JP2014178135A - Deterioration test method of sealant - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a deterioration test method of a sealant that can accurately measure a deterioration state while quickly deteriorating the sealant.SOLUTION: A deterioration test method of a sealant includes: a molding step of molding the sealant so as to become its thickness of 0.05 mm or more and 3 mm or less; a deterioration step of deteriorating the sealant with outdoor exposure or a weatherometer; a measurement step of measuring at least any change of physical change and chemical change of the sealant; and an estimation step of estimating the deterioration state of the sealant on the basis of the result measured by the measurement step.

Description

  The present invention relates to a sealing material deterioration test method for measuring a deterioration state of a sealing material.

  For example, a sealing material is installed at a joint portion of an outer wall of a building. Such a sealing material may partially change to another substance or change characteristics over time. For this reason, in order to judge the replacement | exchange time etc. of a sealing material, a deterioration state is measured or durability is evaluated.

  For example, in Patent Document 1, a test resin to be measured is molded into a thin film that can transmit light, and the test resin is immersed in a corrosive liquid or an exposure test or the like is performed. A method for analyzing the change over time of the test resin is described.

JP-A-8-29341

  In such a technical field, it is required to quickly deteriorate a sealing material to be measured and accurately measure the deterioration state. In the method described in Patent Document 1, the deterioration state cannot be accurately measured, and further accuracy is required.

  Therefore, the present invention is to solve such problems of the prior art, and to provide a sealing material deterioration test method capable of accurately measuring the deterioration state while rapidly deteriorating the sealing material. And

  In order to solve the above-mentioned problems, the sealing material deterioration test method according to the present invention includes a molding step of molding the sealing material to a thickness of 0.05 mm or more and 3 mm or less, and the sealing material is deteriorated by outdoor exposure or a weather resistance tester. A deterioration process, a measurement process that measures at least one of a physical change and a chemical change of the sealing material, and an estimation process that estimates a deterioration state of the sealing material based on a result measured in the measurement process; ,including.

  In the present invention, in the molding step, the sealing material is molded to a thickness of 0.05 mm or more and 3 mm or less. By using a sealing material molded to a thickness of 0.05 mm or more and 3 mm or less as an object for estimating the deterioration state, the sealing material can be rapidly deteriorated while suppressing variation in deterioration. For example, when the sealing material is thin, the sealing material deteriorates quickly. However, the thinner the sealing material, the more easily affected by various factors, and the deterioration tends to occur. Therefore, in the present invention, by setting the thickness of the sealing material to 0.05 mm or more and 3 mm or less, it is possible to accurately measure the deterioration state while rapidly deteriorating the sealing material.

  The sealing material may contain a polyether. In this case, it is possible to estimate the deterioration state of, for example, a building sealing material containing polyether. Further, in the measurement step, the degradation state of the sealing material can be accurately estimated by measuring the chemical change of the polyether and estimating the degradation state of the sealing material based on the measurement result.

  The sealing material may be a one-component polyurethane sealing material. In this case, the deterioration state of the one-component polyurethane sealant can be estimated.

  In the molding step, the sealing material is preferably molded to a thickness of 0.15 mm to 1 mm. By setting the thickness of the sealing material to 0.15 mm or more and 1 mm or less, it is possible to accurately measure the deterioration state while further rapidly deteriorating the sealing material.

  As outdoor exposure, vertical exposure or inclined exposure can be performed. In this case, the sealing material can be deteriorated by vertical exposure or inclined exposure.

  A weathering light tester or a constant temperature and humidity tester can be used as the weathering tester. In this case, the sealing material can be deteriorated using a weathering light tester or a constant temperature and humidity tester.

  In the measurement step, it is preferable to measure a chemical change of the sealing material using a pyrolysis gas chromatography method or a pyrolysis gas chromatography mass spectrometry. In this case, the chemical change of the sealing material can be measured with higher accuracy using these methods.

  In the measurement step, it is preferable to measure the chemical change of the sealing material using a solvent extraction method. In this case, the chemical change of the sealing material can be measured with higher accuracy using this method.

  In the measurement step, it is preferable to measure a chemical change of the sealing material by using a gas chromatography method or a gas chromatography mass spectrometry method in addition to the solvent extraction method. In this case, the chemical change of the sealing material can be measured with higher accuracy using these methods.

  In the measurement step, it is further preferable to measure the chemical change of the sealing material using a nuclear magnetic resonance method. In this case, the chemical change of the sealing material can be measured with higher accuracy using this method.

  In the measuring step, it is preferable to measure the tackiness of the sealing material as a physical change of the sealing material. In this case, the physical change of the sealing material can be measured with higher accuracy using this method.

