CN105237723A - Preparation method of heat-conduction polyurethane material - Google Patents
Preparation method of heat-conduction polyurethane material Download PDFInfo
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Abstract
The invention discloses a preparation method of a heat-conduction polyurethane material, wherein the preparation method includes the following steps: S1, preparation of a pre-polymer: adding graphene oxide in polytetrahydrofuran glycol, heating up, carrying out uniform ultrasonic dispersion, drying, adjusting the temperature, adding isophorone diisocyanate and stannous caprylate, carrying out heat preservation stirring, heating up, carrying out heat preservation stirring, purifying, carrying out vacuum defoaming, and heating up to obtain the pre-polymer; S2, preparation of a chain extender: dissolving 2-bromo-5-nitro-benzotrifluoride in N-methyl pyrrolidone, adding potassium carbonate and 1,4-butanediol, heating up, carrying out heat preservation stirring, and purifying to obtain an intermediate material; and mixing evenly the intermediate material, ethanol, deionized water and a reduced iron powder, dropwise adding concentrated hydrochloric acid, heating up, refluxing, and purifying to obtain the chain extender; and S3, preparation of the heat-resistant heat-conduction polyurethane. The heat-conduction polyurethane material is quick in heat conduction, high in mechanical strength and good in heat resistance.
Description
Technical field
The present invention relates to polyurethane material technical field, particularly relate to a kind of preparation method of heat-conduction polyurethane material.
Background technology
Polyurethane elastomer has high strength, snappiness, the feature of high elongation rate, and there is excellent wear resistance, oil-proofness, resistance to tearing, chemical-resistant, damping performance is good, the regulation range of hardness is large, obtain in a lot of fields and apply widely, but polyurethane elastomer produces larger interior heat-dissipating in a dynamic condition, and the resistance toheat of polyurethane elastomer is poor, under the high temperature conditions, mechanical properties decrease is obvious, cause elastomerics dynamically, use under the condition that temperature is higher, its physical dimension will change, and hardness, strength and modulus performance all declines, thus limit the application of polyurethane elastomer under dynamic and high temperature operating conditions.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of preparation method of heat-conduction polyurethane material, heat conduction of the present invention is fast, and physical strength is high, good heat resistance.
The preparation method of a kind of heat-conduction polyurethane material that the present invention proposes, comprises the steps:
S1, prepare performed polymer: added by graphene oxide in PTMG, heat up, ultrasonic disperse is even, dry, regulate temperature, add isophorone diisocyanate and stannous octoate, insulated and stirred, heat up, insulated and stirred, purifying, vacuum defoamation, heats up and obtains performed polymer;
S2, prepare chainextender: be dissolved in N-Methyl pyrrolidone by bromo-for 2-5-nitro-trifluoromethylbenzene, add salt of wormwood, BDO, heat up, insulated and stirred, purifying obtains intermediate material; By intermediate material, ethanol, deionized water, reduced iron powder mixing, drip concentrated hydrochloric acid, heat up, backflow, purifying obtains chainextender;
S3, prepare heat-resisting heat-conduction polyurethane: added by chainextender in performed polymer, mixing, sulfuration obtains heat-resisting heat-conduction polyurethane material.
Preferably, in S1, graphene oxide is added in PTMG, be warming up to 40-50 DEG C, regulating power is 300-500W, ultrasonic 5-7h, be warming up to 110-120 DEG C, vacuum-drying 2-3h, adjustment temperature is 40-50 DEG C, add isophorone diisocyanate and stannous octoate, insulated and stirred 30-50min, be warming up to 80-90 DEG C, insulated and stirred 2-3h, be warming up to 150-170 DEG C, decompression steams unreacted isophorone diisocyanate, and vacuum defoamation obtains performed polymer.
Preferably, in S1, in PTMG, in-OH and isophorone diisocyanate, the mol ratio of-NCO is 1:4-6.
Preferably, in S1, the weight ratio of graphene oxide, stannous octoate and isophorone diisocyanate is 1-1.5:0.4-0.6:100.
