CN110684172A - Water-pressure-resistant water-based polyurethane resin - Google Patents
Water-pressure-resistant water-based polyurethane resin Download PDFInfo
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- CN110684172A CN110684172A CN201911103401.9A CN201911103401A CN110684172A CN 110684172 A CN110684172 A CN 110684172A CN 201911103401 A CN201911103401 A CN 201911103401A CN 110684172 A CN110684172 A CN 110684172A
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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
- C08G18/08—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
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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
- C08G18/08—Processes
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4202—Two or more polyesters of different physical or chemical nature
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
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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
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a water pressure resistant water-based polyurethane resin, which comprises raw materials including polyol, polyisocyanate, a hydrophilic carboxylic acid chain extender, polycarbonate diol, dimer acid ester diol, a first neutralizer, a second neutralizer, acetone and a stabilizer.
Description
Technical Field
The invention relates to the field of preparation of polyurethane resin, and particularly relates to water-resistant water-soluble polyurethane resin.
Background
Polyurethane is a novel synthetic material, and has high elasticity of rubber and high strength of plastics due to a special molecular structure, so that the polyurethane is rapidly developed in both application range and use quantity in recent decades. The polyurethane synthetic leather has the appearance of soft and natural luster, soft hand feeling and strong real leather feeling, has excellent bonding performance with a base material, good abrasion resistance, deflection resistance, aging resistance, mould resistance and the like, also has the advantages of good cold resistance, ventilation, washability, convenient processing, low price and the like, is the most ideal substitute of natural leather, and is widely applied to the industries of clothing, shoemaking, bags, furniture, sports and the like.
And because a large amount of hydrophilic groups and lower molecular weight exist in the polyurethane resin, the corrosion resistance is poorer than that of the solvent resin of the same type, and the low water pressure resistance of the polyurethane resin easily causes the low tensile strength of the polyurethane resin, so that the service life of the prepared synthetic material is short.
Disclosure of Invention
In order to solve the problems, the invention provides a water-resistant water-based polyurethane resin.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a water pressure resistant water-based polyurethane resin comprises the following raw materials of polyol, polyisocyanate, a hydrophilic carboxylic acid chain extender, polycarbonate diol, dimer acid ester diol, a first neutralizing agent, a second neutralizing agent, acetone and a stabilizer, and the specific preparation method comprises the following steps: the method comprises the following steps: adding polyol, polyisocyanate and a hydrophilic carboxylic acid chain extender into a reaction container, vacuumizing a reaction system, and filling nitrogen for vacuum reaction; step two: stirring is started to mix the solvent in the reaction vessel, the hydrophilic carboxylic acid chain extender is dissolved, and then polycarbonate diol and dimer acid ester diol are added into the reaction vessel; step three: dripping isophorone diisocyanate into the reaction container through a constant pressure funnel, heating to 75 ℃, keeping the temperature for 5 hours, and adding a stabilizer; step four: sampling and detecting the content of the isocyanate group, reducing the temperature to 70 ℃ after the content reaches the standard, and adding a first neutralizer for neutralization reaction; step five: and adding acetone to adjust viscosity, reducing the temperature to be below 30 ℃, adding a second neutralizing agent to perform a neutralization reaction, adding ice water and a solvent while rapidly stirring, performing high-speed dispersion for 1.5h, and removing the acetone under reduced pressure to obtain the waterborne polyurethane resin.
Preferably, the weight parts of the polyhydric alcohol are 80-120 parts, the weight parts of the polyisocyanate are 30-50 parts, the weight parts of the hydrophilic carboxylic acid chain extender are 15-35 parts, the weight parts of the polycarbonate diol are 10-30 parts, the weight parts of the dimer acid ester diol are 10-30 parts, the weight parts of the first neutralizing agent are 3-7 parts, the weight parts of the second neutralizing agent are 4-12 parts, the weight parts of the acetone are 30 parts and the weight parts of the stabilizer are 4-12 parts.
Preferably, the treatment temperature in the first step is 60-150 ℃, and the reaction time is 6-15 hours.
Preferably, the hydrophilic carboxylic acid-based chain extender is dimethylolpropionic acid.
Preferably, the first neutralizing agent is one or more of triethylamine, dimethylethanolamine and ammonia water.
Preferably, the reaction time of the first neutralizing agent in the fourth step is 45 min.
Preferably, the second neutralizing agent is glycine.
Preferably, the reaction time of the second neutralizing agent in the fifth step is 30 min.
