KR20080101462A - Non-solvent typed epoxy base adhensive composition - Google Patents

Abstract

A solvent-free epoxy-based adhesive composition is provided to ensure excellent workability, high adhesive strength, and environment friendly property by generating a low level of volatile organic compound(VOC) or formaldehyde. A solvent-free epoxy-based adhesive composition comprises an epoxy-based resin 5~15 weight% of which viscosity is 5,000~20,000 centi poise; a hardener 3~10 weight% of which viscosity is 100~7,000 centi poise, which contains a polyamide resin; a tackifier 4~8 weight% which is a natural resin; a curing accelerator 1~6 weight%; a diluent 5~10 weight%; a filler 56~88.9 weight%; a dispersing agent 0.1~5 weight%; and additives 0~5 weight%. The epoxy-based resin has 150~300 of equivalent and 2-4 functional groups and is one kind selected from a bisphenol A type epoxy resin, a bisphenol F type epoxy resin and a novolac type epoxy resin.

Description

Non-solvent type epoxy base adhensive composition

1 is a cross-sectional view showing a state in which the flooring adhesive, construction on the concrete with an adhesive composition according to the present invention.

Figure 2 is a schematic diagram showing the process of bonding the flooring on the concrete with the adhesive composition according to the invention.

* Explanation of symbols on the main parts of the drawings

1: concrete 2: solvent-free epoxy adhesive

3: flooring (floorboard)

The present invention relates to a solventless epoxy adhesive composition, and more particularly, to a solventless epoxy adhesive composition mainly used for bonding and constructing floorboards for indoor ondol on concrete floors.

Various flooring materials such as polyvinyl chloride (PVC) flooring, parquet flooring, cork tiles, and carpet tiles are applied to concrete floors of houses, commercial buildings, apartments, etc. using adhesives. At this time, the adhesive to be used should not only have excellent adhesion to adhere the adherend (concrete bottom) and the flooring material, but also be resistant to moisture and alkali, and maintain the adhesive strength so that the dimensional change of the flooring material is less likely to occur.

As the adhesive having such physical properties, two-component resins such as epoxy resins and polyurethane resins are used. One-component resins such as acrylic resins are used as adhesives for cork tiles, but are less suitable for use as wood flooring materials due to their lower adhesive strength than epoxy resins. Accordingly, in order to use the two-component resin, a strong solvent must be used at the time of work, and the toxic odor is generated thereby causing damage to the residents such as environmental pollution and so-called sick house syndrome.

Specifically, an organic solvent such as benzene, toluene, xylene, methyl ethyl ketone (MEX), or a mixed type thereof may be used as the organic solvent of the adhesive using the two-component resin. Therefore, volatile organic compounds (VOCs) or formaldehydes (VOCs), which are harmful to humans and the environment, are released from adhesives, which is problematic.

In order to improve the above problems, alcohols (aqueous) solvents having low or no toxicity such as methanol, ethanol and isopropanol (IPA) are used instead of the organic solvents, but alcohol solvents are also stabilized. For this purpose, there is a problem that their use is increased and there is still a risk of toxicity when exposed to the human body for a long time.

As a coping technology, water-based adhesive products have been released in recent years due to development of products that are harmless to the human body and have environmentally friendly characteristics. Aqueous refers to a method of using a resin obtained by dispersing a fat-soluble resin in a micelle state in water as an emulsification method using a surfactant. Epoxy, urethane, and acrylic emulsion resins are typical. The resins employed in this manner are basically high hydrophilic resins for emulsification and stabilization in water, and thus have disadvantages in that adhesive strength and physical properties are poor. Furthermore, since the adhesive composition contains water, the remaining water after construction causes a decrease in adhesion.

The present invention is to solve the above problems, the object of the present invention is excellent in water resistance, heat resistance, alkali resistance, eliminating the cause of physical property degradation by water of the aqueous product while having environmentally friendly properties and harmless to human body type epoxy It is to provide an adhesive composition.

Still another object of the present invention is to provide a solventless adhesive composition for solvent-free epoxy adhesives having excellent adhesion.

Hereinafter, the present invention will be described in detail.

The solvent-free epoxy adhesive composition according to the present invention has a viscosity of 5 to 15% by weight of an epoxy resin having a viscosity of 5,000 to 20,000 centipois, and a curing agent of 3 to 10 weight of a viscosity of 100 to 7,000 centipois and containing a polyamide resin. %, Natural resin resin tackifier 4-8% by weight, curing accelerator 1-6% by weight, diluent 5-10% by weight, filler 56-88.9% by weight, dispersant 0.1-5% by weight and additive 0-5% by weight Characterized in that configured.

