Preparation method of linear thermal-reversible polyurethane polymer with flame retardancy and polymer

A technology of polyurethane polymer and flame retardant performance, which is applied in the field of polymer material synthesis and preparation, can solve the problems of complex synthesis process, etc., and achieve the effect of simple preparation method, good flame retardancy and short preparation cycle

Inactive Publication Date: 2019-03-15
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the synthesis process of this method is

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 30g of polytetrahydrofuran ether diol (PTMG-1000) with a relative number average molecular weight of 1000 and 3.66g of tetrachlorobisphenol A into a 250ml three-necked flask, melt and stir at 80°C for 25min; then add 9.80g of 4,4-bisphenol Phenylmethane diisocyanate (MDI), stirred rapidly for 5min. Finally, the mixture was aged in a vacuum oven at 80° C. for 5 hours, and then slowly cooled to room temperature to obtain a linear thermoreversible polyurethane polymer with flame retardancy. According to the infrared test under heating and cooling, the synthesized polymer has thermal reversible behavior at about 100°C; and the flame retardant performance test is carried out according to the measurement standard of GB 2406-80 limiting oxygen index, and the limiting oxygen index of the polymer can reach 27.5.

[0025] The molar ratio of polyols and halogenated bisphenol chain extenders is 3:1;

[0026] The NCO to OH molar ratio is 0.98:1.

Embodiment 2

[0028] Add 30g of polytetrahydrofuran ether diol (PTMG-1000) and 8.16g of tetrabromobisphenol A in a 250ml three-necked flask with a relative number average molecular weight of 1000, melt and stir at 90°C for 15min; then add 7.83g of toluene diisocyanate ( TDI-100), stirring rapidly for 3min. Finally, the mixture was aged in a vacuum oven at 85° C. for 4.5 hours, and then slowly cooled to room temperature to obtain a linear thermoreversible polyurethane polymer with flame-retardant properties. According to the infrared test under heating and cooling, the synthesized polymer has thermally reversible behavior at around 95°C; and the flame retardant performance test is carried out according to the measurement standard of GB 2406-80 limiting oxygen index, and the limiting oxygen index of the polymer can reach 29.

[0029] The molar ratio of polyols and halogenated bisphenol chain extenders is 2:1;

[0030] NCO and OH molar ratio is 1:1.

Embodiment 3

[0032] Add 30g of poly-1,4-butylene adipate diol (PBA-1000) with a relative number average molecular weight of 1000 and 5.44g of tetrabromobisphenol A into a 250ml three-necked flask, melt and stir for 30min at 70°C ; Then add 6.89g toluene diisocyanate (TDI-100), and stir rapidly for 4min. Finally, the mixture was aged in a vacuum oven at 90° C. for 3.5 hours, and then slowly cooled to room temperature to obtain a linear thermoreversible polyurethane polymer with flame-retardant properties. According to the infrared test under heating and cooling, the synthesized polymer has thermal reversible behavior at about 95°C; and the flame retardant performance test is carried out according to the measurement standard of GB 2406-80 limiting oxygen index, and the limiting oxygen index of the polymer can reach 30.

[0033] The molar ratio of polyols and halogenated bisphenol chain extenders is 3:1;

[0034] The NCO and OH molar ratio is 0.99:1.

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Abstract

The invention discloses a preparation method of a linear thermal-reversible polyurethane polymer with flame retardancy. The preparation method comprises the following steps: step (1) melting and stirring polyol and a halogenated bisphenol chain extender at 60-80 DEG C for 10-30 min, wherein a molar ratio of the polyol to the halogenated bisphenol chain extender is (2-3) : 1; and step (2) adding anisocyanate compound into a mixture according to a molar ratio of NCO to OH of 0.97-1.02, rapidly stirring for 2-5 min, then placing in a vacuum oven at 70-100 DEG C, curing for 3-5 h, and slowly cooling to room temperature. The preparation method provided by the invention has the advantages of readily available reaction raw materials, simple method and convenient operation, and has great significance in actual application of thermoplastic polyurethane.

Description

technical field [0001] The invention relates to the field of polymer material synthesis and preparation, and furthermore, relates to a method for preparing a linear thermally reversible polyurethane polymer with flame-retardant properties and the polymer. Background technique [0002] Thermoplastic polyurethane has high modulus, high strength, excellent wear resistance, chemical resistance, hydrolysis resistance, high and low temperature resistance and mold resistance due to the existence of phase separation between soft and hard segments and hydrogen bonding between hard segments. Performance, so that it is widely used in shoe materials, cables, clothing, automobiles, medicine and health, pipes, films and sheets, etc., and has become one of the important thermoplastic materials. In particular, the thermoreversible polyurethanes that have emerged in recent years have expanded the functionality of the material itself, but these thermoreversible polyurethanes are as easy to bu...

Claims

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Application Information

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IPC IPC(8): C08G18/76C08G18/66C08G18/48C08G18/42C08G18/32
CPCC08G18/3808C08G18/381C08G18/4238C08G18/4277C08G18/4854C08G18/7614C08G18/7671
Inventor 张军营裴须强刘鑫程珏
Owner BEIJING UNIV OF CHEM TECH
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