JP2007056200A - Luminous coating material and coating method using the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a coating material excellent in functions required for coating materials such as stainproofness, weatherability and protective function to substrates, and also exerting luminousness. <P>SOLUTION: The coating material is a compounded product comprising an organosiloxane oligomer, a catalyst, a silane compound, a titanium compound and a luminous pigment, wherein the viscosity of this compounded product is adjusted to 50-300 mPa.s at 25°C. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a phosphorescent coating material and a coating method using the same, and in particular, a one-pack type phosphorescent property obtained by using a non-contaminating and weather-resistant phosphorescent coating layer relatively easily and without using a solvent. The present invention relates to a coating material and a coating method using the same.

  Things are difficult to see when there is no light source at night. For example, it is difficult to walk in a place where no streetlight is installed, and it is difficult to drive a car. Even indoors, when the light is turned off or there is a sudden power outage, the field of view is blocked and nothing can be seen for a while. In order to solve such a problem, it has been proposed to incorporate a luminous pigment into a material of a product, which has already been applied to various products. However, this method has a disadvantage that the luminous process is complicated and the cost is increased because the luminous pigment must be mixed into the product material at the time of molding.

For this reason, as seen in the following Patent Document 1, a coating material in which a luminous pigment is mixed has been proposed. This is because if the coating material is applied to the surface of the product itself, the light emission appears, so that there is an advantage that it is simpler and less expensive than the one that is incorporated into the product material. However, this preceding example merely imparts phosphorescent properties, and does not take into consideration coating performance such as contamination prevention, weather resistance, and protective function originally required for the coating material (in this respect, an excellent coating material and I can't say).
Japanese Patent Application No. 2000-86966

  The present invention solves the above-described problems, and embodies a light-storing coating material that is excellent in coating performance originally required for a coating material and that exhibits a light-storing property, and a coating method using the same.

  The phosphorescent coating material solved in the present invention is a blend comprising an organosiloxane oligomer, a catalyst, a silane compound, a titanium compound and a phosphorescent pigment as described in claim 1, and the viscosity of the blend is It is adjusted to 50 to 300 mPa · s at 25 ° C. A coating method using a phosphorescent coating material for effectively carrying out the present invention is a coating film having a thickness of 10 μm on a tangible object composed of concrete, debris, paper, plastic, metal, and wood according to claim 8. It comprises a single coating step to be applied below, a repetitive coating step in which the coating step is repeated several times, and a drying step of drying the phosphorescent coating material applied by natural drying or forced drying.

  According to the phosphorescent coating according to the first aspect, the luminescent property is exhibited by the phosphorescent pigment simply by applying it to the surface of the product. In addition, this coating material is a very stable formulation, can sufficiently continue to emit light, and has properties such as non-contamination, weather resistance, acid resistance, and alkali resistance. Of course, since no solvent is required, it is excellent in terms of environment and health. Moreover, according to the coating method of Claim 8, a luminous storage coating layer can be reliably obtained by a simple method.

  The phosphorescent coating material of the present invention (hereinafter simply referred to as coating material) comprises (a) an organosiloxane oligomer, (b) a catalyst, (c) a silane compound, (d) a titanium compound, and (e) a phosphorescent pigment. (F) The viscosity at 25 ° C. is adjusted to 50 to 300 mPa · s. First, each component of this coating material will be described in detail.

(A) Organosiloxane oligomer The organosiloxane oligomer is represented by the following formula (1).
R ^l _s SiO (R ¹ ₂ SiO) _l SiR ^l _s (1)
(In the formula, R ¹ is a hydrogen atom, a hydroxyl group, a halogen atom, or a monovalent organic group having 1 to 8 carbon atoms, and may be the same or different from each other. An organosiloxane oligomer represented by the following formula: Examples of the derivatives include hydrolysates of organosiloxane oligomers and condensates of organosiloxane oligomers. In addition, such an organosiloxane oligomer may be used individually by 1 type, or may be used in mixture of 2 or more types.

Examples of the halogen atom constituting R ¹ include fluorine and chlorine.

