CN112250828A - High-insulation low-temperature-expansion-resistant flame-retardant polyurethane material and preparation method and application thereof - Google Patents
High-insulation low-temperature-expansion-resistant flame-retardant polyurethane material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material, and a preparation method and application thereof, wherein the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material comprises the following components in percentage by mass: 20-60% of low molecular weight polyol, 0-30% of chain extender, 0.1-4% of catalyst, 0.1-2.5% of antioxidant, 0.1-2.5% of defoaming agent, 0.1-2.5% of wetting dispersant, 5-70% of flame retardant, 5-40% of plasticizer, 0-30% of filler and 1-30% of curing agent. The preparation process of the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material is simple, the operation and the control are convenient, the curing time is controllable, and the production process is pollution-free. The material can be used for preventing the fire of cables and through holes in building walls, cable channels and traffic tracks, and can also be used for electrical insulation packaging materials, electrical component pouring sealants, waterproof coatings, anticorrosive coatings, cold-resistant coatings, fireproof expansion sealing elements, adhesives and the like.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material, and a preparation method and application thereof.
Background
Fire protection of power cables in the fields of construction and public transport is an important research topic in the field of fire protection. In the prior art, when the fire-resistant cable is formed, the core material is coated with the fire-resistant insulating tape, so that the cost is increased, and time and labor are wasted. In addition, the fire-proof coating is coated on the surface of the cable, and the flame-retardant wrapping tape is coated, so that the fire hazard can be effectively reduced, and the spread and the propagation of flame can be prevented. However, the traditional cable fireproof coating and the flame-retardant wrapping tape have poor lasting adhesion to the cable, poor fire resistance and short service life, the flame-retardant effect of the cable is weakened after long-term operation, repeated construction is needed, and the operation and maintenance cost and burden of the cable are increased.
In addition, in the fields of building engineering, automobile industry, rail transit and the like, through holes formed when cables, optical cables, bridges, air pipes, groove boxes and the like penetrate through walls and floor slabs need to be separated in a fireproof manner by using fireproof sealant. This not only requires the sealant to have high flame retardancy, but also generally requires high insulation. The common fireproof sealant in the prior art mainly comprises silicone, acrylic acid and polysulfide sealant, and has the defects of poor flame retardant effect, long curing time, poor high and low temperature resistance, poor adhesion to certain substrates, low insulativity and the like.
The polyurethane material is a polymer containing a plurality of carbamate groups (-NHCOO-) on a macromolecular main chain, has the characteristics of higher strength and elasticity, wear resistance, tear resistance, oil resistance, chemical corrosion resistance, high curing speed, large adhesive force, good high and low temperature resistance and the like, and is widely applied to the fields of coatings, adhesives, elastomers, fibers, synthetic leather and foaming materials. However, common polyurethane materials are easy to burn, and have great fire safety hidden dangers when being applied to cables and through holes in building walls, cable channels and traffic tracks for fire prevention. Although the halogen-based flame retardant can be added to obtain excellent flame retardant performance, the halogen-based flame retardant is not environment-friendly, and a large amount of toxic halogen-containing gas can be released in a fire. Therefore, the preparation of an environment-friendly and efficient flame-retardant polyurethane material has become a problem to be solved urgently.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material and a preparation method thereof, which are used for preventing the fire of cables and through holes in building walls, cable channels and traffic tracks, and can also be used for electrical insulation packaging materials, electrical component pouring sealant, waterproof coating, anticorrosive coating, cold-resistant coating, fireproof expansion sealing elements, adhesives and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material comprises the following components in percentage by mass:
preferably, the low molecular weight polyol is at least one of polyester polyol, polyether polyol, hydroxyl-terminated polybutadiene, hydroxyl-terminated nitrile rubber, polycaprolactone polyol, polycarbonate polyol, acrylic polyol, silicone polyol, fluorinated polyol, hydride of liquid polyisoprene having hydroxyl groups, hydride of liquid polybutadiene having hydroxyl groups, castor oil and castor oil derivative.
Preferably, the polyester polyol is at least one of polyethylene glycol adipate glycol, polyethylene-propylene glycol adipate glycol, polyethylene-diethylene glycol adipate glycol, and 1, 4-butylene glycol adipate glycol.
Preferably, the polyether polyol is at least one of polyoxypropylene diol, polyoxypropylene triol and polytetrahydrofuran polyol.
