Luminescent enamel and method of its obtaining

FIELD: paint and varnish coverings.

SUBSTANCE: luminescent enamel contains a mix of solutions of two film-forming components - 50% solution polymethylphenylsiloxane pitch in toluene and 15% solution of a butyl methacrylate copolymer and methacrylic acid or a butyl methacrylate copolymer and amide of methacrylic acid in mixes of organic solvents, a luminescent pigment with long afterglow - strontium-calciumvaluminum silicate, activated by europium and neodymium, if necessary an additional pigment - titanium dioxide or zirconium dioxide, filler - aerosil at the declared proportion of the components. Also the method of obtaining of luminescent enamel and a product, where the described enamel is applied, is described.

EFFECT: allows obtaining coverings with high luminescent effect.

6 cl, 2 tbl, 14 dwg

 

The invention relates to coatings fluorescent type, which can be used for applying the signal labels clearly visible in the absence of external illumination, for example for painting road signs, for the application of distinctive signs, in different locations and in different branches of industry and agriculture.

Known fluorescent paint comprising a binder, daylight fluorescent pigment, solvent, plasticizer, in which the binder used is a copolymer of methyl methacrylate, styrene and Acrylonitrile in a quantity 9-14 wt.% in a mixture of organic solvents containing xylene, toluene or a mixture in any proportion in the amount of 40-70 wt.%, the dioctylphthalate 2-4 wt.%, daylight fluorescent pigment 13-20 wt.% (ed. mon. The USSR 314782, bull. No. 28, 21.11.1971 year).

The paint has insufficient coverage and dries long.

Known fluorescent fluorescent paints based on acrylic, silicone and acrylamide resins [Paint materials and their applications, M.: Goskomizdat, 1963, p.18-21].

Paints based on acrylic resins having a high viscosity of concentrated solutions, it is necessary dilute to enable their application by sprinklers. In addition, there is a need for the La to obtain a coating of the desired thickness and achieve the effect of reflection apply multiple layers (up to 5 layers). The disadvantage of these paints is also a need for additional applied on the fluorescent coating lacquer-filter containing antioxidants to convert or absorb UV component of daylight (300-400 nm), while reducing its harmful effects on the coating. However, the paint filter does not increase the resistance of the paint, which is estimated at 3-6 months.

Known fluorescent coatings for application distinguishing marks on factory equipment, improve visibility on land vehicles, aircraft. Such fluorescent coatings include fluorescent pigments finely dispersed particles of resin, painted with fluorescent dyes. A significant part absorbed from the surrounding space and energy these coatings give back, reflecting, and the unabsorbed portion of the incident light [Reibman A.I. Protective paint coating. Chemistry. Leningrad branch, 1982, s-244].

The disadvantage of these coatings is also the need for varnish filter to improve their light fastness and low weather resistance of the coating and the tendency of the paint to flake when stored.

The closest major signs providing luminescent effect, a prototype of the invention is a printing ink containing the self phosphor and a polymer binder. The phosphor used aluminosilicate strontium-calcium formula SrCa2[2 (Al2O3SiO4)], and as the polymeric binder is a mixture of plasticized polyester resin or phenol-formaldehyde resin with ethyl cellosolve, cyclohexanone and heavy high-boiling petroleum fractions in the following ratio of components, wt.%: the polyester resin plasticized or phenol-25-55, ethyl cellosolve 2-7, cyclohexanone 2-9, heavy high-boiling petroleum fractions 30-70, strontium silicate-calcium 30-70, europium from 0.3 to 3.7, neodymium of 0.1-0.9, polymeric binder 25-70. However, this paint is intended for creation of printed products and does not have sufficient weather resistance (EN 2179565, CL C09D 5/22, 2002).

The technical task of the present invention is the creation of the exposed enamel with prolonged persistence in low light conditions.

To solve this problem is proposed fluorescent enamel containing film-forming component, a fluorescent pigment with a long afterglow - strontium silicate-calcium, activated by europium and neodymium, if necessary, additional pigment is titanium dioxide or zirconium dioxide, filler Aerosil, in which the film-forming component consists of the mixture of film-forming solutions of two components: 50%-aqueous solution of polymethylphenyl siloxane resin in toluene and 15%-aqueous solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and amide of methacrylic acid in a mixture of organic solvents in the following ratio, wt.%:

50%solution of polymethylphenyl siloxane
resin in toluene20-30
15%solution of the copolymer
of butyl methacrylate and methacrylic
acid or a copolymer of butyl methacrylate
and amide of methacrylic acid in the mixture
organic solvents30-40
fluorescent pigment - aluminosilicate
strontium-calcium, activated by europium
and neodymium20-30
filler Aerosil2-8
this additional pigment0-15

As a copolymer of butyl methacrylate and methacrylic acid in the present invention uses a resin BMC-5, and as a copolymer of butyl methacrylate and methacrylic amide acid - resin speakers.