Examples of the organic group having 1 to 8 carbon atoms constituting R ¹ include alkyl groups such as methyl group, ethyl group and propyl group, alkoxyl groups such as methoxy group and ethoxy group, and phenyl group.

R ¹ may be partially substituted by a substituent such as a halogen atom, an amino group, an epoxy group, a carboxyl group, a hydroxyl group, a methacryl group, a mercapto group, a phenyl group, or a vinyl group. A part of the group may be further substituted with the above substituent.

  Among these, an organosiloxane oligomer containing a structure in which a silicon atom is bonded to a hydrolyzable group and / or a hydroxyl group, for example, a condensate of alkoxysilane or a condensate of chlorosilane is preferable. Such an organosiloxane oligomer is co-condensed and fixed with a silane compound, a titanium compound, and a luminous pigment when the coating material according to the present invention is cured. Therefore, a stable coating layer can be obtained.

  In addition, as an organosiloxane oligomer, you may prepare and use said compound, and may use what is marketed. Examples of commercially available organosiloxane oligomers include KC89S and KR400 manufactured by Shin-Etsu Chemical Co., Ltd., XC96-B0446 and XR31-B2230 manufactured by GE Toshiba Silicone Co., Ltd. These organosiloxane oligomers may be used as they are or after hydrolysis.

  Since the base of the organosiloxane oligomer is a resin, the amount is 100 parts by weight.

(B) Catalyst As the catalyst, an acidic compound, an alkaline compound, a salt compound, an amine compound, an organometallic compound and / or a partial hydrolyzate thereof (hereinafter referred to as an organometallic compound and / or a partial hydrolyzate thereof, Organic metal compounds ”). In addition, such a catalyst may be used individually by 1 type, or 2 or more types may be mixed and used for it.

  Examples of the acidic compound include acetic acid, hydrochloric acid, sulfuric acid, phosphoric acid and the like.

  Examples of the alkaline compound include sodium hydroxide and potassium hydroxide.

  Examples of the salt compound include alkali metal salts such as naphthenic acid and octylic acid.

  Examples of the amine compound include aminosilane, ethylenediamine, hexamethylenediamine, diethylenetriamine, triethylenetetramine, alkylamine salts, and quaternary ammonium salts. In addition, various modified amines that can be used as curing agents for epoxy resins are also included.

Examples of organometallic compounds include organic zirconium compounds such as di-n-butoxy bis (ethyl acetoacetate) zirconium and n-butoxy tris (ethyl acetoacetate) zirconium, and di-i-propoxy bis (ethyl acetoacetate). Organic titanium compounds such as acetate) titanium, di-i-propoxy bis (acetylacetate) titanium, organoaluminum compounds such as di-i-propoxy acetylacetonato aluminum, i-propoxy bis (ethylacetoacetate) aluminum, (C ₄ H ₉ ) ₂ Sn (OCOCC ₁₁ H ₂₃ ) ₂ , (C ₄ H ₉ ) ₂ Sn (SCH ₂ COOC ₈ H ₁₇ ) ₂ , (C ₄ H ₉ ) ₂ Sn (SCH ₂ CH ₂ COOC ₈ H ₁₇ ) Organotin compounds such as ₂ and partial hydrolysates thereof.

  The catalyst may be blended in the step of preparing the coating material according to the present invention, may be blended in the coating material in the step of forming the coating film, and further, the step of preparing the coating material and the coating film You may mix | blend with both the process of forming.

  As the catalyst, the above compound may be prepared and used, or a commercially available one may be used. As a commercially available catalyst, Shin-Etsu Chemical Co., Ltd. D-20 which is a polymer (partial hydrolyzate) of tetraalkoxy titanium is mentioned.

  The amount of the catalyst is 0.1 to 40 parts by weight, preferably 0.5 to 35 parts by weight, and more preferably 1 to 30 parts by weight with respect to 100 parts by weight of the organosiloxane oligomer. When the amount of the catalyst exceeds the above upper limit, the storage stability is deteriorated and the curing rate becomes extremely fast, so that it may be difficult to apply the coating material. On the other hand, when the amount of the catalyst exceeds the above lower limit, the curing rate is extremely lowered, and the coating time and the curing time are prolonged. In extreme cases, there is a possibility that the original hardness cannot be expressed due to poor curing.

