The method of receiving polyhexamethylene

 

(57) Abstract:

Purpose: polihexanide as black polymer pigment for black Glubokoye enamels. The inventive method of obtaining polyhexamethylene based on polycondensation of tetranitride pyromellitic acid with p-phenylenediamine and salts of cobalt at a molar ratio of components tetranitro pyromellitic acid : p-phenylenediamine: salt of cobalt = 1: 2: 0,5, respectively, in two-stage introduction of the components into a reaction equal shares, in the environment of phenol at 160-180oC in an atmosphere of inert gas under stirring until the termination of allocation of ammonia. The coatings obtained using the new pigment, have high optical characteristics. table 1.

The invention relates to the field of technical chemistry section of polymeric materials, and more specifically to a method for producing cobalt containing crosslinked polyhexamethylene.

The invention can most effectively be used as a black polymeric pigment for black Glubokoye enamels class True absorbers with high heat, heat and corrosion resistance. The resulting coatings can byteline apparatus, in optical devices, where necessary black, not giving a glare to the details.

Famous black globorotalia enamel, in which the pigment is used carbon black (1,2)

Polymer black pigments are not described in literature.

A method of obtaining polyhexamethylene policemanila different tetranitride and diamines at elevated temperatures in a stream of inert gas (3). The color of these polymers varies from yellow to brown, and therefore they cannot be used as black pigments.

The closest to the essence of the proposed method is a method of obtaining polyhexamethylene by polycondensation of tetranitride pyromellitic acid with p-phenylenediamine in the phenol in acidic medium at 120-180oC in an atmosphere of inert gas (4).

However, the use of a polymer obtained by the method prototype, as the pigment is not possible to obtain enamel with the required optical properties: absorption and emission of solar radiation more than 0.9, and the coefficients of diffuse and specular reflection less than 2.5.

The present invention was to obtain a polymeric material which radiation solar radiation, exceeding 0.9 and coefficients of diffuse and specular reflection less than 2.5.

It turned out that the proposed method of producing crosslinked cobalt containing polyhexamethylene allows you to get structured polymer pigment with a highly developed chain pairing of the formula:

< / BR>
and fine structure (particle size of 30-60 μm). These properties determine the possibility of obtaining black Glubokoye enamels class "True sinks with high coefficients of absorption of solar radiation, diffuse and specular reflection.

The method of obtaining the proposed polyhexamethylene is that the polycondensation of tetranitride pyromellitic acid, p-phenylenediamine and cobalt salts (chloride, acetate, acetylacetonate), taken in a molar ratio of 1:2: 0.5, it is carried out under vigorous stirring in phenol at 160-180oC. in an inert atmosphere at a two-stage introduction of the components in the reaction: initially charged to the reactor phenol and half of the reacting substances (concentration of 0.15 to 0.25 mol /l) and carry out the reaction until the termination of allocation of ammonia, then add the second half of the reacting substances and continue the reaction until the termination of excretion of ammonia.

oC and maintained at this temperature until the termination of excretion of ammonia. Then the reaction mixture is make more of 8.25 g of chloride, 16 g of p-phenylenediamine, 13 g of tetranitride pyromellitic acid and continuing the reaction until the termination or sharp slowdown excretion of ammonia. Upon completion of the reaction, precipitated precipitated polymer is filtered off, washed with alcohol, extracted with alcohol in the apparatus of Soxlet within 24 hours, dried in vacuum over sulphuric acid. The weight of the polymer 50g Examples 2, 3 and 4 see table.

Using the proposed method allows to get the black polymeric pigment for thermo-, heat - and corrosion-resistant black Glubokoye enamels. Coatings based on it have high optical performance: absorption of solar radiation and the emissivity in the same area of 0.96-0.99 are equivocal when the ratio of the coefficients close to unity. The coefficients of diffuse and specular reflection 2-2,2.

The method of receiving polyhexamethylene by polycondensation of the gas, characterized in that the reaction is additionally injected salt of cobalt at a molar ratio of tetranitride pyromellitic acid, p-phenylenediamine and salts of cobalt, which is 1:2:0,5 respectively, and the process is conducted under stirring until the termination of allocation of ammonia in two-stage mode, when the initial reactant concentrations equal to 0.1 to 0.15 m/L.

 

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