CN103396527A - Thermal aging-resistant polyurethane elastomer and preparation method thereof - Google Patents
Thermal aging-resistant polyurethane elastomer and preparation method thereof Download PDFInfo
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- CN103396527A CN103396527A CN2013103221092A CN201310322109A CN103396527A CN 103396527 A CN103396527 A CN 103396527A CN 2013103221092 A CN2013103221092 A CN 2013103221092A CN 201310322109 A CN201310322109 A CN 201310322109A CN 103396527 A CN103396527 A CN 103396527A
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Abstract
The invention provides a thermal aging-resistant polyurethane elastomer. The polyurethane elastomer is formed by mixing a polyurethane prepolymer, a chain extension cross-linking agent and auxiliaries, pouring, demolding and vulcanizing, wherein the polyurethane prepolymer is formed by stirring polymer diol, diisocyanate and a catalyst at the temperature of 50-100 DEG C, and the raw materials respectively comprise the following components in percentage by weight: 47-60wt% of polymer diol, 15-30wt% of diisocyanate, 0-4wt% of catalyst, 8-17wt% of chain extension cross-linking agent and 1-6wt% of auxiliaries. The invention simultaneously provides a preparation method of the thermal aging-resistant polyurethane elastomer. The method has the advantages of simple process and low equipment cost, and the produced polyurethane elastomer has excellent thermal aging resistance.
Description
Technical field
The invention provides a kind of polyurethane elastomer and preparation method thereof, relate in particular to a kind of heat-proof aging polyurethane elastomer, belong to technical field of polymer materials.
Technical background
Urethane has hard soft segment structure, show the resistance to low temperature, wear resistance of many excellences and wide durometer level etc., thereby its application is very extensive.But due to its goods in use ingress of air and interior heat-dissipating cause temperature higher, may cause that thermooxidizing decomposes, make the material property loss and impact is used.For its characteristics, multiple method of modifying is arranged, as adjust its molecular structure, interpolation oxidation inhibitor or mineral filler etc.
" a kind of preparation method of rigid olyurethane " patented technology (CN 201110330929), disclose by introducing the polymer polyatomic alcohol of 3 functionality, makes between polyurethane molecular to produce the resistance toheat that chemically crosslinked improves the rigid olyurethane goods." a kind of method for preparing thermoplastic polyurethane elastomer " patented technology (CN 201310005293), disclose resistance toheat, mechanical property and ageing resistance that the method that adopts inorganic nano-filler to fill Polyurethane Thermoplastic Elastomer improves polyurethane elastomer." a kind of formula of modified polyurethane " patented technology (CN 201210261585), disclose interpolation oxidation inhibitor thio-2 acid silicone grease in February and improved the aerial antioxidant property of urethane.In addition, Wang Shulun etc. have studied impact (Wang Shulun, the Zhai Wen of oxidation inhibitor JPP-100 on urethane wet and heat ageing resistant performance, Tang Zhiyong, etc. the preparation of novel anti-aging polyurethane elastomer and performance, polyurethane industrial, 2008,23 (4): 24-27).Huang Wanli add the research that antioxidant 1010 improved the polyurethane material ageing-resistant performance (Huang Wanli. improve the research of polyurethane material ageing-resistant performance. Anhui chemical industry, 2010,36 (3): 44-47.).
The method that above method forms, adds filler by feed change has improved the resistance toheat of material, but the polyurethane material heat aging property is improved not obvious, and range of application is very limited.
Summary of the invention
The present invention is intended to overcome the prior art defect, and its purpose is to provide a kind of heat-proof aging polyurethane elastomer and preparation method thereof.Preparation technology of the present invention is simple, and prepared polyurethane elastomer mechanical strength is good, and heat aging property is good, can apply the products such as fender, rubber roll and lining.
Realize that the technical scheme that above-mentioned purpose of the present invention adopts is:
A kind of heat-proof aging polyurethane elastomer, this polyurethane elastomer by base polyurethane prepolymer for use as and chain extension-crosslinking agent and auxiliary agent through mixing, cast, the demoulding, sulfuration form, wherein base polyurethane prepolymer for use as is stirred and forms under 50 ~ 100 ℃ of conditions by polymer diatomic alcohol, vulcabond and catalyzer, each component shared mass percent in raw material is respectively: polymer diatomic alcohol-47 ~ 60wt%, vulcabond-15 ~ 30wt%, catalyzer-0 ~ 4wt%, chain extension-crosslinking agent-8 ~ 17wt%, auxiliary agent-1 ~ 6wt%.
