A ONE-COMPONENT TYPE POLYURETHANE PREPOLYMER COMPOSITION

Abstract

A one-component type polyurethane prepolymer composition comprises a reaction product formed through a reaction between reactants comprising (a) at least one polyisocyanate, and (b) a polyol blend comprising at least one bifunctional polyether polyol, wherein the bifunctional polyether polyol is a homopolymer of propylene oxide, homopolymer of butylene oxide, or copolymer of alkylene oxide, and has a number average molecular weight from 3000 g/mol to 9000 g/mol, and at least one trifunctional polyether polyol, wherein the trifunctional polyether polyol is a copolymer of alkylene oxide and end-capped with 10 wt % to 28 wt %, by the total weight of the trifunctional polyether polyol, of ethylene oxide, and has a number average molecular weight from 5000 g/mol to 8000 g/mol, wherein the bifunctional polyether polyol and the trifunctional polyether polyol are present in a parts by weight ratio from 4:1 to 2.5:1, and wherein the polyisocyanate and the polyol blend are present in a parts by weight ratio of from 1:7 to 1:2.5.

Claims

1. A one-component type polyurethane prepolymer composition comprising a reaction product formed through a reaction between reactants comprising (a) at least one polyisocyanate, and (b) a polyol blend comprising at least one bifunctional polyether polyol, wherein the bifunctional polyether polyol is a homopolymer of propylene oxide, homopolymer of butylene oxide, or copolymer of alkylene oxide, and has a number average molecular weight from 3000 g/mol to 9000 g/mol, and at least one trifunctional polyether polyol, wherein the trifunctional polyether polyol is a copolymer of alkylene oxide and end-capped with 10 wt % to 28 wt %, by the total weight of the trifunctional polyether polyol, of ethylene oxide, and has a number average molecular weight from 5000 g/mol to 8000 g/mol, wherein the bifunctional polyether polyol and the trifunctional polyether polyol are present in a parts by weight ratio from 4:1 to 2.5:1, and wherein the polyisocyanate and the polyol blend are present in a parts by weight ratio of from 1:7 to 1:2.5.

2. The one-component type polyurethane prepolymer composition of claim 1, wherein the polyol blend comprises one bifunctional polyether polyol having a number average molecular weight from 3000 g/mol to 5000 g/mol and one trifunctional polyether polyol having a number average molecular weight from 5000 g/mol to 7000 g/mol.

3. The one-component type polyurethane prepolymer composition of claim 1, wherein the polyol blend comprises at least two bifunctional polyether polyol, wherein the first bifunctional polyether polyol has a number average molecular weight from 3000 g/mol to 5000 g/mol, wherein the second bifunctional polyether polyol has a number average molecular weight from 7000 g/mol to 9000 g/mol, wherein the first bifunctional polyether polyol and the second bifunctional polyether polyol are present in a parts by weight ratio of from 3:1 to 1:3.

4. The one-component type polyurethane prepolymer composition of claim 1, wherein the polyisocyanate is selected from a liquid carbodiimide modified MDI, an MDI-50, or a mixture thereof.

5. The one-component type polyurethane prepolymer composition of claim 1, further comprising, from 5 wt % to 13 wt %, based on the total weight of the one-component type polyurethane prepolymer composition, of an organic solvent.

6. The one-component type polyurethane prepolymer composition of claim 1, further comprising from 40 wt % to 60 wt %, based on the total weight of the one-component type polyurethane prepolymer composition, of a filler.

7. A waterproofing coating material comprising the one-component type polyurethane prepolymer composition of claim 1.

Description

EXAMPLES

[0053] I. Raw Materials

[0054] Raw materials and components used in this disclosure are listed below.

