CN101831047A - Synthesis method of high-performance thermoplastic polyurethane elastomer - Google Patents
Synthesis method of high-performance thermoplastic polyurethane elastomer Download PDFInfo
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Abstract
The invention relates to a synthesis method of a high-performance thermoplastic polyurethane elastomer. The synthesis method comprises the following steps of: firstly, adding 0.005-0.1 mol of two or more than two different kinds of oligomer diol (polycaprolactone (PCL), polyethyleneglycol (PEG), polyoxytetramethylene (PTMG), polypropylene glycol (PPG), polyethylene glycol adipate (PEA) or poly hexamethylene adipate (PAA), and the like) and 0.01-0.1 mol of chain extender (C2-C18) to a three-neck flask to form a diol system; heating the diol system to 90-150 DEG C, dewatering in vacuum under the pressure of -85.5 MPa to -95.5 MPa for 1-5h; secondarily, adding 0.01-0.1 mol of vulcabond, increasing the temperature to 80-130 DEG C, reacting at a retained temperature for 1.5-2.5h; degassing and discharging to a die coated with a silicone release agent; and finally, aging reaction substances in the die at 60-150 DEG C for 5-20h; and then, exposing in air for 5-10 days to fully react. The invention has the advantages of low energy consumption, time saving, convenient processing and forming, low production cost and suitability for mass popularization.
Description
Technical field
The invention belongs to the synthesis technical field of polyurethane elastomer, particularly a kind of synthesis method of high-performance thermoplastic polyurethane elastomer.
Background technology
Urethane (PU) elastomerics is meant and contained more carbamate groups functional group (N hour-CO-O-) a class elastomer polymer on macromolecular main chain, it is typical segmented copolymer, usually carry out addition reaction with polyisocyanates earlier by oligomer polyol (polyethers or polyester), form with the chainextender prepared in reaction again.
In urethane (PU) elastomerics, because there is tangible micro phase separation structure in the uncompatibility of soft or hard section, wherein soft section provides elasticity mutually, and hard section plays mutually to strengthen and fills and crosslinked action.Owing to form ability and soft section of the long-chain and the deliquescent difference of the hard section of short chain of hydrogen bond between the polar character of carbamate groups, group, cause soft or hard section thermodynamics incompatible and produce microphase-separated, strong association forms many microcells together and is dispersed in the soft section phase matrix between the hard segment molecule.The urethane of so final formation (PU) material is not the random copolymers on the statistics, but the polymer chain of high-hard section content is arranged very much and be " mixture " of pure soft chain segment almost, and in the two-phase microcell that chemical bond connects, exist interactional hydrogen bond.The hard section effect of playing physical crosslinking point and increased activity filler in the soft segment base matter of rubbery state of strong polarity and hydrogen bond action arranged.
The polyurethane elastomer of existing method preparation is hot and humid, and severe radiation is exposed to the sun for a long time, and the application limitations that continues special conditionss such as solvent soaking is very big, takes place aging easily and degraded, influences its use properties.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of synthesis method of high-performance thermoplastic polyurethane elastomer, adopt two or more different types of polyvalent alcohol, adopt single stage method synthetic thermoplastic polyurethane elastomer, in chemical reaction, carry out the product pre-profiling, can carry out effective and reasonable control to every performance of product easily, can arbitrarily grasp the product that different performance requires, it is simple to have technical process, equipment energy consumption and production cost are low, the characteristics of stable performance.
" high-performance " of the present invention is meant that synthetic Polyurethane Thermoplastic Elastomer shore hardness is 50A～95A, tensile strength is 25～50MPa, elongation at break is 550～1100%, right-angle tearing load 70-300N, angle tear strength 50-335kN/m, compare with common dibasic alcohol product, have hydrolysis, anti-solvent, the higher characteristics of ageing-resistant performance.The high-performance thermoplastic polyurethane elastomer of the present invention's preparation has good ageing-resistant and degradation resistant performance hot and humid under the conditions such as severe radiation, have wide range of applications.
