KR100653402B1 - coloring agent for an infrared lamp, process for producing the same and coloring method using the same - Google Patents

Abstract

The present invention is an infrared lamp manufactured by combining the components containing a copper compound (CuO, Cu (OH) ₂ or Cu ₂ O), aqueous methanol solution, concentrated sulfuric acid, silver nitrate (AgNO ₃ ) aqueous solution, silicon dioxide (SiO ₂ ) and loess coloring agent; A method for producing the colorant; And a coloring method using the coloring agent.

The present invention filters visible light of 700 nm or less, which causes eye fatigue and increases stress, and improves thermal effect by increasing infrared transmittance, and in particular, it is possible to provide a transparent black-red infrared lamp which is free from discoloration due to heat and chemicals. do.

Colorant, coloring method, infrared lamp, filtering, heat effect

Description

Infrared lamp colorant, manufacturing method thereof, and coloring method using same {coloring agent for an infrared lamp, process for producing the same and coloring method using the same}

Figure 1 shows a comparison of the radiation spectrum, the radiation flux (mW), the illuminance according to the wavelength of the colored infrared lamp, Cree lamp and conventional resin lamp in the second embodiment of the present invention.

FIG. 2 is a tissue photograph of an infrared lamp in which a transparent black-red colored infrared lamp is photographed using a scanning electron microscope in Example 2 of the present invention.

The present invention relates to a colorant using an inorganic pigment system for coloring glass, a method for producing the same, and a coloring method using the same.

Clear lamp is a continuous spectrum of 400 nm or more, and visible light and infrared rays are emitted.

Infrared lamps are intended for use in medical, heating, poultry or pig farms, and saunas, using the thermal effects of infrared light. Therefore, since visible light of 400 to 750 nm increases eye stress and increases stress, it is required to filter the visible light area to reduce eye fatigue and further increase a thermal effect.

Conventionally, the filtering of the visible light region is removing the wavelength of less than 600 nm by the red coating. Korean Patent Publication No. 193-0022454 discloses coating a ceramic solution composed of silicon dioxide, aluminum oxide and a resin solution on a precursor glass. In this case, there is a problem that the color is discolored due to the high temperature generated in the resin-coated light bulb, there is a problem that the coating is peeled off when re-coating the silicone resin to prevent breakage of the lamp glass.

Unlike the above, a method of coating a red color using an inorganic pigment has not been disclosed, and the method of coating the red color has a yellow color or a purple color, and the color is not dark.

On the other hand, Korean Patent Publication No. 1994-0006943 discloses color glass by immersing plate glass in a coating solution containing potassium nitrate, sodium nitrate and silver nitrate at a temperature of 450 to 520 ° C. for 10-15 minutes in a coating solution containing copper nitrate or manganese nitrate. Disclosed is a method of manufacturing. This method is effective in the continuous process of plate glass because the place where the solution of the colorant should be high is about 500 ° C, but it is difficult to mass-produce in glass of small size and various shapes such as lighting glass.

In addition, the same principle is also used in the far-infrared radiation incandescent bulb in terms of utilizing the thermal effect. Among these patents for far-infrared radiation, Korean Patent Publication No. 10-0387752 discloses a part of silicon oxide, aluminum oxide, titanium dioxide, zirconium oxide or the like for increasing the far-infrared emissivity on the inner or outer surface of the glass bulb of the incandescent lamp and its mechanism. Far-infrared rays that are beneficial for promoting metabolism and growing plants and animals by coating bio ceramic powders having a particle size of several μm containing all or a small amount of manganese dioxide, copper oxide, calcium oxide, and chromium oxide as a main ingredient. Discloses spinning. The method of coating in this patent is the same as the principle of powder coating the fine powder of the oxide blended.

An object of the present invention is to filter visible light of 700 nm or less and increase the infrared ray transmittance to enhance the thermal effect, and in particular, to provide an infrared lamp colorant free from discoloration due to heat and chemicals, a manufacturing method thereof, and a coloring method using the same. It is done.

The present invention is an infrared ray prepared by combining the components containing a copper compound (CuO, Cu (OH) ₂ or Cu ₂ O), aqueous methanol solution, concentrated sulfuric acid, silver nitrate (AgNO ₃ ) aqueous solution, silicon dioxide (SiO ₂ ) and loess It relates to a lamp colorant.

In the above copper compound (CuO, Cu (OH) ₂ or Cu ₂ O) is 10 to 18% by weight, methanol aqueous solution (80 to 95% by volume) 15 to 40% by weight, concentrated sulfuric acid (95% or more) 18 to 25 Weight%, silver nitrate aqueous solution (90 to 110 wt / vol%) may be included in 12 to 19% by weight, silicon dioxide (SiO ₂ ) 10 to 23% by weight and ocher 2 to 8% by weight.
In the above case, nitric acid means that 110g / vol% solution is dissolved in water (distilled or distilled water) to make 100 ml volume.

