KR20030064660A - polyurethane adhesive for flooring and process - Google Patents

Abstract

PURPOSE: Provided is a quick moisture curing adhesive by reacting with the moisture in the air. The adhesive composition has high adhesive strength, improved heat resistance to be used on ondol floor and high moisture resistance to endure the moisture during monsoon seasons. The composition is used for PVC and rubber tiles and floor materials. CONSTITUTION: The composition comprises: 10-30wt.% of bi-functional polyether polyol with number average molecular weight of 1000-3000; 10-15wt.% of tri-functional polyether polyol with number average molecular weight of 3000-6000; 5.0-13wt.% of toluene diisocyanate, 9.5wt.% of diphenylmethane diisocyanate(MDI) and 0.5-1.0wt.% of polymeric MDI; 0.5wt.% of bi-functional glycol consisting of 1,4-butanediol; 26-30wt.% of filler containing talc; 0.2-0.5wt.% of benzoyl chloride; 0.8-1.0wt.% of sodium silico aluminate; and 9.0-10wt.% of toluene, 8.0-8.5wt.% ethylacetate and 0.5-1.0wt.% of methyl ethyl ketone. The preparation method comprises the following steps of: adding bi-functional polyether polyol and tri-functional polyether polyol into a reactor and heating to 70-120deg.C to eliminate moisture and stirring at 45-60rpm to make a homogeneous liquid; making primary polyurethane prepolymer with terminal NCO by adding diisocyanates composed of TDI, MDI and polymeric MDI and heating under atmospheric pressure and under nitrogen atmosphere at the temperature above 75deg.C for 10-14 hours, and adding bi-functional glycols and chain extenders such as ethylene glycol and 1,4-butanediol to make secondary polyurethane prepolymer; adding to the secondary polyurethane prepolymer, fillers such as talc or calcium carbonate, mixing for 2 hours and adding a reaction retarder such as benzoyl chloride and a moisture absorber such as sodium silico aluminate to make stabilized synthetic materials; and adding solvents such as toluene, ethylacetate and methyl ethyl ketone, and then mixing it for 4 hours.

Description

Polyurethane adhesive composition and its manufacturing method {polyurethane adhesive for flooring and process}

Since general adhesives for floor decoration are manufactured under normal temperature and standard humidity, when adhesives are used under high temperature and high humidity during the rainy season in summer, the adhesive strength decreases due to high temperature and high humidity. When the adhesive construction in the state of low temperature there was a problem such that a lot of time elapsed before curing. In order to improve this, there was a method of curing a short period of time by adding a separate curing accelerator including tin-based catalyst in the market, but this also requires a separate catalyst to be used and added to the adhesive every time the adhesive is used. It became.

In order to supplement the limitations of the adhesives used in the conventional floor decoration materials as described above, using one type of adhesive without the need for a separate curing accelerator, it reacts with moisture in the air during adhesion construction and cures in a short time to improve the workability and cost It is a technical object of the present invention to provide a moisture-curable adhesive that can bring about savings, and also to provide an adhesive capable of improving heat resistance, water resistance, and the like, and improved adhesive strength after construction.

As described above, it is an urgent need to develop an adhesive having a structure that can be easily bonded and cured without deteriorating physical properties such as adhesive strength when the floor decorative material such as a pvc tile is adhered.

The present invention is to provide an adhesive and a method of manufacturing the structure that can use only one type of adhesive without using a separate curing accelerator to improve the workability and adhesion strength in order to meet the needs of the times.

First, the composition of the adhesive according to the present invention will be described.

Adhesive composition according to the present invention

1) bifunctional polyether polyol,

2) trifunctional polyether polyols,

3) diisocyanate,

4) difunctional glycol

5) fillers

6) solvent

7) reaction inhibitor

8) It consists of moisture absorbent.

When the composition of the present invention is 100% by weight of the finished product, it is a preforma of an adhesive raw material, which is 10-30% by weight of bifunctional polyether polyol having a number average molecular weight of 1000-3000 and a number average molecular weight of 3000-6000. 10-15% by weight of trifunctional polyether polyol, 5.0-13% by weight of toluene di-isocyanate, 9.5% by weight of di-phenyl methene di isocianate, and polymeric MDI MDI) to form polyurethane preforma with 0.5-1.0% by weight of di-isocyanate.