TABLE-US-00001 TABLE 1 Raw materials and components Material Description Supplier ISONATE ™ 50 MDI-50 The Dow OP Pure MDI Chemical Company Desmodur CD-C Polycarbodiimide-modified diphenylmethane-4,4′- Covestro MDI diisocyanate with functionality at 2.1 Company VORANATE ™ T- TDI The Dow 80 Type I TDI Chemical Company VORANOL ™ Bifunctional polyether polyol being a The Dow 2000LM polyol homopolymer of propylene oxide; Chemical Mw: 2000 g/mol Company VORANOL ™ Bifunctional polyether polyol being a The Dow 4000LM polyol homopolymer of propylene oxide; Chemical Mw: 4000 g/mol Company VORANOL ™ Bifunctional polyether polyol being a The Dow 8000LM polyol homopolymer of propylene oxide; Chemical Mw: 8000 g/mol Company VORANOL ™ CP- Trifunctional polyether polyol being a copolymer The Dow 3001 polyol of propylene oxide, end-capped with 8.5 wt %, Chemical based on the total weight of the trifunctional Company polyether polyol, of ethylene oxide; Mw: 3000 g/mol VORANOL ™ Trifunctional polyether polyol being a copolymer The Dow 4701 polyol of propylene oxide, end-capped with 13 wt %, Chemical based on the total weight of the trifunctional Company polyether polyol, of ethylene oxide; Mw: 5000 g/mol VORANOL™ CP Trifunctional polyether polyol being a copolymer The Dow 6001 polyol of propylene oxide, end-capped with 15.6 wt %, Chemical based on the total weight of the trifunctional Company polyether polyol, of ethylene oxide; Mw: 6000 g/mol VORANOL ™ Trifunctional polyether polyols being a copolymer The Dow 1447 polyol of propylene oxide, end-capped with 71.2 wt %, Chemical based on the total weight of the trifunctional Company polyether polyol, of ethylene oxide; Mw: 6000 g/mol VORANOL ™ CP Trifunctional polyether polyols being a copolymer The Dow 4610 polyol of propylene oxide, end-capped with 12.5 wt %, Chemical based on the total weight of the trifunctional Company polyether polyol, of ethylene oxide; Mw: 4600 g/mol Chlorinated Plasticizer Danyang paraffin Chemical Additives Co., Ltd. BYK-W 980 Wetting dispersant BYK wetting dispersant 800 mesh calcium Filler Omya carbonate S-150 solvent Aromatic solvent oil Peng Chen New Materials Technology Co., Ltd. DABCO T-12 Curing catalyst Air Products and catalyst Chemicals DMDEE catalyst 2,2′-dimorpholinyldiethyl ether curing catalyst Qingdao Hengke BYK-066 N Defoaming agent BYK defoaming agent

[0055] II. Test Methods

[0056] (a) Viscosity measurement: viscosity (unit: pascal-second (Pa.Math.s)) was measured by advanced Rhometric Expansion System G2 (ARES G2) at the following condition: 25 millimeter (mm) steel parallel plate, temperature at 25° C., shear rate at 0.1/second and screen for 180 seconds.

[0057] (b) Tear Strength Test:

[0058] Film Preparation

[0059] Ethacure 300 curative, available from Albemarle Company, was added into the prepolymer composition. The amounts of curative may be calculated by the following formula:

[00001]$C_{100p}=\frac{\mathrm{NCO}\%\times C_{\mathrm{ew}}\times \%\mathrm{Theory}}{4202}$

[0060] Wherein “C.sub.100p” is the parts curative per 100 parts prepolymer composition, “NCO %”, also called isocyanate content, is the percent of the remaining NCO content of the prepolymer composition, determined by reaction with excess di-n-butylamine and back titration with standardized hydrochloric acid. “C.sub.ew” is the equivalent weight of the curative, and “% Theory” is the stoichiometry for the curative. In general, Ethacure 300 curative has an equivalent weight of 107 and 90% to 95% stoichiometry. Thus, for example, the calculated amount of a curative with an equivalent weight of 107 and 95% stoichiometry cured with a prepolymer composition having 4.8 NCO % would be 11.6 parts of curative per 100 parts prepolymer composition on a mass basis.

[0061] Then, the mixture of prepolymer composition and Ethacure 300 curative was blended by a SpeedMixer laboratory mixer system from FlackTek Inc. at 3000 revolutions per minute (RPM) for 30 seconds, and turned to dark brown, deep purple or even black. Then, the mixture was poured onto a release paper and a film was formed. The film was made at the thickness about 1.0 mm to 1.3 mm, and cured at 80° C. for 30 minutes. After stripping from the release paper, the film was further post cured at 60° C. for 24 hours.