The present invention synthesizes a colorant by dissolving an oxide of a metal in sulfuric acid and a silver nitrate solution as described above. The following easy pigments are characterized by the addition of a large amount in the synthesis step. Therefore, the manufacturing cost of the colorant is considerably lowered. In addition, the pigment in the present invention serves to increase the smooth reaction and dispersion effect of the added reaction product and increase the amount of colorant production, the pigment to be added is mostly silicon dioxide (SiO ₂ ), a small amount of ocher is added.

The synthesized colorant of the present invention is a colloid of copper sulfate (CuSO ₄ · 5H ₂ O) and silver sulfate (Ag ₂ SO ₄ ) is dispersed in sulfate ions, nitrate ions, H ₂ O, methanol, silicon dioxide (SiO ₂ ) and loess It is a slurry solution mixed with.

The viscosity of the colorant of the present invention can be adjusted with aqueous methanol solution (80 to 95% by volume), preferably 1800 ± 200 cP at 23 ℃.

If the solid content of the colorant is too small, it is not applied to the surface of the glass quickly, if too much, the colorant is slippery during the drying process has a problem that the coloring is not good, the solid content of the colorant in the present invention is preferably 80 ± 5% by weight.

If the particle size of silicon dioxide (SiO ₂ ) used as the pigment exceeds 20 μm, the coloring becomes opaque and if it is 20 μm or less, it becomes transparent. Since the particle size of the pigment is an important variable for coloring, the particle size of silicon dioxide (SiO ₂ ) used in the present invention is preferably 20 μm or less.

In the present invention, ocher acts as a parameter of the stabilization and viscosity formation of the colorant.

The colorant of the present invention is applied to the surface of the lamp and then dried and heat-treated to give a transparent black red color, to filter visible light of 700 nm or less and to increase the infrared ray transmittance to enhance the thermal effect, in particular discoloration by heat and chemicals Has no features.

The method for preparing a colorant of the present invention comprises mixing a copper compound (CuO, Cu (OH) ₂ or Cu ₂ O) and silicon dioxide (SiO ₂ ) with an aqueous methanol solution, and then reacting with concentrated sulfuric acid; Adding silver nitrate (AgNO ₃ ) aqueous solution to the solution and reacting with stirring; Adding silicon dioxide (SiO ₂ ) and ocher as pigments to the solution; And pulverizing the particles of the colorant slurry solution synthesized above by adding an aqueous methanol solution.

In detail, the method for preparing a colorant of the present invention is a copper compound (CuO, Cu (OH) ₂ or Cu ₂ O) 10 to 18% by weight and silicon dioxide (SiO ₂ ) 9 to 15% by weight in methanol aqueous solution (80 to 95% by volume) 12 to 17% by weight, and then reacted by adding 18 to 25% by weight of concentrated sulfuric acid (95% or more); Adding 12 to 19 weight% of silver nitrate aqueous solution (90 to 110 wt / vol%) to the solution and reacting with stirring; Adding 1 to 8% by weight of silicon dioxide (SiO ₂ ) and 2 to 8% by weight of ocher as a pigment to the solution; And pulverizing the particles of the colorant slurry solution synthesized above by adding 3 to 23% by weight of an aqueous methanol solution (80 to 95% by volume).

The grinding time depends on the amount of the colorant synthesized and the type of the mill, but in the case of 1L of the synthesized colorant, it is preferable to grind it in a ball mill for about 1 hour. (The particle size of the colorant is MAX 20 µm or less.)

The method of coloring an infrared lamp using the coloring agent of this invention is as follows.

First, the infrared lamp glass was dipped into the colorant at a rate of 5 to 15 seconds / piece, dried under warm air maintained at 55 ± 5 ° C. for 25 ± 10 minutes, and continuously 6 to 20 ° C./min.

Heated for 30 to 90 minutes in an electric furnace maintained at 540 to 600 ℃ by raising the temperature to minutes.

In the above coloring method, the metal ions are diffused into the glass surface layer to be melted and colored by the metal glass, and when the temperature rise of the heat treatment is faster than the suggested speed, the staining or bubbles, etc. are likely to occur. There is a problem. In addition, the heat treatment temperature is good at coloring at 540 to 600 ℃, the concentration and gloss of the coloring at 570 ℃ is the best.

Hereinafter, the present invention will be described in detail through Examples and Test Examples. However, the scope of the present invention is not limited by these examples and experimental examples.

