CN109575220A - It is a kind of to spring back aqueous polyurethaneurea elastomer and preparation method thereof fastly - Google Patents
It is a kind of to spring back aqueous polyurethaneurea elastomer and preparation method thereof fastly Download PDFInfo
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- CN109575220A CN109575220A CN201710910560.4A CN201710910560A CN109575220A CN 109575220 A CN109575220 A CN 109575220A CN 201710910560 A CN201710910560 A CN 201710910560A CN 109575220 A CN109575220 A CN 109575220A
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- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
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- C08G18/40—High-molecular-weight compounds
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/50—Polyethers having heteroatoms other than oxygen
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/12—Polyurethanes from compounds containing nitrogen and active hydrogen, the nitrogen atom not being part of an isocyanate group
Abstract
The present invention discloses fast rebound aqueous polyurethaneurea elastomer of one kind and preparation method thereof, using step charging method, solvent, diisocyanate, crosslinking agent, hydrophilic chain extender, catalyst addition reaction kettle are heated up carry out reaction preparation after mixing, is reacted in cooling and with chemical hydrazine compound is added after dispersion and emulsion.It is reacted using ether macromolecular diamine with isocyanates in the present invention and generates urea bond, so that molecule interchain forms the physical crosslinking that hydrogen bond provides, ketocarbonyl-containing and hydrazine reaction generate the chemical crosslinking of molecule interchain；Hydrogen bond physical crosslinking and ketone hydrazine chemical crosslinking synergistic effect, imitate rubber structure, have high-intensitive and quick resilience performance.
Description
Technical field
The present invention relates to the preparations of the synthesis of aqueous polyurethaneurea lotion and aqueous polyurethane urea elastomers, belong to high score
Sub- Material Field.
Background technique
Aqueous polyurethane refers to the new polyurethane system that organic solvent is replaced using water by medium.Aqueous polyurethane has not
Inflammable, nontoxic, the advantages of viscosity flow is adjustable, easy processing, at the same itself and solvent borne polyurethane have high abrasion, it is tear-resistant,
The good performance of caking property, is widely used in coating, adhesive and elastomer.Polyurethane applied to elastomer is a kind of performance Jie
High molecular synthetic material and rubber phase ratio between rubber and plastics is its main feature is that without containing not in the molecular structure of polyurethane
The chemical bond of saturation, thus its ageing-resistant performance is excellent, long service life.Again, the processing and forming technology of polyurethane is simple, both
One-time cast-forming can be used using single injection-molded again, the change of catalyst type and content can also be passed through
Change, realizes its room temperature curing.But compared with rubber elastomer, common water borne polyurethane elastomer resilience performance is poor, this is
Because sulfuration process of the rubber in forming process makes have a large amount of chemical crosslinking points in rubber elastomer, molecule between crosslinking points
Amount is usually bigger, and the weak physical crosslinking point for only having a small amount of hydrogen bond to provide in normal polyurethane elastomer.
Summary of the invention
The object of the present invention is to provide a kind of aqueous polyurethane urea elastomers and preparation method thereof, improve existing aqueous poly- ammonia
Ester elastomer intensity and the incompatible disadvantage of resilience introduce urea groups structure and provide physical crosslinking point, while guaranteeing suitably
It is chemically crosslinked structure.
Technical purpose of the invention is achieved by following technical proposals:
A kind of aqueous polyurethane urea elastomers and preparation method thereof, are prepared as steps described below:
Step 1, polyalcohol and ether macromolecular diamine are subjected to vacuumize process at 90~120 DEG C, to have carried out
Full dehydration, avoids influence of the water to reaction；
In step 1, it carries out polyalcohol and ether macromolecular diamine to vacuumize 1~2h at 90~120 DEG C.
In step 1, polyalcohol and ether macromolecular diamine place 2- in 100-120 DEG C of high temperature library before vacuumizing
5 days, be 24 hours daily.
Step 2, by after step 1 vacuumize process polyalcohol and ether macromolecular diamine be naturally cooling to 50-55
Degree Celsius, using step charging method, reaction is added in solvent, diisocyanate, the first crosslinking agent, hydrophilic chain extender, catalyst
Kettle is warming up to 60~90 DEG C after mixing and is reacted；
In step 2, reaction temperature is 70-80 degrees Celsius, and the reaction time is 2-10 hours, preferably 5-8 hours.
Step 3, step 2 is naturally cooling to 50-55 degrees Celsius of addition solvents after reaction, so that system viscosity is down to
10000mP.s is reacted hereinafter, being naturally cooling to 20-30 DEG C of addition neutralizers again, and it is Celsius to be naturally cooling to 5-10 later
Degree is added water and carries out high-speed stirred emulsification, forms polyurethane-urea lotion；
In step 3, neutralizer is added and carries out 10~30min of reaction；High-speed stirred speed is per minute 1000-2000
Turn, emulsification times are 10-30min.
