CN1869091A - Method for preparing water polyurethane by solventless method - Google Patents
Method for preparing water polyurethane by solventless method Download PDFInfo
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- CN1869091A CN1869091A CN 200610028156 CN200610028156A CN1869091A CN 1869091 A CN1869091 A CN 1869091A CN 200610028156 CN200610028156 CN 200610028156 CN 200610028156 A CN200610028156 A CN 200610028156A CN 1869091 A CN1869091 A CN 1869091A
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Abstract
A process for preparing water polyurethane by non-solvent method includes such steps as proportional reaction between polyisocyanate and polyol to obtain isocyanate terminated oligomer, cooling, adding water, strong stirring while adding the aqueous solution of triethylamine and ethyldiamine or divinyltriamine, and extending chain while dispersing.
Description
Technical field
The present invention relates to a kind of method of Synthesis of Waterborne Polyurethane method, particularly a kind of method for preparing water polyurethane by solventless.
Background technology
Urethane (PU) is the abbreviation of polyurethane(s) (Polyurethane), and it is a class purposes synthetic materials very widely.Select functional group's number of different numbers and dissimilar functional groups during along with preparation, adopt different synthesis techniques, can prepare the various polyurethane products of different, the apparent form of performance.Simultaneously it also to have property regulation scope such as soft durometer wide, low temperature resistant, snappiness is good, advantages such as strong adhesion.Conventional urethane is based on solvent-borne type, and organic solvent is inflammable and explosive, volatile, smell big, cause atmospheric pollution when using, and more or less has toxicity.Since the end of the sixties, along with the enhancing of each developed country's environmental consciousness and the establishment of environmental regulation, the discharging of the volatile organic compounds (VOC) in the conventional solvent type coating more and more is restricted.Therefore, be that the aqueous polyurethane of dispersion medium also just arises at the historic moment with water, and developed fast.Aqueous polyurethane (WPU) is to be the polyurethane dispersions system of medium with water, have nontoxic, do not fire, free from environmental pollution, energy-conservation, safe, easy damaged is not by advantages such as coating surface, easy to operate and modifications, be widely used as aspects such as hide finishes, textile auxiliary agent, paper industry auxiliary agent, coating and tackiness agent, but also constantly enlarging its Application Areas.Current preparation aqueous polyurethane mainly contains: acetone method, the direct dispersion method of performed polymer, fusion dispersion method, ketimine process and ketone bifurcation piperazine method (Ketimine and Ketamine) etc., above-mentioned these methods have more or less all been used organic solvent in building-up process, what have removed in the later stage, and what have still remains in the finished product.
Summary of the invention
The object of the present invention is to provide a kind of method of method for preparing water polyurethane by solventless.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method of method for preparing water polyurethane by solventless is characterized in that this method may further comprise the steps:
A) with 20～50% polyisocyanates, 5～8% dimethylol propionic acid and 42～75% polyvalent alcohol, mix by weight percentage,, obtain containing the prepolymer of terminal isocyanate group 60～110 ℃ of following stirring reactions 2～4 hours;
B) step a is obtained prepolymer and be cooled to 20～40 ℃, under vigorous stirring, the aqueous solution of triethylamine and polyamine chainextender will be dissolved with, press the aqueous solution: prepolymer=4～2: 1 weight ratio, the aqueous solution is joined in the described prepolymer, be warming up to 60～70 ℃ of reactions 1～2 hour then, chain extension disperses to obtain aqueous polyurethane; Wherein the consumption of polyamine chainextender is 1～3% of a prepolymer weight, the consumption prepolymer weight 3～5% of triethylamine.
Above-mentioned polyisocyanates is: isophorone diisocyanate IPDI or hexamethylene-diisocyanate HDI or tolylene diisocyanate TDI; Above-mentioned polyvalent alcohol is polyester polyol, polyether glycol, 1,4-butyleneglycol, 1,6-hexylene glycol, new for any one or two kinds of above mixtures in glycol, 1,3 butylene glycol, the ethylene glycol; Above-mentioned polyamine chainextender is: quadrol or diethylenetriamine.