For the preparation of solutions of film-forming components is a mixture of organic solvents containing acetone, butylacetate toluene in the ratio 3:3:4 respectively.

The weather resistance of the enamel with long luminescent effect is provided by the use of a mixture of two solutions of film - forming components of polymethylphenyl siloxane resin and a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and methacrylic amide acid and the introduction of the enamel as a fluorescent pigment phosphor with long afterglow - aluminosilicate strontium-calcium activated with europium and neodymium in the amount of 20-30 wt.%.

When you need to improve coverage in the composition of the enamel may be included any additional pigment, for example titanium dioxide or zirconium. However, its presence is optional.

To make the enamel of the desired rheological properties of the composition contains a filler, such as Aerosil.

To achieve the claimed technical result is proposed a method of obtaining a fluorescent enamel of the specified structure.

It is known that the efficiency of phosphors depends on the size of the phosphor particles, their crystal structure and sequence of operations of mixing in the production cycle the production of enamel.

Known method of preparing a fluorescent dye, wherein in the reaction apparatus with a stirrer and a steam-jacketed loads in accordance with the formulations of the second solvent, the plasticizer and copolymer, the temperature in the apparatus is brought to 100-130°C. After complete dissolution of the copolymer download light and daylight fluorescent pigment (ed. mon. The USSR 314782, bull. No. 28, 21.11.1971 year). The paint obtained by this method has insufficient coverage, long dries and does not have sufficient brightness.

Closest to the proposed method of obtaining fluorescent enamel prototype is a technique in which the polymeric binder is mixed with powder of strontium silicate-calcium activated with europium and neodymium. The resulting mixture was passed through rolls kratkotrajno machine (EN 2179656, CL C09D 5/22, 20.02.2002).

Conventional techniques for the manufacture of paint and varnish materials (dispersion in a bead or ball mill) in the manufacture of fluorescent paints lead to the partial destruction of the crystal structure of the phosphor, which reduces the efficiency of the phosphor.

The technical result of the present invention is, in addition to increasing weather resistance, ensuring maximum efficiency of the phosphor.

To obtain the technical result is proposed a method of obtaining a fluorescent enamel by pre-dispersion in a bead mill filler - Aerosil in the Asti 50%-aqueous solution of polymethylphenyl siloxane resin in toluene to milling degree at least 20-30 μm and then adding a fluorescent pigment aluminosilicate strontium-calcium activated with europium and neodymium, the resulting dispersion mixture is injected into the remaining portion of the 50%-aqueous solution of polymethylphenyl siloxane resin in toluene and dispersed advanced no more than 5 minutes, and then mixed with 15%solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and methacrylic amide acid in a mixture of organic solvents consisting of acetone, butyl acetate and toluene in the ratio 3:3:4 respectively.

If necessary, prior to the introduction of the enamel 15%-aqueous solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and methacrylic amide acid in a mixture of organic solvents in the specified solution is injected additional pigment, followed by dispersing the mixture before milling degree not more than 45 μm, after which the suspension is introduced into a suspension of the filler and the fluorescent pigment in a 50%solution of a polymethylphenylsiloxane resin in toluene.

To prepare a 15%solution of a copolymer of butyl methacrylate and methacrylic acid is prepared a mixture of organic solvents of acetone, butyl acetate and toluene in the ratio 3:3:4 respectively.

An example of the method of preparation of the enamel.

Prepared in toluene 50%Rast is the PR of polymethylphenyl siloxane resin. The filler in a bead mill with your prescription number, specified in the examples of table 1, is introduced into part of a 50%aqueous solution of polymethylphenyl siloxane resin in toluene was dispersed to milling degree no more than 20-30 microns, then add fluorescent pigment - strontium silicate-calcium, activated by europium and neodymium with constant mixing these components. The resulting suspension of the filler with fluorescent pigment is injected into the remaining portion of the 50%-aqueous solution of polymethylphenyl siloxane resin and subjected to further dispersion of not more than 5 minutes.

The prepared suspension of the filler with the above fluorescent pigment in a 50%solution of a polymethylphenylsiloxane resin in toluene is mixed with pre-cooked in a mixture of organic solvents containing acetone, butyl acetate and toluene in the ratio 3:3:4 respectively 15%solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and methacrylic amide acid or, if necessary, with additional suspension of the pigment is titanium dioxide or zirconium dioxide, a 15%solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and methacrylic amide acid in the above-mentioned mixture of organic solvents.