Preferably, the stabilizer is UV-531.
As can be seen from the above description of the present invention, compared with the prior art, the present invention has the following advantages:
according to the water pressure resistant water-based polyurethane resin, the polycarbonate diol and the dimer acid ester diol are added as raw materials, so that the tensile strength of the synthesized polyurethane resin is improved, the water pressure resistance is improved, the neutralization degree in synthesis is increased by adding the first neutralizing agent and the second neutralizing agent in the synthesis of the raw materials by an acetone method, and the water resistance of the prepared polyurethane resin is greatly improved.
Drawings
FIG. 1 is a line graph showing the amount of dimer acid ester diol in the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
A water pressure resistant water-based polyurethane resin comprises the following raw materials of polyol, polyisocyanate, a hydrophilic carboxylic acid chain extender, polycarbonate diol, dimer acid ester diol, a first neutralizing agent, a second neutralizing agent, acetone and a stabilizer, and the specific preparation method comprises the following steps: the method comprises the following steps: adding polyol, polyisocyanate and a hydrophilic carboxylic acid chain extender into a reaction container, vacuumizing a reaction system, and filling nitrogen for vacuum reaction; step two: stirring is started to mix the solvent in the reaction vessel, the hydrophilic carboxylic acid chain extender is dissolved, and then polycarbonate diol and dimer acid ester diol are added into the reaction vessel; step three: dripping isophorone diisocyanate into the reaction container through a constant pressure funnel, heating to 75 ℃, keeping the temperature for 5 hours, and adding a stabilizer; step four: sampling and detecting the content of the isocyanate group, reducing the temperature to 70 ℃ after the content reaches the standard, and adding a first neutralizer for neutralization reaction; step five: adding acetone to adjust viscosity, reducing the temperature to be below 30 ℃, adding a second neutralizing agent to perform a neutralization reaction, adding ice water and a solvent while rapidly stirring, performing high-speed dispersion for 1.5h, and removing the acetone under reduced pressure to obtain the waterborne polyurethane resin; 80-120 parts of polyol, 30-50 parts of polyisocyanate, 15-35 parts of hydrophilic carboxylic acid chain extender, 10-30 parts of polycarbonate diol, 10-30 parts of dimer acid ester diol, 3-7 parts of first neutralizer, 4-12 parts of second neutralizer, 30 parts of acetone and 4-12 parts of stabilizer; in the first step, the treatment temperature is 60-150 ℃, and the reaction time is 6-15 hours; the hydrophilic carboxylic acid chain extender is dimethylolpropionic acid; the first neutralizer is one or more of triethylamine, dimethylethanolamine and ammonia water; the reaction time of the first neutralizer in the fourth step is 45 min; the second neutralizing agent is glycine; in the fifth step, the reaction time of the second neutralizing agent is 30 min; the stabilizer is UV-531.
The tensile strength and water pressure resistance of the polyurethane resin using the polycarbonate diol were tested, and the data of the test are shown in the following table:
| name (R) | Water pressure resistance/KPa | Tensile strength/MPa |
| Polycarbonate diol | 32 | 32 |
As can be seen from the above table, the water pressure resistance of the polyurethane resin using the polycarbonate diol was 32KPa, and the tensile strength was 32 MPa.
The purpose of selecting the dimer acid ester dihydric alcohol is to increase the hydrolysis resistance of the polyurethane resin, and the specific weight results of the dimer acid ester dihydric alcohol are shown in the following table:
as can be seen from the above table, the hydrolysis resistance of the polyurethane resin increases with the amount of the dimer acid ester diol, and the highest hydrolysis resistance of the polyurethane resin is obtained at 30 parts.
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 and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. The water pressure resistant waterborne polyurethane resin is characterized in that raw materials comprise polyol, polyisocyanate, hydrophilic carboxylic acid chain extender, polycarbonate diol, dimer acid ester diol, a first neutralizer, a second neutralizer, acetone and a stabilizer, and the specific preparation method comprises the following steps:
the method comprises the following steps: adding polyol, polyisocyanate and a hydrophilic carboxylic acid chain extender into a reaction container, vacuumizing a reaction system, and filling nitrogen for vacuum reaction;
step two: stirring is started to mix the solvent in the reaction vessel, the hydrophilic carboxylic acid chain extender is dissolved, and then polycarbonate diol and dimer acid ester diol are added into the reaction vessel;
step three: dripping isophorone diisocyanate into the reaction container through a constant pressure funnel, heating to 75 ℃, keeping the temperature for 5 hours, and adding a stabilizer;
step four: sampling and detecting the content of the isocyanate group, reducing the temperature to 70 ℃ after the content reaches the standard, and adding a first neutralizer for neutralization reaction;
step five: and adding acetone to adjust viscosity, reducing the temperature to be below 30 ℃, adding a second neutralizing agent to perform a neutralization reaction, adding ice water and a solvent while rapidly stirring, performing high-speed dispersion for 1.5h, and removing the acetone under reduced pressure to obtain the waterborne polyurethane resin.