[0062] Tear Strength Test

[0063] Tear strength test was applied through Trousers Type Method, also called the Double Tongue Method. The film was cut by a molder to trousers like shape with a V-notch fixture. The thickness of the sample was measured prior to the tear strength test. When clamping, sample tongue is clamped in the center of clamps, symmetrical. Two legs of sample, parallel to the direction of tearing, are clamped symmetrically in removable clamps. Pay attention to ensuring each tongue is fixed in clamps, so that tear is parallel to tearing direction when tear starts. Start the machine to tear the sample from both tongue until it was fully broken, marking the end of this test. Tearing load and tearing length of each sample is recorded. The observation should be done on whether tear is processed in the direction of applied force and whether yarns slip away from the fabric. If the sample does not slip away from the clamps and tear is conducted along the direction of applied force, the test results can be acknowledged, otherwise, removed. Tear strength is obtained by dividing the maximum tear load by the thickness of each sample. The test was repeated 3 times to calculate an average tear strength.

[0064] III. Examples

[0065] Inventive Example 1 (IE1)

[0066] 7.3 grams (g) VORANOL™ 4000LM polyol and 2.7 g VORANOL™ CP 6001 polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 megapascal (MPa) or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 parts per million (ppm).

[0067] When the polyol blend was cooled down naturally at room temperature to 65° C., 2.8 g Desmodur CD-C MDI was added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0068] Inventive Example 2 (IE2)

[0069] 7.3 g VORANOL™ 4000LM polyol and 2.7 g VORANOL™ CP 6001 polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0070] When the polyol blend was cooled down naturally at room temperature to 65° C., 2.4 g ISONATE™ 50 OP Pure MDI was added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0071] Inventive Example 3 (IE3)

[0072] 7.3 g VORANOL™ 4000LM polyol and 2.7 g VORANOL™ CP 6001 polyol were mixed in a first flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0073] 1.9 g Desmodur CD-C MDI and 0.8 g ISONATE™ 50 OP Pure MDI were mixed in a second flask with mechanical stiffing to prepare a polyisocyanate blend.

[0074] When the polyol blend was cooled down naturally at room temperature to 65° C., the polyisocyanate blend was poured into the first flask. The mixture in the first flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0075] Inventive Example 4 (IE4)

[0076] 6.0 g VORANOL™ 4000LM polyol, 2.0 g VORANOL™ CP 6001 polyol and 2.0 g VORANOL™ 8000LM polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0077] When the polyol blend was cooled down naturally at room temperature to 65° C., 2.7 g Desmodur CD-C MDI was added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0078] Inventive Example 5 (IE5)

[0079] 6.0 g VORANOL™ 4000LM polyol, 2.0 g VORANOL™ CP 6001 polyol and 2.0 g VORANOL™ 8000LM polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0080] When the polyol blend was cooled down naturally at room temperature to 65° C., 2.4 g ISONATE™ 50 OP Pure MDI was added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0081] Inventive Example 6 (IE6)

[0082] 6.0 g VORANOL™ 4000LM polyol, 2.0 g VORANOL™ CP 6001 polyol and 2.0 g VORANOL™ 8000LM polyol were mixed in a first flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0083] 1.8 g Desmodur CD-C MDI and 0.8 g ISONATE™ 50 OP Pure MDI were mixed in a second flask with mechanical stiffing to prepare a polyisocyanate blend.

[0084] When the polyol blend was cooled down naturally at room temperature to 65° C., the polyisocyanate blend was poured into the first flask. The mixture in the first flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0085] Inventive Example 7 (IE7)

[0086] 36.5 g VORANOL™ 4000LM polyol and 13.5 g VORANOL™ CP 3001 polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0087] When the polyol blend was cooled down naturally at room temperature to 65° C., 13.1 g ISONATE™ 50 OP Pure MDI was added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0088] Inventive Example 8 (IE8)