In step 3, solvent is added reduces the viscosity of reaction system, and solvent adding amount is according to reaction system viscosity test knot
Fruit is determined.The solvent being added in step 3 is consistent with the type of solvent is added in step 2.
Step 4, the second crosslinking agent is added in polyurethane-urea lotion prepared by step 3 to be reacted, later in a vacuum
Solvent is taken under state away to get polyurethane-urea lotion, i.e., the evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer is arrived.
In step 4, when the second crosslinking agent of addition is reacted, keeping high-speed stirred speed is per minute 1000-2000
Turn, the reaction time is 10-30min.
The polyurethane-urea lotion of above-mentioned preparation is carrying out in use, requiring to carry out forming processes, such as leaching according to the prior art
Stain molding, plastic film mulch molding, rotational forming, coated and molded or coating molding, can obtain after water phase in lotion (moisture) evaporation
Obtain polyurethane-urea elastomer.
In the above preparation method, the mass fraction of each raw material components is as follows: 15~30 parts of polyalcohol, ether macromolecular
1~10 part of diamine, 10~30 parts of solvent used in step 2,10~30 parts of diisocyanate, the first 1~10 part of crosslinking agent,
3-8 parts of hydrophilic chain extender, 0.1-0.3 part of catalyst, 1~6 part of neutralizer, 30~50 parts of water, the second 1~5 part of crosslinking agent.
In the above preparation method, the mass fraction of each raw material components is preferred: 20~30 parts of polyalcohol, ether macromolecular
5~10 parts of diamine, 20~30 parts of solvent used in step 2,15~25 parts of diisocyanate, the first 3~8 parts of crosslinking agent,
5-8 parts of hydrophilic chain extender, 0.1-0.3 part of catalyst, 1~5 part of neutralizer, 40~50 parts of water, the second 2~5 parts of crosslinking agent.
Polyalcohol has multiple hydroxyls, is selected from polyadipate-Isosorbide-5-Nitrae-butanediol ester dihydric alcohol, polytetrahydrofuran ether binary
Alcohol or Polyoxypropylene diol.
Ether macromolecular diamine is the polyethylene oxide or polypropylene oxide that end group is amido, and number-average molecular weight is
200~4000, preferably 1000-3000.
Solvent selection organic solvent is selected from acetone, dioxane or n,N-dimethylacetamide.
Diisocyanate is selected from isophorone diisocyanate or hexamethylene diisocyanate.
First crosslinking agent is the reaction monomers containing ketone carbonyl and reactive hydrogen, is selected N- [(1,1- dimethyl -2- acetyl group)
Ethyl]-two hydroxyethylamino propionamide of-β, N ,-two diacetone propionamido- ethylenediamine of N ' or 5- [two (2- ethoxy) amine
Base] -2 pentanone.
Hydrophilic chain extender is hydroxyl carboxylic acid, is selected from dihydromethyl propionic acid or dimethylolpropionic acid.
Catalyst is organotin catalysts, is selected from dibutyl tin dilaurate or stannous octoate.
Neutralizer is selected from triethylamine, sodium hydroxide or potassium hydroxide.
Second crosslinking agent be selected from carbon acid dihydrazide, adipic dihydrazide, sebacic dihydrazide, succinic acid hydrazide ii or
Phthalic acid dihydrazide.
Water-based polyurethane elastomer emulsion (the i.e. evenly dispersed water phase cream for having polyurethane-urea elastomer prepared by the present invention
Liquid) it can be stabilized 12 months or more, use TDZ5-WS centrifuge to carry out centrifugal treating, centrifugation with 3000 revs/min of revolving speed
Rotation 30 minutes without precipitating；With Multisizer 4e Kurt Particle Size Analyzer to lotion carry out granularmetric analysis, partial size between
Between 0.01 to 0.6 micron.Tested polyurethane-urea elastomer prepared by the present invention that (i.e. rotational forming is gone with infrared spectroscopy
Polyurethane-urea elastomer after moisture removal), as shown in Fig. 1,3324.71cm-1Place is the stretching vibration peak of residual hydroxy groups,
2961.07cm-1And 2904.57cm-1It is the stretching vibration peak of C-H on methylmethylene, according to the literature, carbamic acid respectively
The stretching vibration peak of carbonyl is distributed in 1730-1760cm in ester group-1In range, the stretching vibration peak of carbonyl is distributed in urea groups
1680-1715cm-1In range.The stretching vibration peak of carbonyl appears in 1689.54cm in Fig. 1-1, illustrate there is urea groups in polymer
Generation, and have hydrogen bond action.In 1303.37cm-1The absorption peak that place occurs is the vibration peak of C-O-C in ethylene oxide chain, and
Red shift occurs after chain extension, illustrates that hydrogen bond action has occurred between polymer molecule.Infrared spectrum analysis shows monomer according to pre-
Polymerization reaction occurs for phase route, forms polyurethane-urea structure.
