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Synthetic method and application of dibasic acid ester oligomer flame retardant

A technology of dibasic acid ester and synthesis method, which is applied in the field of polyurethane foam, can solve the problems of high polarity of THPO and reduce the mechanical properties of PU, and achieve the effects of good dimensional stability, easy promotion and use, and good flame retardant effect

Active Publication Date: 2021-04-20
湖北省兴发磷化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of production and application, THPO still suffers from the following two disadvantages: the hydroxyl value of THPO is about 1200, which is much higher than the 400-500 of polyols, so in the foaming process, the addition of THPO will significantly reduce the PU Mechanical properties; THPO is very polar and cannot be well dispersed in polyols

Method used

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  • Synthetic method and application of dibasic acid ester oligomer flame retardant
  • Synthetic method and application of dibasic acid ester oligomer flame retardant
  • Synthetic method and application of dibasic acid ester oligomer flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 1 mol of THPO and 0.05% dibutyltin laurate of the mass of THPO into a three-necked flask, adjust the temperature to 10°C, and the pressure of the entire system is about 0.8 atmospheres, add 1 mol of oxalyl chloride drop by drop, about 1 After the dropwise addition, keep the temperature for 3 hours and cool to room temperature to obtain the above-mentioned dibasic acid ester oligomer flame retardant, marked as FR-1.

[0032] According to the NMR results, the structural formula of FR-1 is:

[0033]

[0034] The H NMR spectrum comparison chart of the prepared flame retardant FR-1 and THPO shows that the peak at 3.6ppm belongs to the H of the methylene of THPO, and the chemical shift of the H on the methylene appears obvious after reacting with oxalyl chloride The shift towards high chemical shift direction, located around 4.2 ppm, proves the successful preparation of FR-1.

Embodiment 2

[0036] Add 1 mol of THPO and 0.25% tetrabutyl titanate of THPO mass into a three-necked flask, adjust the temperature to 200°C, the pressure of the whole system is about 0.8 atmospheres, and gradually add 0.5 mol of succinic acid for about 1 hour After the dropwise addition, heat-retain and react for 1 hour, and cool to room temperature to obtain the above-mentioned dibasic acid ester oligomer flame retardant, marked as FR-2.

[0037] The structural formula of FR-2 is:

[0038]

Embodiment 3

[0040] Add 1 mol of THPO and 0.15% stannous chloride of THPO mass into a three-necked flask, adjust the temperature to 180°C, the pressure of the whole system is about 0.8 atmospheres, gradually add 1.2 mol of adipic acid, and add in about 1 hour After the completion of the heat preservation reaction for 5 hours, cooled to room temperature, the above-mentioned dibasic acid ester oligomer flame retardant can be obtained, which is marked as FR-3.

[0041] The structural formula of FR-3 is:

[0042]

[0043] In the formula, R is a linear alkylene group with 4 carbon atoms, n=8.

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Abstract

The invention relates to a synthesis method of a dibasic acid ester oligomer flame retardant and application of the dibasic acid ester oligomer flame retardant in polyurethane foams. The synthesis method comprises the following steps: adding THPO and a certain mass of catalyst into a container, regulating the reaction temperature to 10-200 DEG C and the pressure of the whole system to 0.5-0.8 atm, and gradually adding a certain mass of dibasic acid, anhydride or acyl chloride to obtain a prepolymer, after dropwise adding, carrying out heat preservation reaction for 1-5 hours, and cooling to room temperature, so as to obtain the dibasic acid ester oligomer flame retardant. The prepared flame retardant has the advantages of high compatibility with polyether / polyester polyol, high flame retardant efficiency, simple foaming process and the like, and is suitable for flame retardance of various polyurethane foams.

Description

technical field [0001] The invention belongs to the technical field of preparation of dibasic acid ester oligomer flame retardants, and in particular relates to a preparation method of a dibasic acid ester oligomer flame retardant and a flame-retardant polyurethane foam using the dibasic acid ester oligomer flame retardants. Background technique [0002] Polyurethane foam (PU) is widely used in the packaging of building insulation materials, vehicles, furniture pads and electronic equipment due to its light weight, good chemical stability, corrosion resistance, and excellent weather resistance. Due to the high content of hydrocarbon chain segments and large specific surface area in PU, it is easy to decompose and burn when heated, and its limiting oxygen index (LOI) is only 16-18%; PU produces a large amount of toxic smoke such as hydrogen cyanide and carbon monoxide when burning etc. have brought serious threats to people's lives and property safety. Therefore, the flame r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53C08G18/32C08G101/00
Inventor 黄胜超屈满意陈松曹清章田路王大鹏陈秋阳
Owner 湖北省兴发磷化工研究院有限公司