Method for preparing melamine adduct with acid

FIELD: chemistry of polymers, chemical technology.

SUBSTANCE: invention relates to the improved method for synthesis of melamine adducts with acids of the order: cyanuric, phosphoric, boric acid in the presence of liquid medium that are modifying agents of polymers. Method involves homogenization of melamine and acid powders in a mixer at temperature from 20°C to 80°C and then prepared mixture is subjected for effect by deformation shift at temperature from 20°C to 150°C at the shift rate value 5-400 s-1 and the total deformation shift value from 1.5 x 103 to 2.0 x 105%. The ratio of melamine to acid is from 2:1 to 1:2 preferably. Effect by the deformation shift is carried out in mechanical reactor of auger type. Invention provides simplifying process in synthesis of end substances, significant decreasing consumptions and avoiding pollution of environment.

EFFECT: improved method of synthesis.

2 cl, 10 ex

 

The invention relates to synthetic organic chemistry, and in particular to methods of obtaining derivatives of melamine in the form of adducts with various acids, which can find application in the chemical industry for the production of active fillers or modifiers of polymers to improve operational properties of the latter, such as temperature resistance, fire resistance and other

The number of known methods for obtaining derivatives of melamine by the interaction of initial products in the aquatic environment. For example, a method of obtaining cyanurate melamine (adduct of melamine with cyanuric acid), comprising mixing and grinding of melamine [M] with 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 [Japan patent, JP 54055587, publ. 2.05.1979 g; European patent EP 1438353, publ. 21.07.2004]. The disadvantages of this method are the difficulties in the selection of the target product, associated with the need for filtration, especially in the case of using a small amount of water. Increase the amount of water facilitates the filtering process, however, this leads to an increase in the volume of the reaction system and industrial premises, as well as water consumption. To overcome the giving difficulties in filtering is achieved according to another method, including interaction finely ground source components to the size of the particle diameter of ≤100 μm, with a ratio of M to CC=1:1 (mol), followed by heating, degassing the mixture (water content 50-500% weight.) [the Japan patent JP 55147266, publ. 17.11.1980,]. The selection of the target product is carried out by distillation, water vacuum, followed by drying. The disadvantages of the method is a multistage process requiring high energy consumption associated with the need for fine grinding of the starting materials and the 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, which leads to poisoning of the environment or require the installation of bulky and expensive structures.

A known method of producing melamine pyrophosphate (adduct of melamine with pyrophosphoric acid), which includes stages:

a) interaction of a solution of salts of alkaline metal (Na, K) phosphoric acid with ion exchange resin acid type 0°C;

b) the resulting condensation product (pyrophosphoryl acid) are added to a suspension of M at 0°to obtain the desired adduct [U.S. patent 6268494, publ. 31.07.2001,]. The process of interaction between the components occurs by passing first of 2.5% (wt.) an aqueous solution (dionysiou the Naya water) Terentieva pyrophosphate through a column of ion exchange resin, and then pyrophosphoryl acid (PC) is subjected to interaction with mg of the Target product are filtering, washing with deionized water and drying at 100°C. the Yield of melamine pyrophosphate is 94±1%.

The disadvantage of this method is a multi-stage process, the need for bulky equipment and deionized water.

A known method of producing melamine borate (adduct of melamine with boric acid) [U.S. patent, US 5854155, publ. 29.12.1998,]. The interaction of the initial components is carried out in the presence of caso3in the mixer for 6 hours at 90°and in the atmosphere flow 90% humidity at constant temperature control system. The ratio of initial components: boric acid (Bq) to M is approximately 2:1 (in moles).

The disadvantages of this method are the complexity and the multi-stage process. The yield of the target product is not specified.

