CN103012733A - Method for preparing mono-component normal-temperature self-crosslinking water-based polyurethane - Google Patents
Method for preparing mono-component normal-temperature self-crosslinking water-based polyurethane Download PDFInfo
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- CN103012733A CN103012733A CN2012105542958A CN201210554295A CN103012733A CN 103012733 A CN103012733 A CN 103012733A CN 2012105542958 A CN2012105542958 A CN 2012105542958A CN 201210554295 A CN201210554295 A CN 201210554295A CN 103012733 A CN103012733 A CN 103012733A
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Abstract
The invention discloses a method for preparing mono-component normal-temperature self-crosslinking water-based polyurethane. The method comprises the following steps: taking diol 3-[bis-(2-hydroethyl)] amine-N (1,1-dimethyl-3-butanone) propionamide (DHPA) containing ketone carbonyl as a crosslinking chain extender for preparing polyurethane from isophorone diisocyanate (IPDI) and polyethylene glycol (PEG 3000), adding a hydrophilic chain extender of dimethylolpropionic acid (DMPA), neutralizing the mixture with triethylamine, and adding water for emulsification and separation to obtain the mono-component normal-temperature self-crosslinking water-based polyurethane. The emulsion has the function of self-crosslinking and the characteristics of excellent water and solvent resistances.
Description
Technical field
The present invention relates to a kind of preparation method of single-component ambient self-crosslinking aqueous polyurethane, belong to chemical field.
Technical background
Aqueous polyurethane is take water as medium, and safety and environmental protection is free from environmental pollution, has simultaneously good physical and mechanical properties, and excellent low temperature resistant, weathering resistance are widely used in the fields such as coating, sizing agent, clothing arrangement, leather.But with respect to solvent borne polyurethane, aqueous polyurethane be because the restriction of synthesis technique can only obtain linear structure, and because the introducing of hydrophilic radical, often has the shortcomings such as water-fast, solvent resistance and poor mechanical property.Crosslinked is the effective ways that improve Property of Waterborne Polyurethane, and the aqueous polyurethane of exploitation cold cross-linking becomes an important direction.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of single-component ambient self-crosslinking aqueous polyurethane, the aqueous polyurethane emulsion that obtains has the self-crosslinking function, and emulsion film has excellent water tolerance and solvent resistance.
For realizing above purpose, the preparation method of a kind of single-component ambient self-crosslinking aqueous polyurethane of the present invention, its step is specially:
(1) prepares base polyurethane prepolymer for use as take isophorone diisocyanate (IPDI), polyoxyethylene glycol (PEG3000), dimethylol propionic acid (DMPA) as raw material, be that 81 ℃, rotating speed are stirring reaction 3h under the condition of 900r/min in temperature, look viscosity in the process and change adding solvent N-first class pyrrolidone (NMP), consumption is can make stirring be as the criterion smoothly.
(2) adding 3-[two-(2-hydroxyethyl)] amido-N (1,1-dimethyl-3 butanone) propionic acid amide (DHPA) is to the crosslinked chain extension of performed polymer, and the consumption of DHPA is the 2%-8% of performed polymer quality.
(3) be cooled to 40 ℃, add triethylamine and carry out neutralization reaction generation salt, reaction 3-4min.
(4) add the entry strong stirring, rotating speed is 1800r/min, and emulsification 60min obtains the single-component waterborne polyurethane emulsion capable of self-crosslinking at normal temperature.
The proportioning of performed polymer raw material is in the step (1): the mol ratio of IPDI and PEG1000, DMPA is 1.1:1, and DMPA accounts for 6% of performed polymer quality.
The amount of substance of triethylamine is identical with the amount of substance of DMPA in the step (3).
The consumption of the middle water of step (4) is 2 times of performed polymer total mass.
The beneficial effect that the present invention produces is, this patent is with dibasic alcohol 3-[two-(the 2-hydroxyethyl) of ketocarbonyl-containing] amido-N (1,1-dimethyl-3 butanone) propionic acid amide (DHPA) is crosslinked chainextender, participate in isophorone diisocyanate (IPDI) and prepare in the process of urethane with polyoxyethylene glycol (PEG3000), prepare the single-component waterborne polyurethane emulsion capable of self-crosslinking at normal temperature.After introducing DHPA, because the electronegativity of the Sauerstoffatom on the ketone carbonyl is greater than carbon atom, the electrophilic ability of Sauerstoffatom is strong, so the carbon ribbon on the carbonyl has part positive charge, affine addition reaction occurs the hydrazine that can attract to be rich in electronics, produces carbon nitrogen covalent linkage.Therefore, the emulsion of preparing has the self-crosslinking performance.Because self-crosslinking having occured, formed the macromole tridimensional network, the contact between the macromolecular chain becomes closely, so that water molecules can not enter easily swelling occurs between molecular chain, and the water tolerance solvent resistance strengthens.
