CN101054434A - Technology for processing ultraviolet radiation fast solidification water polyamine resin - Google Patents

Technology for processing ultraviolet radiation fast solidification water polyamine resin Download PDF

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Publication number
CN101054434A
CN101054434A CN 200610039546 CN200610039546A CN101054434A CN 101054434 A CN101054434 A CN 101054434A CN 200610039546 CN200610039546 CN 200610039546 CN 200610039546 A CN200610039546 A CN 200610039546A CN 101054434 A CN101054434 A CN 101054434A
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Prior art keywords
acetone
reactor
high speed
performed polymer
mentioned
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CN 200610039546
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CN101054434B (en
Inventor
于子洲
徐红良
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Yangzhou Chenhua New Materials Co., Ltd.
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于子洲
徐红良
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Abstract

A processing craft for speediness solidifying water polyurethanes resin by ultraviolet light is including following steps: preparing prepolymer; neutralizing emulsification above prepolymer, putting the prepolymer in the blossom barrel, placing under the high speed dissolver, adding 2-5% triethylamine under a low speed with a rotating speed of 850 rpm/min, blending for 1-4 min, rising to 1200 rpm/min, adding the deionized water 1.2-2.4 times to material weight, dissolving under the high speed, drawing the material into the acetone-removing vessel after the prepolymer dissolving completely; removing the acetone, sealing said acetone-removing vessel, setting the pressure in vessel of 500Pa, heating slowly, controlling the temperature under 65 DEG C for 5-6 hours, adding light initiator into the material in a weight ratio of 1:0.01 to 0.1, mixing uniformly. The obtained resin membrane has a high rigidity and a good resistance to abrasion irradiated by ultraviolet light, after the produced speediness solidifying water polyurethanes resin by ultraviolet light forms membrance.

