Reactive type intumescent flame retardant for water-based polyurethane and preparation method of reactive type intumescent flame retardant

An intumescent flame retardant and water-based polyurethane technology, which is applied in the field of fine chemicals, can solve the problems of low content, high functionality that makes the polymerization process difficult to control, and the influence of thermodynamic properties of polyurethane coating materials. It achieves good thermal stability, Easy to control thermodynamic properties and excellent storage stability

Active Publication Date: 2015-04-08
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of phosphorus (14.26%) and nitrogen (6.45%) in the flame retardant disclosed in this patent is low, and the four hydroxyl groups in the molecule react with polyurethane to form a cross-linked network structure. The h

Method used

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  • Reactive type intumescent flame retardant for water-based polyurethane and preparation method of reactive type intumescent flame retardant
  • Reactive type intumescent flame retardant for water-based polyurethane and preparation method of reactive type intumescent flame retardant
  • Reactive type intumescent flame retardant for water-based polyurethane and preparation method of reactive type intumescent flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] (1) Add 34.04g (0.25mol) of pentaerythritol and 230.0g (1.50mol) of phosphorus oxychloride to a 250ml four-neck flask equipped with a mechanical stirrer, a thermometer, and a nitrogen condensing reflux tube, heat in an oil bath, and reflux for reaction. React at 60°C for 4h, then heat up to 100°C for 6h. After distilling off unreacted phosphorus oxychloride under reduced pressure, cool, filter, wash with dichloromethane, filter, and vacuum dry at 70°C to obtain white powdered pentaerythritol diphosphate diphosphoryl chloride with a yield of 83%;

[0043] (2) Add 14.85g (0.05mol) of pentaerythritol diphosphate diphosphoryl chloride and 16.94 (0.12mol) of 2,4-diamino- For 6-methoxy-1,3,5-triazine, add 100ml of acetonitrile, stir, dissolve, add 7.91g (0.10mol) of pyridine, heat in an oil bath, and reflux for reaction. Slowly raise the temperature to 80°C and react for 8h. Cool, filter, wash with acetone, and vacuum dry at 70°C to obtain a white powdery reactive intumesce...

Embodiment 2

[0045] (1) Add 34.04g (0.25mol) of pentaerythritol and 211.6g (1.38mol) of phosphorus oxychloride to a 250ml four-necked flask equipped with a mechanical stirrer, a thermometer, and a nitrogen condensing reflux tube, heat in an oil bath, and reflux for reaction. React at 80°C for 2h, then raise the temperature to 110°C for 4h. After the unreacted phosphorus oxychloride was distilled off under reduced pressure, cooled, filtered, washed with dichloromethane, filtered, and vacuum-dried at 80°C to obtain white powdered pentaerythritol diphosphate diphosphoryl chloride, the yield was 82%;

[0046] (2) Add 14.85g (0.05mol) of pentaerythritol diphosphate diphosphoryl chloride and 12.51 (0.10mol) of 2,4-diamino- 6-methyl-1,3,5-triazine, add 100ml N,N - Dimethylformamide, stirred, dissolved, added 15.18g (0.15mol) triethylamine, heated in an oil bath, reflux reaction. Slowly raise the temperature to 90°C and react for 6h. Cool, filter, wash with methyl ethyl ketone and dichlorometha...

Embodiment 3

[0048] (1) Add 34.04g (0.25mol) of pentaerythritol and 214.7g (1.40mol) of phosphorus oxychloride to a 250ml four-neck flask equipped with a mechanical stirrer, a thermometer, and a nitrogen condensing reflux tube, heat in an oil bath, and reflux for reaction. React at 80°C for 2h, then heat up to 105°C for 6h. After distilling off the unreacted phosphorus oxychloride under reduced pressure, cool, filter, wash with dichloromethane, filter, and vacuum dry at 70°C to obtain white powdered pentaerythritol diphosphate diphosphoryl chloride with a yield of 84%;

[0049] (2) Add 14.85g (0.05mol) of pentaerythritol diphosphate diphosphoryl chloride and 17.79 (0.14mol) of 4,6-diamino- 2-Hydroxy-1,3,5-triazine, add 100ml N,N -Dimethylacetamide, stirred, dissolved, added 9.02g (0.20mol) dimethylamine, heated in an oil bath, reflux reaction. Slowly raise the temperature to 70°C and react for 8h. Cool, filter, wash with acetone and toluene, and vacuum-dry at 80°C to obtain a white powd...

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Abstract

The invention relates to the field of fine chemical engineering materials and specifically relates to a reactive type intumescent flame retardant for water-based polyurethane, which simultaneously contains a carbon source, an acid source, a gas source and active amino groups, and a preparation method of the reactive type intumescent flame retardant. The chemical structure of the reactive type intumescent flame retardant disclosed by the invention is as shown in formula I, the obtained flame retardant does not contain halogen, has relatively high content of phosphorus and nitrogen flame retardant components and shows an aromatic heterocyclic structure, thereby having good stability at high temperature, high char yield, significant intumescence and excellent flame retardance. Two active primary amino hydrogen ions contained in the structure can react with isocyanate to prepare flame-retardant water-based polyurethane, thereby not only effectively solving the problems of poor compatibility, easiness in migration, precipitation and permeation and the like of a traditional complex additive type flame retardant in a water-based polyurethane system, but also overcoming the defect that the physical and mechanical properties of water-based polyurethane become poor caused by the complex additive type flame retardant. When the reactive type intumescent flame retardant provided by the invention is used for preparing water-based polyurethane, the process is easy to control, the properties are easy to regulate, and prepared water-based polyurethane is widely applied to leather finishing, synthetic leather coatings, fabric coatings, building fireproof materials, coating materials, adhesives and other industries. The formula I is described in the specification.

Description

technical field [0001] The invention specifically relates to a reactive intumescent flame retardant for water-based polyurethane containing a carbon source, an acid source, a gas source and an active group amino group and a preparation method thereof, belonging to the field of fine chemicals. Background technique [0002] Intumescent Flame Retardant (IFR), with phosphorus and nitrogen as the main flame retardant components, is a new type of environmentally friendly flame retardant that integrates carbon sources, acid sources and gas sources. When this kind of flame retardant is heated, the phosphorus-nitrogen synergistic flame retardant effect in the molecule can occur, and a uniform and dense carbon foam layer is formed on the surface of the polymer, which has the functions of heat insulation, oxygen insulation, smoke suppression, and drip prevention. etc., and the generated non-combustible gas can dilute the flammable gas released when the polymer burns, and it is a new ty...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08G18/32
Inventor 范浩军章培昆田赛琦陈意何亚洲赵世玉
Owner SICHUAN UNIV
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