Preferably, the chain extender is one or more of ethylene glycol, 1, 4-butanediol, diethylene glycol, dipropylene glycol, 1, 4-bis (hydroxyethoxybenzene), triethanolamine, diethyltoluenediamine, dimethylthiotoluenediamine, 4 '-bis-sec-aminodiphenylmethane, 3' -dichloro-4, 4-diaminodiphenylmethane and methylcyclohexanediamine.
Preferably, the catalyst is one or more of triethylene diamine, dibutyltin dilaurate, stannous octoate, diethylenetriamine, N-ethyl morpholine, zinc naphthenate and organic bismuth.
Preferably, the antioxidant is one or more of antioxidant 1010, antioxidant 245, antioxidant 1035 and antioxidant 1076.
Preferably, the defoaming agent is one or two of BYK-088 and KF 1023.
Preferably, the wetting dispersant is one or two of BYK-110 and BYK 190.
Preferably, the flame retardant is a halogen-free flame retardant, and the mass percent of the halogen-free flame retardant is 10-50% by mass.
Preferably, the halogen-free flame retardant is at least one of magnesium hydroxide, aluminum hydroxide, zinc borate, high-polymerization-degree ammonium polyphosphate, melamine salt, expandable graphite, polysiloxane, pentaerythritol and di-acetal, tri-acetal and diethyl aluminum hypophosphite thereof.
Preferably, the plasticizer is a plasticizer containing no hydroxyl group.
Preferably, the plasticizer is at least one of dioctyl terephthalate DOTP, 1, 2-cyclohexanedicarboxylic acid di (isononyl) ester, ether-esters, medium molecular weight polyesters, low molecular weight polyesters, alkyl benzene sulfonates, phthalates, trimellitates, and phosphate plasticizers
Preferably, the phthalate-based plasticizer is at least one of diisononyl phthalate and diundecyl phthalate.
Preferably, the trimellitate plasticizer is at least one of trioctyl trimellitate, tri-ethylhexyl trimellitate, and tri-isodecyl trimellitate.
Preferably, the phosphate-based plasticizer is at least one of tricresyl phosphate, triisopropylphenyl phosphate, diphenylisooctyl phenyl phosphate, diphenylisodecyl phosphate, trixylenyl phosphate, triphenyl phosphate, triethyl phosphate, bisphenol a bis (diphenyl phosphate), resorcinol bis (diphenyl phosphate), and tributyl phosphate.
Preferably, the filler is at least one of carbon black, white carbon black, talc powder, calcium carbonate, hydrotalcite, kaolin and china clay.
Preferably, the curing agent is at least one of MDI, polymeric MDI, liquefied MDI, HDI trimer, HDI biuret, PPDI, NDI and IPDI trimer.
The invention also aims to provide a preparation method of the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material, which comprises the following steps:
(1) weighing the raw material components according to the mass percentage;
(2) drying the flame retardant, the filler and the antioxidant anti-aging agent at 100-120 ℃ for 12-48 hours;
(3) adding low molecular weight polyol, a plasticizer, a defoaming agent, a catalyst, a wetting dispersant and a chain extender into a reactor, and uniformly stirring;
(4) adding the dried flame retardant, the filler and the antioxidant into a reactor, and starting vacuum and stirring;
(5) raising the temperature, controlling the temperature in the reactor to be 90-110 ℃, and stirring for 0.5-10 hours under a vacuum condition;
(6) after stirring, stopping vacuumizing, cooling to below 40-70 ℃, and discharging to obtain a polyurethane resin mixture;
(7) and uniformly mixing the polyurethane resin mixture and the curing agent according to the mass ratio of the polyurethane resin mixture to the curing agent of 100: 1-100: 30, and discharging to obtain the high-insulation low-temperature-resistant flame-retardant polyurethane material.
Preferably, in the step (3), the stirring speed of the stirring is 1rpm to 200rpm
Preferably, in the step (5), the temperature increase specifically includes a first temperature increase stage and a second temperature increase stage; the initial temperature of the first temperature rise stage is between room temperature and 40 ℃, the termination temperature is between 70 and 80 ℃, and the temperature rise rate of the first temperature rise stage is between 0.1 and 20 ℃/min; the initial temperature of the second temperature rise stage is 70-80 ℃, the termination temperature is 90-110 ℃, and the temperature rise rate is 0.1-20 ℃/min.
Preferably, in the step (5), the vacuum degree under the vacuum condition is-0.08 to-0.1 MPa, and the stirring speed of the stirring is 1rpm to 200 rpm.