Embodiment
Embodiment 1:
Under rotating speed 900r/min, 81 ℃ condition, prepare base polyurethane prepolymer for use as take isophorone diisocyanate (IPDI), polyoxyethylene glycol (PEG3000), dimethylol propionic acid (DMPA) as raw material, reaction 3h, the mol ratio of IPDI and PEG1000, DMPA is 1.1:1, and DMPA accounts for 6% of performed polymer quality.Look viscosity in the process and change adding solvent N-first class pyrrolidone (NMP).Adding 3-[two-(2-hydroxyethyl)] amido-N (1,1-dimethyl-3 butanone) propionic acid amide (DHPA) is to the crosslinked chain extension of performed polymer, and the consumption of DHPA is 2% of performed polymer quality.Be cooled to 40 ℃, add triethylamine and carry out neutralization reaction generation salt, reaction 3min.The amount of substance of triethylamine is identical with the amount of substance of DMPA.Rotating speed is increased to 1800r/min, adds emulsifying water 60min, the consumption of water is 2 times of performed polymer total mass.Obtain the single-component waterborne polyurethane emulsion capable of self-crosslinking at normal temperature.
The degree of crosslinking of aqueous polyurethane emulsion is 20%, and water-intake rate is 18%.
Embodiment 2:
Under rotating speed 900r/min, 81 ℃ condition, prepare base polyurethane prepolymer for use as take isophorone diisocyanate (IPDI), polyoxyethylene glycol (PEG3000), dimethylol propionic acid (DMPA) as raw material, reaction 3h, the mol ratio of IPDI and PEG1000, DMPA is 1.1:1, and DMPA accounts for 6% of performed polymer quality.Look viscosity in the process and change adding solvent N-first class pyrrolidone (NMP).Adding 3-[two-(2-hydroxyethyl)] amido-N (1,1-dimethyl-3 butanone) propionic acid amide (DHPA) is to the crosslinked chain extension of performed polymer.The consumption of DHPA is 4% of performed polymer quality.Be cooled to 40 ℃, add triethylamine and carry out neutralization reaction generation salt, reaction 3min.The amount of substance of triethylamine is identical with the amount of substance of DMPA.Rotating speed is increased to 1800r/min, adds emulsifying water 60min, the consumption of water is 2 times of performed polymer total mass.Obtain the single-component waterborne polyurethane emulsion capable of self-crosslinking at normal temperature.
The degree of crosslinking of aqueous polyurethane emulsion is 40%, and water-intake rate is 15%.
Embodiment 3:
Under rotating speed 900r/min, 81 ℃ condition, prepare base polyurethane prepolymer for use as take isophorone diisocyanate (IPDI), polyoxyethylene glycol (PEG3000), dimethylol propionic acid (DMPA) as raw material, reaction 3h, the mol ratio of IPDI and PEG1000, DMPA is 1.1:1, and DMPA accounts for 6% of performed polymer quality.Look viscosity in the process and change adding solvent N-first class pyrrolidone (NMP).Adding 3-[two-(2-hydroxyethyl)] amido-N (1,1-dimethyl-3 butanone) propionic acid amide (DHPA) is to the crosslinked chain extension of performed polymer.The consumption of DHPA is 6% of performed polymer quality.Be cooled to 40 ℃, add triethylamine and carry out neutralization reaction generation salt, reaction 3min.The amount of substance of triethylamine is identical with the amount of substance of DMPA.Rotating speed is increased to 1800r/min, adds emulsifying water 60min, the consumption of water is 2 times of performed polymer total mass.Obtain the single-component waterborne polyurethane emulsion capable of self-crosslinking at normal temperature.
The degree of crosslinking of aqueous polyurethane emulsion is 68%, and water-intake rate is 11%.