Examples from science is the use of specific sootnoshenii components are shown in table 1.

For all examples were produced samples of coating thickness 60-80 µm. Fluorescent enamel was applied to a substrate pre-coated with a layer of enamel as-599 thickness of 20-30 μm. Measuring the brightness was performed after irradiation of the samples by the incandescent lamp.

Table 2 shows the characteristics of the proposed structures fluorescent enamel: stability of luminescent characteristics of enamel, weather resistance and brightness of the coating compared to the prototype.

Samples enamels were subjected to accelerated tests simulating operation of coatings in atmospheric conditions by the method 2 GOST 9.401-91 for 15 cycles, which corresponds to two years of operation under field conditions. Evaluation of the condition of coating after test was carried out according to GOST 9.407-84. The stability of the luminescent properties of the coatings were characterized by the ratio of brightness of coatings subjected to the tests, to the brightness of the coatings to the test.

State data samples of the coatings obtained using the present invention and shown in the examples in table 2, show that they are considerably superior to the prototype in weather resistance and brightness of the glow.

In luminescent enamel had not been used for combination with the phosphor film-forming composition consisting of a mixture of solutions of polyphenylsiloxane the OIC resin and copolymer of butylmethacrylate methacrylic acid, claimed in this invention, which determines its novelty.

It was established experimentally that the change in the ratio of film-forming, as the change in the concentration of fluorescent pigment outside the claimed does not improve weather resistance, ensuring maximum efficiency of the phosphor in low light conditions, which confirms the inventive step of this technical solution (Examples 13 and 14 in tables 1 and 2).

The obtained fluorescent enamel claimed composition can be applied by spray to create a signal label, clearly visible in the absence of external illumination, for example for painting road signs, for applying distinctive signs on factory equipment, improve visibility on land vehicles, aircraft, in different areas and in different branches of industry and agriculture. On the surface of such products fluorescent enamel claimed composition is applied on pre-coated with a layer thickness of 20-30 microns of enamel as-599.

The composition of the enamel AC 599 contains suspension of pasta ACT (pigment, expanded resin and plasticizer) and acrylic resin in a mixture of organic solvents with addition of plasticizer and corresponds to THE 6-10-849-80. Enamel AC-599 as a result, the attendance for painting various surfaces by special technology and has the following specifications: viscosity by viscometer B3-246 with the nozzle diameter of 4 mm at a temperature of (20,0± 0,5)°14-20 sec; mass fraction of solids 34-40%; drying time to degree 3 at a temperature of (20±2)°With no more than 2 hours; the film hardness by pendulum device: M-3 is not less than 0.4$; TML (pendulum a) is not less than 0.2 of atmospheric air; the elasticity of the film at the bend of not more than 1 mm of Enamel is applied by spraying. If necessary, dilute with solvent P-5A. The consumption of single-layer coating 59-89 g/sq.m. Warranty shelf-life 6 months from date of manufacture.

To improve luminescent effect before applying the enamel on the surface of the products it is advisable to apply the paint reflective layer containing reflex components, for example aluminium powder or glass microspheres with a particle size of 80-150 microns.

In the manufacture of a road sign or other products having a metal surface, it is pre-degreased, washed with water and dried. On the resulting mirror surface and then put a layer of the reflector, for example, any white paint, and then, if necessary, a reflective layer containing glass microspheres with a particle size of 80-150 μm, and then dried layer of the enamel is applied by spray fluorescent enamel of the proposed structure.

When applied luminescent enamel on concrete curb that separates the road from the pavement, the walls in the production of the public premises after sanding and priming the surface of the applied intermediate layer of enamel as-599 thickness of not more than 25 μm, then the fluorescent layer of enamel.

Table 1
Recipe samples enamels
ComponentsExamples
The component content in the enamel, wt.%
1234567891011121314
50%solution of polymethylphenyl siloxane resin in toluene3030252522222020252530301835
15%solution of a copolymer of butyl methacrylate and methacrylic acid30-39-40-40-35-40-26-
15%solution of a copolymer of butyl methacrylate and methacrylic amide acid-30-39-40 -40-35-40-42
the aluminosilicate strontium-calcium, activated by europium and neodymium2828303030302020252520203218
Titanium dioxide44----151510108817-
The Zirconia44----1515101088-2
Aerosil88668855552273