Preferably, in the step (6), the cooling rate of the cooling is 0.1-20 ℃/min.
Preferably, in the step (7), the polyurethane resin mixture and the curing agent are stirred and vacuum defoamed during uniform mixing.
Preferably, in the step (7), after discharging, curing for 2-10 hours in an oven at 40-100 ℃ to obtain the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material.
The third purpose of the invention is to provide the application of the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material in fire prevention of cables and through holes in building walls, cable channels and traffic tracks.
The fourth purpose of the invention is to provide the application of the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material in electric insulation packaging materials, electric component pouring sealants, waterproof coatings, anticorrosive coatings, cold-resistant coatings, fireproof expansion sealing elements and adhesives.
The invention has the beneficial effects that:
(1) the high-insulation low-temperature-resistant expansion flame-retardant polyurethane material provided by the invention can be instantly and obviously expanded and foamed under the action of heat or open fire, so that the fire spread is prevented, and a good fireproof and heat-insulating effect can be achieved.
(2) The high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material provided by the invention has the advantages of good lasting adhesion to cables, long service life, good air tightness and insulativity at normal temperature and low temperature, and good acid and alkali resistance and chemical corrosion resistance.
(3) The invention has simple preparation process, convenient operation and control, controllable curing time and no pollution in the production process.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is described in further detail below. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material provided by the invention is prepared from low-molecular-weight polyol, a chain extender, a catalyst, an antioxidant, a defoaming agent, a wetting dispersant, a flame retardant, a plasticizer, a filler and a curing agent. The high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material comprises, by mass, 20-60% of low-molecular-weight polyol, 0-30% of chain extender, 0.1-4% of catalyst, 0.1-2.5% of antioxidant, 0.1-2.5% of defoaming agent, 0.1-2.5% of wetting dispersant, 5-70% of flame retardant, 5-40% of plasticizer, 0-30% of filler and 1-30% of curing agent. The flame retardant is preferably a halogen-free flame retardant, and when the flame retardant is a halogen-free flame retardant, the mass ratio of the flame retardant is 10-50%; the plasticizer is a plasticizer containing no hydroxyl group. The high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material provided by the invention can be used for preventing fire of cables and through holes in building walls, cable channels and traffic tracks, and can also be used for electric insulation packaging materials, electric component pouring sealants, waterproof, anticorrosion, cold-resistant, fireproof coatings, fireproof expansion sealing elements, adhesives and the like. The high-insulation low-temperature-resistant expansion flame-retardant polyurethane material provided by the invention can be instantly and obviously expanded and foamed under the action of heat or open fire, prevents fire from spreading, has good fireproof and heat-insulating effects, has good lasting adhesive force on substrates such as cables, metals, concrete and the like, is long in service life, good in normal-temperature and low-temperature air tightness and insulativity, and good in acid and alkali resistance and chemical corrosion resistance.
The following is a detailed description of the components of the high-insulation, low-temperature expansion-resistant and flame-retardant polyurethane material provided by the present invention.
The low molecular weight polyol in the present invention is preferably at least one of polyester polyol, polyether polyol, hydroxyl-terminated polybutadiene, hydroxyl-terminated nitrile rubber, polycaprolactone polyol, polycarbonate polyol, acrylic polyol, silicone polyol, fluorinated polyol, hydride of liquid polyisoprene having hydroxyl group, hydride of liquid polybutadiene having hydroxyl group, castor oil and castor oil derivative.
The polyester polyol in the present invention is preferably at least one of polyethylene adipate glycol, polyethylene-propylene adipate glycol, polyethylene-diethylene adipate glycol, and 1, 4-butylene adipate glycol.
The polyether polyol in the present invention is preferably at least one of polyoxypropylene diol, polyoxypropylene triol and polytetrahydrofuran polyol.
The chain extender in the present invention is preferably one or more of ethylene glycol, 1, 4-butanediol, diethylene glycol, dipropylene glycol, 1, 4-bis (hydroxyethoxybenzene), triethanolamine, diethyltoluenediamine, dimethylthiotoluenediamine, 4 '-bis-sec-butylaminodiphenylmethane, 3' -dichloro-4, 4-diaminodiphenylmethane, and methylcyclohexanediamine.
The catalyst in the invention is preferably one or more than two of triethylene diamine, dibutyltin dilaurate, stannous octoate, diethylenetriamine, N-ethyl morpholine, zinc naphthenate and organic bismuth.