(C) Silane compound The silane compound is represented by the following formula (2).
R ² _m SiR ³ _{4 -m} (2)
(Wherein R ² represents a hydrogen atom or a monovalent organic group having 1 to 8 carbon atoms, and R ³ represents a halogen atom, a hydroxyl group or a monovalent alkoxyl group having 1 to 8 carbon atoms. In the case where a plurality of them are present, they may be the same as or different from each other, where m is an integer of 0 to 3.). Examples of the derivatives include hydrolysates of silane compounds and condensates of silane compounds. In addition, such a silane compound may be used individually by 1 type, or 2 or more types may be mixed and used for it.

Examples of the organic group having 1 to 8 carbon atoms constituting R ² include alkyl groups such as methyl group, ethyl group, and propyl group, vinyl group, and phenyl group.

Further, a part of R ² is substituted with a substituent such as vinyl group, epoxy group, styryl group, methacryloxy group, acryloxy group, amino group, ureido group, halogen atom, mercapto group, sulfide group, isocyanate group, carboxyl group, etc. May be.

Examples of the halogen atom constituting R ³ include fluorine and chlorine. The monovalent alkoxyl group 1 of 1 to 8 carbon atoms constituting the R ^3, a methoxy group, an ethoxy group, n- propoxy group, i- propoxy group, and the like.

  Specific examples of such silane compounds include tetraalkoxysilanes such as tetramethoxysilane, trialkoxysilanes such as methyltrimethoxysilane, dialkoxysilanes such as dimethyldimethoxysilane, and monoalkoxysilanes such as trimethylmethoxysilane. Examples include chlorosilanes such as alkoxysilanes and trichlorosilane.

  Among these, trialkoxysilanes and trichlorosilanes are preferable, and among them, a silane coupling agent having both a reactive group that chemically bonds with an organic substance and a reactive group that chemically reacts with an inorganic substance is preferable. This is because the silane coupling agent accelerates curing and imparts the effect of improving crosslinkability and adhesiveness.

  As such a silane coupling agent, specifically, vinyltrichlorosilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropyltriethoxysilane, 3-methacryloxypropyltriethoxysilane, Examples include 3-acryloxypropyl trimethoxysilane, 3-aminopropyltrimethoxysilane, and p-styryltrimethoxysilane.

  As the silane compound, the above compound may be prepared and used, or a commercially available one may be used. Examples of commercially available silane compounds include KBM-403 manufactured by Shin-Etsu Chemical Co., Ltd. The silane compound may be used as it is or after hydrolysis.

  In this invention, a silane compound is 0.1-20 weight part with respect to 100 weight part of organosiloxane oligomers, Preferably it is 0.5-15 weight part, More preferably, 1.5-10 weight part is preferable. If the amount of the silane compound exceeds the above upper limit, cracks or surface bleed out may occur. On the other hand, when the amount of the silane compound exceeds the lower limit, there is a possibility of causing an improvement in adhesion and poor crosslinking.

(D) Titanium compound The titanium compound is represented by the following (3).
R _4n Ti (OR ⁵ ) _4-n (3)
(In the formula, R ⁴ represents an organic group having 1 to 8 carbon atoms, and when a plurality of R ⁴ are present, they may be the same or different. R ⁵ is an alkyl group having 1 to 6 carbon atoms. Represents an organic group selected from the group consisting of an acyl group having 1 to 6 carbon atoms and a phenyl group, and may be the same or different when a plurality of them are present, and n is 0-3. And a titanium acylate represented by the above formula (3) and a derivative thereof. In addition, even if these titanium compounds are single 1 type, arbitrary 2 or more types of mixtures may be sufficient as them.

  Examples of titanium alcoholate and titanium acylate derivatives include hydrolysates and condensates thereof, chelate compounds thereof, hydrolysates and condensates of these chelate compounds.

