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Phosphate melamine salt type nitrogen and phosphorus intumescent flame retardant as well as preparation method and application thereof

A technology of intumescent flame retardant and phosphoric acid ester, which is applied in the field of phosphoric ester melamine salt nitrogen-phosphorus intumescent flame retardant and its preparation, can solve the problems of poor compatibility and easy moisture absorption, so as to improve the flame retardant performance and reduce the The effect of simple and easy feeding process and preparation method

Pending Publication Date: 2017-05-17
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of traditional hybrid phosphorus-nitrogen series intumescent flame retardants such as poor compatibility with the matrix, and easy moisture absorption, etc. Amine-salt nitrogen-phosphorous expansion flame retardant and preparation method thereof for preparing halogen-free flame-retardant silicone rubber composite material with excellent flame-retardant properties

Method used

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  • Phosphate melamine salt type nitrogen and phosphorus intumescent flame retardant as well as preparation method and application thereof
  • Phosphate melamine salt type nitrogen and phosphorus intumescent flame retardant as well as preparation method and application thereof
  • Phosphate melamine salt type nitrogen and phosphorus intumescent flame retardant as well as preparation method and application thereof

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Effect test

Embodiment 1

[0036] Step 1: Add 25g of hexamethylolmelamine into a 500ml four-neck flask, control the temperature at -10°C, add 12.5g of phosphorus oxychloride drop by drop with a constant pressure dropping funnel, and pass nitrogen gas, and react at constant temperature for 7 hours , After the reaction, the brown-yellow viscous intermediate HTP was obtained. Step 2: Add 300ml of deionized water to 45g of the intermediate HTP, stir until the intermediate HTP is completely dissolved, add 15g of melamine, and raise the temperature to 50°C for 5 hours. Use triethylamine to adjust the pH value to neutral, cool to room temperature, filter, wash, and dry to obtain a light yellow powder, that is, phosphate melamine salt-based nitrogen-phosphorus expansion flame retardant (HTPME). The infrared spectrogram of the phosphate ester melamine salt nitrogen-phosphorous expansion flame retardant prepared in this embodiment is as follows: figure 1 shown. In the infrared spectrum of HTPME, 3555-3030cm -1...

Embodiment 2

[0038] Step 1: Add 25g of hexamethylolmelamine into a 500ml four-neck flask, control the temperature at 0°C, add 25g of phosphorus oxychloride dropwise with a constant pressure dropping funnel, and pass argon gas, and react at constant temperature for 5 hours. After the reaction, the brown-yellow viscous intermediate HTP was obtained. Step 2: Add 300ml of deionized water to 30g of the intermediate HTP, stir until the intermediate HTP is completely dissolved, add 5g of melamine, and raise the temperature to 75°C for 7 hours. Use sodium hydroxide to adjust the pH value to neutral, cool to room temperature, filter, wash, and dry to obtain a light yellow powder, that is, phosphate melamine salt nitrogen-phosphorus intumescent flame retardant. The thermal weight loss curve of the phosphate ester melamine salt nitrogen-phosphorous expansion flame retardant prepared in this embodiment is as follows figure 2 shown. At 700°C, the residual carbon content is 21.5%. The stronger the c...

Embodiment 3

[0040]Step 1: Add 25g of hexamethylolmelamine into a 500ml four-neck flask, control the temperature at 10°C, add 37.5g of phosphorus oxychloride drop by drop with a constant pressure dropping funnel, and pass helium gas, and react at constant temperature for 4 hours , After the reaction, the brown-yellow viscous intermediate HTP was obtained. Step 2: Add 400ml of deionized water to 35g of the intermediate HTP, stir until the intermediate HTP is completely dissolved, add 10g of melamine, and raise the temperature to 100°C for 5 hours. Use potassium hydroxide to adjust the PH value to neutral, cool to room temperature, filter, wash and dry to obtain a light yellow powder, that is, a phosphate melamine salt-based nitrogen-phosphorus intumescent flame retardant. The third step: according to the mass ratio of 70.5:27.5:2, methyl vinyl silicone rubber, phosphate melamine salt nitrogen phosphorus expansion flame retardant, 2,5-dimethyl-2,5-bis(tert-butyl Peroxy)hexane was kneaded in...

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Abstract

The invention discloses a phosphate melamine salt type nitrogen and phosphorus intumescent flame retardant as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) performing a reaction on hexamethylol melamine and phosphorus oxychloride in the introduction of an inert gas at minus 10 DEG C to 10 DEG C so as to generate a nitrogen and phosphorus containing intermediate HTP; and (2) dissolving the HTP and melamine into water, performing a reaction at 50-100 DEG C, adjusting the pH value to be neutral, cooling to the room temperature, filtering, washing, and drying, thereby obtaining the phosphate melamine salt type nitrogen and phosphorus intumescent flame retardant. By adopting the phosphate melamine salt type nitrogen and phosphorus intumescent flame retardant, a carbon source, an acid source and a gas source are integrated, the defects that a conventional mixed intumescent flame retardant is low in computability and liable to absorb moisture can be overcome, the tedious feeding process in application can be also alleviated, and another idea is provided for structural design of an intumescent flame retardant. In the process that a silicon rubber composite material is processed and prepared, the intumescent flame retardant is high in computability with silicon rubber, high in machining property and simple and feasible in preparation method, and an obtained composite material is high in flame retardancy.

Description

technical field [0001] The invention belongs to the field of flame retardant synthesis and application, and in particular relates to a phosphoric ester melamine salt nitrogen-phosphorous expansion flame retardant and a preparation method and application thereof. Background technique [0002] Since the commercialization of silicone rubber in the 1940s, the development of silicone rubber products has continued to progress, and various new products have emerged one after another, which has become one of the important parts of the national economy. Due to its excellent biocompatibility, chemical resistance, insulation, weather resistance, etc., silicone rubber is widely used in biology, medical treatment, transportation, food hygiene, electronic appliances and other fields. The structural main chain of silicone rubber is -Si-O-inorganic segment, which should not be easy to burn, but the side groups of the molecular main chain contain a large amount of C and H, which endows silic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/529C08L83/04C08L83/07C08L83/08C08K5/14C07F9/6584
CPCC08K5/529C07F9/6584C08K5/14C08L2201/02C08L2201/22C08L83/04
Inventor 薛锋丁勇贾志欣罗远芳贾德民
Owner SOUTH CHINA UNIV OF TECH
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