The antioxidant in the present invention is preferably one or more of antioxidant 1010, antioxidant 245, antioxidant 1035, and antioxidant 1076.
The antifoaming agent in the present invention is preferably one or both of BYK-088 and KF 1023.
The wetting dispersant in the present invention is preferably one or both of BYK-110 and BYK 190.
The halogen-free flame retardant in the invention is preferably at least one of magnesium hydroxide, aluminum hydroxide, zinc borate, ammonium polyphosphate with high polymerization degree, melamine salt, expandable graphite, polysiloxane, pentaerythritol and di-acetal, tri-acetal and diethyl aluminum hypophosphite thereof.
The plasticizer in the present invention is preferably at least one of dioctyl terephthalate DOTP, 1, 2-cyclohexanedicarboxylic acid di (isononyl) ester, ether-esters, medium molecular weight polyesters, low molecular weight polyesters, alkyl benzene sulfonates, phthalates, trimellitates, and phosphate plasticizers. Wherein the phthalate plasticizer is at least one of diisononyl phthalate and di (undecyl) phthalate; the trimellitate plasticizer is at least one of trioctyl trimellitate, tri-ethylhexyl trimellitate and tri-isodecyl trimellitate; the phosphate plasticizer is at least one of tricresyl phosphate, triisopropylphenyl phosphate, diphenylisooctyl phenyl phosphate, diphenylisodecyl phosphate, trixylenyl phosphate, triphenyl phosphate, triethyl phosphate, bisphenol A bis (diphenyl phosphate), resorcinol bis (diphenyl phosphate), and tributyl phosphate.
The filler in the invention is at least one of carbon black, white carbon black, talcum powder, calcium carbonate, hydrotalcite, kaolin and argil.
The curing agent in the present invention is preferably at least one of MDI, polymeric MDI, liquefied MDI, HDI trimer, HDI biuret, PPDI, NDI and IPDI trimer.
The preparation method of the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material provided by the invention comprises the following steps:
(1) weighing the raw material components (the raw material components) according to the mass percentage;
(2) drying the flame retardant, the filler and the antioxidant anti-aging agent at 100-120 ℃ for 12-48 hours;
(3) adding low molecular weight polyol, a plasticizer, a defoaming agent, a catalyst, a wetting dispersant and a chain extender into a reactor, and uniformly stirring at a stirring speed of 1-200 rpm;
(4) adding the dried flame retardant, the filler and the antioxidant into a reactor, and starting vacuum and stirring;
(5) raising the temperature, and stirring for 0.5-10 hours under the vacuum condition of-0.08-0.1 MPa and the stirring speed of 1-200 rpm under the condition that the temperature in the reactor is controlled to be 90-110 ℃; the temperature rise is realized by dividing into two temperature rise stages, wherein the initial temperature of the first temperature rise stage is room temperature to 40 ℃, the termination temperature is 70 to 80 ℃, and the temperature rise rate of the first temperature rise stage is 0.1 to 20 ℃/min; the initial temperature of the second temperature rise stage is 70-80 ℃, the termination temperature is 90-110 ℃, and the temperature rise rate is 0.1-20 ℃/min.
(6) After stirring, stopping vacuumizing, cooling to below 40-70 ℃ at a cooling rate of 0.1-20 ℃/min, and discharging to obtain a polyurethane resin mixture;
(7) uniformly mixing the polyurethane resin mixture and the curing agent according to the mass ratio of 100: 1-100: 30 (polyurethane resin mixture: curing agent), and discharging.
In the step (7), after the polyurethane resin mixture and the curing agent are uniformly mixed and discharged, the mixture is sealed and packaged, is used as a flame-retardant polyurethane sealant, and can be cured in a use state. Or after discharging, placing the material in an oven at 40-100 ℃ for curing for 2-10 hours to prepare the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material.
The preparation process is simple, the operation and control are convenient, the curing time is controllable, and the production process is pollution-free.
The present invention will be specifically described below with reference to specific examples.
