Dye to polymers adding method

FIELD: production of painted optically transparent polymeric films used in microelectronics, quantum electronics and opto-electronics.

SUBSTANCE: method for adding dye to polymers comprises steps of drawing polymer in adsorption-active liquid medium containing dissolved dye; further drying of polymer and annealing it; using as polymer non-oriented polymeric film of amorphous polymer; annealing polymer in temperature range beginning from temperature of polymer vitrifying till temperature of chemical decomposition of polymer with dye. Polymer is dried and annealed without holding it in tensioned state in direction of drawing.

EFFECT: possibility of realizing simplified process for producing optically transparent painted polymeric films.

4 ex

 

The invention relates to the field of injection of the dye in the polymer required to obtain colored optically transparent polymer films (Dps), which can be used in microelectronics (OLEDs), quantum electronics (microlasers), optoelectronics (recording systems and long term data storage) obtain the microfiche, mapping, etc.

There is a method of injecting dye into the polymer by dissolving the polymer and dye in a common solvent and then applying the resulting solution on a flat surface and evaporation of the solvent [W. Brutting, S. Berleb, Muckt A.G. // Organic electronics 2, 2001, 1-36].

The disadvantage of this way to obtain a film containing the dye, is its high complexity and low-tech, and often observed phase separation in the system, resulting in release of low-molecular component in a separate phase with subsequent aggregation into particles of larger size. The consequence is a sharp deterioration in the optical and other performance properties of the obtained polymer film containing the dye.

There is a method of injecting dye into the polymer by treating the polymer fibers with dye solution [Melnikov B.N. Dyeing fibers // the encyclopedia of polymers. T.I. S. Soviet encyclopedia. Mosk is and. 1972]. The disadvantages of this method is its low speed, because it is based on spontaneously-reaching processes of diffusion of the dye into the polymer structure, and narrow the scope of its applicability only for dyes, thermodynamically compatible with the polymer.

Closest to the claimed is a method of injecting dye into the polymer (polymer fiber-based fibre-forming crystallizable polymers by extrusion of the polymer in the form of a fiber in an adsorption-active liquid medium (AAS)containing dissolved dye, followed by drying of the polymer and its annealing carried out in terms of retention of the polymer in tension in the direction of drawing [Guthrie R.T. Pat. USA No. 4001367, 1977, CL 264-154] - prototype.

This method is based on the well-known phenomenon of crazing of polymers that occur in the process of stretching a polymer elongated shape (polymer PL, fibers, rods, ribbons, etc) specially selected adsorption-active liquid medium (AAS), which can be used, for example, hydrocarbons, alcohols, ketones, etc. In these conditions in the process of drawing the polymer occurs the system of interconnected microscopic pores, so-called crazes, environmental filled polymer liquid. Under the hood of polymers in AGS containing dissolved dye, rest the R dye initially fills the formed polymer crazes, then in the process of further drawing is the collapse occurred in the polymer structure and the complete closure of the formed pores, followed by pushing smaller molecules AGS of the polymer and mechanical capture a larger dye molecules and durable committing them throughout the volume of the polymer.

The disadvantages of this method are its applicability only to fibre-forming (semi-crystalline) polymers, such as polyolefins, polyesters, polyamides, etc. capable of large deformations, in which there is a collapse of the structure of the polymer, followed by trapping of the dye molecules. In addition, semi-crystalline polymers, due to their two-phase structure, as a rule, do not have sufficient optical clarity that is not possible to obtain optically transparent polymers containing dye. Also implemented in this method the drying and annealing of the extruded colored polymer is carried out in terms of retention of the polymer in tension in the direction of drawing, and with the aim to permanently fix the polymer structure, lead to the production of oriented polymer, which also adversely affects the optical properties of the polymer and does not allow to obtain optically transparent colored polymers.

An object of the invention are the two who is developing a method of injecting dye in the polymer, allowing to obtain optically transparent colored polymer PL.

This technical result is achieved in that in the method of injecting dye into the polymer by extrusion of the polymer in AGS containing dissolved dye, followed by drying of the polymer and its annealing, the polymer used undirected PL amorphous polymer, the annealing of the polymer is carried out at a temperature of from the glass transition temperature of the polymer to a temperature chemical decomposition of the polymer with the dye, and drying of the polymer and its annealing is conducted without retention of the polymer in tension in the direction of drawing.

As the original polymer in the proposed method can be used undirected Square of the amorphous polymer, such as polymethylmethacrylate (PMMA), polystyrene (PS), polyvinyl chloride (PVC), polycarbonate (PC), etc. Use as polymer undirected PL is due to the fact that the process of injecting dye is associated with the stretching of the polymer, as for Sq oriented amorphous polymers such process is difficult. Can be used as amorphous homopolymers and their copolymers, as well as two-component and multicomponent mixtures of amorphous polymers. This srednevekovoy molecular mass (Mw) the original polymer and the thickness of the Square can be varied within wide limits, e.g. the measures from 10,000 to several million, and from 5 to 1000 microns, respectively.

