JP3353246B2 - Durability test method and test equipment - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a test method and a test apparatus for evaluating the durability of an article and its material, for example, an organic material used outdoors, an article made of the organic material, and an organic material. TECHNICAL FIELD The present invention relates to a test method and a test apparatus used in a test for evaluating the durability of an article or the like coated with a test piece.

[0002]

2. Description of the Related Art As a durability test method for evaluating the durability of an organic material such as a paint, there are a test method of exposing a test piece made of an organic material outdoors (outdoor exposure test) and a method of tracking the sun. There is a test method for exposing the test object to the condensed light (sun tracking condensing exposure test). Further, as another test method, for example, using a sunshine weather meter, ultraviolet carbon weather meter, xenon weather meter, due panel weather meter, metal halide weather meter, and the like, irradiating the test object with light from an artificial light source. There is a test method for accelerating deterioration (accelerated weather resistance deterioration test).

As a method for speeding up a durability test, as disclosed in Japanese Patent Application Laid-Open No. 48-60695, a salt spray test for evaluating corrosion of steel by seawater is used for the test. A method of employing salt water obtained by adding hydrogen peroxide as salt water is disclosed.

[0004]

In the durability test for evaluating the durability by light irradiation or light exposure, it takes a long time such as at least several months to deteriorate the test object. Therefore, the durability test requires a long time. Although the salt spray test described above is intended to speed up the durability test, it is a durability test method in a limited special field of evaluating the corrosion of steel by seawater, and is an organic material, an organic material. It cannot be applied to a durability test for evaluating the weather resistance of an article composed of:

Accordingly, an object of the present invention is a test for evaluating weather resistance of, for example, an organic material, an article made of the organic material, an article coated with the organic material, etc. To significantly reduce the time required for the test.

[0006]

SUMMARY OF THE INVENTION The present invention relates to a durability test method and a durability test apparatus for evaluating the weather resistance of an organic material, an article made of the organic material, an article coated with the organic material, and the like. The durability test method and the durability test apparatus include an organic material, an article made of the organic material, or an organic material.
Hydrogen peroxide, a test piece consisting of an article coated with a material ,
By simultaneously applying an aqueous solution of an oxidizing agent selected from peracids, persalts, hypohalous acids, and hypohalites and light, the deterioration of the test object is promoted and the durability is evaluated. It is a feature.

In the durability test according to the present invention, when the test object is irradiated with light, hydrogen peroxide, peracids, and persalts are applied to the test object.
, Hypohalous acids and hypohalites
Water solutions of the oxidizing agent is intended to act at the same time. What
Hereinafter, in this specification, "hydrogen peroxide, peracids,
Salts, hypohalous acids, and hypohalites
The term “oxidizing agent” is abbreviated as “oxidizing agent” as appropriate. Generally, deterioration of a material is a phenomenon in which the material absorbs light energy to become an active species and reacts chemically with oxygen in the atmosphere to be chemically deteriorated. However, in the durability test according to the present invention, the above-described chemical reaction is performed. Is promoted, deterioration of the test object is remarkably promoted, and the time required for the test of the test object is greatly reduced.

[0008]

[0009] In the durability test method, the test object
As a means for applying a solution of the oxidizing agent, it is preferable to employ a means for contacting water <br/> liquid oxidation agent to the test object. In the durability test method, it is preferable that the test object is immersed in the aqueous solution.

In the durability test method, it is preferable that the aqueous solution is brought into contact with the test object by dropping or spraying. In the durability test method, an oxidizing agent
As a means for allowing the aqueous solution of the oxidizing agent to act, it is also possible to employ a means for causing an aqueous solution of the oxidizing agent to permeate the test object and then causing light to act on the test object at the same time as the oxidizing agent .