Spin coating molding is carried out with aqueous polyurethaneurea elastomer emulsions prepared by the present invention, after moisture evaporation in lotion i.e.
Can get polyurethane-urea elastomer, carry out Mechanics Performance Testing according to GBT 528-2009, elastomer tensile strength between 15~
35MPa, for elongation at break between 200%~1000%, stretch breaking strength is 1-3MPa.Compared with prior art, the present invention uses
Ether macromolecular diamine is reacted with isocyanates generates urea bond, hands over so that molecule interchain forms the physics that hydrogen bond provides
Connection, is added hydrazine after adding water emulsification to disperse and ketocarbonyl-containing reaction generates the chemical crosslinking of molecule interchain, and there is no emulsion structures
Generate destruction；Hydrogen bond physical crosslinking and ketone hydrazine chemical crosslinking synergistic effect, imitate rubber structure, have high-intensitive and quickly rebound
Performance.
Based on aqueous polyurethaneurea elastomer emulsions of the invention as film forming matter, rubber powder, coalescing agent and face is blended
Filler forms aqueous polyurethane track material, and wherein film forming matter is 30-60 mass parts, and 30-60 mass parts of rubber powder, film forming helps
1-10 mass parts of agent, 10-30 mass parts of pigments and fillers, preferably film forming matter be 40-60 mass parts, 30-50 mass parts of rubber powder,
5-10 mass parts of coalescing agent, 10-20 mass parts of pigments and fillers.
Rubber powder size is distributed within the scope of 0.1~2mm, is selected from natural rubber rubber powder, butadiene-styrene rubber rubber powder, neoprene glue
Powder, ethylene propylene diene rubber rubber powder, thermoplastic styrene class elastomer rubber powder or polyurethane-type thermoplastic elastomer rubber powder.
Pigments and fillers are selected from talcum powder, calcium carbonate, white carbon black, diatomite, kaolin or powdered whiting, powdered object
Material, partial size are 200-500 mesh.
Coalescing agent forms (coalescing agent by aqueous wetting dispersing agent, defoaming agent, thickener, delustering agent and pH adjusting agent
1-10 mass parts), wherein 1-6 mass parts of aqueous wetting dispersing agent, 0.1-0.5 mass parts of defoaming agent, 1-3 quality of thickener
Part, 0.1-0.5 mass parts of 0.1-0.5 mass parts of delustering agent and pH adjusting agent.
Carry out Mechanics Performance Testing according to GBT 528-2009, the stretch breaking strength of track material in 0.6MPa~1.5MPa,
Elongation at break is between 60~200%.Construct runway using above-mentioned track material and aqueous polyurethane urea elastomers, runway by
Elastic layer and the anti-slip layer being arranged on elastic layer form, and wherein elastic layer thickness is in 6~10mm, and anti-slip layer thickness is in 1-2mm；
Elastic layer is formed by track material, using the setting of aqueous polyurethaneurea elastomer emulsions (using spraying, brushing, coating or leaching
Stain) on elastic layer, anti-slip layer is formed after molding.
Compared with prior art, the aqueous polyurethane track material applied to sports ground of the invention has preferable rebound
Property and mechanical strength, drying time meet construction requirement, while being formulated and technique is environmentally protective, commercially available raw material can be used in raw material,
Convenient to use and preparation.
Detailed description of the invention
Fig. 1 is the infrared spectrum of polyurethane-urea prepared by the present invention.
Specific embodiment
The present invention will be further described with reference to embodiments, but does not limit the scope of the invention.What embodiment used
Polyalcohol and ether macromolecular diamine are placed 2-5 days in 100-120 DEG C of high temperature library before vacuumizing, and are daily 24 hours.
Direct market is mostly used to buy using raw material, such as Yangzhou Chemical Co., Ltd., Hang Seng, Tianjin Ke Wei chemical reagents corporation.
Embodiment 1
It step 1, is the polycyclic oxygen third of amido by Polyoxypropylene diol -1000 (number-average molecular weight 1000) and end group
Alkane -1000 (number-average molecular weight 1000) carries out vacuumize process 1h at 120 DEG C, to be dehydrated completely；
Step 2, by after step 1 vacuumize process Polyoxypropylene diol -1000 (number-average molecular weight 1000) and
Polypropylene oxide -1000 is naturally cooling to 55 degrees Celsius, using step charging method, by solvent acetone, isophorone diisocyanate
Ester,-two hydroxyethylamino propionamide of the first crosslinking agent N- [(1,1- dimethyl -2- acetyl group) ethyl]-β, hydrophilic chain extender dihydroxy
Methylpropanoic acid, catalyst dibutyl tin dilaurate addition reaction kettle are warming up to 90 DEG C after mixing and carry out reaction 2 hours,
Middle polyalcohol 30g, ether macromolecular diamine 10g, solvent 20g, isophorone diisocyanate 30g, the first crosslinking agent 10g,
Hydrophilic chain extender 8g, catalyst 0.3g；
Step 3, step 2 is naturally cooling to 55 degrees Celsius of addition solvent acetones after reaction, so that system viscosity is down to
10000mP.s, then be naturally cooling to 30 DEG C of addition neutralizer triethylamine 6g and carry out reaction 30min, it is Celsius that it is naturally cooling to 5 later
Degree is added water and carries out high-speed stirred emulsification, and mixing speed is 1500 turns per minute, emulsification times 30min, forms polyurethane-urea cream
Liquid；
Step 4, the second crosslinking agent adipic dihydrazide 5g is added in polyurethane-urea lotion prepared by step 3 to be reacted
30min, being kept stirring speed is 1500 turns per minute, takes solvent under state away in a vacuum later to get newborn to polyurethane-urea
Liquid, i.e., the evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer.