  According to the present invention, it is possible to accurately measure the deterioration state while rapidly deteriorating the sealing material.

It is process drawing which shows the preparatory process of the deterioration test method of a to-be-tested object. It is process drawing which shows the creation process of the sealing material used at a preparation process. It is a figure which shows the preparation procedure of the sealing material used at a preparation process. It is a figure which shows schematic structure of a pyrolysis gas chromatography mass spectrometer. It is a figure which shows the pyrogram of a sealing material. It is a graph which shows the relationship between a peak area ratio and accelerated deterioration time. It is process drawing which shows the test process of the deterioration test method of a to-be-tested object.

  Hereinafter, embodiments of a deterioration test method for a sealing material according to the present invention will be described in detail with reference to the drawings.

  In this embodiment, a deterioration test method for measuring a deterioration state of a sealing material using a sealing material as a test object will be described. As a sealing material to be subjected to this deterioration test, a one-component polyurethane-based sealing material containing polyether can be used. As an example, such a sealing material is used outdoors, such as being arranged at the joint of the outer wall of a building.

<Preparation process>
First, a preparation process is performed before performing a deterioration test of a sealing material as a test object. In this preparation step, an index (see FIG. 6) used when performing a deterioration test of the sealing material is calculated. Hereinafter, the preparation process will be described with reference to FIG. As shown in FIG. 1, a plurality of sheets formed by molding a sealing material used in the preparation process are formed (step S101). Here, a one-component polyurethane sealant containing the same polyether as the sealant to be subjected to the deterioration test is used.

  Here, a method for molding a sealing material used in the preparation process will be described. First, as shown in FIG. 2 and FIG. 3A, a pair of adhesive tapes 20 is pasted on the surface of the smooth plate 10 so as to sandwich the sealing material forming region 50 provided on the surface of the plate 10, and the weir 20A. (Step S201: dam formation step). In addition, a pair of adhesive tape 20 is arrange | positioned so that it may mutually become parallel (refer FIG.3 (d)). When the adhesive tape 20 is used, the weir 20 </ b> A can be easily formed simply by being attached to the plate 10. Here, it is not limited to providing a pair of adhesive tapes, and the adhesive tape 20 may be provided so that the weir 20A surrounds at least a part of the sealing material forming region 50.

  As the adhesive tape 20, a cellophane tape, a paper tape, a tape coated with a metal foil (aluminum foil or copper foil, etc.) coated with an adhesive on one surface, an acetate tape (mending tape) or the like is used. Can be used. As the adhesive tape 20, other materials may be used as long as they have a uniform thickness and are not stretchable and do not cause a chemical change that reacts with the sealing material and affects the deterioration test. In addition, as the plate 10, for example, an aluminum alloy plate subjected to anodizing, a metal plate other than the aluminum alloy, a resin plate, a straight plate, a plate formed of stone, or a plate formed of a ceramic material, etc. A plate that has a smooth surface and does not cause chemical changes that react with the sealing material and affect the deterioration test can be used.

  Next, as shown in FIG.2 and FIG.3 (b), the sealing material 30 is arrange | positioned in the sealing material formation area 50 (step S202: test body arrangement | positioning process). The sealing material 30 immediately after being disposed in the sealing material forming region 50 is in a state before being cured and can be easily molded.

  Next, as shown in FIG.2 and FIG.3 (c), the spatula 40 is slid on the weir 20A (on a pair of adhesive tape 20), and the sealing material 30 is shape | molded by fixed thickness (step S203: Molding). Process). As the spatula 40, a stainless steel spatula whose end is formed in a straight line is used.

  Thereby, as shown in FIG.3 (d), the sealing material 30 shape | molded by the height of the weir 20A can be obtained. In the present embodiment, one or a plurality of adhesive tapes 20 are attached to form a weir 20A having a height of 0.05 mm to 3 mm, more preferably 0.15 mm to 1 mm. The sealing material 30 is molded to a corresponding thickness. The sealing material 30 thus molded has a thickness that does not transmit light. In addition, the sealing material 30 can be easily shape | molded by desired thickness by stacking the adhesive tape 20 in multiple numbers and arrange | positioning on the surface of the board 10. FIG.

  After the sealing material 30 is molded into a thin film, the sealing material 30 is dried (for example, cured at room temperature for 2 weeks), and the adhesive tape 20 is removed. By removing the adhesive tape 20, it is possible to prevent the adhesive tape 20 from adhering to the sealing material 30 when the adhesive tape 20 deteriorates.