[0011]

In durability testing method according to the present invention DETAILED DESCRIPTION OF THE INVENTION As a means for applying a solution of an oxidizing agent to the device to be tested, means for immersing the test object to the aqueous solution, the aqueous solution test object For contacting by dripping or spraying , acid
After the aqueous solution of the agent is allowed to permeate the test object, means for causing light to simultaneously act in the test object can be employed. Upper hexane agent, hydrogen peroxide, peracids, peracid salts, hypohalous acids, is suitably selected from hypohalite salts. Preferred for hydrogen peroxide among its causes further promote degradation.

In order to carry out these durability test methods,
As a means for applying light to the device under test, a wavelength of 400 nm
A light source including the following light can be employed.A container for accommodating the test object and an acid
It is possible to use a durability test apparatus provided with a means for applying an aqueous solution of the agent and a means for applying light. In general, outdoor deterioration of a material is a phenomenon in which the material absorbs light energy to become an active species, and reacts with oxygen in the atmosphere to chemically deteriorate. In the present invention, the test object, by the action of an aqueous solution of the oxidizing agent to the irradiation and simultaneous light, and promote chemical reactions described above, but to reproduce the deterioration of outdoor materials at high accelerator magnification is there.

[0013]

[0014]

[0015] In the durability test according to the present invention, the acid agent, preferably be used, in particular hydrogen peroxide
Ku, as the concentration of the water solution is effective in the range of 0.001 wt% to 60 wt%, more preferably in the range of 0.01 wt% to 10 wt%. The concentration of hydrogen peroxide is 0.
When the amount is less than 001% by weight, the effect of the present invention cannot be exhibited due to a low rate of promotion of deterioration.
If the concentration of hydrogen peroxide exceeds 60% by weight , the deterioration will be too fast to stop the deterioration under appropriate processing conditions, and the accuracy of the test will be reduced. When the concentration is in the range of 0.01 % by weight to 10% by weight , the reproducibility of the test is ensured and the test with improved accuracy can be performed in a short time.

[0016] In the durability test according to the present invention, if the hydrogen peroxide is employed as an acid agent, for use in contact with the test object hydrogen peroxide as an aqueous solution, the temperature of the test object is 0
It is preferable that the temperature is from 120C to 120C. When the temperature of the test object is lower than 0 ° C., the effect of the present invention cannot be exhibited due to a low rate of acceleration of deterioration, and when the temperature of the test object is higher than 120 ° C., In some cases, chemical reactions that cannot occur outdoors may occur and the intended test purpose may not be achieved.

In the durability test according to the present invention , the oxidizing agent
The light that acts with the aqueous solution is not particularly limited as long as it has energy for activating the material constituting the test object. However, since many industrially important materials interact with light having a wavelength of 400 nm or less, 400n wavelength
It is preferable to include light of m or less. In the durability test according to the present invention, all the light sources used in the conventional weather resistance deterioration test can be adopted. Specifically, in addition to sunlight, xenon lamps, metal halide lamps, carbon arcs, light generated from artificial light sources such as ultraviolet fluorescent lamps alone or in combination of these lights can be used. Can be used in combination.

[0018]

(Example 1) A steel plate (7 cm) was used as a test object.
A coated plate prepared by applying electrodeposition, intermediate coating, and overcoating (white solid) coating on (× 15 cm × 0.8 mm).
0.5 g of sodium hypochlorite (hexahydrate: a reagent manufactured by Wako Pure Chemical Industries), which is a liquid substance, is uniformly applied to the painted surface of this painted plate, and is left in a thermostat set at 40 ° C. And about 6
Light from an ultraviolet fluorescent lamp was irradiated for 10 hours from a distance of 0 mm. An optical filter made of glass was provided between the coated plate as a test object and the fluorescent lamp, and the wavelength of light reaching the coated plate was adjusted to be in a range of 295 nm to 400 nm.