By gained polyurethane-urea lotion plastic film mulch, places and formed within 1 day (i.e. 24 hours) up to poly- under 20-25 degrees Celsius of room temperature
Urethane urea elastomers.
Embodiment 2
It step 1, is the polycyclic oxygen second of amido by polytetrahydrofuran ether dihydric alcohol -600 (number-average molecular weight 600) and end group
Alkane -2000 (number-average molecular weight 2000) carries out vacuumize process 2h at 90 DEG C, to be dehydrated completely；
Step 2, by after step 1 vacuumize process polytetrahydrofuran ether dihydric alcohol -600 (number-average molecular weight 600) and
End group be amido polyethylene oxide -2000 (number-average molecular weight 2000) be naturally cooling to 50 degrees Celsius, using a step feed method,
By solvent dioxane, hexamethylene diisocyanate, the first crosslinking agent 5- [two (2- ethoxy) amidos] -2 pentanone, hydrophilic
Chain extender dimethylolpropionic acid, catalyst dibutyl tin dilaurate are added reaction kettle and are warming up to 60 DEG C of progress after mixing instead
Answer 10 hours, wherein polyalcohol 15g, ether macromolecular diamine 1g, solvent 10g, hexamethylene diisocyanate 10g, first
Crosslinking agent 1g, hydrophilic chain extender 3g, catalyst 0.1g；
Step 3, step 2 is naturally cooling to 50 degrees Celsius of addition solvent dioxane after reaction, so that system viscosity
It is down to 8000mP.s, then is naturally cooling to 20 DEG C of addition neutralizer sodium hydroxide 1g and carries out reaction 10min, is naturally cooling to later
8 degrees Celsius of addition water carry out high-speed stirred emulsification, and mixing speed is 2000 turns per minute, emulsification times 10min, form polyurethane
Urea lotion；
Step 4, the second crosslinking agent carbon acid dihydrazide 1g is added in polyurethane-urea lotion prepared by step 3 to be reacted
10min, being kept stirring speed is 2000 turns per minute, takes solvent under state away in a vacuum later to get newborn to polyurethane-urea
Liquid, i.e., the evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer.
By gained polyurethane-urea lotion plastic film mulch, places and formed within 1 day (i.e. 24 hours) up to poly- under 20-25 degrees Celsius of room temperature
Urethane urea elastomers.
Embodiment 3
It step 1, is the poly- of amido by polyadipate-Isosorbide-5-Nitrae-butanediol ester dihydric alcohol (number-average molecular weight 1000) and end group
Propylene oxide -2000 (number-average molecular weight 2000) carries out vacuumize process 1.5h at 100 DEG C, to be dehydrated completely；
Step 2, by polyadipate-Isosorbide-5-Nitrae after step 1 vacuumize process-butanediol ester dihydric alcohol (number-average molecular weight
1000) and polypropylene oxide -1000 (number-average molecular weight 1000) is naturally cooling to 52 degrees Celsius, will be molten using step charging method
Agent n,N-dimethylacetamide, isophorone diisocyanate, first-two diacetone propionamido- ethylenediamine of crosslinking agent N, N ',
Hydrophilic chain extender dihydromethyl propionic acid, octoate catalyst stannous addition reaction kettle are warming up to 80 DEG C after mixing and carry out reaction 5
Hour, wherein polyalcohol 20g, ether macromolecular diamine 5g, solvent 30g, isophorone diisocyanate 25g, the first crosslinking
Agent 8g, hydrophilic chain extender 5g, catalyst 0.2g；
Step 3, step 2 is naturally cooling to 55 degrees Celsius of addition solvent acetones after reaction, so that system viscosity is down to
7500mP.s, then be naturally cooling to 25 DEG C of addition neutralizer potassium hydroxide 5g and carry out reaction 20min, it is naturally cooling to 10 later and takes the photograph
Family name's degree is added water and carries out high-speed stirred emulsification, and mixing speed is 2000 turns per minute, emulsification times 20min, forms polyurethane-urea
Lotion；
Step 4, the second crosslinking agent sebacic dihydrazide 3g is added in polyurethane-urea lotion prepared by step 3 to be reacted
20min, being kept stirring speed is 1000 turns per minute, takes solvent under state away in a vacuum later to get newborn to polyurethane-urea
Liquid, i.e., the evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer.
