CN101696259A - Method for preparing composite water-based polyurethane - Google Patents
Method for preparing composite water-based polyurethane Download PDFInfo
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- CN101696259A CN101696259A CN200910035885A CN200910035885A CN101696259A CN 101696259 A CN101696259 A CN 101696259A CN 200910035885 A CN200910035885 A CN 200910035885A CN 200910035885 A CN200910035885 A CN 200910035885A CN 101696259 A CN101696259 A CN 101696259A
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Abstract
The invention discloses a method for preparing composite water-based polyurethane. The method comprises the following steps of: adding polyether, epoxy resin, toluene diisocynate and rude MdI into a kettle, then adding a catalyst into the kettle, and preheating and prepolymerizing the mixture; measuring -NCO value, adding dimethylopropionic acid, after reacting the mixture, measuring -NCO value again; reducing the temperature, adding acetone, stirring the mixed solution, discharging the obtained product; placing the obtained product into a dispersion barrel, adding triethylamine into the dispersion barrel, stirring the mixture, adding water, and dispersing the mixed solution at a high speed; after dispersing the mixed solution uniformly, adding ethidene diamine, performing a chain extending reaction, and then stirring the obtained solution at a reduced speed; sealing and standing the obtained solution, then filtering the obtained solution and discharging the filter. The method overcomes the shortage of short-time use after the mixing of two components because the conventional oil polyurethane uses an irritant solvent, reduces waste and protects environment, has the advantages of non-toxicity and light smell by taking water as a solvent, and makes an adhesive achieve the adhesive strength by heating and activating the adhesive when clothes are bonded so as to achieve effect of good hand feeling after bonding and good water washing property.
Description
Technical field
The present invention relates to a kind of preparation method of binding agent, is a kind of Synthesis of Waterborne Polyurethane method specifically, is mainly used in fields such as clothes, timber.
Background technology
Urethane (English Polyurethane, being called for short PU) binding agent is meant and contains the amino methyl group (NHCOO-) or isocyanate group (suction stick N=C=O) in molecular chain, because of containing two kinds of strong polar groups, timber, leather, fabric, pottery, glass, metal, rubber etc. there is good bounding force.
Be applied to now apparel industry be mainly oiliness (two component) urethane and latex class tackiness agent is main.Oiliness urethane shortcoming is mainly: 1 contains solvent, and pungency is bigger, contains harmful materials such as formaldehyde, and the textiles that exports to American-European market for a part brings a lot of problems; 2 is now with the current, and the time solidifies and loses adhesive effect once long.Latex class main drawback: 1 ammonia flavor is heavier, and operative employee's influence is bigger; 2 water-soluble poor effect, and rubber is aging easily in the latex, loses intensity.
Aqueous polyurethane is the system of solvent as dispersion medium with water, have pollution-free, safe and reliable, intermiscibility is good, be easy to modification, mechanical property can good characteristic.Water base polyurethane because nontoxic, nonflammable, free from environmental pollution, energy-conservation, safe and reliable, with characteristics such as operation modification etc. it is used widely in fields such as fabric, leather, covering with paint, timber.But abroad some aqueous polyurethane product prices are very high, the very fierce industry of this competition of textiles and inapplicable at home, and most textile products are also using the oiliness polyurethane products.
Summary of the invention
Goal of the invention: the preparation method who the purpose of this invention is to provide the composite aqueous polyurethane that low, the anti-washing performance of a kind of price is good, bond strength is high.
Technical scheme: in order to solve the problems of the technologies described above, the present invention has adopted following technical scheme:
A kind of preparation method of composite aqueous polyurethane, it comprises following step:
(1) 80～120 parts of polyethers, 3～8 parts of Resins, epoxy, 30～40 parts of tolylene diisocyanates, 4～9 parts of thick MDI are added reactor, add 0.01～0.02 part of catalyzer, be heated to 70～85 ℃ of pre-polymerizations 1～3 hour;
(2) 20～40 minutes measurements-nco values in advance, reach 5.5-6 after, add 7～12 parts of dimethylol propionic acids, reacted 2～5 hours, and measurement-nco value arrives specialized range 4.5-5 once more; Be cooled to 45～60 ℃, add 50～70 parts acetone, stir and be cooled to 30～50 ℃, discharging;
(3) put into the dispersion bucket immediately, add 5～8 parts of triethylamines, stirred 3～8 minutes, add 300～400 parts in water, disperse with the rotating speed more than 1000 rev/mins;
(4) disperse to add 0.5～3 part of quadrol after 3～8 minutes, continue chain extending reaction, reduction of speed stirred 1～3 hour to 30-50 rev/min;
(5) airtight static, filter discharging.
