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A kind of preparation method of tung oil polyol

A technology of tung oil polyol and tung oil, which is applied in the field of polyurethane materials, can solve the problems of low reaction selectivity, lower product hydroxyl value, cross-linking side reactions, etc., achieve good biodegradability, prevent cross-linking side reactions, and make raw materials available The effect of regeneration

Active Publication Date: 2020-08-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, with the molecular oxygen / aldehyde catalytic oxidation system, the reaction temperature for vegetable oil to achieve a good epoxidation effect is usually above 65°C. It is not highly resistant, so cross-linking side reactions are prone to occur, resulting in a decrease in the hydroxyl value of the product and an increase in viscosity. Therefore, the molecular oxygen / aldehyde catalytic oxidation system is difficult to be used for the catalytic oxidation of tung oil polyols.

Method used

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  • A kind of preparation method of tung oil polyol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 500 g of tung oil, 70 g of acetaldehyde, 2.5 g of azobisisobutyronitrile, 150 g of n-hexanoic acid, and 50 g of deionized water into the autoclave, and stir evenly. Then feed nitrogen into the autoclave to replace the air in the autoclave for 3 times. After the replacement, fill the autoclave with an oxygen / nitrogen mixed gas with a volume ratio of 5 / 95 until the pressure in the autoclave reaches 7.5 MPa. Start stirring, control the reaction temperature to 70° C., react for 3.5 hours, and end the reaction. Open the purge valve to reduce the system pressure to normal pressure, and cool down to normal temperature. After the reaction system is separated, remove the water phase, wash the oil phase with 10wt% sodium bicarbonate aqueous solution to neutrality, and then wash it with 70°C hot water product 3 times. The washed product was distilled at 2000 Pa and 80°C for 2 hours to obtain tung oil polyol. After testing, the hydroxyl value is 246mgKOH / g, the viscosity is 7...

Embodiment 2

[0029] Add 500 g of tung oil, 90 g of propionaldehyde, 2.5 g of azobisisobutyronitrile, 100 g of n-hexanoic acid, and 50 g of deionized water into the autoclave, and stir evenly. Then feed nitrogen into the autoclave to replace the air in the autoclave for 3 times. After the replacement is completed, fill the autoclave with an oxygen / nitrogen mixed gas with a volume ratio of 5 / 95 until the pressure in the autoclave reaches 6.5 MPa. Start stirring, control the reaction temperature to 80° C., react for 2.5 hours, and end the reaction. The pressure of the system was lowered to normal pressure by opening the purge valve, and the temperature was lowered to normal temperature, and then the reaction system was washed with hot water at 70° C. for 3 times. The washed product was distilled at 2000 Pa and 80°C for 2 hours to obtain tung oil polyol. After testing, the hydroxyl value is 234mgKOH / g, the viscosity is 7210mPa·s, the acid value is 0.70mgKOH / g, the moisture is less than 0.1wt%...

Embodiment 3

[0031] Add 500 g of tung oil, 115 g of n-butyraldehyde, 3.8 g of azobisisoheptanonitrile, 200 g of n-hexanoic acid, and 50 g of deionized water into the autoclave, and stir evenly. Then feed nitrogen into the autoclave to replace the air in the autoclave for 3 times. After the replacement, fill the autoclave with an oxygen / nitrogen mixed gas with a volume ratio of 5 / 95 until the pressure in the autoclave reaches 8.5 MPa. Start stirring, control the reaction temperature to 65° C., react for 4 hours, and end the reaction. The pressure of the system was lowered to normal pressure by opening the purge valve, and the temperature was lowered to normal temperature, and then the reaction system was washed with hot water at 70° C. for 3 times. The washed product was distilled at 2000 Pa and 80°C for 2 hours to obtain tung oil polyol. After testing, the hydroxyl value is 208mgKOH / g, the viscosity is 7040mPa·s, the acid value is 0.68mgKOH / g, the moisture is less than 0.1wt%, and the yie...

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Abstract

The invention relates to a tung oil polyol preparation method, which comprises: adding tung oil, a hydroxylating reagent, deionized water, a co-oxidant aldehyde compound and a free radical initiator into an autoclave, introducing nitrogen gas into the autoclave to replace the air in the autoclave, and after completing the replacing, inflating the autoclave with oxygen / nitrogen mixed gas until the pressure in the autoclave achieve 6.0-8.5 MPa; starting stirring, controlling the reaction temperature at 65-80 DEG C, carrying out a reaction for 2.5-4.5 h, and ending the reaction; and reducing the pressure of the reaction system to a normal pressure, reducing the temperature to a room temperature, and carrying out water washing and pressure reducing distillation to obtain tung oil polyol. According to the present invention, the conjugated double bond of tung oil can improve the reactivity of the epoxy group, the molecular oxygen / aldehyde system is used to catalyze the epoxidation reaction, and the hydroxylating reagent is added while the epoxidation is performed, such that the occurrence of the cross-linked side reaction can be effectively avoided, and the tung oil polyol product can be synthesized; and the prepared tung oil polyol has the hydroxyl value of 120-270 mgKOH / g, the acid value of less than 1.0 mgKOH / g, the moisture content of less than 0.1 wt% and the yield of more than 92%, and is suitable for the preparation of polyurethane materials.

Description

technical field [0001] The invention belongs to the field of polyurethane materials, and in particular relates to a preparation method of tung oil polyol. 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 scarcity...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/36C07C67/26C07C69/33C08G101/00
CPCC07C67/26C07D301/16C07D303/42C08G18/36C08G2110/0025C07C69/33
Inventor 李风华李澜鹏白富栋乔凯王领民
Owner CHINA PETROLEUM & CHEM CORP