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A kind of method and application of bio-oil for preparing polyol

A polyol and bio-oil technology, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., can solve the problems of catalysts that cannot be recycled repeatedly and high toxicity, so as to avoid white pollution, reduce the discharge of three wastes, Effects from a wide range of sources

Active Publication Date: 2016-06-15
ZHEJIANG HENGFENG NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Alkoxylation ring-opening is also carried out under homogeneous catalytic conditions such as fluoboric acid, the catalyst cannot be recycled repeatedly, and the toxicity is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A kind of bio-oil preparation method of polyol of the present embodiment comprises the following steps:

[0016] The first step methyl esterification reaction process

[0017] Stir and mix rapeseed oil and methanol, control the mass ratio of bio-oil and methanol to 1:0.25, add potassium fluoride-supported magnesium oxide solid base catalyst, the amount of catalyst is 1% of the total mass of reactants, and heat at 70°C After stirring for 1.5h, the catalyst was recovered by filtration, excess methanol was distilled off, and layered, the upper layer was fatty acid methyl ester, and the yield was 98%, and the lower layer was glycerol, which was collected;

[0018] Synthesis of the 2nd step ionic liquid catalyst

[0019] Stir equimolar pyridine and propane sultone at room temperature for 72 hours to form a white ylide precipitate, filter the formed ylide, wash with ether three times, dry, and then acidify with equimolar tungstic acid , to obtain an ionic liquid catalyst wi...

Embodiment 2

[0024] A kind of bio-oil preparation method of polyol of the present embodiment comprises the following steps:

[0025] The first step methyl esterification reaction process

[0026] Stir and mix soybean oil and methanol, control the mass ratio of bio-oil and methanol to 1:0.25, add potassium fluoride-supported magnesium oxide solid base catalyst, the catalyst dosage is 0.8% of the total mass of reactants, and heat and stir at 65°C After 1.0h, the catalyst was recovered by filtration, the catalyst could be directly reused, excess methanol was distilled off, and layered, the upper layer was fatty acid methyl ester with a yield of 95%, and the lower layer was collected from glycerin;

[0027] Synthesis of the 2nd step ionic liquid catalyst

[0028] Stir equimolar methylimidazole and propane sultone at room temperature for 72 hours to form a white ylide precipitate, filter the formed ylide, wash 3 times with ether, dry, and then use equimolar phosphotungsten Acidification with ...

Embodiment 3

[0033] A kind of bio-oil preparation method of polyol of the present embodiment comprises the following steps:

[0034] The first step methyl esterification reaction process

[0035] Stir and mix cottonseed oil and methanol, control the mass ratio of bio-oil and methanol to 1:0.3, add potassium fluoride-supported magnesium oxide solid base catalyst, the catalyst dosage is 1% of the total mass of reactants, and heat and stir at 70°C After 2 hours, the catalyst was recovered by filtration, the catalyst could be reused directly, excess methanol was distilled off, and layered, the upper layer was fatty acid methyl ester with a yield of 99%, and the lower layer was collected from glycerin;

[0036] Synthesis of the 2nd step ionic liquid catalyst

[0037] Stir the equimolar butyl imidazole and butane sultone at room temperature for 72 hours to form a white ylide precipitate, filter the formed ylide, wash 3 times with ether, dry, and then, use an equimolar silicon Acidification wit...

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Abstract

The invention discloses a method for preparing polyol by using bio-oil. The method comprises the following steps: firstly performing methyl esterification, namely, performing ester exchange on biolipid and methanol under the catalysis of potassium fluoride loaded magnesium oxide solid alkali, converting the obtained product into fatty acid methyl ester with small molecular weight and byproduct glycerol, filtering to recycle the catalyst, and separating lower-layer glycerol; performing epoxidation on upper-layer fatty acid methyl ester in 30% of hydrogen peroxide under the catalysis of ionic liquid so as to form epoxidized fatty acid methyl ester.; then adding the glycerol in the methyl esterification process, continuously performing alkoxide ring-opening under the catalysis of ionic liquid, introducing hydroxyl, and finally separating liquid to recycle the ionic liquid catalyst, reducing pressure and distilling the upper-layer to remove water so as to obtain low-viscosity bio-oil-based polyol. The raw material is easily available, recyclable and good in biodegradability, the preparation process is environmental friendly, the industrial three-waste emission is small, the product structure and a hydroxyl value are adjustable, the application range is wide, and the environment influence level is low.

Description

technical field [0001] The invention relates to a method and application for preparing polyols from biological oil, and belongs to the technical field of organic chemical synthesis. Background technique [0002] Polyurethane materials have been widely valued for their excellent performance, wide range of uses, and various types. The research and attention to them have become increasingly close. In recent years, they have become the sixth largest synthetic material in the field of polymers. Polyurethane polyols are generally polyoxyalkylene polyols with high functionality and high hydroxyl value (low molecular weight), that is, "polyether polyols". Polyether polyols are usually prepared by ring-opening polymerization of high-functionality small molecule alcohols or amine initiators with propylene oxide (PO), ethylene oxide (EO), etc. under the action of a catalyst. Although the structural properties of this type of rigid foam polyether can be adjusted through the selection o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/31C07C69/675C07C69/732C08G18/28C09D175/04C09J175/04
CPCY02P20/584
Inventor 山柏芳梁学正
Owner ZHEJIANG HENGFENG NEW MATERIAL
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