To achieve these goals, the technical solution used in the present invention is:
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer may further comprise the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be two or more different types of oligopolymer dibasic alcohol and the 0.005～0.1mol chainextender dibasic alcohol of 0.005～0.1mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; The dibasic alcohol system is heated to 90～150 ℃, and-95.5～-85.5MPa vacuum under pressure dehydration 1～5 hour and stirring, be cooled to then 50～80 ℃ standby;
Secondly, add the vulcabond of 0.01～0.1mol in the standby dibasic alcohol system after last step vacuum hydro-extraction, isocyanate index remains on 0.5-1.5, is warming up to 80～130 ℃ again, insulation reaction 1.5～2.5 hours; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould of last step is placed 60～150 ℃ of slakings 5～20 hours, and then be exposed in the air 120-240 hour, reach and react completely.
Said oligopolymer dibasic alcohol is polycaprolactone (PCL), polyoxyethylene glycol (PEG), polytetrahydrofuran (PTMG), polypropylene glycol (PPG), polyethylene glycol adipate (PEA) or poly-hexanodioic acid hexylene glycol ester (PAA) etc.; Said chainextender dibasic alcohol is that carbonatoms is C
2-C
18Dibasic alcohol.
The invention has the beneficial effects as follows:
One, the present invention has synthesized the novel high-performance Polyurethane Thermoplastic Elastomer by a kind of method of simple and fast.This method energy consumption is low, saves time, and machine-shaping is convenient, and is all applicable to this elastomerics to the method for all thermoplastics machine-shapings.Synthetic Polyurethane Thermoplastic Elastomer shore hardness is 50A～95A, and tensile strength is 25～50MPa, and elongation at break is 550～1100%, right-angle tearing load 70-300N, angle tear strength 50-335kN/m.The polyurethane elastomer of tensile strength, elongation at break, right-angle tearing load and the more single oligopolymer dibasic alcohol preparation of angle tear strength all has raising.
Two, the present invention has synthesized mechanical property, and the new polyurethane elastomer of high comprehensive performance is compared with common dibasic alcohol product and to have been improved hydrolysis, anti-solvent, performance such as ageing-resistant.
Three, the present invention adopts single stage method reaction synthesis of polyurethane elastomerics, two or more different types of oligopolymer dibasic alcohol and chainextender small molecules dibasic alcohol are formed the dibasic alcohol system that mixes, after adding isocyanic ester then, the back discharging stirs rapidly, but straight forming is to required goods, also can be made into pellet and carry out secondary processing, greatly reduce production cost, be suitable for large-scale promotion production.With dibasic alcohol system and vulcabond direct reaction, need not in the reaction process to add other main raw materials once more, shortened the reaction times greatly, reduced reaction cost.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail.
Embodiment one
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer may further comprise the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be the ethylene glycol of polycaprolactone (PCL), polyoxyethylene glycol (PEG) and the 0.01mol of 0.005mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; The dibasic alcohol system is heated to 90 ℃, and-85.5MPa vacuum under pressure dehydration 1 hour and stir, be cooled to then 50 ℃ standby;
Secondly, add the vulcabond of 0.01mol in the standby dibasic alcohol system after last step vacuum hydro-extraction, isocyanate index remains on 0.5, is warming up to 80 ℃ again, insulation reaction 2 hours; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould of last step is placed 70 ℃ of slakings 10 hours, and then be exposed in the air 120 hours, reach and react completely.
Embodiment two
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be polyoxyethylene glycol (PEG), polytetrahydrofuran (PTMG) and the 0.09molC8 dibasic alcohol of 0.06mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 95 ℃, and in-following the vacuum hydro-extraction of 92.5Mpa 2 hours and stir, be cooled to then 60 ℃ standby;
Secondly, add the 0.08mol vulcabond after vacuum hydro-extraction and in the dibasic alcohol system of cooling, isocyanate index remains on 0.8, is warming up to 120 ℃ again, 2 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould of last step is placed 80 ℃ of slakings 8 hours, and then be exposed in the air 120 hours and react completely to reach.
