CN105732938A - Preparation method of polyester-polyether-type aqueous polyurethane leather finishing agent - Google Patents
Preparation method of polyester-polyether-type aqueous polyurethane leather finishing agent Download PDFInfo
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- CN105732938A CN105732938A CN201510571340.4A CN201510571340A CN105732938A CN 105732938 A CN105732938 A CN 105732938A CN 201510571340 A CN201510571340 A CN 201510571340A CN 105732938 A CN105732938 A CN 105732938A
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- polyester
- leather
- aqueous polyurethane
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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
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
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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
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/90—Applications
- C08G2261/93—Applications in textiles, fabrics and yarns
Abstract
A preparation method of a polyester-polyether-type aqueous polyurethane leather finishing agent. The leather finishing agent is prepared from following components, by weight, 8-55% of polyester polyol, 10-66% of polyether polyol, (the polyester polyol and the polyether polyol both account for 65-80%), 15-30% of diisocyanates, 0.2-0.6% of a crosslinker, 2.5-6.0% of a hydrophilic chain extender, 0.5-1.0% of a binary amine chain extender, and 0.02-0.06% of an organic tin catalyst. The hydrophilic chain extender is dimethylolpropionic acid or sodium 1,2-dihydroxy-3-propylsulfonate. The preparation method includes the following steps: 1) dehydrating the polyester polyol and the polyether polyol; 2) adding the diisocyanates, the hydrophilic chain extender, the crosslinker and the organic tin catalyst to perform a pre-polymerization reaction until the concentration of -NCO reaches theoretical value; and 3) dissolving the prepolymer in acetone, adding deionized water, adding the binary amine chain extender to perform further chain extending reaction, and vacuumizing the reaction system to remove the acetone to prepare the leather finishing agent. The leather finishing agent has high tensile strength, high breaking elongation rate and low water absorption rate.
Description
(1) technical field
The present invention relates to a kind of aqueous polyurethane leather and be coated with the preparation method of reagent, be specifically related to the preparation method of a kind of polyether polyester type Aqueous Polyurethane Leather Finishing Agent.
(2) background technology
Leather finishing agent is the general designation covering with paint, lacquer, colour wash, etc. the class leather agent protecting and beautifying leather for leather surface, and it is the most formulated by film former, coloured material, solvent and auxiliary agent, and wherein film forming matter is the basis of leather finishing agent.Leather finishing agent has very important effect in leather manufacture, can increase leather attractive in appearance, extends leather and uses the time, significantly improve quality and the class of leatherware, increases commercial value.Along with change of consumer perceptive and the proposition of environmental issue, finishing agent is had higher requirement by people, and therefore, the research to leather finishing agent is the most in recent years.
Casein is that the leather that people use the earliest is coated with reagent, and it is a kind of material extracted from milk.Owing to using casein to cover with paint, lacquer, colour wash, etc., its film forming is hard, inextensibility, be easily broken off, inspiratory strong, be weak to wet rubbing, and extract from milk and do not meet demand for development.Nitrocellulose solution started formally be applied to leather finishing agent and be commercialized in nineteen twenty, and nitrocellulose can increase the water resistance of coating, as surface layer brightener.But, nitrocellulose class finishing agent is the most ageing-resistant, use during plasticizer is readily volatilized makes the hardening embrittlement of coating, under ultraviolet light irradiates, coating can be turned to be yellow, thus, nitrocellulose class finishing agent is not the most widely used in leather is modified.
1933, first emulsion acrylic resin was used for leather finish in Germany, has quickly obtained application.Acrylic resin is covered with paint, lacquer, colour wash, etc. and natural resin and other resin-phase ratio, has the performance of uniqueness, and it is combined with collagen by force, film strength height, high resilience, good weatherability, ageing-resistant performance are excellent, with low cost, the physical property that imparting leather is good.But acrylic acid is thermoplastic resin, there is the shortcomings such as " hot sticky, cold short ", not solvent resistant in its film, limits its use.Polyurethane is also known as polyurethanes, it is by the macromolecular compound of polyisocyanates with multi-hydroxy compound effects, it is characterized on macromolecular chain containing a lot carbamate groups repeated, therefore, there is the performance such as good intensity, wear-resisting, solvent resistant, and can be by changing the structure of compound, the size of molecular weight, the performance making polyurethane is the most adjusted.Polyurethane is used in leather finishing agent, and its filming performance is good, is firmly bonded, and coating has high glaze, high-wearing feature, high resiliency, water-fast, weather-proof, cold-resistant, chemical-resistant resistance, the resultant Leather good hand feeling of covering with paint, comfortable, can be greatly improved the class of resultant Leather.
