JP3351747B2 - 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. The present invention relates to a durability test method and a test apparatus employed for a test for evaluating the weather resistance 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). In addition, as a special test method, for example, sunshine weather meter, ultraviolet carbon weather meter, xenon weather meter,
A test method for accelerating deterioration by irradiating light from an artificial light source to the test object using a Dew panel weather meter, a metal halide weather meter, or the like (accelerated weathering deterioration test)
There is.

[0003]

However, in the above-mentioned methods for evaluating the durability by the outdoor exposure test and the sun tracking light exposure test, it takes a long time such as at least several months to deteriorate the test object. Since it is necessary and the durability test requires a long time, it is impossible to quickly evaluate the durability.

In the method for evaluating durability by the accelerated weathering deterioration test described above, the deterioration state of the test object does not match the outdoor deterioration state of articles, materials, etc. There is a problem that it cannot be reproduced sufficiently. In the case of outdoor deterioration of articles, materials, and the like, the fine morphology of the surface includes a mixture of minute undulations and minute holes in a typical coating film. On the other hand, in the accelerated weathering deterioration test described above, the surface exhibits a fine shape mainly composed of minute undulations to reduce gloss, and cannot reproduce a fine form of outdoor deterioration.

It is therefore an object of the present invention is, for example, a test method for evaluating an organic material, an article made of organic material, the weather resistance of the article or the like which is coated with organic material, such organic
Machine material, an article made of the organic material, or the organic material.
An object of the present invention is to accelerate the deterioration of a test object made of a covered article at a high speed magnification and sufficiently reproduce outdoor deterioration.

[0006]

SUMMARY OF THE INVENTION The present invention relates to a durability test method and a durability test apparatus for evaluating 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 may be an organic material, an article made of the organic material, or the organic material.
First step of allowing an aqueous solution of an oxidizing agent other than oxygen and ozone and light to act on a test object made of an article coated with a material substantially simultaneously, and applying one or more of water, oxygen and light to the test object. And the second step of operating substantially simultaneously when a plurality of these are operated is performed sequentially and / or alternately. here
Thus, the present invention relates to an organic material,
The weather resistance of such articles, articles coated with the organic material, etc.
A durability test method and a durability test apparatus to be evaluated.
Hereinafter, in this specification, an organic material, comprising the organic material
Test object consisting of an article or an article coated with the organic material
The body is simply abbreviated as a test object.

In the durability test method according to the present invention,
The oxidizing agent in the first step can be appropriately selected from hydrogen peroxide, ozone, peracids, persalts, hypohalous acids, hypohalous salts, and chlorine. Preferably, hydrogen is employed.
In the durability test method according to the present invention, in the second step, a means for immersing in hot water, a means for irradiating light in a gas containing water vapor and oxygen, a means for exposing outdoors, and the like can be employed. In addition, sunlight and artificial light sources can be used as the light sources in the first and second steps.

[0008] These durability testing methods include a container for accommodating a test object, a means for allowing an aqueous solution of an oxidizing agent and light to act on the test object at substantially the same time, and applying water, oxygen and light to the test object. In the case where one or a plurality of these elements act, and when a plurality of these elements act, it can be suitably carried out by a durability test apparatus provided with means for causing them to act substantially simultaneously.

[0009]

In the durability test and the durability test apparatus according to the present invention, a first step of causing an aqueous solution of an oxidizing agent and light to act on a test object at substantially the same time; And one or more of water, oxygen, and light, and the second step of causing the two or more to act substantially simultaneously is performed sequentially and / or alternately.

[0010] In the case of deterioration of a paint film or the like outdoors, minute holes and undulations generally occur on the surface. Of the above steps, in the first step, the action of the oxidizing agent aqueous solution and the light causes microscopic holes on the surface to promote deterioration. For example, the resin is lost due to an oxidation reaction around the pigment due to the photocatalysis of a certain pigment in the coating film, and a fine hole is formed to accelerate the deterioration.

Further, in the second step, a slight undulation is generated on the surface, and the deterioration can be promoted. That is, when water is applied, a part of the coating film or the like is transformed into a low-molecular substance by hydrolysis with water, is lost by extraction or volatilization, and the coating film or the like shrinks to generate a slight undulation on the surface. Deterioration is promoted. When light is applied, a low-molecular substance is generated by an oxidation reaction involving light, and is lost by extraction and volatilization in the same manner as described above. When oxygen is applied, a low molecular weight substance is generated by the oxidation reaction, and a slight swell is generated as described above. In the present invention, the first
By combining the steps (1) and (2), microholes and undulations similar to those in the outdoors are generated together to promote the degradation, so that the degradation in the outdoors can be reproduced.