Embodiment three
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, at the capacity that agitator, thermometer are housed is the C18 dibasic alcohol that adds the polyethylene glycol adipate (PEA) that total amount is 0.012mol, poly-hexanodioic acid hexylene glycol ester (PAA) and 0.005mol in the there-necked flask of 500ml, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 90 ℃, and in-95.5Mpa vacuum under pressure dehydration 3 hours and stir, be cooled to then 80 ℃ standby;
Secondly, the vulcabond of adding 0.07mol after vacuum hydro-extraction and in the dibasic alcohol system of cooling, isocyanate index remains on 1.5, is warming up to 130 ℃ again, 2.5 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould in the last step is placed 150 ℃ of slakings 6 hours, and then be exposed in the air 192 hours and react completely to reach.
Embodiment four
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be the C5 dibasic alcohol of polytetrahydrofuran (PTMG), polypropylene glycol (PPG), polyethylene glycol adipate (PEA) and the 0.093mol of 0.1mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 95 ℃, and in-90.5Mpa vacuum under pressure dehydration 5 hours and stir, be cooled to then 50 ℃ standby;
Secondly, add the vulcabond of 0.086mol in the dibasic alcohol system after vacuum hydro-extraction, be warming up to 120 ℃ again, 2 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould in the last step is placed 60 ℃ of slakings 20 hours, and then be exposed in the air 144 hours and react completely to reach.
Embodiment five
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be polycaprolactone (PCL), polyoxyethylene glycol (PEG), the polytetrahydrofuran (PTMG) of polycaprolactone (PCL), polyoxyethylene glycol (PEG), polytetrahydrofuran (PTMG) and the 0.1mol of 0.005mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 150 ℃, and in-85.5Mpa vacuum under pressure dehydration 5 hours and stir, be cooled to then 70 ℃ standby;
Secondly, add the vulcabond of 0.1mol in the dibasic alcohol system after vacuum hydro-extraction, isocyanate index remains on 1.0, is warming up to 80 ℃ again, 1.5 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould in the last step is placed 60 ℃ of slakings 5 hours, and then be exposed in the air 240 hours and react completely to reach.
Embodiment six
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be the C10 dibasic alcohol of polyoxyethylene glycol (PEG), polytetrahydrofuran (PTMG), polypropylene glycol (PPG), polyethylene glycol adipate (PEA) and the 0.1mol of 0.05mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 150 ℃, and in-following the vacuum hydro-extraction of 95.5Mpa 3 hours and stir, be cooled to then 69 ℃ standby;
Secondly, add the vulcabond of 0.09mol in the dibasic alcohol system after vacuum hydro-extraction, be warming up to 120 ℃ again, 1.5 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould in the last step is placed 60 ℃ of slakings 20 hours, and then be exposed in the air 240 hours and react completely to reach.
Claims (7)
1. synthesis method of high-performance thermoplastic polyurethane elastomer may further comprise the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be two or more different types of oligopolymer dibasic alcohol and the 0.005～0.1mol chainextender dibasic alcohol of 0.005～0.1mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; The dibasic alcohol system is heated to 90～150 ℃, and-95.5～-85.5MPa vacuum under pressure dehydration 1～5 hour and stirring, be cooled to then 50～80 ℃ standby;
Secondly, add the vulcabond of 0.01～0.1mol in the standby dibasic alcohol system after last step vacuum hydro-extraction, isocyanate index remains on 0.5-1.5, is warming up to 80～130 ℃ again, insulation reaction 1.5～2.5 hours; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould of last step is placed 60～150 ℃ of slakings 5～20 hours, and then be exposed in the air 120-240 hour, reach and react completely;
Said oligopolymer dibasic alcohol is polycaprolactone (PCL), polyoxyethylene glycol (PEG), polytetrahydrofuran (PTMG), polypropylene glycol (PPG), polyethylene glycol adipate (PEA) or poly-hexanodioic acid hexylene glycol ester (PAA); Said chainextender dibasic alcohol is that carbonatoms is C
2-C
18Dibasic alcohol.
