CN115160530A - Preparation method of high-solid-content waterborne polyurethane - Google Patents
Preparation method of high-solid-content waterborne polyurethane Download PDFInfo
- Publication number
- CN115160530A CN115160530A CN202210920053.XA CN202210920053A CN115160530A CN 115160530 A CN115160530 A CN 115160530A CN 202210920053 A CN202210920053 A CN 202210920053A CN 115160530 A CN115160530 A CN 115160530A
- Authority
- CN
- China
- Prior art keywords
- chain extender
- weight
- temperature
- acetone
- solid content
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
-
- 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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
-
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
-
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
-
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to a preparation method of high-solid-content waterborne polyurethane, which comprises the following steps: adding polyalcohol and antioxidant into a reaction kettle, and dehydrating in vacuum at 110 ℃; adding isocyanate and a catalyst under the protection of nitrogen to carry out prepolymerization reaction; adding a hydrophilic chain extender, a cross-linking agent, micromolecular alcohol and acetone into the reaction kettle at the temperature of 60-80 ℃ to continue to react for 2-4 h, adding a water-soluble chain extender Poly-EPS (PPS) and acetone into the reaction kettle to continue to react for 1-2 h at the temperature of 60-70 ℃, and diluting the mixture with acetone to obtain a prepolymerization product; adding aqueous solution of triethylamine under high-speed dispersion, and finally carrying out chain extension reaction by using diamine chain extender; finally removing acetone to obtain a 60% solid aqueous polyurethane product. The 60% solid content aqueous polyurethane emulsion prepared by the invention has good comprehensive performance, good film forming property and dispersibility, low viscosity, and stable and easy storage.
Description
Technical Field
The invention relates to the technical field of high polymers, in particular to a preparation method of high-solid-content waterborne polyurethane.
Background
With the enhancement of environmental awareness of people, the safety problem of materials is more emphasized, and higher standards and requirements are put forward for packaging adhesives for compounding, leather coatings and other living goods. The Waterborne Polyurethane (WPU) is a polyurethane emulsion which adopts water as a dispersion medium, has the advantages of simple use, no toxicity, no environmental pollution and the like besides the excellent performance of solvent type polyurethane, and can be successfully applied to the industries of light textile, leather, wood processing, building, papermaking and the like. However, as the waterborne polyurethane adopts water as a solvent, the surface tension of medium water is too large and the heat is high, so that the surface spreading is poor, the drying time is long, the compounding of a film and a base material is poor, and the mechanical property is reduced in the film forming process; the hydrophilic groups which promote the stable dispersion of the waterborne polyurethane in the medium water can cause the film-forming water resistance of the waterborne polyurethane to be poor and the waterborne polyurethane to be easy to absorb water; when the waterborne polyurethane is emulsified and dispersed, the high-viscosity organic phase can cause difficult dispersion, large emulsion particle size and lower emulsion solid content.
Disclosure of Invention
In view of the above, it is necessary to provide a method for producing a high-solid content aqueous polyurethane, which addresses the problems of the prior art.
A preparation method of high-solid content waterborne polyurethane comprises the following steps:
(1) Vacuum dehydration: mixing oligomer polyol and antioxidant, and dehydrating for 1-2 h at the temperature of 110-120 ℃ and the vacuum degree of-0.09 MPa;
(2) Prepolymerization reaction: introducing nitrogen into a reaction kettle, adding polyisocyanate and a polyurethane catalyst under the protection of the nitrogen, and reacting for 1-4 h at the temperature of 75-85 ℃;
(3) Chain extension reaction: continuously reacting hydrophilic chain extender, cross-linking agent, micromolecular alcohol and acetone in a reaction kettle at the temperature of 60-80 ℃ for 2-4 h, then adding water-soluble chain extender Poly-EPS (PPS) and acetone, and continuously reacting for 1-2 h at the temperature of 60-70 ℃;
(4) Water dispersion: adjusting the temperature to 0-20 ℃, then dripping deionized water and a neutralizing agent into the mixture for emulsification, then flowing diamine chain extender into the mixture, strongly stirring the mixture at the stirring speed of 1200-1700 r/min, and carrying out chain extension for 10min +/-1 min;
(5) Removing acetone: removing acetone under the conditions that the temperature is 50 +/-5 ℃ and the vacuum degree is-0.08 MPa to obtain the waterborne polyurethane with the solid content of 60 percent.
In one embodiment, the oligomer polyol is one or more of adipic acid series polyol, polycaprolactone diol, polycarbonate diol, polyether polyol.