By gained polyurethane-urea lotion plastic film mulch, places and formed within 1 day (i.e. 24 hours) up to poly- under 20-25 degrees Celsius of room temperature
Urethane urea elastomers.
Embodiment 4
It step 1, is the polycyclic oxygen third of amido by Polyoxypropylene diol -4000 (number-average molecular weight 4000) and end group
Alkane -4000 (number-average molecular weight 4000) carries out vacuumize process 1h at 100 DEG C, to be dehydrated completely；
Step 2, by after step 1 vacuumize process Polyoxypropylene diol -4000 (number-average molecular weight 4000) and
End group be amido polypropylene oxide -4000 (number-average molecular weight 4000) be naturally cooling to 50 degrees Celsius, using a step feed method,
By solvent n,N-dimethylacetamide, isophorone diisocyanate, first-two diacetone propionamido- second of crosslinking agent N, N '
Diamines, hydrophilic chain extender dimethylolpropionic acid, octoate catalyst stannous are added reaction kettle and are warming up to 90 DEG C of progress after mixing
Reaction 5 hours, wherein polyalcohol 20g, ether macromolecular diamine 10g, solvent 20g, isophorone diisocyanate 15g, the
One crosslinking agent 3g, hydrophilic chain extender 5g, catalyst 0.1g；
Step 3, step 2 is naturally cooling to 52 degrees Celsius of addition solvent n,N-dimethylacetamide after reaction, so that
System viscosity is down to 9000mP.s, then is naturally cooling to 25 DEG C of addition neutralizer triethylamine 3g and carries out reaction 30min, natural later
It is cooled to 5 degrees Celsius of addition water and carries out high-speed stirred emulsification, mixing speed is 1500 turns per minute, emulsification times 25min, is formed
Polyurethane-urea lotion；
Step 4, the second crosslinking agent carbon acid dihydrazide 5g is added in polyurethane-urea lotion prepared by step 3 to be reacted
15min, being kept stirring speed is 1500 turns per minute, takes solvent under state away in a vacuum later to get newborn to polyurethane-urea
Liquid, i.e., the evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer.
By gained polyurethane-urea lotion plastic film mulch, places and formed within 1 day (i.e. 24 hours) up to poly- under 20-25 degrees Celsius of room temperature
Urethane urea elastomers.
Embodiment 5
It step 1, is the polypropylene oxide-of amido by Polyoxypropylene diol -600 (number-average molecular weight 600) and end group
200 (number-average molecular weights 200) carry out vacuumize process 1h at 90 DEG C, to be dehydrated completely；
Step 2, by after step 1 vacuumize process Polyoxypropylene diol -600 (number-average molecular weight 600) and end
Base is that the polypropylene oxide -200 (number-average molecular weight 200) of amido is naturally cooling to 50 degrees Celsius, will be molten using step charging method
Agent n,N-dimethylacetamide, hexamethylene diisocyanate, first-two diacetone propionamido- ethylenediamine of crosslinking agent N, N ',
Hydrophilic chain extender dihydromethyl propionic acid, catalyst dibutyl tin dilaurate be added reaction kettle be warming up to after mixing 70 DEG C into
Row reaction 8 hours, wherein polyalcohol 30g, ether macromolecular diamine 5g, solvent 25g, hexamethylene diisocyanate 15g, the
One crosslinking agent 3g, hydrophilic chain extender 5g, catalyst 0.3g；
Step 3, step 2 is naturally cooling to 50 degrees Celsius of addition solvent n,N-dimethylacetamide after reaction, so that
System viscosity is down to 7000mP.s, then is naturally cooling to 20 DEG C of addition neutralizer triethylamine 2g and carries out reaction 15min, natural later
It is cooled to 5 degrees Celsius of addition water and carries out high-speed stirred emulsification, mixing speed is 2000 turns per minute, emulsification times 15min, is formed
Polyurethane-urea lotion；
Step 4, the second crosslinking agent succinic acid hydrazide ii 2g is added in polyurethane-urea lotion prepared by step 3 to be reacted
30min, being kept stirring speed is 2000 turns per minute, takes solvent under state away in a vacuum later to get newborn to polyurethane-urea
Liquid, i.e., the evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer.
By gained polyurethane-urea lotion plastic film mulch, places and formed within 1 day (i.e. 24 hours) up to poly- under 20-25 degrees Celsius of room temperature
Urethane urea elastomers.
Mechanics Performance Testing is carried out according to GBT 528-2009 with polyurethane-urea elastomer prepared by above-described embodiment 1-5,
Elastomer tensile strength is between 15~35MPa, and for elongation at break between 200%~1000%, stretch breaking strength is 1-3MPa.
The evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer prepared using above-described embodiment 1-5 is film forming matter, altogether
Mixed rubber powder, coalescing agent and pigments and fillers form aqueous polyurethane track material, using mechanical stirring 300-500 turns of realities per minute
It is existing evenly dispersed, thickener is added in aqueous polyurethaneurea lotion, stirs evenly, is added aqueous wetting dispersing agent, delustering agent,
PH adjusting agent, defoaming agent are uniformly dispersed；Pigments and fillers are added, stir evenly；Rubber powder is added, stirs evenly；It filters and packages i.e.
It can.When construction application, direct spraying construction, track material is formulated specific as follows:
The embodiment 1 of track material formula
The evenly dispersed aqueous phase emulsion 60g for having polyurethane-urea elastomer, the 500 mesh calcium carbonate 30g, 200 of the preparation of embodiment 1
Mesh butadiene-styrene rubber rubber powder 60g, coalescing agent 10g, in which: the aqueous wetting dispersing agent BYK-154 of 6g, 3g thickener PVC, 0.2g disappear
Photo etching (model: MH828), 0.5gpH regulator (model: AMP-95), 0.3g defoaming agent (model: SD998).
The embodiment 2 of track material formula
The evenly dispersed aqueous phase emulsion 30g for having polyurethane-urea elastomer, the 500 mesh white carbon black 10g, 200 of the preparation of embodiment 2
Mesh neoprene rubber powder 30g, coalescing agent 8g, in which: 4g aqueous wetting dispersing agent BYK-154,2.5g thickener PVC, 0.5g
Delustering agent (model: MH828), 0.5gpH regulator (model: AMP-95), 0.5g defoaming agent (model: SD998).
The embodiment 3 of track material formula
The evenly dispersed aqueous phase emulsion 40g for having polyurethane-urea elastomer, the 200 mesh diatomite 20g, 200 of the preparation of embodiment 3
Mesh natural rubber rubber powder 40g, coalescing agent 5g, in which: 2g aqueous wetting dispersing agent BYK-154,1.5g thickener PVC, 0.5g
Delustering agent (model: MH828), 0.5gpH regulator (model: AMP-95), 0.5g defoaming agent (model: SD998).
The embodiment 4 of track material formula
The evenly dispersed aqueous phase emulsion 50g for having polyurethane-urea elastomer, the 300 mesh kaolin 15g, 200 of the preparation of embodiment 4
Mesh neoprene rubber powder 30g, coalescing agent 6g, in which: the aqueous wetting dispersing agent BYK-154 of 4g, 1g thickener PVC, 0.5g disappear
Photo etching (model: MH828), 0.3gpH regulator (model: AMP-95), 0.2g defoaming agent (model: SD998).
The embodiment 5 of track material formula
The evenly dispersed aqueous phase emulsion 50g for having polyurethane-urea elastomer, the 300 mesh talcum powder 20g, 200 of the preparation of embodiment 5
Mesh ethylene propylene diene rubber rubber powder 50g, coalescing agent 5, in which: 2g aqueous wetting dispersing agent BYK-154,2g thickener PVC, 0.2g
Delustering agent (model: MH828), 0.3gpH regulator (model: AMP-95), 0.5g defoaming agent (model: SD998).
The track material prepared to the embodiment 1-5 of above-mentioned track material formula carries out mechanics according to GBT 528-2009
Performance test, the stretch breaking strength of track material is in 0.6MPa~1.5MPa, and elongation at break is between 60~200%.
Runway is constructed using above-mentioned track material and aqueous polyurethane urea elastomers, runway is by elastic layer and is arranged in elasticity
Anti-slip layer composition on layer, wherein elastic layer thickness is in 6mm, and anti-slip layer thickness is in 2mm；Elastic layer is formed by track material, is adopted
With aqueous polyurethaneurea elastomer emulsions setting (using spraying, brushing, coating or dipping) on elastic layer, formed after molding
Anti-slip layer.Surface drying time (23 ± 2 DEG C): 2mm thickness coatings, 1h；It does solid work the time (23 ± 2 DEG C): 2mm thickness coatings, 48h,
It is tested after building runway, as shown in the table:
| Project | Index | As a result |
| Impact absorbing | 35~50 | 45 |
| Tensile strength | ≥0.5 | 1.5MPa |
| Elongation rate of tensile failure | ≥40 | 200% |
| Compression recovery rate | >=90% | 98% |
| Flame retardant grade | I | I |
In addition, can intuitively be experienced by fanning news method, product produced by the present invention is not pungent, substantially tasteless, thus
It is found that the present invention has lower VOC emission, more preferably environmental-protecting performance is shown.