In the above formula (3), R ⁴ is an organic group having 1 to 8 carbon atoms, specifically, an alkyl group such as methyl group, ethyl group, n-propyl group, i-propyl group, acetyl group, Examples include acyl groups such as propionyl groups.

R ⁴ may be partially substituted with, for example, a halogen atom, an amino group, or a hydroxyl group, and a part of these substituents may be further substituted with the above substituent.

  Specific examples of titanium alcoholate include tetra-i-propoxytitanium, tetra-n-butoxytitanium, tetra-t-butoxytitanium, di-i-propoxy bis (ethylacetoacetate) titanium, and di-i-propoxy. Bis (acetyl acetate) titanium, di-i-propoxy bis (lactate) titanium, di-i-propoxy bis (acetylacetonato) titanium, di-n-butoxy bis (triethanolaminato) titanium, di -N-butoxy bis (acetylacetonato) titanium, tetrakis (2-ethylhexyloxy) titanium, etc. are mentioned. Of these, di-i-propoxy bis (acetylacetonato) titanium is preferred.

  Specific examples of titanium acylate and titanium acylate chelate compounds include dihydroxy / titanium dibutyrate, di-i-propoxy / titanium diacetate, bis (acetylacetonato) / titanium diacetate, and bis (acetylacetate). Nato) -titanium dipropionate, di-i-propoxy-titanium dipropionate, di-i-propoxy-titanium dimalonate, di-i-propoxy-titanium dibenzoylate, di-n-butoxy-zirconium diacetate , Di-i-propyl aluminum monomalonate and the like. Of these, dihydroxy titanium dibutyrate and di-i-propoxy titanium diacetate are preferred.

  A chelate compound of titanium alcoholate and titanium acylate can be obtained by reacting these with a chelating agent such as β-diketone and β-ketoester. In addition, hydrolyzate and condensate of titanium alcoholate and titanium acylate or hydrolyzate and condensate of these chelate compounds can be obtained by adding water to titanium alcoholate and titanium acylate or these chelate compounds. It is done.

  As the titanium compound, the above-mentioned compound may be prepared and used, or a commercially available one may be used. Examples of the commercially available condensate of titanium alcoholate include T-50 manufactured by Nippon Soda Co., Ltd.

  The amount of the titanium compound that can be used in the present invention is 0.1 to 50 parts by weight, preferably 1 to 40 parts by weight, and more preferably 2 to 30 parts by weight with respect to 100 parts by weight of the organosiloxane oligomer. When the amount of the titanium compound exceeds the above upper limit, the transparency may be lowered. Moreover, when the amount of the titanium compound exceeds the lower limit, the antifouling performance and the water repellent function may be deteriorated.

(E) Luminescent Pigment A pigment that is contained in a coating material and stores light energy to emit light, and those described below are commercially available. The amount is preferably 10 to 40 parts by weight, more preferably 10 to 30 parts by weight based on 100 parts by weight of the total of the organosiloxane oligomer, catalyst, silane compound and titanium compound.

(F) Viscosity The viscosity of the coating material of the present invention is adjusted to 50 to 300 mPa · s at 25 ° C., but more preferably in the range of 100 to 150 mPa · s. This is because if the viscosity is too high, the fluidity is inferior, the resistance increases, and it becomes difficult to spread the coating with a specified amount (coating thickness) or less with respect to the base. It is because formation of a coating film becomes difficult because of inferiority. In addition, this viscosity can be adjusted with the quantity which adds a thickener, Polyoxide, methylcellulose, etc. are mentioned as this thickener. The viscosity in this case is a value measured by a measuring device used for ordinary viscosity measurement such as a rotational viscometer.

  Since the coating material of the present invention is generally low in viscosity and is one-component, a propellant such as liquefied petroleum gas (LPG), dimethyl ether (DME), chlorofluorocarbons, nitrogen gas, carbon dioxide gas It can also be used as an aerosol by mixing it with a spray can.

  Next, a coating method using the above coating material will be described. First, this coating method is divided into three steps: (a) a once-applying step, (b) an over-applying step, and (c) a drying step. The details will be described below.

