CN106632985A - Polyurethane foam material, preparation method and uses thereof - Google Patents
Polyurethane foam material, preparation method and uses thereof Download PDFInfo
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- CN106632985A CN106632985A CN201510740470.6A CN201510740470A CN106632985A CN 106632985 A CN106632985 A CN 106632985A CN 201510740470 A CN201510740470 A CN 201510740470A CN 106632985 A CN106632985 A CN 106632985A
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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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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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
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- 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
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4072—Mixtures of compounds of group C08G18/63 with other macromolecular compounds
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/63—Block or graft polymers obtained by polymerising compounds having carbon-to-carbon double bonds on to polymers
- C08G18/632—Block or graft polymers obtained by polymerising compounds having carbon-to-carbon double bonds on to polymers onto polyethers
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/77—Polyisocyanates or polyisothiocyanates having heteroatoms in addition to the isocyanate or isothiocyanate nitrogen and oxygen or sulfur
- C08G18/78—Nitrogen
- C08G18/79—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates
- C08G18/797—Nitrogen characterised by the polyisocyanates used, these having groups formed by oligomerisation of isocyanates or isothiocyanates containing carbodiimide and/or uretone-imine groups
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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
- C08G2110/00—Foam properties
- C08G2110/0041—Foam properties having specified density
- C08G2110/0058—≥50 and <150kg/m3
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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
- C08G2110/00—Foam properties
- C08G2110/0041—Foam properties having specified density
- C08G2110/0066—≥ 150kg/m3
-
- 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
- C08G2110/00—Foam properties
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The present invention discloses a polyurethane foam material and a preparation method thereof. The preparation method comprises: uniformly mixing and stirring a polyether polyol composition A and a modified isocyanate prepolymer B according to a certain ratio, pouring into a mold, and aging to obtain the polyurethane foam material, wherein the polyether polyol composition A comprises a mixed polyether polyol, a foaming agent, a chain extender, a catalyst, and, if necessary, an inorganic filler and a pigment paste, and the modified isocyanate prepolymer B comprises urethane modified isocyanate and carbodiimide modified isocyanate. According to the present invention, the polyurethane foam material has a density of 80-160 kg/m<3> and a hardness of ASKER C 10-40, and has characteristics of good gas permeability and low permanent compression deformation; and the material has good processing characteristics, the mold expansion during shrinkage and mold opening is avoided, and the defective rate of the product is reduced.
Description
Technical field
The present invention relates to a kind of polyurethane foamed material and its production and use.
Background technology
People when motion, is completed by the strength of foot, is thus had than larger load
Impulsive force concentrate on foot；Along with foot can produce substantial amounts of perspiration, growing for foot antibacterial is reduced
Foot environmental amenity degree.The sole of most sport shoess be provided with damping and it is high-elastic the characteristics of, but
It is to rely solely on sole to improve the comfort level of motion, it is clear that not enough.
Traditional sport shoe-pad mostly is high density and returns power EVA, and this material resilience force and pliability are all higher than it
His material, the performance of damping is also very outstanding, but eva foam breathability extreme difference, it is easily caused foot odor；
Have again be exactly EVA shoe pad Compression Set it is poor, reduce service life.
There is one kind to be exactly high density polyurethane foam shoe pad on the market, can be used for sport shoess shoe pad.Polyurethane
Full name is polyurethanes, is containing the system of the macromolecular compound for repeating carbamate groups on main chain
Claim.It is formed with dihydroxy or polyol addition polymerization by organic diisocyanate or polyisocyanates.
The resistance to ozone of polyurethane, ageing-resistant ability are strong, and performance will not be decreased obviously with the prolongation of time, greatly prolong
The service life of shoe pad foam.Microporous polyurethane elastic foam is due to excellent wearability, ageing-resistant
Performance, fabulous resilience, during the materials such as sole, steering wheel for vehicle, furniture armrest have been widely used in.
Chinese publication CN101864164B discloses a kind of production method of polyurethane insole material, should
Invention does not limit species, molecular weight and degree of functionality of polyethers etc., polyurethane material prepared in the method
Although material can cause in this case the permanent of material with relatively low density and preferable breathability
Compressive deformation can be raised.
Chinese publication CN101585901B disclose a kind of polyurethane foamed material and preparation method thereof and
Purposes, the good permeability of prepared polyurethane material, permanent compression set are low, but the technical scheme cannot
Take into account breathability, permanent compression set and the aspect performance of density three of polyurethane foamed material.
Therefore need to seek a kind of new polyurethane foamed material to be applied to insole material, it should have good
Breathability well, low-density and low permanent compression set.
