KR100988040B1 - Polyurethane-modified waterproof coating material and producing method of the same - Google Patents

Abstract

The present invention relates to a polyurethane-modified asphalt waterproof coating composition and a method for producing excellent physical and chemical properties such as adhesion, water resistance (water resistance), durability, wear resistance, and permanent elasticity. Specifically, 5 to 50% by weight of petroleum-based asphalt, 1 to 20% by weight of isocyanate compound, 10 to 50% by weight of hydroxyl resin having a number average molecular weight of 100 to 100,000, and 20 to 50% by weight of surface-treated reactivity It relates to a polyurethane-modified asphalt waterproof coating composition and a method for producing the same, comprising an inorganic filler.

Asphalt, Paint, Polyurethane, Waterproof

Description

Polyurethane-modified waterproof coating material and producing method of the same}

The present invention relates to a composition of a polyurethane-modified asphalt waterproof coating agent having excellent physical and chemical properties such as adhesion, water resistance (water resistance), durability, abrasion resistance, and permanent elasticity, and a manufacturing method thereof.

Asphalt waterproofing agent produced in Korea is produced after mixing and dissolving asphalt in petroleum solvent. In addition, asphalt can be prepared by dissolving a mixture of polymer modifiers, such as US Patent No. 3985694, in a petroleum-based solvent, and the epoxy, amine, carboxylic acid, and hydroxyl functional groups in the main chain as shown in Korean Patent Application Publication No. 97-700234. It can be prepared by mixing a curing agent such as amine, alcoholic acid, polyol, polyacid. In addition, as disclosed in Korean Patent Application Publication No. 96-701955, a method of increasing the viscosity by adding an oxidizing agent ferric chloride (FeCL) is also disclosed.

        Asphalt waterproofing coating prepared by this method is not compatible with asphalt components, resin components, aromatic components, osmotic components, etc. in asphalt, so phase separation during long-term storage or high temperature storage results in aging and phase separation due to the inherent curability of asphalt. However, there is a problem that a poor phenomenon occurs by exposure of foreign matter.

The purpose of the present invention is to chemically react petroleum-based asphalt, isocyanate-based compounds, synthetic resins having a number-average molecular weight of 100 to 100000 with hydroxy groups, and reactive inorganic materials that are surface-treated, thereby improving adhesion, abrasion resistance, durability, aging resistance, permanent elasticity, and the like. The present invention provides a composition of polyurethane modified asphalt waterproofing agent and a method of manufacturing the same which have excellent physical and chemical properties.

Still another object of the present invention is to provide a polyurethane modified asphalt waterproof coating composition which improves the physical properties of the coating agent by improving the compatibility and dispersibility of the inorganic filler with the resin by surface treatment of the inorganic filler.

5 to 50% by weight of petroleum-based asphalt, 1 to 20% by weight of isocyanate compound, 10 to 50% by weight of synthetic resin having a number average molecular weight of 100 to 100,000, and 20 to 50% by weight of surface-treated reactive inorganic filler It provides a polyurethane modified asphalt waterproof coating composition comprising a.

It also provides a method for producing the composition comprising the following steps.

5 to 50% by weight of petroleum asphalt and 10 to 50% by weight of petroleum solvent are mixed and dissolved, then 1 to 20% by weight of isocyanate is added and the amount of free isocyanate becomes 40 to 60% of the theoretical value. First reaction step to proceed the reaction at 25 ~ 40 ℃;

A secondary reaction step of mixing the reaction mixture with the surface-treated reactive inorganic filler in an amount of 20-50% by weight and proceeding at room temperature until the amount of free isocyanate is 10-20% based on the theoretical value;

10 to 50% by weight of a synthetic resin having a number average molecular weight of 100 to 100,000 having a hydroxy group in the secondary reaction product is mixed and dispersed, and the reaction is performed until the homogeneous solution is formed without free isocyanate after 25 to 55 ° C. 3rd step.

 According to the present invention, a waterproof coating agent exhibiting waterproofness of asphalt, elasticity of polyurethane, and heat resistance and weather resistance of an inorganic material is produced. This waterproof coating agent is an economical civil building material that reinforces the durability of building with excellent waterproofness, index, corrosion protection and anti-corrosion property when applied to concrete, cement and steel structures.

In addition, the surface treatment of the inorganic filler improves the compatibility and dispersibility of the inorganic filler with the resin, ultimately increasing the physical properties of the coating agent more efficiently.

5-50% by weight of petroleum-based asphalt, 1-20% by weight of isocyanate compound, 10-50% by weight of synthetic resin having a number average molecular weight of 100-100000, 20-50% by weight of surface-treated reactive inorganic filler It provides a polyurethane modified asphalt waterproofing coating composition comprising a.

