CN109265641A - Low temperature resistant low-density polyurethane soles article combination material and preparation method thereof - Google Patents
Low temperature resistant low-density polyurethane soles article combination material and preparation method thereof Download PDFInfo
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- CN109265641A CN109265641A CN201810731736.4A CN201810731736A CN109265641A CN 109265641 A CN109265641 A CN 109265641A CN 201810731736 A CN201810731736 A CN 201810731736A CN 109265641 A CN109265641 A CN 109265641A
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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
-
- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B13/00—Soles; Sole-and-heel integral units
- A43B13/02—Soles; Sole-and-heel integral units characterised by the material
- A43B13/04—Plastics, rubber or vulcanised fibre
-
- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4202—Two or more polyesters of different physical or chemical nature
-
- 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)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Footwear And Its Accessory, Manufacturing Method And Apparatuses (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention belongs to technical field of polyurethane elastomer, it is specifically related to a kind of low temperature resistant low-density polyurethane soles article combination material and preparation method thereof.The combination material is made of the component A and B component of weight fraction ratio A:B=100:65-105, and component A raw material composition is as follows: polyester ether polylol A, polyester polyol B, polyether polymer polyalcohol C, chain extender, crosslinking agent, foam stabilizer, catalyst and foaming agent；B component is polyalcohol modified isocyanates, NCO content 18-25%.Low temperature resistant low-density polyurethane soles are prepared using combination provided by the invention material, effectively solve the problems, such as polyester and polyethers intersolubility in A material, the polyether polymer polyalcohol of addition can be purchased to obtain with reasonable prices on the market, without increasing cost of material；The low-density sole that combination material according to the invention is prepared has excellent resistance to low temperature.
Description
Technical field
The invention belongs to technical field of polyurethane elastomer, are specifically related to a kind of low temperature resistant low-density polyurethane soles system
Product combination material and preparation method thereof.
Background technique
Polyurethane material has superior physical mechanical property, acid-alkali-corrosive-resisting performance, high-mechanic performance and hardness model
The advantages that enclosing width has become one of the mainstay material in sole market, is now widely used in production playshoes, sport footwear, safety
Shoes and sandals etc..PU body raw material for producing sole can be divided into polyester-type and polyether-type two by polyalcohol used
Class.Most of polyurethane shoe bottom materials account for about the 80% of polyurethane shoe material market based on polyester-type currently on the market.Polyester type shoes
The characteristics of bottom be good mechanical property but intolerant to hydrolysis and poor performance at low temperatures, polyether-type sole bad mechanical property still have preferably
Hydrolysis and lower temperature resistance.Using polyester, there are intersolubilities with polyethers physical mixed profile material.
Cost can be substantially reduced by reducing polyurethane shoe-sole density, and can provide lighter dress experience, but
It is to reduce the problems such as density would generally bring the decline of mechanical performance, sole dimensions stability is poor.It can be with for polyester-type footwear material
Method by adding Polyester Polymer Polyols is improved, but polyester type polymer polyatomic alcohol viscosity is higher, produces work
The more complex higher cost of skill, currently on the market without the suitably universal product of price；If being added in polyester bodies raw material poly-
Ether polymer polyalcohol can then have polyester and polyethers intersolubility difference.
Summary of the invention
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of low temperature resistant low-density polyurethane soles product group
Close material.Combination material of the invention can effectively solve the problems, such as A material in polyester and polyethers intersolubility, and without increase raw material at
This, the low-density sole that combination material according to the invention is prepared has excellent resistance to low temperature；Present invention simultaneously provides
Preparation method.
Low temperature resistant low-density polyurethane soles article combination material of the present invention, the combination material is by weight fraction ratio A:B
The component A and B component of=100:65~105 form, in which:
For component A in terms of mass fraction, raw material composition is as follows:
B component is polyalcohol modified isocyanates, NCO content 18-25%；In terms of mass fraction, raw material is formed such as
Under:
0~10 part of polyester ether polylol A
15~25 parts of polyester polyol D
75~85 parts of isocyanates.
