CN104829799A - Preparation method of high-temperature-resistant puncture-resistant polyurethane elastomer - Google Patents
Preparation method of high-temperature-resistant puncture-resistant polyurethane elastomer Download PDFInfo
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- CN104829799A CN104829799A CN201510243704.6A CN201510243704A CN104829799A CN 104829799 A CN104829799 A CN 104829799A CN 201510243704 A CN201510243704 A CN 201510243704A CN 104829799 A CN104829799 A CN 104829799A
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- polyurethane elastomer
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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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
-
- 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
- C08G18/73—Polyisocyanates or polyisothiocyanates acyclic
-
- 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
- C08G2380/00—Tyres
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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 invention relates to a preparation method of a high-temperature-resistant puncture-resistant polyurethane elastomer. The preparation method comprises the following steps: carrying out two-step solution polymerization on polycarbonate dibasic alcohol, diisocyanate and a chain extender to obtain the polyurethane elastomer; pressing the synthesized polyurethane elastomer into a sheet at 170 DEG C, carrying out cold pressing at room temperature under the pressure of 1.0 MPa for 60 seconds, putting the mold filled with the polyurethane elastomer in a 100-140-DEG C vacuum drying oven, carrying out vacuum curing for 16-24 hours, taking out, annealing in air to cool to room temperature, and standing at room temperature for 5-8 days. The prepared polyurethane elastomer has the advantages of favorable mechanical properties, favorable dynamic mechanical properties at high temperature and excellent puncture resistance, and is suitable for tires, rubber rollers and other materials used under high stress-strain conditions.
Description
Technical field
The invention belongs to polyurethane elastomer field, particularly the high temperature resistant puncture resistant method for preparing polyurethane elastic body of one.
Background technology
Polyurethane elastomer is soft section with polyvalent alcohol, is hard section with polyisocyanates and small molecule chain extender, because of the thermodynamics uncompatibility of soft or hard section, presents a kind of performance between rubber and plastics.Its property regulation scope is wide, have excellent mechanical property and wear resistance, good chemical-resistant reagent and the performance such as low temperature resistant.But polyurethane elastomer at high temperature material internal structure is easily destroyed, when generally using more than 80 DEG C, the over-all properties of material declines a lot.Elastic polyurethane is through being usually used on national defense industry and engineering tyre in addition, and working conditions is severe, and the puncture resistant Capability Requirement for polyurethane elastomer is higher, but is not seen in and report for the research of puncture resistant polyurethane elastomer.
Aliphatic isocyanates and polycarbonate diol is chosen in the present invention.Reason is, isocyanic ester and polyvalent alcohol are acyclic straight on the one hand, and segment is soft, is easy to form crystallization, can promotes the mechanical property of material.And the hard section crystalline melt temperature serving as filler effect is higher, make polyurethane elastomer at high temperature also can keep higher mechanical property, resistance to elevated temperatures is excellent.In addition, by regulation and control heat-treatment temperature range and heat treatment time, can regulate and control crystal property, obtaining high thermal resistance can better polyurethane elastomer.On the other hand polycarbonate diol oxygen element content is high, and with to be all aliphatic isocyanate-compatible good, soft or hard is intersegmental can form hydrogen bond, and Dynamic loss modulus is higher, when being subject to high speed impact effect, and can loss major part energy.The second-order transition temperature of soft section is close to room temperature simultaneously, and temperature range is wide, when making polyurethane elastomer be subject to the impact of sharp objects, in moment with vitreous state distortion, can promote the puncture resistant ability of polyurethane elastomer.
Summary of the invention
The object of this invention is to provide a kind of high temperature resistant puncture resistant method for preparing polyurethane elastic body, the mechanics of elastic bodies perfect performance obtained, dynamic properties keeps better at a higher temperature, and puncture resistance is excellent, the material such as tire, rubber roll used under being applicable to strong stress-strain condition.