Preferably, in S2, bromo-for 2-5-nitro-trifluoromethylbenzene is dissolved in N-Methyl pyrrolidone, add salt of wormwood, BDO, be warming up to 140-150 DEG C, insulated and stirred 20-25h, filters, gets filtrate evaporated under reduced pressure N-Methyl pyrrolidone and obtain intermediate material; By intermediate material, ethanol, deionized water, reduced iron powder mixing, drip concentrated hydrochloric acid, be warming up to 70-90 DEG C with the speed of 0.5-1ml/min, backflow 10-15h, filter, get filtrate evaporated under reduced pressure ethanol, add mixing solutions recrystallization, drying under reduced pressure obtains chainextender.
Preferably, in S2, the weight ratio of the bromo-5-nitro-trifluoromethylbenzene of 2-, salt of wormwood, BDO is 3-3.5:1:0.5-0.7.
Preferably, in S2, the weight ratio of intermediate material, ethanol, deionized water, reduced iron powder, concentrated hydrochloric acid is 20-30:25-30:15-20:13-19:1-1.5.
Preferably, in S2, mixed solvent is the mixture of ethanol, ether, water composition, and the volume ratio of ethanol, ether, water is 50-60:5-15:25-35.
Preferably, in S3, add in performed polymer by after chainextender melting, be warming up to 80-90 DEG C, stir 2-3min with the speed of 500-600r/min, be warming up to 110-120 DEG C, adjustment pressure is 12-14MPa, a sulfuration 20-40min, adjustment temperature is that 100-110 DEG C, post cure 20-24h obtain heat-resisting heat-conduction polyurethane material.
Preferably, in S3, the weight ratio of performed polymer and chainextender is 3-5:0.5-0.9.
In above-mentioned S2, the bromo-5-nitro-trifluoromethylbenzene of 2-is dissolved in the effect of N-Methyl pyrrolidone, and the effect of mixing solutions is recrystallization, does not specify its consumption, according to concrete operations determination consumption.
The graphene oxide that the present invention selects has excellent thermostability, mechanical property and thermal conductivity,-OH on graphene oxide can react with isophorone diisocyanate, graphene oxide is dispersed in PTMG uniformly on the one hand, react with isophorone diisocyanate, dispersed graphene oxide in the performed polymer that reaction is generated, greatly increase thermal conductivity of the present invention and mechanical property, in isophorone diisocyanate, the mole number of-NCO is greater than the mole number of-OH in PTMG on the other hand, the performed polymer molecular chain structure that PTMG and isophorone diisocyanate are obtained by reacting is neat, can greatly increase thermotolerance of the present invention and mechanical property, graphene oxide and PTMG act synergistically, and all react with isophorone diisocyanate, the performed polymer obtained has neat chain structure and homodisperse graphene oxide, can greatly increase thermal conductivity of the present invention, thermotolerance and mechanical property, containing fluorin radical in the chainextender that BDO obtains through the bromo-5-nitro-trifluoromethylbenzene modification of 2-, this chainextender and prepolymer reaction, introduce fluorin radical in urethane, considerably increases thermotolerance of the present invention and mechanical property, fluorin radical, homodisperse graphene oxide, neat chain structure are coordinated mutually, interact, considerably increase thermotolerance of the present invention, thermal conductivity and mechanical property.