Wherein:
Polyester ether polylol A is by small molecule dihydric alcohol, small molecule polyether polyol and adipic acid by polycondensation reaction system
, number-average molecular weight 1000-4000.
Small molecule dihydric alcohol is the mixture of one or more of ethylene glycol, diethylene glycol or 1,4-butanediol；Small point
Sub- polyether polyol is the polyether polyol that degree of functionality is 1.9-2.2, molecular weight is 500-1500.
Polyester polyol B be one or more of ethylene glycol, diethylene glycol or 1,4-butanediol mixture and oneself two
One or both of acid or terephthalic acid (TPA) are made by polycondensation reaction, number-average molecular weight 1000-3500；Polyether polymer
It is 1.9-2.2 that polyalcohol C, which is with degree of functionality, polyether polyol of the molecular weight for 500-2500 is basic polyethers, with styrene or
The graft copolymerization of one or both of acrylonitrile is made.
Chain extender be ethylene glycol (EG), diglycol (DEG), 1,4- butanediol (1,4-BG), 1,3- propylene glycol (1,
3-PDO), one or more of dipropylene glycol (DPG) or 1,6-HD；Crosslinking agent is triethanolamine (TEA), diethyl
One or more of hydramine (DEOA), glycerol or trimethylolpropane.
Foam stabilizer uses polysiloxanes-oxyalkylene block copolymer；Catalyst in component A is tertiary amine catalyst；
Foaming agent is water.
Foam stabilizer is DC-193 (US Air gasification chemical product Co., Ltd)；Tertiary amine catalyst is triethylene diamine.
Isocyanates in B component is pure MDI, Carbodiimide-Modified MDI, MDI-50 or polymeric MDI (being commonly called as thick MDI)
One of or it is a variety of；Polyester polyol D is the mixture of one or more of ethylene glycol, diethylene glycol or 1,4-butanediol
It is made with adipic acid by polycondensation reaction, number-average molecular weight 1000-2500.
The preparation method of low temperature resistant low-density polyurethane soles article combination material of the present invention, specifically includes following step
It is rapid:
(1) preparation of component A material: by the polyester ether polylol A measured, polyester polyol B, polyether polymer polyalcohol
C, in component A ratio investment reaction kettle under chain extender, crosslinking agent, foam stabilizer, catalyst and foaming agent room temperature, stirring 1-2 is small
When after up to component A；
(2) preparation of B component material: anti-by being put under polyester ether polylol A and polyester polyol D room temperature based on formula ratio
It answers in kettle, stirring is warming up to 90-110 DEG C, and dehydration degassing 2-3 hours, are then cooled to 50 DEG C, metering is added under vacuum condition
Isocyanates, 80-85 DEG C after reaction 2-3 hours up to B component；
(3) in use, A, B component are injected separately into low-pressure casting machine batch can, compare A:B=100:65 according to parts by weight
~105 ratio injects 40-60 DEG C of mold after mixing component A and B component at head, die sinking obtains low temperature resistant after 4-5min
The sole of low-density.
Compared with the prior art, the present invention has the following beneficial effects:
Using combination provided by the invention material prepare low temperature resistant low-density polyurethane soles, effectively solve A material in polyester with
Polyethers intersolubility problem both containing polyester segment or had contained polyether segment mainly in polyether ester, with polyester and polyethers have compared with
Good intermiscibility, the polyether polymer polyalcohol of addition are purchased to obtain with reasonable prices on the market, without increase raw material at
This；The low-density sole that combination material according to the invention is prepared has excellent resistance to low temperature.
