CN114230755A - High-solid-content strong-adhesion waterborne polyurethane emulsion and preparation method thereof - Google Patents
High-solid-content strong-adhesion waterborne polyurethane emulsion and preparation method thereof Download PDFInfo
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- CN114230755A CN114230755A CN202111579875.8A CN202111579875A CN114230755A CN 114230755 A CN114230755 A CN 114230755A CN 202111579875 A CN202111579875 A CN 202111579875A CN 114230755 A CN114230755 A CN 114230755A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/61—Polysiloxanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3228—Polyamines acyclic
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3855—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur
- C08G18/3857—Low-molecular-weight compounds having heteroatoms other than oxygen having sulfur having nitrogen in addition to sulfur
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
Abstract
The invention discloses a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight: 11-23% of organic silicon polyol, 10-13% of polyether polyol, 10-13% of isocyanate, 1.5-2% of small molecular polyol, 1.5-2.5% of small molecular amine, 2-3.5% of neutralizer, 10-12% of acetone and 42-43% of deionized water. The invention discloses a preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion. The invention ensures sufficient folding strength and anti-embossing strength, improves the solid content of the transfer glue by introducing sulfonate hydrophilic groups, and introduces the organic silicon polyol resin to strengthen the adhesive force with the aluminum layer, thereby effectively strengthening the bonding firmness of the aluminum layer and paper and ensuring that the problems of poor transfer and aluminum layer falling off cannot occur in the transfer process. In addition, the preparation method is simple, easy to operate and mild in reaction condition.
Description
Technical Field
The invention relates to the technical field of aqueous polyurethane emulsion, in particular to aqueous polyurethane emulsion with high solid content and strong adhesive force and a preparation method thereof.
Background
At present, the traditional polyurethane emulsion transfer adhesive has the defects of low solid content, low composite fastness and low folding resistance and compression resistance, so that the problems of easy aluminum layer shedding and poor transfer in the transfer process are caused when the traditional polyurethane emulsion transfer adhesive is applied to composite production of an aluminizer and paper.
Disclosure of Invention
The invention aims to provide a high-solid-content high-adhesion waterborne polyurethane emulsion and a preparation method thereof, which are characterized in that the solid content of transfer glue is improved by introducing sulfonate hydrophilic groups while ensuring sufficient folding strength and anti-embossing strength, and the adhesion with an aluminum layer is enhanced by introducing organosilicon polyol resin, so that the bonding firmness of the aluminum layer and paper is effectively enhanced, and the problems of poor transfer and aluminum layer falling in the transfer process are solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a high-solid-content strong-adhesion waterborne polyurethane emulsion, which comprises the following raw materials in percentage by weight:
in some specific embodiments, the silicone polyol is a silicone diol, the polyether polyol is a polyether triol, and the molecular weights of the silicone diol and the polyether triol are 2000-3000.
In some preferred embodiments, the silicone polyol may be selected from the products available from the blue star silicone company under the tradename RHODORSIL OIL 1647V 60 or RHODORSIL OIL 1647V 80.
In some preferred embodiments, the polyether polyol may be selected from the products available from eastern Dow of Shandong Lanzhong GmbH under the designation 10LD76E or DEP-5631 ED.
In some embodiments, the isocyanate is selected from any one of isophorone diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, and m-xylylene diisocyanate.
In some embodiments, the small molecule polyol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol, and 1, 6-hexanediol in a mass ratio of 5:3: 2.
In some specific embodiments, the small molecule amine consists of sulfamate and ethylenediamine in a mass ratio of 6: 4.
In some embodiments, the neutralizing agent is selected from any one of N, N dimethylethanolamine and triethylamine.
In some preferred embodiments, the high-solid-content strong-adhesion aqueous polyurethane emulsion consists of the following raw materials in percentage by weight:
in a second aspect, the invention provides a preparation method of the aqueous polyurethane emulsion with high solid content and strong adhesive force, which comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under the vacuum condition, and then cooling to 40-50 ℃;
s2, adding isocyanate, controlling the temperature at 95-115 ℃, stirring and reacting for 4-5 h, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 0.5-1 h after complete dissolution;
s3, reducing the temperature to 40-45 ℃, adding a neutralizing agent, adding deionized water, stirring for 1-1.5 h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Compared with the prior art, the invention provides the high-solid-content strong-adhesion waterborne polyurethane emulsion and the preparation method thereof, and the aqueous polyurethane emulsion has the following beneficial effects:
the invention ensures sufficient folding strength and anti-embossing strength, and simultaneously most importantly, the solid content of the transfer glue is improved by introducing the sulfonate hydrophilic group, and the adhesion with the aluminum layer is enhanced by introducing the organic silicon polyol resin, so that the bonding firmness of the aluminum layer and paper is effectively enhanced, and the problems of poor transfer and aluminum layer falling in the transfer process are avoided. In addition, the preparation method is simple, easy to operate and mild in reaction condition.
Detailed Description
The technical solutions of the present invention will be described clearly and completely by the detailed embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The starting materials used in the following examples are all commercially available.