The present invention also provides above-mentioned heat-proof aging method for preparing polyurethane elastic body, and its technique is as follows: at first in reactor, add 47 ~ 60wt% polymer diatomic alcohol, 1 ~ 6h dewaters under 80 ~ 120 ℃ of conditions; Then add 15 ~ 30wt% vulcabond and 0 ~ 4wt% catalyzer, in 50 ~ 100 ℃ of stirring 1 ~ 5h, make base polyurethane prepolymer for use as; Base polyurethane prepolymer for use as is mixed with the agent of 8 ~ 17wt% chain extension-crosslinking and 1 ~ 6wt% auxiliary agent, cast, the demoulding, finally revulcanization 10 ~ 48h under 60 ~ 120 ℃ of conditions, make polyurethane elastomer.
Described polymer diatomic alcohol is one or both in PTMG, polypropylene glycol and polycaprolactone glycol, and the molecular weight of polymer diatomic alcohol is 1000 ~ 4000.
Described vulcabond is Toluene-2,4-diisocyanate, 4-vulcabond, 4, one or both in 4 '-diphenylmethanediisocyanate, hexamethylene vulcabond and isophorone diisocyanate.
Described catalyzer is a kind of in triethylene diamine, dibutyl tin dilaurate and stannous octoate.
Described chain extension-crosslinking agent is 3,3 '-bis-chloro-4,4 '-diaminodiphenyl-methane, 3, one or both in 5-dimethythiotoluene diamine, BDO, ethylene glycol and diethanolamine.
Described auxiliary agent is the mixture of dioctyl phthalate (DOP), antioxidant 1010, Tinuvin101 and the chloro-2-hydroxy diphenyl of 2,4,4-tri-ether.
Adopt the prepared heat-proof aging polyurethane elastomer of method provided by the invention through experiment test, its thermal ageing resistant performance improves obviously, and this preparation technology is simple.
Embodiment
Below in conjunction with specific embodiment, the present invention is done to detailed specific description, but protection scope of the present invention is not limited to following examples.
Raw material unification related in following examples of the present invention is described below: auxiliary agent is the mixture of dioctyl phthalate (DOP), antioxidant 1010, Tinuvin101 and the chloro-2-hydroxy diphenyl of 2,4,4-tri-ether.In following examples, repeat no more.
Embodiment 1
The heat-proof aging polyurethane elastomer that provides in the present embodiment, its preparation process is as follows:
In reactor, add 51 ~ 57wt% polymer diatomic alcohol, 1 ~ 3h dewaters under 80 ~ 100 ℃ of conditions; Then add 20 ~ 25wt% vulcabond and 3 ~ 4wt% catalyzer, in 50 ~ 70 ℃ of stirring 1 ~ 3h, make base polyurethane prepolymer for use as; Base polyurethane prepolymer for use as is mixed with the agent of 12 ~ 17wt% chain extension-crosslinking and 1 ~ 3wt% auxiliary agent, cast, the demoulding, finally revulcanization 10 ~ 20h under 60 ~ 85 ℃ of conditions, make polyurethane elastomer.
In the present embodiment: vulcabond is Toluene-2,4-diisocyanate, the 4-vulcabond; Catalyzer is triethylene diamine; Polymer diatomic alcohol is PTMG, and molecular weight is 1000 ~ 2000; The chain extension-crosslinking agent is 3,3 '-bis-chloro-4,4 '-diaminodiphenyl-methane.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 37.8 ~ 38.7MPa, and elongation at break is 573 ~ 652%, and aging back draft intensity is 38.1 ~ 39.2MPa, and elongation at break is 593 ~ 648%.
Embodiment 2
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 1:
In the present embodiment: vulcabond is Toluene-2,4-diisocyanate, the 4-vulcabond; Catalyzer is triethylene diamine; Polymer diatomic alcohol is PTMG, and molecular weight is 2000 ~ 3000; The chain extension-crosslinking agent is 3,3 '-bis-chloro-4, the mixture of 4 '-diaminodiphenyl-methane and 3,5-dimethythiotoluene diamine.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 48.9 ~ 52.1MPa, and elongation at break is 528 ~ 586%, and aging back draft intensity is 47.9 ~ 51.8MPa, and elongation at break is 545 ~ 591%.