In general, outdoor deterioration of articles and materials (hereinafter referred to as materials, etc.) is a phenomenon that occurs when materials and the like are chemically altered by the action of water, oxygen, and light in the environment. Among these actions, the action involving water is to transform a part of the material or the like by the hydrolysis reaction into a low molecular substance, and to extract and volatilize the low molecular substance from the surface of the material. When the material or the like undergoes alteration to a low-molecular substance, and extraction or volatilization of the low-molecular substance from the surface occurs, fine undulations occur on the surface of the material or the like due to these phenomena. For example,
When the material is a painted article, a coating material, when the above-mentioned alteration, extraction, and volatilization occur, the resin portion excluding the pigment shrinks, and as a result, a fine undulation occurs on the surface of the coating film. Surface gloss is reduced.

[0013] The action involving light is to impart light energy to the material or the like to make the material or the like an active species, and to react the material or the like with oxygen in the atmosphere to generate various chemical bonds; and / or To be cut off. As a result, a part of the material or the like is transformed into a low-molecular substance, and the low-molecular substance is extracted and volatilized from the surface of the material.

In the action involving light, for example, in the case of a painted article or a coating material, some pigments have a photocatalytic action. May occur. One of the features of the fine morphology in this case is that the resin around the pigment near the surface of the coating film is lost and fine holes are formed on the coating film surface. This morphological change reduces the gloss of the coating film, as well as minute undulations.

Observation of the fine morphology of the surface of the coating film deteriorated outdoors reveals that fine undulations and fine holes are usually mixed.
It is recognized that the above-described action of generating both the fine undulations and the fine holes is provided. Therefore, in order to promote and reproduce the degradation that occurs outdoors, one or both of the effects of generating minute undulations due to water or light,
It is necessary to accelerate both the action of generating a minute hole by light. In this respect, the above-mentioned conventional accelerated weathering deterioration test cannot reproduce the deterioration effect outdoors, and is not a sufficient test intended to reproduce the deterioration outdoors.

On the other hand, the durability test according to the present invention promotes deterioration that cannot be reproduced by the conventional accelerated weathering deterioration test, and accurately balances the various actions described above, thereby making it possible to perform outdoor deterioration. And reproduces and promotes the same deterioration. In the durability test according to the present invention, for example, the fine morphology of the surface of the coating film deteriorated outdoors is promoted and reproduced.

[0017]

DESCRIPTION OF THE PREFERRED EMBODIMENTS A durability test according to the present invention is a first test.
And a second step. The first step is to apply an aqueous solution of an oxidizing agent and light to the test object substantially simultaneously, and the second step is to apply water, oxygen and One or more of the light is applied, and when these are applied, the light is applied substantially simultaneously.
Is to carry out these sequentially and / or alternately.

Specifically, if the first step and the second step are referred to as an A step and a B step, the order of execution of each step is as follows.
AB, BA, ABAB ..., AB1-B2-A
-B1-B2 ... etc. can be adopted. However,
B1 and B2 mean B processes having different contents.
Hereinafter, the first step and the second step in the durability test according to the present invention may be referred to as an A step and a B step.

The step A is a step in which an aqueous solution of an oxidizing agent and light are allowed to act on the test object at substantially the same time, and among the deterioration effects involving light, the deterioration that produces fine holes is promoted and reproduced. . In this step, the oxidizing agent can be appropriately selected from hydrogen peroxide, ozone, peracids, persalts, hypohalous acids, hypohalous salts, and chlorine. An oxidizing agent can also be employed.
Each selected oxidizing agent is used in the form of an aqueous solution, and is used in the method of immersing the test object in the above-mentioned aqueous solution, and in the method of dropping or spraying the above-mentioned aqueous solution on the surface of the test object to flow down the surface of the test object it can. Alternatively, each oxidizing agent can be made to act substantially simultaneously by irradiating each oxidizing agent from the aqueous solution to the test object by the above-described method and irradiating light with the aqueous solution removed.