[0089] 36.5 g VORANOL™ 4000LM polyol and 13.5 g VORANOL™ CP 4610 polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0090] When the polyol blend was cooled down naturally at room temperature to 65° C., 12.5 g ISONATE™ 50 OP Pure MDI was added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0091] Inventive Example 9 (IE9)

[0092] 195.6 g VORANOL™ 4000LM polyol, 72.3 g VORANOL™ CP 6001 polyol, 108.4 g chlorinated paraffin, 455.1 g 800 mesh calcium carbonate and 1.2 g BYK-W 980 wetting dispersant were mixed in a flask with mechanical stirring to prepare a mixture. Then, the mixture was heated to 120° C. At the condition that the mixture was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the mixture was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0093] When the mixture was cooled down naturally at room temperature to 65° C., 51.6 g ISONATE™ 50 OP Pure MDI, 1.2 g BYK-W 980 wetting dispersant and 83.2 g S-150 solvent were added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 30 minutes. Then, the mixture was heated to 85° C. The mixture then was being continuously and mechanically stirred and was allowed to react for 2 hours while the temperature of the mixture was controlled at a range of 80° C. to 85° C.

[0094] The mixture was then cooled down naturally at room temperature to 60° C. 0.9 g DABCO T-12 catalyst and 1.3 g DMDEE catalyst dissolved in 27.7 g S-150 solvent, and 1.5 g BYK-066 N defoaming agent were further added into the flask. The mixture was mixed under 60° C. for 30 minutes.

[0095] Then, the mixture was defoamed for 5 minutes at a pressure of −0.09 MPa or less controlled by vacuuming to obtain the inventive one-component type polyurethane prepolymer composition.

[0096] Inventive Example 10 (IE10)

[0097] 196.2 g VORANOL™ 4000LM polyol, 72.6 g VORANOL™ CP 6001 polyol, 121.2 g chlorinated paraffin, 446.5 g 800 mesh calcium carbonate and 1.55 g BYK-W 980 wetting dispersant were mixed in a flask with mechanical stirring to prepare a mixture. Then, the mixture was heated to 120° C. At the condition that the mixture was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the mixture was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0098] When the mixture was cooled down naturally at room temperature to 65° C., 35.7 g VORANATE™ T-80 Type I TDI, 1.55 g BYK-W 980 wetting dispersant and 90.9 g S-150 solvent were added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 30 minutes. Then, the mixture was heated to 85° C. The mixture then was being continuously and mechanically stirred and was allowed to react for 2 hours while the temperature of the mixture was controlled at a range of 80° C. to 85° C.

[0099] The mixture was then cooled down naturally at room temperature to 60° C. 1.0 g DABCO T-12 catalyst and 0.4 g DMDEE catalyst dissolved in 30.3 g S-150 solvent, and 2.1 g BYK-066 N defoaming agent were further added into the flask. The mixture was mixed under 60° C. for 30 minutes.

[0100] Then, the mixture was defoamed for 5 minutes at a pressure of −0.09 MPa or less controlled by vacuuming to obtain the inventive one-component type polyurethane prepolymer composition.

[0101] Comparative Example 1 (CE1)

[0102] 7.3 g VORANOL™ 2000LM polyol and 2.7 g VORANOL™ 4701 polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0103] When the polyol blend was cooled down naturally at room temperature to 65° C., 3.5 g Desmodur CD-C MDI was added into the flask. The mixture in the flask was being continuously mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0104] Comparative Example 2 (CE2)

[0105] 7.3 g VORANOL™ 2000LM polyol and 2.7 g VORANOL™ 4701 polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0106] When the polyol blend was cooled down naturally at room temperature to 65° C., 3.0 g ISONATE™ 50 OP Pure MDI was added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0107] Comparative Example 3 (CE3)

[0108] 7.3 g VORANOL™ 2000LM polyol and 2.7 g VORANOL™ 4701 polyol were mixed in a first flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0109] 2.3 g Desmodur CD-C MDI and 1.0 g ISONATE™ 50 OP Pure MDI were mixed in a second flask with mechanical stiffing to prepare a polyisocyanate blend.