The coated plate is washed with water and dried after light irradiation, and a gloss meter GM-3D (manufactured by Murakami Color Research Laboratory)
The gloss was measured at 60 °. The 60-degree gloss immediately after preparation of the coated plate was 94, and the 60-degree gloss after light irradiation under the above conditions was 75. (Comparative Example 1) Using a coated plate prepared in the same manner as the coated plate of Example 1 as a test object, the plurality of coated plates were allowed to stand still in a thermostat set at 40 ° C, and the same as in Example 1. Under the conditions described above, light from an ultraviolet fluorescent lamp was irradiated for 1000 hours. During this time, each of the coated plates was taken out at an appropriate light irradiation time, washed with water and dried, and the gloss at 60 ° was measured as in Example 1. The 60-degree gloss of each coated plate had the same value as the 60-degree gloss 94 immediately after preparation and did not change until the irradiation time was up to 1000 hours. (Example 2) A coated plate (3.5 cm x 15 cm x 0.8 mm) prepared in the same manner as the coated plate of Example 1 was used as a test object, and 30 wt. % Reagent (manufactured by Wako Pure Chemical Industries, Ltd.) diluted with ion-exchanged water.
wt. Approximately 150 ml of a hydrogen peroxide solution in a cylindrical quartz glass container (diameter: 43 mm, height: 200 mm, thickness: 2 m)
m) and sealed with silicone rubber. A plurality of containers in this state were prepared, and these containers were arranged in a constant temperature bath set at 40 ° C. so that the coating surface of the coating plate faced the front with respect to the light source. Under similar conditions, about 60
Light from an ultraviolet fluorescent lamp was applied from a distance of mm.

During the light irradiation time up to 100 hours, each of the coated plates was taken out at an appropriate light irradiation time, washed and dried, and the gloss at 60 ° was measured as in Example 1. The 60-degree gloss immediately after preparation of each coated plate was 94, and 1
The 60-degree gloss of the coated plate irradiated with light for 00 hours was 5.
The 60-degree gloss of the coated plate taken out during each irradiation time during this period is as shown in FIG. (Comparative Example 2) A painted plate similar to the painted plate of Example 2 (3.5
cm × 15cm × 0.8mm) and about 150 ion-exchanged water
ml was placed in a cylindrical quartz glass container (diameter 43 mm, height 200 mm, thickness 2 mm) and sealed with silicone rubber. A plurality of containers in this state were irradiated with light from an ultraviolet fluorescent lamp from a distance of about 60 mm under the same conditions as in Example 2 in a thermostat set at 40 ° C., as in Example 2. The 60 ° gloss of the coated plate taken out at every irradiation time was measured. The 60-degree gloss of the coated plate was the same as the 60-degree gloss 94 immediately after the preparation of each coated plate and did not change at all up to the irradiation time of 300 hours. (Example 3) 3 wt. % Aqueous hydrogen peroxide instead of 1 wt. %, Except that an aqueous sodium peroxocarbonate solution was used.
The 0 degree gloss was measured. FIG. 2 shows the obtained results. (Example 4) A plurality of painted plates prepared in the same manner as the painted plate of Example 1 were used as test pieces and subjected to a deterioration test using a sunshine weather meter (manufactured by Suga Test Machine). In this experiment, a test was conducted under the same conditions as in Example 2 except that 0.01 wt% hydrogen peroxide solution prepared in the same manner as in Example 2 was used instead of the high-purity water used for the water load by spraying. In the same manner as described above, 6
The 0 degree gloss was measured. The 60-degree gloss immediately after the preparation of each coated plate was 94, and the 60-degree gloss of the coated plate after a test time of 500 hours was 51. FIG. 3 shows the 60-degree gloss of the coated plate during each test time during this period. (Comparative Example 3) Using a plurality of painted plates prepared in the same manner as the painted plate of Example 1 as a test object, using the sunshine weather meter used in Example 4, all tests were performed under normal conditions. As in Example 4, the 60-degree gloss of each coated plate was measured. The 60-degree gloss immediately after the preparation of each coated plate was 94, and the 60-degree gloss of the coated plate after a test time of 1000 hours was 9
It was one. During this period, 6 times of painted plate
The 0 degree gloss is shown in FIG. (Example 5) A coated plate prepared in the same manner as the coated plate of Example 1 was used as a test object, and the 30 wt.
% Hydrogen peroxide solution at 20 ° C. for 30 minutes, during which no light was applied. Thereafter, the coated plate was taken out of the hydrogen peroxide solution and immediately washed with water for 5 seconds.
It was left standing in a thermostat at 0 ° C., and irradiated with light from an ultraviolet fluorescent lamp for 10 hours from a distance of about 60 mm, and the 60 ° gloss of the coated plate after the irradiation was measured. The 60 degree gloss immediately after preparation of the coated plate was 94, and the 60 degree gloss after irradiation was 88. (Comparative Example 4) Using a coated plate prepared in the same manner as the coated plate of Example 1 as an object to be tested, an outdoor exposure test was performed in Okinawa for up to 24 months. The 60 degree gloss of the coated plate was measured. 6 immediately after preparation of painted plate
The 0 degree gloss was 94, and the 60 degree gloss 24 months after the exposure test was 67. FIG. 5 shows the 60-degree gloss of the coated plate for each exposure time during this period.