Example 1:
the raw materials and the preparation process of the polyurethane material with high insulation and low temperature expansion resistance comprise:
50g of hydroxyl-terminated polybutadiene, 25g of polyoxypropylene glycol, 25g of castor oil, 100g of triisopropylphenyl phosphate, 25g of trioctyl trimellitate, 3g of BYK-088, 2g of dibutyltin dilaurate, 3g of BYK-110 and 15g of 1, 4-butanediol are added into a reactor and stirred uniformly at room temperature. Then 50g of expandable graphite, 20g of ammonium polyphosphate, 5g of melamine, 5g of pentaerythritol, 2g of antioxidant 245 and 1g of antioxidant 1010 which are dried at the temperature of 120 ℃ for 24 hours are added into a reactor, and are mixed and stirred for 6 hours at the temperature of 110 ℃ under the vacuum condition. And after stirring, stopping vacuumizing, cooling to below 50 ℃, and discharging to obtain the polyurethane resin mixture. And finally, adding 40g of curing agent MDI into the polyurethane resin mixture, uniformly mixing and discharging. Curing for 6 hours in an oven at the temperature of 80 ℃ to obtain the high-insulation low-temperature-resistant expansion flame-retardant polyurethane material.
Example 2:
the raw materials and the preparation process of the polyurethane material with high insulation and low temperature expansion resistance comprise:
75g of hydroxyl-terminated polybutadiene, 25g of polyethylene glycol adipate glycol, 75g of triphenyl phosphate, 25g of diisononyl phthalate, 2g of BYK-088, 2g of KF1023, 2g of diethylenetriamine, 3g of BYK-110 and 10g of 1, 4-bis (hydroxyethoxybenzene) are added into a reactor and stirred uniformly at room temperature. Then 100g of expandable graphite after drying treatment at 120 ℃ for 12 hours, 20g of aluminum diethylphosphinate, 20g of china clay and 2g of antioxidant 245 are added into a reactor, and the mixture is mixed and stirred at 90 ℃ under vacuum conditions for 10 hours. And after stirring, stopping vacuumizing, cooling to below 40 ℃, and discharging to obtain the polyurethane resin mixture. And finally, adding 25g of curing agent polymeric MDI into the polyurethane resin mixture, uniformly mixing and discharging. Curing for 8 hours in an oven at 60 ℃ to obtain the high-insulation low-temperature-resistant expansion flame-retardant polyurethane material.
Example 3:
75g of hydroxyl-terminated polybutadiene, 25g of polytetrahydrofuran polyol, 75g of castor oil, 50g of triphenyl phosphate, 30g of resorcinol bis (diphenyl phosphate), 6g of KF1023, 2g of dibutyltin dilaurate, 4g of BYK-110 and 20g of diethyltoluenediamine were added to a reactor, and stirred at room temperature. Then 30g of ammonium polyphosphate, 10g of melamine, 10g of pentaerythritol, 10g of aluminum hydroxide and 0.5g of antioxidant 1035 which are dried at 120 ℃ for 48 hours are added into a reactor, and mixed and stirred at 110 ℃ for 6 hours under vacuum conditions. And after stirring, stopping vacuumizing, cooling to below 70 ℃, and discharging to obtain the polyurethane resin mixture. And finally, adding 25g of curing agent HDI biuret into the polyurethane resin mixture, uniformly mixing, and discharging. Curing for 4 hours in an oven at the temperature of 90 ℃ to obtain the high-insulation low-temperature-resistant expansion flame-retardant polyurethane material.
Example 4:
75g of hydroxyl-terminated polybutadiene, 25g of castor oil, 75g of triisopropylphenyl phosphate, 3g of BYK-088, 6g of N-ethyl morpholine, 3g of BYK-110 and 15g of 4, 4' -bis-sec-butylaminodiphenylmethane are added into a reactor and stirred uniformly at room temperature. Then 100g of expandable graphite after drying treatment for 48 hours at 100 ℃, 40g of ammonium polyphosphate, 5g of talcum powder and 3g of antioxidant 245 are added into a reactor, and are mixed and stirred for 8 hours at the temperature of 100 ℃ under the vacuum condition. And after stirring, stopping vacuumizing, cooling to below 40 ℃, and discharging to obtain the polyurethane resin mixture. And finally, adding 25g of curing agent MDI into the polyurethane resin mixture, uniformly mixing and discharging. Curing for 6 hours in an oven at the temperature of 80 ℃ to obtain the high-insulation low-temperature-resistant expansion flame-retardant polyurethane material.