Specific embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
Low temperature resistant low-density polyurethane soles article combination material described in the present embodiment 1, the combination material is by weight fraction ratio
The component A and B component of A:B=100:65 forms, in which:
For component A in terms of mass fraction, raw material composition is as follows:
B component is polyalcohol modified isocyanates, NCO content 25%；In terms of mass fraction, raw material composition is as follows:
0 part of polyester ether polylol A
15 parts of polyester polyol D
85 parts of isocyanates.
Component A material: with polyether polyol, ethylene glycol, diethylene glycol and the adipic acid that molecular weight is 500, degree of functionality is 1.9
The polyester ether polylol A that number-average molecular weight is 2500 is made by polycondensation reaction；Spent glycol, diethylene glycol and 1,4-butanediol
In with adipic acid by polycondensation reaction be made number-average molecular weight be 1000 polyester polyol B；With degree of functionality for 2.2, molecular weight
Polyether polyol for 1500 is basic polyethers, and polyether polymer polyalcohol C is made with graft polymerization.Chain extender is second
Glycol, diglycol and 1,4- butanediol；Crosslinking agent is triethanolamine and diethanol amine；Foam stabilizer is DC-193, catalysis
Agent is triethylene diamine and foaming agent water.Each raw material in formula is proportionally mixed, is stirred 1 hour, sampling is tested
Up to component A after qualification.
B component material: it is 2500 that number-average molecular weight, which is made, by polycondensation reaction with adipic acid in spent glycol, 1,4-butanediol
Polyester polyol D；Isocyanates is pure MDI, Carbodiimide-Modified MDI and MDI-50.It will be above-mentioned poly- based on formula ratio
It is put into reaction kettle under ester polyol D room temperature, stirring is warming up to 100 DEG C, and dehydration degassing 2 hours, then cool down under vacuum condition
When to 50 DEG C, the isocyanates of metering is added, is reacted at 80 DEG C 2 hours, after the assay was approved up to B component.
In use, A material and B material are injected separately into low-pressure casting machine batch can, A is expected according to the ratio of A:B=100:65
It is injected in mold after being mixed at the head with B material, mold temperature is maintained at 50 DEG C, and die sinking i.e. molding after five minutes obtains density and is
330kg/m3Sole, sole is placed at room temperature for test size stability and resistance to low temperature after 72h, as a result cubical contraction≤
0.3%, at -30 DEG C sole carry out 90 ° of warping strength bendings experiments 50,000 times it is flawless.
Embodiment 2
Low temperature resistant low-density polyurethane soles article combination material described in the present embodiment 2, the combination material is by weight fraction ratio
The component A and B component of A:B=100:85 forms, in which:
For component A in terms of mass fraction, raw material composition is as follows:
B component is polyalcohol modified isocyanates, NCO content 21%；In terms of mass fraction, raw material composition is as follows:
4 parts of polyester ether polylol A
16 parts of polyester polyol D
80 parts of isocyanates.
Component A material: with polyether polyol, diethylene glycol and the adipic acid that molecular weight is 1500, degree of functionality is 2.2 by contracting
The polyester ether polylol A that number-average molecular weight is 4000 is made in poly- react；Spent glycol, diethylene glycol and adipic acid are anti-by polycondensation
The polyester polyol B that number-average molecular weight is 3500 should be made；It is with the polyether polyol that degree of functionality is 1.9, molecular weight is 2500
Basic polyether is graft-polymerized with the mixture of styrene and acrylonitrile and polyether polymer polyalcohol C is made.Chain extender is second two
Alcohol, dipropylene glycol and 1,6-HD；Crosslinking agent is glycerol and trimethylolpropane；Foam stabilizer is DC-193, catalyst
For triethylene diamine and foaming agent water.Each raw material in formula is proportionally mixed, is stirred 2 hours, conjunction of testing is sampled
Up to component A after lattice.