A kind of high temperature resistant puncture resistant method for preparing polyurethane elastic body, this polyurethane elastomer is formed by two-step approach solution polymerization by PCDL, vulcabond and chainextender, product tabletted under the condition of 170 DEG C of synthesis, then at room temperature to cold pressing 60s with the pressure of 1.0MPa, finally the mould that polymkeric substance is housed is placed on vacuum cooked 16-24h in the vacuum drying oven of 100-140 DEG C, after taking-up, room temperature is down in annealing in atmosphere, and at room temperature places 5-8 days.
Described colding pressing makes material produce cold crystallization in fast cooling process, and crystallization affects mechanical property and the high-temperature behavior of material.
Described vacuum cooked temperature is more than order-disorder transition temperature, below melt temperature, concrete within the scope of 100-140 DEG C.
The described vacuum cooked time is 16-24h, and the anneal in this operation later stage in addition, all for making material crystalline structure more perfect.
Described PCDL is that manufacturer is Nippon Polyurethane Industry Co., Ltd. by carbonic ether and 1,6-hexylene glycol Reactive Synthesis.The number-average molecular weight of PCDL is generally 500-5000, is preferably 600-4000, more preferably 1000-3000.
Described vulcabond is aliphatic hexamethylene diisocyanate (HDI), and chainextender is butyleneglycol.
The mol ratio of isocyano of the present invention and hydroxyl is 1-1.02.
A kind of high temperature resistant puncture resistant method for preparing polyurethane elastic body, the present invention utilizes two-step approach, reacts in DMF (DMF) solution.Massfraction is after dewatering at the vacuum tightness of PCDL at-0.1MPa of 68.6-70.5wt%, the temperature of 120 DEG C by the first step, mix with the vulcabond of 29.5-31.4wt%, react three hours in 70 DEG C of nitrogen atmospheres, make base polyurethane prepolymer for use as.Second step base polyurethane prepolymer for use as and butyleneglycol feed intake according to mass ratio 100:10.3-12.7, react two hours, put into 70 DEG C of vacuum drying oven vacuum dryings after resultant vacuum defoamation at 80 DEG C.Product tabletted under the condition of 170 DEG C of synthesis, then at room temperature to cold pressing 60s with the pressure of 1.0MPa, finally the mould that polymkeric substance is housed is placed on vacuum cooked 16-24h in the vacuum drying oven of 100-140 DEG C, after taking-up, room temperature is down in annealing in atmosphere, and at room temperature places 5-8 days.
The present invention's product used is commercially available prod.
Compared with modern technologies, this invention has following feature:
Polyurethane elastomer obtained by the present invention, Mechanical Properties of Products is excellent, and dynamic properties keeps better at a higher temperature, and puncture resistant ability is excellent, the material such as tire, rubber roll used under being applicable to strong stress-strain condition.
Embodiment
For making object of the present invention, technical scheme clearly, below in conjunction with specific embodiment, the present invention is described in detail, but do not limit the present invention in any form.Those of ordinary skill in the art can make various corresponding distortion according to the present invention, but these all should belong to protection scope of the present invention.
The method that the puncture resistant ability of film specifies according to USS ASTMD4833-07 is tested, and test rate is 300mm/min, and film thickness 2mm, diameter is greater than 50mm.
Embodiment 1
(1) be 2000 by molecular weight, massfraction is dewater at the vacuum tightness of PCDL at-0.1MPa of 70.5wt%, the temperature of 120 DEG C, then add the HDI of 29.5wt%, react three hours in 70 DEG C of nitrogen atmospheres, make base polyurethane prepolymer for use as.
(2) performed polymer and butyleneglycol feed intake according to mass ratio 100:12.7, react two hours, put into 70 DEG C of vacuum drying oven vacuum dryings after resultant vacuum defoamation under 80 DEG C of nitrogen atmospheres.
(3) product synthesized tabletted under the condition of 170 DEG C, then at room temperature to cold pressing 60s with the pressure of 1.0MPa, finally the mould that polymkeric substance is housed is placed on vacuum cooked 24h in the vacuum drying oven of 120 DEG C, after taking-up, room temperature is down in annealing in atmosphere, and at room temperature places 7 days.Its main performance index is in table 1.