The content of the invention
Object of the present invention is to provide a kind of polyurethane foamed material, by poly- to dominant response component
The design of ethoxylated polyhydric alcohol compositionss and modified isocyanate prepolymer so that the polyurethane foamed material of gained
Under conditions of with excellent mechanical performances, not only with good breathability and relatively low density, also very
Big degree reduces Compression Set.
It is a further object to provide a kind of preparation method of the polyurethane foamed material, this system
, compared to prior art, the method process is simple, combination material room temperature is storage-stable, nodeless mesh for Preparation Method,
Can be operated in room temperature, and the swollen mould that can be prevented effectively from when shrinking and molding, reduce the secondary of product
Product rate.
The present invention will also provide the polyurethane foamed material to be used to prepare the purposes of shoe pad.
To reach object above, technical scheme is as follows：
A kind of polyurethane foamed material, it is anti-by polyether glycol composition A and modified isocyanate prepolymer B
Should obtain, the polyurethane foamed material density is 80-160kg/m3；The polyurethane foamed material
ASKER C hardness is 10-40, and percent opening is 90-100% according to ASTM D6226-05 standard testings, is pressed
Contracting permanent deformation is 2-10% according to ASTM D-395-B standard testings.
In the present invention, [NCO] group is combined with the polyether polyol in the modified isocyanate prepolymer B
The mol ratio of [OH] group in thing A is 1.02-1.2:1；It is preferred that 1.06-1.15:1.
In the present invention, the polyether glycol composition A includes：
(a) admixtured polyether polyhydric alcohol, including：
Polyether polyol (1), its average functionality in 2-4, number-average molecular weight in 2000-8000, preferably
4000-6000, its ethylene oxide content in 10-20wt%, preferred 13-17wt%；
Optional polyether polyol (2), is obtained by styrene, acrylonitrile compolymer graft modification, and solid content is
20-45wt%, in 2-4, in 2000-8000, its ethylene oxide content exists number-average molecular weight its average functionality
10-20wt%；
Polyether polyol (3), its average functionality in 2-4, number-average molecular weight in 2000-8000, preferably
4000-6000, its ethylene oxide content in 50-100wt%, preferred 70-100wt%.
The polyether glycol composition A also includes (b) composite assistants, including：The foaming agent of 1-3 weight portions,
The catalyst of 0.2-1 weight portions, the inorganic filler of the chain extender of 2-10 weight portions and 0-20 weight portions and
The mill base of 0-5 weight portions；
By weight, (a) the admixtured polyether polyhydric alcohol:(b) composite assistants=100:3.2-39.
As a kind of preferred scheme, in the present invention, in terms of the weight of (a) admixtured polyether polyhydric alcohol, gather
The content of ethoxylated polyhydric alcohol (1) is 20-99wt%, preferred 30-80wt%, and the content of polyether polyol (2) is 0-75
Wt%, preferred 15-65wt%, the content of polyether polyol (3) is 1-8wt%, preferred 2-5wt%.
In the present invention, the foaming agent in described composite assistants (b) can be selected from H2O、N2、CO2, chlorine fluorine
One or more of hydrocarbon compound, HCFC compound；Preferably, the foaming agent is selected from H20。
In the present invention, the chain extender in described composite assistants (b) can be selected from diglycol, a contracting two
One kind in Propylene Glycol, ethylene glycol, Propylene Glycol, 1,4- butanediols and Polyethylene Glycol that number-average molecular weight is 200
Or it is various.
In the present invention, the catalyst in described composite assistants (b) can be selected from amines catalyst, it is preferable that
The amines catalyst is selected from double (dimethylaminoethyl) ether, triethylenediamine, N, N- dimethyleyelohexanes
One or more in amine, five methyl diethylentriamine and dimethylethanolamine.
In the present invention, in described composite assistants (b), inorganic filler is also included when necessary；Preferably, institute
State one or more that inorganic filler can be selected from Pulvis Talci, kieselguhr and ground calcium carbonate.
Used as a kind of preferred technical scheme, the present invention introduces inorganic filling out when polyurethane insole foam is prepared
Material, inorganic filler due to organic macromolecule poor compatibility, cause the local defect of foam, also can improve
Opening.
In the present invention, in described composite assistants (b), when necessary also include mill base, the mill base include but
The one kind being not limited in red slurry, orange pulp, yellow pulp, green slurry, blue slurry, purple slurry and black slurry
Or it is various.