Example 1 Preparation of Infrared Lamp Colorant

34 g of copper oxide (CuO) and 30 g of silicon dioxide (SiO ₂ ) were mixed with 44 mL of an aqueous methanol solution (95% by volume), and then 28 mL of concentrated sulfuric acid (96%) was added and reacted. Silver nitrate in this solution 20 mL of an aqueous solution (100 wt / vol%) was added and reacted with stirring. To this solution, 9 g of silicon dioxide (SiO ₂ ) and 12 g of ocher were added. The colorant of the present invention was prepared by pulverizing all of the synthesized colorant slurry solution while adding 50 mL of an aqueous methanol solution (95% by volume) for 1 hour. Here, silicon dioxide (SiO ₂ ) was used having a particle size of 20 μm or less.

Comparative Example 1. Preparation of Infrared Lamp Colorant

Silicon dioxide (SiO) with particle size exceeding 20㎛₂A colorant was prepared in the same manner as in Example 1 except that was used.

Example 2. Coloring of Infrared Lamps

The infrared lamp glass was dipped at a rate of 10 seconds / piece using the colorant prepared in Example 1 and dried for 30 minutes under a warm air maintained at 55 ° C, and subsequently heated to 10 ° C / min and maintained at 570 ° C. The infrared lamp was colored by heat treatment for 90 minutes at.

Example 3. Coloring of Infrared Lamps

Using the colorant prepared in Comparative Example 1, The infrared lamp was colored in the same manner as in Example 2 except that the heat treatment was performed for 50 minutes.

Example 4. Coloring of Infrared Lamps

The infrared lamp was colored in the same manner as in Example 2 except that the heat treatment was performed for 30 minutes.

Test Example 1. Thermal Effect Test of Infrared Lamp

In order to test the thermal effects of the infrared lamps colored by the colorant of the present invention, the temperatures of each of the infrared lamps, the cree lamps and the existing resin coating lamps colored in Examples 2, 3 and 4 were measured under the same conditions.

The experimental results are shown in Table 1.

Type of lamp (250 W) Surface temperature (℃) Remarks Cree lamp 180 Lamp clear glass before coloring Conventional resin lamp 200 Opaque red painted product Darkness Lamp according to Example 2 270 Transparent black rose (90 minutes heat treatment) Lamp according to Example 3 270 Opaque black rose (50 minutes heat treatment) Lamp according to Example 4 245 Transparent black rose color (30 minutes heat treatment)

As shown in Table 1, the surface temperature after the coloring of the existing resin coating product was increased by 20 ℃ compared to the Cree lamp, the surface temperature of the infrared lamp according to Examples 2 and 3 of the present invention was increased by 90 ℃, transparent The surface temperature of the thing (Example 2) and the opaque thing (Example 3) was the same at 270 degreeC. The surface temperature of the infrared lamp according to Example 4 of the present invention, which was slightly lower in color density, was 45 ° C. higher than the surface temperature of the conventional resin coating product.

From the above results, it was confirmed that the thermal effect of the infrared lamp colored with the coloring agent of the present invention is very excellent.

Test Example 2 Heat resistance and chemical resistance test of the infrared lamp

In order to test the heat resistance of the colored infrared lamp according to the present invention, for each infrared lamp colored in Examples 2, 3, and 4, the color of the lamp by the heat emitted by the lamp itself is turned on until the lamp life is over. And transparency changes were observed. This test is to compare the heat resistance of the infrared lamps according to the present invention with the existing lamps that have undergone a change in color during the use of the bulb. The test method was applied until the end of the lamp life by applying a voltage of 120 VOLT to the infrared lamp.

As a result of the heat resistance test, no change in color and transparency of the colored portion was observed in each of the infrared lamps colored in Examples 2, 3 and 4.

For the infrared lamps colored in Examples 2, 3 and 4 to test the chemical resistance of the colored infrared lamps according to the present invention, the lamp surface was immersed in aqua regia and acetone for 1 week to change color and erosion of the lamps. Was observed.

This test was carried out by dipping in aqua regia and by dipping in acetone to verify solvent resistance.

As a result of chemical resistance test, no color change or erosion was observed in the colored part of all infrared lamps.

Test Example 3 Test of Visible Light Filtering Effect of Infrared Lamp

In Example 2, an experiment was performed to compare radiation spectrum, radiation flux (mW), and illuminance according to wavelengths of colored infrared lamps, clear lamps, and conventional resin lamps.

Radiation spectrum analysis was performed by applying power (222W) to the infrared lamp and measuring the illuminance, radiant flux and chromaticity coordinates using a spherical photometer and a total flux meter and obtaining color from the chromaticity coordinates.

The experimental results are shown in FIG.