As a chain extender used in the present invention, 0.5% by weight of bifunctional glycols such as ethylene glycol and 1,4butanediol are used. As the filler, talc or calcium carbonate is used, preferably 26-30% by weight, and benzoyl corride as a reaction inhibitor for inhibiting self-reaction during storage of the polyurethane preforma formed as described above. 0.2-0.5 wt% of (benzoyl chloride), 0.8-1.0 wt% of sodium sillico alluminate as a water absorbent to absorb moisture, and 9.0-10.0 wt% of toluene It is characterized by producing a moisture-curable polyurethane one-component adhesive, the final product by adding a solvent of 8.0-8.5% by weight of ethyl acetate, 0.5-1.0% by weight of methyl ethyl ketone.

The following is a manufacturing method for producing the polyurethane one-component adhesive, wherein each of the composition ratios mentioned in the composition,

(1) Pump the bifunctional polyether polyol and trifunctional polyether polyol into the reactor, heat it to a temperature of 70 ° C -120 ° C, remove the water in the polyol, and make a uniform liquid. After stirring at -60 RPM,

(2) Di-isocyanate, such as toluene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), or polymeric MDI, was added and reacted for 10-14 hours at 75 ° C or above in an atmospheric pressure and nitrogen atmosphere. To produce a primary polyurethane preforma having a group,

(3) A bifunctional glycol such as ethylene glycol, 1,4 butanediol, which is a chain extender, is added to the primary polyurethane preforma produced as described above to produce a secondary polyurethane preforma.

(4) After adding talc or calcium carbonate as a filler to the secondary polyurethane preformer for 2 hours or more, and adding benzoyl corrolide and water absorbing sudsilico aluminate as a reaction inhibitor to stabilize the composite. ,

(5) Moisture-curable polyurethane with 9,000-13,000 CPS / 20 ° C, solid content of 70-90% of solids which is easy to work by adding solvent such as toluene, ethyl acetate, methyl ethyl ketone and mixing for 4 hours or more A liquid adhesive is prepared.

Hereinafter, the present invention will be described in detail with reference to Examples.

(Example 1)

The raw materials and the additives according to the first embodiment of the present invention are represented by weight%.

20% by weight of bifunctional polyether polyol

15% by weight of trifunctional polyether polyol

Toluene diisocyanate 13 weight

0.5% by weight of ethylene glycol

Calcium Carbonate 30% by weight

Benzoyl corrolide 0.5 wt%

Sudden silico aluminate 1.0 wt%

Toluene 10% by weight

Ethyl acetate 8.5% by weight

Methyl ethyl ketone 1.5 wt%

20 wt% of the bifunctional polyether polyol (number average molecular weight 1,000-3000) and 15 wt% of trifunctional polyether polyol (number average molecular weight 3,000-6,000) are pumped into the reactor, and After heating to C -120。 C and removing the water possessed by polyol and stirring it at 45-60 RPM to make a uniform liquid phase, 13% by weight of toluene diisocyanate with an equivalent ratio of NCO / OH = 6.0 or less is added and normal pressure, Reaction was carried out at 75 ° C. for 10-14 hours in a nitrogen atmosphere to produce a primary polyurethane preforma having a terminal NCO group, and a secondary polyurethane preforma was produced using 0.5 wt% of ethylene glycol as a chain extender. .

Benzoyl corride 0.5 as a reaction inhibitor for inhibiting the self-reaction during the storage of the polyurethane preformer by adding 30% by weight of calcium carbonate as a filler and mixing for 2 hours. 1.0% by weight of sudium silica aluminate, which is a water absorbent to absorb water by weight and water, was added, and after stabilizing the composite, 10% by weight of toluene, 8.5% by weight of ethyl acetate, and 1.5% by weight of methyl ethyl ketone were used The mixture was added for 4 hours or more to prepare a moisture-curable polyurethane one-component adhesive having a viscosity of 9,000-13,000 CPS / 20 ° C and a solid content of 70-90%. The physical property test result of 90 ° C peel adhesion strength, which is the most important property of the polyurethane one-component adhesive prepared as above, is as follows.After 24 hours, it is 6.6 at 20 ° C and 5.12 at 5 ° C. There was no problem in using, and after 48 hours, it was relatively good at 20 ° C 14.63 and 5 ° C 6.06.

Properties Example 20 ℃ 5 ℃ 90 ° peeling adhesive strength O / T: 15 minutes (unit: kgf / 25mm) 2 hours later 0.36 0.59 8 hours later 0.68 0.94 After 24 hours 6.6 5.12 After 48 hours 14.63 6.06

Example 2

The raw materials and the additives according to the second embodiment of the present invention are represented by weight%.