Content carries out the adjustment of preparation process according to the present invention, and aqueous polyurethaneurea elastomer emulsions, poly- ammonia can be achieved
The preparation of ester urea elastomers and track material, and show almost the same performance.The present invention has been done illustratively above
Description, it should explanation, in the case where not departing from core of the invention, it is any it is simple deformation, modification or other
Field technical staff can not spend the equivalent replacement of creative work to each fall within protection scope of the present invention.
Claims (10)
1. a kind of aqueous polyurethane urea elastomers, which is characterized in that prepared as steps described below:
Step 1, polyalcohol and ether macromolecular diamine are subjected to vacuumize process at 90~120 DEG C, it is completely de- to carry out
Water avoids influence of the water to reaction；
Step 2, by after step 1 vacuumize process polyalcohol and ether macromolecular diamine to be naturally cooling to 50-55 Celsius
Solvent, diisocyanate, the first crosslinking agent, hydrophilic chain extender, catalyst are added reaction kettle and mixed by degree using step charging method
60~90 DEG C are warming up to after closing uniformly to be reacted；
Step 3, step 2 is naturally cooling to 50-55 degrees Celsius of addition solvents after reaction, so that system viscosity is down to
10000mP.s is reacted hereinafter, being naturally cooling to 20-30 DEG C of addition neutralizers again, and it is Celsius to be naturally cooling to 5-10 later
Degree is added water and carries out high-speed stirred emulsification, forms polyurethane-urea lotion；
Step 4, it the second crosslinking agent is added is reacted in polyurethane-urea lotion prepared by step 3, later state in a vacuum
Under take solvent away to get to polyurethane-urea lotion, i.e., the evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer, in which: each
The mass fraction of raw material components is as follows: 15~30 parts of polyalcohol, 1~10 part of ether macromolecular diamine, and 10~30 parts of solvent, two
10~30 parts of isocyanates, the first 1~10 part of crosslinking agent, 3-8 parts of hydrophilic chain extender, 0.1-0.3 part of catalyst, neutralizer 1
~6 parts, 30~50 parts of water, the second 1~5 part of crosslinking agent.
2. a kind of aqueous polyurethane urea elastomers according to claim 1, which is characterized in that the quality of each raw material components
Number is preferred: 20~30 parts of polyalcohol, 5~10 parts of ether macromolecular diamine, and 20~30 parts of solvent used in step 2, two
15~25 parts of isocyanates, the first 3~8 parts of crosslinking agent, 5-8 parts of hydrophilic chain extender, 0.1-0.3 part of catalyst, neutralizer 1~
5 parts, 40~50 parts of water, the second 2~5 parts of crosslinking agent.
3. a kind of aqueous polyurethane urea elastomers according to claim 1, which is characterized in that in step 1, by polyalcohol
It carries out vacuumizing 1~2h at 90~120 DEG C with ether macromolecular diamine；Polyalcohol is selected from polyadipate-Isosorbide-5-Nitrae-fourth two
Alcohol ester dihydric alcohol, polytetrahydrofuran ether dihydric alcohol or Polyoxypropylene diol；It is amine that ether macromolecular diamine, which is end group,
The polyethylene oxide or polypropylene oxide of base, number-average molecular weight are 200~4000, preferably 1000-3000.
4. a kind of aqueous polyurethane urea elastomers according to claim 1, which is characterized in that in step 2, reaction temperature
It is 70-80 degrees Celsius, the reaction time is 2-10 hours, preferably 5-8 hours；Solvent selection organic solvent is selected from acetone, two
Six ring of oxygen or n,N-dimethylacetamide；Diisocyanate is selected from two isocyanide of isophorone diisocyanate or hexa-methylene
Acid esters；First crosslinking agent is the reaction monomers containing ketone carbonyl and reactive hydrogen, selects N- [(1,1- dimethyl -2- acetyl group) second
Base]-two hydroxyethylamino propionamide of-β, N ,-two diacetone propionamido- ethylenediamine of N ' or 5- [two (2- ethoxy) amidos]-
2 pentanone；Hydrophilic chain extender is hydroxyl carboxylic acid, is selected from dihydromethyl propionic acid or dimethylolpropionic acid；Catalyst is urged for organotin
Agent is selected from dibutyl tin dilaurate or stannous octoate.
5. a kind of aqueous polyurethane urea elastomers according to claim 1, which is characterized in that in step 3, solvent is added
The viscosity of reaction system is reduced, solvent adding amount is determined that is be added in step 3 is molten according to reaction system viscosity test results
Agent is consistent with the type of solvent is added in step 2；Neutralizer is added and carries out 10~30min of reaction；High-speed stirred speed is every point
1000-2000 turns of clock, emulsification times are 10-30min；Neutralizer is selected from triethylamine, sodium hydroxide or potassium hydroxide.
6. a kind of aqueous polyurethane urea elastomers according to claim 1, which is characterized in that in step 4, be added second
When crosslinking agent is reacted, keeping high-speed stirred speed is 1000-2000 turns per minute, and the reaction time is 10-30min；The
Two crosslinking agents are selected from carbon acid dihydrazide, adipic dihydrazide, sebacic dihydrazide, succinic acid hydrazide ii or M-phthalic acid two
Hydrazides.