(Embodiment 1 of Test Apparatus) FIG. 6 illustrates an apparatus that can easily implement the present invention. DUT is UV irradiation through the walls of the optical filter and the quartz glass container while being immersed in an aqueous solution of an acid agent. Since the above quartz glass container is installed in a thermostat, the test object is maintained at a predetermined temperature.

(Embodiment 2 of Test Apparatus) FIG. 7 shows another embodiment of the test apparatus for suitably executing the durability test according to the present invention. The test apparatus includes a casing 11, a liquid tank 1
2, a supporting mechanism 13 and a light source 14, and the inside of the casing 11 is configured to function as a thermostat. The liquid tank 12 is disposed at the bottom in the casing 11, the support mechanism 13 is disposed at a central portion in the casing 11 so as to be rotatable about a horizontal axis, and the light source 14 is disposed inside the casing 11. 13 is disposed at the center of rotation.

The liquid tank 12 is intended to accommodate the aqueous solution of an acid agent, the support mechanism 13 is located in central casing 11, during rotation, the aqueous solution of the partially liquid tank 12 of the lower end portion They are arranged so as to be sequentially immersed. The support mechanism 13 is a cylindrical cage-type rotating body, and the inside of the cylindrical shape is configured such that the device under test 15 is attached to face the center of rotation. The light source 14 is located at the center of rotation in the casing 11, and faces the front surface of all the test pieces 15 mounted in the support mechanism 13.

In the test apparatus, the support mechanism 13
A rotation mechanism around the horizontal axis is rotated at a constant speed by a drive mechanism (not shown), and the rotation speed can be adjusted within a range of 1 to 100 rotations / hour. For this reason, each DUT 15 rotates at a predetermined speed in a constant temperature bath while being attached to the support mechanism 13, and during this time, each DUT 15 intermittently contacts the aqueous solution in the liquid tank 12. Immersion is repeated, and is constantly exposed to light emitted from the light source 14.

As a result, while each test object 15 is immersed in the aqueous solution, escapes from the liquid tank 12 and is wet with the aqueous solution, the water evaporates and the aqueous solution of the oxidizing agent is concentrated, and each test object 15 is concentrated. Since light irradiation is performed in all states before contacting with or penetrating into the surface of the test body 15 and before being immersed in the aqueous solution, and the light irradiation state is repeatedly received, each test object The deterioration of the body 15 is efficiently promoted. (Consideration) Referring to Example 1 and Comparative Example 1, by applying an aqueous solution of an oxidizing agent to a coated plate as a test object, deterioration of the coating film due to light is promoted, and decrease in gloss of the coated plate is short. It can be seen that it is reproduced in time. Example 2 and Example 3
Referring to Comparative Example 2 and, by immersing the coated plate is tested body in an aqueous solution of an acid agent, it can be seen that the reduction in the gloss of the coated plate is reproduced in a short time.