In the present invention, the polyether glycol composition A, viscosity is 1000-3000mPas, preferably
1200-2000mPa·s；The modified isocyanate prepolymer B, viscosity is 80-699mPas, preferred 100-450
mPa·s。
In the present invention, the modified isocyanate prepolymer B, its NCO content is 16-28wt%, preferably
18-24wt%, including：
C the content of () urethane modified isocyanate (being also called urethane-modified polyisocyanates) is 60-99
Wt%, preferred 70-98wt%, with the gross weight meter of the modified isocyanate prepolymer B, it is by polyhydric alcohol
(c1) the urethane modified isocyanate of the NCO end-blockings for obtaining with isocyanates (c2) reaction, the polyhydric alcohol (c1)
Average functionality is 2-3；
(d) Carbodiimide-Modified isocyanates 1-40wt%, preferred 2-30wt%, with the modified Carbimide.
The gross weight meter of ester prepolymer B；Balance of urethane modified isocyanate.
Used as a kind of preferred scheme, in the present invention, described polyhydric alcohol (c1) includes following component：
E () dihydroxylic alcohols, account for the 0-30wt% of polyether polyol (c1) gross weight, preferred 1-20wt%, the binary
The preferred diglycol of alcohol, dipropylene glycol, 1,2- Propylene Glycol, 1,3- Propylene Glycol, 1,4- butanediols, 1,3-
One or more in butanediol, tripropylene glycol；
F () polyether polyol, accounts for the 10-60wt% of polyether polyol (c1) gross weight, preferred 20-50wt%,
Average functionality 2-3, number-average molecular weight is 100-12000, preferred 1000-11000, by oxirane and ring
One kind or its combination in Ethylene Oxide is formed through ring-opening polymerisation；
G () polyether polyol, accounts for the 30-90wt% of polyether polyol (c1) gross weight, preferred 40-80wt%,
Average functionality is 2-3, and number-average molecular weight is 2000-12000, preferred 4000-10000, by expoxy propane Jing
Cross ring-opening polymerisation to form.
In the present invention, the isocyanates (c2) can be selected from aliphatic, cycloaliphatic and aromatic isocyanate
In one or more, the degree of functionality of the aliphatic, cycloaliphatic and aromatic isocyanate is 2-6, excellent
Select toluene di-isocyanate(TDI) and/or methyl diphenylene diisocyanate, more preferably diphenyl methane -4,4 '-two isocyanides
Acid esters and diphenyl methane -2, the mixture of 4 '-diisocyanate, wherein, with the gross weight meter of isocyanates (c2),
Diphenyl methane -4, the content of 4 '-diisocyanate is 90-100wt%, preferred 95-99wt%.
Used as a kind of preferred scheme, in the present invention, the isocyanates (c2) can be selected from ten thousand magnificent chemical productions
MDI100, the Carbodiimide-Modified isocyanates can be selected from ten thousand magnificent chemical productions
CDMDI100L。
Opening (breathability) and the soft and hard segments of the polyurethane foam degree that is mutually separated is relevant.Phase separation degree
Higher, foamed open cell is better, and vice versa；NCO group generates urea, the richness of different molecular with water reaction
Urea hard section is gathered into urea phase hard area because of hydrogen bond action, is produced due to the thermodynamics incompatibility of soft and hard segments micro-
It is separated, but microphase-separated is usually incomplete, that is, have a small amount of hard section to be mutually dispersed in soft section phase, causes
Phase separation degree is deteriorated.High ethylene oxide content polyether polyol used in inventive formulation, in soft section phase
Containing substantial amounts of oxygen ethylene group, all or part of urea phase can be dissolved so that soft section is mutually purer, phase point
It is higher from degree.
While high ethylene oxide content polyether polyol improves split-phase degree, hard segment content can also be reduced,
Further improve the Compression Set of foam.This is because polyurethane foam is containing polyureas and polyurethane
Ester block copolymer, polyester soft segment determines the elasticity of foam and rubber mass characteristic, and especially foam is in load feelings
Segment mobility under condition.The urea hard section produced by isocyanates be foam provide basic hardness with by force
Degree, what urea aggregation was leaned on together is the interaction of intermolecular N-H-N hydrogen bonds.And just because of the hard phase region of urea
Exist, foam in load conditions, can occur sliding with the urea phase region segment of hydrogen bonded, reset with new
Conformation is adapting to this compressive state.After unloading, due to the presence of permanent crosslinking in foam, foam has fast
The trend of quick-recovery, but and because the recovery of the urea phase region segment for occurring to reset needs the regular hour, institute
To produce certain permanent deformation.