B component material: more for 1000 polyester by the obtained number-average molecular weight of polycondensation reaction with 1,4-butanediol and adipic acid
First alcohol D；Isocyanates is Carbodiimide-Modified MDI and MDI-50.By the above-mentioned polyester ether polylol A based on formula ratio and gather
It is put into reaction kettle under ester polyol D room temperature, stirring is warming up to 100 DEG C, and dehydration degassing 2 hours, then cool down under vacuum condition
When to 50 DEG C, the isocyanates of metering is added, is reacted at 80 DEG C 2 hours, after the assay was approved up to B component.
In use, A material and B material are injected separately into low-pressure casting machine batch can, A is expected according to the ratio of A:B=100:85
It is injected in mold after being mixed at the head with B material, mold temperature is maintained at 55 DEG C, and die sinking i.e. molding after five minutes obtains density and is
290kg/m3Sole, sole is placed at room temperature for test size stability and resistance to low temperature after 72h, as a result cubical contraction≤
0.8%, at -30 DEG C sole carry out 90 ° of warping strength bendings experiments 50,000 times it is flawless.
Embodiment 3
Low temperature resistant low-density polyurethane soles article combination material described in the present embodiment 3, the combination material is by weight fraction ratio
The component A and B component of A:B=100:105 forms, in which:
For component A in terms of mass fraction, raw material composition is as follows:
B component is polyalcohol modified isocyanates, NCO content 18%；In terms of mass fraction, raw material composition is as follows:
10 parts of polyester ether polylol A
15 parts of polyester polyol D
75 parts of isocyanates.
Component A material: with molecular weight is 1000, degree of functionality is 2.0 polyether polyol, diethylene glycol and 1,4-butanediol with
The polyester ether polylol A that number-average molecular weight is 2500 is made by polycondensation reaction for adipic acid；In spent glycol, 1,4-butanediol with
The polyester polyol B that number-average molecular weight is 2000 is made by polycondensation reaction in adipic acid, terephthalic acid (TPA)；Be 2.0 with degree of functionality,
The polyether polyol that molecular weight is 500 is basic polyethers, and polyether polymer polyalcohol C is made with graft polymerization.Chain extension
Agent is diglycol, 1,4- butanediol and dipropylene glycol；Crosslinking agent is diethanol amine and glycerol；Foam stabilizer is DC-
193, catalyst is triethylene diamine and foaming agent water.Each raw material in formula is proportionally mixed, stirs 1.5 hours, takes
Sample is tested after qualification up to component A.
B component material: spent glycol, diethylene glycol and 1,4-butanediol and adipic acid are made by polycondensation reaction and count equal molecule
The polyester polyol D that amount is 2000；Isocyanates is pure MDI and Carbodiimide-Modified MDI.It will be above-mentioned poly- based on formula ratio
It is put into reaction kettle under ether-ether polyalcohol A and polyester polyol D room temperature, stirring is warming up to 100 DEG C, and degassing is dehydrated under vacuum condition
2 hours.When being then cooled to 50 DEG C, the isocyanates of metering is added, is reacted at 80 DEG C 2 hours, after the assay was approved up to B group
Point.
In use, A material and B material are injected separately into low-pressure casting machine batch can, A is expected according to the ratio of A:B=100:105
It is injected in mold after being mixed at the head with B material, mold temperature is maintained at 50 DEG C, and die sinking i.e. molding after five minutes obtains density and is
305kg/m3Sole, sole is placed at room temperature for test size stability and resistance to low temperature after 72h, as a result cubical contraction≤
0.5%, at -30 DEG C sole carry out 90 ° of warping strength bendings experiments 50,000 times it is flawless.
Claims (9)
1. a kind of low temperature resistant low-density polyurethane soles article combination material, it is characterised in that: the combination material is by weight fraction ratio A:B
The component A and B component of=100:65~105 form, in which:
For component A in terms of mass fraction, raw material composition is as follows:
B component is polyalcohol modified isocyanates, NCO content 18-25%；In terms of mass fraction, raw material composition is as follows:
0~10 part of polyester ether polylol A
15~25 parts of polyester polyol D
75~85 parts of isocyanates.
