Low density and flame retardant two-component polyurethane potting formulation
Patent Information
- Authority / Receiving Office
- EP · EP
- Patent Type
- Applications
- Current Assignee / Owner
- DDP SPECIALTY ELECTRONICS MATERIALS US LLC
- Filing Date
- 2023-08-03
- Publication Date
- 2026-06-10
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Figure PCTCN2023110935-FTAPPB-I100001 
Figure PCTCN2023110935-FTAPPB-I100002 
Figure PCTCN2023110935-FTAPPB-I100003
Abstract
Description
LOW DENSITY AND FLAME RETARDANT TWO-COMPONENT POLYURETHANE POTTING FORMULATIONBACKGROUND
[0001] As electric vehicle technology advances, demands are increasing for vehicles that are lighter weight and capable of traveling longer distances. This in turn creates a demand of each component manufacturer to keep weight low. At the same time, for certain applications such as battery potting materials, flame retardance is also an important requirement. Two-component polyurethane foaming potting materials have been widely adopted by battery assembly manufacturerer and electrical vehicle suppliers. The main advantage for these foaming potting materials is their low density, ranging from 0.2-0.5 g / cm3. However, foaming potting materials usually result in uneven surfaces after fully curing cured, which creates additional problems. There is a need in the art for alternative low density potting materials which also meet flame retardance standards.SUMMARY
[0002] Described herein is an improved potting formulation with low density yet excellent flame retardance. The formulation generally comprises:
[0003] a) a first component comprising:
[0004] i) a prepolymer prepared by reacting a first polyol with an excess of an isocyanate such that the prepolymer is end-capped with one or more isocyanate residues; the prepolymer being present at 30%to 80%by weight of the first component;
[0005] ii) a first flame retardant mixture comprising 1) a first halogenated organophosphate and 2) a first halogen-free phosphate; wherein the first flame retardant mixture is present at 10%to 65%by weight of the first component, and the mixture comprises more of the first halogenated organophosphate than the first halogen-free phosphate;
[0006] b) a second component comprising:
[0007] i) 40%to 80%of a second polyol by weight of the second component;
[0008] ii) a second flame retardant mixture comprising 1) a second halogenated organophosphate and 2) a second halogen-free phosphate; wherein the second flame retardant mixture is present at 5%to 40%by weight of the second component, and wherein the second halogenated organophosphate and the second halogen-free phosphate are present in the second component at a weight ratio ranging from 5: 1 to 1: 2;
[0009] iii) 0.01%to 5%of a defoamer by weight of the second component;
[0010] iv) 0.005%to 0.2%of a catalyst capable of catalyzing the reaction of a hydroxyl group with an isocyanate group, by weight of the second component;
[0011] c) 0.1%to 50%by weight of the potting formulation of a low-density filler, present in the first component, the second components, or both components, the low-density filler having a density of less than 1 g / cm3;
[0012] The uncured potting formulation is in the form of a kit in which the first and second components are not mixed prior to use. In some embodiments, the first and second components have a first and second density, respectively, and the average of the first and second densities at 25℃ is less than 1 g / cm3.
[0013] Also described is a cured potting formulation made by mixing the first and second components of the potting formulation and allowing the mixture to cure. Also described is a process for curing the potting formulation, comprising mixing the first and second components of the potting formulation and allowing the mixture to cure.DETAILED DESCRIPTION
[0014] The disclosed potting formulation generally comprises two parts, a first (isocyanate) component, and a second (polyol) component. The potting formulation exists at least initially as an uncured kit in which the first and second components are not mixed prior to use. As discussed above, an advantage of the disclosed potting material is its low density, enabling for instance lighter weight and longer driving distance for electric vehicles. In some embodiments, the first and second components have a first and second density, respectively, and the average of the first and second densities at 25℃ is less than 1 g / cm3, as measured using a density cup, e.g., less than 0.95 g / cm3, less than 0.90 g / cm3, or less than 0.85 g / cm3. In one embodiment, the average of the first and second densities at 25℃ is 0.6 g / cm3 to 0.85 g / cm3. As demonstrated in the Examples below, despite having such low densities, flame retardance was surprisingly maintained with a combination of halogenated and halogen-free phosphates, which enabled the formulations to meet the UL94 V0 flame retardance standard.