7. a kind of aqueous polyurethaneurea method for producing elastomers, which is characterized in that prepared as steps described below:
Step 1, polyalcohol and ether macromolecular diamine are subjected to vacuumize process at 90~120 DEG C, it is completely de- to carry out
Water avoids influence of the water to reaction；
Step 2, by after step 1 vacuumize process polyalcohol and ether macromolecular diamine to be naturally cooling to 50-55 Celsius
Solvent, diisocyanate, the first crosslinking agent, hydrophilic chain extender, catalyst are added reaction kettle and mixed by degree using step charging method
60~90 DEG C are warming up to after closing uniformly to be reacted；
Step 3, step 2 is naturally cooling to 50-55 degrees Celsius of addition solvents after reaction, so that system viscosity is down to
10000mP.s is reacted hereinafter, being naturally cooling to 20-30 DEG C of addition neutralizers again, and it is Celsius to be naturally cooling to 5-10 later
Degree is added water and carries out high-speed stirred emulsification, forms polyurethane-urea lotion；
Step 4, it the second crosslinking agent is added is reacted in polyurethane-urea lotion prepared by step 3, later state in a vacuum
Under take solvent away to get to polyurethane-urea lotion, i.e., the evenly dispersed aqueous phase emulsion for having polyurethane-urea elastomer, in which: each
The mass fraction of raw material components is as follows: 15~30 parts of polyalcohol, 1~10 part of ether macromolecular diamine, and 10~30 parts of solvent, two
10~30 parts of isocyanates, the first 1~10 part of crosslinking agent, 3-8 parts of hydrophilic chain extender, 0.1-0.3 part of catalyst, neutralizer 1
~6 parts, 30~50 parts of water, the second 1~5 part of crosslinking agent；The mass fraction of each raw material components is preferred: 20~30 parts of polyalcohol,
5~10 parts of ether macromolecular diamine, 20~30 parts of solvent used in step 2,15~25 parts of diisocyanate, the first crosslinking
3~8 parts of agent, 5-8 parts of hydrophilic chain extender, 0.1-0.3 part of catalyst, 1~5 part of neutralizer, 40~50 parts of water, the second crosslinking agent
2~5 parts.
8. a kind of aqueous polyurethaneurea method for producing elastomers according to claim 7, which is characterized in that in step 1
In, it carries out polyalcohol and ether macromolecular diamine to vacuumize 1~2h at 90~120 DEG C；Polyalcohol, which is selected from, gathers oneself two
Acid-Isosorbide-5-Nitrae-butanediol ester dihydric alcohol, polytetrahydrofuran ether dihydric alcohol or Polyoxypropylene diol；Ether macromolecular binary
Amine is the polyethylene oxide or polypropylene oxide that end group is amido, and number-average molecular weight is 200~4000, preferably 1000-
3000；In step 2, reaction temperature is 70-80 degrees Celsius, and the reaction time is 2-10 hours, preferably 5-8 hours；Solvent choosing
Organic solvent is selected, acetone, dioxane or n,N-dimethylacetamide are selected from；Diisocyanate is selected from two isocyanide of isophorone
Acid esters or hexamethylene diisocyanate；First crosslinking agent is the reaction monomers containing ketone carbonyl and reactive hydrogen, selects N-
- two hydroxyethylamino propionamide of [(1,1- dimethyl -2- acetyl group) ethyl]-β, N,-two diacetone propionamido- ethylenediamine of N ' or
Person 5- [two (2- ethoxy) amidos] -2 pentanone；Hydrophilic chain extender is hydroxyl carboxylic acid, is selected from dihydromethyl propionic acid or dihydroxy first
Base butyric acid；Catalyst is organotin catalysts, is selected from dibutyl tin dilaurate or stannous octoate.
9. a kind of aqueous polyurethaneurea method for producing elastomers according to claim 7, which is characterized in that in step 3
In, solvent, which is added, reduces the viscosity of reaction system, and solvent adding amount is determined according to reaction system viscosity test results, step
The solvent being added in 3 is consistent with the type of solvent is added in step 2；Neutralizer is added and carries out 10~30min of reaction；High-speed stirred
Speed is 1000-2000 turns per minute, and emulsification times are 10-30min；Neutralizer is selected from triethylamine, sodium hydroxide or hydrogen
Potassium oxide；In step 4, when the second crosslinking agent of addition is reacted, keeping high-speed stirred speed is per minute 1000-2000
Turn, the reaction time is 10-30min；Second crosslinking agent is selected from carbon acid dihydrazide, adipic dihydrazide, sebacic dihydrazide, fourth
Dihydrazi or isophthalic dihydrazide.
10. the aqueous polyurethane urea elastomers as described in one of claim 1-6 are preparing the application in track material.
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