Compared with prior art, the inventive method has following outstanding substantive distinguishing features and remarkable advantage: the inventive method is not fully not with an organic solvent, thereby demonstrated fully aqueous polyurethane nontoxic, do not fire, free from environmental pollution, energy-conservation, safe, easy damaged is not by advantages such as coating surfaces, and it is simple to operate, cost is low, excellent product performance, suitable for mass production.
Concrete embodiment:
Embodiment one: the pure and mild 3g dimethylol propionic acid of polyester binary that adds 30.4g in thermometer, reflux condensing tube, churned mechanically four-hole bottle are housed, be heated to 110 ℃, 30 minutes postcooling to 80 of vacuum hydro-extraction ℃ under this temperature add 16.6gIPDI 60 ℃ of reactions 4 hours down.Subsequently, be cooled to 20 ℃, add the deionized water 112ml that is dissolved with 2.24g triethylamine and 1.12g quadrol under the high-speed stirring, be warming up to 60 ℃ of reactions 1 hour then.Obtain solid content and be 30% polyurethane dispersions system.
Recording its breaking tenacity behind dried coating film is 22.54MPa, and elongation at break is 453.0%
Embodiment two: add 27.12g polyester diol, 6.78g polyether Glycols and 3g dimethylol propionic acid in thermometer, reflux condensing tube, churned mechanically four-hole bottle are housed, be heated to 110 ℃, 30 minutes postcooling to 80 of vacuum hydro-extraction ℃ under this temperature add 13.1gIPDI 110 ℃ of reactions 4 hours down.Subsequently, be cooled to 40 ℃, under high-speed stirring, add the deionized water 134ml that is dissolved with 2.26g triethylamine and 0.824g diethylenetriamine, be warming up to 60 ℃ of reactions 1 hour then.Obtain solid content and be 25% polyurethane dispersions system.
Recording its breaking tenacity behind dried coating film is 16.82MPa, and elongation at break is 574.9%.
Embodiment three: add 23.12g polyester diol, 6.78g polyether Glycols, 0.18g 1 in thermometer, reflux condensing tube, churned mechanically four-hole bottle are housed, 4 butyleneglycols and 3g dimethylol propionic acid, be heated to 110 ℃, 30 minutes postcooling to 80 of vacuum hydro-extraction ℃ under this temperature, add 16.5g IPDI, 110 ℃ were reacted 4 hours down.Subsequently, be cooled to 40 ℃, under high-speed stirring, add the deionized water 1361 that is dissolved with 2.26g triethylamine and 0.824g diethylenetriamine, be warming up to 60 ℃ of reactions 1 hour then.Obtain solid content and be 25% polyurethane dispersions system.Recording its breaking tenacity behind dried coating film is 19.25a, and elongation at break is 549.9%.
Claims (2)
1. the method for a method for preparing water polyurethane by solventless is characterized in that this method may further comprise the steps:
A, the polyisocyanates with 20～50%, 5～8% dimethylol propionic acid and 42～75% polyvalent alcohol mix by weight percentage, 60～110 ℃ of following stirring reactions 2～4 hours, obtain containing the prepolymer of terminal isocyanate group;
B, step a is obtained prepolymer be cooled to 20～40 ℃, under vigorous stirring, the aqueous solution of triethylamine and polyamine chainextender will be dissolved with, press the aqueous solution: prepolymer=4～2: 1 weight ratio, the aqueous solution is joined in the described prepolymer, be warming up to 60～70 ℃ of reactions 1～2 hour then, chain extension disperses to obtain aqueous polyurethane; Wherein the consumption of polyamine chainextender is 1～3% of a prepolymer weight, the consumption prepolymer weight 3～5% of triethylamine.
2. the method for method for preparing water polyurethane by solventless according to claim 1 is characterized in that, above-mentioned polyisocyanates is: isophorone diisocyanate IPDI or hexamethylene-diisocyanate HDI or tolylene diisocyanate TDI; Above-mentioned polyvalent alcohol is polyester polyol, polyether glycol, 1,4-butyleneglycol, 1,6-hexylene glycol, new for any one or two kinds of above mixtures in glycol, 1,3 butylene glycol, the ethylene glycol; Above-mentioned polyamine chainextender is: quadrol or diethylenetriamine.