[0015] I. First (Isocyanate) Component
[0016] A. Isocyanate End-Capped Prepolymer
[0017] The first component comprises a a prepolymer prepared by reacting a first polyol with an excess of an isocyanate such that the prepolymer is end-capped with one or more isocyanate residues. In some embodiments, the prepolymer can be present at 30%to 80%by weight of the first component, e.g., 45%to 65%by weight of the first component. Because an excess of isocyanate can be used to ensure adequate end-capping, the first component in some embodiments will also comprise an excess of unreacted isocyanate. In one embodiment, the first component comprises 20-40%, e.g., 25-35%by weight of unreacted isocyanate.
[0018] i. Isocyanate
[0019] The isocyanate used to make the prepolymer can include any monomeric isocyanate commonly used with polyurethane technology. In one embodiment, the isocyanate comprises an aromatic isocyanate, an aliphatic isocyanate, or a mixture thereof. In a further embodiment, the isocyanate comprises isophorone diisocyanate (IPDI) , dicyclohexyl methane diisocyanate (HMDI) , hexamethylene diisocyanate (HDI) , 4, 4-diphenylmethane diisocyanate (MDI) or a polymeric variant thereof, 4, 4’-methylenediphenyl diisocyanate, or a mixture thereof. In another embodiment, the isocyanate comprises a mixture of polymeric 4, 4-diphenylmethane diisocyanate (MDI) , 4, 4-diphenylmethane diisocyanate (MDI) , and 4, 4’-methylenediphenyl diisocyanate.
[0020] Other suitable isocyanates include 4, 4’-methylene-diphenyldiisocyanate; 2, 2’-methylenediphenyldiisocyanate; 2, 4-methylene-diphenyldiisocyanate; toluene diisocyanate (TDI) ; toluene-2, 4-diisocyanate; toluene-2, 6-diisocyanate; naphthyl-ene-1, 5-diisocyanate; methoxyphenyl-2, 4-diisocyanate; diphenyl-methane-4, 4’-diisocyanate; diphenylmethane-2, 4’-diisocyanate; 4, 4’-bi-phenylene diisocyanate; 3, 3’-dimethoxy-4, 4’-biphenyl diisocyanate; 3, 3’-dimethyl-4-4’-biphenyl diisocyanate; 3, 3’-dimethyl-diphenyl methane-4, 4’-diisocyanate; 4, 4’, 4"-triphenyl methane triisocyanate; toluene-2, 4, 6-triisocyanate; 4, 4, -dimethyl-di-phenylmethane-2, 2,, 5, 5’-tetraisocyanate; and mixtures thereof.
[0021] Any polymer of a monomeric isocyanate can also be used to make a larger prepolymer, including in combination with monomeric isocyanates. Examples include any derivative or polymer of the above described isocyanates. Other examples include polyisocyanates that contain urethane, urea, biuret, caibodiimide, uretoneimine, allophonate or other groups formed by reaction of isocyanate groups. The isocyanate component can also include polymeric MDI (a mixture of MDI and polyMDI that is commonly referred to as “polymeric MDF” ) . Other examples include “liquid MDI" products that are mixtures of MDI and polyMDI derivatives that have biuret, carbodiimide, uretoneimine or allophonate linkages.