2. according to the said a kind of synthesis method of high-performance thermoplastic polyurethane elastomer of claim 1, it is characterized in that, may further comprise the steps:
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer may further comprise the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be the ethylene glycol of polycaprolactone (PCL), polyoxyethylene glycol (PEG) and the 0.01mol of 0.005mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; The dibasic alcohol system is heated to 90 ℃, and-85.5MPa vacuum under pressure dehydration 1 hour and stir, be cooled to then 50 ℃ standby;
Secondly, add the vulcabond of 0.01mol in the standby dibasic alcohol system after last step vacuum hydro-extraction, isocyanate index remains on 0.5, is warming up to 80 ℃ again, insulation reaction 2 hours; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould of last step is placed 70 ℃ of slakings 10 hours, and then be exposed in the air 120 hours, reach and react completely.
3. according to the said a kind of synthesis method of high-performance thermoplastic polyurethane elastomer of claim 1, it is characterized in that, may further comprise the steps:
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, be that to add total amount in the there-necked flask of 500ml be polyoxyethylene glycol (PEG), polytetrahydrofuran (PTMG) and the 0.09molC of 0.06mol at the capacity that agitator, thermometer are housed
8Dibasic alcohol is formed the dibasic alcohol system, and the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 95 ℃, and in-following the vacuum hydro-extraction of 92.5Mpa 2 hours and stir, be cooled to then 60 ℃ standby;
Secondly, add the 0.08mol vulcabond after vacuum hydro-extraction and in the dibasic alcohol system of cooling, isocyanate index remains on 0.8, is warming up to 120 ℃ again, 2 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould of last step is placed 80 ℃ of slakings 8 hours, and then be exposed in the air 120 hours and react completely to reach.
4. according to the said a kind of synthesis method of high-performance thermoplastic polyurethane elastomer of claim 1, it is characterized in that, may further comprise the steps:
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, be the C that adds the polyethylene glycol adipate (PEA) that total amount is 0.012mol, poly-hexanodioic acid hexylene glycol ester (PAA) and 0.005mol in the there-necked flask of 500ml at the capacity that agitator, thermometer are housed
18Dibasic alcohol is formed the dibasic alcohol system, and the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 90 ℃, and in-95.5Mpa vacuum under pressure dehydration 3 hours and stir, be cooled to then 80 ℃ standby;
Secondly, the vulcabond of adding 0.07mol after vacuum hydro-extraction and in the dibasic alcohol system of cooling, isocyanate index remains on 1.5, is warming up to 130 ℃ again, 2.5 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould in the last step is placed 150 ℃ of slakings 6 hours, and then be exposed in the air 192 hours and react completely to reach.
5. according to the said a kind of synthesis method of high-performance thermoplastic polyurethane elastomer of claim 1, it is characterized in that, may further comprise the steps:
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, be that to add total amount in the there-necked flask of 500ml be the C of polytetrahydrofuran (PTMG), polypropylene glycol (PPG), polyethylene glycol adipate (PEA) and the 0.093mol of 0.1mol at the capacity that agitator, thermometer are housed
5Dibasic alcohol is formed the dibasic alcohol system, and the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 95 ℃, and in-90.5Mpa vacuum under pressure dehydration 5 hours and stir, be cooled to then 50 ℃ standby;
Secondly, add the vulcabond of 0.086mol in the dibasic alcohol system after vacuum hydro-extraction, be warming up to 120 ℃ again, 2 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould in the last step is placed 60 ℃ of slakings 20 hours, and then be exposed in the air 144 hours and react completely to reach.
6. according to the said a kind of synthesis method of high-performance thermoplastic polyurethane elastomer of claim 1, it is characterized in that, may further comprise the steps:
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, at the capacity that agitator, thermometer are housed is that to add total amount in the there-necked flask of 500ml be polycaprolactone (PCL), polyoxyethylene glycol (PEG), the polytetrahydrofuran (PTMG) of polycaprolactone (PCL), polyoxyethylene glycol (PEG), polytetrahydrofuran (PTMG) and the 0.1mol of 0.005mol, form the dibasic alcohol system, the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 150 ℃, and in-85.5Mpa vacuum under pressure dehydration 5 hours and stir, be cooled to then 70 ℃ standby;
Secondly, add the vulcabond of 0.1mol in the dibasic alcohol system after vacuum hydro-extraction, isocyanate index remains on 1.0, is warming up to 80 ℃ again, 1.5 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould in the last step is placed 60 ℃ of slakings 5 hours, and then be exposed in the air 240 hours and react completely to reach.