[0110] When the polyol blend was cooled down naturally at room temperature to 65° C., the polyisocyanate blend was poured into the first flask. The mixture in the first flask was being continuously mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0111] Comparative Example 4 (CE4)

[0112] 36.5 g VORANOL™ 4000LM polyol and 13.5 g VORANOL™ 1447 polyol were mixed in a flask with mechanical stiffing to prepare a polyol blend. Then, the polyol blend was heated to 120° C. At the condition that the polyol blend was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the polyol blend was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0113] When the polyol blend was cooled down naturally at room temperature to 65° C., 12.5 g ISONATE™ 50 OP Pure MDI was added into the flask. The mixture in the flask was being continuously mechanically stirred and was allowed to react for 7 hours to obtain the inventive one-component type polyurethane prepolymer composition.

[0114] Comparative Example 5 (CE5)

[0115] 181.5 g VORANOL™ 2000LM polyol, 82.9 g VORANOL™ 4701 polyol, 106.4 g chlorinated paraffin, 450.0 g 800 mesh calcium carbonate and 1.15 g BYK-W 980 wetting dispersant were mixed in a flask with mechanical stirring to prepare a mixture. Then, the mixture was heated to 120° C. At the condition that the mixture was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the mixture was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0116] When the mixture was cooled down naturally at room temperature to 65° C., 64.0 g ISONATE™ 50 OP Pure MDI, 1.15 g BYK-W 980 wetting dispersant and 81.9 g S-150 solvent were added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 30 minutes. Then, the mixture was heated to 85° C. The mixture then was being continuously and mechanically stirred and was allowed to react for 2 hours while the temperature of the mixture was controlled at a range of 80° C. to 85° C.

[0117] The mixture was then cooled down naturally at room temperature to 60° C. 0.9 g DABCO T-12 catalyst and 1.3 g DMDEE catalyst dissolved in 27.3 g S-150 solvent, and 1.5 g BYK-066 N defoaming agent were further added into the flask. The mixture was mixed under 60° C. for 30 minutes.

[0118] Then, the mixture was defoamed for 5 minutes at a pressure of −0.09 MPa or less controlled by vacuuming to obtain the inventive one-component type polyurethane prepolymer composition.

[0119] Comparative Example 6 (CE6)

[0120] 186.2 g VORANOL™ 2000LM polyol, 80.1 g VORANOL™ 4701 polyol, 120.1 g chlorinated paraffin, 442.4 g 800 mesh calcium carbonate and 1.5 g BYK-W 980 wetting dispersant were mixed in a flask with mechanical stirring to prepare a mixture. Then, the mixture was heated to 120° C. At the condition that the mixture was controlled at the temperature range of from 115° C. to 120° C. and that the vacuum level of the flask was controlled at −0.09 MPa or less, the mixture was dehydrated for 2 hours to decrease water content to a level lower than 200 ppm.

[0121] When the mixture was cooled down naturally at room temperature to 65° C., 44.6 g VORANATE™ T-80 Type I TDI, 1.5 g BYK-W 980 wetting dispersant and 90.1 g S-150 solvent were added into the flask. The mixture in the flask was being continuously and mechanically stirred and was allowed to react for 30 minutes. Then, the mixture was heated to 85° C. The mixture then was being continuously and mechanically stirred and was allowed to react for 2 hours while the temperature of the mixture was controlled at a range of 80° C. to 85° C.

[0122] The mixture was then cooled down naturally at room temperature to 60° C. 1.0 g DABCO T-12 catalyst and 0.4 g DMDEE catalyst dissolved in 30.0 g S-150 solvent, and 2.0 g BYK-066 N defoaming agent were further added into the flask. The mixture was mixed under 60° C. for 30 minutes.

[0123] Then, the mixture was defoamed for 5 minutes at a pressure of −0.09 MPa or less controlled by vacuuming to obtain the inventive one-component type polyurethane prepolymer composition.

[0124] The formulations and the test results for Inventive Examples 1-10 and Comparative Examples 1-6 are as reported in Tables 2, 3 and 4.