Aqueous Polyurethane Leather Finishing Agent is the binary colloidal system with water as disperse medium, compared with solvent borne polyurethane, has the advantages such as nontoxic, nonflammable, free from environmental pollution.In recent years, along with improving and the enhancing of people's environmental consciousness of environmental legislation, the development of aqueous polyurethane is promoted.Aqueous polyurethane can be divided into polyester-type aqueous polyurethane and polyether type aqueous polyurethane according to raw material, utilizes that the Aqueous Polyurethane Leather Finishing Agent appearance of film that PEPA is Material synthesis is good, have preferable mechanical property, and its water resistance is poor；Using polyether polyol is that Material synthesis Aqueous Polyurethane Leather Finishing Agent film pliability and resistance to water are preferable, but its mechanical property is poor.Therefore, use polyester diol and polyether Glycols to be mixed into raw material and prepare Aqueous Polyurethane Leather Finishing Agent, the mutual supplement with each other's advantages of the two can be made, improve the performance of Aqueous Polyurethane Leather Finishing Agent.
Chinese patent literature CN 102050936B discloses the synthesis technique of a kind of single-component water-based polyurethane decorative paint for leather, Aqueous Polyurethane Leather Finishing Agent is synthesized for primary raw material with polyether-tribasic alcohol, polyester diol, toluene di-isocyanate(TDI), but not mentioned mechanical performance and resistance to water.
Chinese patent literature CN 102924683A discloses a kind of color inhibition leather finishing agent aqueous pu dispersions and preparation method thereof, and the method lays particular emphasis on yellowing resistance energy, and its mechanical performance is relatively low, and its high tensile only has 20Mpa.
Chinese patent literature CN 102924683A discloses a kind of anion water-soluble polyurethane disperse system for finishing leather and preparation method thereof.Although the aqueous polyurethane mechanical performance of the method synthesis makes moderate progress, but hot strength and elongation at break can not reach optimum simultaneously, and not mentioned water resistance,
In sum, lack a kind of hot strength at present high, Aqueous Polyurethane Leather Finishing Agent that elongation at break is high and water absorption rate is low and preparation method thereof.
(3) summary of the invention
It is an object of the invention to provide a kind of hot strength high, the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester that elongation at break is high and water absorption rate is low.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester, the polyether type aqueous polyurethane decorative paint for leather of described polyester is made up of the component of following percetage by weight:
Described preparation method comprises the steps:
(1) after PEPA and polyether polyol being carried out processed, control temperature and add diisocyanate, hydrophilic chain extender, cross-linking agent and organotin catalysts at 60～90 DEG C, described hydrophilic chain extender is dihydromethyl propionic acid (DMPA) or 1,2-dihydroxy-3-N-morpholinopropanesulfonic acid sodium (DHPA), control temperature and carry out prepolymerization reaction at 60～90 DEG C, until-NCO concentration reaches theoretical value, obtain prepolymer；
(2) by after prepolymer acetone solution, adding deionized water emulsifying in performed polymer, add diamine chain extenders and carry out further chain extending reaction 20～30min, then evacuation is sloughed acetone and is obtained the polyether type aqueous polyurethane decorative paint for leather of polyester.
Further, described diisocyanate is one or more the mixture in isoflurane chalcone diisocyanate (IPDI), hexamethylene diisocyanate (HDI), toluene di-isocyanate(TDI) (TDI), methyl diphenylene diisocyanate (MDI).
Further, described PEPA is any one or two or more mixture in polyadipate-BDO, polyadipate ethylene glycol, polyadipate diglycol, polyadipate neopentyl glycol.
Further, described polyether polyol is any one or two or more mixture in polypropylene glycol (PPG), PTMG (PTMEG), polyether polyol with high activity (DP).
Further, described cross-linking agent is trimethylolpropane (TMP).
Further, one or more the mixture during described diamine chain extenders is ethylenediamine, propane diamine, isophorone diamine.
Further, described organotin catalysts is dibutyl tin dilaurate or stannous octoate.
Further, the polyether type aqueous polyurethane decorative paint for leather of described polyester is preferably made up of the component of following percetage by weight:
Further, polyether polyol is 1:3～7:1 with the weight ratio of PEPA.