Embodiment 3
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 1:
In the present embodiment: vulcabond is Toluene-2,4-diisocyanate, 4-vulcabond and 4, the mixture of 4 '-diphenylmethanediisocyanate; Catalyzer is triethylene diamine; Polymer diatomic alcohol is PTMG, and molecular weight is 3000 ~ 4000; The chain extension-crosslinking agent is 3,3 '-bis-chloro-4, the mixture of 4 '-diaminodiphenyl-methane and BDO.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 39.5 ~ 40.7MPa, and elongation at break is 565 ~ 622%, and aging back draft intensity is 37.8 ~ 38.7MPa, and elongation at break is 575 ~ 628%.
Embodiment 4
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 1:
In the present embodiment: vulcabond is Toluene-2,4-diisocyanate, the mixture of 4-vulcabond and hexamethylene vulcabond; Catalyzer is triethylene diamine; Polymer diatomic alcohol is the mixture of polypropylene glycol and polycaprolactone glycol, and the molecular weight of polypropylene glycol is 1000 ~ 2000, and the molecular weight of polycaprolactone glycol is 3000 ~ 4000; The chain extension-crosslinking agent is 3,3 '-bis-chloro-4, the mixture of 4 '-diaminodiphenyl-methane and ethylene glycol.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 38.8 ~ 39.7MPa, and elongation at break is 559 ~ 609%, and aging back draft intensity is 38.2 ~ 39.9MPa, and elongation at break is 548 ~ 625%.
Embodiment 5
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 1:
In the present embodiment: vulcabond is Toluene-2,4-diisocyanate, the mixture of 4-vulcabond and isophorone diisocyanate; Catalyzer is triethylene diamine; Polymer diatomic alcohol is the mixture of polypropylene glycol and polycaprolactone glycol, and the polypropylene glycol molecular weight is 2000 ~ 3000, and the molecular weight of polycaprolactone glycol is 1000 ~ 2000; The chain extension-crosslinking agent is 3,3 '-bis-chloro-4, the mixture of 4 '-diaminodiphenyl-methane and diethanolamine.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 40.9 ~ 42.7MPa, and elongation at break is 525 ~ 612%, and aging back draft intensity is 41.5 ~ 42.9MPa, and elongation at break is 556 ~ 609%.
Embodiment 6
The heat-proof aging polyurethane elastomer that provides in the present embodiment, its preparation process is as follows:
In reactor, add 47 ~ 53wt% polymer diatomic alcohol, 3 ~ 5h dewaters under 90 ~ 110 ℃ of conditions; Then add 24 ~ 30wt% vulcabond and 1 ~ 3wt% catalyzer, in 65 ~ 85 ℃ of stirring 2 ~ 4h, make base polyurethane prepolymer for use as; Base polyurethane prepolymer for use as is mixed with the agent of 10 ~ 15wt% chain extension-crosslinking and 2 ~ 5wt% auxiliary agent, cast, the demoulding, finally revulcanization 20 ~ 36h under 80 ~ 100 ℃ of conditions, make polyurethane elastomer.
In the present embodiment: vulcabond is 4,4 '-diphenylmethanediisocyanate; Catalyzer is dibutyl tin dilaurate; Polymer diatomic alcohol is polypropylene glycol, and molecular weight is 1000 ~ 2000; The chain extension-crosslinking agent is 3,5-dimethythiotoluene diamine.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 35.9 ~ 38.7MPa, and elongation at break is 546 ~ 598%, and aging back draft intensity is 36.8 ~ 38.9MPa, and elongation at break is 550 ~ 605%.
Embodiment 7
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 6:
In the present embodiment: vulcabond is 4, the mixture of 4 '-diphenylmethanediisocyanate and hexamethylene vulcabond; Catalyzer is dibutyl tin dilaurate; Polymer diatomic alcohol is polypropylene glycol, and molecular weight is 2000 ~ 3000; The chain extension-crosslinking agent is the mixture of 3,5-dimethythiotoluene diamine and BDO.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 35.7 ~ 38.1MPa, and elongation at break is 552 ~ 601%, and aging back draft intensity is 36.2 ~ 38.4MPa, and elongation at break is 568 ~ 621%.
Embodiment 8
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 6:
In the present embodiment: vulcabond is 4, the mixture of 4 '-diphenylmethanediisocyanate and isophorone diisocyanate; Catalyzer is dibutyl tin dilaurate; Polymer diatomic alcohol is polypropylene glycol, and molecular weight is 3000 ~ 4000; The chain extension-crosslinking agent is the mixture of 3,5-dimethythiotoluene diamine and ethylene glycol.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 37.1 ~ 39.2MPa, and elongation at break is 563 ~ 623%, and aging back draft intensity is 37.9 ~ 39.8MPa, and elongation at break is 553 ~ 641%.