As for the petroleum-based asphalt in this invention, it is preferable to use the asphalt which has the penetration | invasion degree of 25 degreeC 100-400, and the dynamic viscosity of 60 degreeC has a range of 0.001-1.0 m <2> / s. As this asphalt is the final material of petroleum products, it is economically advantageous and waterproof. However, when added too much, the elongation in the final physical properties may result in poor, it is preferable to use 5 to 50% by weight.

The isocyanate compound in the present invention may be isophorone diisocyanate (IPDI), methylene diisocyanate (MDI), nuxamethylene diisocyanate (HMDI), isopron diisocyanate (IPDI), or a mixture of two or more thereof.

This serves as a curing agent, it is preferable to add 1 to 20% by weight.

The synthetic resin of the present invention is a synthetic resin having a number average molecular weight of 100 ~ 100,000 with a hydroxyl group. Any one or two or more synthetic resins selected from acrylic resins, vinyl resins, polyester resins, polyether resins, polyester resins, rubber modified resins, polybutadiene resins, and petroleum resins may be selected and added. Preferably, a polyester resin, a polyacrylic resin, or a polybutadiene resin having a number average molecular weight of 100 to 100,000 may be selected. The synthetic resin is for reinforcing adhesion and increasing tensile strength, heat resistance, durability, and coating strength (or elasticity). The addition ratio is preferably 10 to 50% by weight.

The inorganic filler in the present invention is surface-treated with a silane coupling agent, and any one or two or more selected from titanium oxide, silica, calcium carbonate, mica, talc, wollastonite, bentonite, and the like may be added. This inorganic filler serves to improve the durability and heat resistance of the final product. If too little is added, the improvement of durability and heat resistance is insignificant. If too much is added, the adhesion of the coating agent is inferior. Therefore, it is preferable to add 20 to 50% by weight.

At this time, since these inorganic fillers have a problem of poor compatibility with filler and resin when simply added and mixed, it is important to surface-treat the coupling agent which is a silane compound for compatibility and even dispersibility of the inorganic filler with resin. . The silane compound is tetramethoxysilane (TMOS), tetraethoxysilane

Tetraethoxysilane (TEOS), methyltrimethoxy silane (methyltrimethoxy silane), methyltriethoxy silane (methyltriethoxy silane), aminopropyltrimethoxy silane (Aminopropyltrimethoxy silane) or one or more selected may be used.

In order to achieve the object of the present invention provides a manufacturing method as follows.

(First reaction stage)

5-50% by weight of petroleum asphalt and 10-50% by weight of a petroleum solvent are mixed and dissolved, followed by reacting 1 to 20% by weight of an isocyanate monomer. After the reaction at 25 to 40 ° C. for 3 to 5 hours, the first reaction is completed when the amount of free isocyanate becomes 40 to 60 wt% of the theoretical value.

The petroleum solvent may be used a general petroleum solvent such as kerosene, diesel, solvent, mineral oil. This petroleum solvent serves as a function of viscosity control of asphalt and facilitates dispersibility.

Among the structures of R-NCO of diisocyanate, NCO (isocyanic acid type structure) can be quantitatively analyzed by a wet analysis method, and the quantitative analysis of NCO at the initial stage of the reaction is called a theoretical value of isocyanate. The quantitative analysis of the NCO measured during the reaction is confirmed as a ratio to the initial NCO theory to determine the stage of the reaction. Only when the reaction proceeds in this step can be induced to improve the physical properties of the uniform asphalt adhesive through the urethane reaction of the present invention.

(Second reaction stage)

20-50 wt% of the surface-reactive reactive inorganic filler is mixed with the primary reaction product, and the room temperature reaction is performed until the amount of free isocyanate is 10-20 wt% of the theoretical value. At this time, the inorganic filler uses any one or a mixture of two or more selected from titanium oxide, silica, calcium carbonate, mica, talc, wollastonite, bentonite, etc., which have been surface treated with a silane coupling agent.

(3rd reaction step)

One or two or more selected from acrylic resin, vinyl resin, polyester resin, poly ether resin, polystyrene resin, rubber modified resin, polybutadiene resin, petroleum resin, etc., in the secondary reaction product, number average molecular weight of 100 to 100,000 10 to 50% by weight of the mixed resin and dispersed after the cross-linking reaction proceeds at 25 ~ 55 ℃ after the reaction is carried out until the free isocyanate is uniform solution without the presence.

The coating composition of the present invention can be used as such, and in particular, in order to improve heat resistance and durability, a polyisocyanate compound may be added and used during construction. As a result, it is possible to flexibly use the suitable physical properties according to the use purpose or construction conditions of the waterproofing coating agent. At this time, the compounding quantity of this polyisocyanate compound can be 3-15 weight part of polyisocyanate compounds, More preferably, 5-10 weight part with respect to 100 weight part of polyurethane modified asphalt waterproofing coatings from a viewpoint of adhesive force.