The solvent-free epoxy adhesive composition according to the present invention contains a low viscosity epoxy resin and a curing agent because it does not contain a solvent.

Specifically, the epoxy resin has a viscosity of 5,000 to 20,000 centipoas, an equivalent weight of 150 to 300, preferably having 2 to 4 functional groups, and specific examples thereof include epoxy resins of bisphenol-A type and bisphenol-F. Epoxy resins of the type or Novlac type epoxy resins.

The curing agent is preferably a curing agent having a rigid structure such as aromatic (Aromatic) in order to increase the resin strength after curing, but such a structure has a viscosity of 10,000 centipoas or more basically has a problem of workability. In the present invention, a diluent is basically used to lower the viscosity. However, since the organic solvent and a solvent such as alcohol or aqueous water are not used, there is a limit in controlling the viscosity with the diluent alone. A low viscosity curing agent in the range of 100-7,000 centipois is therefore preferred for curing agent selection. More preferably, it is the range of 500-3,000 centipoas viscosity.

As said hardening | curing agent, it is good to use resin, such as a polyamide type or a polyamine type, individually or in mixture. Reactive functional water can be used for both the multifunctional curing agent in the monofunctional group.

As the tackifier, any resin that satisfies the initial tack can be used. However, the resin used as a tackifier is a resin having a low molecular weight, the drying is slow, and a resin having a high molecular weight is bad or fast dispersibility, the adhesive state is showing a lot of differences depending on the degree of their mixing, so the selection of the adhesive resin is also an important factor. . In the present invention, a natural resin was used as the tackifier. The natural resin may be any resin used as a tackifier among the resins present in nature, but representative examples thereof include ester rosin such as ester gum, hydrogenated rosin and natural rosin such as high rosin. Can be. If more than the above amount is used, there is a problem in that the long-term storage in the adhesive composition (migration) to inhibit storage stability, or inhibit the adhesive strength after complete curing. When used below the above amount, there is a problem that the initial adhesion characteristics are poor, causing separation between deposits before complete curing.

The curing accelerator acts to speed up the curing of the adhesive to shorten the adhesion time and increase the strength. All of the conventionally used curing accelerators having the above characteristics can be used, and in particular, nonylphenol, trisphenol, bisphenol or lithium carbonite is preferably used.

The content of the curing accelerator is 1 to 6% by weight.

When the content is in the above range, it is possible to significantly shorten the curing time of the adhesive, in particular, there is an effect that can significantly improve the low temperature curing properties. When an excessive amount is used in the above range, the properties of adhesive strength, workability, and viscosity are significantly worsened, and curing may proceed too quickly, thereby reducing the pot life. If the amount is used within the above range, complete curing does not occur, or a long time is required for complete curing.

The diluent has suitable fluidity and flowability when the flooring construction works, and has the purpose of use for improving thixotropy, bone formation, coating property and pot life while having permeability suitable for variation of plywood and difference in absorbency. As the reaction functional group of the diluent, a viscosity of 10 to 1,000 centipoas is preferable while having functional groups such as epoxy, amine, amide, isocyanate, alcohol, and acid. The number of functional groups is preferably in the range of 5 to 10% by weight while having 1 to 2 functional groups. When the above amount is used, it adversely affects bone formation and storage stability, and when it is used below this amount, it is difficult to control the viscosity.

As the reactive diluent component, a product having 16 or more carbon atoms and a molecular weight of 250 or more should be selected so as not to affect the human body and the environment. In particular, it is suitable to use polyethylene glycol, glycerol (Glycerol), glycidyl ether (Glycidyl ether), polyethylene glycol butyl ether, polypropylene glycol and the like.

The adhesive composition of the present invention further comprises a filler to increase physical properties such as dimensional stability and heat resistance, the amount of which is 56 to 88.9% by weight based on the total composition weight. As the filler, any compound can be used as long as this object can be achieved. Representative examples include calcium carbonate (CaCo ₃ ) and clay (Clay), diatomaceous earth, silica (SiO ₂ ). Inorganic fillers are also aimed at reducing the shrinkage during curing to compensate for workability and reducing costs by controlling the viscosity of the adhesive.