Example 1
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 60 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with the trademark of 10LD76E of Shandong Lanxingdao Limited company, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is isophorone diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizing agent is triethylamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 45 ℃;
s2, adding isocyanate, controlling the temperature at 105 ℃, stirring and reacting for 4.5 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 1 hour after complete dissolution;
s3, reducing the temperature to 45 ℃, adding a neutralizing agent, adding deionized water, strongly stirring for 1.2h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Example 2
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 60 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with the trademark of 10LD76E of Shandong Lanxingdao Limited company, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is toluene diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizing agent is triethylamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 45 ℃;
s2, adding isocyanate, controlling the temperature at 105 ℃, stirring and reacting for 4.5 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 1 hour after complete dissolution;
s3, reducing the temperature to 45 ℃, adding a neutralizing agent, adding deionized water, strongly stirring for 1.2h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Example 3
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 60 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with the trademark of 10LD76E of Shandong Lanxingdao Limited company, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is hexamethylene diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizing agent is triethylamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 45 ℃;
s2, adding isocyanate, controlling the temperature at 105 ℃, stirring and reacting for 4.5 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 1 hour after complete dissolution;
s3, reducing the temperature to 45 ℃, adding a neutralizing agent, adding deionized water, strongly stirring for 1.2h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Example 4
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 60 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with the trademark of 10LD76E of Shandong Lanxingdao Limited company, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is m-xylylene diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizing agent is triethylamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 45 ℃;
s2, adding isocyanate, controlling the temperature at 105 ℃, stirring and reacting for 4.5 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 1 hour after complete dissolution;
s3, reducing the temperature to 45 ℃, adding a neutralizing agent, adding deionized water, strongly stirring for 1.2h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Example 5
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 80 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with the trademark of 10LD76E of Shandong Lanxingdao Limited company, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is isophorone diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizing agent is triethylamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 45 ℃;
s2, adding isocyanate, controlling the temperature at 105 ℃, stirring and reacting for 4.5 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 1 hour after complete dissolution;
s3, reducing the temperature to 45 ℃, adding a neutralizing agent, adding deionized water, strongly stirring for 1.2h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Example 6
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 60 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with a DEP-5631ED (product designation of DEP-5631 ED) of Shandong Lanxingdong GmbH, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is isophorone diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizing agent is triethylamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 45 ℃;
s2, adding isocyanate, controlling the temperature at 105 ℃, stirring and reacting for 4.5 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 1 hour after complete dissolution;
s3, reducing the temperature to 45 ℃, adding a neutralizing agent, adding deionized water, strongly stirring for 1.2h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Example 7
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 60 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with the trademark of 10LD76E of Shandong Lanxingdao Limited company, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is isophorone diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizer is N, N dimethylethanolamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 45 ℃;
s2, adding isocyanate, controlling the temperature at 105 ℃, stirring and reacting for 4.5 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 1 hour after complete dissolution;
s3, reducing the temperature to 45 ℃, adding a neutralizing agent, adding deionized water, strongly stirring for 1.2h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Example 8
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 60 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with the trademark of 10LD76E of Shandong Lanxingdao Limited company, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is isophorone diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizing agent is triethylamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 40 ℃;
s2, adding isocyanate, controlling the temperature at 95 ℃, stirring for reaction for 5 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reaction for 1 hour after complete dissolution;
s3, reducing the temperature to 45 ℃, adding a neutralizing agent, adding deionized water, strongly stirring for 1.5h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
Example 9
The embodiment provides a high-solid-content strong-adhesion waterborne polyurethane emulsion which comprises the following raw materials in percentage by weight:
wherein the organosilicon polyol is a product of Rhodorsil OIL 1647V 60 of Lanzhong organosilicon company, and the molecular weight of the organosilicon polyol is 2000-3000; the polyether polyol is a product with the trademark of 10LD76E of Shandong Lanxingdao Limited company, and the molecular weight of the polyether polyol is 2000-3000; the isocyanate is isophorone diisocyanate; the micromolecular polyalcohol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol with the mass ratio of 5:3: 2; the micromolecule amine consists of sulfamate and ethylenediamine according to the mass ratio of 6: 4; the neutralizing agent is triethylamine.
The preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under a vacuum condition, and then cooling to 50 ℃;
s2, adding isocyanate, controlling the temperature at 115 ℃, stirring and reacting for 4 hours, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 0.5 hour after complete dissolution;
s3, reducing the temperature to 40 ℃, adding a neutralizing agent, adding deionized water, stirring strongly for 1h, adding ethylenediamine after complete emulsification, and then fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
In order to verify the beneficial effects of the invention, the performance test of the high solid content and strong adhesive force aqueous polyurethane emulsion prepared in the embodiment 1-9 is carried out.
(1) The solid content of the aqueous polyurethane emulsion prepared in the examples 1 to 9 and the commercially available product transfer adhesive was tested according to the GB/T2793-1995 standard. Specific results are shown in table 1 below.