Embodiment 4:
Under rotating speed 900r/min, 81 ℃ condition, prepare base polyurethane prepolymer for use as take isophorone diisocyanate (IPDI), polyoxyethylene glycol (PEG3000), dimethylol propionic acid (DMPA) as raw material, reaction 3h, the mol ratio of IPDI and PEG1000, DMPA is 1.1:1, and DMPA accounts for 6% of performed polymer quality.Look viscosity in the process and change adding solvent N-first class pyrrolidone (NMP).Adding 3-[two-(2-hydroxyethyl)] amido-N (1,1-dimethyl-3 butanone) propionic acid amide (DHPA) is to the crosslinked chain extension of performed polymer.The consumption of DHPA is 8% of performed polymer quality.Be cooled to 40 ℃, add triethylamine and carry out neutralization reaction generation salt, reaction 3min.The amount of substance of triethylamine is identical with the amount of substance of DMPA.Rotating speed is increased to 1800r/min, adds emulsifying water 60min, the consumption of water is 2 times of performed polymer total mass.Obtain the single-component waterborne polyurethane emulsion capable of self-crosslinking at normal temperature.
The degree of crosslinking of aqueous polyurethane emulsion is 78%, and water-intake rate is 7%.
Claims (8)
1. the preparation method of a single-component ambient self-crosslinking aqueous polyurethane, it is characterized in that: step is as follows:
(1) prepares base polyurethane prepolymer for use as take isophorone diisocyanate (IPDI), polyoxyethylene glycol (PEG3000), dimethylol propionic acid (DMPA) as raw material, 81 ℃ of stirring reaction 3h look viscosity and change adding solvent N-first class pyrrolidone (NMP) in the process;
(2) adding 3-[two-(2-hydroxyethyl)] amido-N (1,1-dimethyl-3 butanone) propionic acid amide (DHPA) is to the crosslinked chain extension of performed polymer;
(3) be cooled to 40 ℃, add triethylamine and carry out neutralization reaction generation salt, reaction 3-4min;
(4) add entry strong stirring emulsification 60min, obtain the single-component waterborne polyurethane emulsion capable of self-crosslinking at normal temperature.
2. the preparation method of a kind of single-component ambient self-crosslinking aqueous polyurethane as claimed in claim 1, it is characterized in that: the proportioning of performed polymer raw material is in the described step (1): the mol ratio of IPDI and PEG1000, DMPA is 1.1:1, and DMPA accounts for 6% of performed polymer quality.
3. the preparation method of a kind of single-component ambient self-crosslinking aqueous polyurethane as claimed in claim 1 is characterized in that: the consumption of NMP is can make stirring be as the criterion smoothly in the described step (1).
4. the preparation method of a kind of single-component ambient self-crosslinking aqueous polyurethane as claimed in claim 1 is characterized in that: mixing speed is 900r/min in the described step (1).
5. the preparation method of a kind of single-component ambient self-crosslinking aqueous polyurethane as claimed in claim 1 is characterized in that: the consumption of DHPA is the 2%-8% of performed polymer quality in the described step (2).
6. the preparation method of a kind of single-component ambient self-crosslinking aqueous polyurethane as claimed in claim 1 is characterized in that: the amount of substance of triethylamine is identical with the amount of substance of DMPA in the described step (3).
7. the preparation method of a kind of single-component ambient self-crosslinking aqueous polyurethane as claimed in claim 1 is characterized in that: the consumption of water is 2 times of performed polymer total mass in the described step (4).
8. the preparation method of a kind of single-component ambient self-crosslinking aqueous polyurethane as claimed in claim 1 is characterized in that: the rotating speed that stirs in the described step (4) is 1800r/min.