Wherein, described polyethers is PPG210; Described Resins, epoxy is E51; Described tolylene diisocyanate is TDI-80; Described catalyzer is a dibutyl tin dilaurate.
Wherein, the airtight immobilized time is 24 hours in the step (5), and described 180 orders that are filtered into filter.
The present invention adopts polyether glycol, and tolylene diisocyanate (TDI) is as synthetic main body, and Resins, epoxy adopts dimethylol propionic acid (DMPA) to make ionization reagent, thereby makes this aqueous polyurethane that good water dispersible and self-emulsifying be arranged as linking agent.Employing-NCO base high viscosity performed polymer adds acetone and reduces viscosity, and the hydrophilic monomer chain extension adds entry under the high-speed stirring, makes waterborne polyurethane binders.Polyethers provides soft section, and TDI provides hard segment structure, adds MDI and obtains higher modulus and tear strength; It mainly is to make urethane crosslinks form reticulated structure that Resins, epoxy is introduced, to obtain the excellent water tolerance energy.
Polyether glycol-OH group and vulcabond-NCO radical reaction:
DMPA participates in the chain extending reaction of urethane, and the low activity carboxyl under preserving in reaction can be converted into ammonium salt or an alkali metal salt, therefore makes urethane have water-soluble and automatic emulsifying performance.
Beneficial effect: (1) the present invention has overcome existing oiliness urethane and has used the pungency solvent, and the drawback that two components can only use after mixing has at short notice reduced waste, again environmental protection.(2) the present invention adopts water as solvent, nontoxic, lighter odor, heat-activated when clothes are bonding makes tackiness agent reach bond strength, and bonding back feel is better, wash durability is good, dry after at room temperature laundry was machine-washed 2 hours after lining was compound again and wash, circulate so repeatedly more than 5 times, lining is not thrown off; And operate, use all very convenient.(3) far below external product, the sale price of the water-based PU that this proportioning is produced is at 15-20 unit/kg on cost for aqurous ployurethane of the present invention, and the external product price all is not less than 50 yuan/kg.
The performance of the existing polyurethane binder of the present invention and market compares:
Embodiment:
According to following embodiment, can better understand the present invention.Yet, those skilled in the art will readily understand that the described concrete material proportion of embodiment, processing condition and result thereof only are used to illustrate the present invention, and should also can not limit the present invention described in detail in claims.
Among the following embodiment: PPG210 can be buied by Nanjing, Nanjing Petro-Chemical Corporation, Resins, epoxy E51 can be buied by Wuxi City A Erzi chemical industry company limited, toluene two different hydrogen acid ether TDI-80 can be buied by Dahua Group Co., Ltd., Cangzhou City, Hebei Prov., can buy by Qingdao urethane novel material company limited, dibutyl tin dilaurate can be buied by the East China Normal University chemical plant, and acetone is buied by Yanshan Petrochemical; Triethylamine can be buied by Changzhou rising sun east chemical industry company limited; Quadrol can use the product of the brilliant chemical reagent of Yixing City factory.
Embodiment 1:
With 100 parts polyethers PPG210,5 parts Resins, epoxy E51,34.05 parts of toluene two different hydrogen acid ether TDI-80,6.08 the thick MDI (diphenylmethanediisocyanate) of part adds reactor, adds 0.015 part dibutyl tin dilaurate, be heated to 78 ℃, pre-polymerization two hours; Shift to an earlier date 30 minutes measurement-nco values ,-nco value is pressed Di-n-Butyl Amine chemical determination among the GB/T1722.After-nco value reaches 5.5～6, add 9 parts of dimethylol propionic acids, reacted 3.5 hours, and once more measurement-nco value at 4.5～5 o'clock; Be cooled to 50 ℃, add 60 parts acetone, stir and be cooled to 40 ℃, discharging; Put into immediately and disperse bucket, add 6.78 parts triethylamine, stirred 5 minutes, add 357 parts in water, high speed dispersion more than 1000 rev/mins; High speed dispersion 5 minutes, the back that is uniformly dispersed adds 1.5 parts quadrol, continues chain extending reaction, and reduction of speed to 50 rev/min stirred 2.5 hours; Airtight static 24 hours, 180 orders filtered, discharging.
