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Metal ion modified melamine polyphosphate and preparation method and application thereof

A technology for modifying melamine polyphosphate and metal ions, which is applied in non-metallic elements, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of low purity of polycondensation products, low thermal stability, long polycondensation time, etc., and achieve The reaction process is stable and controllable, the high temperature stability is good, and the flame retardant effect is excellent

Inactive Publication Date: 2017-06-13
HANGZHOU JLS FLAME RETARDANTS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Both Chinese patent application CN101014645A and Chinese patent application CN1314898A adopt phosphoric acid and melamine to prepare melamine orthophosphate, and then prepare melamine polyphosphate by high-temperature polycondensation reaction in an ammonia atmosphere. This method consumes a lot of energy and has a long polycondensation time. During the polycondensation process, it is easy to generate a large amount of phosphoric acid mist, which is easy to corrode the equipment and requires high energy consumption for the equipment.
[0008] The patent EP1789475B1 introduces metal-containing melamine polyphosphate, which first prepares metal phosphate salt, and then reacts with melamine to prepare metal melamine phosphate salt. The product has high metal ion content, reduced phosphorus content, and reduced flame retardancy
[0009] Chinese patent CN1733778A reports the use of metal ion modified melamine polyphosphate, the reaction is carried out in a solvent, and the reaction is carried out in 3 steps, the reaction steps are many, the technological process is complicated, and the purity of the polycondensation product in the later stage is not high
[0014] 3. The thermal stability is low, the initial decomposition temperature is 310°C, and the acidity is relatively high. The acid released after the decomposition of melamine polyphosphate catalyzes the degradation of nylon, which reduces the performance of the polymer.

Method used

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  • Metal ion modified melamine polyphosphate and preparation method and application thereof
  • Metal ion modified melamine polyphosphate and preparation method and application thereof
  • Metal ion modified melamine polyphosphate and preparation method and application thereof

Examples

Experimental program
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Embodiment 1

[0041] (1) According to the molar ratio of melamine to phosphorus = 0.95:1, slowly add polyphosphoric acid with a degree of polymerization n of 1.2 into melamine under stirring, heat up to 80°C and react for 10 hours to obtain white powder melamine Polyphosphate prepolymer;

[0042] (2) According to the molar ratio of the metal compound and melamine as 1:10, add the metal compound to the melamine polyphosphate prepolymer, wherein the metal oxide is aluminum hydroxide, stir evenly and heat up to 270°C, and react for 5 hours. Metal ion modified melamine polyphosphate was obtained.

Embodiment 2

[0044] (1) According to the molar ratio of melamine to phosphorus = 1.15:1, slowly add polyphosphoric acid with a degree of polymerization n of 10 into melamine under stirring, heat up to 300°C and react for 1 hour to obtain white powder melamine Polyphosphate prepolymer;

[0045] (2) According to the molar ratio of the metal compound to melamine is 1:20, add the metal compound to the melamine polyphosphate prepolymer, wherein the metal oxide is magnesium hydroxide, stir evenly and heat up to 350°C, and react for 0.5h That is, the metal ion modified melamine polyphosphate is obtained.

Embodiment 3

[0047] (1) According to the molar ratio of melamine to phosphorus = 1.12:1, slowly add polyphosphoric acid with a degree of polymerization n of 8 into melamine under stirring, heat up to 150°C and react for 6 hours to obtain melamine in the form of white powder Polyphosphate prepolymer;

[0048](2) According to the molar ratio of the metal compound to melamine is 1:12, add the metal compound to the melamine polyphosphate prepolymer, wherein the metal oxide is zinc hydroxide, stir evenly and heat up to 300°C, and react for 3 hours. Metal ion modified melamine polyphosphate was obtained.

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Abstract

The invention discloses a metal ion modified melamine polyphosphate. A molecular formula of the metal ion modified melamine polyphosphate is as shown in formula (I): (as shown in the description) (I), wherein M is metal ions, z is a valence state of metal ions M, n is an average polymerization degree of polyphosphoric acid, and n is greater than or equal to 2. The metal ion modified melamine polyphosphate is good in high-temperature stability, excellent in flame retardant effect and wide in application range. The invention also discloses a preparation method of the metal ion melamine polyphosphate. The preparation method comprises the following steps: (1) slowly adding polyphosphoric acid into melamine at a stirring state, heating to facilitate the reaction, and obtaining a melamine polyphosphate prepolymer; and (2) adding a metal compound into the melamine polyphosphate prepolymer, uniformly stirring, heating to facilitate the reaction, and obtaining the metal ion modified melamine polyphosphate. The preparation method is simple in procedures, moderate in reaction condition, stable and controllable in reaction process, low in energy consumption, small in environmental pollution, and basically free from corroding a device pipeline.

Description

technical field [0001] The invention relates to a halogen-free flame retardant, in particular to a metal ion-modified melamine polyphosphate with high thermal stability and a preparation method and application thereof. Background technique [0002] As a halogen-free flame retardant, melamine polyphosphate has the characteristics of halogen-free, low toxicity and environmental protection compared with the original halogen-containing flame retardant. [0003] Gordon L.Nelson clearly proposed in the "Fire and Polymers" page 228-231 pages published on May 9, 1990 by melamine and phosphoric acid to synthesize melamine polyphosphoric acid detailed preparation method and reaction equation. [0004] [0005] In addition, in 2003, the Polyphosphate Flame Retardantswith Increased Heat Resistance article published by Ind.Eng.Chem.Res described in detail the method that melamine polyphosphate products also adopt high-temperature polycondensation of orthophosphate to prepare melamine ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/56C08L77/06C08K9/02C08K5/3492C08K13/06C08K7/14
CPCC01B25/40C09K21/12C07D251/56C08K5/34928C08K7/14C08K9/02C08K13/06C08L2201/02C08L2201/08C08L2201/22C08L77/06
Inventor 朱峰刘君锭邵江斌
Owner HANGZHOU JLS FLAME RETARDANTS CHEM
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