  In the following description, the base area to be processed in a single coating process is referred to as a coating zone. Any material described above can be applied to the base.

(I) Once coating process First, an appropriate amount of coating material is sprayed onto a predetermined coating zone of the base by spraying so that there is no coating spot with a coating tool. In addition, the amount of the coating material is such that the effective application amount in the application zone is 100 g / m ² or less, from the viewpoints of economy, prevention of coating unevenness, shortening the time to the next process by early drying, and suppressing cracks, etc. preferable. The spraying operation is preferably completed within 30 minutes because the curing gradually proceeds with time.

(B) Overcoat process Once the application process has been completed, an appropriate amount of coating material is sprayed onto the application zone in a manner similar to that in the application process so that there are no spots.

As for the amount of the coating material at the time of overcoating, it is preferable that the effective coating amount in the coating zone is 100 g / m ² or less in order to prevent cracking, promote drying, and ensure a uniform film thickness. The overcoating step is preferably performed after 10 to 120 minutes after the completion of the coating step, because the silanolation reaction proceeds and the coating film is firmly integrated.

(C) Drying process After the overcoating process is completed for all target application zones, the process is left to stand for natural drying or forced drying. In the case of natural drying, for example, it is left for 1 to 2 hours or more, preferably 3 hours or more in a place with indoor ventilation equipment that is not directly exposed to outside air. In the case of forced drying, after naturally drying for 15 minutes or more, preferably about 30 to 60 minutes, using a hot air dryer, an infrared long wave dryer, an infrared medium wave dryer, an infrared short wave (far infrared) dryer or the like. The tank is dried for 5 to 60 minutes, preferably about 15 minutes, so that the atmospheric temperature in the tank is 50 to 150 ° C., preferably 60 to 70 ° C.

  As described above, if the coating material and the coating method according to the present invention are used, a non-contaminating and light-resistant coating layer that is not affected by the ultraviolet region, has strong acid resistance and alkali resistance, and has good weather resistance can be used with a solvent. Without being relatively easy to obtain. Since this coating layer is present, the substrate is protected from acid resistance, alkali resistance, ultraviolet resistance, water permeability resistance, and the like, and at the same time, emits light.

  Hereinafter, the present invention will be described with reference to examples, but the present invention is not limited thereto. In the examples, the viscosity is a value at 25 ° C.

(Sample preparation)
100 g of KC89S (manufactured by Shin-Etsu Chemical Co., Ltd., viscosity 70 mPa · s) whose substituent is a methyl group and the hydrolyzable alkoxy group is a methoxy group, and 0.5 g of epoxysilane KBM-403 (manufactured by Shin-Etsu Chemical Co., Ltd.) 5 g of di-i-propoxy bis (acetylacetonato) titanium T-50 (manufactured by Nippon Soda Co., Ltd.), 3 g of titanium catalyst D-20 (manufactured by Shin-Etsu Chemical Co., Ltd.), and phosphorescent pigment (manufactured by Easy Bright) ) 20 g was stirred with a magnetic stirrer until uniform to obtain a coating material (sample 1) having a viscosity of 130 mPa · S.

  A coating material (sample 2) having a viscosity of 140 mPa · s was obtained by the same composition and procedure as sample 1 except that methylmethyl type KR500 was used as the organosiloxane oligomer.

  A coating material (sample 3) having a viscosity of 110 mPa · s was obtained by the same composition and procedure as sample 1 except that di-i-propoxy bis (acetylacetonato) titanium was not added.

(Initial performance test)
The coating material of Sample 1 was applied by spraying so that there was no smear on the standard application plate. The coating on the standard coating plate was carried out on three types of coating plates A, B, and C by changing the number of coatings once, twice, and three times. In addition, in the case of applying twice and three times, the coating was performed by the same method as the first after 60 minutes after the first or second coating was completed.

