Method of producing melamine cyanurate

FIELD: chemistry.

SUBSTANCE: described is an improved method of producing melamine cyanurate which is used in different compositions as a flame retardant. The method involves reaction of cyanuric acid and melamine in molar ratio of 1:1 in the presence of 2-30% water of the weight of dry reactants at temperature ranging from 10 to 100°C in countercurrent air streams at pressure of 2-10 kgf/cm2. The method can be realised continuously.

EFFECT: end product is obtained with high output with low power consumption.

1 cl, 5 ex

 

The invention relates to organic chemistry, in particular to an improved method of obtaining cyanurate melamine, which is used in various compositions as a flame retardant.

A method of obtaining cyanurate melamine (CM) interaction of melamine (M) and cyanuric acid (CC) when the mixing ratio from 1:9 to 9:1 (wt.) in the aquatic environment (from 20 to 2000 wt.% to the weight of the whole mixture) in a cylindrical two-bladed mixer at 0-250°C for from 5 minutes to 5 hours (patent JP 54055587, publ. 02.05.1979). The disadvantages of this method are the difficulties in the selection of the target product, associated with the necessity of filtering, drying, grinding CM.

A method of obtaining cyanurate melamine, comprising heating the dry powder mixture M and the Central Committee at 250-500°C in the absence of a liquid medium (patent US 5493023, publ. 20.02.1996). The ratio of M and CC is from 1:0.5 to 1:2,0 (in moles), preferably from 1:0.9 to 1:1.1 to. The process should preferably be conducted in an inert gas, for example, N2. Pre-mixing the components at room temperature. Practically, this method is carried out by the interaction of the components in the melt. Due to the difference of temperature sublimation M and CC process is accompanied by loss of reagents. In addition, you need expensive equipment (autoclave), and the process is accompanied by large energy consumption, tie nymi with the need to maintain a high temperature for a long time (several hours).

Closest to the claimed invention is a process involving the interaction of melamine and cyanuric acid at a ratio of M:CC=1:1 (mol) followed by heating, degassing the mixture (water content ranges from 50 to 500 wt.%). For ease of use mixing finely ground to a size of diameter of particles ≤100 µm source components (patent JP 55147266, publ. 17.11.1980).

The selection of the target product is carried out by distillation, water vacuum, followed by drying. The disadvantage of this method is a multistage process requiring high energy consumption associated with the need for fine grinding of initial products and vacuum. Drying of the product, except energy (hot air), accompanied by large losses of the target product, which is carried away by the air stream into the atmosphere, causing environmental pollution and requires bulky and expensive treatment facilities.

The objective of the proposed technical solution is the creation of a method of obtaining the desired products in high yield, without much water and energy consumption, which can be carried out continuously.

The problem is solved in that a method of obtaining cyanurate melamine, which is that the mixture consisting of melamine, cyanuric acid in aspect] is to mol per mole (1:1), water, comprising 2-30% by weight of dry reagents, served in the reaction zone in counter-flow air pressure of 2-10 kgf/cm2at a temperature of from 10°C. to 100°C.

Failure to comply with conditions of the method reduces the quality and yield of the target product, increase energy costs.

The use of the proposed technical solutions were able to achieve a high percentage of the yield of the target product, reducing energy costs by reducing the number of used process water, exceptions stages of drying, grinding, prosea. Another advantage of the proposed method is the possibility of its implementation in a continuous mode.

To obtain a product with different dispersion and prevent it from sticking and agglomeration in the process in a continuous mode in the initial mixture of reactants is added antistatic agent with a half-life leakage of electrostatic charges ≤10. As the antistatic agent may be used surfactants in the form of 2-5%solutions or emulsions, alcohols, for example methanol or ethanol in an amount of 0.1-5% of the amount of water that is introduced into the material during processing, or their mixture. In addition, some of the devices and filters place the device for periodic shaking.

Things is the outer coat of the present invention is illustrated by the following examples.

Example 1.

The reaction mixture (in kg) of 1.9 melamine, 1,93 cyanuric acid ratio mol per mol and 0,97 water (25% by weight of dry reagents) for 40 seconds served in the reaction zone of 80 cm3in opposing streams of air with a pressure of 2 MPa (kgf/cm2), a temperature of 100°C and a bulk velocity of 150 nm3/h each.

At the outlet of the reaction zone receive cyanurate melamine in the amount of 3.84 kg with a basic substance content of about 96%, moisture 0.3% and with a particle size of 75-130 mm. The residence time of the reactants in the reaction zone ~0,001 sec.

Example 2.

The reaction mixture (in kg) of 2.5 melamine, 2,6 cyanuric acid and 0.8 water (16% by weight of dry products), within 45 sec served in the reaction zone of 80 cm3in opposing streams of air with a pressure of 6 MPa (kgf/cm2), a temperature of 55°C and a bulk velocity of 225 nm3/h each.

Get cyanurate melamine in the amount of 5,12 kg with a basic substance content of about 95%, moisture 0.4% and with a particle size of 50-100 μm. The residence time of the reactants in the reaction zone ~of 0.0005 s.

Example 3.

The reaction mixture (in kg) of 1.26 melamine, 1,3 cyanuric acid and 0.05 water (2% by weight of dry reagents)for 20 sec served in the reaction zone of 80 cm3as in examples 1 and 2, at a pressure of 10 MPa (kgf/cm2),10°C and a bulk velocity of 300 nm 3/h each.

Get to 2.57 kg cyanurate melamine with a basic substance content of about 95%, moisture 0.45% and with a particle size of 20-50 microns. The residence time of the reactants in the reaction zone ~of 0.0005 s.

Example 4.

The reaction mixture, consisting of 1.9 kg of melamine, 1,93 kg cyanuric acid and 1.16 kilograms of water (30% by weight of dry reagents), for 40 sec served in the reaction zone of 80 cm3in opposing streams of air with a pressure of 2 MPa (kgf/cm2), a temperature of 100°C and a bulk velocity of 150 nm3/h each.

At the outlet of the reaction zone receive cyanurate melamine in the amount 3,81 kg with a basic substance content of about 95% and moisture of 0.5%. The particle size of 75-130 mm. The residence time of the reactants in the reaction zone ~0,001 sec.

Example 5.

Melamine and cyanuric acid in a molar ratio, and water in an amount of 5% by weight of dry reactants are continuously fed into the mixer at a temperature of 20°C and then into the reaction zone of 80 cm3in opposing streams of air with a pressure of 10 ATM and a bulk velocity of 200 nm3/h each.

At the outlet of the reaction zone, the product passing through the system pylenakoplenie, enters into the drive and then then is loaded into big bags or bags. Get cyanurate melamine with a basic substance content of about 95%, moisture of 0.45% and a particle size of 20-50 microns.

The way the floor is placed cyanurate melamine, including the interaction between cyanuric acid and melamine in a molar ratio of 1:1 in the presence of water, wherein the water content is 2-30% by weight of dry reagents, the mixture of reagents is introduced into the reaction zone at a temperature of from 10 to 100°C in opposing streams of air 2-10 kgf/cm2.



 

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9 cl, 4 ex, 3 tbl

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23 cl, 1 dwg, 7 tbl, 14 ex

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