Closest to the claimed invention is a method of obtaining cyanurate of melamine adduct M CC), comprising heating the dry powder mixture M and the Central Committee at 250-500°in the absence of any liquid medium, and the sizes of the particles M, and the Committee shall each not exceed 20 μm [US patent, US 5493023, publ. 20.02.1996]. The ratio of M to the CC is from 1:0.5 to 1:2,0 (in moles), preferably from 1:0.9 to 1:1.1 to. The process W is lateline to carry out in an inert gas environment, as, for example, N2. Pre-mixing the components at room temperature. Essentially this method is carried out by interaction of the components in the melt (melting point M is 250°and the temperature at which sublimation - 210°C, the melting point of the Central Committee is 360°and the temperature at which sublimation - 230°)). In this regard, the process is accompanied by the loss of reagent due to sublimation. In addition, you need expensive equipment (autoclave), the process is accompanied by large energy costs associated with the need to maintain high temperature in the continuation of a large period of time (up to several hours).

The objective of the invention is to provide a method that allows to obtain adducts M with different acids in single process mode. Furthermore, the method could be implemented without much water and energy to obtain the target product with great output and would be environmentally friendly, would not require phase separation or recovery of the final product.

The problem is solved in that a versatile way to obtain various adducts M with acids: cyanuric or pyrophosphoric, or boron in the absence of a liquid medium. How is that powdered M and acid pre-d is genesereth in the mixer at a temperature of from 20° up to 80°S, then the resulting homogeneous mixture is exposed to shear at a temperature of from 20 to 150°s at shear rate 5-400 with-1and total shear strain 1.5·103to 2.0·105%. The ratio of M to acid (molar) is mainly from 2:1 to 1:2. In the case of use as acid cyanuric get adduct M with any of the tautomeric forms of the acid, or a mixture thereof. In the case of use as acid pyrophosphoric or boric get adduct M with the corresponding acid. All adducts are obtained in powder form. The duration of the effect of shear deformation is mainly from 3 to 30 minutes. The effect of shear deformation can be performed on mechanochemical reactor screw type.

The solution of this problem was made possible thanks to the fact that the process of interaction of initial reagents is carried out in contrast to the known methods in the solution, and not in the melt, and by the interaction of initial products in solid powdered state under the action of shearing strain.

The magnitude of the shear strain was determined by the known method [A.S., SU 1423657, publ. in 1988], based on the following parameters:

γ shear deformation;

ω - the speed of rotation of the screw mixer (100 rpm or 628 rad/min);/p>

Q - the performance of the device (0.14 kg/min);

L is the length of the shear zone (6×10-2m).

Ri- radius of the inner shell of the mixer (27,5·10-3m);

ρ - density polymer, kg/m3(930 kg/m3);

S is a sectional area of the working zone (0,4·10-3m2);

R0- the average radius of the cross section of the grinding element (26,0·103m).

The content of the obtained adducts was determined by the intensity of the corresponding characteristic bands in the IR spectra of the reaction products.

The structure of the obtained adducts have been proven coincidence DTA curves and temperatures at the beginning of sublimation for adduct M from the Central Committee and cyanurate melamine accordingly, the presence of x-ray scattering curves of the adduct M PC crystalline reflections at the corners 20: 8,25°, 18,0° and 27.5°characteristic of melamine pyrophosphate, as well as the presence in the IR spectra of the obtained adducts bands, characteristic for cyanurate melamine, melamine pyrophosphate and melamine borate, respectively.

The invention can be illustrated by the following examples.

Example 1. 252 g of powdered M mixed with 258 g of powder of the Central Committee (molar ratio 1:1) in a paddle mixer periodic operation at 40°C. Further obtained from the ect is exposed to shear strain in mechanochemical reactor screw type at 80° With the average shear rate 60-1to the total shear strain, 5.0×104% within 10 minutes. The yield of adduct M CC 95 wt.%, purity adduct 97%. The content of the adduct M CC was determined by the intensity of the characteristic band at 1090 cm-1the IR spectrum of the reaction product. A certain method DTA the temperature at which sublimation of the resulting adduct is 295°S, which is typical for cyanurate melamine.