The present invention has been also carried out improving in the selection of isocyanates, present invention employs urethane modification technology,
I.e. polyhydric alcohol first reacts with isocyanates, forms the end NCO performed polymers of macromolecular chain, the segment for eventually forming
On the other hand structure is more regular, and this performed polymer can also significantly improve the resilience of product, and, urethane is modified skill
Art can effectively control viscosity, exothermic heat of reaction, the reactivity of reactant, i.e. primary response and be unlikely to viscous
Degree increases too fast, good to ensure material mobility, it is ensured that the defect such as products appearance is pin-free.Again
Have, select in the polyhydric alcohol of urethane modified isocyanate, the polyethers of the preferred loopful Ethylene Oxide of the present invention is more
First alcohol, hence it is evident that improve the opening of foam, increased breathability.
" optional " expression in the present invention is with or without.
Present invention also offers a kind of preparation method of polyurethane foamed material, comprises the following steps：
(1) admixtured polyether polyhydric alcohol (a) and composite assistants (b) are mixed to get into the polyether polyol by stirring
Compositionss A, wherein, whipping temp is controlled at 5-50 DEG C, preferred 30-45 DEG C；
(2) described polyhydric alcohol (c1) is mixed with isocyanates (c2), mixing temperature is controlled at 50-100 DEG C, excellent
60-85 DEG C is selected, the urethane modified isocyanate that NCO end-blockings are generated in mixture is made；Control NCO end-blockings
The temperature of urethane modified isocyanate preferred 40-60 DEG C, adds carbonization two sub- at 30-70 DEG C in mixture
Amine modified isocyanate stirs, and obtains the modified isocyanate prepolymer B；
(3) by step (1) gained polyether glycol composition A and step (2) gained modified isocyanate prepolymer B
Mixing makes it carry out foamable reaction, and while foaming chain growth is carried out, when the foaming in reactant and chain increase
When long reaction is fully completed, the polyurethane foamed material is obtained final product；
Wherein, step (3) mixture is during reaction, in the presence of liquid condition, temperature control
Make at 15-25 DEG C, preferred 18-22 DEG C.
In the preparation method of polyurethane foam of the present invention, each component mixing process can refer to
Mixing method commonly used in the art realizing, wherein, mixing apparatus, mixing velocity, incorporation time etc. can
Being the conventional equipment in this area and parameter；In addition, in (3) the step of preparation method of the present invention
Mixed foaming process when foaming and propagation process, wherein reactant are in liquid condition can steep machine in such as case
Deng carrying out in conventional consersion unit, when reactant starts to solidify to form polyurethane foamed material, Ke Yitong
Cross by through mixing and carry out a period of time preliminary foamable reaction liquid mixture be transferred in mould carry out it is ripe
Change, wherein, the parameter such as time, mold temperature, curing time of initial reaction can refer to art technology
The parameter that personnel commonly use is configured.
Although it should be noted that the equipment not being limited in above-mentioned reactions steps, temperature, time, speed
Knowledge familiar to those skilled in the art is can refer to etc. factor to be controlled, but the control of these factors must
Carry out under conditions of must limiting in preparation method of the present invention, such as the extent of reaction, reactant state,
And be defined by obtaining polyurethane foamed material of the present invention.
The present invention still further provides purposes of the polyurethane foamed material of the present invention in shoe pad is prepared.
Concrete application method：Can be by polyurethane foamed material Jing cut-parts of the present invention, laminating, hot-forming, most
After cut into shoe pad finished product, also can be according to method application familiar to other skilled in the art.
The polyurethane foamed material of the present invention has good breathability and relatively low permanent compression set and relatively low
Density, and inventive formulation has good technique processing characteristics, it is to avoid swollen mould when shrinking and molding,
Reduce the defect rate of product.
Specific embodiment
With reference to embodiments the present invention is described further, and the following examples can make this specialty
Technical staff is more fully understood the present invention, but limits the present invention never in any form.