7. according to the said a kind of synthesis method of high-performance thermoplastic polyurethane elastomer of claim 1, it is characterized in that, may further comprise the steps:
A kind of synthesis method of high-performance thermoplastic polyurethane elastomer comprises the steps:
At first, be that to add total amount in the there-necked flask of 500ml be the C of polyoxyethylene glycol (PEG), polytetrahydrofuran (PTMG), polypropylene glycol (PPG), polyethylene glycol adipate (PEA) and the 0.1mol of 0.05mol at the capacity that agitator, thermometer are housed
10Dibasic alcohol is formed the dibasic alcohol system, and the content ratio between different types of oligopolymer dibasic alcohol without limits; Heat this system to 150 ℃, and in-following the vacuum hydro-extraction of 95.5Mpa 3 hours and stir, be cooled to then 69 ℃ standby;
Secondly, add the vulcabond of 0.09mol in the dibasic alcohol system after vacuum hydro-extraction, be warming up to 120 ℃ again, 1.5 hours insulation reaction time; Degassing back discharging is to the mould that scribbles silicone oil mold release agent;
At last, the reactant in the mould in the last step is placed 60 ℃ of slakings 20 hours, and then be exposed in the air 240 hours and react completely to reach.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558830A (en) * | 2012-02-10 | 2012-07-11 | 上海联景高分子材料有限公司 | Preparation method of transparent film-grade thermoplastic polyurethane elastomer |
| CN106034384A (en) * | 2015-01-19 | 2016-10-19 | 深圳市堃琦鑫华股份有限公司 | Component plugging method |
| CN108084400A (en) * | 2017-12-29 | 2018-05-29 | 美瑞新材料股份有限公司 | A kind of preparation method of high-performance thermoplastic polyurethane elastomer |
| CN109232856A (en) * | 2018-08-03 | 2019-01-18 | 山东诺威聚氨酯股份有限公司 | The preparation method of high highly-elastic urethane elastomer thoroughly |
| CN114057971A (en) * | 2020-08-05 | 2022-02-18 | 北京化工大学 | Thermoplastic polyurethane elastomer and preparation method thereof |
-
2010
- 2010-05-18 CN CN201010176295A patent/CN101831047A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558830A (en) * | 2012-02-10 | 2012-07-11 | 上海联景高分子材料有限公司 | Preparation method of transparent film-grade thermoplastic polyurethane elastomer |
| CN106034384A (en) * | 2015-01-19 | 2016-10-19 | 深圳市堃琦鑫华股份有限公司 | Component plugging method |
| CN106034384B (en) * | 2015-01-19 | 2019-07-05 | 深圳市堃琦鑫华股份有限公司 | A kind of plug-in method |
| CN108084400A (en) * | 2017-12-29 | 2018-05-29 | 美瑞新材料股份有限公司 | A kind of preparation method of high-performance thermoplastic polyurethane elastomer |
| CN108084400B (en) * | 2017-12-29 | 2020-08-04 | 美瑞新材料股份有限公司 | Preparation method of high-performance thermoplastic polyurethane elastomer |
| CN109232856A (en) * | 2018-08-03 | 2019-01-18 | 山东诺威聚氨酯股份有限公司 | The preparation method of high highly-elastic urethane elastomer thoroughly |
| CN109232856B (en) * | 2018-08-03 | 2021-04-09 | 山东一诺威聚氨酯股份有限公司 | Preparation method of high-permeability high-elasticity polyurethane elastomer |
| CN114057971A (en) * | 2020-08-05 | 2022-02-18 | 北京化工大学 | Thermoplastic polyurethane elastomer and preparation method thereof |
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Open date: 20100915 |