(2) The adhesive strength of the aqueous polyurethane emulsions prepared in examples 1 to 9 and the commercially available product transfer adhesives was tested according to GB/T2791-1995. Specific results are shown in table 1 below.
(3) The waterborne polyurethane emulsion prepared in the embodiment 1-9 and a commercially available product transfer adhesive are sprayed to form a film, and then a folding experiment is carried out to test the folding times when bursting occurs. Specific results are shown in table 1 below.
(4) The aqueous polyurethane emulsion prepared in the examples 1 to 9 and a commercially available product transfer adhesive are respectively applied to the composite production of an aluminizer and paper, and a 3M strong adhesive tape is used for testing the adhesive force to see whether the aluminizer falls off or not. Specific results are shown in table 1 below.
Table 1 results of performance testing
The results in table 1 show that the aqueous polyurethane emulsion with high solid content and strong adhesive force prepared by the invention has high solid content, high bonding strength, high adhesive force, good bonding performance and good folding resistance, effectively enhances the bonding fastness of the aluminizer and paper, and ensures that the problems of poor transfer and aluminum layer shedding can not occur in the transfer process.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. The high-solid-content high-adhesion waterborne polyurethane emulsion is characterized by comprising the following raw materials in percentage by weight:
2. the high-solid-content high-adhesion waterborne polyurethane emulsion according to claim 1, wherein the organosilicon polyol is organosilicon diol, the polyether polyol is polyether triol, and the molecular weights of the organosilicon diol and the polyether triol are 2000-3000.
3. The aqueous polyurethane emulsion with high solid content and strong adhesion as claimed in claim 1, wherein the silicone polyol is selected from products of the blue star silicone company under the trade name of Rhodorsil OIL 1647V 60 or Rhodorsil OIL 1647V 80.
4. The aqueous polyurethane emulsion with high solid content and strong adhesion of claim 1, wherein the polyether polyol is selected from products of Shandong Lanxingdao GmbH under the trademark of 10LD76E or DEP-5631 ED.
5. The high-solid-content high-adhesion waterborne polyurethane emulsion according to claim 1, wherein the isocyanate is any one selected from isophorone diisocyanate, toluene diisocyanate, hexamethylene diisocyanate, and m-xylylene diisocyanate.
6. The high-solid-content high-adhesion waterborne polyurethane emulsion of claim 1, wherein the small-molecular polyol consists of 2, 2-dimethylolpropionic acid, 1, 4-butanediol and 1, 6-hexanediol in a mass ratio of 5:3: 2.
7. The high-solid-content high-adhesion waterborne polyurethane emulsion of claim 1, wherein the small molecule amine consists of sulfamate and ethylenediamine in a mass ratio of 6: 4.
8. The high-solid-content high-adhesion aqueous polyurethane emulsion according to claim 1, wherein the neutralizing agent is selected from any one of N, N-dimethylethanolamine and triethylamine.
9. The high-solid-content high-adhesion waterborne polyurethane emulsion according to claim 1, which is characterized by comprising the following raw materials in percentage by weight:
10. the preparation method of the high-solid-content strong-adhesion waterborne polyurethane emulsion as claimed in any one of claims 1 to 9, wherein the method comprises the following steps:
s1, weighing the raw materials of the components according to the proportion, uniformly mixing the organic silicon polyol, the polyether polyol and the micromolecule polyol, heating to 120 ℃, dehydrating for 2 hours under the vacuum condition, and then cooling to 40-50 ℃;
s2, adding isocyanate, controlling the temperature at 95-115 ℃, stirring and reacting for 4-5 h, then cooling to 60 ℃, adding acetone, and adding sulfamate for reacting for 0.5-1 h after complete dissolution;
s3, reducing the temperature to 40-45 ℃, adding a neutralizing agent, adding deionized water, stirring for 1-1.5 h, adding ethylenediamine after complete emulsification, and fully dispersing;
and S4, removing acetone to obtain the high-solid-content strong-adhesion waterborne polyurethane emulsion.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827571A (en) * | 2012-09-28 | 2012-12-19 | 广东多正化工科技有限公司 | Preparation method of water-based polyurethane adhesive |
| CN106118428A (en) * | 2016-07-28 | 2016-11-16 | 上海乘鹰新材料有限公司 | A kind of waterproof scratch resistant aqueous polyurethane coating and preparation method thereof |
| US20200325266A1 (en) * | 2019-04-12 | 2020-10-15 | Nan Ya Plastics Corporation | Method for preparing aqueous polyurethane dispersion |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827571A (en) * | 2012-09-28 | 2012-12-19 | 广东多正化工科技有限公司 | Preparation method of water-based polyurethane adhesive |
| CN106118428A (en) * | 2016-07-28 | 2016-11-16 | 上海乘鹰新材料有限公司 | A kind of waterproof scratch resistant aqueous polyurethane coating and preparation method thereof |
| US20200325266A1 (en) * | 2019-04-12 | 2020-10-15 | Nan Ya Plastics Corporation | Method for preparing aqueous polyurethane dispersion |
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