  Returning to FIG. 1, after creating the sealing material 30, an accelerated deterioration test is performed on the plurality of sealing materials 30 to obtain a plurality of sealing materials 30 having different accelerated deterioration test times (step S <b> 102: deterioration process). Here, as an example, the sealing material 30 is arranged in a constant temperature and humidity tester, and the conditions for the accelerated deterioration test are a temperature of 80 ° C. and a humidity of 5% to 7%.

  Next, a chemical change is measured about the sealing material 30 after an accelerated deterioration test (step S103). Here, measuring the chemical change of the sealing material 30 means measuring the amount of a substance whose production amount increases or decreases with the deterioration of the sealing material 30 over time. Specifically, the entire thermal decomposition product of the sealing material 30 and the thermal decomposition product derived from the polyether portion are measured. The ratio of the entire sample and the amount of the thermal decomposition product derived from the polyether part tends to increase in proportion to the deterioration of the sealing material 30. For this reason, the ratio of the amount of thermal decomposition products becomes larger as the sealing material 30 has a longer accelerated deterioration test time.

  In the present embodiment, the entire sample and the amount of the pyrolysis product derived from the polyether part are analyzed by pyrolysis gas chromatography mass spectrometry (PyGC / MS method). Here, the pyrolysis gas chromatography mass spectrometer will be described. As shown in FIG. 4, the pyrolysis gas chromatography mass spectrometer 1 includes a sample injection section 2, a pyrolysis apparatus 3, a column 4, a splitter 5, a detector 6, an interface 7, and a mass spectrometer 8. Composed. A sealing material 30 to be analyzed is put into the sample injection unit 2. The thermal decomposition apparatus 3 rapidly heats and decomposes the sealing material 30 introduced from the sample injection unit 2.

  Gas generated by heating / decomposing the sealing material 30 is introduced into the column 4 from the thermal decomposition apparatus 3 by the carrier gas G. When performing gas chromatographic analysis, gas is introduced into the detector 6 through the splitter 5, and analysis is performed in the detector 6. Further, gas is introduced into the interface 7 through the splitter 5 and then introduced into the mass spectrometer 8, and mass analysis is performed in the mass spectrometer 8.

  As a result of the analysis by the pyrolysis gas chromatography mass spectrometer 1, a pyrogram shown in FIG. 5 is obtained as an example. In this pyrogram, a peak is detected for each substance. The content of each substance is represented by the peak area. In this embodiment, paying attention to the thermal decomposition product derived from a polyether part among these peaks, the area of the peak which shows the thermal decomposition product derived from a polyether part is calculated | required. Moreover, the area of all the peaks of the thermal decomposition product in a sample is calculated | required. The area of the peak of the pyrolysis product derived from the polyether part and the area of all the peaks of the pyrolysis product in the sample are obtained for each of the plurality of sealing materials 30 having different accelerated degradation test times.

Next, using the analysis result in the pyrolysis gas chromatography / mass spectrometer 1, the area ratio of the peak of the pyrolysis product derived from the entire sample and the polyether part in the sealing material 30 that has not been subjected to the accelerated deterioration test (A ) And the area ratio (B) of the peak of the thermal decomposition product derived from the polyether portion and the polyether part in the sealing material 30 subjected to the accelerated deterioration test (step S104). The area ratio of the peak indicating the thermal decomposition product derived from the polyether portion increases as the accelerated deterioration test time increases. The change ratio (peak area ratio (Ct)) of the peak area ratio (Bt) after the accelerated deterioration (accelerated deterioration time t) is obtained by the following formula using the peak area ratio (A) where the accelerated deterioration test is not performed as a reference. .
Peak area ratio (Ct) = peak area ratio (Bt) ÷ peak area ratio (A)

  Next, the obtained peak area ratio (Ct) and the accelerated deterioration time (t) are associated with each other, and a graph shown in FIG. 6 is obtained as an example (step S105). In the graph shown in FIG. 6, the horizontal axis represents the accelerated deterioration time (here, the unit of the accelerated deterioration time is “day”), and the vertical axis represents the peak area ratio. Further, here, a straight line L1 indicating the relationship between the accelerated deterioration time and the peak area ratio is obtained.

  In addition, the thickness of the sealing material 30 used when obtaining the straight line L1 is 0.15 mm. A straight line L2 indicates a correspondence relationship between the peak area ratio and the accelerated deterioration time when the sealing material 30 having a thickness of 2 mm is used. Thus, when the thickness of the sealing material 30 is reduced, the increase in the peak area ratio increases with the passage of the accelerated deterioration time, that is, there is a tendency to deteriorate quickly. However, when the thickness of the sealing material 30 is reduced, the sealing material 30 is easily affected by various factors, and variations in deterioration are likely to occur.