Further, in step (1), the feed temperature of diisocyanate, hydrophilic chain extender, cross-linking agent and organotin catalysts and prepolymerization reaction temperature control respectively at 60～70 DEG C.
Compared with prior art, the beneficial effects of the present invention is and the invention provides that to meet hot strength high, elongation at break is high and the Aqueous Polyurethane Leather Finishing Agent of water absorption rate these triple requirements low.
(4) detailed description of the invention:
Embodiment 1: put into DP-2000 200g and polyadipate neopentyl glycol 200g in four-hole boiling flask, 120 DEG C of evacuation dehydration 2h, after being cooled to 70 DEG C, add IPDI 145g, 1,2-dihydroxy-3-N-morpholinopropanesulfonic acid sodium 20g, trimethylolpropane 2g, dibutyl tin dilaurate 4, adds 150g acetone solution after 60～70 DEG C of reaction to-NCO concentration reach theoretical value.Being poured into by performed polymer in Scattered Kettle, be cooled to 35 DEG C, high-speed stirred (3000r/min) adds deionized water 500g, adds ethylenediamine 4g, high-speed stirred 20～30min.Aqueous polyurethane emulsion is obtained after 50～60 DEG C of low pressure evacuation take off acetone.
Its test result is as follows:
Hot strength: 42.5MPa.
Elongation at break: 510%.
Water absorption rate: 12.5%
Prepared Aqueous Polyurethane Leather Finishing Agent tension failure method for testing strength measures according to GB/T15232-1994 ,-NCO concentration monitor the method in described step be by di-n-butylamine method monitoring system-change of NCO content.Water absorption rate assay method: sample film is dried under vacuum under 24h, room temperature and takes a certain amount of glued membrane (m1) be immersed in 20 DEG C of distilled water and take out after 2h, surface moisture is quickly wiped with filter paper, weigh (m immediately2).Water absorption rate P computing formula:
Embodiment 2-5
Operational approach is with embodiment 1, and concrete formula and result do not exist together and be shown in Table 1:
Table 1
Claims (10)
1. a preparation method for the polyether type aqueous polyurethane decorative paint for leather of polyester, the polyether type aqueous polyurethane leather of described polyester
Finishing agent is made up of the component of following percetage by weight:
Described preparation method comprises the steps:
(1) after PEPA and polyether polyol being carried out processed, control temperature 60～90 DEG C add diisocyanate,
Hydrophilic chain extender, cross-linking agent and organotin catalysts, described hydrophilic chain extender is dihydromethyl propionic acid or 1,2-dihydroxy-3-third
Sodium sulfonate, controls temperature and carries out prepolymerization reaction at 60～90 DEG C, until-NCO concentration reaches theoretical value, obtain prepolymer；
(2) by after prepolymer acetone solution, in performed polymer, add deionized water emulsifying, add diamine chain extenders and carry out
Further chain extending reaction 20～30min, then evacuation is sloughed acetone and is obtained the polyether type aqueous polyurethane decorative paint for leather of polyester.
2. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as claimed in claim 1, it is characterised in that: institute
State the polyether type aqueous polyurethane decorative paint for leather of polyester to be made up of the component of following percetage by weight:
3. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as claimed in claim 2, it is characterised in that: poly-
Ethoxylated polyhydric alcohol is 1:3～7:1 with the weight ratio of PEPA.
4. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as described in one of claims 1 to 3, its feature exists
In: described diisocyanate be isoflurane chalcone diisocyanate, hexamethylene diisocyanate, toluene di-isocyanate(TDI), two
One or more mixture in methylenebis phenyl isocyanate.
5. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as described in one of claims 1 to 3, its feature exists
In: described PEPA be polyadipate-1,4-butanediol, polyadipate ethylene glycol, polyadipate diglycol,
Any one or two or more mixture in polyadipate neopentyl glycol.
6. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as described in one of claims 1 to 3, its feature exists
In: described polyether polyol be in polypropylene glycol, PTMG, polyether polyol with high activity any one or two
Plant above mixture.
7. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as described in one of claims 1 to 3, its feature exists
In: described cross-linking agent is trimethylolpropane.
8. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as described in one of claims 1 to 3, its feature exists
In: described diamine chain extenders is one or more the mixture in ethylenediamine, propane diamine, isophorone diamine.
9. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as described in one of claims 1 to 3, its feature exists
In: described organotin catalysts is dibutyl tin dilaurate or stannous octoate.
10. the preparation method of the polyether type aqueous polyurethane decorative paint for leather of polyester as described in one of claims 1 to 3, its feature
Being: in step (1), feed temperature and the pre-polymerization of diisocyanate, hydrophilic chain extender, cross-linking agent and organotin catalysts are anti-
Temperature is answered to control respectively at 60～70 DEG C.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106047126A (en) * | 2016-08-10 | 2016-10-26 | 福建宝利特科技股份有限公司 | Leather surface treating agent and processing method thereof |
| CN106244744A (en) * | 2016-08-22 | 2016-12-21 | 福建隆上超纤有限公司 | A kind of modified finishing agent for leather and preparation method thereof |
| CN106380575A (en) * | 2016-09-21 | 2017-02-08 | 无锡市莱瑟新材料科技有限公司 | Resin special for air mechanical foaming type polyurethane base and preparation method thereof |
| CN107011494A (en) * | 2017-05-23 | 2017-08-04 | 深圳市润天智数字设备股份有限公司 | A kind of preparation method of aqueous polyurethane dispersion |
| CN107033764A (en) * | 2017-04-26 | 2017-08-11 | 福建宝利特科技股份有限公司 | A kind of leather finishing degree inorganic agent |
| CN109553752A (en) * | 2018-12-06 | 2019-04-02 | 南通高盟新材料有限公司 | A kind of fabric coating aqueous polyurethane emulsion of low water absorption and preparation method thereof |
| CN109651951A (en) * | 2018-11-15 | 2019-04-19 | 广东菲安妮皮具股份有限公司 | A kind of viscous high tenacity skin side oil of the height based on aqueous polyurethane |
| CN111808260A (en) * | 2020-07-29 | 2020-10-23 | 四川尤博瑞新材料有限公司 | Thermosensitive condom based on waterborne polyurethane and preparation method thereof |
| CN114057987A (en) * | 2020-08-03 | 2022-02-18 | 东成化学有限公司 | Water-dispersible polyurethane-urea resin composition for synthetic leather and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106047126A (en) * | 2016-08-10 | 2016-10-26 | 福建宝利特科技股份有限公司 | Leather surface treating agent and processing method thereof |
| CN106244744A (en) * | 2016-08-22 | 2016-12-21 | 福建隆上超纤有限公司 | A kind of modified finishing agent for leather and preparation method thereof |
| CN106244744B (en) * | 2016-08-22 | 2018-06-29 | 福建隆上超纤有限公司 | It is a kind of for modification finishing agent of leather and preparation method thereof |
| CN106380575A (en) * | 2016-09-21 | 2017-02-08 | 无锡市莱瑟新材料科技有限公司 | Resin special for air mechanical foaming type polyurethane base and preparation method thereof |
| CN106380575B (en) * | 2016-09-21 | 2018-11-27 | 无锡市莱瑟新材料科技有限公司 | A kind of aero-mechanical foaming type polyurethane bass is resin dedicated and preparation method thereof |
| CN107033764A (en) * | 2017-04-26 | 2017-08-11 | 福建宝利特科技股份有限公司 | A kind of leather finishing degree inorganic agent |
| CN107011494A (en) * | 2017-05-23 | 2017-08-04 | 深圳市润天智数字设备股份有限公司 | A kind of preparation method of aqueous polyurethane dispersion |
| CN109651951A (en) * | 2018-11-15 | 2019-04-19 | 广东菲安妮皮具股份有限公司 | A kind of viscous high tenacity skin side oil of the height based on aqueous polyurethane |
| CN109553752A (en) * | 2018-12-06 | 2019-04-02 | 南通高盟新材料有限公司 | A kind of fabric coating aqueous polyurethane emulsion of low water absorption and preparation method thereof |
| CN111808260A (en) * | 2020-07-29 | 2020-10-23 | 四川尤博瑞新材料有限公司 | Thermosensitive condom based on waterborne polyurethane and preparation method thereof |
| CN111808260B (en) * | 2020-07-29 | 2021-05-25 | 四川尤博瑞新材料有限公司 | Thermosensitive condom based on waterborne polyurethane and preparation method thereof |
| CN114057987A (en) * | 2020-08-03 | 2022-02-18 | 东成化学有限公司 | Water-dispersible polyurethane-urea resin composition for synthetic leather and preparation method thereof |
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