Embodiment 9
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 6:
In the present embodiment: vulcabond is 4, the mixture of 4 '-diphenylmethanediisocyanate and isophorone diisocyanate; Catalyzer is dibutyl tin dilaurate; Polymer diatomic alcohol is polypropylene glycol, and molecular weight is 2000 ~ 3000; The chain extension-crosslinking agent is the mixture of 3,5-dimethythiotoluene diamine and diethanolamine.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 37.4 ~ 38.6MPa, and elongation at break is 593 ~ 665%, and aging back draft intensity is 38.1 ~ 39.5MPa, and elongation at break is 601 ~ 672%.
Embodiment 10
The heat-proof aging polyurethane elastomer that provides in the present embodiment, its preparation process is as follows:
In reactor, add 55 ~ 60wt% polymer diatomic alcohol, 4 ~ 6h dewaters under 100 ~ 120 ℃ of conditions; Then add 15 ~ 21wt% vulcabond and 2 ~ 3wt% catalyzer, in 80 ~ 100 ℃ of stirring 3 ~ 5h, make base polyurethane prepolymer for use as; Base polyurethane prepolymer for use as is mixed with the agent of 12 ~ 17wt% chain extension-crosslinking and 4 ~ 6wt% auxiliary agent, cast, the demoulding, finally revulcanization 36 ~ 48h under 95 ~ 120 ℃ of conditions, make polyurethane elastomer.
In the present embodiment: vulcabond is the hexamethylene vulcabond; Catalyzer is stannous octoate; Polymer diatomic alcohol is polycaprolactone glycol, and molecular weight is 3000 ~ 4000; The chain extension-crosslinking agent is BDO.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 42.1 ~ 44.8MPa, and elongation at break is 602 ~ 648%, and aging back draft intensity is 43.1 ~ 45.7MPa, and elongation at break is 589 ~ 639%.
Embodiment 11
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 10:
In the present embodiment: vulcabond is the mixture of hexamethylene vulcabond and isophorone diisocyanate; Catalyzer is stannous octoate; Polymer diatomic alcohol is polycaprolactone glycol, and molecular weight is 2000 ~ 3000; The chain extension-crosslinking agent is the mixture of BDO and ethylene glycol.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 38.1 ~ 40.2MPa, and elongation at break is 589 ~ 626%, and aging back draft intensity is 39.1 ~ 40.7MPa, and elongation at break is 598 ~ 645%.
Embodiment 12
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 10:
In the present embodiment: vulcabond is the mixture of hexamethylene vulcabond and isophorone diisocyanate; Catalyzer is stannous octoate; Polymer diatomic alcohol is polycaprolactone glycol, and molecular weight is 1000 ~ 2000; The chain extension-crosslinking agent is the mixture of BDO and diethanolamine.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 36.7 ~ 39.7MPa, and elongation at break is 549 ~ 583%, and aging back draft intensity is 37.2 ~ 39.9MPa, and elongation at break is 585 ~ 602%.
Embodiment 13
The heat-proof aging polyurethane elastomer that provides in the present embodiment, its preparation process is as follows:
In reactor, add 55 ~ 60wt% polymer diatomic alcohol, 3 ~ 5h dewaters under 90 ~ 110 ℃ of conditions; Then add 25 ~ 30wt% vulcabond and 0% catalyzer, in 65 ~ 85 ℃ of stirring 2 ~ 4h, make base polyurethane prepolymer for use as; Base polyurethane prepolymer for use as is mixed with the agent of 8 ~ 12wt% chain extension-crosslinking and 4 ~ 6wt% auxiliary agent, cast, the demoulding, finally revulcanization 36 ~ 48h under 95 ~ 120 ℃ of conditions, make polyurethane elastomer.
In the present embodiment: vulcabond is isophorone diisocyanate; Catalyzer is stannous octoate; Polymer diatomic alcohol is the mixture of PTMG and polypropylene glycol, and the molecular weight of PTMG is 1000 ~ 2000, and the molecular weight of polypropylene glycol is 3000 ~ 4000; The chain extension-crosslinking agent is ethylene glycol.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 36.4 ~ 39.2MPa, and elongation at break is 589 ~ 637%, and aging back draft intensity is 36.8 ~ 38.4MPa, and elongation at break is 598 ~ 649%.