As can be seen in Figure 1, the wavelength of the energy radiated from the Cree lamp is visible and infrared continuous spectrum of more than 400 nm, and in the conventional resin coating lamps filtered visible light from 400 to 600 nm A continuous spectrum of infrared light was observed. On the other hand, in the infrared lamps colored with the coloring agent of the present invention, a continuous spectrum of infrared light filtered with visible light of 700 nm or less was observed.

In addition, it was confirmed that the radiation rate and illuminance of the infrared lamps colored with the colorant of the present invention were significantly reduced compared to the cree lamps and the conventional resin coating lamps. Compared with the lamp surface temperature test results of Table 1, the reduced radiant flux can be analyzed as a factor in raising the lamp surface temperature.

The color of the light radiated from the cree lamp was yellow and the resin coating lamp was dark red. The color of the infrared lamps colored with the colorant of the present invention was observed as black red (black rose).

Experimental Example 4 Observation of Image of Scanning Electron Microscope

The tissue of the infrared lamp implanted in Example 2 of the present invention was observed by scanning electron microscopy (acceleration voltage is 20 kV and magnified 10,000 times).

The photograph taken is shown in FIG. 2.

As can be seen in FIG. 2, the surface of the infrared lamp coated by the present invention colored in transparent black and red was observed to be clean and with a few nano sized pinholes. When viewed through the light with the naked eye, it was observed to be transparent and free of foreign objects or pinholes.

The infrared lamp colored by the present invention filters visible light of 700 nm or less, which causes eye fatigue and increases stress, and improves thermal effect by increasing infrared transmittance, so that it is not only for poultry farms, pig farms, but also for heating, heating, and medical care. It can be used safely and effectively, and in particular, it is excellent in heat resistance and chemical resistance by heat and chemicals.

Claims (9)

An infrared lamp colorant prepared by combining components including a copper compound (CuO, Cu (OH) ₂ or Cu ₂ O), an aqueous methanol solution, concentrated sulfuric acid, an aqueous solution of silver nitrate (AgNO ₃ ), silicon dioxide (SiO ₂ ) and loess. The method of claim 1, wherein the copper compound (CuO, Cu (OH) ₂ or Cu ₂ O) is 10 to 18% by weight, methanol aqueous solution (80 to 95% by volume) 15 to 40% by weight, concentrated sulfuric acid (95% or more) 18 to 25% by weight silver, aqueous solution of silver nitrate (90 to 110 wt / vol%) 12 to 19% by weight, silicon dioxide (SiO ₂ ) is characterized in that it comprises 10 to 23% by weight and ocher 2 to 8% by weight Infrared lamp colorant. The infrared lamp colorant according to claim 1, wherein the colorant has a viscosity of 1800 ± 200 cP at 23 ° C. and a solid content of 80 ± 5 wt%. The infrared lamp colorant according to claim 1, wherein the particle size of silicon dioxide (SiO ₂ ) is 20 µm or less. Mixing a copper compound (CuO, Cu (OH) ₂ or Cu ₂ O) and silicon dioxide (SiO ₂ ) with an aqueous methanol solution, and then reacting by adding concentrated sulfuric acid; Adding silver nitrate (AgNO ₃ ) aqueous solution to the solution and reacting with stirring; Adding silicon dioxide (SiO ₂ ) and ocher as pigments to the solution; And pulverizing the particles of the colorant slurry solution synthesized above by adding an aqueous methanol solution. The method according to claim 5, wherein the copper compound (CuO, Cu (OH) ₂ or Cu ₂ O) 10 to 18% by weight and silicon dioxide (SiO ₂ ) 9 to 15% by weight of methanol aqueous solution (80 to 95% by volume) 12 to After mixing with 17 wt%, reacting by adding 18-25 wt% of concentrated sulfuric acid (95% or more); Adding 12 to 19 weight% of silver nitrate aqueous solution (90 to 110 wt / vol%) to the solution and reacting with stirring; Adding 1 to 8% by weight of silicon dioxide (SiO ₂ ) and 2 to 8% by weight of ocher as a pigment to the solution; And pulverizing the particles of the colorant slurry solution synthesized above by adding 3 to 23% by weight of an aqueous methanol solution (80 to 95% by volume). The coloring method of the infrared lamp of Claim 1 which apply | coats the coloring agent of Claim 1 to infrared lamp glass, and heats it in the electric furnace maintained at 540-600 degreeC continuously heating up at 6-20 degreeC / min. The method for coloring an infrared lamp according to claim 7, wherein the infrared lamp glass is applied to the colorant by dipping at a rate of 5 to 15 seconds / piece and dried for 15 to 35 minutes under a warm air maintained at 50 to 60 ° C. . 8. The method for coloring an infrared lamp according to claim 7, wherein the heat treatment time is 30 to 90 minutes.

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