Preferred embodiments of the present invention are as follows. However, this is only an example for the implementation of the invention, it is apparent from the position of those skilled in the art that the technical concept of the invention is not limited to the embodiments.

Example 1 Preparation of Polyurethane Modified Asphalt Waterproofing Coating Composition

(First reaction stage)

     500 g of asphalt for asphalt (asphalt cement), 500 g of diesel oil, dissolved in a three-necked stainless reactor, and slowly dissolved at 50 ° C., 50 g of TDI (toluenediisocyanate) was added and maintained at 25 to 40 ° C. for 3 hours to react with asphalt to maintain the amount of free isocyanate. The reaction is stopped when quantitative analysis reaches 50% of the theoretical value.

(Second reaction stage)

After diluting 10 g of aminopropyltrimethoxy silane in 500 g of solvent naphtha in a separate stainless steel reactor, adding 500 g of 200 mesh silica powder, dispersing it for 3 hours, and surface-treating the first reaction solution After mixing the surface-treated silica slowly while stirring, the reaction proceeds so that the amount of free isocyanate is 10 to 20% based on the theoretical value.

(3rd reaction step)

     50 g of ethylene glycol-modified polyol (molecular weight 1000) having a hydroxyl group was added to the secondary reaction solution, and free isocyanate was completely reacted at 40 to 50 ° C. to complete the synthesis.

The characteristics of the synthesized composition of the present invention are as follows.

Appearance is black viscous liquid, specific gravity is 1.4 (25 degreeC), and a viscosity is 6000-8000 cps (25 degreeC). Soluble in solvent naphtha, aromatic solvent.

[Test 1] Performance test of asphalt waterproofing agent

As a result of the comparison test between the polyurethane modified asphalt waterproof coating agent and the conventional asphalt waterproofing agent, the polyurethane modified asphalt waterproof coating agent was excellent in adhesion, abrasion resistance, flexural strength, elasticity, heat resistance, and aging resistance. Details are shown in Table 1.

[Table 1] Comparison of existing waterproof coating agent and effect

[Test 2] Comparison of tensile strength and elongation rate with existing waterproof coating agent

The tensile performance of this invention is compared with a comparative example and an experiment is carried out. Figure 1a is a test piece of the coating film produced according to the embodiment of the present invention, Figure 1b is a conventional air brown asphalt coating product (hereinafter referred to as ABA) as a comparative example. Tensile strength and elongation are measured for comparison of tensile performance. Three specimens of the present invention and ABA are prepared. The specimens are cured for 4 days in the specimen form, and the specimen standard is KS M 6518.

After each specimen has been left in the standard condition for at least one hour, the specimen is attached to a tensile tester with a bleeding interval of 60 mm and tensioned until the specimen breaks at a tensile speed of 500 mm / min.

[Table 2] Tensile performance test results

Table 2 is the experimental results, Figure 2 is a photograph of the specimen cut in the tensile performance test of the specimen.

In the present invention, as shown in the above table, the tensile strength was improved by about 2 times compared to the existing product, and the elongation was also improved by 2.5 times. Figure 2a is a cutting picture of the present invention because of high tensile strength and elongation was cut without deformation of the body. However, the ABA of c 2 b did not retain its shape and was increased, but was cut off in its extended state without being restored.

The experimental results show that the present invention has excellent durability due to the high tensile strength and excellent adaptability to expansion and contraction of the lower surface (concrete bottom, etc.) after being constructed by the large elongation.

1 is a photograph of the specimen prepared for the tensile performance test

Figure 2 is a photograph of the specimen cut through the tensile performance test

Claims (4)

delete delete delete 5-50 wt% of petroleum asphalt and 10-50 wt% of petroleum solvent are mixed and dissolved, and then 1-20 wt% of isocyanate compound is added and the amount of free isocyanate is 40-60% of the theoretical value. The first reaction step of proceeding with the reaction at 25 ~ 40 ℃ until the time point; A second reaction step of mixing the surface-reactive reactive inorganic filler in the first reaction product at 20 to 50% by weight and proceeding at room temperature until the amount of free isocyanate is 10 to 20% based on the theoretical value; 10 to 50% by weight of a synthetic resin having a number average molecular weight of 100 to 100,000 having a hydroxy group in the secondary reaction product is mixed and dispersed, and the reaction is performed until the homogeneous solution is formed without free isocyanate after 25 to 55 ° C. Third reaction step: Method of producing a polyurethane modified asphalt waterproofing coating composition comprising a.

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