Referring to Comparative Example 3 and Example 4, by contacting with spraying an aqueous solution of an acid agent to the coated plate is the test object, that reduction in the gloss of the coated plate is reproduced in a short time Understand. This result makes it possible to apply the present invention to the conventional accelerated weathering test, thereby increasing the deterioration promotion rate and increasing the usefulness.

Comparative Example 4 is an exposure test in which the coated plate, which is the test object of each example, is exposed outdoors and deteriorated. The time required for the 60-degree gloss of the coated plate to be reduced to 90 is 12 months in the exposure test, whereas 8 hours in Example 2, 12 hours in Example 3, and 160 hours in Example 4.
The time is 1000 hours in Comparative Example 3. Therefore, the deterioration promotion magnifications of the respective examples for the exposure test were 1100 times, 730 times, and 55 times, respectively, and Comparative Example 3
Is 8.8 times. Considering these degradation promotion factors, it can be understood that the promotion of degradation in each embodiment of the present invention is extremely excellent.

[Brief description of the drawings]

FIG. 1 is a graph showing a relationship between light irradiation time and 60-degree gloss in Example 2 of the present invention.

FIG. 2 is a graph showing a relationship between light irradiation time and 60-degree gloss in Example 3.

FIG. 3 is a graph showing a relationship between test time and 60-degree gloss in Example 4.

FIG. 4 is a graph showing the relationship between test time and 60-degree gloss in Comparative Example 3 of the present invention.

FIG. 5 is a graph showing the relationship between outdoor exposure time and 60-degree gloss in Comparative Example 4.

FIG. 6 is a schematic configuration diagram showing a durability test apparatus according to an example of the present invention.

FIG. 7 is a schematic configuration diagram illustrating a durability test apparatus according to an example of the present invention.

[Explanation of symbols]

11 ... constant temperature bath, an aqueous solution of 12 ... oxidation agent, 13 ... a quartz glass container, 14 ... light source, 15 ... device to be tested, 21 ... casing, 22 ... liquid tank, 23 ... supporting mechanism, 24 ... light source, 25 ...
DUT.

──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-9-119893 (JP, A) JP-A-48-60695 (JP, A) JP-A-63-222240 (JP, A) JP-A 64-64 66542 (JP, A) JP-A-4-138338 (JP, A) JP-A-1-277738 (JP, A) JP-B 1-28897 (JP, B2) JP-B 2-1259 (JP, B2) Weathering (light) resistance of elastomers-The first joint research report-, Musashino Create, July 3, 1994, p. 21-23 (58) Field surveyed (Int. Cl. ⁷ , DB name) G01N 17/00 JICST file (JOIS)

Claims (4)

(57) [Claims] An organic material, an article comprising the organic material or
Simultaneously applying light and an aqueous solution of an oxidizing agent selected from hydrogen peroxide, peracids, persalts, hypohalous acids, and hypohalous salts to a test object composed of an article coated with the organic material. A durability test method characterized in that deterioration of a test object is promoted to evaluate durability. 2. The durability test method according to claim 1, wherein the means for applying light to the device under test has a wavelength of 400.
A durability test method, which employs a light source containing light of nm or less. 3. The durability test method according to claim 1, wherein the aqueous solution of the oxidizing agent is applied to the test object by using a hydrogen peroxide aqueous solution having a concentration of 0.001 to 60% by weight. A durability test method characterized by contacting with a test piece. 4. An organic material, an article comprising the organic material or
Simultaneously applying light and an aqueous solution of an oxidizing agent selected from hydrogen peroxide, peracids, persalts, hypohalous acids, and hypohalous salts to a test object composed of an article coated with the organic material. A durability test apparatus for performing a durability test for evaluating the durability by accelerating the deterioration of the test object by using a container accommodating the test object and the test object accommodated in the container. Means for applying an aqueous solution of the agent;
A durability test apparatus comprising means for applying light.