2. The water-pressure resistant aqueous polyurethane resin according to claim 1, wherein: the weight parts of the polyhydric alcohol are 80-120 parts, the weight parts of the polyisocyanate are 30-50 parts, the weight parts of the hydrophilic carboxylic acid chain extender are 15-35 parts, the weight parts of the polycarbonate diol are 10-30 parts, the weight parts of the dimer acid ester diol are 10-30 parts, the weight parts of the first neutralizer is 3-7 parts, the weight parts of the second neutralizer is 4-12 parts, the weight parts of the acetone is 30 parts and the weight parts of the stabilizer are 4-12 parts.
3. The water-pressure resistant aqueous polyurethane resin according to claim 1, wherein: in the first step, the treatment temperature is 60-150 ℃, and the reaction time is 6-15 hours.
4. The water-pressure resistant aqueous polyurethane resin according to claim 1, wherein: the hydrophilic carboxylic acid chain extender is dimethylolpropionic acid.
5. The water-pressure resistant aqueous polyurethane resin according to claim 1, wherein: the first neutralizer is one or more of triethylamine, dimethylethanolamine and ammonia water.
6. The water-pressure resistant aqueous polyurethane resin according to claim 1, wherein: the reaction time of the first neutralizing agent in the fourth step is 45 min.
7. The water-pressure resistant aqueous polyurethane resin according to claim 1, wherein: the second neutralizing agent is glycine.
8. The water-pressure resistant aqueous polyurethane resin according to claim 1, wherein: and the reaction time of the second neutralizing agent in the fifth step is 30 min.
9. The water-pressure resistant aqueous polyurethane resin according to claim 1, wherein: the stabilizer is UV-531.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911103401.9A CN110684172A (en) | 2019-11-12 | 2019-11-12 | Water-pressure-resistant water-based polyurethane resin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911103401.9A CN110684172A (en) | 2019-11-12 | 2019-11-12 | Water-pressure-resistant water-based polyurethane resin |
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| CN110684172A true CN110684172A (en) | 2020-01-14 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613451A (en) * | 2009-08-05 | 2009-12-30 | 辽宁恒星精细化工（集团）有限公司 | High-content aqueous polyurethane latex and preparation method |
| CN105111399A (en) * | 2015-09-21 | 2015-12-02 | 宜兴市华夏化工材料有限公司 | Water pressure resistant water-based polyurethane resin |
| CN107266650A (en) * | 2017-07-14 | 2017-10-20 | 合肥思敬齐化工材料有限责任公司 | Water pressure resistance waterproof polyurethane fabric finish and preparation method thereof |
| CN107523204A (en) * | 2017-09-22 | 2017-12-29 | 安庆市虹泰新材料有限责任公司 | A kind of preparation method of the polyurethane aqueous coating adhesive of dimer acid type |
-
2019
- 2019-11-12 CN CN201911103401.9A patent/CN110684172A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613451A (en) * | 2009-08-05 | 2009-12-30 | 辽宁恒星精细化工（集团）有限公司 | High-content aqueous polyurethane latex and preparation method |
| CN105111399A (en) * | 2015-09-21 | 2015-12-02 | 宜兴市华夏化工材料有限公司 | Water pressure resistant water-based polyurethane resin |
| CN107266650A (en) * | 2017-07-14 | 2017-10-20 | 合肥思敬齐化工材料有限责任公司 | Water pressure resistance waterproof polyurethane fabric finish and preparation method thereof |
| CN107523204A (en) * | 2017-09-22 | 2017-12-29 | 安庆市虹泰新材料有限责任公司 | A kind of preparation method of the polyurethane aqueous coating adhesive of dimer acid type |
Non-Patent Citations (1)
| Title |
|---|
| 杨青，: ""水性高耐水压聚氨酯涂层胶"", 《染整技术》 * |
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Application publication date: 20200114 |