The method of obtaining fluorescent fluorescent pigments

 

(57) Abstract:

The invention relates to the production of fluorescent fluorescent pigments, which can be used for coloring plastics, manufacturing brightly coloured advertising polymer films. Describes how to obtain fluorescent fluorescent pigments using a mixture of phosphor and dye, high temperature processing of the reaction mixture with acid and drying, and the mixture is subjected to a mixture of urea or melamine, benzosulfimide or p-toluensulfonate, urotropine and the dye With Rhodamine or Rhodamine 6g in performe followed by the addition of the phosphor, the phosphor and the dye is used in an amount of from 1 to 3% by weight of the total mixture, the condensation of the resulting mixture with a gradual increase in temperature prior to the formation of resinous products the hot reaction mixture with a solution of oxalic acid with the addition of dinitrosopentamethylene acid to pH 6-7 and drying at 165oC. table 2.

The present invention relates to methods for fluorescent fluorescent pigments, which can be used for coloring plastics, manufacturing brightly coloured R is santich pigments, which are solid solutions of phosphors or dyes in polyester, urea -, melamine-formaldehyde and other polycondensation resins (A. C. the USSR 192328, op. 06.02.1967 in BI 5; A. S. USSR 248204, op. 10.07.1969 in BI 23; A. C. SU 1484826, op. 07.06.89. in BI 21 and so on].

Optical performance pigments (brightness, the ability to paint and etc.) strongly depend on the composition and size of the pigment particles. Reducing the size of the latter reduces the consumption of pigments for coloring. The grinding of the pigments on the basis of the condensation resin in fine powder energy-intensive, consuming time [A. S. USSR 192328, op. 06.02.1967 in BI 5], which is a disadvantage of this 10 way. This disadvantage is only partially resolved upon receipt of the pigment and the composition proposed in the invention Composition to obtain the fluorescent pigment" [A. C. SU, 1484826 A1, op. 07.06.89 in BI 21].

Closest to the proposed invention is [A. S. USSR 235890] a method of obtaining a fluorescent fluorescent pigments based on urea resin using benzene - or p-toluensulfonate, phosphor 3-methoxybenzonitrile, 1,3,5-triphenyltetrazolium and dye selected from the group of: rhodamine, rhodamine 6g, sulphonated is to work with these compounds at a certain ratio with subsequent treatment of the reaction mixture with a mineral acid to a pH of 1-3. This method allows you to obtain a pigment in the form of a homogeneous colored powder with a small remainder prosave on the sieve 0.1 (1.5-1.95). However, this method assumes that the synthesis of urea resin, and the treatment of the reaction mixture after the condensation of a sufficiently large amount of acid, which complicates the process.

The aim of the invention is to simplify the process, increasing the yield of the fine fractions of pigment by grinding and prosave, increasing the brightness of the pigment. This objective is achieved in that according to the method of obtaining fluorescent fluorescent pigments using a mixture of phosphor and dye, high temperature processing of the reaction mixture with acid and drying, characterized in that the mixture is subjected to a mixture of urea (urea or melamine, benzosulfimide or p-toluensulfonate, paraform, urotropine, dye selected from the group triarylmethane diadinoxanthin dyes: rhodamine, rhodamine 6g, followed by the addition of phosphor in the following ratio, wt.h.:

Urea or melamine - 45-55

Benzosulfimide or p-toluensulfonyl - 9-1o 3% of the total mass

the condensation of the resulting mixture with a gradual increase in temperature prior to the formation of resinous products, the hot reaction mixture with a solution of oxalic acid with the addition of dinitrosopentamethylene acid (not less than 30% of the total amount of acid, but not more than 6% of the total weight of the pigment) to pH 6-7 and drying at 165oC. the Drying is completed after the termination of the emission of volatile. Obtained after drying the semi-finished crumbles easily and frays.

The amount of dye and the phosphor is limited due to the phenomenon of "clearing" of the fluorescence characteristic of such systems.

The number dinitrosopentamethylene acid should not exceed 6% of the total mass of the obtained pigment (increase begins to decrease brightness, with a slight increase in output of fines). Drying of the product at 160-165oAllows you to complete all the condensation reaction, to remove volatile, i.e., to improve consumer quality pigments.

The use of the composition of urotropine increases the brightness of the pigment, probably due to the synthesis of resin a slightly different composition compared to the resin obtained from the components without the latter, due to clonality improve abrasion pigment in powder, probably in two moments: the evolution of a gas by decomposition and the effect on the mechanism for obtaining resin (introduction dinitrosopentamethylene acid already at the time of mixing the main components also gave the effect of improving the abrasion, i.e., it indicates the complexity of the action of the additive in the composition).

The invention is illustrated by the following examples.

Example 1

A mixture consisting of 50 g of urea, 10 g of p-toluensulfonate, 10 g of methenamine, handle 56 g Performa (formalin 40%), in which pre-dissolved dye rhodamine 6g in the amount of 1.5 g, mix, add Luminor 3-methoxybenzene in the amount of 0.35 g, is heated on a sand bath in the reaction vessel to 105oWith and condense with constant removal of water up until the temperature rises to 135oWith, then introduce a solution of oxalic acid containing 30% dinitroresorcinol acid up until the pH of the system will not be equal to 6, after which the resin is poured on the metal strip and placed for drying in a heat chamber (165oC). Drying finish after the termination of the emission of volatile. Obtained after drying the semi-finished crumbles easily and frays.

Example 2.

< / the, it is assumed that methenamine is completely decomposed to formaldehyde and ammonia

< / BR>
Example 3.

The same as in example 1, but acid treatment make only oxalic acid.

Example 4.

The same as in example 2, but acid treatment make only oxalic acid.

Example 5.

The same as in example 1, but the urea is replaced by melamine.

Example 6.

The same as in example 5, but the phosphor is fully replaced by the dye.

The properties of the pigments obtained in examples 1-6, are presented in table. 1.

The analysis of table. 1 shows that the proposed method produces pigments, not inferior in its basic characteristics (chem. resistance, heat resistance, weather resistance) prototype, while having a higher reflectance in a short time abrasion powder.

The time of grinding the pigment to the optimal size (sifting through a sieve 270 K) is reduced by 60%, while the output of the working fraction is 98%.

Thus, the proposed method allows to reduce the energy consumption for grinding, to increase the output of the labor faction, to increase the degree of grinding, which ultimately opolitan for coloring polymer films based on cellulose ethers, PVC compositions, LDPE, adding color ready industrially-produced enamels. The results are presented in table. 2.

The method of obtaining fluorescent fluorescent pigments using a mixture of phosphor and dye, high temperature processing of the reaction mixture with acid and drying, characterized in that the mixture is subjected to a mixture of urea or melamine, benzosulfimide or p-toluensulfonate, urotropine and the dye With Rhodamine or Rhodamine 6g in performe followed by the addition of phosphor in the following ratio, wt.h.:

Urea or melamine - 45-55

Benzosulfimide or p-toluensulfonyl - 9-11

Methenamine - 48-52

Paraform - 51-61

The phosphor and the dye is From 1 to 3% by weight of the total mixture

the condensation of the resulting mixture with a gradual increase in temperature prior to the formation of resinous products, the hot reaction mixture with a solution of oxalic acid with the addition of dinitrosopentamethylene acid to pH 6-7 and drying at 165oC.

 

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