  Here, the deterioration state of the substance after the accelerated deterioration test is correlated with the deterioration state with the passage of actual time. For this reason, the peak area ratio of the substance that has passed the actual time (T) is applied to the straight line L1 shown in FIG. 6 to obtain the accelerated deterioration time (t). The acceleration magnification (M) is obtained from the ratio of the actual time (T) and the accelerated deterioration time (t). The service life limit accelerated deterioration time is obtained by arbitrarily setting the service life limit and placing the peak area ratio of this substance on the straight line L1. By multiplying this by the acceleration factor (M), the service life of the substance can be obtained.

<Test process>
Next, the deterioration test of the sealing material which is a test object is performed. Here, as an example, the deterioration state of the sealing material collected from the building is estimated. As shown in FIG. 7, first, the chemical change of the thermal decomposition product of the whole sealing material as the test object and the thermal decomposition product derived from the polyether part is measured (step S301: measurement process). In the present embodiment, the contents of the pyrolysis product of the entire sample and the pyrolysis product derived from the polyether portion are analyzed by pyrolysis gas chromatography mass spectrometry in the same manner as described above.

  Next, by using the analysis result of the pyrolysis gas chromatography mass spectrometer 1, the area ratio of the peak of the entire sample and the pyrolysis product derived from the polyether part in the sealing material that has not been subjected to the accelerated degradation test described above, and Then, the area ratio of the peak of the thermal decomposition product derived from the entire sample and the polyether part in the sealing material as the test object is obtained (step S302: calculation step).

  Next, the deterioration state of the sealing material, which is the test object, is estimated using the calculated area ratio of the entire sample and the peak of the pyrolysis product derived from the polyether part (step S303: estimation step). As an example, the peak area ratio is calculated based on the calculated total area of the sample and the peak area ratio of the pyrolysis product derived from the polyether portion and the peak area ratio (A) where no accelerated deterioration test is performed, and the straight line shown in FIG. The accelerated deterioration time is obtained based on L1. By multiplying this accelerated deterioration time by the acceleration magnification indicating the relationship between the accelerated deterioration time and the actual elapsed time of the test object, the deterioration state of the sealing material as the test object can be grasped. Further, the service life can be obtained by the product of the accelerated deterioration time and the acceleration magnification that reach the arbitrarily set service life limit. Furthermore, the life until the service life can be obtained from the difference between the service life and the actual elapsed time. For example, in the graph shown in FIG. 6, when the thickness of the sealing material is 0.15 mm, the acceleration magnification is about 40 times. Moreover, you may obtain | require the accelerated deterioration time of a test object using the straight line L2 (when the thickness of a sealing material is 2 mm) shown in FIG. In this case, the acceleration magnification is about 16 times.

  The present embodiment is configured as described above, and a sealing material molded to a thickness of 0.05 mm or more and 3 mm or less is used as a test object for estimating a deterioration state, so that the sealing material is quickly deteriorated while suppressing variation in deterioration. be able to. For example, when the sealing material is thin, the sealing material deteriorates quickly. However, the thinner the sealing material, the more easily affected by various factors, and the deterioration tends to occur. Therefore, in this embodiment, by setting the thickness of the sealing material to 0.05 mm or more and 3 mm or less, it is possible to accurately measure the deterioration state while rapidly deteriorating the sealing material.

  In addition, by setting the thickness of the sealing material to 0.15 mm or more and 1 mm or less, it is possible to accurately measure the deterioration state while further rapidly deteriorating the sealing material.

  The sealing material may contain a polyether. In this case, it is possible to estimate the deterioration state of, for example, a building sealing material containing polyether. Further, in the measurement step, the degradation state of the sealing material can be accurately estimated by measuring the chemical change of the polyether and estimating the degradation state of the sealing material based on the measurement result.

  The sealing material may be a one-component polyurethane sealing material. In this case, the deterioration state of the one-component polyurethane sealant can be estimated.

  By measuring the chemical change of the sealing material using pyrolysis gas chromatography mass spectrometry, the chemical change of the sealing material can be measured with higher accuracy.

  Although one embodiment of the present invention has been described above, the present invention is not limited to the above embodiment. For example, in the above embodiment, after obtaining the correspondence relationship between the peak area ratio and the accelerated deterioration time shown in FIG. 6 using the sealing material 30 as a test body in the preparation process, the sample was collected from an actual building in the test process. The deterioration state of the sealing material was estimated. In addition to this, when the deterioration states of the sealing materials having different components are compared, these sealing materials may be formed into a thin film by the method described in the above test step. Since the sealing material is molded into a thin film as described above, deterioration of the sealing material is promoted, so that the deterioration state of the sealing materials can be compared quickly.