2. low temperature resistant low-density polyurethane soles article combination material according to claim 1, it is characterised in that: polyether ester is more
First alcohol A is to be made by small molecule dihydric alcohol, small molecule polyether polyol and adipic acid by polycondensation reaction, and number-average molecular weight is
1000-4000。
3. low temperature resistant low-density polyurethane soles article combination material according to claim 2, it is characterised in that: small molecule two
First alcohol is the mixture of one or more of ethylene glycol, diethylene glycol or 1,4-butanediol；Small molecule polyether polyol is official
The polyether polyol that energy degree is 1.9-2.2, molecular weight is 500-1500.
4. low temperature resistant low-density polyurethane soles article combination material according to claim 1, it is characterised in that: polyester polyols
Alcohol B is in the mixture and adipic acid or terephthalic acid (TPA) of one or more of ethylene glycol, diethylene glycol or 1,4-butanediol
One or two by polycondensation reaction be made, number-average molecular weight 1000-3500；Polyether polymer polyalcohol C is with function
Degree is 1.9-2.2, the polyether polyol that molecular weight is 500-2500 is basic polyethers, with one of styrene or acrylonitrile or
Two kinds of graft copolymerizations are made.
5. low temperature resistant low-density polyurethane soles article combination material according to claim 1, it is characterised in that: chain extender is
One of ethylene glycol, diglycol, 1,4- butanediol, 1,3- propylene glycol, dipropylene glycol or 1,6-HD or
It is several；Crosslinking agent is one or more of triethanolamine, diethanol amine, glycerol or trimethylolpropane.
6. low temperature resistant low-density polyurethane soles article combination material according to claim 1, it is characterised in that: foam stabilizer is adopted
With polysiloxanes-oxyalkylene block copolymer；Catalyst is tertiary amine catalyst；Foaming agent is water.
7. low temperature resistant low-density polyurethane soles article combination material according to claim 6, it is characterised in that: foam stabilizer is
DC-193；Tertiary amine catalyst is triethylene diamine.
8. low temperature resistant low-density polyurethane soles article combination material according to claim 1, it is characterised in that: in B component
Isocyanates be one of pure MDI, Carbodiimide-Modified MDI, MDI-50 or polymeric MDI or a variety of；Polyester polyol D
It is that the mixture of one or more of ethylene glycol, diethylene glycol or 1,4-butanediol and adipic acid are made by polycondensation reaction,
Number-average molecular weight is 1000-2500.
9. a kind of preparation method of low temperature resistant low-density polyurethane soles article combination material described in claim 1, feature exist
In: specifically includes the following steps:
(1) preparation of component A material: by the polyester ether polylol A measured, polyester polyol B, polyether polymer polyalcohol C, expand
It is put into reaction kettle under chain agent, crosslinking agent, foam stabilizer, catalyst and foaming agent room temperature in component A ratio, after stirring 1-2 hours
Up to component A；
(2) preparation of B component material: reaction kettle will be put under polyester ether polylol A and polyester polyol D room temperature based on formula ratio
In, stirring is warming up to 90-110 DEG C, and dehydration degassing 2-3 hours, are then cooled to 50 DEG C, the isocyanide of metering is added under vacuum condition
Acid esters, 80-85 DEG C after reaction 2-3 hours up to B component；
(3) in use, A, B component are injected separately into low-pressure casting machine batch can, according to parts by weight than A:B=100:65~
105 ratio injects 40-60 DEG C of mold after mixing component A and B component at head, die sinking obtains low temperature resistant low after 4-5min
The sole of density.
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| CN111875785A (en) * | 2020-08-04 | 2020-11-03 | 湖南恒旺新材料科技有限公司 | Polyether ester multi-block copolymerized dihydric alcohol, synthesis method and application of reactive hot melt adhesive |
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Application publication date: 20190125 |