22% by weight of bifunctional polyether polyol

13% by weight of trifunctional polyether polyol

9.5% by weight of diphenylmethane diisocyanate

8.0% by weight of toluene diisocyanate

0.5 wt% of polymeric MD

1,4 butanediol 0.5% by weight

Talc 27% by weight

Benzoyl corrolide 0.5 wt%

Sudden silico aluminate 1.0 wt%

Toluene 9.0 wt%

Ethyl Acetate 8.0 wt%

1.0% by weight of methyl ethyl ketone

The raw materials and additives were prepared in the same manner as in Example 1, and the 90 ° C peel adhesive strength test results of the polyurethane one-component adhesive prepared as described above were as follows, and after 20 hours, 20 ° C 9.03, 5 Adhesion strength was good at 8.73 ° C, especially at low temperature of 5 ° C at 8.73.

Properties Example 20 ℃ 5 ℃ 90 ° peeling adhesive strength O / T: 15 minutes (unit: kgf / 25mm) 2 hours later 0.77 0.49 8 hours later 5.5 1.34 After 24 hours 9.03 8.73 After 48 hours 11.91 8.73

Using the moisture-curable polyurethane one-component adhesive according to the present invention when constructing and adhering flooring materials such as pvc tiles, rubber tiles, and heavy walking flooring materials, they can be cured in a short time by self-reaction and at the same time, higher adhesion than conventional adhesives. As it has strength, heat resistance, and water resistance, it can be used without any problem even at high temperature such as ondol, and it can withstand high humidity in summer and rainy season, and it is a disadvantage of conventional adhesive when it is installed in low humidity and temperature in winter. In order to shorten the curing time due to long-term phosphorus curing time, in the existing method of additionally using a curing accelerator including tin-based catalyst, the curing time is shortened and after construction only by the one-component adhesive composition of the present invention without the use of a separate curing accelerator. As an invention to have a high adhesive strength, it is possible to obtain the effect of improving workability and physical properties Invention.

Claims (4)

In the adhesive used for floor covering materials, such as PVC tile and a rubber tile; (1) 10-30% by weight of bifunctional polyether polyol with a number average molecular weight of 1000-3000, (2) 10-15% by weight of the trifunctional polyether polyol of the number average molecular weight 3000-6000, (3) 5.0-13% by weight of toluene diisocyanate (TDI), 9.5% by weight of diphenylmethane diisocyanate, 0.5-1.0% by weight of polymeric mdiai, (4) 0.5% by weight of bifunctional glycol consisting of 1,4 butanediol, (5) 26-30% by weight of the filler composed of talc, (6) 0.2-0.5% by weight of benzoyl corride, (7) 0.8-1.0% by weight of silicon silica aluminate, (8) 9.0-10% by weight of toluene, 8.0-8.5% by weight of ethyl acetate, 0.5-1.0% by weight of methyl ethyl ketone, moisture-curable polyurethane adhesive composition Polyurethane adhesive manufacturing method consisting of the following steps; (1) Pump bifunctional polyether polyols and trifunctional polyether polyols into a reactor and heat them at a temperature of 70 ° C to 120 ° C to remove water in the polyol and to form a uniform liquid phase. After stirring at -60 RPM, (2) A diisocyanate consisting of toluene diisocyanate (TDI), diphenylmethane diisocyanate (MDI), and polymer Mdiai was added, and reacted at 75 ° C. for 10-14 hours at atmospheric pressure and in a nitrogen atmosphere. A primary polyurethane preforma having a group is produced, and a bifunctional glycol such as ethylene glycol and 1,4 butanediol, which is a chain extender, is added to produce a secondary polyurethane preforma, (3) adding talc or calcium carbonate as a filler to the secondary polyurethane preforma for 2 hours or more, and adding benzoyl corride and sudsilic aluminate as a water absorbent as a reaction inhibitor to stabilize the composite. After the deadline, (4) A method for producing a moisture-curable polyurethane adhesive, comprising adding a solvent such as toluene, ethyl acetate, methyl ethyl ketone, and mixing for 4 hours or more. The polyurethane adhesive composition of claim 1, wherein the bifunctional glycol is ethylene glycol. The polyurethane adhesive composition of claim 1, wherein the filler is calcium carbonate.