Example 5:
adding 75g of hydroxyl-terminated polybutadiene, 25g of castor oil, 35g of triisopropylphenyl phosphate, 35g of diphenylisooctyl phenyl phosphate, 5g of BYK-088, 6g of N-ethyl morpholine, 3g of BYK-110 and 15g of dipropylene glycol into a reactor, and uniformly stirring at room temperature. Then 120g of expandable graphite after drying treatment at 110 ℃ for 24 hours, 15g of hydrotalcite, 5g of calcium carbonate, 4g of antioxidant 1035 and 2g of antioxidant 1076 are added into a reactor, and the mixture is mixed and stirred for 4 hours at the temperature of 100 ℃ under vacuum conditions. And after stirring, stopping vacuumizing, cooling to below 40 ℃, and discharging to obtain the polyurethane resin mixture. And finally, adding 25g of curing agent IPDI trimer into the polyurethane resin mixture, uniformly mixing, and discharging. Curing for 4 hours in an oven at the temperature of 80 ℃ to obtain the high-insulation low-temperature-resistant expansion flame-retardant polyurethane material.
Comparative example:
100g of hydroxyl-terminated polybutadiene, 75g of dioctyl phthalate and 3g of BYK-110 are added into a reactor and stirred uniformly at room temperature. Then 50g of calcium carbonate, 20g of argil and 3g of antioxidant 245 which are dried for 24 hours at 120 ℃ are added into a reactor, and are mixed and stirred for 6 hours at the temperature of 110 ℃ under the vacuum condition. After stirring, vacuumizing is stopped, the temperature is reduced to below 50 ℃, 6g of dibutyltin dilaurate is added, and the mixture is stirred uniformly to obtain a component A. Adding 80g of polyoxypropylene diol into a reaction kettle at normal temperature, heating to 90 ℃, stirring, vacuumizing, degassing and dehydrating for 2 hours, cooling to 40 ℃, adding 45g of curing agent MDI, heating to 80 ℃, reacting for 2 hours, cooling to 40 ℃, and adding 15g of dioctyl phthalate to obtain a component B. When in use, A, B components are mixed according to the weight ratio of 1:1, and are cured in an oven at the temperature of 80 ℃ for 6 hours to prepare the polyurethane material.
The properties of the high-insulation, low-temperature expansion-resistant and flame-retardant polyurethane materials prepared in the above examples 1 to 5 and the properties of the polyurethane material prepared in the comparative example were measured, and the measurement methods were as follows:
1. and (3) testing the flame retardant grade: the test is carried out by referring to the standard UL 94 'test for burning plastic materials of equipment and appliance parts' and the dripping condition is observed, the vertical burning test is divided into three grades of V-0, V-1 and V-2, wherein the V-0 grade is the highest grade of the flame retardant effect.
2. And (3) testing the insulating property: the test is carried out on a volume surface resistance measuring instrument by referring to the GB/T1692-2008 determination of insulation resistivity of vulcanized rubber, the test temperature is 23 +/-2 ℃, and the relative humidity is 50% +/-5%. The volume resistivity is more than 1011The sample of Ω · cm was evaluated as O, and the volume resistivity was less than 1011The Ω · m sample was evaluated as ×.
3. And (3) low temperature resistance test: the test is carried out on a rubber low-temperature brittleness tester by referring to a single sample method for testing the low-temperature brittleness of vulcanized rubber in standard GB/T1682-2014.
The results are shown in Table 1.
TABLE 1 Properties of polyurethane materials prepared in examples 1-4 and comparative examples
It can be seen from Table 1 that the flame retardant rating, insulation and low temperature resistance of the highly insulating, low temperature expansion resistant flame retardant polyurethane materials prepared in examples 1-5 of the present invention are higher than those of the polyurethane materials prepared in the comparative example. And the highly insulating, low temperature expansion resistant flame retardant polyurethane materials prepared in examples 1-5 quickly self-extinguished the sample after the flame was removed after ignition until no flaming melt drips within a certain time interval and a cotton pad one foot below the test sample could not be ignited. The polyurethane material prepared in the comparative example ignited and had a melt dripping, which ignited the cotton pad. In summary, the high-insulation and low-temperature-expansion-resistant flame-retardant polyurethane materials prepared in the embodiments 1 to 5 of the invention have obviously better expansion flame-retardant property, insulation property and low-temperature resistance than those of the comparative examples.
The foregoing is only a preferred embodiment of the present invention; the scope of the invention is not limited thereto. Any person skilled in the art should be able to cover the technical scope of the present invention by equivalent or modified solutions and modifications within the technical scope of the present invention.
