A kind of branched phosphorus-nitrogen flame retardant and preparation method thereof

A flame retardant and branched phosphorus technology, which is applied in the field of new branched phosphorus-nitrogen flame retardants and their preparation, can solve the problems of deterioration of mechanical properties of polymer matrix materials, poor compatibility of polymer materials, poor water resistance, etc. , achieve excellent flame retardant effect, good thermal stability, and reduce production cost

Active Publication Date: 2018-03-02
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional intumescent flame retardants have disadvantages such as poor water resistance, poor durability, poor compatibility with polymer materials, and easy migration, which eventually lead to deterioration of the mechanical properties of polymer matrix materials.

Method used

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  • A kind of branched phosphorus-nitrogen flame retardant and preparation method thereof
  • A kind of branched phosphorus-nitrogen flame retardant and preparation method thereof
  • A kind of branched phosphorus-nitrogen flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The branched phosphorus-nitrogen type flame retardant in this embodiment is based on three (2-hydroxyethyl) isocyanurate and phosphorus oxydichloride raw materials, and the branched phosphorus-nitrogen type flame retardant is obtained under the action of a catalyst and an acid-binding agent. flame retardant. Wherein, the phosphoryl dichloride is selected from phenoxy phosphoryl dichloride, the solvent is selected from pyridine, the catalyst is selected from 4-dimethylaminopyridine, and the acid-binding agent is selected from triethylamine.

[0035] a. Dissolve 6.3294g (0.03mol) of phosphoryl dichloride in 128.9215mL (126.5880g) of pyridine to obtain a phosphoryl dichloride solution, then add 6.2627g of triethylamine and 0.1848g of 4-dimethylaminopyridine; g (0.02mol) three (2-hydroxyethyl) isocyanurate was dissolved in 106.8296mL (104.8960g) pyridine to obtain three (2-hydroxyethyl) isocyanurate solution;

[0036] b. Add phosphorus oxydichloride solution to a three-nec...

Embodiment 2

[0042] The difference between this example and Example 1 is that the acid-binding agent is changed from triethylamine to pyridine.

[0043]a. Dissolve 6.3294g (0.03mol) of phosphoryl dichloride in 128.9215mL (126.5880g) of pyridine to obtain a phosphoryl dichloride solution, then add 0.1848g of 4-dimethylaminopyridine; dissolve 5.2448g (0.02mol) of tri (2-hydroxyethyl) isocyanurate was dissolved in 106.8296mL (104.8960g) pyridine to obtain three (2-hydroxyethyl)isocyanurate solution;

[0044] b. Add phosphorus oxychloride solution to the three-necked flask equipped with a stirrer, constant pressure dropping funnel and reflux condenser at -10-0°C, and add tris(2- Hydroxyethyl) isocyanurate solution, the time of dropping is 1.5h, and the insulation reaction is 0.5 hours after the dropping;

[0045] c. Raise the temperature to 40°C, keep it warm for 12 hours, and place it in an ice-water bath at 0°C to end the reaction;

[0046] d. Suction filtration, washing, and drying of the...

Embodiment 3

[0049] The difference between this example and Example 1 is that the molar mass ratio of tris(2-hydroxyethyl)isocyanurate and phosphoryl dichloride is changed from the original 1:1.5 to 1:1.

[0050] a. Dissolve 4.2196g (0.02mol) of phosphoryl dichloride in 85.9477mL (84.3920g) of pyridine to obtain a phosphoryl dichloride solution, then add 4.1751g of triethylamine and 0.1848g of 4-dimethylaminopyridine; Dissolve g (0.02mol) tris (2-hydroxyethyl) isocyanurate in 106.8296mL (104.8960g) pyridine to obtain tris (2-hydroxyethyl) isocyanurate solution, then add;

[0051] b. Add phosphorus oxydichloride solution to a three-necked flask equipped with a stirrer, a constant pressure dropping funnel and a reflux condenser at 0°C, and add tris(2-hydroxyethyl) dropwise to the three-necked flask by starvation drop method ) isocyanurate solution, dropwise for 1h, and keep warm for 1 hour after the dropwise addition;

[0052] c. Raise the temperature to 40°C, keep it warm for 12 hours, and...

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Abstract

The invention discloses a branched phosphorus-nitrogen flame retardant and a preparation method thereof, and relates to the field of flame retardants and their synthesis. The branched phosphorus-nitrogen flame retardant has a branched structure, which makes it have good dispersibility in the polymer; it contains more triazine ring and benzene ring structure, and has good thermal stability and carbon formation. The novel branched phosphorus-nitrogen flame retardant prepared by the invention takes tris(2-hydroxyethyl) isocyanurate and phosphorus oxychloride as main raw materials, adopts the starvation dropwise addition method, and mixes tris(2-hydroxyethyl) Ethyl) isocyanurate solution is dropped into phosphorus oxychloride solution containing acid binding agent and catalyst to obtain branched phosphorus-nitrogen flame retardant. The branched phosphorus-nitrogen flame retardant prepared by the invention has continuous reaction process, simple process, low reaction cost and broad application prospect.

Description

technical field [0001] The invention relates to the field of flame retardants and their synthesis, in particular to a novel branched phosphorus-nitrogen type flame retardant and a preparation method thereof. Background technique [0002] Flame retardant is an additive that can make polymers and related materials not easy to catch fire or slow down the burning speed. Generally, flame retardants can be divided into halogen-containing flame retardants and halogen-free flame retardants, among which halogen-containing flame retardants will produce a large amount of toxic smoke and corrosive gases during combustion, causing serious pollution to the environment People's lives and property pose a huge threat. In view of the serious disadvantages of halogen-containing flame retardants, halogen-free flame retardants have become one of the important development directions of flame retardants in the future. [0003] Among the halogen-free flame-retardant polymer materials, the intumes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/04
Inventor 李锦春许亮宋艳张鑫
Owner CHANGZHOU UNIV
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