Description

Technology for processing ultraviolet radiation fast solidification water polyamine resin
Technical field
The present invention relates to the complete processing of polyurethane, relate in particular to a kind of complete processing of ultraviolet radiation fast solidification water polyurethane resin.
Background technology
UV curable aqueous polyurethane resin has good comprehensive performances because of it and the outstanding feature of environmental protection is widely used in paint field.Chinese patent application number " 94111058.3 ", name is called the patented technology of " a kind of ultraviolet light fast solidification paint ", disclose a kind of ultraviolet light fast solidification paint, it is made up of with an amount of ratio ternary light-cured resin, five yuan of photosensitive diluents and photosensitive properties-correcting agent, solidifying agent and flow agent.This coating has fast setting, high gloss, and high adhesive force, high tenacity, resistance toheat is superior, shelf-stable, aging-resistant advantage.But its hardness is lower, and is not wear-resisting.
Summary of the invention
The present invention is directed to above defective a kind of energy fast setting is provided, and solidify rear surface hardness height, the ultraviolet radiation fast solidification water polyurethane resin that wear resistance is good.
Technical scheme of the present invention is: it may further comprise the steps:
1), preparation performed polymer;
A), polycaprolactone and TriMethylolPropane(TMP) are inserted in the container, melt with steam, stand-by;
B), under the normal temperature, the above-mentioned polycaprolactone that melts 18~40% is dropped in the reactors, add 3~7.5% pairs of hydroxymethyl propionic acids simultaneously, reactor is heated to 65 ℃, drops into 25~45% isoflurane chalcone diisocyanate again, slowly heat up, be heated to 100 ℃, be incubated 2 ~ 3 hours;
C), then, be cooled to 55 ℃, add 2 ~ 3% TriMethylolPropane(TMP)s, at this moment,, then,, be warming up to 70 ℃, be incubated 0.5 ~ 1.5 hour the material in reactor heating with the water in the steam discharge reacting kettle jacketing;
D), 17.45 ~ 35% acetone is inserted one and drip basin, drip basin UNICOM reactor, lower the temperature during dropping, when reducing to 60 ~ 65 ℃, add 0.01 ~ 0.05% tin laurate and 1 ~ 2% Hydroxyethyl acrylate in the reactor, temperature of reaction kettle is heated to 62 ~ 68 ℃ again, and is incubated 1 ~ 2 hour;
E), then, evenly stir for the acetone that drips joins in the reactor, be cooled to 30 ~ 45 ℃ again above-mentioned;
2), above-mentioned performed polymer carried out in and emulsification, with the performed polymer plum blossom bucket of packing into, place under the high speed dispersor, open low speed earlier, rotating speed is 850 rev/mins, adds 2~5% triethylamines, stirs 1~4 minute, open again at a high speed, rotating speed is 1200 rev/mins, is incorporated as the deionized water of 1.6~2.4 times of weight of material, carries out high speed dispersion, after performed polymer scatter fully, the acetone still is taken off in the material suction;
3), take off acetone, take off the sealing of acetone still with above-mentioned, it is 500Pa that the still internal pressure is set, and slowly heats, temperature is controlled at below 65 ℃, the time is 5~6 hours,
4), the weight ratio by 1: 0.01~0.1 adds light trigger in the material again, stirs, make.
Technology of the present invention is introduced two keys in polyurethane molecular many, the content height of hard section in the molecule, thus make the curing cross-linked density of resin film layer bigger, improved the hardness and the wear resisting property of resin film layer after the UV-irradiation; The ultraviolet radiation fast solidification water polyurethane resin that technology of the present invention makes after forming rete, the hardness height of the resin film layer of gained after UV-irradiation, wear resistance is good.
Embodiment
Embodiment 1
1), preparation performed polymer;
A), polycaprolactone and TriMethylolPropane(TMP) are inserted in the container, melt with steam, stand-by;
B), under the normal temperature, the above-mentioned polycaprolactone that melts 18% is dropped in the reactor, add 3% pair of hydroxymethyl propionic acid simultaneously, reactor is heated to 65 ℃, drop into 45% isoflurane chalcone diisocyanate again, slowly heat up, be heated to 100 ℃, be incubated 3 hours;
C), then, be cooled to 55 ℃, add 2% TriMethylolPropane(TMP), at this moment,, then,, be warming up to 70 ℃, be incubated 1.5 hours the material in reactor heating with the water in the steam discharge reacting kettle jacketing;
D), 26.99% acetone inserted one drip basin, drip basin UNICOM reactor, lower the temperature during dropping, when reducing to 60 ℃, add 0.01% tin laurate and 1% Hydroxyethyl acrylate in the reactor, temperature of reaction kettle is heated to 62 ℃ again, and is incubated 2 hours;