The dispersant is a modified polyester compound or the like, and the additive is an ink, a thickener, liquid paraffin, or the like.

Solvent-free epoxy-based adhesive composition according to the present invention has been transported at the construction site for bonding and construction of flooring material on the cement floor surface, respectively

(i) 10-30 wt% epoxy resin, 5-20 wt% tackifier, 1-12 wt% diluent, 28-83.9 wt% filler, 0.1-5 wt% dispersant and 0-5 wt% additive Subject slurry in slurry state and

(ii) slurry consisting of 20 to 60% by weight of curing agent, 0.1 to 12% by weight of curing accelerator, 5 to 20% by weight of diluent, 38 to 89.8% by weight of filler, 0.1 to 5% by weight of dispersant and 0 to 5% by weight of other additives. It is prepared by mixing the curing agent slurry in a state.

It is preferable that the viscosity of the main slurry is 25,000 centipoas level, the viscosity of the curing agent slurry is 20,000 centipois level, and the viscosity of the solvent-free epoxy adhesive composition mixed therewith is 30,000 centipoas.

Hereinafter, the present invention will be described in detail through examples and comparative examples.

However, the present invention is not limited by the following examples.

Example  One

First, a solvent-free epoxy adhesive composition having a composition as shown in Table 3 is prepared by mixing a main slurry having a composition as shown in Table 1 below and a curing agent slurry having a composition as shown in Table 2 in a 1: 1 equivalent ratio.

Next, the prepared solvent-free epoxy adhesive composition is applied on the concrete 1 as shown in FIG. 2 to form a bone.

Next, the flooring material 3 is placed on the solventless epoxy adhesive 2 formed on the concrete 1 so that the bone is formed, and then a load is applied to the flooring material 3 on the concrete 1. , Construction.

The results of evaluating the amount of volatile organic compounds and formaldehyde released, adhesive strength and workability after construction are shown in Table 10.

Theme Slurry Composition ingredient content Epoxy resin 20 wt% Tackifier 12 wt% diluent 10 wt% Filler 57 wt% Dispersant 0.2 wt% additive 0.8 wt%

Hardener Slurry Composition ingredient content Hardener 10 wt% Curing accelerator 8 wt% diluent 10 wt% Filler 71 wt% Dispersant 0.2 wt% additive 0.8 wt%

Solvent-free epoxy adhesive composition ingredient content Epoxy resin 10 wt% Hardener 5 wt% Tackifier 6 wt% Curing accelerator 4 wt% diluent 10 wt% Filler 64 wt% Dispersant 0.2 wt% additive 0.8 wt%

Comparative Example  One

First, a water-soluble epoxy adhesive composition having a composition as shown in Table 6 is prepared by mixing a main slurry having a composition as shown in Table 4 below and a curing agent slurry having a composition as shown in Table 5 in a 1: 1 equivalent ratio.

Next, the prepared water-soluble epoxy adhesive composition is applied on the concrete 1 as shown in FIG. 2 to form bone.

Next, the flooring material 3 is placed on the water-soluble epoxy adhesive 2 formed on the concrete 1 so that the bone is formed, and then a load is applied to the flooring material 3 on the concrete 1. It was constructed.

The results of evaluating the amount of volatile organic compounds and formaldehyde released, adhesive strength and workability after construction are shown in Table 10.

Theme Slurry Composition ingredient content Epoxy resin 20 wt% Tackifier 12 wt% Methanol 10 wt% Filler 57 wt% Dispersant 0.2 wt% additive 0.8 wt%

Hardener Slurry Composition ingredient content Hardener 12 wt% Curing accelerator 5 wt% Methanol 10 wt% Filler 72 wt% Dispersant 0.2 wt% additive 0.8 wt%

Water Soluble Epoxy Adhesive Composition ingredient content Epoxy resin 10 wt% Hardener 5 wt% Tackifier 6 wt% Curing accelerator 4 wt% Methanol 10 wt% Filler 64 wt% Dispersant 0.2 wt% additive 0.8 wt%

Comparative Example  2

First, an aqueous epoxy adhesive composition having the composition shown in Table 9 is prepared by mixing a main slurry having the composition shown in Table 7 below and a curing agent slurry having the composition shown in Table 8 in a 1: 1 equivalent ratio.

Next, the prepared aqueous epoxy adhesive composition is applied onto the concrete 1 as shown in FIG. 2 to form bone.