Example 2. Performed analogously to example 1, but in contrast, the temperature in the mixer 20°and in mechanochemical reactor 120°C. Exit 98 wt.%, purity adduct 99%.

Example 3. Performed analogously to example 1, but in contrast, the temperature in the mixer 80°and in mechanochemical reactor 150°C. Output 94 wt.%, purity adduct 95%.

Example 4. Performed as in example 2, but in contrast, the average shear rate is equal to 5-1that the total shear strain is 1.5×103%and the duration of exposure 30 minutes. Yield 60%, purity adduct 65%.

Example 5. Performed as in example 2, but in contrast, the average speed of the shift is equal to 400-1the overall amount of shear strain - 2,0×105%and the duration of exposure of 3 minutes. Exit 98%, purity adduct of 98.5%.

Example 6. 252 g of powdered M mixed with 178 g of powdery the PC (molar ratio 2:1) in a paddle mixer periodic operation at 20° C. Next, the resulting mixture is subjected to the effects of shear deformation mechanochemical reactor screw type at 20°C, average shear rate 5 s-1to the total shear strain, equal to 1.5×103% within 30 minutes. The yield of adduct M PC 75 wt.%, purity adduct 80%. The content of the adduct M PC was determined by the intensity of the characteristic bands 1690 cm-1and 1720 cm-1the IR spectrum of the reaction product.

Example 7. Performed analogously to example 6, but in contrast, the average speed of the shift is equal to 400-1the overall amount of shear strain - 2,0×105%and the duration of exposure of 3 minutes. The output 96%, purity adduct 97%.

Example 8. 252 g of powdered M mixed with 124 g of powdered Bq (molar ratio 1:2) in a paddle mixer periodic operation at 20°C. Next, the resulting mixture is exposed to shear deformation in mechanochemical reactor screw type at 20°C, average shear rate 5 s-1to the total shear strain, equal to 1.5×103% within 30 minutes. The yield of adduct M Bq 60 wt.%, purity adduct 65%. The content of the adduct M Bq was determined by the intensity of the characteristic bands 3395 cm-1the IR spectrum of the reaction product.

Example 9. Performed analogously to example 8, but in contrast, the average speed with the vig is 400 -1the overall amount of shear strain - 2,0×105%and the duration of exposure of 3 minutes. Yield 97%, purity adduct 98%.

Example 10. Performed analogously to example 9, but in contrast, the temperature in the mixer 80°and in mechanochemical reactor 150°C. the Yield 92%, purity adduct 95%.

As seen from the above examples, the claimed method allows to obtain adducts of melamine with various acids in single process mode. Furthermore, the method is carried out without large water and energy consumption to obtain the target product with a large output and thus is environmentally friendly, requires no phase separation or recovery of the final product.

1. The method of obtaining adduct of melamine with an acid selected from the range: cyanuric, provostry, boric in the absence of a liquid medium, which consists in the fact that powdered melamine and acid pre-homogenized in the mixer at a temperature of from 20 to 80°S, then the resulting homogeneous mixture is exposed to shear at a temperature of from 20 to 150°s at shear rate 5-400 with-1and total shear strain 1.5·103to 2.0·105%.

2. The method according to claim 1, characterized in that the molar ratio of melamine to acid is 2:1÷1:2.

3. The method according to claim 2, characterized in that as to the slots use cyanuric acid with getting adduct of melamine with any of the tautomeric forms of the acid, or mixtures thereof.

4. The method according to claim 2, characterized in that the acid used pyrophosphoryl acid with getting adduct of melamine with pyrophosphoric acid.

5. The method according to claim 2, characterized in that the acid used boric acid to obtain adduct of melamine with boric acid.

6. The method according to any one of claims 1 to 5, characterized in that the duration of the effect of shear deformation is mainly from 3 to 30 minutes

7. The method according to any one of claims 1 to 5, characterized in that the effect of shear deformation is carried out on mechanochemical reactor screw type.



 

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