E), then, evenly stir for the acetone that drips joins in the reactor, be cooled to 30 ℃ again above-mentioned;
2), above-mentioned performed polymer carried out in and emulsification, with the performed polymer plum blossom bucket of packing into, place under the high speed dispersor, open low speed earlier, rotating speed is 850 rev/mins, adds 2% triethylamine, stirs 1~4 minute, open again at a high speed, rotating speed is 1200 rev/mins, is incorporated as the deionized water of 1.6 times of weight of material, carries out high speed dispersion, after performed polymer scatter fully, the acetone still is taken off in the material suction;
3), take off acetone, take off the sealing of acetone still with above-mentioned, it is 500Pa that the still internal pressure is set, and slowly heats, temperature is controlled at below 65 ℃, the time is 6 hours,
4), the weight ratio by 1: 0.01 adds light trigger in the material again, stirs, make.
Embodiment 2
1), preparation performed polymer;
A), polycaprolactone and TriMethylolPropane(TMP) are inserted in the container, melt with steam, stand-by;
B), under the normal temperature, the above-mentioned polycaprolactone that melts 29% is dropped in the reactor, add 5% pair of hydroxymethyl propionic acid simultaneously, reactor is heated to 65 ℃, drop into 30% isoflurane chalcone diisocyanate again, slowly heat up, be heated to 100 ℃, be incubated 2.5 hours;
C), then, be cooled to 55 ℃, add 2.5% TriMethylolPropane(TMP), at this moment,, then,, be warming up to 70 ℃, be incubated 1 hour the material in reactor heating with the water in the steam discharge reacting kettle jacketing;
D), 28.47% acetone inserted one drip basin, drip basin UNICOM reactor, lower the temperature during dropping, when reducing to 63 ℃, add 0.03% tin laurate and 1.5% Hydroxyethyl acrylate in the reactor, temperature of reaction kettle is heated to 65 ℃ again, and is incubated 1.5 hours;
E), then, evenly stir for the acetone that drips joins in the reactor, be cooled to 38 ℃ again above-mentioned;
2), above-mentioned performed polymer carried out in and emulsification, with the performed polymer plum blossom bucket of packing into, place under the high speed dispersor, open low speed earlier, rotating speed is 850 rev/mins, adds 3.5% triethylamine, stirs 1~4 minute, open again at a high speed, rotating speed is 1200 rev/mins, is incorporated as the deionized water of 2 times of weight of material, carries out high speed dispersion, after performed polymer scatter fully, the acetone still is taken off in the material suction;
3), take off acetone, take off the sealing of acetone still with above-mentioned, it is 500Pa that the still internal pressure is set, and slowly heats, temperature is controlled at below 65 ℃, the time is 5.5 hours,
4), the weight ratio by 1: 0.05 adds light trigger in the material again, stirs, make.
Embodiment 3
1), preparation performed polymer;
A), polycaprolactone and TriMethylolPropane(TMP) are inserted in the container, melt with steam, stand-by;
B), under the normal temperature, the above-mentioned polycaprolactone that melts 40% is dropped in the reactor, add 7.5% pair of hydroxymethyl propionic acid simultaneously, reactor is heated to 65 ℃, drop into 25% isoflurane chalcone diisocyanate again, slowly heat up, be heated to 100 ℃, be incubated 2 hours;
C), then, be cooled to 55 ℃, add 3% TriMethylolPropane(TMP), at this moment,, then,, be warming up to 70 ℃, be incubated 1.5 hours the material in reactor heating with the water in the steam discharge reacting kettle jacketing;
D), 17.45% acetone inserted one drip basin, drip basin UNICOM reactor, lower the temperature during dropping, when reducing to 65 ℃, add 0.05% tin laurate and 2% Hydroxyethyl acrylate in the reactor, temperature of reaction kettle is heated to 68 ℃ again, and is incubated 1 hour;
E), then, evenly stir for the acetone that drips joins in the reactor, be cooled to 45 ℃ again above-mentioned;
2), above-mentioned performed polymer carried out in and emulsification, with the performed polymer plum blossom bucket of packing into, place under the high speed dispersor, open low speed earlier, rotating speed is 850 rev/mins, adds 5% triethylamine, stirs 1~4 minute, open again at a high speed, rotating speed is 1200 rev/mins, is incorporated as the deionized water of 2.4 times of weight of material, carries out high speed dispersion, after performed polymer scatter fully, the acetone still is taken off in the material suction;
3), take off acetone, take off the sealing of acetone still with above-mentioned, it is 500Pa that the still internal pressure is set, and slowly heats, temperature is controlled at below 65 ℃, the time is 5 hours,
4), the weight ratio by 1: 0.1 adds light trigger in the material again, stirs, make.