Next, the flooring material 3 is placed on the water-based epoxy adhesive 2 formed on the concrete 1 so that a valley is formed, and then a load is applied to the flooring material 3 on the concrete 1. It was constructed.

The results of evaluating the amount of volatile organic compounds and formaldehyde released, adhesive strength and workability after construction are shown in Table 10.

Theme Slurry Composition ingredient content Epoxy resin 20 wt% Tackifier 12 wt% water 10 wt% Filler 57 wt% Dispersant 0.2 wt% additive 0.8 wt%

Hardener Slurry Composition ingredient content Hardener 10 wt% Curing accelerator 8 wt% water 5 wt% diluent 10 wt% Filler 71 wt% Dispersant 0.2 wt% additive 0.8 wt%

Aqueous Epoxy Adhesive Composition Composition ingredient content Epoxy resin 10 wt% Hardener 5 wt% Tackifier 6 wt% Curing accelerator 4 wt% water 5 wt% diluent 5 wt% Filler 64 wt% Dispersant 0.2 wt% additive 0.8 wt%

Property evaluation result division Standard standard Example 1 Comparative Example 1 Comparative Example 2 Formaldehyde Release (mg / ㎡h) 0.02 (Based on Environmental Mark) 0 0.001 0 Total Volatile Organic Compound Emissions (mg / ㎡h) 0.40 (Based on Environmental Mark) 0.080 0.05 0.07 Volatile Organic Compound Content (% by weight) 0.1 0.074 4.000 0.010 Adhesive strength (kgf / ㎠) Standard room temperature 8.16 35.55 35.1 21.6 Domestic consumption 5.1 24.77 22.3 13.2 Heat resistant 5.1 29.84 30.5 18.7 Workability Mixed workability - Great Great usually Bone formation rate - Great Great usually Pot life (minutes) - 300 (± 60) 150 (± 60) 240 (± 60)

In Table 10, formaldehyde emission and total volatile organic compound emission were measured by indoor air quality test method (Ministry of Environment Notice 2004-80), and volatile organic compound content was measured by ISO 11890-1: 2000 (E) method. Adhesion strength was measured by KSF 3818: 2003 method, mixing workability and bone formation rate by visual and sensory tests, and pot life was measured by KS M3705 method.

The present invention is environmentally friendly because it does not emit volatile organic compounds (VOC) or formaldehyde, it is excellent in workability and adhesive strength.

Claims (10)

5 to 15% by weight of epoxy resin with a viscosity of 5,000 to 20,000 centipoas, 3 to 10% by weight of a curing agent containing a polyamide resin with a viscosity of 100 to 7,000 centipoas and a tackifier 4 to 8 of natural resin A solvent-free epoxy adhesive composition comprising weight%, curing accelerator 1-6 wt%, diluent 5-10 wt%, filler 56-88.9 wt%, dispersant 0.1-5 wt% and additive 0-5 wt% . The solvent-free epoxy adhesive composition according to claim 1, wherein the epoxy resin has an equivalent weight of 150 to 300 and has 2 to 4 functional groups. The non-solvent type epoxy adhesive composition according to claim 1, wherein the epoxy resin is one selected from a bisphenol-A type epoxy resin, a bisphenol-F type epoxy resin, and a Novolac type epoxy resin. The solvent-free epoxy adhesive composition according to claim 1, wherein the curing agent is one selected from polyamide resin, polyamine resin, and mixed resins thereof. The solvent-free epoxy adhesive composition according to claim 1, wherein the tackifier is one selected from a natural rosin resin, an ester rosin resin, and a hydrogenated rosin resin. The non-solvent type epoxy adhesive composition according to claim 1, wherein the curing accelerator is one selected from nonylphenol, trisphenol, bisphenol, and lithium carbonate resin. The diluent is one or more selected from polyethylene glycol, glycerol, glycidyl ether, polyethylene glycol butyl ether, and polypropylene glycol having 16 or more carbon atoms and a molecular weight of 250 or more. Solvent free epoxy adhesive composition. The solvent-free epoxy adhesive composition according to claim 1, wherein the filler is one selected from calcium carbonate, clay, kaolin, and silica. The solvent-free epoxy adhesive composition according to claim 1, wherein the dispersant is a modified polyester compound. The solvent-free epoxy adhesive composition according to claim 1, wherein the additive is one selected from ink, biodiesel, and liquid paraffin.

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