The present invention it is raw materials used including：
The copolyether polyhydric alcohol of the starting of the glycerol of Polyol 1, oxirane and expoxy propane, oxirane contains
Amount 15%, molecular weight 5000, degree of functionality 3, hydroxyl value 33.7mgKOH/g；
The trimethylolpropanes of Polyol 2 and tetramethylolmethane starting, oxirane is more with the copolyether of expoxy propane
First alcohol, ethylene oxide content 17%, molecular weight 6000, degree of functionality 3.5, hydroxyl value 32.7mgKOH/g；
The starting of the glycerol of Polyol 3, styrene, acrylonitrile compolymer graft modification polyether polyol, solid content 30%,
Ethylene oxide content 12%, molecular weight 6000, degree of functionality 3, hydroxyl value 28.1mgKOH/g；
The starting of the glycerol of Polyol 4, styrene, acrylonitrile compolymer graft modification polyether polyol, solid content 42%,
Ethylene oxide content 15%, molecular weight 4000, degree of functionality 3, hydroxyl value 42.1mgKOH/g；
The copolyether polyhydric alcohol of the starting of the glycerol of Polyol 5, oxirane and expoxy propane, oxirane contains
Amount 70%, molecular weight 5000, degree of functionality 3, hydroxyl value 33.7mgKOH/g；
The copolyether polyhydric alcohol of the starting of the tetramethylolmethanes of Polyol 6, oxirane and expoxy propane, oxirane
Content 85%, molecular weight 3000, degree of functionality 4, hydroxyl value 74.8mgKOH/g；
The starting of Polyol7 glycerol, oxirane homopolymerization polyether polyol, molecular weight 8000, degree of functionality 3, hydroxyl
Value 21.0mgKOH/g；
Polyol8 diglycols, molecular weight 106.1, degree of functionality 2；
Polyol91, ammediol, molecular weight 76.1, degree of functionality 2；
The copolyether polyhydric alcohol of the starting of Polyol10 glycerol, oxirane and expoxy propane, oxirane
End-blocking copolymerization, ethylene oxide content 14%, molecular weight 6000, degree of functionality 3, hydroxyl value 28.1mgKOH/g；
The starting of Polyol11 dipropylene glycol, expoxy propane homopolymerization polyether polyol, molecular weight 2000, degree of functionality 2,
Hydroxyl value 56.1mgKOH/g；
The starting of Polyol12 glycerol, expoxy propane homopolymerization polyether polyol, molecular weight 8000, degree of functionality 3,
Hydroxyl value 21.0mgKOH/g；
The starting of Polyol13 glycerol, expoxy propane homopolymerization polyether polyol, molecular weight 12000, degree of functionality 3,
Hydroxyl value 14.0mgKOH/g；
Foaming agent, water；
Chain extender, ethylene glycol；
Chain extender, BDO；
Chain extender, dipropylene glycol；
Catalyst, double (dimethylaminoethyl) ethers；
Catalyst, triethylenediamine；
Catalyst, dimethylethanolamine；
Inorganic filler, Pulvis Talci；
Inorganic filler, kieselguhr；
Mill base；
Methyl diphenylene diisocyanate, ten thousand China's chemistry, MDI-100；Wherein '-two of diphenyl methane -4,4 are different
The content of cyanate is 98wt%；
Carbodiimide-Modified isocyanates, ten thousand China's chemistry, CDMDI100L.
The preparation of modified isocyanate prepolymer B (Isocynate1-4)：
It should be noted that the preparation scheme of the B component is calculated according to B component 1000g, it is different
The weight portion of the B component used in embodiment is different, and implementation process is with the weight of B component used in different embodiments
Amount part is defined.
Viscosity adopts GB/T 12009.3-89 standard testings.
The preparation of Isocynate1：550g is added in equipped with agitator, thermometer, the there-necked flask of nitrogen tube
Methyl diphenylene diisocyanate, is heated to 60-70 DEG C, is subsequently adding Polyol8, Polyol9 and Polyol10,
Its quality for adding is respectively 15g, 20g and 215g.Temperature is risen to into 80 DEG C, with 50 revs/min of speed
After stirring 2 hours, stirring products therefrom temperature is adjusted to into 40 DEG C, adds 200g Carbodiimide-Modifieds
Isocyanates, stir 0.5 hour, obtain Isocynate1, and the NCO content of Isocynate1 is controlled in 19.9-20.9
Wt%, viscosity is 650mPas；
The preparation of Isocynate2：500g is added in equipped with agitator, thermometer, the there-necked flask of nitrogen tube
Methyl diphenylene diisocyanate, is heated to 60-70 DEG C, is subsequently adding Polyol8, Polyol10 and Polyol12,
Its quality for adding is respectively 20g, 105g and 105g.Temperature is risen to into 80 DEG C, with 100 revs/min of speed
After degree stirring 2 hours, stirring products therefrom temperature is adjusted to into 50 DEG C, adds 270g carbodiimides and change
Property isocyanates, stir 0.5 hour, obtain Isocynate2, the NCO content control of Isocynate2 exists
22.3-23.3wt%, viscosity is 130mPas；
The preparation of Isocynate3：450g is added in equipped with agitator, thermometer, the there-necked flask of nitrogen tube
Methyl diphenylene diisocyanate, is heated to 60-70 DEG C, is subsequently adding Polyol10 and Polyol11, and it adds
The quality for entering is respectively 225g and 225g.Temperature is risen to into 80 DEG C, it is little with 200 revs/min of speed stirring 2
Shi Hou, by stirring products therefrom temperature 60 DEG C are adjusted to, and add 100g Carbodiimide-Modified isocyanates,
Stirring 0.5 hour, obtains Isocynate3, and the NCO content of Isocynate3 is controlled in 16.1-17.1wt%,
Viscosity is 350mPas；
The preparation of Isocynate4：500 2 are added in equipped with agitator, thermometer, the there-necked flask of nitrogen tube
Methylenebis phenyl isocyanate, is heated to 60-70 DEG C, is subsequently adding Polyol10 and Polyol11, its addition
Quality be respectively 100 and 380g, temperature is risen to into 80 DEG C, after being stirred 2 hours with 200 revs/min of speed,
Stirring products therefrom temperature is adjusted to into 60 DEG C, 20g Carbodiimide-Modified isocyanates are added, is stirred
0.5 hour, Isocynate4 is obtained, the NCO content of Isocynate4 is controlled in 16.1-17.1wt%, and viscosity is
300mPa·s。
The concrete weight portion of different component raw material described in embodiment and comparative example and the testing standard of product are
List in detail in table 1, strict implement the step of test process is according to described in different testing standards,
Therefore in the specific implementation step of embodiment and comparative example, each component ratio and testing procedure are no longer listed.
