CN113736246A - Casting polyurethane for fitness equipment and preparation method thereof - Google Patents
Casting polyurethane for fitness equipment and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a casting polyurethane for fitness equipment and a preparation method thereof, wherein components such as polydimethylsiloxane diol, 1, 3-adamantane diol, toluene diisocyanate, a chain extender and the like are used as main components for polyurethane casting in the scheme, the casting polyurethane is widely applied to buildings and lives with excellent performance, but the casting polyurethane has poor heat resistance and water resistance and greatly limits the application of the casting polyurethane, so that in order to improve the comprehensive performance, the polydimethylsiloxane diol is introduced, and a hydrophobic organic silicon chain segment migrates and is enriched to the surface, so that the surface tension of the polyurethane can be greatly reduced, the hydrophobic performance is improved, and the heat resistance and the mechanical property of the polyurethane can be improved. The preparation method disclosed by the invention is reasonable in process design and simple to operate, and the prepared polyurethane not only has excellent mechanical properties, but also is improved in overall hydrophobic property and heat resistance, can be widely applied to the fields of fitness equipment, buildings and the like, and has higher practicability.
Description
Technical Field
The invention relates to the technical field of polyurethane, in particular to cast polyurethane for fitness equipment and a preparation method thereof.
Background
Polyurethane elastomers are a class of polymer synthetic materials with excellent comprehensive performance, and comprise casting polyurethane elastomers, thermoplastic polyurethane elastomers, mixing polyurethane elastomers and the like, and because of having excellent toughness, elasticity and low-temperature resistance, the polyurethane elastomers are widely applied to the fields of traffic, buildings, sports products, medical appliances and the like at present; but the application of the composite material is greatly limited due to poor heat resistance and water resistance.
Based on the situation, the pouring type polyurethane for the fitness equipment and the preparation method thereof are disclosed, so that the technical problem is solved.
Disclosure of Invention
The invention aims to provide casting polyurethane for fitness equipment and a preparation method thereof, and aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of casting polyurethane for fitness equipment comprises the following steps:
(1) mixing citric acid monohydrate, ethanol and deionized water, adding calcium nitrate tetrahydrate and diammonium hydrogen phosphate, continuously stirring, adjusting pH, adding polyethylene glycol, stirring, adding silicon carbide nanowires, reacting for 2.5-3h under heat preservation, centrifuging, collecting, sequentially washing with ethanol and deionized water, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent, washing and drying to obtain a modified silicon carbide nanowire;
(2) mixing and ultrasonically treating modified silicon carbide nanowires and tetrahydrofuran, adding octaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, ultrasonically dispersing for 20-30min, carrying out reflux reaction for 45-48h in a nitrogen atmosphere, filtering, washing, and vacuum drying to obtain pretreated silicon carbide;
(3) mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 80-85 ℃, carrying out heat preservation reaction, cooling to 45-50 ℃, adding dehydrated polyether polyol, heating to 80-85 ℃, carrying out heat preservation reaction, adding a chain extender, stirring, carrying out vacuum defoaming, pouring into a mold, curing, transferring into an oven, vulcanizing at 100-110 ℃ for 16-20h, taking out, and cooling to obtain a finished product.
The optimized scheme comprises the following steps:
(1) mixing citric acid monohydrate, ethanol and deionized water, stirring for 20-30min, adding calcium nitrate tetrahydrate and diammonium hydrogen phosphate, continuing stirring for 30-40min, adjusting pH, adding polyethylene glycol, stirring for 50-60min, adding silicon carbide nanowires, reacting for 2.5-3h under heat preservation, centrifuging, collecting, washing with ethanol and deionized water in sequence, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent for 30-40min, washing and drying to obtain a modified silicon carbide nanowire;
(2) mixing modified silicon carbide nanowires and tetrahydrofuran, performing ultrasonic treatment for 2-2.5h, adding octaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, performing ultrasonic dispersion for 20-30min, performing reflux reaction for 45-48h under a nitrogen atmosphere at the reaction temperature of 70-75 ℃, filtering, washing, and performing vacuum drying to obtain pretreated silicon carbide;
(3) mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 80-85 ℃, carrying out heat preservation reaction for 2-2.5h, cooling to 45-50 ℃, adding dehydrated polyether polyol, heating to 80-85 ℃, carrying out heat preservation reaction for 2-3h, adding a chain extender, stirring for 1-2min, pouring into a mold after vacuum defoaming, curing for 30-60min, transferring into an oven, vulcanizing for 16-20h at 110 ℃, taking out, and cooling to obtain a finished product.