The deterioration caused in the test object in the step A is, for example, when the test object is a painted object, mainly causes a phenomenon in which fine holes are formed on the surface of the coating film. The main reaction is an oxidation reaction caused by acting simultaneously. In this oxidation reaction, depending on the type of the oxidizing agent employed, the oxygen element may be bonded to the test object, or an element other than the oxygen element may be bonded to the test object. In general, oxidation due to deterioration occurring when an organic material or the like is used outdoors is oxidation in which an oxygen element is bonded. Therefore, in order to reproduce deterioration occurring outdoors, an oxidation reaction involving the oxygen element must be performed. Need to occur.

When an oxidizing agent which causes an oxidation reaction involving an oxygen element is employed in the step A, the oxidation reaction by oxygen can be caused only in the step A. When such an oxidizing agent is not used in the step A, the oxidation reaction by oxygen cannot be caused only in the step A, but the content of the step B following the step A must be set appropriately. Thereby, the element can be replaced to cause an oxidation reaction by oxygen. In this case, the step B needs to have at least means for causing oxygen to act.

In step B, one or more of water, oxygen, and light are applied to the test object. When a plurality of these are applied, they are applied substantially simultaneously. As the B step, specifically, B1 treatment, B2 treatment,
B3 processing, B4 processing, B5 processing, B6 processing and the like can be mentioned. In each of these treatments, B1 treatment: treatment of immersing the test object in warm water B2 treatment: treatment of irradiating light while immersing the test object in warm water B3 treatment: oxygen partial pressure of 0.2 atm or more as warm water of B2 treatment Treatment using water containing dissolved oxygen in equilibrium with B4 treatment: treatment of irradiating the test object with light in a gas containing water vapor B5 treatment: B4 treatment is carried out by including oxygen of 0.2 atm or more in the gas. Treatment B6 treatment: A treatment for performing one of the conventional weathering deterioration tests including water as a load factor. As the weather resistance deterioration test according to the prior art, an outdoor exposure test, a sun tracking light exposure test, and various accelerated weather resistance deterioration tests using an artificial light source can be used.

The light employed in the steps A and B is not particularly limited as long as it has energy for activating the material constituting the device under test, but most industrially important materials have a wavelength of 400 nm or less. It preferably contains light having a wavelength of 400 nm or less, since the light interacts with the light having the wavelength of 400 nm. 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 halides, carbon arcs, light generated from artificial light sources such as ultraviolet fluorescent lamps alone, and these lights can be used in combination. An optical filter can be used in combination.

In the step B, when an artificial environment is used, the temperature of the test object is in the range of 0 to 120 ° C. When the temperature of the test object is lower than 0 ° C., the intended effect of the present invention cannot be obtained because the deterioration promoting magnification is low, and when the temperature of the test object is higher than 120 ° C. Therefore, the intended effect of the present invention cannot be obtained because a chemical reaction that does not occur occurs.

The deterioration caused in the test object by the step B mainly causes a phenomenon that a minute undulation is generated on the surface of the coating film when the test object is a painted object. The B step includes various kinds of processing such as B1 processing to B6 processing,
In performing the durability test according to the present invention, in selecting a combination of the process A and the process B, it is not necessary to select the process B, which can achieve the same effect in the selected process A.

The test apparatus of the present invention comprises a container for accommodating a test object, means for causing an aqueous solution of an oxidizing agent and light to act on the test object at substantially the same time, and applying water, oxygen and light to the test object. When one or a plurality of them are operated, and when a plurality of these are operated, it is realized by a configuration including means for operating substantially simultaneously. The container accommodating the test object is a translucent material when irradiating light through the container wall, and particularly preferably a material that transmits ultraviolet light when a light source including ultraviolet light is used. In this case, a suitable material is quartz glass.

As a means for causing the test object to be exposed to the aqueous solution of the oxidizing agent and the light at the same time, irradiating the test object with the light from a light source in a state where the test object is immersed in the aqueous solution of the oxidizing agent. Can be At this time, in order to adjust the deterioration rate of the test object, it is preferable to have a function of keeping the temperature in the container constant. In order to keep the temperature in the container constant, it is effective to provide a temperature control device.

As the light source, sunlight or an artificial light source can be used. When an artificial light source is used, it is preferable to incorporate this into the device. As the artificial light source, a light source used in an existing accelerated weathering tester such as a xenon lamp, a metal halide lamp, and an ultraviolet fluorescent lamp can be used. In order to adjust the spectral distribution of light from these light sources, it is advantageous to provide an appropriate optical filter between the light source and the device under test.