Embodiment 14
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 13:
In the present embodiment: vulcabond is isophorone diisocyanate; Catalyzer is stannous octoate; Polymer diatomic alcohol is the mixture of PTMG and polypropylene glycol, and the molecular weight of PTMG is 2000 ~ 3000, and the molecular weight of polypropylene glycol is 1000 ~ 2000; The chain extension-crosslinking agent is the mixture of ethylene glycol and diethanolamine.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 38.5 ~ 40.5MPa, and elongation at break is 569 ~ 638%, and aging back draft intensity is 37.9 ~ 39.9MPa, and elongation at break is 585 ~ 647%.
Embodiment 15
The heat-proof aging polyurethane elastomer that provides in the present embodiment, except following raw material, its preparation process is with embodiment 13:
In reactor, add 55 ~ 60wt% polymer diatomic alcohol, 3 ~ 5h dewaters under 90 ~ 110 ℃ of conditions; Then add 25 ~ 30wt% vulcabond and 0wt% catalyzer, in 65 ~ 85 ℃ of stirring 2 ~ 4h, make base polyurethane prepolymer for use as; Base polyurethane prepolymer for use as is mixed with the agent of 8 ~ 12wt% chain extension-crosslinking and 4 ~ 6wt% auxiliary agent, cast, the demoulding, finally revulcanization 36 ~ 48h under 95 ~ 120 ℃ of conditions, make polyurethane elastomer.
In the present embodiment: vulcabond is isophorone diisocyanate; Polymer diatomic alcohol is the mixture of PTMG and polycaprolactone glycol, and the molecular weight of PTMG is 3000 ~ 4000, and the molecular weight of polycaprolactone glycol is 2000 ~ 3000; The chain extension-crosslinking agent is diethanolamine.
The prepared polyurethane elastomer of the present embodiment is tested through 150 ℃ of aging 3d: aging front tensile strength is 39.1 ~ 42.3MPa, and elongation at break is 529 ~ 586%, and aging back draft intensity is 39.5 ~ 42.7MPa, and elongation at break is 538 ~ 597%.
Claims (7)
1. heat-proof aging polyurethane elastomer, it is characterized in that this polyurethane elastomer by base polyurethane prepolymer for use as and chain extension-crosslinking agent and auxiliary agent through mixing, cast, the demoulding, sulfuration form, wherein base polyurethane prepolymer for use as is stirred and forms under 50 ~ 100 ℃ of conditions by polymer diatomic alcohol, vulcabond and catalyzer, each component shared mass percent in raw material is respectively: polymer diatomic alcohol-47 ~ 60wt%, vulcabond-15 ~ 30wt%, catalyzer-0 ~ 4wt%, chain extension-crosslinking agent-8 ~ 17wt%, auxiliary agent-1 ~ 6wt%.
2. method for preparing polyurethane elastic body claimed in claim 1, it is characterized in that: in reactor, add 47 ~ 60wt% polymer diatomic alcohol, 1 ~ 6h dewaters under 80 ~ 120 ℃ of conditions; Then add 15 ~ 30wt% vulcabond and 0 ~ 4wt% catalyzer, in 50 ~ 100 ℃ of stirring 1 ~ 5h, make base polyurethane prepolymer for use as; Base polyurethane prepolymer for use as is mixed with the agent of 8 ~ 17wt% chain extension-crosslinking and 1 ~ 6wt% auxiliary agent, cast, the demoulding, finally revulcanization 10 ~ 48h under 60 ~ 120 ℃ of conditions, make polyurethane elastomer.
3. method for preparing polyurethane elastic body according to claim 2, it is characterized in that: described polymer diatomic alcohol is one or both in PTMG, polypropylene glycol and polycaprolactone glycol, and the molecular weight of polymer diatomic alcohol is 1000 ~ 4000.
4. method for preparing polyurethane elastic body according to claim 2, it is characterized in that: described vulcabond is Toluene-2,4-diisocyanate, 4-vulcabond, 4, one or both in 4 '-diphenylmethanediisocyanate, hexamethylene vulcabond and isophorone diisocyanate.
5. method for preparing polyurethane elastic body according to claim 2 is characterized in that: described catalyzer is a kind of in triethylene diamine, dibutyl tin dilaurate and stannous octoate.
6. method for preparing polyurethane elastic body according to claim 2, it is characterized in that: described chain extension-crosslinking agent is 3,3 '-bis-chloro-4,4 '-diaminodiphenyl-methane, 3, one or both in 5-dimethythiotoluene diamine, BDO, ethylene glycol and diethanolamine.
7. method for preparing polyurethane elastic body according to claim 2, it is characterized in that: described auxiliary agent is the mixture of dioctyl phthalate (DOP), antioxidant 1010, Tinuvin101 and the chloro-2-hydroxy diphenyl of 2,4,4-tri-ether.
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