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| CN 200610028156 CN1869091A (en) | 2006-06-27 | 2006-06-27 | Method for preparing water polyurethane by solventless method |
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| CN 200610028156 CN1869091A (en) | 2006-06-27 | 2006-06-27 | Method for preparing water polyurethane by solventless method |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173037B (en) * | 2007-09-13 | 2010-05-19 | 上海大学 | Method for producing aquosity mylar by chain extension method |
| CN101824272A (en) * | 2010-04-09 | 2010-09-08 | 王兆进 | Environmentally friendly waterbone polyurethane coating for wall paper and preparation method thereof |
| CN101544741B (en) * | 2009-04-30 | 2011-11-23 | 上海大学 | Method for preparing dianion type water-based light-cured polyurethane resin through chain extending method |
| CN102702471A (en) * | 2012-06-27 | 2012-10-03 | 惠州市汉诺新材料有限公司 | Method for preparing solvent-free aqueous polyurethane dispersion |
| CN102758359A (en) * | 2012-07-06 | 2012-10-31 | 河南永合塑胶有限公司 | Polyurethane synthetic leather cleaning production process based on direct coating method |
| CN102977764A (en) * | 2012-11-21 | 2013-03-20 | 青岛文创科技有限公司 | Weather-resistant leather finishing agent |
| CN103319682A (en) * | 2013-07-11 | 2013-09-25 | 清远市美乐仕油墨有限公司 | Low-luster aqueous polyurethane dispersion for leather, and preparation method and application thereof |
| CN103554416A (en) * | 2013-10-22 | 2014-02-05 | 安吉华诚纳米科技有限公司 | Synthesizing method and application of waterborne polyurethane |
| CN103937435A (en) * | 2014-03-31 | 2014-07-23 | 浙江耐和实业有限公司 | Method for preparing solvent-free waterborne polyurethane resin for synthesizing leather bonding layer |
| CN105566594A (en) * | 2016-01-29 | 2016-05-11 | 佛山市聚成生化技术研发有限公司 | Preparation method of cow leather coating agent containing polyurethane and prepared cow leather coating agent |
| CN107417873A (en) * | 2017-04-07 | 2017-12-01 | 中国科学院长春应用化学研究所 | A kind of aqueous polyurethane dispersion and its non-solvent preparation |
| CN107488404A (en) * | 2017-09-04 | 2017-12-19 | 上海丹韵投资管理有限公司 | A kind of automobile-used aqueous polyurethane coating and preparation method thereof |
| CN107522841A (en) * | 2017-08-24 | 2017-12-29 | 温州大学 | A kind of method that solventless method prepares carboxylic acid/sulfonic acid mixed type high-solid content water-based polyurethane |
| CN108623778A (en) * | 2017-03-15 | 2018-10-09 | 中国科学院福建物质结构研究所 | A kind of method that organic solvent-free prepares aqueous polyurethane dispersion |
| CN109021909A (en) * | 2018-06-25 | 2018-12-18 | 福建华夏蓝新材料科技有限公司 | A kind of low surface tension water-based polyurethane adhesive and preparation method thereof |
| CN109096467A (en) * | 2018-08-24 | 2018-12-28 | 黄山中泽新材料有限公司 | A kind of solvent-free composite high-strength high temperature resistance polyester type polyurethane resin |
| CN109485827A (en) * | 2018-10-26 | 2019-03-19 | 湖北大学 | A kind of preparation method of aqueous polyurethane |
-
2006
- 2006-06-27 CN CN 200610028156 patent/CN1869091A/en active Pending
Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173037B (en) * | 2007-09-13 | 2010-05-19 | 上海大学 | Method for producing aquosity mylar by chain extension method |
| CN101544741B (en) * | 2009-04-30 | 2011-11-23 | 上海大学 | Method for preparing dianion type water-based light-cured polyurethane resin through chain extending method |