In the optimized scheme, in the step (1), the preparation steps of the silicon carbide nanowire are as follows: and mixing silicon dioxide and carbon powder, transferring the mixture into an absolute ethyl alcohol solution, carrying out ultrasonic dispersion for 2-3h, drying, transferring the dried mixture into a crucible, and sintering for 2-3h to obtain the silicon carbide nanowire.
In an optimized scheme, the sintering process parameters are as follows: the sintering atmosphere is argon, the sintering temperature is 1400-1500 ℃, and the heating rate is 4-5 ℃/min.
In the optimized scheme, in the step (1), the silane coupling agent is KH-560.
In a more optimized scheme, the polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
In an optimized scheme, the polyether polyol is dehydrated in advance, and the method comprises the following steps: taking polyether polyol, dehydrating for 2-3h at the temperature of 100-110 ℃ and the pressure of 0.6KPa, and cooling to 40-50 ℃ for later use.
In the most preferred embodiment, in step (1), the pH is adjusted to 9.
According to an optimized scheme, the polyurethane is prepared by the preparation method of the casting polyurethane for the fitness equipment.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a preparation method of casting polyurethane for fitness equipment, wherein components such as polydimethylsiloxane diol, 1, 3-adamantane diol, toluene diisocyanate, chain extender and the like are used as main components for polyurethane casting in the scheme, the casting polyurethane is widely applied to buildings and lives with excellent performance, but the casting polyurethane has poor heat resistance and water resistance and greatly limits the application of the casting polyurethane, so that in order to improve the comprehensive performance, the polydimethylsiloxane diol is introduced, and a hydrophobic organic silicon chain segment migrates and gathers to the surface, so that the surface tension of the polyurethane is greatly reduced, the hydrophobic performance is improved, and the heat resistance and the mechanical performance of the polyurethane can also be improved; on the basis, rigid groups can be introduced by introducing the 1, 3-adamantanediol, so that the heat resistance and the mechanical property of the polyurethane are further improved.
Meanwhile, hydroxyapatite and silicon carbide nanowires are introduced, the hydroxyapatite is generally used in medical drug carriers or medical coatings and has excellent biocompatibility, but the hydroxyapatite is creatively applied to the field of polyurethane elastomers, so that the elastomers can be effectively reinforced, and the mechanical properties of the elastomers can be improved; however, in the conventional processing technology of polyurethane, hydroxyapatite and silicon carbide nanowires are generally used as reinforcing materials to be mixed and directly added into the components, but when the adding amount of the reinforcing materials in the polyurethane is large, the overall performance of the polyurethane is affected, and after the reinforcing materials are directly added, the silicon carbide nanowires and the hydroxyapatite are easy to agglomerate, and the mechanical performance of the whole polyurethane is also affected; aiming at the problem, the hydroxyapatite and the silicon carbide nanowires are firstly compounded, the hydroxyapatite is coated on the surfaces of the silicon carbide nanowires, the dispersing performance of the silicon carbide nanowires can be improved through the treatment, the hydroxyapatite and the silicon carbide nanowires can be compounded to form a composite reinforcing material, and the mechanical property of the polyurethane is improved to a great extent.
On the basis, octa-aminopropyl silsesquioxane is introduced, grafted to the surface of hydroxyapatite, the surface amino group of the octa-aminopropyl silsesquioxane is subjected to a crosslinking reaction with an isocyanate group in a polyurethane prepolymer, an inorganic composite reinforcing material is introduced into polyurethane in a covalent bond mode, and due to the introduction of a silicon element, the surface hydrophobic property of the polyurethane is improved.
Silicon dioxide and carbon powder are mixed and then sintered as raw materials to obtain the silicon carbide nanowire, the silicon carbide nanowire is integrally in a bead-shaped structure in series, and compared with conventional silicon carbide nanowires and silicon carbide particles, the composite reinforcing material and polyurethane can be embedded by introducing the structure, so that the mechanical property of the polyurethane is improved, the specific surface area is higher, the grafting effect of the composite reinforcing material and octaaminopropyl silsesquioxane is more excellent, and the hydrophobicity and the heat resistance of the integral polyurethane are improved more obviously.