Embodiment 2
(1) be 1000 by molecular weight, massfraction is dewater at the vacuum tightness of PCDL at-0.1MPa of 68.6wt%, the temperature of 120 DEG C, then add the HDI of 31.4wt%, react three hours in 70 DEG C of nitrogen atmospheres, make base polyurethane prepolymer for use as.
(2) performed polymer and butyleneglycol feed intake according to mass ratio 100:10.3, react two hours, put into 70 DEG C of vacuum drying oven vacuum dryings after resultant vacuum defoamation under 80 DEG C of nitrogen atmospheres.
(3) product synthesized tabletted under the condition of 170 DEG C, then at room temperature to cold pressing 60s with the pressure of 1.0MPa, finally the mould that polymkeric substance is housed is placed on vacuum cooked 16h in the vacuum drying oven of 140 DEG C, after taking-up, room temperature is down in annealing in atmosphere, and at room temperature places 6 days.Its main performance index is in table 1.
Embodiment 3
(1) be 2000 by molecular weight, massfraction is dewater at the vacuum tightness of PCDL at-0.1MPa of 70.0wt%, the temperature of 120 DEG C, then adds the HDI of 30.0wt%, reacts three hours in 70 DEG C of nitrogen atmospheres, make it mix, make base polyurethane prepolymer for use as.
(2) performed polymer and butyleneglycol feed intake according to mass ratio 100:12.6, react two hours, put into 70 DEG C of vacuum drying oven vacuum dryings after resultant vacuum defoamation under 80 DEG C of nitrogen atmospheres.
(3) material synthesized tabletted under the condition of 170 DEG C, then at room temperature to cold pressing 60s with the pressure of 1.0MPa, finally the mould that polymkeric substance is housed is placed on vacuum cooked 24h in the vacuum drying oven of 100 DEG C, after taking-up, room temperature is down in annealing in atmosphere, and at room temperature places 8 days.Its main performance index is in table 1.
Comparative example 1 and non-heat treated sample contrast
(1) be 2000 by molecular weight, massfraction is dewater at the vacuum tightness of PCDL at-0.1MPa of 70.5wt%, the temperature of 120 DEG C, then add the HDI of 29.5wt%, react three hours in 70 DEG C of nitrogen atmospheres, make base polyurethane prepolymer for use as.
(2) performed polymer and butyleneglycol feed intake according to mass ratio 100:12.7, react two hours, put into 70 DEG C of vacuum drying oven vacuum dryings after resultant vacuum defoamation under 80 DEG C of nitrogen atmospheres.
Comparative example 2 and polyether-type sample contrast
(1) be 2000 by molecular weight, massfraction is dewater at the vacuum tightness of polytetrahydrofuran dibasic alcohol at-0.1MPa of 70.5wt%, the temperature of 120 DEG C, then add the HDI of 29.5wt%, react three hours in 70 DEG C of nitrogen atmospheres, make base polyurethane prepolymer for use as.
(2) performed polymer and butyleneglycol feed intake according to mass ratio 100:12.7, react two hours, put into 70 DEG C of vacuum drying oven vacuum dryings after resultant vacuum defoamation under 80 DEG C of nitrogen atmospheres.
(3) material synthesized tabletted under the condition of 170 DEG C, then at room temperature to cold pressing 60s with the pressure of 1.0MPa, finally the mould that polymkeric substance is housed is placed on vacuum cooked 16h in the vacuum drying oven of 120 DEG C, after taking-up, room temperature is down in annealing in atmosphere, and at room temperature places 7 days.Its main performance index is in table 1.
Comparative example 3 and MDI type sample contrast
(1) be 2000 by molecular weight, massfraction is dewater at the vacuum tightness of PCDL at-0.1MPa of 67.4wt%, the temperature of 120 DEG C, then add the MDI of 32.6wt%, react three hours in 70 DEG C of nitrogen atmospheres, make base polyurethane prepolymer for use as.
(2) performed polymer and butyleneglycol feed intake according to mass ratio 100:8.5, react two hours, put into 70 DEG C of vacuum drying oven vacuum dryings after resultant vacuum defoamation under 80 DEG C of nitrogen atmospheres.