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| CN2012105542958A CN103012733A (en) | 2012-12-19 | 2012-12-19 | Method for preparing mono-component normal-temperature self-crosslinking water-based polyurethane |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980792A (en) * | 2014-05-30 | 2014-08-13 | 陕西科技大学 | Room-temperature ketone-hydrazine-crosslinked VOC (Volatile Organic Compounds)-free water-based paint and preparation method thereof |
| CN104194610A (en) * | 2014-09-11 | 2014-12-10 | 北京东方雨虹防水技术股份有限公司 | Self-crosslinked one-component polyurethane waterproofing coating |
| CN104311775A (en) * | 2014-09-23 | 2015-01-28 | 李本明 | Polyaniline modified self-cross-linking waterborne polyurethane preparation method |
| CN104311772A (en) * | 2014-11-13 | 2015-01-28 | 苏州誉之铖贸易有限责任公司 | Environmentally friendly waterborne polyurethane emulsion |
| CN104312361A (en) * | 2014-09-24 | 2015-01-28 | 徐广苓 | Preparation method of self-crosslinked acrylate anticorrosive coating |
| CN104311774A (en) * | 2014-09-23 | 2015-01-28 | 李本明 | Preparation method of hollow micro-bead filled epoxy self-cross-linked modified polyurethane |
| CN104311785A (en) * | 2014-09-24 | 2015-01-28 | 徐广苓 | Preparation method of flame-retardant type self-crosslinked spraying polyurea elastic emulsion |
| CN104311784A (en) * | 2014-09-23 | 2015-01-28 | 李本明 | Polyaniline modified waterborne polyurethane preparation method |
| CN104312413A (en) * | 2014-09-24 | 2015-01-28 | 徐广苓 | Preparation method of titanium nano self-crosslinked organic anticorrosive coating |
| CN112621925A (en) * | 2020-12-17 | 2021-04-09 | 广西贵港市泰翔木业有限公司 | PP film faced decorative high-performance board and production process thereof |
| CN112659282A (en) * | 2020-12-17 | 2021-04-16 | 广西贵港市泰翔木业有限公司 | B1Novel PP film veneering process of formaldehyde-free flame-retardant board |
| CN112706237A (en) * | 2020-12-17 | 2021-04-27 | 广西贵港市泰翔木业有限公司 | Formaldehyde-free ecological plate coated high-tensile-strength PP film facing process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102492110A (en) * | 2011-12-07 | 2012-06-13 | 富思特新材料科技有限公司 | Preparation method for waterborne polyurethane applied to elastic coating |
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2012
- 2012-12-19 CN CN2012105542958A patent/CN103012733A/en active Pending
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| CN102492110A (en) * | 2011-12-07 | 2012-06-13 | 富思特新材料科技有限公司 | Preparation method for waterborne polyurethane applied to elastic coating |
Non-Patent Citations (1)
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| 王爱东: "单组分常温自交联水性聚氨酯的合成与性能研究", 《中国优秀博硕士学位论文全文数据库 (硕士) 工程科技Ⅰ辑》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980792A (en) * | 2014-05-30 | 2014-08-13 | 陕西科技大学 | Room-temperature ketone-hydrazine-crosslinked VOC (Volatile Organic Compounds)-free water-based paint and preparation method thereof |
| CN104194610A (en) * | 2014-09-11 | 2014-12-10 | 北京东方雨虹防水技术股份有限公司 | Self-crosslinked one-component polyurethane waterproofing coating |
| CN104311775A (en) * | 2014-09-23 | 2015-01-28 | 李本明 | Polyaniline modified self-cross-linking waterborne polyurethane preparation method |
| CN104311774A (en) * | 2014-09-23 | 2015-01-28 | 李本明 | Preparation method of hollow micro-bead filled epoxy self-cross-linked modified polyurethane |
| CN104311784A (en) * | 2014-09-23 | 2015-01-28 | 李本明 | Polyaniline modified waterborne polyurethane preparation method |
| CN104312361A (en) * | 2014-09-24 | 2015-01-28 | 徐广苓 | Preparation method of self-crosslinked acrylate anticorrosive coating |
| CN104311785A (en) * | 2014-09-24 | 2015-01-28 | 徐广苓 | Preparation method of flame-retardant type self-crosslinked spraying polyurea elastic emulsion |
| CN104312413A (en) * | 2014-09-24 | 2015-01-28 | 徐广苓 | Preparation method of titanium nano self-crosslinked organic anticorrosive coating |
| CN104311772A (en) * | 2014-11-13 | 2015-01-28 | 苏州誉之铖贸易有限责任公司 | Environmentally friendly waterborne polyurethane emulsion |
| CN112621925A (en) * | 2020-12-17 | 2021-04-09 | 广西贵港市泰翔木业有限公司 | PP film faced decorative high-performance board and production process thereof |
| CN112659282A (en) * | 2020-12-17 | 2021-04-16 | 广西贵港市泰翔木业有限公司 | B1Novel PP film veneering process of formaldehyde-free flame-retardant board |
| CN112706237A (en) * | 2020-12-17 | 2021-04-27 | 广西贵港市泰翔木业有限公司 | Formaldehyde-free ecological plate coated high-tensile-strength PP film facing process |
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Application publication date: 20130403 |