In one embodiment, the polyether polyol is one or two of polyoxypropylene diol and polyoxypropylene triol, the molecular weight of the polyether polyol is 500-5000, and the average hydroxyl value of the polyether polyol is 10mgKOH/g-300 mgKOH/g.
In one embodiment, the isocyanate is one or two of isophorone diisocyanate, dicyclohexylmethane diisocyanate, and 1, 6-hexamethylene diisocyanate.
In one embodiment, the hydrophilic chain extender is one or two of dimethylolpropionic acid and dimethylolbutyric acid;
the diamine chain extender is one or more of ethylenediamine, butanediamine, hydroxyethyl ethylenediamine and isophorone diamine.
In one embodiment, the antioxidant is one or two of 2, 6-di-tert-butyl-p-cresol and pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
In one embodiment, the catalyst is one or more of dibutyltin dilaurate, octyl stannous, organic bismuth and organic zinc.
In one embodiment, the cross-linking agent is one or two of glycerol and trimethylolpropane;
the small molecular alcohol is one or more of ethylene glycol, 1,4 butanediol and 1,6 hexanediol.
In one embodiment, the neutralizing agent is one or two of triethylamine, triethanolamine and ammonia water.
In one embodiment, the high-solid water-containing polyurethane comprises, by weight, 80-100 parts of oligomer polyol, 25-45 parts of polyisocyanate, 4-5 parts of water-soluble chain extender Poly-EPS (PPS), 1-3 parts of hydrophilic chain extender, 1-10 parts of diamine chain extender, 0.1-0.3 part of antioxidant, 0.1-0.2 part of catalyst, 0-2 parts of cross-linking agent, 1.5-2.5 parts of neutralizer, 0-4 parts of small molecular alcohol and 90-105 parts of deionized water.
According to the preparation method of the high-solid-content waterborne polyurethane, the dosage of the hydrophilic chain extender is reduced by optimizing the polyol and the water-soluble chain extender and introducing the water-soluble chain extender Poly-EPS (PPS), so that the solid content of the waterborne polyurethane is increased, and the high-solid-content waterborne polyurethane resin with high comprehensive performance is obtained.
The 60% solid content aqueous polyurethane emulsion prepared by the invention has good comprehensive performance, good film forming property and dispersibility, low viscosity, and stable and easy storage.
Drawings
FIG. 1 is an infrared spectrum of the high-solid content aqueous polyurethane prepared by the present invention;
FIG. 2 is a SEM image of 5000 times of the cross section of the high-solid aqueous polyurethane coating film prepared by the invention;
FIG. 3 is an SEM image of 20000 times of the cross section of the high solid content aqueous polyurethane coating film prepared by the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments accompanying figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
As used herein, the term "consisting of 8230; preparation" is synonymous with "comprising". As used herein, the terms "comprises," "comprising," "includes," "including," "has," "having," "contains" or any other variation thereof, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or range defined by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise specified, the range is intended to include the endpoints thereof, and all integers and fractions within the range.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1
First, 90g of 1, 4-butanediol adipate diol having a molecular weight of 2000, 10g of polyoxypropylene diol having a molecular weight of 2000 and 0.3g of pentaerythritol tetrakis [ beta- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ] were charged into a 500ml four-necked flask equipped with a stirrer and a thermometer, and dehydrated at a temperature of 110 ℃ under a vacuum of-0.09 MPa for 1 hour; then introducing nitrogen, adding 28g of isophorone diisocyanate and 0.1g of dibutyltin dilaurate under the protection of nitrogen, reacting for 3h at the temperature of 75 ℃, then adding 2.4g of dimethylolpropionic acid, 2.0g of trimethylolpropane and 50g of acetone, controlling the temperature to be 75 ℃, continuing to react for 3h, reducing the temperature, diluting with 100g of acetone, adding 4g of water-soluble chain extender Poly-EPS (PPS) at the temperature of 60 ℃, reacting for 2h, further adding 30g of acetone for diluting, adding a mixture of 1.8g of triethylamine and 77.6g of deionized water under high-speed dispersion, controlling the water temperature to be below 20 ℃, then adding 4g of isophorone diamine and 16g of deionized water to obtain an aqueous polyurethane emulsion, and finally carrying out reduced pressure distillation on the obtained aqueous polyurethane emulsion under the conditions that the temperature is 50 ℃ and the vacuum degree is-0.08 MPa, and removing the acetone to obtain the high-solid content aqueous polyurethane.