As AAS you can use various organic compounds such as alcohols, ketones, hydrocarbons and so on, as well as binary and multicomponent solutions, including aqueous solutions. We have experimentally found that as AAS you can use organic or aqueous solutions of ionic and nonionic surfactants, the concentration of which in solution can be varied within wide limits.

As the injected dye, you can use any soluble in used AAS dyes such as brilliant green, Sudan, 2-Rhodamine, Sudan-4, etc. as well as mixtures of these dyes.

Hood PL can be performed in a wide temperature range, for example from freezing temperature used AAS to boiling point in the case, if this temperature is below the glass transition temperature of the polymer and the temperature of the chemical decomposition of the dye. Hood PL can be done with different speeds, for example, from 1×10-2up to 1×105mm/min Degree of extraction can be varied within wide limits, for example from 2% before breaking Sq. Geometrical dimensions of the original Square can be any.

Drying of the polymer after extraction can be performed in a wide temperature range, for example from the freezing temperature of the solvent until t is mperature vitrification of the polymer.

Annealing of the polymer can be performed in a wide temperature range, for example from a glass transition temperature of the polymer to a temperature chemical decomposition of the polymer with the dye. The need for annealing the polymer at a temperature equal to or above its glass transition temperature, due to the fact that only in these conditions in the annealing process is complete healing fibrillar-porous structure of crazes, krizovany the polymer containing the dye undergoes shrinkage, fully restores its size, loses acquired as a result of the extraction of molecular orientation and fully restores its structure and properties, including optical transparency.

When this is introduced into the polymer dye is evenly distributed in the polymeric matrix. However, the above processes occur only if the drying of the polymer and its annealing is conducted without retention of the polymer in tension in the direction of extrusion, i.e. the polymer is released from the clamps of the stretching device, in other words, is transferred to the free state.

Drying of the polymer and its annealing can be performed during different time, and duration of these processes depends on the process temperature, the boiling point AAGS, the chemical nature of the polymer and the thickness of the poly the agreement PL.

The advantages of the proposed method are illustrated in the following examples.

Example 1.

Undirected PL amorphous PS with Mw=200000 and a glass transition temperature of 90°With a thickness of 70 μm is fixed in the clamps manual stretching device, then pull at 40°with a speed of 1 mm/min 10% to 0.05 g/l solution of brilliant green dye in ethanol. After that, an elongated Square released from the clamps of the tensile device, and then dried at 30°C for 60 min in a free state. Then the specified PL also in the free state annealed for 20 min at a temperature of 130°With that 40°exceeds the glass transition temperature of PS. Get transparent PL from PS, uniformly colored green.

Example 2.

Undirected PL amorphous PMMA with Mw=150000 and a glass transition temperature 115°With a thickness of 100 μm is fixed in the clamps manual stretching devices, are then pulled out at 25°With 25% with a speed of 10 mm/min, 0.04 g/l ethanol solution of the dye indigotindisulfonate potassium. After that, an elongated Square released from the clamps of the tensile device, then first dried at 20°C for 30 min in a free state in a vacuum Cabinet, then VL in the free state is annealed for 30 min at a temperature of 150°With that at 35°To exceed the AET glass transition temperature of PMMA. Get a Square of transparent PMMA, uniformly colored blue.

Example 3.

Undirected PL amorphous PC with Mw=23000 and a glass transition temperature of 145°With a thickness of 250 μm is fixed in the clamps manual stretching devices, are then pulled at 20°With 50% with a speed of 20 mm/min to 0.08 g/l ethanol solution of the dye rhodamine C. After that, an elongated Square released from the clamps of the tensile device, and then dried at 50°C for 60 min in a free state in a vacuum Cabinet. Then the specified PL also in the free state is annealed for 10 minutes at a temperature of 160°With that on 15°exceeds the glass transition temperature of the PC. Get transparent Dps from PC, uniformly painted in pink color.

Example 4.

Undirected PL amorphous PVC with Mw=250000 and a glass transition temperature of 70°With a thickness of 80 μm is fixed in the clamps manual stretching device, then pull with 15°With 20% with a speed of 50 mm/min in 0.04 g/l solution in n-heptane dye Sudan 2. Elongated Square released from the clamps of the tensile device, and then dried at 20°C for 60 min in a free state. Then the specified PL also in the free state is annealed for 40 min at a temperature of 100°With that on 30°exceeds the glass transition temperature of PVC. Get transparent P is PVC, uniformly orange in color.

The method of injecting dye into the polymer by extrusion of the polymer in an adsorption-active liquid medium containing the dissolved dye, followed by drying of the polymer and its annealing, characterized in that the polymer used as unoriented polymer film made of amorphous polymer, the annealing of the polymer is carried out at a temperature of from the glass transition temperature of the polymer to a temperature chemical decomposition of the polymer with the dye, and drying of the polymer and its annealing is conducted without retention of the polymer in tension in the direction of drawing.



 

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