One-step preparation method of polyol with soybean oil

A technology of soybean oil and polyols, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of epoxy soybean oil loss, cumbersome steps, and waste of time

Inactive Publication Date: 2010-06-23
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The soybean oil polyol synthesized by this two-step method has a hydroxyl value between 200-600mgKOH / g, but it also has its disadvantages. Because the epoxidized soybean oil needs to be purified in the middle, the steps are cumbersome, time-wasting, and in the separation process. loss of epoxidized soybean oil

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 (two-step method)

[0019] The soybean oil of 80ml (the iodine value is divided into and preferably between 80-240), 16ml glacial acetic acid, 0.16ml vitriol oil are added in the 250mL there-necked flask with stirrer, this there-necked flask is transferred in the water bath, And control the temperature to 50°C, then add 48ml of hydrogen peroxide dropwise. During the process of adding hydrogen peroxide, the rate of addition must be controlled, and the addition should be completed within about 1 hour, so that the heat released by the reaction of hydrogen peroxide and glacial acetic acid will not increase the temperature of the material by more than 2°C. After the reaction was carried out for 6 hours, the oil phase was separated with a separatory funnel to obtain epoxidized soybean oil. Then the second step, get 80ml of epoxidized soybean oil, 60mL of methanol, 10ml of water, 2ml of fluoroboric acid (40% aqueous solution) and join in the epoxidized soybean oi...

Embodiment 2

[0020] Embodiment 2 (two-step method)

[0021] Mix 48ml of hydrogen peroxide, 16ml of glacial acetic acid, and 5 grams of cationic resin (for example, 7321 type strong acidic cationic exchange resin, domestic, can be used repeatedly, and have been converted into hydrogen form before use) as solution I, take 80ml of soybean oil and add Transfer to a 250mL three-necked flask with a stirrer, transfer the three-necked flask to a water bath to heat and stir, the temperature is controlled at 55°C, and then add the mixed solution I dropwise. Control the rate of addition and complete the addition within about 1 hour, so that the heat released from the reaction of hydrogen peroxide and glacial acetic acid will not increase the temperature of the material by more than 2°C. After reacting for 6 hours, filter, recover and regenerate the cation exchange resin, ready for next use. Separation with a separatory funnel to separate the oil phase to obtain epoxidized soybean oil. Then the seco...

Embodiment 3

[0022] Embodiment 3 (one-step method)

[0023] Mix 60ml of glacial acetic acid, 0.16ml of concentrated sulfuric acid, and 48ml of hydrogen peroxide to obtain solution I; mix 60mL of methanol, 6ml of water, and 2ml of fluoboric acid (40% aqueous solution) to obtain solution II. Take 80ml of soybean oil (the iodine value is preferably between 80-240) and add it to a 500mL three-necked flask with a stirrer, turn this three-necked flask into a water bath and heat and stir, then add the mixed solution II , and control the temperature to about 55°C. Then the mixed solution I was added dropwise, and the dropwise addition was completed within 1 hour. After the dropwise addition, the reaction was continued for 5 hours, and the reaction temperature was always controlled at about 55°C. After the end, separate the liquid with a separatory funnel, and add a little NaCl to separate the oil phase. Add ammonia water for neutralization, and wash the oil phase with water repeatedly until the...

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Abstract

The invention discloses a one-step synthesis preparation method of soybean oil polyol. In the last patent 200710151008.8, the two-step synthesis method of soybean oil polyol is provided. According to the same principle, the two-step method is evolved into the one-step method, and the soybean oil is directly synthesized into polyol by the one-step method. The invention has the advantages that: the middle separation process of epoxidized soybean oil and water is eliminated, and simultaneously the process that the PH value is adjusted to be neutral is eliminated, so that the reaction cycle is greatly shortened, thereby, the reaction time is shortened to 5 to 8 hours; and simultaneously, the loss of epoxidized soybean oil during middle treatment is also eliminated, and the obtained polyol hydroxyl value after the reaction is between 200 to 500mgKOH / g; and the viscosity can be controlled by changing distillation temperature. The polyol is mainly used to partly or fully replace polyether or polyester polyols to synthesize polyurethane foam.

Description

technical field [0001] The invention relates to a preparation process of soybean oil polyol. On the basis of the foregoing, the two-step method is synthesized into a one-step method to prepare polyols, which can partially or completely replace polyether or polyester polyols to synthesize polyurethane foam plastics. Background technique [0002] With the increasing crisis of natural non-renewable resources such as oil and the greenhouse effect. Based on considerations of economy, environmental friendliness and sustainability, people pay more attention to bio-renewable resources. In the polyurethane industry, the preparation of soybean oil polyols instead of petroleum-based polyols for the synthesis of polyurethanes has attracted more and more attention. [0003] As mentioned above, there are four common methods for preparing soybean oil polyols: 1) transesterification method. 2) Ozonation method, which first breaks unsaturated double bonds with ozone, and then prepares hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/31C07C69/675
Inventor 李渊王玉峰
Owner TIANJIN POLYTECHNIC UNIV
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