Example 2
Firstly, 100g of polyester polyol formed by mixing 1, 4-butanediol adipate with molecular weight of 2000 and neopentyl glycol and 0.3g of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] are added into a 500ml four-necked bottle with a stirrer and a thermometer, and dehydration is carried out for 2h under the conditions that the temperature is 120 ℃ and the vacuum degree is-0.09 MPa; then introducing nitrogen, adding 33g of dicyclohexylmethane diisocyanate and 0.1g of dibutyltin dilaurate under the protection of nitrogen, reacting for 3h at the temperature of 75 ℃, adding 2.5g of dimethylolpropionic acid, 1.0g of trimethylolpropane, 1.2g of 1,4 butanediol and 52g of acetone, controlling the temperature at 75 ℃ and continuing to react for 3h, cooling, diluting with 100g of acetone, adding 4.2g of water-soluble chain extender Poly-EPS (PPS) at the temperature of 70 ℃ for reacting for 2h, further adding 30g of acetone for diluting, adding a mixture of 1.8g of triethylamine and 79g of deionized water under high-speed dispersion, controlling the water temperature to be below 20 ℃, then adding 1.5g of ethylenediamine and 13.5g of deionized water to obtain an aqueous polyurethane emulsion, and finally decompressing and distilling the obtained aqueous polyurethane emulsion under the conditions of 50 ℃ and the vacuum degree of-0.08 MPa to remove the acetone to obtain the high-solid-content aqueous polyurethane.
Example 3
First, 100g of polycarbonate diol having a molecular weight of 2000 and 0.2g of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] were charged into a 500ml four-necked flask equipped with a stirrer and a thermometer, and dehydrated for 2 hours at a temperature of 120 ℃ and a vacuum degree of-0.09 MPa; then introducing nitrogen, adding 35g of isophorone diisocyanate and 0.1g of dibutyltin dilaurate under the protection of nitrogen, reacting for 3h at the temperature of 75 ℃, then adding 3.0g of dimethylolpropionic acid, 0.5g of trimethylolpropane, 0.8g of 1,4 butanediol and 45g of acetone, controlling the temperature at 75 ℃ to continue reacting for 3h, cooling, diluting with 90g of acetone, adding 5.0g of water-soluble chain extender Poly-EPS (PPS) at the temperature of 65 ℃ to react for 2h, further adding 25g of acetone to dilute, adding a mixture of 2.26g of triethylamine and 63.5g of deionized water under high-speed dispersion, controlling the water temperature below 20 ℃, then adding 7.0g of isophorone diamine and 28g of deionized water to obtain an aqueous polyurethane emulsion, and finally decompressing and distilling the aqueous polyurethane under the conditions of 50 ℃ and vacuum degree of-0.08 MPa to remove acetone to obtain the high-solid-content aqueous polyurethane.
Example 4
First, 80g of polycarbonate diol having a molecular weight of 2000, 20g of polyoxypropylene glycol having a molecular weight of 2000 and 0.3g of pentaerythritol tetrakis [ beta- (3, 5-di-t-butyl-4-hydroxyphenyl) propionate ] were put into a 500ml four-necked flask equipped with a stirrer and a thermometer, and dehydrated for 2 hours at a temperature of 120 ℃ and a vacuum degree of-0.09 MPa; then introducing nitrogen, adding 41.3g of dicyclohexylmethane diisocyanate and 0.15g of organic bismuth under the protection of nitrogen, reacting for 3h at the temperature of 75 ℃, then adding 2.8g of dimethylolpropionic acid, 3.8g of 1.4 butanediol and 40g of acetone, simultaneously controlling the temperature to be 75 ℃, continuing to react for 3h, cooling, diluting with 85g of acetone, adding 4.5g of water-soluble chain extender Poly-EPS (PPS) at the temperature of 70 ℃, reacting for 2h, then adding 24g of acetone for diluting, adding a mixture of 2.1g of triethylamine and 79.6g of deionized water under high-speed dispersion, controlling the water temperature to be below 20 ℃, then adding 6g of isophorone diamine and 24g of deionized water to obtain an aqueous polyurethane emulsion, and finally carrying out reduced pressure distillation on the obtained aqueous polyurethane emulsion under the conditions of the temperature of 50 ℃ and the vacuum degree of-0.08 MPa, and removing the acetone to obtain the high-solid content aqueous polyurethane.
The high solid content aqueous polyurethane prepared in the above examples 1 to 4 was tested, and the test method and results were as follows:
solid content detection was carried out according to GB/T11175-2002 synthetic resin emulsion test method, and it was found that the solid contents of examples 1 to 4 were all 60%.