Means for allowing one or more of water, oxygen and light to act on the test object, and when applying a plurality of these, substantially simultaneously, include outdoor exposure and sun-tracking condensing exposure according to existing technologies. Even if various accelerated weathering tests using artificial light sources are used, the aqueous solution of the oxidizing agent and the aqueous solution of the oxidizing agent in the means for causing light to act on the test object substantially simultaneously are pure water and air containing steam. Means replaced with the above may be used.

Next, the configuration of the apparatus will be described more specifically.
The test object is placed in a quartz glass container and placed in a thermostat. One surface of the wall of the water bath is made of quartz glass or a glass plate that also serves as an appropriate optical filter, and an artificial light source selected from a xenon lamp, a metal halide lamp, an ultraviolet fluorescent lamp, and the like is passed through the glass plate and a wall made of quartz glass. The test object is irradiated with light.

At the bottom of the quartz glass container, an opening and a reciprocating pipe leading to the outside of the constant temperature bath are provided so that a liquid or a gas can be introduced into the inside thereof.
It is connected to a device that introduces various liquids or gases into a quartz glass container according to the test time program. In the process to be introduced into the quartz glass container, hydrogen peroxide water can be used in the process A, and pure water or air adjusted to a constant temperature and humidity in the process B, or a special mixed gas with a higher oxygen partial pressure than air can be used in the process B Can be used. The test is performed automatically by the device according to a preset time program.

[0032]

EXAMPLES AND COMPARATIVE EXAMPLES The durability test method according to the present invention,
Examples and comparative examples of the present invention will be described in order to explain the test apparatus and the test apparatus in more detail. However, the present invention is not limited to only these examples. In the following examples and comparative examples, when an aqueous solution of hydrogen peroxide (hereinafter referred to as hydrogen peroxide solution) is employed as the aqueous solution of the oxidizing agent, the aqueous solution is a hydrogen peroxide reagent (concentration of 3).
(0% by weight: manufactured by Wako Pure Chemical Industries, Ltd.) with ion-exchanged water and adjusted to a predetermined concentration. Example 1 A steel plate (7 cm × 15 cm) was used as a test object.
× 0.8 mm), and a coated plate prepared by applying electrodeposition, intermediate coating, and top coating (white solid) was adopted. The coated plate was subjected to an outdoor exposure test according to the method specified in JISZ2381. However, in this outdoor exposure test,
The surface of the coated plate being exposed is repeatedly sprayed with a 0.1% by weight aqueous solution of hydrogen peroxide once a day at noon for 10 seconds to wet the entire surface of the coated plate with the same hydrogen peroxide solution. went.

By this operation, part of the hydrogen peroxide penetrates into the interior of the coated plate and acts substantially simultaneously with sunlight. The outdoor exposure test was performed in Aichi Prefecture from May to six months. After completion of the outdoor exposure test, the painted plate is washed with water and dried, and a gloss meter GM-3D (manufactured by Murakami Color Research Laboratory)
And the fine morphology of the surface of the coated plate was measured with a scanning electron microscope (JSM-89 manufactured by JEOL Ltd.).
0 type).

The 60-degree gloss immediately after preparation of the coated plate was 94, and the 60-degree gloss after completion of the outdoor exposure test under the above conditions was 75. In addition, in the observation of the fine morphology of the surface of the coated plate with a scanning electron microscope, fine undulations and fine holes were confirmed on the surface of the coated plate, which coincided with the morphology characteristic of outdoor degradation. (Comparative Example 1) A plurality of painted plates were prepared according to JISZ23 using a painted plate prepared in the same manner as the painted plate of Example 1 as a test object.
Subject to the outdoor exposure test according to the method specified in 81, while measuring the 60-degree gloss of the coated plate for each test period,
The fine morphology of the surface of the coated plate was observed with a scanning electron microscope.

The 60-degree gloss of the coated plate after exposure for the same period as in Example 1 is not substantially different from the 60-degree gloss 94 immediately after its preparation, and the fine morphology of the surface of the coated plate. No changes were observed. The coated plate after the outdoor exposure test after 3 years had a gloss of 60 degrees of 80, and it was confirmed that minute undulations and small holes were mixed on the surface of the coated plate. (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 the coated plate was immersed in warm water at 80 ° C for 24 hours. A cylindrical quartz glass container (diameter 43 mm, height 200 mm,
(2 mm thick) and sealed with a silicone rubber stopper. A plurality of containers in this state are prepared, and these containers are kept at 40 ° C.
Was placed upright so that the painted surface of the painted plate faced the front with respect to the light source, and irradiated with ultraviolet fluorescent light from a distance of about 60 mm.