Cooperate the different garment lining, add different ratios vinyl acetate ester-ethylene copolymerization emulsions (VAE), regulate just sticking and final tackiness agent and solidify back lining feel.
Embodiment 2:
With 80 parts polyethers PPG210,3.5 parts Resins, epoxy E51,30 parts of toluene two different hydrogen acid ether TDI-80,4.5 the thick MDI (diphenylmethanediisocyanate) of part adds reactor, adds 0.01 part dibutyl tin dilaurate, be heated to 72 ℃, pre-polymerization 1.5 hours; Shift to an earlier date 25 minutes measurement-nco values ,-nco value is pressed Di-n-Butyl Amine chemical determination among the GB/T1722.After reaching 5.5～6, add 7 parts of dimethylol propionic acids, reacted 2.5 hours, and when measurement-nco value is in 4.5～5 scope once more; Be cooled to 45 ℃, add 50 parts acetone, stir and be cooled to 30 ℃, discharging; Put into immediately and disperse bucket, add 5 parts triethylamine, stirred 4 minutes, add 320 parts in water, high speed dispersion more than 1000 rev/mins; High speed dispersion 4 minutes, the back that is uniformly dispersed adds 0.7 part quadrol, continues chain extending reaction, and reduction of speed to 30 rev/min stirred 2 hours; Airtight static 24 hours, 180 orders filtered, discharging.
Cooperate the different garment lining, add different ratios vinyl acetate ester-ethylene copolymerization emulsions (VAE), regulate just sticking and final tackiness agent and solidify back lining feel.
Embodiment 3:
With 120 parts polyethers PPG210,8 parts Resins, epoxy E51,40 parts toluene two different hydrogen acid ether TDI-80,9 parts thick MDI (diphenylmethanediisocyanate) adds reactor, adds 0.02 part dibutyl tin dilaurate, be heated to 82 ℃, pre-polymerization 3 hours; Shift to an earlier date 40 minutes measurement-nco values ,-nco value is pressed Di-n-Butyl Amine chemical determination among the GB/T1722.After reaching 5.5～6, add 12 parts of dimethylol propionic acids, reacted 5 hours, and once more measurement-nco value at 4.5～5 o'clock; Be cooled to 55 ℃, add 70 parts acetone, stir and be cooled to 50 ℃, discharging; Put into immediately and disperse bucket, add 8 parts triethylamine, stirred 8 minutes, add 400 parts in water, high speed dispersion more than 1000 rev/mins; High speed dispersion 7.5 minutes, the back that is uniformly dispersed adds 3 parts quadrol, continues chain extending reaction, and reduction of speed to 40 rev/min stirred 3 hours; Airtight static 24 hours, 180 orders filtered, discharging.
Cooperate the different garment lining, add different ratios vinyl acetate ester-ethylene copolymerization emulsions (VAE), regulate just sticking and final tackiness agent and solidify back lining feel.
Claims (7)
1. the preparation method of a composite aqueous polyurethane is characterized in that, it comprises following step:
(1) 80～120 parts of polyethers, 3～8 parts of Resins, epoxy, 30～40 parts of tolylene diisocyanates, 4～9 parts of thick MDI are added reactor, add 0.01～0.02 part of catalyzer, be heated to 70～85 ℃ of pre-polymerizations 1～3 hour;
(2) 20～40 minutes measurements-nco values in advance, reach 5.5～6 after, add 7～12 parts of dimethylol propionic acids, reacted 2～5 hours, and measurement-nco value arrives specialized range 4.5～5 once more; Be cooled to 45～60 ℃, add 50～70 parts acetone, stir and be cooled to 30～50 ℃, discharging;
(3) put into the dispersion bucket, add 5～8 parts of triethylamines, stirred 3～8 minutes, add 300～400 parts in water, disperse with the rotating speed more than 1000 rev/mins;
(4) disperse to add 0.5～3 part of quadrol after 3～8 minutes, continue chain extending reaction, reduction of speed stirred 1～3 hour to 30-50 rev/min;
(5) airtight static, filter discharging.
