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Method for synthesizing melamine cyanurate salt

A technology of melamine cyanurate salt and melamine, which is applied in organic chemistry and other fields, and can solve the problems of fine particle size of the product, large amount of water consumption, and high cost of raw materials

Active Publication Date: 2010-07-28
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of using the liquid phase method to synthesize MCA are mainly that the water consumption is large, and the particle size of the product is finer, and the filtration efficiency is poor, which affects the improvement of the productivity of the whole process, and the high price of cyanuric acid is used as the raw material to synthesize MCA, and the raw material cost is relatively high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] First weigh 48 grams of urea, 28.56 grams of melamine, dispersant NH 4 NO 3 6 grams, put into a mixer and mix uniformly to obtain a mixture. Preheat a 1000mL four-neck bottle equipped with an electric heating mantle, agitator, thermometer, condenser, and ammonia gas absorption system to 270°C, add the above-mentioned mixed mixture, start the agitator, and then inject nitrogen gas to take away the generated ammonia Start the above-mentioned ammonia gas absorption system for recovery; when the temperature reaches 200°C, the material becomes viscous, and when the temperature continues to rise to 270°C, the material solidifies and becomes a white powdery intermediate product, and the reaction is maintained for 1 hour since feeding. Then the intermediate product was cooled to below 100°C (≤100°C, the same below), 456 grams of water was added, the temperature was raised to 100°C, and the reaction was maintained at this temperature for 10 hours. Then filter while it is still...

Embodiment 2

[0016] First weigh 48 grams of urea, 30.24 grams of melamine, and 6 grams of dispersant ammonium chloride, put them into a mixer and mix them uniformly to obtain a mixture. Heat a 1000mL four-neck flask equipped with an electric heating mantle, stirrer, thermometer, condenser, and ammonia gas absorption system to 280°C, add the above mixture, start the stirrer, feed nitrogen to take away the generated ammonia gas, and start the The above-mentioned ammonia gas absorption system is recovered. When the temperature reaches 200°C, it becomes viscous, and when the temperature continues to rise to 280°C, the material solidifies and becomes a white powdery intermediate product. After the reaction is maintained for 1 hour, the intermediate product is cooled to below 100°C, and 456 grams of water are added. , then warming up to 100°C, keeping the reaction at this temperature for 10 hours, filtering while hot, washing with 800 grams of boiling water until neutral, and drying the filter c...

Embodiment 3

[0018] First weigh 48 grams of urea, 28.56 grams of melamine, and 6 grams of dispersant ammonium chloride, put them into a mixer and mix them evenly to obtain a mixture. Preheat a 1000mL four-necked bottle equipped with an electric heating mantle, agitator, thermometer, condenser, and ammonia gas recovery system to 290°C, add the above-mentioned mixed mixture, start the agitator, and then inject chlorine gas to take away the generated ammonia Start the above-mentioned ammonia gas absorption system for absorption; when the temperature reaches 200°C, the material becomes viscous, and when the temperature continues to rise to 290°C, the material solidifies and becomes a white powdery intermediate product, which remains for 1 hour after feeding. , lower the temperature of the intermediate product below 100°C (≤100°C, the same below), add 514 grams of water, then raise the temperature to 100°C, and keep the reaction at this temperature for 10 hours. Then filter while hot, wash with...

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Abstract

The process of synthesizing melamine cyanurate includes the following steps: mixing urea, melamine and ammonium salt as dispersant in certain proportion to obtain mixture; pre-heating the reactor to 270-295 deg.c, starting the stirrer, leading nitrogen to the reactor, adding the mixture to the reactor, heating the material to 270-290 deg.c, and reacting for 60-70 min to obtain white powdered intermediate product; adding water in 14-18 times the weight of melamine to the intermediate product, heating to 100 deg.c, reacting for 10 hr, hot filtering, washing the filter cake with boiled water, stoving, and crushing to obtain melamine cyanurate product. The melamine cyanurate product of the process has purity of 99.5 % and yield up to 95.5 %, and is applied as fire retardant.

Description

technical field [0001] The invention relates to a method for synthesizing an environment-friendly nitrogen-based flame retardant melamine cyanurate. Background technique [0002] In recent years, as people's awareness of protecting ecology and the environment has increased, products marked with green have emerged as the times require, challenging traditional flame retardant materials, especially halogen flame retardants represented by polybrominated diphenyl ethers , has been severely challenged due to toxicity and corrosion issues. According to relevant literature records, a large number of applied research shows that both halogen and phosphorus will produce harmful substances in the combustion process. It is reported that melamine cyanurate (MCA hereinafter the same) is by far the most representative green flame retardant. MCA is a nitrogen-based flame retardant, white crystal, and greasy powder, odorless, non-toxic, specific gravity 1.5-1.6, insoluble in water and other...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/56C07D251/32
Inventor 刘福安姜丹蕾李耀先张宏宇吕日红韩铁良石占崇刘长青于洪涛王艳
Owner BC P INC CHINA NAT PETROLEUM CORP