Preparation method of organism-based polyalcohol based on epoxidized plant oil and hydroxylamine compound

A bio-based polyol and epoxy vegetable oil technology, which is applied in the preparation of organic compounds, carboxylic acid amide preparation, chemical instruments and methods, etc., can solve the problem of high cost of industrial use of ozone

Inactive Publication Date: 2011-08-03
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In the above method for preparing vegetable oil-based polyols, the alcoholysis reaction described in method 1) is usually carried out at high temperature; in method 2), the industrial use cost of ozone is relatively high

Method used

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  • Preparation method of organism-based polyalcohol based on epoxidized plant oil and hydroxylamine compound
  • Preparation method of organism-based polyalcohol based on epoxidized plant oil and hydroxylamine compound
  • Preparation method of organism-based polyalcohol based on epoxidized plant oil and hydroxylamine compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 250ml reactor, 25g of epoxidized soybean oil and 16g of 2-hydroxypropylamine were added, the above mixture was stirred evenly, and the temperature was raised to 90°C, and the stirring was continued, and the reaction was carried out for 24h. Then the reaction system was washed with high-purity water to remove unreacted 2-hydroxypropylamine, and the water was removed by rotary evaporation to obtain a viscous liquid. Add 3.7% hydrochloric acid to make the system weakly acidic, stir the system at 25°C for 30 minutes, then add 10% aqueous sodium hydroxide solution to make the system weakly alkaline. Add 250 mL of chloroform to extract the reaction product, and wash the organic phase with water for more than three times, each time with 250 mL of water. The organic phase is taken out, and the organic solvent is removed by a rotary evaporator to obtain a polyol product. product of 1 H NMR spectrum as figure 2 shown.

Embodiment 2

[0029] In a 250ml reactor, add 25g of epoxidized soybean oil and 20g of 2-hydroxypropylamine, stir the above mixture evenly, and raise the temperature to 90°C, continue stirring, and the reaction proceeds for 24h. Then the reaction system was washed with high-purity water to remove unreacted 2-hydroxypropylamine, and the water was removed by rotary evaporation to obtain a viscous liquid. Add acetic acid for treatment to make the system weakly acidic, stir the system at 75°C for one hour, then add 10% aqueous sodium hydroxide solution to make the system weakly alkaline. Add 250 mL of chloroform to extract the reaction product, and wash the organic phase with water for more than three times, each time with 250 mL of water. The organic phase is taken out, and the organic solvent is removed by a rotary evaporator to obtain a polyol product.

Embodiment 3

[0031] In a 250ml reactor, 25g of epoxidized soybean oil and 12g of ethanolamine were added, the above mixture was stirred evenly, and the temperature was raised to 90°C, stirring was continued, and the reaction was carried out for 24h. Then the reaction system was washed with high-purity water to remove unreacted ethanolamine, and the water was removed by rotary evaporation to obtain a viscous liquid. Add 2% benzene methanesulfonic acid to make the system weakly acidic, stir the system at 75°C for one hour, then add 10% potassium hydroxide aqueous solution to make the system weakly alkaline. Add 250 mL of diethyl ether to extract the reaction product, and wash the organic phase with water for more than three times, each time with 250 mL of water. The organic phase is taken out, and the organic solvent is removed by a rotary evaporator to obtain a polyol product.

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Abstract

The invention relates to a preparation method of organism-based polyalcohol based on epoxidized plant oil and a hydroxylamine compound. The preparation method is characterized by comprising the following steps: 1) mixing the epoxidized plant oil with the hydroxylamine compound for reaction, carrying out ring-opening reaction on amino of the epoxidized plant oil and an epoxy group, and simultaneously reacting with an ester bond so as to generate an amido bond, thereby further generating a polyalcohol compound; 2) successively processing reaction products with acid and alkali so as to mainly remove the unreacted hydroxylamine compound; and 3) further separating and purifying so as to obtain the organism-based polyalcohol. In the preparation method, the regenerative resource plant oil is used as a main raw material; and reaction lines are novel and simple; and the obtained product is suitable for polyurethane material preparation and the like, and belongs to the technical fields of chemical materials and production thereof.

Description

technical field [0001] The invention relates to a method for preparing bio-based polyols based on epoxy vegetable oil and hydroxylamine compounds, and belongs to the technical field of chemical materials and their production. Background technique [0002] In recent years, the production of vegetable oil-based polyols has aroused great interest of scientists from various countries. Vegetable oil polyol is an important renewable resource, which can react with diisocyanate compounds to form polyurethane, and is a good substitute raw material for petroleum-based polyol compounds. The methods for preparing vegetable oil-based polyols mainly contain at present: [0003] 1) Carry out alcoholysis reaction of vegetable oil and polyol to generate polyol. The polyhydric alcohol used is usually glycerol, and the obtained polyhydroxy compound is usually diacylglyceride or monoacylglyceride, and the alcoholysis reaction is usually carried out in the presence of a catalyst. (Pro. Polym....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C237/08C07C237/04C07C231/02C08G18/32
Inventor 王平苗士达张松平苏志国
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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