Embodiment 1
Under room temperature, component A raw material is put in reactor successively, using high shear agitation device 10 points are stirred
Clock, the speed of stirring is 1500 revs/min, is discharged as component A, and viscosity is 1400mPas；Adjust respectively
The component A and Isocynate2 are put into case bubble machine by the temperature of whole component A and Isocynate2 to 22 DEG C
Stirring 22 seconds, in being poured into 35 DEG C of mould, ripening is molded after 20 minutes, obtains of the present invention poly-
Urethane foam；The polyurethane foam room temperature is placed into 30 hours afterwards, mechanical property is tested.
Embodiment 2
Under room temperature, component A raw material is put in reactor successively, using high shear agitation device 15 points are stirred
Clock, the speed of stirring is 2500 revs/min, is discharged as component A, and viscosity is 2800mPas；Adjust respectively
The temperature of whole component A and Isocynate3 is put into the component A with Isocynate3 to 21 DEG C and 18 DEG C
Case bubble machine is stirred 20 seconds, and in being poured into 30 DEG C of mould, ripening is molded after 25 minutes, obtains institute of the present invention
The polyurethane foam stated；The polyurethane foam room temperature is placed into 30 hours afterwards, mechanical property is tested.
Embodiment 3
Proportioning raw materials according to embodiment 3 described in table 1 are implemented, and implementation steps are same as Example 2, its
In, component A viscosity is 1600mPas.
Embodiment 4
Under room temperature, component A raw material is put in reactor successively, using high shear agitation device 8 points are stirred
Clock, the speed of stirring is 2500 revs/min, is discharged as component A, and viscosity is 1900mPas；Adjust respectively
The temperature of whole component A and Isocynate2 is put into the component A with Isocynate2 to 24 DEG C and 18 DEG C
Case bubble machine is stirred 20 seconds, and in being poured into 30 DEG C of mould, ripening is molded after 26 minutes, obtains institute of the present invention
The polyurethane foam stated；The polyurethane foam room temperature is placed into 30 hours afterwards, mechanical property is tested.
Embodiment 5
Under room temperature, component A raw material is put in reactor successively, using high shear agitation device 12 points are stirred
Clock, the speed of stirring is 2200 revs/min, is discharged as component A, and viscosity is 1900mPas；Adjust respectively
The temperature of whole component A and Isocynate4 is put into the component A with Isocynate4 to 22 DEG C and 18 DEG C
Case bubble machine is stirred 21 seconds, and in being poured into 33 DEG C of mould, ripening is molded after 25 minutes, obtains institute of the present invention
The polyurethane foam stated；The polyurethane foam room temperature is placed into 30 hours afterwards, mechanical property is tested.
Embodiment 6
Under room temperature, component A raw material is put in reactor successively, using high shear agitation device 10 points are stirred
Clock, the speed of stirring is 2000 revs/min, is discharged as component A, and viscosity is 1100mPas；Adjust respectively
The temperature of whole component A and Isocynate3 is put into the component A with Isocynate3 to 20 DEG C and 22 DEG C
Case bubble machine is stirred 20 seconds, and in being poured into 35 DEG C of mould, ripening is molded after 22 minutes, obtains institute of the present invention
The polyurethane foam stated；The polyurethane foam room temperature is placed into 30 hours afterwards, mechanical property is tested.