The viscosity was measured according to GB/T2794-2013 viscosity Single Cylinder rotational viscometer method for determination of adhesive viscosity, and it was found that the viscosity of example 1 was 100 cps/25 ℃, the viscosity of examples 2 and 3 was 300cps/25 ℃ and the viscosity of example 4 was 200 cps/25 ℃.
As shown in figure 1, the result of the infrared spectrogram shows that the product prepared by the invention has a polyurethane structure and has the performance of a polyurethane material; in addition, as shown in fig. 2 and fig. 3, it can be seen from the scanning electron microscope images of the cross section of the coating film that the nanoparticles of the product prepared by the preparation method of the present invention are uniformly dispersed in the aqueous polyurethane emulsion, and thus it can be seen that the amount of the hydrophilic chain extender is reduced by introducing the water-soluble chain extender Poly-EPS (PPS), such that the aqueous polyurethane emulsion with 60% solid content and good stability can be prepared, and the film forming property is good, such that the user's requirements can be satisfied.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of high-solid content waterborne polyurethane is characterized by comprising the following steps:
(1) Vacuum dehydration: mixing oligomer polyol and antioxidant, and dehydrating for 1-2 h at the temperature of 110-120 ℃ and the vacuum degree of-0.09 MPa;
(2) Prepolymerization reaction: introducing nitrogen into a reaction kettle, adding polyisocyanate and a polyurethane catalyst under the protection of the nitrogen, and reacting for 1-4 h at the temperature of 75-85 ℃;
(3) Chain extension reaction: continuously reacting hydrophilic chain extender, cross-linking agent, micromolecular alcohol and acetone in a reaction kettle at the temperature of 60-80 ℃ for 2-4 h, then adding water-soluble chain extender Poly-EPS (PPS) and acetone, and continuously reacting for 1-2 h at the temperature of 60-70 ℃;
(4) Water dispersion: adjusting the temperature to 0-20 ℃, then dripping deionized water and a neutralizing agent into the emulsion, then flowing diamine chain extender into the emulsion, strongly stirring the mixture at the stirring speed of 1200-1700 r/min for chain extension of 10min +/-1 min;
(5) Removing acetone: removing acetone under the conditions that the temperature is 50 +/-5 ℃ and the vacuum degree is-0.08 MPa to obtain the waterborne polyurethane with the solid content of 60 percent.
2. The method of claim 1, wherein the oligomer polyol is one or more selected from adipic acid-series polyol, polycaprolactone diol, polycarbonate diol, and polyether polyol.
3. The method for preparing the high-solid content waterborne polyurethane as claimed in claim 2, wherein the polyether polyol is one or both of polyoxypropylene diol and polyoxypropylene triol, the molecular weight of the polyether polyol is 500-5000, and the average hydroxyl value of the polyether polyol is 10mgKOH/g-300 mgKOH/g.
4. The method of claim 1, wherein the isocyanate is one or two of isophorone diisocyanate, dicyclohexylmethane diisocyanate, and 1, 6-hexamethylene diisocyanate.
5. The preparation method of the high-solid content waterborne polyurethane as claimed in claim 1, wherein the hydrophilic chain extender is one or two of dimethylolpropionic acid and dimethylolbutyric acid;
the diamine chain extender is one or more of ethylenediamine, butanediamine, hydroxyethyl ethylenediamine and isophorone diamine.
6. The method of claim 1, wherein the antioxidant is one or two of 2, 6-di-tert-butyl-p-cresol and pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
7. The method for preparing the high-solid content waterborne polyurethane as claimed in claim 1, wherein the catalyst is one or more of dibutyltin dilaurate, stannous octyl ester, organic bismuth and organic zinc.
8. The method for preparing the high-solid-content waterborne polyurethane as claimed in claim 1, wherein the cross-linking agent is one or both of glycerol and trimethylolpropane;
the small molecular alcohol is one or more of ethylene glycol, 1,4 butanediol and 1,6 hexanediol.
9. The method for preparing the high-solid content aqueous polyurethane according to claim 1, wherein the neutralizing agent is one or two of triethylamine, triethanolamine and ammonia water.