  The coated sample thus prepared was cured at about 25 ° C. for 7 days, and then examined for phosphorescent properties, water repellency, overcoat adhesion, and coating film thickness. The results are shown in Table 1 below. The phosphorescence time was evaluated visually, the water repellency was evaluated based on the water contact angle measured with a contact angle meter (CA-Z) manufactured by Kyowa Interface Chemical, and the coating adhesion was JISK5600 5-6 grid Evaluation was made according to the test. The coating thickness was calculated by calculating the volume from the weight and density of the applied coating material and assuming the volume loss after reaction as 20%.

  As shown in Table 1, as the coating material of Sample 1 was repeatedly applied, the phosphorescence time became longer. In addition, the coating material of Sample 1 exhibited sufficient phosphorescent property and strong water repellency even when applied only once, and also exhibited strong coating adhesion.

(Weather resistance test)
On the half of the standard coating plate, the sample 1 was coated in the same manner as in Example 2 by changing the A, B, and C types to once and twice. And what was cured for 7 days was performed for 2000 hours in the weathering resistance acceleration | stimulation test (sunshine weather meta acceleration | stimulation test method). The results are shown in Table 2 below.

  As shown in Table 2, no abnormality was found in the weathering acceleration test or the one-year exposure test.

(Comparative performance test)
Sample 1, Sample 2, and Sample 3 were coated twice on the standard coating plate by the same method as in Example 2, and the light storage time, surface smoothness, and coating thickness were examined. The results are shown in Table 3. In addition, the meanings of the symbols in Table 3 are: ◎: no coating group, no reflection group, ×: there are coating group, reflection group. As shown in Table 3, Sample 1 was able to form a coating layer having a uniform light-emission time, a flat surface and a uniform coating thickness. The phosphorescence time and the coating thickness were evaluated in the same manner as in Example 2. Further, the surface smoothness was visually evaluated for the presence of smears and reflection spots.

(Comparison endurance test)
Sample 1, Sample 2, and Sample 3 were coated on the standard coating plate twice in the same manner as in Example 2 and exposed to the outdoors for a long period of time for water repellency (water contact angle), fingerprint adhesion, and dirt. The change was investigated. The results are shown in Table 4.

  Here, water repellency (water contact angle) was measured by the same method as in Example 2. Further, the color difference L is a difference between lightness values before and after exposure measured using a Minolta color difference meter CR-300. In addition, as for the meaning of the symbol in Table 4, dirt (visually) evaluated the dirt adhesion of the surface visually. The meanings of the symbols in Table 4 are as follows: ◎: Smoke does not adhere, ○: Smoke adheres thinly but can be easily wiped with dry cotton cloth, △: Smoke adheres but can be wiped with dry cotton cloth, × : Smoke adheres greatly and is difficult to wipe with a dry cotton cloth.

  As shown in Table 4, by applying the materials 1, 2, and 3, the water repellency of the standard coated plate was maintained over a long period of 36 months. In addition, when the sample 1 is applied, the performances of color difference and dirt (visually) are less likely to deteriorate than when the sample 2 or 3 is applied, and in particular, the sample 1 decreases until 36 months after the start of exposure. I did not.

(Component amount determination test)
Organosiloxane oligomer constituting the coating material (KC89S described in Example 1), catalyst (mixture X40-2309A of phosphoric acid and organosiloxane manufactured by Shin-Etsu Chemical Co., Ltd., and D-20 described in Example 1) In order to examine the effect of the ratio of the silane compound (KBM-403 described in Example 1) and the titanium compound (T-50 described in Example 1) on the properties of the coating material, samples 4 having different amounts thereof were used. Sample 15 was prepared in the same manner as in Example 1 and tested for touch drying time, curability, pencil hardness, fingerprint adhesion, adhesiveness, and coatability. The luminous pigment was 20 parts by weight. And unified. The results are shown in the following (I) to (III).

  Here, each said test was done as follows using the standard coating board which applied each sample twice so that an effective application quantity might be set to 80 g / in the room | chamber temperature of 25 degreeC. First, the touch-drying time was measured by touching with a finger until no longer adhered. The curability was evaluated by wiping with a wet cotton cloth after carbon was attached to the coating film after 2 hours of application. In addition, the meaning of the symbol in each table | surface is (circle): complete removal, (triangle | delta): It remained thin, x: It cannot be removed. The pencil hardness was evaluated according to JISK5600 5-4 scratch hardness (pencil method) after 24 hours and after 7 days. The fingerprint adhesion was evaluated based on the presence or absence of fingerprints by pressing the finger for 3 seconds. In addition, the meaning of the symbol in each table | surface is (circle): No adhesion | attachment, (triangle | delta): Easy wiping off, x: Wiping off is difficult. The adhesiveness was evaluated according to JIS K5600 5-6 cross cut test. In the coating test, the transparency and smoothness of the coating film were observed and evaluated by feeling and visual observation. In addition, the symbol in each table | surface means that it is (circle): easy, (triangle | delta): a little difficult, and x: impossibility that the coating film of a once coating and the coating film of a multiple-coating satisfy | fill the said reference | standard.

(I) Influence of catalyst amount As shown in Table 5, when the amount of catalyst added to the coating material was changed, when the amount of catalyst was small (sample 4), it took time to cure and the hardness of the coating layer On the other hand, when the amount of catalyst was large (Sample 7), it was difficult to reapply the coating material. Moreover, when the amount of the catalyst with respect to 100 parts by weight of the organosiloxane oligomer was in the range of 0.5 to 30 parts by weight, good properties were exhibited.

(II) Influence of the amount of silicon compound As shown in Table 6, when the amount of silicon compound is small (Sample 8), the adhesion of the coating layer is lowered and the coating layer is easily peeled off. When the amount of the compound was large (Sample 11), it took time to cure and the hardness of the coating layer was low. Moreover, when the amount of the silicon compound relative to 100 parts by weight of the organosiloxane oligomer was in the range of 0.1 to 20 parts by weight, good properties were exhibited.

(III) Influence of Titanium Compound As shown in Table 7, when the amount of the titanium compound is small (Sample 12), fingerprints are likely to adhere to the coating layer, and conversely, when the amount of the titanium compound is large (Sample 15). ), It was difficult to repeat the coating material. Moreover, when the amount of the titanium compound relative to 100 parts by weight of the organosiloxane oligomer was in the range of 0.1 to 50 parts by weight, good properties were exhibited.

Claims (11)

  Luminescent coating material comprising a composition comprising an organosiloxane oligomer, a catalyst, a silane compound, a titanium compound, and a luminous pigment, the viscosity of which is adjusted to 50 to 300 mPa · s at 25 ° C   The phosphorescent coating material according to claim 1, wherein the organosiloxane oligomer has one or more substituents.   The phosphorescent coating material according to claim 1 or 2, wherein the catalyst is an acid compound, an alkali compound, a salt compound, or an organometallic compound.   The phosphorescent coating material according to claim 1, wherein the silane compound contains at least a silane coupling agent.   The phosphorescent coating material according to claim 4, wherein the silane compound has any functional group of glycidyl group, amino group, and vinyl group.   The phosphorescent coating material according to claim 1, wherein the titanium compound is di-i-propoxy bis (acetylacetonato) titanium.   The phosphorescent coating material according to claim 1, wherein the livestock pigment is a metal compound-based pigment. Applying the phosphorescent coating material according to any one of claims 1 to 7 at a coating film of 10 μm or less to a tangible object composed of concrete, earth, paper, plastic, metal, and wood;
A layering process that repeats the coating process several times,
A drying step of drying the phosphorescent coating material applied by natural drying or forced drying, and a coating method using the phosphorescent coating material.   The phosphorescent according to claim 8, wherein the coating process is completed within 30 minutes immediately after the start of the coating operation, and is allowed to stand for 10 to 120 minutes after the coating process is completed to allow the silanolization reaction to proceed, and then the overcoating process is performed. Coating method using conductive coating material.   The coating method using the luminous coating material in any one of Claims 8-9 which performs an overpainting process twice or more.   The drying step is a step of performing natural drying for 3 hours or more or a step of forced drying at 50 to 150 ° C for 5 to 60 minutes after performing natural drying for 30 to 60 minutes. Coating method using phosphorescent coating material.