Claims (27)
1. A high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material is characterized by comprising the following components in percentage by mass:
2. the highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 1, wherein the low molecular weight polyol is at least one of polyester polyol, polyether polyol, hydroxyl terminated polybutadiene, hydroxyl terminated nitrile rubber, polycaprolactone polyol, polycarbonate polyol, acrylic polyol, silicone polyol, fluorinated polyol, hydride of liquid polyisoprene containing hydroxyl groups, hydride of liquid polybutadiene containing hydroxyl groups, castor oil and castor oil derivatives.
3. The highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 2, wherein the polyester polyol is at least one of polyethylene adipate glycol, polyethylene adipate-propylene glycol, polyethylene adipate-diethylene glycol, and polyethylene adipate-1, 4-butylene glycol.
4. The highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 2, wherein the polyether polyol is at least one of polyoxypropylene diol, polyoxypropylene triol, and polytetrahydrofuran polyol.
5. The highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 1, wherein the chain extender is one or more of ethylene glycol, 1, 4-butanediol, diethylene glycol, dipropylene glycol, triethanolamine, diethyltoluenediamine, dimethylthiotoluenediamine, 4' -bis-sec-butylaminodiphenylmethane, and methylcyclohexanediamine.
6. The highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 1, wherein the catalyst is one or more of triethylenediamine, dibutyltin dilaurate, stannous octoate, diethylenetriamine, N-ethyl morpholine, zinc naphthenate, and organic bismuth.
7. The high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material as claimed in claim 1, wherein the antioxidant is one or more of antioxidant 1010, antioxidant 245, antioxidant 1035 and antioxidant 1076.
8. The high insulation, low temperature expansion resistant flame retardant polyurethane material according to claim 1, wherein the defoaming agent is one or both of BYK-088 and KF 1023.
9. The highly insulating, low temperature expansion resistant flame retardant polyurethane material of claim 1, wherein the wetting dispersant is one or both of BYK-110 and BYK 190.
10. The high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material according to claim 1, wherein the flame retardant is a halogen-free flame retardant, and the mass percentage of the halogen-free flame retardant is 10-50% by mass.
11. The highly insulating, low temperature resistant intumescent flame retardant polyurethane material of claim 10, wherein said halogen free flame retardant is at least one of magnesium hydroxide, aluminum hydroxide, zinc borate, high degree of polymerization ammonium polyphosphate, melamine salts, expandable graphite, polysiloxane, pentaerythritol and its di-, tri-, and diethyl aluminum hypophosphite.
12. The highly insulating, low temperature expansion resistant flame retardant polyurethane material of claim 1, wherein the plasticizer is a plasticizer without hydroxyl groups.
13. The highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 12, wherein the plasticizer is at least one of dioctyl terephthalate DOTP, 1, 2-cyclohexanedicarboxylate di (isononyl) ester, ether-esters, medium molecular weight polyesters, low molecular weight polyesters, alkyl benzene sulfonates, phthalates, trimellitates, and phosphate plasticizers.
14. The highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 13, wherein the phthalate ester plasticizer is at least one of diisononyl phthalate and di (undecyl) phthalate.
15. The highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 13, wherein the trimellitate plasticizer is at least one of trioctyl trimellitate, tri-ethylhexyl trimellitate, and tri-isodecyl trimellitate.
16. A high insulation, low temperature expansion resistant flame retardant polyurethane material according to claim 13, wherein the phosphate based plasticizer is at least one of tricresyl phosphate, triisopropylphenyl phosphate, diphenylisooctyl phenyl phosphate, diphenylisodecyl phosphate, trixylenyl phosphate, triphenyl phosphate, triethyl phosphate, bisphenol a bis (diphenyl phosphate), resorcinol bis (diphenyl phosphate), and tributyl phosphate.
17. The highly insulating, low temperature expansion resistant, flame retardant polyurethane material of claim 1, wherein the filler is at least one of carbon black, white carbon black, talc, calcium carbonate, graphene, hydrotalcite, kaolin, and china clay.
18. The highly insulating, low temperature expansion resistant flame retardant polyurethane material of claim 1, wherein the curing agent is at least one of MDI, polymeric MDI, liquefied MDI, HDI trimer, HDI biuret, PPDI, NDI and IPDI trimer.