The invention discloses a preparation method of casting polyurethane for fitness equipment, which has the advantages of reasonable process design and simple operation, and the prepared polyurethane not only has excellent mechanical property, but also improves the overall hydrophobic property and heat resistance, can be widely applied to the fields of fitness equipment, buildings and the like, and has higher practicability.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a preparation method of casting polyurethane for fitness equipment comprises the following steps:
(1) mixing silicon dioxide and carbon powder, transferring the mixture into an absolute ethyl alcohol solution, carrying out ultrasonic dispersion for 2 hours, drying, transferring the mixture into a crucible, sintering, wherein the sintering atmosphere is argon, the temperature is increased to 1400 ℃ at the temperature increase rate of 4 ℃/min, and the sintering time is 3 hours, so as to obtain the silicon carbide nanowire. The molar ratio of the carbon powder to the silicon dioxide is 1: 3;
mixing and stirring 5g of citric acid monohydrate, 50mL of ethanol and 140mL of deionized water for 20min, adding 3g of calcium nitrate tetrahydrate and 1g of diammonium hydrogen phosphate, continuously stirring for 30min, adjusting the pH to 9, adding 9.5g of polyethylene glycol, stirring for 50min, adding 8g of silicon carbide nanowires, carrying out heat preservation reaction for 2.5h, centrifugally collecting, washing by sequentially adopting ethanol and deionized water, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent for 30min, washing and drying to obtain a modified silicon carbide nanowire; the silane coupling agent is KH-560; the silane coupling agent accounts for 5% of the mass of the material A;
(2) mixing modified silicon carbide nanowires and tetrahydrofuran, performing ultrasonic treatment for 2 hours, adding octaaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, performing ultrasonic dispersion for 20 minutes, performing reflux reaction for 45 hours at 75 ℃ in a nitrogen atmosphere, filtering, washing, and performing vacuum drying to obtain pretreated silicon carbide; the mass ratio of the modified silicon carbide nanowire to the octaminopropyl silsesquioxane is 1: 5;
(3) taking polyether polyol, dehydrating for 3h at 100 ℃, and cooling to 40 ℃ for later use, wherein the pressure is 0.6 KPa.
Mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 80 ℃, carrying out heat preservation reaction for 2.5 hours, cooling to 45 ℃, adding dehydrated polyether polyol, heating to 80 ℃, carrying out heat preservation reaction for 3 hours, adding a chain extender, stirring for 2 minutes, casting into a mold after vacuum defoaming, curing for 45 minutes, transferring into an oven, vulcanizing for 20 hours at 100 ℃, taking out, and cooling to obtain a finished product. The polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
The high-performance polyurethane elastomer comprises, by mass, 65 parts of toluene diisocyanate, 10 parts of polydimethylsiloxane diol, 8 parts of 1, 3-adamantane diol, 180 parts of polyether polyol, 8 parts of pretreated silicon carbide and 6 parts of chain extender.
Example 2:
a preparation method of casting polyurethane for fitness equipment comprises the following steps:
(1) mixing silicon dioxide and carbon powder, transferring the mixture into an absolute ethyl alcohol solution, carrying out ultrasonic dispersion for 2.5h, drying, transferring the mixture into a crucible, sintering, wherein the sintering atmosphere is argon, heating to 1450 ℃ at a heating rate of 5 ℃/min, and sintering for 2.5h to obtain the silicon carbide nanowire. The molar ratio of the carbon powder to the silicon dioxide is 1: 3;
mixing and stirring 5g of citric acid monohydrate, 50mL of ethanol and 140mL of deionized water for 25min, adding 3g of calcium nitrate tetrahydrate and 1g of diammonium hydrogen phosphate, continuously stirring for 35min, adjusting the pH to 9, adding 9.5g of polyethylene glycol, stirring for 55min, adding 8g of silicon carbide nanowires, carrying out heat preservation reaction for 2.5h, centrifugally collecting, washing by sequentially adopting ethanol and deionized water, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent for 35min, washing and drying to obtain a modified silicon carbide nanowire; the silane coupling agent is KH-560; the silane coupling agent accounts for 5% of the mass of the material A;
(2) taking modified silicon carbide nanowires and tetrahydrofuran, mixing and ultrasonically treating for 2.2h, adding octaaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, ultrasonically dispersing for 25min, carrying out reflux reaction for 47h under the nitrogen atmosphere, wherein the reaction temperature is 72 ℃, filtering, washing, and vacuum drying to obtain pretreated silicon carbide; the mass ratio of the modified silicon carbide nanowire to the octaminopropyl silsesquioxane is 1: 5;
(3) taking polyether polyol, dehydrating at 105 ℃ for 2.5h under the pressure of 0.6KPa, and cooling to 45 ℃ for later use.
Mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 82 ℃, carrying out heat preservation reaction for 2.2 hours, cooling to 48 ℃, adding dehydrated polyether polyol, heating to 82 ℃, carrying out heat preservation reaction for 2.5 hours, adding a chain extender, stirring for 2 minutes, casting into a mold after vacuum defoaming, curing for 45 minutes, transferring into an oven, vulcanizing for 18 hours at 105 ℃, taking out, and cooling to obtain a finished product. The polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
The high-performance polyurethane elastomer comprises, by mass, 65 parts of toluene diisocyanate, 10 parts of polydimethylsiloxane diol, 8 parts of 1, 3-adamantane diol, 180 parts of polyether polyol, 8 parts of pretreated silicon carbide and 6 parts of chain extender.
Example 3:
a preparation method of casting polyurethane for fitness equipment comprises the following steps:
(1) mixing silicon dioxide and carbon powder, transferring the mixture into an absolute ethyl alcohol solution, carrying out ultrasonic dispersion for 3 hours, drying, transferring the mixture into a crucible, sintering, wherein the sintering atmosphere is argon, the temperature is increased to 1500 ℃ at the temperature increase rate of 5 ℃/min, and the sintering time is 2 hours, so as to obtain the silicon carbide nanowire. The molar ratio of the carbon powder to the silicon dioxide is 1: 3;
mixing and stirring 5g of citric acid monohydrate, 50mL of ethanol and 140mL of deionized water for 30min, adding 3g of calcium nitrate tetrahydrate and 1g of diammonium hydrogen phosphate, continuously stirring for 40min, adjusting the pH to 9, adding 9.5g of polyethylene glycol, stirring for 60min, adding 8g of silicon carbide nanowires, carrying out heat preservation reaction for 3h, centrifugally collecting, washing by sequentially adopting ethanol and deionized water, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent for 40min, washing and drying to obtain a modified silicon carbide nanowire; the silane coupling agent is KH-560; the silane coupling agent accounts for 5% of the mass of the material A;
(2) mixing and ultrasonically treating modified silicon carbide nanowires and tetrahydrofuran for 2.5h, adding octaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, ultrasonically dispersing for 30min, carrying out reflux reaction for 48h under a nitrogen atmosphere at the reaction temperature of 75 ℃, filtering, washing, and vacuum drying to obtain pretreated silicon carbide; the mass ratio of the modified silicon carbide nanowire to the octaminopropyl silsesquioxane is 1: 5;
(3) taking polyether polyol, dehydrating for 2h at 110 ℃, and cooling to 50 ℃ for later use, wherein the pressure is 0.6 KPa.
Mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 85 ℃, carrying out heat preservation reaction for 2 hours, cooling to 50 ℃, adding dehydrated polyether polyol, heating to 85 ℃, carrying out heat preservation reaction for 2 hours, adding a chain extender, stirring for 2 minutes, pouring into a mold after vacuum defoaming, curing for 45 minutes, transferring into an oven, vulcanizing for 16 hours at 110 ℃, taking out, and cooling to obtain a finished product. The polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
The high-performance polyurethane elastomer comprises, by mass, 65 parts of toluene diisocyanate, 10 parts of polydimethylsiloxane diol, 8 parts of 1, 3-adamantane diol, 180 parts of polyether polyol, 8 parts of pretreated silicon carbide and 6 parts of chain extender.