(3) material synthesized tabletted under the condition of 170 DEG C, then at room temperature to cold pressing 60s with the pressure of 1.5MPa, finally the mould that polymkeric substance is housed is placed on vacuum cooked 16h in the vacuum drying oven of 140 DEG C, after taking-up, room temperature is down in annealing in atmosphere, and at room temperature places 7 days.Its main performance index is in table 1.
Table 1. main performance index
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Hardness/Shao A | 93 | 90 | 91 | 90 | 93 | 92 |
| Tensile strength/MPa | 45.2 | 42.7 | 47.8 | 32.6 | 43.5 | 40.3 |
| Elongation at break/% | 735 | 695 | 721 | 631 | 825 | 624 |
| R value | 1.07 | 1.18 | 1.34 | 4.01 | 3.94 | 4.41 |
| Puncture resistant power/N | 882 | 822 | 839 | 723 | 682 | 624 |
R value is the ratio of the storage modulus of test sample at 60 DEG C and 120 DEG C, and its ratio is less, and resistance toheat is better.
Claims (4)
1. a high temperature resistant puncture resistant method for preparing polyurethane elastic body, it is characterized in that, this polyurethane elastomer is formed by two-step approach solution polymerization by PCDL, vulcabond and chainextender, polyurethane elastomer tabletted under the condition of 170 DEG C of synthesis, then at room temperature to cold pressing 60s with the pressure of 1.0MPa, finally the mould that polyurethane elastomer is housed is placed on vacuum cooked 16-24h in the vacuum drying oven of 100-140 DEG C, after taking-up, room temperature is down in annealing in atmosphere, and at room temperature places 5-8 days.
2. the high temperature resistant puncture resistant method for preparing polyurethane elastic body of one according to claim 1, it is characterized in that, two-step approach flow process is, massfraction is after dewatering at the vacuum tightness of PCDL at-0.1MPa of 68.6-70.5wt%, the temperature of 120 DEG C by the first step, mix with the vulcabond of 29.5-31.4wt%, under 70 DEG C of nitrogen atmospheres, reaction makes base polyurethane prepolymer for use as in three hours; Second step base polyurethane prepolymer for use as and butyleneglycol, according to mass ratio 100:10.3-12.7, react two hours, put into 70 DEG C of vacuum drying oven vacuum dryings after polyurethane elastomer vacuum defoamation at 80 DEG C.
3. the high temperature resistant puncture resistant method for preparing polyurethane elastic body of one according to claim 1, is characterized in that, PCDL number-average molecular weight scope is 500-5000.
4. the high temperature resistant puncture resistant method for preparing polyurethane elastic body of one according to claim 1, is characterized in that, vulcabond is hexamethylene diisocyanate, and chainextender is butyleneglycol.
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| CN201510243704.6A CN104829799A (en) | 2015-05-13 | 2015-05-13 | Preparation method of high-temperature-resistant puncture-resistant polyurethane elastomer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131235A (en) * | 2015-09-19 | 2015-12-09 | 烟台德邦科技有限公司 | Synthesis method of thermoplastic polyurethane elastomer |
| CN107446098A (en) * | 2017-06-30 | 2017-12-08 | 苏州奥斯汀新材料科技有限公司 | A kind of high temperature resistant puncture resistant method for preparing thermoplastic polyurethane elastomer |
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| CN103012725A (en) * | 2013-01-21 | 2013-04-03 | 江苏斯泰达新能源科技发展有限公司 | Polyurethane raw liquid for rubber rolls available for mould-free casting |
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2015
- 2015-05-13 CN CN201510243704.6A patent/CN104829799A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103012725A (en) * | 2013-01-21 | 2013-04-03 | 江苏斯泰达新能源科技发展有限公司 | Polyurethane raw liquid for rubber rolls available for mould-free casting |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131235A (en) * | 2015-09-19 | 2015-12-09 | 烟台德邦科技有限公司 | Synthesis method of thermoplastic polyurethane elastomer |
| CN107446098A (en) * | 2017-06-30 | 2017-12-08 | 苏州奥斯汀新材料科技有限公司 | A kind of high temperature resistant puncture resistant method for preparing thermoplastic polyurethane elastomer |
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Application publication date: 20150812 |