2. the preparation method of a kind of composite aqueous polyurethane according to claim 1, it is characterized in that: described polyethers is PPG210.
3. the preparation method of a kind of composite aqueous polyurethane according to claim 1, it is characterized in that: described Resins, epoxy is E51.
4. the preparation method of a kind of composite aqueous polyurethane according to claim 1, it is characterized in that: described tolylene diisocyanate is TDI-80.
5. the preparation method of a kind of composite aqueous polyurethane according to claim 1, it is characterized in that: described catalyzer is a dibutyl tin dilaurate.
6. the preparation method of a kind of composite aqueous polyurethane according to claim 1, it is characterized in that: the airtight immobilized time is 24 hours in the step (5).
7. the preparation method of a kind of composite aqueous polyurethane according to claim 1 is characterized in that: 180 orders that are filtered into described in the step (5) filter.
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| CN200910035885A CN101696259A (en) | 2009-10-09 | 2009-10-09 | Method for preparing composite water-based polyurethane |
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| CN200910035885A CN101696259A (en) | 2009-10-09 | 2009-10-09 | Method for preparing composite water-based polyurethane |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757533A (en) * | 2011-04-28 | 2012-10-31 | 比亚迪股份有限公司 | Aqueous polyurethane emulsion, preparation method thereof and two-component aqueous silver powder coating composition |
| CN105348981A (en) * | 2015-11-13 | 2016-02-24 | 安徽广源科技发展有限公司 | Environmental-friendly anti-cracking water-borne coating |
| CN105348984A (en) * | 2015-11-13 | 2016-02-24 | 安徽广源科技发展有限公司 | Impact-resistant eco-friendly aqueous paint |
| CN105348982A (en) * | 2015-11-13 | 2016-02-24 | 安徽广源科技发展有限公司 | High-toughness environmental-friendly water-borne coating |
| CN110452654A (en) * | 2019-08-27 | 2019-11-15 | 江苏龙蟠科技股份有限公司 | A kind of roof of the vehicle single-component water-based polyurethane adhesive and preparation method thereof |
| CN110894279A (en) * | 2019-11-29 | 2020-03-20 | 山东天庆科技发展有限公司 | Water-based epoxy polyurethane veneering adhesive and preparation method thereof |
| CN112239642A (en) * | 2020-11-04 | 2021-01-19 | 佰耐立新材料科技有限公司 | Formula and preparation method of waterborne polyurethane aldehyde-free reaction adhesive |
-
2009
- 2009-10-09 CN CN200910035885A patent/CN101696259A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757533A (en) * | 2011-04-28 | 2012-10-31 | 比亚迪股份有限公司 | Aqueous polyurethane emulsion, preparation method thereof and two-component aqueous silver powder coating composition |
| CN102757533B (en) * | 2011-04-28 | 2015-01-14 | 比亚迪股份有限公司 | Aqueous polyurethane emulsion, preparation method thereof and two-component aqueous silver powder coating composition |
| CN105348981A (en) * | 2015-11-13 | 2016-02-24 | 安徽广源科技发展有限公司 | Environmental-friendly anti-cracking water-borne coating |
| CN105348984A (en) * | 2015-11-13 | 2016-02-24 | 安徽广源科技发展有限公司 | Impact-resistant eco-friendly aqueous paint |
| CN105348982A (en) * | 2015-11-13 | 2016-02-24 | 安徽广源科技发展有限公司 | High-toughness environmental-friendly water-borne coating |
| CN110452654A (en) * | 2019-08-27 | 2019-11-15 | 江苏龙蟠科技股份有限公司 | A kind of roof of the vehicle single-component water-based polyurethane adhesive and preparation method thereof |
| CN110452654B (en) * | 2019-08-27 | 2021-10-12 | 江苏龙蟠科技股份有限公司 | Single-component water-based polyurethane adhesive for automobile roof and preparation method thereof |
| CN110894279A (en) * | 2019-11-29 | 2020-03-20 | 山东天庆科技发展有限公司 | Water-based epoxy polyurethane veneering adhesive and preparation method thereof |
| CN112239642A (en) * | 2020-11-04 | 2021-01-19 | 佰耐立新材料科技有限公司 | Formula and preparation method of waterborne polyurethane aldehyde-free reaction adhesive |
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Open date: 20100421 |