Preparation method of phosphorus-containing halogen-free environmentally-friendly flame-retardant polyester polyol

A flame retardant polyester and polyol technology, which is applied in the preparation of phosphorus-containing halogen-free environment-friendly flame retardant polyester polyol, and in the field of polyester polyol preparation, can solve the problem of human injury, reduced flame retardant performance, and volatility in confined spaces. The concentration of internal organic matter exceeds the standard and other problems, so as to achieve the effect of less by-products, fewer reaction steps and high yield

Active Publication Date: 2014-08-27
XUCHUAN CHEM SUZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the flame retardant of polyurethane is mainly realized by adding flame retardant later. The flame retardant performance achieved by this method will gradually decrease with time. In addition, since the flame retardant added afterward is usually a small molecule liquid substance, it is used For automotive interior and building interior materials, it will cause the concentration of volatile organic compounds in the confined space to exceed the stan

Method used

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  • Preparation method of phosphorus-containing halogen-free environmentally-friendly flame-retardant polyester polyol
  • Preparation method of phosphorus-containing halogen-free environmentally-friendly flame-retardant polyester polyol
  • Preparation method of phosphorus-containing halogen-free environmentally-friendly flame-retardant polyester polyol

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Embodiment 1

[0029] In a 500ml reaction flask equipped with a stirrer, nitrogen protection and condensing reflux device, add 174.36g, 0.81mol LDOPO and 93.6g, 0.81mol maleic acid, raise the temperature to slowly rise to 100-105°C, start stirring and nitrogen, and react After 180 minutes, add 117.95, 0.81moL adipic acid and 113.83g, 1.83moL ethylene glycol. After completely melting, slowly raise the temperature to 150-155°C to carry out esterification and dehydration reaction. After the dehydration is completed, raise the temperature to 200-210°C ℃, carry out transesterification reaction, after 180 minutes of reaction, check the acid value and hydroxyl value every 30 minutes.

[0030] The theoretical hydroxyl value of the phosphorus-containing polyester polyol synthesized in this embodiment is: 56mgKOH / g;

[0031] The theoretical average molecular weight (number average) of the phosphorus-containing polyester polyol synthesized by the present embodiment is: 2000;

[0032] The theoretical p...

Embodiment 2

[0035] In a 500ml reaction flask equipped with a stirrer, nitrogen protection and condensing reflux device, add 134.3g, 0.62mol LDOPO and 72.12g, 0.62mol maleic acid, heat up to 105-110°C slowly, start stirring and nitrogen, and react After 100 minutes, add 155g, 1.06moL of adipic acid and 38.6g, 0.43moL of 1,4-butanediol. After completely melting, slowly raise the temperature to 155-160°C for esterification and dehydration reaction. After the dehydration is completed, raise the temperature to 210-220°C, carry out transesterification reaction, after 150 minutes of reaction, check the acid value and hydroxyl value every 30 minutes, after the acid value and hydroxyl value pass the test, cool down to below 100°C, and discharge the material for packaging.

[0036] The theoretical hydroxyl value of the phosphorus-containing polyester polyol synthesized in this embodiment is: 224mgKOH / g;

[0037] The theoretical average molecular weight (number average) of the phosphorus-containing ...

Embodiment 3

[0041]In a 500ml reaction flask equipped with a stirrer, nitrogen protection and condensing reflux device, add 202.3g, 0.94mol LDOPO and 108.7g, 0.94mol maleic acid, raise the temperature to slowly rise to 110-115°C, start stirring and nitrogen, and react After 130 minutes, add 87.17g, 0.60moL of adipic acid and 43.17g, 0.48moL of 1,4-butanediol. After complete melting, slowly raise the temperature to 155-160°C for esterification and dehydration reaction. After the dehydration is completed, raise the temperature to 225-235°C, carry out transesterification reaction, after 120 minutes of reaction, check the acid value and hydroxyl value every 30 minutes, after the acid value and hydroxyl value pass the test, cool down to below 100°C, and discharge the material for packaging.

[0042] The theoretical hydroxyl value of the phosphorus-containing polyester polyol synthesized in this embodiment: 11.2mgKOH / g;

[0043] The theoretical average molecular weight (number average) of the ph...

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Abstract

The invention provides a preparation method of phosphorus-containing halogen-free environmentally-friendly flame-retardant polyester polyol. The method comprises the steps that with DOPO being starting material, firstly, the DOPO reacts with dibasic acid or dibasic acid anhydride to generate a DOPO complex intermediate; secondly, esterification dehydration reaction is performed on the generated intermediate, small-molecules polyol and dibasic acid or dibasic acid anhydride at 150 DEG C-160 DEG C; after the dehydration reaction is over, the temperature is raised to 200 DEG C-250 DEG C for transesterification, wherein the reaction time is 1 h-3 h, and in this way, the polyester polyol is obtained. The prepared polyester polyol is not conventional polyester polyol but the polyester polyol containing the phosphorus element, has the reactivity with isocyanate and can be used for permanent flame retardant modification of polyurethane products. As the phosphorus element is introduced to the polyester polyol, the polyester polyol contains phosphorus and is free of halogen, environmentally friendly and capable of inflaming retarding.

Description

technical field [0001] The invention belongs to the field of preparation methods of chemical products, and relates to a preparation method of polyester polyol, in particular to a preparation method of phosphorus-containing halogen-free environment-friendly flame-retardant polyester polyol. Background technique [0002] Polyester polyol is a class of chemical intermediates with a wide range of uses. It is mainly used in the production of polyurethane products, including thermoplastic polyurethane, polyurethane soft foam, polyurethane rigid foam, solvent-based polyurethane resin and water-based polyurethane resin. [0003] In many civilian products of polyurethane, certain flame retardant performance is required, such as: polyurethane rigid foam used for external wall insulation, polyurethane soft foam used for sofa and car seat lining, used for the production of synthetic leather for sofas, automobiles, etc. Polyurethane resins for upholstery and architectural upholstery. ...

Claims

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Application Information

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IPC IPC(8): C08G63/692C08G63/78C08G18/46
Inventor 夏佳弟吕华波江平
Owner XUCHUAN CHEM SUZHOU
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