Embodiment
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
A preparation method for heat-conduction polyurethane material, comprises the steps:
S1, prepare performed polymer: added by graphene oxide in PTMG, be warming up to 40 DEG C, regulating power is 500W, ultrasonic 5h, be warming up to 120 DEG C, vacuum-drying 2h, temperature is regulated to be 50 DEG C, add isophorone diisocyanate and stannous octoate, insulated and stirred 30min, be warming up to 90 DEG C, insulated and stirred 2h, be warming up to 170 DEG C, decompression steams unreacted isophorone diisocyanate, vacuum defoamation obtains performed polymer, wherein, in PTMG, in-OH and isophorone diisocyanate, the mol ratio of-NCO is 1:4, graphene oxide, the weight ratio of stannous octoate and isophorone diisocyanate is 1.5:0.4:100,
S2, prepare chainextender: be dissolved in N-Methyl pyrrolidone by bromo-for 2-5-nitro-trifluoromethylbenzene, add salt of wormwood, BDO, be warming up to 150 DEG C, insulated and stirred 20h, filter, get filtrate evaporated under reduced pressure N-Methyl pyrrolidone and obtain intermediate material, by intermediate material, ethanol, deionized water, reduced iron powder mixes, concentrated hydrochloric acid is dripped with the speed of 1ml/min, be warming up to 70 DEG C, backflow 15h, filter, get filtrate evaporated under reduced pressure ethanol, add mixing solutions recrystallization, drying under reduced pressure obtains chainextender, wherein, the bromo-5-nitro-trifluoromethylbenzene of 2-, salt of wormwood, 1, the weight ratio of 4-butyleneglycol is 3:1:0.7, intermediate material, ethanol, deionized water, reduced iron powder, the weight ratio of concentrated hydrochloric acid is 20:30:15:19:1, mixed solvent is ethanol, ether, the mixture of water composition, and ethanol, ether, the volume ratio of water is 60:5:35,
S3, prepare heat-resisting heat-conduction polyurethane: add in performed polymer by after chainextender melting, be warming up to 80 DEG C, 2min is stirred with the speed of 600r/min, be warming up to 120 DEG C, adjustment pressure is 12MPa, a sulfuration 40min, temperature is regulated to be 100 DEG C, post cure 24h obtains heat-resisting heat-conduction polyurethane material, and wherein, the weight ratio of performed polymer and chainextender is 3:0.9.
Embodiment 2
A preparation method for heat-conduction polyurethane material, comprises the steps:
S1, prepare performed polymer: added by graphene oxide in PTMG, be warming up to 50 DEG C, regulating power is 300W, ultrasonic 7h, be warming up to 110 DEG C, vacuum-drying 3h, temperature is regulated to be 40 DEG C, add isophorone diisocyanate and stannous octoate, insulated and stirred 50min, be warming up to 80 DEG C, insulated and stirred 3h, be warming up to 150 DEG C, decompression steams unreacted isophorone diisocyanate, vacuum defoamation obtains performed polymer, wherein, in PTMG, in-OH and isophorone diisocyanate, the mol ratio of-NCO is 1:6, graphene oxide, the weight ratio of stannous octoate and isophorone diisocyanate is 1:0.6:100,
S2, prepare chainextender: be dissolved in N-Methyl pyrrolidone by bromo-for 2-5-nitro-trifluoromethylbenzene, add salt of wormwood, BDO, be warming up to 140 DEG C, insulated and stirred 25h, filter, get filtrate evaporated under reduced pressure N-Methyl pyrrolidone and obtain intermediate material, by intermediate material, ethanol, deionized water, reduced iron powder mixes, concentrated hydrochloric acid is dripped with the speed of 0.5ml/min, be warming up to 90 DEG C, backflow 10h, filter, get filtrate evaporated under reduced pressure ethanol, add mixing solutions recrystallization, drying under reduced pressure obtains chainextender, wherein, the bromo-5-nitro-trifluoromethylbenzene of 2-, salt of wormwood, 1, the weight ratio of 4-butyleneglycol is 3.5:1:0.5, intermediate material, ethanol, deionized water, reduced iron powder, the weight ratio of concentrated hydrochloric acid is 30:25:20:13:1.5, mixed solvent is ethanol, ether, the mixture of water composition, and ethanol, ether, the volume ratio of water is 50:15:25,
S3, prepare heat-resisting heat-conduction polyurethane: add in performed polymer by after chainextender melting, be warming up to 90 DEG C, 3min is stirred with the speed of 500r/min, be warming up to 110 DEG C, adjustment pressure is 14MPa, a sulfuration 20min, temperature is regulated to be 110 DEG C, post cure 20h obtains heat-resisting heat-conduction polyurethane material, and wherein, the weight ratio of performed polymer and chainextender is 5:0.5.
Embodiment 3
A preparation method for heat-conduction polyurethane material, comprises the steps:
S1, prepare performed polymer: added by graphene oxide in PTMG, be warming up to 43 DEG C, regulating power is 450W, ultrasonic 5.5h, be warming up to 118 DEG C, vacuum-drying 2.2h, temperature is regulated to be 47 DEG C, add isophorone diisocyanate and stannous octoate, insulated and stirred 35min, be warming up to 87 DEG C, insulated and stirred 2.3h, be warming up to 165 DEG C, decompression steams unreacted isophorone diisocyanate, vacuum defoamation obtains performed polymer, wherein, in PTMG, in-OH and isophorone diisocyanate, the mol ratio of-NCO is 1:4.5, graphene oxide, the weight ratio of stannous octoate and isophorone diisocyanate is 1.4:0.45:100,
S2, prepare chainextender: be dissolved in N-Methyl pyrrolidone by bromo-for 2-5-nitro-trifluoromethylbenzene, add salt of wormwood, BDO, be warming up to 147 DEG C, insulated and stirred 21h, filter, get filtrate evaporated under reduced pressure N-Methyl pyrrolidone and obtain intermediate material, by intermediate material, ethanol, deionized water, reduced iron powder mixes, concentrated hydrochloric acid is dripped with the speed of 0.9ml/min, be warming up to 75 DEG C, backflow 14h, filter, get filtrate evaporated under reduced pressure ethanol, add mixing solutions recrystallization, drying under reduced pressure obtains chainextender, wherein, the bromo-5-nitro-trifluoromethylbenzene of 2-, salt of wormwood, 1, the weight ratio of 4-butyleneglycol is 3.1:1:0.65, intermediate material, ethanol, deionized water, reduced iron powder, the weight ratio of concentrated hydrochloric acid is 22:28:16:17:1.2, mixed solvent is ethanol, ether, the mixture of water composition, and ethanol, ether, the volume ratio of water is 58:8:33,
S3, prepare heat-resisting heat-conduction polyurethane: add in performed polymer by after chainextender melting, be warming up to 82 DEG C, 2.2min is stirred with the speed of 570r/min, be warming up to 117 DEG C, adjustment pressure is 12MPa, a sulfuration 35min, temperature is regulated to be 102 DEG C, post cure 23h obtains heat-resisting heat-conduction polyurethane material, and wherein, the weight ratio of performed polymer and chainextender is 3.5:0.8.
Embodiment 4
A preparation method for heat-conduction polyurethane material, comprises the steps:
S1, prepare performed polymer: added by graphene oxide in PTMG, be warming up to 47 DEG C, regulating power is 350W, ultrasonic 6.5h, be warming up to 112 DEG C, vacuum-drying 2.8h, temperature is regulated to be 43 DEG C, add isophorone diisocyanate and stannous octoate, insulated and stirred 45min, be warming up to 83 DEG C, insulated and stirred 2.7h, be warming up to 155 DEG C, decompression steams unreacted isophorone diisocyanate, vacuum defoamation obtains performed polymer, wherein, in PTMG, in-OH and isophorone diisocyanate, the mol ratio of-NCO is 1:5.5, graphene oxide, the weight ratio of stannous octoate and isophorone diisocyanate is 1.2:0.55:100,
S2, prepare chainextender: be dissolved in N-Methyl pyrrolidone by bromo-for 2-5-nitro-trifluoromethylbenzene, add salt of wormwood, BDO, be warming up to 143 DEG C, insulated and stirred 23h, filter, get filtrate evaporated under reduced pressure N-Methyl pyrrolidone and obtain intermediate material, by intermediate material, ethanol, deionized water, reduced iron powder mixes, concentrated hydrochloric acid is dripped with the speed of 0.7ml/min, be warming up to 85 DEG C, backflow 12h, filter, get filtrate evaporated under reduced pressure ethanol, add mixing solutions recrystallization, drying under reduced pressure obtains chainextender, wherein, the bromo-5-nitro-trifluoromethylbenzene of 2-, salt of wormwood, 1, the weight ratio of 4-butyleneglycol is 3.3:1:0.55, intermediate material, ethanol, deionized water, reduced iron powder, the weight ratio of concentrated hydrochloric acid is 28:26:18:15:1.4, mixed solvent is ethanol, ether, the mixture of water composition, and ethanol, ether, the volume ratio of water is 52:12:27,
S3, prepare heat-resisting heat-conduction polyurethane: add in performed polymer by after chainextender melting, be warming up to 88 DEG C, 2.8min is stirred with the speed of 530r/min, be warming up to 113 DEG C, adjustment pressure is 14MPa, a sulfuration 25min, temperature is regulated to be 108 DEG C, post cure 21h obtains heat-resisting heat-conduction polyurethane material, and wherein, the weight ratio of performed polymer and chainextender is 4.5:0.6.