19. A method for preparing a highly insulating, low temperature expansion resistant flame retardant polyurethane material according to any of claims 1-18, comprising the steps of:
(1) weighing the raw material components according to the mass percentage;
(2) drying the flame retardant, the filler and the antioxidant at the temperature of 100-120 ℃ for 12-48 hours;
(3) adding low molecular weight polyol, a plasticizer, a defoaming agent, a catalyst, a wetting dispersant and a chain extender into a reactor, and uniformly stirring;
(4) adding the dried flame retardant, the filler and the antioxidant into a reactor, and starting vacuum and stirring;
(5) raising the temperature, controlling the temperature in the reactor to be 90-110 ℃, and stirring for 0.5-10 hours under a vacuum condition;
(6) after stirring, stopping vacuumizing, cooling to below 40-70 ℃, and discharging to obtain a polyurethane resin mixture;
(7) and uniformly mixing the polyurethane resin mixture and the curing agent according to the mass ratio of the polyurethane resin mixture to the curing agent of 100: 1-100: 30, and discharging to obtain the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material.
20. The method for preparing a highly insulating, low temperature expansion resistant, flame retardant polyurethane material according to claim 19, wherein in the step (3), the stirring speed of the stirring is 1rpm to 200 rpm.
21. The method for preparing a highly insulating, low temperature expansion resistant and flame retardant polyurethane material according to claim 19, wherein in the step (5), the temperature increase comprises a first temperature increase stage and a second temperature increase stage; the initial temperature of the first temperature rise stage is between room temperature and 40 ℃, the termination temperature is between 70 and 80 ℃, and the temperature rise rate of the first temperature rise stage is between 0.1 and 20 ℃/min; the initial temperature of the second temperature rise stage is 70-80 ℃, the termination temperature is 90-110 ℃, and the temperature rise rate is 0.1-20 ℃/min.
22. The method for preparing a highly insulating, low temperature expansion resistant, flame retardant polyurethane material according to claim 19, wherein in step (5), the vacuum degree under vacuum is-0.08 to-0.1 MPa, and the stirring speed of the stirring is 1rpm to 200 rpm.
23. The preparation method of the high-insulation low-temperature-expansion-resistant flame-retardant polyurethane material according to claim 19, wherein in the step (6), the cooling rate of the cooling is 0.1-20 ℃/min.
24. The method for preparing a highly insulating, low temperature expansion resistant, flame retardant polyurethane material according to claim 19, wherein in step (7), the polyurethane resin mixture and the curing agent are stirred and vacuum defoamed during uniform mixing.
25. The preparation method of the high-insulation low-temperature-resistant flame-retardant polyurethane material according to claim 19, wherein in the step (7), after the discharging, the polyurethane material is cured in an oven at 40-100 ℃ for 2-10 hours to obtain the high-insulation low-temperature-resistant expansion flame-retardant polyurethane material.
26. Use of a highly insulating, low temperature expansion resistant flame retardant polyurethane material according to any of claims 1 to 18 for fire protection of building walls, cable channels, cables in traffic tracks and through-going holes.
27. Use of the highly insulating, low temperature expansion resistant flame retardant polyurethane material according to any of claims 1-18 in electrical insulation packaging materials, electrical component potting adhesives, water-proof coatings, corrosion-resistant coatings, cold-resistant coatings, fire-resistant expansion seals and adhesives.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115584196A (en) * | 2022-09-05 | 2023-01-10 | 大昇新材料(浙江)有限公司 | Rail trolley bus pantograph insulation coating and preparation method thereof |
| CN117578309A (en) * | 2024-01-17 | 2024-02-20 | 杭州洪鑫电力科技有限公司 | Cable insulation installation assembly and method |
| CN117578309B (en) * | 2024-01-17 | 2024-05-03 | 杭州洪鑫电力科技有限公司 | Cable insulation installation assembly and method |
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| CN103881047A (en) * | 2014-03-06 | 2014-06-25 | 上海赛沃化工材料有限公司 | High-insulation hydrolysis-preventing polyurethane filling and sealing material and preparation method thereof |
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| CN102010588A (en) * | 2010-10-25 | 2011-04-13 | 黎明化工研究院 | Low-viscosity polyurethane potting material and preparation method and use thereof |
| CN103881047A (en) * | 2014-03-06 | 2014-06-25 | 上海赛沃化工材料有限公司 | High-insulation hydrolysis-preventing polyurethane filling and sealing material and preparation method thereof |
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| CN115584196A (en) * | 2022-09-05 | 2023-01-10 | 大昇新材料(浙江)有限公司 | Rail trolley bus pantograph insulation coating and preparation method thereof |
| CN117578309A (en) * | 2024-01-17 | 2024-02-20 | 杭州洪鑫电力科技有限公司 | Cable insulation installation assembly and method |
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