Comparative example 1:
a preparation method of casting polyurethane for fitness equipment comprises the following steps:
(1) mixing silicon dioxide and carbon powder, transferring the mixture into an absolute ethyl alcohol solution, carrying out ultrasonic dispersion for 2.5h, drying, transferring the mixture into a crucible, sintering, wherein the sintering atmosphere is argon, heating to 1450 ℃ at a heating rate of 5 ℃/min, and sintering for 2.5h to obtain the silicon carbide nanowire. The molar ratio of the carbon powder to the silicon dioxide is 1: 3;
mixing and stirring 5g of citric acid monohydrate, 50mL of ethanol and 140mL of deionized water for 25min, adding 3g of calcium nitrate tetrahydrate and 1g of diammonium hydrogen phosphate, continuously stirring for 35min, adjusting the pH to 9, adding 9.5g of polyethylene glycol, stirring for 55min, adding 8g of silicon carbide nanowires, carrying out heat preservation reaction for 2.5h, centrifugally collecting, washing by sequentially adopting ethanol and deionized water, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent for 35min, washing and drying to obtain a modified silicon carbide nanowire; the silane coupling agent is KH-560; the silane coupling agent accounts for 5% of the mass of the material A;
(2) taking modified silicon carbide nanowires and tetrahydrofuran, mixing and ultrasonically treating for 2.2h, adding octaaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, ultrasonically dispersing for 25min, carrying out reflux reaction for 47h under the nitrogen atmosphere, wherein the reaction temperature is 72 ℃, filtering, washing, and vacuum drying to obtain pretreated silicon carbide; the mass ratio of the modified silicon carbide nanowire to the octaminopropyl silsesquioxane is 1: 5;
(3) taking polyether polyol, dehydrating at 105 ℃ for 2.5h under the pressure of 0.6KPa, and cooling to 45 ℃ for later use.
Mixing pretreated silicon carbide and polydimethylsiloxane diol, adding toluene diisocyanate, heating to 82 ℃, carrying out heat preservation reaction for 2.2 hours, cooling to 48 ℃, adding dehydrated polyether polyol, heating to 82 ℃, carrying out heat preservation reaction for 2.5 hours, adding a chain extender, stirring for 2 minutes, carrying out vacuum defoaming, pouring into a mold, curing for 45 minutes, transferring into an oven, vulcanizing at 105 ℃ for 18 hours, taking out, and cooling to obtain a finished product. The polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
The high-performance polyurethane sealant comprises the following components, by mass, 65 parts of toluene diisocyanate, 10 parts of polydimethylsiloxane diol, 180 parts of polyether polyol, 8 parts of pretreated silicon carbide and 6 parts of chain extender.
Comparative example 1 a process modification was made on the basis of example 2, and 1, 3-adamantanediol was not introduced in comparative example 1, and the contents of the remaining components and the process parameters were identical to those in example 2.
Comparative example 2:
a preparation method of casting polyurethane for fitness equipment comprises the following steps:
(1) mixing silicon dioxide and carbon powder, transferring the mixture into an absolute ethyl alcohol solution, carrying out ultrasonic dispersion for 2.5h, drying, transferring the mixture into a crucible, sintering, wherein the sintering atmosphere is argon, heating to 1450 ℃ at a heating rate of 5 ℃/min, and sintering for 2.5h to obtain the silicon carbide nanowire. The molar ratio of the carbon powder to the silicon dioxide is 1: 3;
mixing and stirring 5g of citric acid monohydrate, 50mL of ethanol and 140mL of deionized water for 25min, adding 3g of calcium nitrate tetrahydrate and 1g of diammonium hydrogen phosphate, continuously stirring for 35min, adjusting the pH to 9, adding 9.5g of polyethylene glycol, stirring for 55min, adding 8g of silicon carbide nanowires, carrying out heat preservation reaction for 2.5h, centrifugally collecting, washing by sequentially adopting ethanol and deionized water, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent for 35min, and washing and drying to obtain pretreated silicon carbide; the silane coupling agent is KH-560; the silane coupling agent accounts for 5% of the mass of the material A;
(2) taking polyether polyol, dehydrating at 105 ℃ for 2.5h under the pressure of 0.6KPa, and cooling to 45 ℃ for later use.
Mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 82 ℃, carrying out heat preservation reaction for 2.2 hours, cooling to 48 ℃, adding dehydrated polyether polyol, heating to 82 ℃, carrying out heat preservation reaction for 2.5 hours, adding a chain extender, stirring for 2 minutes, casting into a mold after vacuum defoaming, curing for 45 minutes, transferring into an oven, vulcanizing for 18 hours at 105 ℃, taking out, and cooling to obtain a finished product. The polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
The high-performance polyurethane elastomer comprises, by mass, 65 parts of toluene diisocyanate, 10 parts of polydimethylsiloxane diol, 8 parts of 1, 3-adamantane diol, 180 parts of polyether polyol, 8 parts of pretreated silicon carbide and 6 parts of chain extender.
Comparative example 2 a process modification was made on the basis of example 2, in comparative example 2 no octaaminopropyl silsesquioxane was introduced and the remaining component content and process parameters were in accordance with example 2.
Comparative example 3:
a preparation method of casting polyurethane for fitness equipment comprises the following steps:
(1) mixing and stirring 5g of citric acid monohydrate, 50mL of ethanol and 140mL of deionized water for 25min, adding 3g of calcium nitrate tetrahydrate and 1g of diammonium phosphate, continuously stirring for 35min, adjusting the pH to 9, adding 9.5g of polyethylene glycol, stirring for 55min, adding 8g of silicon carbide microspheres, carrying out heat preservation reaction for 2.5h, centrifugally collecting, washing by sequentially adopting ethanol and deionized water, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent for 35min, washing and drying to obtain modified silicon carbide; the silane coupling agent is KH-560; the silane coupling agent accounts for 5% of the mass of the material A;
(2) taking modified silicon carbide and tetrahydrofuran, mixing and ultrasonically treating for 2.2h, adding octaaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, ultrasonically dispersing for 25min, carrying out reflux reaction for 47h under the nitrogen atmosphere, wherein the reaction temperature is 72 ℃, filtering, washing, and vacuum drying to obtain pretreated silicon carbide; the mass ratio of the modified silicon carbide to the octaminopropyl silsesquioxane is 1: 5;
(3) taking polyether polyol, dehydrating at 105 ℃ for 2.5h under the pressure of 0.6KPa, and cooling to 45 ℃ for later use.
Mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 82 ℃, carrying out heat preservation reaction for 2.2 hours, cooling to 48 ℃, adding dehydrated polyether polyol, heating to 82 ℃, carrying out heat preservation reaction for 2.5 hours, adding a chain extender, stirring for 2 minutes, casting into a mold after vacuum defoaming, curing for 45 minutes, transferring into an oven, vulcanizing for 18 hours at 105 ℃, taking out, and cooling to obtain a finished product. The polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
The high-performance polyurethane elastomer comprises, by mass, 65 parts of toluene diisocyanate, 10 parts of polydimethylsiloxane diol, 8 parts of 1, 3-adamantane diol, 180 parts of polyether polyol, 8 parts of pretreated silicon carbide and 6 parts of chain extender.
Comparative example 3 a process change was made on the basis of example 2, in comparative example 3 conventional silicon carbide particle microspheres were used, and the content of the remaining components and the process parameters were the same as those of example 2.
Comparative example 4:
a preparation method of casting polyurethane for fitness equipment comprises the following steps:
(1) mixing silicon dioxide and carbon powder, transferring the mixture into an absolute ethyl alcohol solution, carrying out ultrasonic dispersion for 2.5h, drying, transferring the mixture into a crucible, sintering, wherein the sintering atmosphere is argon, heating to 1450 ℃ at a heating rate of 5 ℃/min, and sintering for 2.5h to obtain the silicon carbide nanowire. The molar ratio of the carbon powder to the silicon dioxide is 1: 3;
mixing and stirring the silicon carbide nanowires, the hydroxyapatite and the silane coupling agent for 35min, and washing and drying to obtain a mixture; the silane coupling agent is KH-560; the silane coupling agent is 5% of the mixed mass of the silicon carbide nanowire and the hydroxyapatite; the mass ratio of the silicon carbide nano wire to the hydroxyapatite is 1: 1.
(2) mixing the mixture and tetrahydrofuran, performing ultrasonic treatment for 2.2h, adding octaaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, performing ultrasonic dispersion for 25min, performing reflux reaction for 47h in a nitrogen atmosphere at the reaction temperature of 72 ℃, filtering, washing, and performing vacuum drying to obtain a pretreated mixture; the mass ratio of the mixture to the octaaminopropyl silsesquioxane is 1: 5;
(3) taking polyether polyol, dehydrating at 105 ℃ for 2.5h under the pressure of 0.6KPa, and cooling to 45 ℃ for later use.