10. The preparation method of the high-solid content aqueous polyurethane according to any one of claims 1 to 9, wherein the high-solid content aqueous polyurethane comprises 80 to 100 parts by weight of oligomer polyol, 25 to 45 parts by weight of polyisocyanate, 4 to 5 parts by weight of water-soluble chain extender Poly-EPS (PPS), 1 to 3 parts by weight of hydrophilic chain extender, 1 to 10 parts by weight of diamine chain extender, 0.1 to 0.3 part by weight of antioxidant, 0.1 to 0.2 part by weight of catalyst, 0 to 2 parts by weight of crosslinking agent, 1.5 to 2.5 parts by weight of neutralizer, 0 to 4 parts by weight of small molecular alcohol and 90 to 105 parts by weight of deionized water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210920053.XA CN115160530A (en) | 2022-08-02 | 2022-08-02 | Preparation method of high-solid-content waterborne polyurethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210920053.XA CN115160530A (en) | 2022-08-02 | 2022-08-02 | Preparation method of high-solid-content waterborne polyurethane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115160530A true CN115160530A (en) | 2022-10-11 |
Family
ID=83476698
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210920053.XA Pending CN115160530A (en) | 2022-08-02 | 2022-08-02 | Preparation method of high-solid-content waterborne polyurethane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115160530A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597369A (en) * | 2008-06-06 | 2009-12-09 | 佛山市南海霸力化工制品有限公司 | Contain high solid content polyurethane emulsion of alicyclic sulfonic acid type hydrophilic chain extending agent and preparation method thereof |
| 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 |
| CN103305175A (en) * | 2013-06-14 | 2013-09-18 | 华南理工大学 | Environmental-friendly high-solid-content aqueous-polyurethane adhesive for shoes and preparation method thereof |
| CN105384900A (en) * | 2015-12-16 | 2016-03-09 | 武汉工程大学 | Method for preparing high solid content anionic aqueous polyurethane dispersion |
-
2022
- 2022-08-02 CN CN202210920053.XA patent/CN115160530A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597369A (en) * | 2008-06-06 | 2009-12-09 | 佛山市南海霸力化工制品有限公司 | Contain high solid content polyurethane emulsion of alicyclic sulfonic acid type hydrophilic chain extending agent and preparation method thereof |
| 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 |
| CN103305175A (en) * | 2013-06-14 | 2013-09-18 | 华南理工大学 | Environmental-friendly high-solid-content aqueous-polyurethane adhesive for shoes and preparation method thereof |
| CN105384900A (en) * | 2015-12-16 | 2016-03-09 | 武汉工程大学 | Method for preparing high solid content anionic aqueous polyurethane dispersion |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kurimoto et al. | Mechanical properties of polyurethane films prepared from liquefied wood with polymeric MDI | |
| Liu et al. | Preparation and properties of waterborne polyurethanes with natural dimer fatty acids based polyester polyol as soft segment | |
| Deng et al. | Effects of the reagent ratio on the properties of waterborne polyurethanes-acrylate for application in damping coating | |
| DE3426875C2 (en) | Process for the production of polyurethanes with outstanding hydrolysis resistance | |
| CN114075322A (en) | Waterborne polyurethane resin emulsion and preparation method thereof | |
| CN114133541B (en) | High-hydrolysis-resistance polyester polyol, preparation method thereof and application thereof in waterborne polyurethane resin | |
| CN112409564A (en) | Non-desolventizing water-based nonionic polyurethane and preparation method thereof | |
| CN113980571A (en) | Waterborne polyurethane waterproof coating and preparation method and application thereof | |
| US5436056A (en) | Method of producing a high molecular weight aliphatic polyester and film thereof | |
| CN112851898A (en) | Self-extinction waterborne polyurethane resin, preparation method and application | |
| CN110845981A (en) | Environment-friendly water-based polyurethane adhesive for automobiles and preparation method thereof | |
| CN109535372A (en) | A kind of aqueous polyurethane and preparation method thereof | |
| CN109880575B (en) | Waterborne polyurethane adhesive and preparation method thereof | |
| CN113980225A (en) | Hydroxypropyl distarch phosphate modified waterborne polyurethane resin and preparation method thereof | |
| CN115160530A (en) | Preparation method of high-solid-content waterborne polyurethane | |
| CN112980376A (en) | Waterborne polyurethane adhesive and preparation method thereof | |
| CN111936565B (en) | Coated body | |
| CN112279992A (en) | UV-curable water-based resin and preparation method and application thereof | |
| EP3572474B1 (en) | Biomaterial-based uv coating composition | |
| CN110845838A (en) | Polycarbonate type polyurethane film and preparation thereof | |
| Bayat et al. | Synthesis and characterization of transparent 1-package PUD based on castor oil and polyethylene glycol | |
| CN113956429A (en) | Thermoplastic polyurethane elastomer and preparation method thereof | |
| JPS6021655B2 (en) | automotive glass run | |
| Kwon et al. | Effect of chemical structure on the properties of UV-cured polyurethane acrylates films | |
| Wang et al. | Synthesis of waterborne polyurethane dispersions with glycolyzed product from pet waste: Effect of hard segment content on its properties |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |