.5g of concentrated sulfuric acid, 300g of butanol, and 50g of deionized water into a 2000mL three-neck flask, heat up to 40°C and stir well. Then slowly add 450g of 30wt% hydrogen peroxide solution dropwise under vigorous stirring, and control the dropping rate to keep the reaction temperature at about 50°C. After the dropwise addition, keep the temperature at 50°C for 4h. After the reaction was completed, the layers were separated, and the water phase was removed to obtain an oil phase.

[0029] Stir and mix the above-prepared oil phase with 200 g of diethanolamine, 50 g of ethanol, and 1 g of hydrochloric acid, and heat up to 40° C. under nitrogen protection. Under vigorous stirring, 180 g of 37% formaldehyde solution was added dropwise; after the dropwise addition, the temperature was raised to 80° C. under vigorous stirring and the reaction was continued for 3 hours. After the reaction was over, the layers...

Embodiment 2

[0031] Add 500g tung oil, 125g formic acid (85wt% solution), 0.5g concentrated sulfuric acid, 300g butanol, and 50g deionized water into a 2000mL three-neck flask, heat up to 45°C and stir well. Then slowly add 450g of 30wt% aqueous hydrogen peroxide dropwise under vigorous stirring, and control the rate of addition to keep the reaction temperature at about 65°C. After the dropwise addition, keep the temperature at 65°C for 6h. After the reaction was completed, the layers were separated, and the water phase was removed to obtain an oil phase.

[0032] Stir and mix the above-prepared oil phase with 200 g of diethanolamine, 50 g of ethanol, and 1 g of hydrochloric acid, and heat up to 40° C. under nitrogen protection. Under vigorous stirring, 180 g of 37% formaldehyde solution was added dropwise; after the dropwise addition, the temperature was raised to 90° C. under vigorous stirring and the reaction continued for 3 hours. After the reaction was over, the layers were left to s...

Embodiment 3

[0034] Add 500g tung oil, 125g formic acid (85wt% solution), 0.5g concentrated sulfuric acid, 300g butanol, and 50g deionized water into a 2000mL three-neck flask, heat up to 35°C and stir well. Then slowly add 450g of 30wt% hydrogen peroxide solution dropwise under vigorous stirring, and control the dropping rate to keep the reaction temperature at about 40°C. After the dropwise addition, keep the temperature at 40°C for 6h. After the reaction was completed, the layers were separated, and the water phase was removed to obtain an oil phase.

[0035] Stir and mix the above-prepared oil phase with 200 g of diethanolamine, 50 g of ethanol, and 1 g of hydrochloric acid, and heat up to 40° C. under nitrogen protection. Under vigorous stirring, 180 g of 37% formaldehyde solution was added dropwise; after the dropwise addition, the temperature was raised to 50° C. under vigorous stirring and the reaction continued for 2 hours. After the reaction was over, the layers were left to sta...

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Abstract

The invention relates to a preparation method for tung oil polyhydric alcohol with high hydroxyl value. The method comprises the following steps: (1) mixing tung oil, carboxylic acid, an acid catalyst, a hydroxylation reagent and deionized water, heating to 35-45 DEG C, dropwise adding a hydrogen peroxide solution while stirring while maintaining the temperature at 40-65 DEG C, and maintaining the reaction temperature for 2-8h after the ending of the dropwise adding, standing for layering after the ending of the reaction, and separating a water phase, thereby acquiring an oil phase; (2) mixing the oil phase with hydroxy-containing amine agents, adding ethyl alcohol and an inorganic acid catalyst, heating to 30-40 DEG C under nitrogen protection, dropwise adding an aldehyde agent while stirring, heating to 50-90 DEG C while violently stirring and continuously reacting for 1-5h after the ending of the dropwise adding, standing for layering after the ending of the reaction, neutralizing the oil phase, washing with water and performing reduced pressure distillation, thereby acquiring the tung oil polyhydric alcohol with high hydroxyl value. According to the invention, the hydroxylation agent is added in the epoxidation process, so that a cross-linking side reaction can be effectively avoided, a tung oil conjugated triene bond after loop opening is replaced, the cross-linking can be effectively avoided in the amine methylation process and the tung oil polyhydric alcohol with high hydroxyl value is acquired.

Description

technical field [0001] The invention belongs to the field of polyurethane materials, and in particular relates to a high-hydroxyl value tung oil polyol and a preparation method thereof. Background technique [0002] With the gradual depletion of global petrofossil resources, the development and utilization of biomass resources have attracted much attention. Vegetable oil is a triglyceride of long carbon chain acid containing double bonds. It is widely distributed in nature and has a wide variety. Common ones include tung oil, soybean oil, linseed oil, corn oil, rapeseed oil, peanut oil, olive oil, Palm oil, castor oil, etc. Due to its special structure and degradability, the polymers obtained from vegetable oils are not only low in cost, but also environmentally friendly, and are widely used in polyurethane, biodiesel, coatings, biomedical and other fields. [0003] Polyurethane materials have been widely used in industry and people's daily life due to their good mechanica...

Claims

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Application Information

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IPC IPC(8): C07C249/02
CPCC07C249/02
Inventor 李政李澜鹏白富栋薛冬乔凯王领民
Owner CHINA PETROLEUM & CHEM CORP
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