In this embodiment, a glass light filter (filter glass) is provided between the quartz glass container and the fluorescent lamp.
Is installed, and the wavelength of light reaching the painted plate is 295nm ~
It was adjusted to be in the range of 400 nm. During this time, each of the coated plates was taken out at an appropriate light irradiation time, and the gloss at 60 degrees was measured in the same manner as in Example 1, and the fine morphology of the surface of the coated plate after the light irradiation time of 50 hours was observed. .
The 60 degree gloss immediately after preparation of each coated plate was 94, and the 60 degree gloss after light irradiation for 50 hours was 40. The 60-degree gloss after light irradiation for each irradiation time during this period is as shown in FIG. Regarding the fine morphology of the surface of the coated plate after 50 hours of light irradiation time, it was confirmed that minute undulations and fine holes were mixed on the surface of the coated plate, which coincided with the characteristic morphology of outdoor deterioration. . (Comparative Example 2) A painted plate similar to the painted plate of Example 2 (3.5
(cm × 15 cm × 0.8 mm) as a test object, immersed the coated plate in hot water of 80 ° C.
ml quartz glass container (diameter 43 mm,
(Height: 200 mm, thickness: 2 mm) and sealed with a silicone rubber stopper. A plurality of containers in this state are placed in a thermostat set at 40 ° C. for approximately 60 m under the same conditions as in Example 2.
Example 2 Irradiation with ultraviolet fluorescent light from a distance of m
Similarly to the above, the 60-degree gloss after light irradiation for each irradiation time was measured, and the fine morphology of the surface of the coated plate after 50 hours of light irradiation time was observed.

The 60-degree gloss immediately after the preparation of each coated plate was 94, and the 60-degree gloss after light irradiation for 50 hours was 89.
As for the fine morphology of the surface of the coated plate after 50 hours of light irradiation, slight undulations were slightly observed on the surface of the coated plate, but fine holes characteristic of outdoor deterioration were not recognized. (Comparative Example 3) A painted plate similar to the painted plate of Example 2 (3.5
cm × 15 cm × 0.8 mm), and a durability test was performed under the same conditions as in Example 2 except that the immersion of the coated plate in hot water at 80 ° C. was omitted. The subsequent 60 degree gloss was measured and the fine morphology of the surface of the coated plate was observed. The 60 degree gloss immediately after preparation of the coated plate was 94, and the 60 degree gloss after light irradiation for 50 hours was 58. Regarding the fine morphology of the surface of the coated plate, fine holes characteristic of outdoor deterioration were recognized on the surface of the coated plate, but fine undulation, which is another characteristic, was not recognized. (Example 3) A coated plate similar to the coated plate of Example 1 (3.5
cm × 15 cm × 0.8 mm) as a test object, and the following three kinds of treatments, treatment 1 and treatment 2 were performed on the coated plate.
And Process 3 were sequentially and repeatedly performed. Each treatment was as follows: Treatment 1: immersing the coated plate in deionized water at 60 ° C. for 6 hours Treatment 2: placing the coated plate in a quartz glass container in the same manner as in Example 2, and adding 0.5% by weight of hydrogen peroxide solution Approximately 150 ml, sealed with a silicone rubber stopper, and kept at 60 ° C. and irradiated with ultraviolet fluorescent light for 3 hours. Treatment 3: Remove the hydrogen peroxide solution from the quartz glass container of Treatment 2 and rinse with deionized water After that, about 2 ml of deionized water was left in the container, the container was sealed again with a silicone rubber stopper, and the light of an ultraviolet fluorescent lamp was irradiated at 60 ° C. for 15 hours in the same manner as in Treatment 2.

Process 1 is the first B step. As shown in process 1 of FIG. 2, the coated plate is immersed in deionized water in a constant temperature water bath maintained at 60 ° C. The process 2 is the step A. As shown in the process 2 in FIG. 2, specifically, a coated glass plate and a quartz glass container containing a hydrogen peroxide solution are put in a thermostat maintained at 60 ° C. One surface of the wall surface of the constant temperature bath is a filter glass, and light from an ultraviolet fluorescent lamp is irradiated through this surface.