TABLE-US-00002 TABLE 2 Formulations and test results of Inventive Examples 1-6 and Comparative Examples 1-3 IE1 IE2 IE3 IE4 IE5 IE6 CE1 CE2 CE3 VORANOL ™ 4000LM polyol (g) 7.3 7.3 7.3 6.0 6.0 6.0 — — — VORANOL ™ 8000LM polyol (g) — — — 2.0 2.0 2.0 — — — VORANOL ™ CP 6001 polyol (g) 2.7 2.7 2.7 2.0 2.0 2.0 — — — VORANOL ™ 2000LM polyol (g) — — — — — — 7.3 7.3 7.3 VORANOL ™ 4701 polyol (g) — — — — — — 2.7 2.7 2.7 Desmodur CD-C MDI (g) 2.8 — 1.9 2.7 — 1.8 3.5 — 2.3 ISONATE ™ 50 OP Pure MDI (g) — 2.4 0.8 — 2.4 0.8 — 3.0 1.0 Viscosity (Pa.s) 15.7 6.4 12.5 14.9 9.1 12.5 34.3 12.2 16.1 Phase separation No No No No No No No No No

TABLE-US-00003 TABLE 3 Formulations and test results of Inventive Examples 7-8 and Comparative Example 4 IE7 IE8 CE4 VORANOL ™ 4000LM polyol (g) 36.5 36.5 36.5 VORANOL ™ 1447 polyol (g)     13.5 VORANOL ™ CP-3001 polyol (g) 13.5     VORANOL ™ CP 4610 polyol (g)   13.5   ISONATE ™ 50 OP Pure MDI (g) 13.1 12.5 12.5 Viscosity (Pa.s) 14.4 10.6 12.5 Phase separation No No Yes

TABLE-US-00004 TABLE 4 Formulations and test results of Inventive Examples 9-10 and Comparative Examples 5-6 IE9 IE10 CE5 CE6 VORANOL ™ 2000LM polyol (g)     181.5 186.2 VORANOL ™ 4701 polyol (g)     82.9 80.1 VORANOL ™ 4000LM polyol (g) 195.6 196.2     VORANOL ™ CP 6001 polyol (g) 72.3 72.6     Chlorinated paraffin (g) 108.4 121.2 106.4 120.1 BYK-W 980 wetting dispersant (g) 2.4 3.1 2.3 3.0 800 mesh calcium carbonate (g) 455.1 446.5 450.0 442.4 ISONATE ™ 50 OP Pure MDI (g) 51.6   64.0   VORANATE ™ T-80 Type I TDI   35.7   44.6 S-150 solvent(g) 110.9 121.2 109.2 120.1 DABCO T-12 catalyst (g) 0.9 1.0 0.9 1.0 DMDEE catalyst (g) 1.3 0.4 1.3 0.4 BYK-066 N defoaming agent (g) 1.5 2.1 1.5 2.0 Viscosity (Pa.s) 5.0 8.3 6.0 14.4 Tear Strength (Newton/millimeter) 22.0 17.9 18.0 15.3 Phase separation No No No No

[0125] IV. Results

[0126] IE1, IE4 and CE1 used equivalent amount of Desmodur CD-C MDI, but different polyol blends. IE2, IE5 and CE2 used equivalent amount of ISONATE™ 50 OP Pure MDI, but different polyol blends. IE 3, IE 6 and CE 3 used equivalent amount of the blend of Desmodur CD-C MDI and ISONATE™ 50 OP Pure MDI, but different polyol blends. The inventive examples using the polyol blend of the present invention in each group exhibit significantly lowered viscosities compared with the comparative examples in each group respectively.

[0127] CE4 uses the polyol blend comprising VORANOL™ 1447 polyol, which is a trifunctional polyether polyol end-capped with 71.2 wt %, based on the total weight of the trifunctional polyether polyol, of ethylene oxide. Undesired phase separation occurred in CE4 due to the high ethylene oxide content. In contrast, IE7 and IE8 using the polyol blend of the present invention do not have the phase separation issue.

[0128] IE9 and CE5 used equivalent amount of polyisocyanate and additives, but different polyol blends. IE10 and CE6 used equivalent amount of polyisocyanate and additives, but different polyol blends. IE9 and IE10 using the polyol blend of the present invention exhibit significantly lowered viscosities compared with CE5 and CE6.