Embodiment 5
A preparation method for heat-conduction polyurethane material, comprises the steps:
S1, prepare performed polymer: added by graphene oxide in PTMG, be warming up to 45 DEG C, regulating power is 400W, ultrasonic 6h, be warming up to 115 DEG C, vacuum-drying 2.5h, temperature is regulated to be 45 DEG C, add isophorone diisocyanate and stannous octoate, insulated and stirred 40min, be warming up to 85 DEG C, insulated and stirred 2.5h, be warming up to 160 DEG C, decompression steams unreacted isophorone diisocyanate, vacuum defoamation obtains performed polymer, wherein, in PTMG, in-OH and isophorone diisocyanate, the mol ratio of-NCO is 1:5, graphene oxide, the weight ratio of stannous octoate and isophorone diisocyanate is 1.3:0.5:100,
S2, prepare chainextender: be dissolved in N-Methyl pyrrolidone by bromo-for 2-5-nitro-trifluoromethylbenzene, add salt of wormwood, BDO, be warming up to 145 DEG C, insulated and stirred 22h, filter, get filtrate evaporated under reduced pressure N-Methyl pyrrolidone and obtain intermediate material, by intermediate material, ethanol, deionized water, reduced iron powder mixes, concentrated hydrochloric acid is dripped with the speed of 0.8ml/min, be warming up to 80 DEG C, backflow 13h, filter, get filtrate evaporated under reduced pressure ethanol, add mixing solutions recrystallization, drying under reduced pressure obtains chainextender, wherein, the bromo-5-nitro-trifluoromethylbenzene of 2-, salt of wormwood, 1, the weight ratio of 4-butyleneglycol is 3.2:1:0.6, intermediate material, ethanol, deionized water, reduced iron powder, the weight ratio of concentrated hydrochloric acid is 25:27:17:16:1.3, mixed solvent is ethanol, ether, the mixture of water composition, and ethanol, ether, the volume ratio of water is 55:10:30,
S3, prepare heat-resisting heat-conduction polyurethane: add in performed polymer by after chainextender melting, be warming up to 85 DEG C, 2.5min is stirred with the speed of 550r/min, be warming up to 115 DEG C, adjustment pressure is 13MPa, a sulfuration 30min, temperature is regulated to be 105 DEG C, post cure 22h obtains heat-resisting heat-conduction polyurethane material, and wherein, the weight ratio of performed polymer and chainextender is 4:0.7.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (10)
1. a preparation method for heat-conduction polyurethane material, is characterized in that, comprises the steps:
S1, prepare performed polymer: added by graphene oxide in PTMG, heat up, ultrasonic disperse is even, dry, regulate temperature, add isophorone diisocyanate and stannous octoate, insulated and stirred, heat up, insulated and stirred, purifying, vacuum defoamation, heats up and obtains performed polymer;
S2, prepare chainextender: be dissolved in N-Methyl pyrrolidone by bromo-for 2-5-nitro-trifluoromethylbenzene, add salt of wormwood, BDO, heat up, insulated and stirred, purifying obtains intermediate material; By intermediate material, ethanol, deionized water, reduced iron powder mixing, drip concentrated hydrochloric acid, heat up, backflow, purifying obtains chainextender;
S3, prepare heat-resisting heat-conduction polyurethane: added by chainextender in performed polymer, mixing, sulfuration obtains heat-resisting heat-conduction polyurethane material.