Process 3 is a second B-fixed process, as shown in Process 3 in FIG. 2, in which the same apparatus as in Process 2 is used, but the inside of the quartz glass container is made to have a high humidity air atmosphere. Performing the above-described processes 1, 2, and 3 in this order as one cycle is repeated 5 cycles, and the 60-degree gloss is measured at the end of each cycle by the same means as in the first embodiment. At the same time, the fine morphology of the surface of the coated plate at the completion of 5 cycles was observed. FIG. 2 shows the outline of the apparatus used in this example and the entire processing sequence, and FIG. 3 shows the 60-degree gloss for each cycle.

The 60-degree gloss immediately after the preparation of each coated plate was 94, and after the completion of 5 cycles, the 60-degree gloss was 30. Regarding the fine morphology of the surface of the coated plate, a slight undulation was observed on the surface of the coated plate. It was confirmed that minute holes were present, which was consistent with the characteristic of outdoor deterioration. (Example 4) A sunshine weather meter (manufactured by Suga Test Instruments) was modified to add a set of sprays installed to load high-purity water, and a coating plate similar to the coating plate of Example 1 (3. 5cm × 15cm × 0.8m
m) was used as a test sample, and the durability test was carried out by mounting this coated plate with such a modified apparatus in accordance with a standard test order in a sunshine weather meter.

The test conditions were the standard conditions for a sunshine weather meter, but prior to loading with high-purity water, a concentration of 0.0% was applied for 10 minutes from an additional spray device.
A step of loading 1% by weight aqueous hydrogen peroxide with light was added. The coated plate was taken out at every elapse of a predetermined test time, the gloss was measured at 60 degrees by the same means as in Example 1, and the fine morphology of the surface of the coated plate after 500 hours of the test time was observed. FIG. 4 shows the 60-degree gloss of the coated plate at each elapse of the test time.

The 60-degree gloss immediately after the preparation of each coated plate was 94, and the 60-degree gloss after a test time of 500 hours was 52. In addition, regarding the fine morphology of the surface of the coated plate after the elapse of the test time of 500 hours, it was confirmed that minute undulations and fine holes were mixed on the surface of the coated plate, and the characteristic morphology of outdoor deterioration was confirmed. Matched. (Comparative Example 4) A painted plate similar to the painted plate of Example 1 (3.5
cm × 15 cm × 0.8 mm) as a test object, and using the coated plate with the sunshine weathermeter used in Example 4, a durability test was performed for 1200 hours under all normal conditions in the sunshine weathermeter. By the same means as in Example 1, the 60-degree gloss was measured at each elapse of each test time, and the fine morphology of the surface of the coated plate after 1200 hours was observed. FIG. 5 shows the measurement results of the 60-degree gloss for each elapse of the test time.

The 60 ° gloss immediately after preparation of the coated plate was 94, and the 60 ° gloss after 1200 hours was 90.
Regarding the fine morphology of the surface of the coated plate, slight undulation was slightly recognized on the surface of the coated plate, but fine holes characteristic of outdoor deterioration were not recognized. (Example 5) 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 the concentration of hydrogen peroxide solution in Example 1 was 0.25.
Example 1 except that the water solution was replaced by a 1% by weight aqueous solution of chlorine.
A durability test was carried out under the same conditions as those described above, and the 60 ° gloss and fine morphology of the coated plate were observed.

The 60 degree gloss immediately after the preparation of the coated plate was 94, and the 60 degree gloss after the test was 85. Regarding the fine morphology of the surface of the coated plate, fine undulations and small holes were confirmed on the surface of the coated plate, which coincided with a characteristic characteristic of outdoor deterioration. (Discussion) (1) Comparative Example 1 is an example including only the B step of the two types of steps A and B, which constitute the durability test according to the present invention. Step A, which is a treatment for wetting the surface of the coated plate with a hydrogen peroxide solution, is added. Referring to the results of the durability test of each of these examples, it can be seen that in Example 1, deterioration occurring outdoors was promoted.

