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New process for preparing modified melamine polyphosphate

A melamine polyphosphate, melamine technology, applied in the direction of organic chemistry, can solve the problems of plastic products harm, weight loss, difficult to control MPOP and other problems

Active Publication Date: 2011-07-20
ZHEJIANG RES INST OF CHEM IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) Synthesis of melamine and polyphosphoric acid, this process requires methanol as a solvent, the production workshop needs explosion-proof design, and the investment in infrastructure is large;
[0006] (2) Synthesis of melamine and sodium polyphosphate, this process needs to add hydrochloric acid, the product contains a large amount of sodium chloride, needs to be washed with water, produces a large amount of industrial wastewater, and is not cleaned thoroughly, and the chloride ions in it will bring harm to plastic products;
[0007] (3) Using phosphorus pentoxide and diammonium hydrogen phosphate (or ammonium dihydrogen phosphate) as raw materials to catalyze the synthesis of MPOP, the synthesis time of this process is relatively long, requiring more than 10 hours, and the synthetic product loses a lot of weight at around 300°C;
[0008] (4) Use melamine, phosphorus pentoxide and oxalic acid as raw materials to synthesize MPOP. Due to the use of phosphorus pentoxide as a raw material, the process reacts violently and emits toxic CO gas, which is difficult to control to obtain qualified MPOP
The initial decomposition temperature of melamine polyphosphate prepared by this method is about 340-350°C, and the reaction polymerization time is longer, which takes 8-12 hours

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 3000ml reactor equipped with a stirrer and a thermometer, first add 1467g of water, then add 228g of 85% phosphoric acid, and 35g of crystalline type II ammonium polyphosphate (APP-II, degree of polymerization n>1000), heat up to 70 ℃, then slowly add melamine 294g, continue to heat up to about 95 ℃ and react for 2 hours. Cool to about 40°C or room temperature in an air or water bath, and then perform solid-liquid separation. The filter cake was dried at 130°C for 8 hours to obtain the product. Take 100 g of the product, then polymerize at 330° C. for 90 minutes, then cool the reaction product at room temperature, and pulverize to obtain a modified melamine polyphosphate, which appears as a white powder. The performance data are shown in Table 1.

Embodiment 2

[0029] In a 3000ml reactor equipped with a stirrer and a thermometer, first add 1467g of water, then add 228g of 85% phosphoric acid, and 17.5g of crystalline type II ammonium polyphosphate (APP-JI, polymerization degree n>1000), slowly add Melamine 300g, then continue to heat up to 95 ℃ and react for 4 hours. After cooling to 30°C at room temperature, solid-liquid separation was performed. The filter cake was dried at 130°C for 6 hours to obtain the product. 100 g of the product was polymerized at 350° C. for 70 minutes, and then the reaction product was cooled at room temperature and pulverized to obtain a modified melamine polyphosphate, which appeared as a white powder. The performance data are shown in Table 1.

Embodiment 3

[0031] In a 3000ml reactor equipped with a stirrer and a thermometer, first add 1467g of water, then add 228g of 85% phosphoric acid, and 26.3g of crystalline type II ammonium polyphosphate (APP-II, polymerization degree n>1000), slowly add 300g of melamine, then continue to heat up to about 98°C and react for 3 hours. Cool to 40° C. at room temperature, and then perform solid-liquid separation. The filter cake was dried at 130°C for 6 hours to obtain the product. 100 g of the product was polymerized at 450° C. for 20 minutes, and then the reaction product was cooled at room temperature and pulverized to obtain a modified melamine polyphosphate, which appeared as a white powder. The performance data are shown in Table 1.

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PUM

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Abstract

The invention discloses a new process for preparing modified melamine polyphosphate, which comprises the following steps: (1) adding water, phosphoric acid and a modifier into a reaction kettle, and heating to 20-70 DEG C; (2) adding melamine, heating to 90-100 DEG C, and reacting for 2-5 hours; (3) cooling the product obtained after the reaction in the step (2), filtering, and drying; and (4) carrying out polymerization reaction on the product, which is subjected to the step (3), at 300-450 DEG C for 10-120 minutes. The synthesis and modification of the melamine polyphosphate are carried out synchronously, so that the invention has the advantages of short reaction time, low requirements for raw materials, simple and convenient technical operation, and low environmental pollution; the prepared melamine polyphosphate has the advantages of favorable compatibility with resin, low solubility in water, and excellent thermal stability, and the temperature can reach about 360 DEG C when the weight loss is 2%, so that the modified melamine polyphosphate can satisfy the processing requirements of no halogen and flame retardancy for glass fiber reinforced nylon and polyester.

Description

technical field [0001] The invention relates to a high thermal stability halogen-free flame retardant and a preparation process thereof, in particular to a new preparation process of an environment-friendly phosphorus-nitrogen series flame retardant. Background technique [0002] Melamine polyphosphate, the English name is melamine polyphosphate, referred to as MPOP, which has excellent heat resistance (decomposition temperature above 300°C) and high temperature water resistance. It is widely used as a halogen-free and environmentally friendly flame retardant, and can be used in almost all plastics. , including thermoplastics and thermosetting plastics, especially suitable for engineering plastics processed at higher temperatures, such as glass fiber reinforced nylon, polyester (PBT, PET) and other polymer materials for halogen-free flame retardant, used as additive flame retardant agent. [0003] Compared with the bromine-containing flame retardants currently used in large...

Claims

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Application Information

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IPC IPC(8): C08G79/04C07D251/00C08L85/02C08K5/3492
Inventor 毛树标陆凤英戴稼盛黄新艳吴纪虎郑冬芳杨箭
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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