Claims (1)

1, technology for processing ultraviolet radiation fast solidification water polyamine resin is characterized in that, it may further comprise the steps:
1), preparation performed polymer;
A), polycaprolactone and TriMethylolPropane(TMP) are inserted in the container, melt with steam, stand-by;
B), under the normal temperature, the above-mentioned polycaprolactone that melts 18~40% is dropped in the reactors, add 3~7.5% pairs of hydroxymethyl propionic acids simultaneously, reactor is heated to 65 ℃, drops into 25~45% isoflurane chalcone diisocyanate again, slowly heat up, be heated to 100 ℃, be incubated 2 ~ 3 hours;
C), then, be cooled to 55 ℃, add 2 ~ 3% TriMethylolPropane(TMP)s, at this moment,, then,, be warming up to 70 ℃, be incubated 0.5 ~ 1.5 hour the material in reactor heating with the water in the steam discharge reacting kettle jacketing;
D), 17.45 ~ 35% acetone is inserted one and drip basin, drip basin UNICOM reactor, lower the temperature during dropping, when reducing to 60 ~ 65 ℃, add 0.01 ~ 0.05% tin laurate and 1 ~ 2% Hydroxyethyl acrylate in the reactor, temperature of reaction kettle is heated to 62 ~ 68 ℃ again, and is incubated 1 ~ 2 hour;
E), then, evenly stir for the acetone that drips joins in the reactor, be cooled to 30 ~ 45 ℃ again above-mentioned;
2), above-mentioned performed polymer carried out in and emulsification, with the performed polymer plum blossom bucket of packing into, place under the high speed dispersor, open low speed earlier, rotating speed is 850 rev/mins, adds 2~5% triethylamines, stirs 1~4 minute, open again at a high speed, rotating speed is 1200 rev/mins, is incorporated as the deionized water of 1.6~2.4 times of weight of material, carries out high speed dispersion, after performed polymer scatter fully, the acetone still is taken off in the material suction;
3), take off acetone, take off the sealing of acetone still with above-mentioned, it is 500Pa that the still internal pressure is set, and slowly heats, temperature is controlled at below 65 ℃, the time is 5~6 hours,
4), the weight ratio by 1: 0.01~0.1 adds light trigger in the material again, stirs, make.
CN2006100395463A 2006-04-13 2006-04-13 Technology for processing ultraviolet radiation fast solidification water polyamine resin Withdrawn - After Issue CN101054434B (en)

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Application Number Priority Date Filing Date Title
CN2006100395463A CN101054434B (en) 2006-04-13 2006-04-13 Technology for processing ultraviolet radiation fast solidification water polyamine resin

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CN101054434B CN101054434B (en) 2012-06-13

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102977758A (en) * 2012-12-24 2013-03-20 上海应用技术学院 UV (ultraviolet) photocured water-based fluorine-containing polyurethane latex film and preparation method thereof
CN104193946A (en) * 2014-09-15 2014-12-10 山东天庆科技发展有限公司 Self-extinction polyurethane resin and preparation method thereof

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1256900A (en) * 1968-12-19 1971-12-15
US4532316A (en) * 1984-05-29 1985-07-30 W. L. Gore & Assoc., Inc. Phase separating polyurethane prepolymers and elastomers prepared by reacting a polyol having a molecular weight of 600-3500 and isocyanate and a low molecular weight chain extender in which the ratios of reactants have a limited range
US6127505A (en) * 1995-02-02 2000-10-03 Simula Inc. Impact resistant polyurethane and method of manufacture thereof
US6221999B1 (en) * 1999-09-10 2001-04-24 Uniroyal Chemical Company, Inc. High resilience, high clarity polyurethane elastomer
CN1272356C (en) * 2004-07-13 2006-08-30 清华大学 Process for preparing medical polyurethane and modeling product under single mold microwave radiation

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102977758A (en) * 2012-12-24 2013-03-20 上海应用技术学院 UV (ultraviolet) photocured water-based fluorine-containing polyurethane latex film and preparation method thereof
CN102977758B (en) * 2012-12-24 2015-02-11 上海应用技术学院 UV (ultraviolet) photocured water-based fluorine-containing polyurethane latex film and preparation method thereof
CN104193946A (en) * 2014-09-15 2014-12-10 山东天庆科技发展有限公司 Self-extinction polyurethane resin and preparation method thereof

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Address after: 225800, No. 231 Middle Road, Cao Town, Baoying County, Yangzhou, Jiangsu

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Address before: 225800, Yangzhou County, Baoying province Jiangsu Town Road No. 231, Chen Chen new materials Limited by Share Ltd

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Patentee before: Xu Hongliang

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