Taking the pretreated mixture, polydimethylsiloxane diol and 1, 3-adamantanediol, mixing, adding toluene diisocyanate, heating to 82 ℃, carrying out heat preservation reaction for 2.2 hours, cooling to 48 ℃, adding dehydrated polyether polyol, heating to 82 ℃, carrying out heat preservation reaction for 2.5 hours, adding a chain extender, stirring for 2 minutes, casting into a mold after vacuum defoaming, curing for 45 minutes, transferring into an oven, vulcanizing for 18 hours at 105 ℃, taking out, and cooling to obtain a finished product. The polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
The anti-blocking agent comprises, by mass, 65 parts of toluene diisocyanate, 10 parts of polydimethylsiloxane diol, 8 parts of 1, 3-adamantane diol, 180 parts of polyether polyol, 8 parts of a pretreatment mixture and 6 parts of a chain extender.
Comparative example 4 a process change was made on the basis of example 2, in comparative example 3 silicon carbide nanowires and hydroxyapatite were directly added, and the contents of the remaining components and process parameters were identical to those of example 2.
Detection experiment:
the following property tests were carried out on the polyurethane elastomers prepared in examples 1 to 3 and comparative examples 1 to 4, respectively:
1. an electronic universal testing machine is adopted to detect the mechanical property of the sample, the tensile strength is measured according to the GB/T528-2009 method, and the measured sample is a dumbbell-shaped sample; the elongation at break is determined according to the method of GB/1040-.
2. The static water contact angle of the samples was measured using a contact angle measuring instrument, and each sample was measured at 10 points at intervals, and the average value was calculated and recorded.
3. And (3) testing the thermal stability of the sample by adopting a thermogravimetric analyzer, heating up under the nitrogen atmosphere at a heating rate of 10 ℃/min, detecting the temperature of 10% and 70% of weight loss and recording.
And (4) conclusion: the invention discloses a preparation method of casting polyurethane for fitness equipment, which has the advantages of reasonable process design and simple operation, and the prepared polyurethane not only has excellent mechanical property, but also improves the overall hydrophobic property and heat resistance, can be widely applied to the fields of fitness equipment, buildings and the like, and has higher practicability.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of casting polyurethane for fitness equipment is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing citric acid monohydrate, ethanol and deionized water, adding calcium nitrate tetrahydrate and diammonium hydrogen phosphate, continuously stirring, adjusting pH, adding polyethylene glycol, stirring, adding silicon carbide nanowires, reacting for 2.5-3h under heat preservation, centrifuging, collecting, sequentially washing with ethanol and deionized water, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent, washing and drying to obtain a modified silicon carbide nanowire;
(2) mixing and ultrasonically treating modified silicon carbide nanowires and tetrahydrofuran, adding octaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, ultrasonically dispersing for 20-30min, carrying out reflux reaction for 45-48h in a nitrogen atmosphere, filtering, washing, and vacuum drying to obtain pretreated silicon carbide;
(3) mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 80-85 ℃, carrying out heat preservation reaction, cooling to 45-50 ℃, adding dehydrated polyether polyol, heating to 80-85 ℃, carrying out heat preservation reaction, adding a chain extender, stirring, carrying out vacuum defoaming, pouring into a mold, curing, transferring into an oven, vulcanizing at 100-110 ℃ for 16-20h, taking out, and cooling to obtain a finished product.
