The method of producing copper phthalocyanine

 

(57) Abstract:

Usage: as a chemical reagent, the pigment of the active component of the catalyst for redox reactions. The inventive product is copper phthalocyanine. Synthesis of copper phthalocyanine are under pressure to 1.5 MPa at 160 To 200C, molar ratio of reactants phthalic anhydride, the source of copper chloride one-or divalent copper, copper sulfate, urea and the catalyst (ammonium molybdate, titanium tetrachloride and boric acid), equal 1 (0,25 0,3) (2,5 3,5) (0,1 0,15), in the presence of a hydrophobic solvent mineral oil in the amount of 300 to 800 wt.h. solvent at 592 wt.h.phthalic anhydride. table 4.

The invention relates to the field of chemistry of phthalocyanines and porphyrins, namely the synthesis of copper phthalocyanine complex, used as a pigment, and catalyst of a number of redox processes, such as reduction of nitrogen oxides to nitrogen and water.

Known methods for producing copper phthalocyanine by the reaction of phthalic anhydride, phthalimide or its derivatives, urea, catalyst, source of copper in solvents of low alilovic esters benzo is some of hydroxides of alkali metals [3]

The closest in technical essence and the achieved effect is a method of producing copper phthalocyanine, namely, that 592 wt.h. phthalic anhydride; 960 wt. including urea; 105 wt.h. CuCl2or CuSO4; 80 wt. h TiCl4; 18 wt.h. 3, 4, 5, 6-tetrahydropyrimido and 4 500 wt.h. sultanol heated 5 hours at a temperature of 180-190aboutFrom and after cleaning they receive 570 wt.h. the copper phthalocyanine [4]

The main disadvantage of this method of obtaining a low degree of conversion of phthalic anhydride in phthalocyanine copper component 93,14% This is due to significant excess consumption of urea (twice) compared to stoichiometric, the process of synthesis at atmospheric pressure and temperatures thermodynamically favorable for the formation of gaseous decomposition products of urea. Specified complicates the process of purification of the target substance, leads to the ablation of parts of phthalic anhydride and its derivatives, significant amounts under these temperatures and pressures are in the vapor phase from the reaction zone.

The objective of the invention is to increase the yield of the target substance by reducing the output side of the decomposition products of urea and before thetsa by selecting optimal conditions (temperature, pressure, ratio of components, solvent) process.

It is known that the limiting stage of the target reaction is a stage of polymerization generated in the reaction sphere molecules phthalonitrile, which are then closed in the macrocycle, coordinating around a Central metal atom [B. D. Berezin. Coordination compounds of porphyrins and phthalocyanine. M. Nauka, 1978, 279 S.

4C8H4N2+M __ (C8H4N2)4M

The authors analysis of thermodynamics of phase polymerization shows that its running in the direction of polymer formation favors the increase of pressure (PL. 2) and decreasing temperature (table. 1).

Lowering the temperature and increasing the pressure also reduces thermodynamic probability of decomposition of urea in the presence of water formed in the reaction zone, to ammonia and carbon dioxide

NH2--NH O=C=N-H____ N C-O-H NH3+CO2< / BR>
which significantly reduces the removal of phthalic anhydride and intermediate compounds (in particular phthalonitrile) with gaseous decomposition products, and also provides a more pure target product. In addition, loss of phthalic anhydride and its prodvigaetsa towards formation of a liquid phase, as indicated by the increase of the evaporation temperature (table. 3).

The combination of these factors provides a more complete conversion of phthalic anhydride in the target product. However, at temperatures below 160aboutWith the rate of formation of copper phthalocyanine is small, due to the kinetics of the reaction.

The essence of the invention is the synthesis of copper phthalocyanine under pressure to 1.5 MPa at a temperature of 160-200aboutWith a molar ratio of reagents phthalic anhydride, the source of copper chloride copper (I) or (II), copper sulfate), urea, catalyst (ammonium molybdate, titanium tetrachloride, boric acid), equal 1:(0,25-0,3):(2,5-3,5):(0,1-0,15), in the presence of a hydrophobic solvent.

Comparative analysis of the proposed solutions with the prototype shows that the inventive method differs from the known fact that the process is conducted under pressure and under conditions preventing the entrainment of phthalic anhydride and its derivatives in the gas phase.

The method is implemented as follows: in the heating apparatus equipped with a stirrer, download phthalic anhydride, the source of copper ion, urea, catalyst, mineral oil and heated under pressure and continuous paramashiva the market implementation of the method in different conditions and with varying proportions of reagents are given in table. 4. As seen from the above examples, the highest yield of the product is carried out under the conditions of example 4. This method of synthesis of copper phthalocyanine implemented on a pilot unit with a capacity of 100 kg per day.

The METHOD of producing COPPER PHTHALOCYANINE, which consists in the interaction of phthalic anhydride, the source of copper ion, urea, catalyst in an inert solvent under heating, wherein the process is conducted under pressure to 1.5 MPa, a temperature of 160 200oWith a molar ratio of initial reagents phthalic anhydride source of copper ion urea catalyst, equal 1 (0,25 0,30) (2,5 3,5) (0,1 0,15), and as the solvent used mineral oil in the amount of 300 to 800 wt.h. solvent at 592 wt.h. phthalic anhydride.

 

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