2. the preparation method of heat-conduction polyurethane material according to claim 1, it is characterized in that, in S1, graphene oxide is added in PTMG, be warming up to 40-50 DEG C, regulating power is 300-500W, ultrasonic 5-7h, be warming up to 110-120 DEG C, vacuum-drying 2-3h, adjustment temperature is 40-50 DEG C, adds isophorone diisocyanate and stannous octoate, insulated and stirred 30-50min, be warming up to 80-90 DEG C, insulated and stirred 2-3h, be warming up to 150-170 DEG C, decompression steams unreacted isophorone diisocyanate, and vacuum defoamation obtains performed polymer.
3. the preparation method of heat-conduction polyurethane material according to claim 1 or 2, is characterized in that, in S1, in PTMG, in-OH and isophorone diisocyanate, the mol ratio of-NCO is 1:4-6.
4. the preparation method of heat-conduction polyurethane material according to any one of claim 1-3, it is characterized in that, in S1, the weight ratio of graphene oxide, stannous octoate and isophorone diisocyanate is 1-1.5:0.4-0.6:100.
5. the preparation method of heat-conduction polyurethane material according to any one of claim 1-4, it is characterized in that, in S2, bromo-for 2-5-nitro-trifluoromethylbenzene is dissolved in N-Methyl pyrrolidone, adds salt of wormwood, BDO, be warming up to 140-150 DEG C, insulated and stirred 20-25h, filters, gets filtrate evaporated under reduced pressure N-Methyl pyrrolidone and obtain intermediate material; By intermediate material, ethanol, deionized water, reduced iron powder mixing, drip concentrated hydrochloric acid, be warming up to 70-90 DEG C with the speed of 0.5-1ml/min, backflow 10-15h, filter, get filtrate evaporated under reduced pressure ethanol, add mixing solutions recrystallization, drying under reduced pressure obtains chainextender.
6. the preparation method of heat-conduction polyurethane material according to any one of claim 1-5, it is characterized in that, in S2, the weight ratio of the bromo-5-nitro-trifluoromethylbenzene of 2-, salt of wormwood, BDO is 3-3.5:1:0.5-0.7.
7. the preparation method of heat-conduction polyurethane material according to any one of claim 1-6, it is characterized in that, in S2, the weight ratio of intermediate material, ethanol, deionized water, reduced iron powder, concentrated hydrochloric acid is 20-30:25-30:15-20:13-19:1-1.5.
8. the preparation method of heat-conduction polyurethane material according to any one of claim 1-7, is characterized in that, in S2, mixed solvent is the mixture of ethanol, ether, water composition, and the volume ratio of ethanol, ether, water is 50-60:5-15:25-35.
9. the preparation method of heat-conduction polyurethane material according to any one of claim 1-8, it is characterized in that, in S3, add in performed polymer by after chainextender melting, be warming up to 80-90 DEG C, 2-3min is stirred with the speed of 500-600r/min, be warming up to 110-120 DEG C, adjustment pressure is 12-14MPa, a sulfuration 20-40min, adjustment temperature is that 100-110 DEG C, post cure 20-24h obtain heat-resisting heat-conduction polyurethane material.
10. the preparation method of heat-conduction polyurethane material according to any one of claim 1-9, it is characterized in that, in S3, the weight ratio of performed polymer and chainextender is 3-5:0.5-0.9.
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| CN116426113A (en) * | 2023-04-10 | 2023-07-14 | 浙江恒亿达复合材料有限公司 | High-compression-resistance fiber-reinforced polyurethane composite board and preparation method thereof |
| CN116426113B (en) * | 2023-04-10 | 2024-02-27 | 浙江恒亿达复合材料有限公司 | High-compression-resistance fiber-reinforced polyurethane composite board and preparation method thereof |
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