Comparative example 1
Proportioning raw materials according to comparative example 1 described in table 1 are implemented, and implementation steps are same as Example 1.
Comparative example 2
Proportioning raw materials according to comparative example 3 described in table 1 are implemented, and implementation steps are same as Example 3.
In claims of the present invention and description, polyether glycol composition A and modified isocyanate are pre-
Although the preparation of polymers B is sequential in narration, the order in this narration is not restricted
Condition, because the order of the preparation regardless of both, technical scheme is substantially the same.
Obtained foam carries out cutting out sample test, wherein method for testing air permeability according to ASTM and GB standards
With reference to ASTM D6226-05《The standard test method of the open pore chamber content of rigid cellular plastics》, institute's total
According to the opening that can directly characterize polyurethane foamed material, there is material high opening rate to represent that it has preferably
Breathability.
The each reactive component formula of polyurethane foam of the embodiment of table 1 and comparative example is with transitivity contrast
Index is that [NCO] is poly- with described in isocyanate index, i.e. modified isocyanate prepolymer B in table 1
The mol ratio of [OH] in ethoxylated polyhydric alcohol compositionss A.
By embodiment 1 and comparative example 1 pair, when embodiment 4,5 is contrasted as can be seen that adopting with comparative example 2
With the polyurethane foam prepared by formula, the regulation and control of each component ratio and preparation method in scope of the present invention
Foam material, under conditions of with excellent mechanical performances, while having highly-breathable, low permanent compression set concurrently
With the aspect characteristic of low-density three.
Claims (11)
1. a kind of polyurethane foamed material, it is characterised in that by polyether glycol composition A and modified isocyanide
Acid esters prepolymer B reactions are obtained, and [NCO] group is more with the polyethers in the modified isocyanate prepolymer B
The mol ratio of [OH] group in first alcohol composition A is 1.02-1.2:1；It is preferred that 1.06-1.15:1.
2. polyurethane foamed material according to claim 1, it is characterised in that the polyether polyol group
Compound A, including：
(a) admixtured polyether polyhydric alcohol, including：Polyether polyol (1), its average functionality is 2-4, and number is equal
Molecular weight is 2000-8000, preferred 4000-6000, and its ethylene oxide content is 10-20wt%, preferably
13-17wt%；Optional polyether polyol (2), is obtained by styrene, acrylonitrile compolymer graft modification, Gu
Content is 20-45wt%, and its average functionality is 2-4, and number-average molecular weight is 2000-8000, its oxirane
Content is 10-20wt%；Polyether polyol (3), its average functionality is 2-4, and number-average molecular weight is 2000-8000,
It is preferred that 4000-6000, its ethylene oxide content is 50-100wt%, preferred 70-100wt%.
3. polyurethane foamed material according to claim 2, it is characterised in that with (a) admixtured polyether
The weight meter of polyhydric alcohol, wherein, the content of polyether polyol (1) is 20-99wt%, preferred 30-80wt%,
The content of polyether polyol (2) is 0-75wt%, preferred 15-65wt%, and the content of polyether polyol (3) is 1-8
Wt%, preferred 2-5wt%.
4. the polyurethane foamed material according to Claims 2 or 3, it is characterised in that the polyether polyols
Alcohol composition A, also includes：
(b) composite assistants, including：The foaming agent of 1-3 weight portions, the catalyst of 0.2-1 weight portions, 2-10 weights
The chain extender of amount part and inorganic filler and the mill base of 0-5 weight portions of 0-20 weight portions；
By weight, (a) the admixtured polyether polyhydric alcohol:(b) composite assistants=100:3.2-39.
5. the polyurethane foamed material according to any one of claim 1-4, it is characterised in that described to change
Property isocyanate prepolymer B, its NCO content be 16-28wt%, preferred 18-24wt%, including：
C the content of () urethane modified isocyanate is 60-99wt%, preferred 70-98wt%, with described modified different
The gross weight meter of cyanate prepolymer B, the urethane modified isocyanate is by polyhydric alcohol (c1) and isocyanates (c2)
Reaction is obtained, and polyhydric alcohol (c1) average functionality is 2-3；
D the content of () Carbodiimide-Modified isocyanates is 1-40wt%, preferred 2-30wt%, changed with described
The gross weight meter of property isocyanate prepolymer B.