[0022] ii. First Polyol
[0023] Suitable first polyols for making the prepolymer can vary and can be a diol or triol. In general, the second component can comprise 40-80%, e.g., 45-65%, by weight of the second polyol. The first polyol can be any glycerin initiated propoxylated or ethoxylated polyol or any propoxylated or ethoxylated polyol prepared from alternative tri-functional and bis-functional starters. In some embodiments, the first polyol can be a polyether polyol or mixture of polyether polyols. In other embodiments, the first polyol can be a homopolymer or copolymer of propylene oxide, or a copolymer of propylene oxide with 70 wt%to 99 wt%propylene oxide and from 1 wt%to 30 wt%ethylene oxide. If two or more polyether polyols are present, it can be preferred that at least one of the polyols is such a copolymer of propylene oxide and ethylene oxide. In the case of a copolymer, the propylene oxide and ethylene oxide can be randomly copolymerized, block copolymerized, or both. In some embodiments, 50%or more of the hydroxyl groups of the polyether polyol or mixture of polyether polyols are primary hydroxyl, with the remainder of the hydroxyl groups being secondary hydroxyl groups. In another embodiment, 70%or more of the hydroxyl groups in the polyether polyol or mixture thereof can be primary hydroxyl groups.
[0024] In some embodiments, the first polyol has a hydroxyl functionality ranging from 2 to 6. In a further embodiment, the first polyol has a molecular weight of 1,000-6,000 g / mol. In one embodiment, the first polyol is polypropylene glycol, for example a propylene glycol having a molecular weight of 2,000 g / mol and a hydroxyl functionality of 2.
[0025] B. First Flame Retardant Mixture
[0026] The first component includes a first flame retardant mixture present at 10-65%by weight of the first component. In other embodiments, the first flame retardant mixture is present at 20-65%, 30-65%, 40-65%, or 40-55%by weight of the first component. In general, the first flame retardant mixture comprises a first halogenated organophosphate along with a first halogen-free phosphate, where the first flame retardant mixture comprises more of the first halogenated organophosphate than the first halogen-free phosphate.
[0027] Suitable halogenated phosphates include for instance chlorinated or brominated organophosphates. Non-limiting examples include Tris (1, 3-dichloro-2-propyl) phosphate (TDCPP) , Tris (1-chloro-2-propyl) phosphate (TCPP) , Tris (2, 3-dichloro-1-propyl) phosphate, and Tris (2-chloroethyl) phosphate (TCEP) . In one embodiment, the first halogenated phosphate is TCPP. Any suitable halogen-free phosphate can be used in combination with the halogenated organophosphate. An example includes melamine polyphosphate. In one embodiment, the first halogenated phosphate is TCPP and the first halogen-free phosphate is melamine polyphosphate.
[0028] II. Second (Polyol) Component
[0029] A. Second Polyol
[0030] Suitable second polyols for the polylol component can vary and can be a diol or triol. The term “second” polyol is used to clarify that the second polyol can be the same or different from the first polyol. For example, the second polyol can be any glycerin initiated propoxylated or ethoxylated polyol or any propoxylated or ethoxylated polyol prepared from alternative tri-functional and bis-functional starters. In some embodiments, the second polyol can be a polyether polyol or mixture of polyether polyols. In other embodiments, the second polyol can be a homopolymer or copolymer of propylene oxide, or a copolymer of propylene oxide with 70 wt%to 99 wt%propylene oxide and from 1 wt%to 30 wt%ethylene oxide. If two or more polyether polyols are present, it can be preferred that at least one of the polyols is such a copolymer of propylene oxide and ethylene oxide. In the case of a copolymer, the propylene oxide and ethylene oxide can be randomly copolymerized, block copolymerized, or both. In some embodiments, 50%or more of the hydroxyl groups of the polyether polyol or mixture of polyether polyols are primary hydroxyl, with the remainder of the hydroxyl groups being secondary hydroxyl groups. In another embodiment, 70%or more of the hydroxyl groups in the polyether polyol or mixture thereof can be primary hydroxyl groups.
[0031] In some embodiments, the second polyol has a hydroxyl functionality ranging from 2 to 6. In a further embodiment, the second polyol has a molecular weight of 1,000-6,000 g / mol. In one embodiment, the second polyol is polypropylene glycol, for example a propylene glycol having a molecular weight of 2,000 g / mol and a hydroxyl functionality of 2. In other embodiments, the second polyol comprises a polypropylene glycol having a molecular weight of 300-3,000 g / mol and a hydroxyl functionality of 2-3, a polyether polyol having a molecular weight of 3,000-6,000 g / mol and a hydroxyl functionality of 2-3, or a mixture thereof.