| CN101824272A (en) * | 2010-04-09 | 2010-09-08 | 王兆进 | Environmentally friendly waterbone polyurethane coating for wall paper and preparation method thereof |
| CN102702471A (en) * | 2012-06-27 | 2012-10-03 | 惠州市汉诺新材料有限公司 | Method for preparing solvent-free aqueous polyurethane dispersion |
| CN102758359A (en) * | 2012-07-06 | 2012-10-31 | 河南永合塑胶有限公司 | Polyurethane synthetic leather cleaning production process based on direct coating method |
| CN102977764A (en) * | 2012-11-21 | 2013-03-20 | 青岛文创科技有限公司 | Weather-resistant leather finishing agent |
| CN103319682A (en) * | 2013-07-11 | 2013-09-25 | 清远市美乐仕油墨有限公司 | Low-luster aqueous polyurethane dispersion for leather, and preparation method and application thereof |
| CN103319682B (en) * | 2013-07-11 | 2015-08-26 | 清远市美乐仕油墨有限公司 | A kind of leather low gloss aqueous polyurethane dispersion and its preparation method and application |
| CN103554416A (en) * | 2013-10-22 | 2014-02-05 | 安吉华诚纳米科技有限公司 | Synthesizing method and application of waterborne polyurethane |
| CN103554416B (en) * | 2013-10-22 | 2016-02-03 | 安吉华诚纳米科技有限公司 | A kind of preparation method and use of aqueous polyurethane |
| CN103937435B (en) * | 2014-03-31 | 2015-11-11 | 浙江耐和实业有限公司 | For the synthesis of the preparation method of the solvent-free waterborne polyurethane resin of leather adhesive linkage |
| CN103937435A (en) * | 2014-03-31 | 2014-07-23 | 浙江耐和实业有限公司 | Method for preparing solvent-free waterborne polyurethane resin for synthesizing leather bonding layer |
| CN105566594A (en) * | 2016-01-29 | 2016-05-11 | 佛山市聚成生化技术研发有限公司 | Preparation method of cow leather coating agent containing polyurethane and prepared cow leather coating agent |
| CN108623778A (en) * | 2017-03-15 | 2018-10-09 | 中国科学院福建物质结构研究所 | A kind of method that organic solvent-free prepares aqueous polyurethane dispersion |
| CN107417873A (en) * | 2017-04-07 | 2017-12-01 | 中国科学院长春应用化学研究所 | A kind of aqueous polyurethane dispersion and its non-solvent preparation |
| CN107417873B (en) * | 2017-04-07 | 2020-07-31 | 中国科学院长春应用化学研究所 | Aqueous polyurethane dispersion and solvent-free preparation method thereof |
| CN107522841A (en) * | 2017-08-24 | 2017-12-29 | 温州大学 | A kind of method that solventless method prepares carboxylic acid/sulfonic acid mixed type high-solid content water-based polyurethane |
| CN107522841B (en) * | 2017-08-24 | 2020-04-07 | 温州大学 | Method for preparing carboxylic acid/sulfonic acid mixed high-solid-content aqueous polyurethane by solvent-free method |
| CN107488404A (en) * | 2017-09-04 | 2017-12-19 | 上海丹韵投资管理有限公司 | A kind of automobile-used aqueous polyurethane coating and preparation method thereof |
| CN109021909A (en) * | 2018-06-25 | 2018-12-18 | 福建华夏蓝新材料科技有限公司 | A kind of low surface tension water-based polyurethane adhesive and preparation method thereof |
| CN109096467A (en) * | 2018-08-24 | 2018-12-28 | 黄山中泽新材料有限公司 | A kind of solvent-free composite high-strength high temperature resistance polyester type polyurethane resin |
| CN109485827A (en) * | 2018-10-26 | 2019-03-19 | 湖北大学 | A kind of preparation method of aqueous polyurethane |
| CN109485827B (en) * | 2018-10-26 | 2021-02-19 | 湖北大学 | Preparation method of waterborne polyurethane |
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