  Pyrolysis gas chromatography / mass spectrometry was used to measure the chemical change of the pyrolysis product derived from the polyether part, but pyrolysis gas chromatography or solvent extraction may be used. . Moreover, when measuring the chemical change of the thermal decomposition product derived from a polyether part, in addition to the solvent extraction method, you may use a gas chromatography method or a gas chromatography mass spectrometry. Moreover, when measuring the chemical change of the thermal decomposition product derived from a polyether part, you may use a nuclear magnetic resonance method in addition to a solvent extraction method. Even if these measuring methods are used, the chemical change of the thermal decomposition product derived from the polyether part can be accurately measured.

  Moreover, when performing the accelerated deterioration test of the sealing material 30, the constant temperature and humidity tester as a weathering tester was used, but besides this, a weathering light tester as a weathering tester may be used. Further, a weathering tester other than the constant temperature and humidity tester and the weathering light tester may be used. Furthermore, when performing an accelerated deterioration test, outdoor exposure may be performed without using a weathering tester. When performing outdoor exposure, vertical exposure or inclination exposure (for example, installation by tilting 30 degrees toward the south side, or installation vertically) can also be performed. Moreover, you may perform combining the accelerated deterioration test in a weathering tester, and the accelerated deterioration test in outdoor exposure.

  Moreover, in order to judge the deterioration state of the sealing material 30, although the chemical change of the thermal decomposition product derived from a polyether part was measured, the method of measuring the physical change of the sealing material 30 was used. Also good. For example, the change in the adhesiveness of the sealing material 30 can be measured. Specifically, after the metal plate is pressed against the molded sealing material 30 with a constant load for a certain period of time, the metal plate is pulled at a constant speed, and the stress may be measured with a load cell. Thus, quantitative measurement becomes possible by measuring the adhesiveness of the sealing material whose adhesiveness increases due to thermal degradation.

  DESCRIPTION OF SYMBOLS 1 ... Pyrolysis gas chromatography mass spectrometer, 2 ... Sample injection part, 3 ... Pyrolysis apparatus, 4 ... Column, 5 ... Splitter, 6 ... Detector, 7 ... Interface, 8 ... Mass spectrometer, 10 ... Plate, DESCRIPTION OF SYMBOLS 20 ... Adhesive tape, 20A ... Weir, 30 ... Sealing material, 40 ... Spatula, 50 ... Sealing material formation area, G ... Carrier gas.

Claims (11)

A molding step of molding the sealing material to a thickness of 0.05 mm to 3 mm;
A deterioration step of degrading the sealing material by outdoor exposure or a weathering tester;
A measuring step for measuring a change in at least one of a physical change and a chemical change in the sealing material;
Based on the result measured in the measurement step, an estimation step for estimating the deterioration state of the sealing material,
Test method for deterioration of sealing material containing   The deterioration test method for a sealing material according to claim 1, wherein the sealing material contains a polyether.   The deterioration test method for a sealing material according to claim 2, wherein the sealing material is a one-component polyurethane-based sealing material.   The deterioration test method for a sealing material according to any one of claims 1 to 3, wherein, in the molding step, the sealing material is molded to a thickness of 0.15 mm to 1 mm.   The deterioration test method for a sealing material according to any one of claims 1 to 4, wherein the outdoor exposure is vertical exposure or inclined exposure.   The deterioration test method for a sealing material according to any one of claims 1 to 4, wherein the weather resistance tester is a weather resistance light tester or a constant temperature and humidity tester.   The said measurement process measures the chemical change of the said sealing material using a pyrolysis gas chromatography method or a pyrolysis gas chromatography mass spectrometry, The method as described in any one of Claims 1-6. Sealing material deterioration test method.   The deterioration test method for a sealing material according to any one of claims 1 to 6, wherein in the measurement step, a chemical change of the sealing material is measured using a solvent extraction method.   The sealing material deterioration test method according to claim 8, wherein in the measuring step, the chemical change of the sealing material is further measured using a gas chromatography method or a gas chromatography mass spectrometry method.   The sealing material deterioration testing method according to claim 8, wherein in the measuring step, a chemical change of the sealing material is further measured using a nuclear magnetic resonance method.   The deterioration test method for a sealing material according to any one of claims 1 to 6, wherein, in the measuring step, the adhesiveness of the sealing material is measured as a physical change of the sealing material.

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