(2) Comparative Example 2 is an example comprising only the B step in which the ultraviolet irradiation in the hydrogen peroxide water, which is the A step in Example 2, is replaced with the ultraviolet irradiation in pure water corresponding to the B step. Comparative Example 3 is an example of omitting the warm water immersion which is Step B in Example 2 and including only Step A. Referring to the results of the durability test of these comparative examples,
In Comparative Example 2 including only the B step, no minute holes characteristic of outdoor deterioration were not observed, whereas in Comparative Example 3 including only the A step, minute undulations characteristic of outdoor deterioration were not observed. unacceptable. In contrast, in the second embodiment,
Both small holes and minute undulations characteristic of outdoor deterioration are recognized, and it is understood that outdoor deterioration is reproduced with high accuracy.

(3) In the third embodiment, a series of processes in which the steps A and B constituting the present invention are mixed is repeatedly performed to efficiently reproduce a temporal change of a material due to outdoor deterioration. It is an example which shows a test device and a test procedure. (4) In the fourth embodiment, a test apparatus capable of performing the weather resistance test according to the present invention is configured by slightly modifying the existing accelerated weather resistance test apparatus. This is an embodiment that achieves an advantageous effect. In the test apparatus, the process A of the present invention is realized by using light emitted from the light source of the apparatus by spraying a hydrogen peroxide solution onto the surface of the coated plate, and the hydrogen peroxide solution is applied to the coated plate. The time other than the time acting on the surface realizes the process B, and the time A
Steps and B steps can be performed sequentially and / or alternately. It is apparent from Example 4 that the intended effect of the present invention can be obtained by comparison with the result of Comparative Example 4.

(5) Example 5 is an example in which an oxidizing agent in which an element other than oxygen acts is used as the oxidizing agent in step A of the present invention. It is clear that the effect intended by the present invention can be obtained also by the oxidizing agent on which the element acts.

[Brief description of the drawings]

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

FIG. 2 is an explanatory diagram showing each processing step, its apparatus, and its order in Embodiment 3;

FIG. 3 is a graph showing the relationship between the number of duty cycles and 60-degree gloss in Example 3.

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

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

──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Kazuyuki Tate 41 Toyota Chuo R & D Laboratories Co., Ltd., 41-cho, Yokomichi, Nagakute-cho, Aichi-gun, Aichi Prefecture (56) References JP-A-63-222240 JP-A-9-119893 (JP, A) JP-A-48-60695 (JP, A) JP-A-64-66542 (JP, A) JP-A-4-138338 (JP, A) JP-A 1-277738 (JP, A) Japanese Patent Publication No. 2-1259 (JP, B2) Japanese Patent Publication No. 1-28897 (JP, B2) Weathering (light) resistance of elastomers-The first joint research report-, Musashino Create, July 1994 3 days, p. 21-23 (58) Field surveyed (Int. Cl. ⁷ , DB name) G01N 17/00 JICST file (JOIS)

Claims (6)

(57) [Claims] An organic material, an article comprising the organic material or
A first step of allowing an aqueous solution of an oxidizing agent excluding oxygen and ozone and light to act on a test object composed of an article coated with the organic material substantially simultaneously; and applying one of water, oxygen and light to the test object. Alternatively, a durability test method is characterized in that the step of causing a plurality of elements to act and the second step of causing them to act substantially simultaneously is performed sequentially and / or alternately. 2. The durability test method according to claim 1, wherein the oxidizing agent in the first step is selected from hydrogen peroxide, peracids, persalts, hypohalous acids, and hypohalites. A durability test method characterized by being selected. 3. The durability test method according to claim 1, wherein a means of immersing in hot water is employed as the second step. 4. The durability test method according to claim 1, wherein a means for irradiating light in a gas containing water vapor and oxygen is used as the second step. Test method. 5. An organic material, an article comprising the organic material or
A first step of applying an aqueous solution of an oxidizing agent excluding oxygen and ozone and light substantially simultaneously to a test object made of the article coated with the organic material, and a step of immersing the test object in warm water;
A second step having at least one of the steps of irradiating the test object with light in a gas containing water vapor and oxygen, sequentially and / or alternately. 6. A durability test apparatus for performing the durability test method according to any one of claims 1, 2, 3, 4, and 5, wherein the apparatus comprises an organic material, an article made of the organic material, or an article made of the organic material.
A container for accommodating a test object consisting of an article coated with an organic material, and means to act substantially simultaneously an aqueous solution and light oxidant excluding oxygen and ozone in the test object, 該被specimen <br And a means for causing one or more of water, oxygen and light to act, and when the plural act, to act substantially simultaneously.