Inflaming retarding bio-based polyhydric alcohol and preparation method thereof

A bio-based polyol, flame-retardant technology, applied in the direction of cyanide reaction preparation, organic compound preparation, carboxylate preparation, etc., can solve non-degradable problems, and achieve non-degradable, reduced dependence, enhanced phase Capacitance and Adhesion Effects

Active Publication Date: 2014-12-24
PANZHIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, tung oil is used as raw material, which is easy to obtain and is a bio-renewable resource, which helps reduce the dependence of the polyurethane industry on petroleum raw materials, is conducive to sustainable development, and also solves the non-degradable problem of existing petroleum-based polyurethane foam plastics

Method used

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  • Inflaming retarding bio-based polyhydric alcohol and preparation method thereof
  • Inflaming retarding bio-based polyhydric alcohol and preparation method thereof
  • Inflaming retarding bio-based polyhydric alcohol and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Step a: In a 250mL three-necked flask, add 6.7gKOH, 60mL methanol and 30mL water, stir and heat to 70°C, quickly add 29.9g tung oil, the reaction time is 2h, and after refining, 28.6g of light yellow liquid tungoleic acid, acid The value is 195.8mg / g;

[0052] Steps b and c: Add 13.8g glycerol and 6.2g boric acid into a four-necked flask, under the protection of inert gas, control the temperature at 200°C, and the reaction time is 1.5h, then refine to obtain boric acid diglyceride, then add 28.7g tung oil acid and 0.3g p-toluenesulfonic acid, the temperature is controlled at 220°C, and after 2 hours of reaction, the glyceryl oleic acid borate is obtained. Glyceride product 35.2g;

[0053] Step d: Take 20 g of monoglyceride oleic acid, add 1.48 g of formic acid (85%), and 0.1 mL of phosphoric acid into a 250 mL three-necked flask, stir, add 10.2 g of hydrogen peroxide (30%) dropwise, and react at 60 ° C for 6 h. After being refined, epoxy oleic acid ester was obtained,...

Embodiment 2

[0058] Step a: In a 250mL three-necked flask, add 7.8g NaOH, 70mL ethanol and 35mL water, stir and heat to 60°C, quickly add 34.9g tung oil, the reaction time is 1.5h, and after refining, 32.8g of light yellow liquid tungoleic acid is obtained, The acid value is 199.5mg / g;

[0059] Steps b and c: Add 16.5g glycerin and 9.3g boric acid into a four-neck flask, under the protection of inert gas, control the temperature at 180°C, and the reaction time is 2h, then refine to obtain boric acid diglyceride, then add 34.8g oleic acid and 0.4g of phosphoric acid, the temperature is controlled at 230°C, and after 1.5h of reaction to obtain boric acid glycerides, at room temperature, use 2mol / L hydrochloric acid solution to hydrolyze glycerol borates, and then obtain monoglycerides of oleic acid after refining 39.4g;

[0060] Step d: Take 25g of monoglyceride oleic acid, add 1.85g of formic acid (85%), and 0.1ml of phosphoric acid into a 250ml three-necked flask, stir, add 12.7g of hydro...

Embodiment 3

[0065] Step a: In a 250mL three-necked flask, add 7.8g NaOH, 70mL ethanol and 35mL water, stir and heat to 60°C, quickly add 34.9g tung oil, the reaction time is 1.5h, and after refining, 32.8g of light yellow liquid tungoleic acid is obtained, The acid value is 199.5mg / g;

[0066] Steps b and c: Add 16.5g glycerin and 9.3g boric acid into a four-neck flask, under the protection of inert gas, control the temperature at 180°C, and the reaction time is 2h, then refine to obtain boric acid diglyceride, then add 34.8g oleic acid and 0.4g of phosphoric acid, the temperature is controlled at 230°C, and after 1.5h of reaction to obtain boric acid glycerides, at room temperature, use 2mol / L hydrochloric acid solution to hydrolyze glycerol borates, and then obtain monoglycerides of oleic acid after refining 39.4g;

[0067] Step d: Take 25g of monoglyceride oleic acid, add 1.85g of formic acid (85%), and 0.1ml of phosphoric acid into a 250ml three-necked flask, stir, add 12.7g of hydro...

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Abstract

The invention belongs to the field of chemical synthesis and particularly relates to a preparation method of inflaming retarding bio-based polyhydric alcohol. The preparation method includes the following steps: enabling tung oil to have saponification reaction in a solvent to generate eleostearic acid, conducting esterification on glycerin and boric acid to generate boric acid diglyceride, then enabling the boric acid diglyceride and the eleostearic acid to have esterification reaction to generate tung oil acid boric acid glyceride, then hydrolyzing the tung oil acid boric acid glyceride to generate eleostearic acid monoglyceride, then adding an epoxidizing agent into the eleostearic acid monoglyceride to conduct epoxidation reaction to generate epoxy tung oil acid ester, meanwhile utilizing a silane coupling agent to modify expansible graphite, and finally enabling the epoxy eleostearic acid ester to react with a ring opening agent. The bio-based polyhydric alcohol obtained through the method can replace petrochemical polyether polyhydric alcohol to prepare polyurethane foaming plastic, and dependence on petrochemical products is reduced.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a flame-retardant bio-based polyol and a preparation method thereof. Background technique [0002] As we all know, expandable graphite (EG) is one of the high-quality flame retardants of polyurethane foam. Under high temperature conditions, EG is heated rapidly, and the intercalated substances between graphite sheets are thermally decomposed, vaporized, or oxidized and reduced with graphite. The reaction produces a large amount of gas. The connection between the graphite sheets is first expanded by the gas, and the distance between the graphite sheets expands again, forming a fluffy expanded graphite. The expansion multiple can reach hundreds of times. The purpose of flame retardant polyurethane foam. [0003] However, EG has poor compatibility with polyurethane foam, which makes it difficult to disperse EG particles in the polyurethane foam matrix. At the same time...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C08K9/06C08K3/04
CPCC07C51/09C07C67/31C07C227/04C07D301/14C07F5/04C07F7/1892C08G18/36C07C57/12C07C69/58C07C229/30
Inventor 周才龙李玉峰杨塑张湖川王晓波李博陈祖团
Owner PANZHIHUA UNIV
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