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Phosphorus-nitrogen synergistic flame-retardant polyester diol and preparation method thereof

A polyester diol, synergistic flame retardant technology, applied in the field of new functional polyester diol, can solve the problems of unstable structure of the final product, unfavorable for processing and application, hindering wide application, etc. The effect of advanced combustion technology, stable structure and low preparation cost

Active Publication Date: 2017-12-01
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, FRC-6 itself is easily decomposed by heat, and the reaction conditions are difficult to control. When the ratio of FRC-6 to reactants, reaction temperature and reaction steps are not well controlled, it is difficult to obtain the final product or the structure of the final product obtained is unstable, thus hindering Its wide application in polymer synthesis
In addition, the materials synthesized by FRC-6 as a reactive flame retardant are mostly colored, which is not conducive to subsequent further processing and application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The steps of this embodiment are as follows:

[0027] Step 1. Take adipic acid (8.8g) and melt it at 120°C in a reactor equipped with a PTFE stirring paddle, a thermometer and a nitrogen inlet;

[0028] Step 2: After adipic acid is melted, cool down to 85°C, add FRC-6 (7.7g), catalyst T-12 (0.12g), remove nitrogen at the same time, and install a water separator device;

[0029] Step 3: Add toluene (8.8g), gradually raise the temperature to 105°C, the heating rate is 5°C / 10min, and water will continue to flow out from the lower end of the water separator;

[0030] Step 4. After the reaction until no more water comes out from the lower end of the water separator, add 1,6-hexanediol (7.1g) and react for 2 hours. Remove the water separator and connect the four-necked bottle to a vacuum pump (vacuum degree is 0.05 MPa), and gradually increase the temperature to 155°C;

[0031] Step 5. After that, test the acid value of the system every 50 minutes until the acid value drops...

Embodiment 2

[0034] The preparation steps are the same as in Example 1.

[0035] The raw materials and their dosage are: adipic acid (8.8g), FRC-6 (12.24g), catalyst T-12 (0.12g), toluene (8.8g), 1,6-hexanediol (4.96g). The vacuum degree of the vacuum pump is 0.08MPa.

[0036] The conversion rate is 92.7%. The phosphorus-nitrogen synergistic flame-retardant polyester diol (PNJZ-2) prepared in this example is light brown paste solid, the hydroxyl value is 127 mgKOH / g, the molecular weight is 1590, and the phosphorus content is 14.7%.

Embodiment 3

[0038] The preparation steps are the same as in Example 1.

[0039] The raw materials and their dosage are: adipic acid (8.8g), FRC-6 (10.71g), catalyst T-12 (0.12g), toluene (8.8g), 1,6-hexanediol (5.67g). The vacuum degree of the vacuum pump is 0.08MPa.

[0040] The conversion rate is 93.1%. The phosphorus nitrogen synergistic flame retardant polyester diol (PNJZ-3) prepared in this example is milky white paste solid, the hydroxyl value is 130 mgKOH / g, the molecular weight is 1510, and the phosphorus content is 9.71%.

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Abstract

The invention provides phosphorus-nitrogen synergistic flame-retardant polyester diol and a preparation method thereof. The phosphorus-nitrogen synergistic flame-retardant polyester diol is prepared through reaction of the following raw materials of dibasic acid, dibasic alcohol, [[bis(2-ethoxyl]amino)methyl]diethyl phosphate (FRC-6), a catalyst and azeotrope at a certain ratio. The phosphorus-nitrogen synergistic flame-retardant polyester diol is stable in structure and adjustable in content of phosphorus and nitrogen elements, the hydroxyl value is 120-160mgKOH / g, the phosphorus-nitrogen synergistic flame-retardant polyester diol is good in heat stability, high in char yield and good in flame retardant property, simple in preparation technology and environment-friendly, and can be used as a main reaction material of polymer materials, such as polyurethane.

Description

technical field [0001] The invention belongs to the field of novel functional polyester diols, and in particular relates to a phosphorus- and nitrogen-containing polyester diol and a preparation method thereof. Background technique [0002] With the protection and attention of human beings to the green environment, flame-retardant polyurethane plastic products are more and more popular. Polyurethane flame-retardant methods include additive flame-retardant and reactive flame-retardant. The additive flame retardant is to directly add the flame retardant through physical action, and disperse the flame retardant in the polyurethane matrix. The most common and effective method is to add small molecule flame retardants. The common types are: inorganic flame retardants, phosphorus-nitrogen flame retardants, halogenated phosphate flame retardants, etc. Such as tris(2-chloropropyl)phosphate TCPP, dimethyl methylphosphate DMMP, tris(dibromopropyl)phosphate TBPP, trichloroethylphospha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/692C08G63/85C08G63/86C08G63/87
CPCC08G63/692C08G63/85C08G63/866C08G63/87
Inventor 顾丽敏于倩薛伟
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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