Table 2
Properties of enamels, depending on the composition of the a and external influences
IndexExamples
Proto GUI1234567891011121314
The brightness of the enamel sample after 60 min after termination of the excitation light, MCD/m2103033323235'353030313127271823
The change of brightness of enamel samples, subjected to the tests for resistance to atmospheric conditions, oted0,201,000,910,940,940,890,890,930,930,940,940,960,960,500,78
Resistance method GOST 9.401-91AS ADAZADAS AD1AS AD1AS AD1AS AD1AS AD1AS AD1AS AD1AS IS AS AD1AS AD1AS AD1ASS AD2 AZ

1. Fluorescent enamel containing film-forming component, a fluorescent pigment with a long afterglow - strontium silicate-calcium, activated by europium and neodymium, if necessary, additional pigment is titanium dioxide or zirconium dioxide, filler Aerosil, in which the film-forming component consists of a mixture of two solutions of film-forming components - 50%-aqueous solution of polymethylphenyl siloxane resin in toluene and 15%-aqueous solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and methacrylic amide acid in a mixture of organic solvents in the following ratio, wt.%:

50%solution of polymethylphenyl siloxane resin in toluene20-30
15%solution of a copolymer of butyl methacrylate and methacrylic acid, or
copolymer of butyl methacrylate and methacrylic amide acid in organic solvents30-40
fluorescent pigment - strontium silicate-calcium, activated by europium and neodymium20-30
specified additional the additional pigment 0-15
filler Aerosil2-8

2. Fluorescent enamel according to claim 1, in which 15%solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and methacrylic amide acid contains a mixture of organic solvents acetone, butyl acetate and toluene in the ratio 3:3:4 respectively.

3. The method of obtaining fluorescent enamel according to claim 1 by pre-dispersion in a bead mill filler - Aerosil in parts of a 50%aqueous solution of polymethylphenyl siloxane resin in toluene to milling degree at least 20-30 μm and then adding a fluorescent pigment - aluminosilicate strontium-calcium activated with europium and neodymium, the resulting dispersion mixture is injected into the remaining portion of the 50%-aqueous solution of polymethylphenyl siloxane resin in toluene and dispersed optionally not more than 5 min, and then mixed with 15%solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer of butyl methacrylate and methacrylic amide acid in a mixture of organic solvents, consisting of acetone, butyl acetate and toluene in the ratio 3:3:4 respectively.

4. The method according to claim 3, in which prior to the introduction of the enamel 15%-aqueous solution of a copolymer of butyl methacrylate and methacrylic acid or a copolymer Buti is the amide methacrylate and methacrylic acid in a mixture of organic solvents in the specified solution add additional pigment, followed by dispersing the mixture before milling degree not more than 45 μm, then the obtained suspension is injected into a suspension of the filler and the fluorescent pigment - aluminosilicate strontium-calcium activated with europium and neodymium in a 50%solution of a polymethylphenylsiloxane resin in toluene.

5. Fluorescent enamel according to claim 1, used for drawing on traffic signs, signal labels, distinctive signs, in different locations.

6. Articles containing the enamel layer of the AU-599 thickness of 20-30 μm, optionally, reflective paint layer, over which is applied a fluorescent enamel composition according to claim 1.



 

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3 cl, 2 tbl

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2 tbl

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11 cl, 2 tbl, 2 ex

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2 cl, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: invention relates to compositions for flame resistant coating production on wood, especially coloured coatings that shift wood to the hard-flammable material group. The composition for flame resistant coating of wood is described. It contains 8.5-28.0% weight ratio of polyorganosiloxane, 4.0-25.0% weight ratio of a pigment, 2.0-15.0% weight ratio of the filler - muscovite, 2.0-5.0 % weight ratio of trischlorinepropylphosphate as a plasticiser, 0.8-3.0% weight ratio of the rheological additive - bentonite clay and organic solvent, additionally the composition has 4.0-15.0 % weight ratio of alkyd lacquer PF-60 and/or propenoic copolymer BMK-5 which are used as a repining modifier, 10.0-40.0 % weight ratio of ammonium polyphosphate and/or the aluminosilicate filling agent as a flame retarder, organic solvent. At the same time the composition contains polymethylphenylsiloxane laquer "КО-075" or polyphenylsiloxane resin 139-297 as polyorganosiloxane, dolomite or diatomaceous silica or micronised calcspar or zirconium dioxide or micronised agilite or its blend with at least one of them as a filling agent, as a pigment it contains titanium dioxide or chrome oxide or iron - manganese, blended oxide or red ferric oxide, as an organic solvent - xylene or solvent naphtha or propanone or butyl acetate or its mixture.

EFFECT: coatings prepared on the basis of such composition have flame retardant properties and high resistance to proportional action of water.

5 cl, 2 tbl, 11 ex

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