6. polyurethane foamed material according to claim 5, it is characterised in that described polyhydric alcohol (c1)
Comprising following component：
E () dihydroxylic alcohols, account for the 0-30wt% of polyether polyol (c1) gross weight, preferred 1-20wt%, the binary
The preferred diglycol of alcohol, dipropylene glycol, 1,2- Propylene Glycol, 1,3- Propylene Glycol, 1,4- butanediols, 1,3-
One or more in butanediol, tripropylene glycol；
F () polyether polyol, accounts for the 10-60wt% of polyether polyol (c1) gross weight, preferred 20-50wt%,
Average functionality 2-3, number-average molecular weight is 100-12000, preferred 1000-11000, by oxirane and ring
One kind or its combination in Ethylene Oxide is formed through ring-opening polymerisation；
G () polyether polyol, accounts for the 30-90wt% of polyether polyol (c1) gross weight, preferred 40-80wt%,
Average functionality is 2-3, and number-average molecular weight is 2000-12000, preferred 4000-10000, by expoxy propane Jing
Cross ring-opening polymerisation to form.
7. polyurethane foamed material according to claim 6, it is characterised in that the polyether polyol group
Compound A, viscosity is 1000-3000mPas, preferred 1200-2000mPas；The modified isocyanate is pre-
Polymers B, viscosity is 80-699mPas, preferred 100-450mPas.
8. polyurethane foamed material according to claim 5, it is characterised in that the isocyanates (c2)
Selected from degree of functionality be the aliphatic of 2-6, one or more of cycloaliphatic and aromatic isocyanate, preferred first
Phenylene diisocyanate and/or methyl diphenylene diisocyanate, more preferably diphenyl methane -4,4 '-diisocyanate
With diphenyl methane -2, the mixture of 4 '-diisocyanate, wherein, with the gross weight meter of isocyanates (c2), institute
Diphenyl methane -4 are stated, the content of 4 '-diisocyanate is 90-100wt%, preferred 95-99wt%.
9. the polyurethane foamed material according to any one of claim 1-8, it is characterised in that described
Polyurethane foamed material density is 80-160kg/m3；The ASKERC hardness of the polyurethane foamed material is
10-40, percent opening is 90-100% according to ASTM D6226-05 standard testings, Compression Set according to
ASTMD-395-B standard testings are 2-10%.
10. the preparation method of the polyurethane foamed material any one of a kind of claim 1-9, its feature
It is to comprise the following steps：
(1) admixtured polyether polyhydric alcohol (a) and composite assistants (b) are mixed to get into the polyether polyol by stirring
Compositionss A, wherein, whipping temp is controlled at 5-50 DEG C, preferred 30-45 DEG C；
(2) described polyether polyol (c1) is mixed with isocyanates (c2), mixing temperature is controlled at 50-100 DEG C,
It is preferred that 60-85 DEG C, obtain urethane modified isocyanate；The temperature of urethane modified isocyanate is controlled at 30-70 DEG C,
It is preferred that 40-60 DEG C, add Carbodiimide-Modified isocyanates to stir in urethane modified isocyanate,
Obtain the modified isocyanate prepolymer B；
(3) by step (1) gained polyether glycol composition A and step (2) gained modified isocyanate prepolymer B
Hybrid reaction obtains the polyurethane foamed material；
Wherein, step (3) mixture is during reaction, in the presence of liquid condition, temperature control
Make at 15-25 DEG C, preferred 18-22 DEG C.
11. polyurethane foamed materials or claim 10 side of preparation according to any one of claim 1-9
Polyurethane foamed material prepared by method is preparing the purposes of shoe pad.
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| CN108484859A (en) * | 2018-03-20 | 2018-09-04 | 泉州市安仕登鞋服有限公司 | It is a kind of can self-heating polyurethane insole preparation method |
| CN110183711A (en) * | 2019-05-18 | 2019-08-30 | 陈建飞 | One kind being used in casting type camouflage color colour mixture polyurathamc manufacture method of sole |
| CN111447851A (en) * | 2017-12-13 | 2020-07-24 | 巴斯夫欧洲公司 | Method for producing polyurethane foam shoe pad |
| CN113185666A (en) * | 2021-05-10 | 2021-07-30 | 广东足迹鞋业有限公司 | Shoe pad with good elasticity and manufacturing process |
| CN113527616A (en) * | 2021-06-21 | 2021-10-22 | 佳化化学科技发展（上海）有限公司 | Polyurethane common soft foam and preparation method thereof |
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| CN116265504A (en) * | 2021-12-16 | 2023-06-20 | 长华化学科技股份有限公司 | Modified isocyanate and preparation method and application thereof |
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| CN115054576A (en) * | 2022-06-22 | 2022-09-16 | 湖南幻影三陆零科技有限公司 | Single-component polyurethane foam film coating agent and preparation method and application thereof |
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