2. The method for preparing the casting polyurethane for the fitness equipment according to claim 1, wherein the casting polyurethane comprises the following steps: the method comprises the following steps:
(1) mixing citric acid monohydrate, ethanol and deionized water, stirring for 20-30min, adding calcium nitrate tetrahydrate and diammonium hydrogen phosphate, continuing stirring for 30-40min, adjusting pH, adding polyethylene glycol, stirring for 50-60min, adding silicon carbide nanowires, reacting for 2.5-3h under heat preservation, centrifuging, collecting, washing with ethanol and deionized water in sequence, and drying to obtain a material A;
mixing and stirring the material A and a silane coupling agent for 30-40min, washing and drying to obtain a modified silicon carbide nanowire;
(2) mixing modified silicon carbide nanowires and tetrahydrofuran, performing ultrasonic treatment for 2-2.5h, adding octaminopropyl silsesquioxane and N' N-dicyclohexylcarbodiimide, performing ultrasonic dispersion for 20-30min, performing reflux reaction for 45-48h under a nitrogen atmosphere at the reaction temperature of 70-75 ℃, filtering, washing, and performing vacuum drying to obtain pretreated silicon carbide;
(3) mixing pretreated silicon carbide, polydimethylsiloxane diol and 1, 3-adamantanediol, adding toluene diisocyanate, heating to 80-85 ℃, carrying out heat preservation reaction for 2-2.5h, cooling to 45-50 ℃, adding dehydrated polyether polyol, heating to 80-85 ℃, carrying out heat preservation reaction for 2-3h, adding a chain extender, stirring for 1-2min, pouring into a mold after vacuum defoaming, curing for 30-60min, transferring into an oven, vulcanizing for 16-20h at 110 ℃, taking out, and cooling to obtain a finished product.
3. The method for preparing the casting polyurethane for the fitness equipment according to claim 2, wherein the casting polyurethane comprises the following steps: in the step (1), the preparation steps of the silicon carbide nanowire are as follows: and mixing silicon dioxide and carbon powder, transferring the mixture into an absolute ethyl alcohol solution, carrying out ultrasonic dispersion for 2-3h, drying, transferring the dried mixture into a crucible, and sintering for 2-3h to obtain the silicon carbide nanowire.
4. The method of preparing a cast polyurethane for fitness equipment according to claim 3, wherein the cast polyurethane comprises the following steps: the sintering process parameters are as follows: the sintering atmosphere is argon, the sintering temperature is 1400-1500 ℃, and the heating rate is 4-5 ℃/min.
5. The method for preparing the casting polyurethane for the fitness equipment according to claim 2, wherein the casting polyurethane comprises the following steps: in the step (1), the silane coupling agent is KH-560.
6. The method for preparing the casting polyurethane for the fitness equipment according to claim 2, wherein the casting polyurethane comprises the following steps: the polyether polyol is polytetrahydrofuran ether glycol; the chain extender is MOCA.
7. The method of preparing a cast polyurethane for fitness equipment according to claim 6, wherein the cast polyurethane comprises the following steps: the polyether polyol is dehydrated in advance, and the method comprises the following steps: taking polyether polyol, dehydrating for 2-3h at the temperature of 100-110 ℃ and the pressure of 0.6KPa, and cooling to 40-50 ℃ for later use.
8. The method for preparing the casting polyurethane for the fitness equipment according to claim 2, wherein the casting polyurethane comprises the following steps: in step (1), the pH is adjusted to 9.
9. Polyurethane produced by the process for the production of a cast polyurethane for fitness equipment according to any one of claims 1 to 8.
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| US3746692A (en) * | 1971-10-21 | 1973-07-17 | Dow Chemical Co | Rigid polyurethane compositions |
| CN104140666A (en) * | 2014-07-30 | 2014-11-12 | 东莞市吉鑫高分子科技有限公司 | High-abrasion-resistance transparent thermoplastic polyurethane elastomer for ball film and manufacturing method thereof |
| CN104177581A (en) * | 2013-05-27 | 2014-12-03 | 拜耳材料科技(中国)有限公司 | Polyurethane composition for polyurethane composite material |
| WO2015159875A1 (en) * | 2014-04-15 | 2015-10-22 | 宇部興産株式会社 | Cast-molded heat-curable polyurethane elastomer |
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Patent Citations (4)
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| US3746692A (en) * | 1971-10-21 | 1973-07-17 | Dow Chemical Co | Rigid polyurethane compositions |
| CN104177581A (en) * | 2013-05-27 | 2014-12-03 | 拜耳材料科技(中国)有限公司 | Polyurethane composition for polyurethane composite material |
| WO2015159875A1 (en) * | 2014-04-15 | 2015-10-22 | 宇部興産株式会社 | Cast-molded heat-curable polyurethane elastomer |
| CN104140666A (en) * | 2014-07-30 | 2014-11-12 | 东莞市吉鑫高分子科技有限公司 | High-abrasion-resistance transparent thermoplastic polyurethane elastomer for ball film and manufacturing method thereof |
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