[0032] B. Second Flame Retardant Mixture
[0033] The second flame retardant mixture generally comprises a second halogenated organophosphate and a second halogen-free phosphate. The second flame retardant mixture is generally present at 5%to 40%by weight of the second component, e.g., 10-30%or 10-25%. In addition, the second halogenated organophosphate and the second halogen-free phosphate are present in the second component at a weight ratio ranging from 5: 1 to 1: 2, e.g., 4: 1 to 1: 1 or 3.5: 1 to 1.1.
[0034] The term “second” halogenated organophosphate and “second” halogen-free phosphate is used to clarify that the first and second halogenated and halogen-free flame retardants can be the same or different. Suitable halogenated phosphates include for instance chlorinated or brominated organophosphates. Non-limiting examples include Tris (1, 3-dichloro-2-propyl) phosphate (TDCPP) , Tris (1-chloro-2-propyl) phosphate (TCPP) , Tris (2, 3-dichloro-1-propyl) phosphate, and Tris (2-chloroethyl) phosphate (TCEP) . In one embodiment, the first halogenated phosphate is TCPP. Any suitable halogen-free phosphate can be used in combination with the halogenated organophosphate. An example includes melamine polyphosphate. In one embodiment, the second halogenated phosphate is TCPP and the second halogen-free phosphate is melamine polyphosphate.
[0035] C. Defoamer
[0036] In some embodiments, the second component comprises 0.01%to 5%by weight of a defoamer, also known in the art as an air release agent. In a further embodiment, the formulation comprises 0.05%to 2%of the defoamer by weight of the second component. Any known defoamer can be used such as silicone-or non-silicone-based defoamers. Examples include those commercially available from BYK, e.g., BYK A 535, available from BYK Additives.
[0037] III. Catalyst
[0038] The adhesive formulation can include a catalyst capable of catalyzing the reaction of a hydroxyl group with an isocyanate group. The catalyst can be present in the isocyanate component, the polyol component, or both. In some examples, the catalyst is present in the polyol component. In other examples, the catalyst is present in the polyol component but not in the isocyanate component.
[0039] The catalyst can include, for example, one or more latent room temperature (25℃) organometallic catalysts. The latent room temperature organometallic catalysts can contain tin, zinc, bismuth, or a combination thereof. For example, the latent room temperature organometallic catalyst can include one or more catalysts such as zinc alkanoates, bismuth alkanoates, dialkyl tin alkanoates, dialkyl tin mercaptides, dialkyl tin bis (alkyl-mercaptoacetates) , dialkyltin thioglycolates, or mixtures thereof. Specific examples include dioctyltinmercaptide, dibutylmercaptidem, dibutylmercaptide, dibutylmercaptide, bis (dodecylthio) dimethylstannane, dimethytin bis (2-ethylhexylmercaptoacetate) , dioctylcarboxylates, dioctyltinneodecanoate, and mixtures thereof.
[0040] Another catalyst useful in the adhesive formulation is any catalyst that can be further heat activated (referred to as “thermosensitive catalysts” ) or otherwise catalyze the reaction. In one embodiment, such catalysts can include for example amines-based solid amine catalysts such as a cyclic amidine catalyst compound, e.g., 1, 8-diazabicyclo [5.4.0] undec-7-ene (DBU) , 1, 5-diazabicyclo [4.3.0] non-5-ene, 2, 4, 6-tris- (dimethylaminomethyl) -phenol, and mixtures thereof.
[0041] In a further embodiment, the adhesive formulation can include a combination of a latent tin-containing catalyst and a thermosensitive amine-based catalysts. Both the tin-containing organic catalyst and the amine-based catalyst can be readily formulated into the isocyanate component, the polyol component, or both the isocyanate component and the polyol component.
[0042] In a further embodiment, any non-tin-based metal-organic catalyst which exhibits similar curing kinetics or catalytic profile of the tin-based catalyst described above can be used as the catalyst ingredient in the adhesive formulation. For example, useful bismuth-based catalysts include bismuth (III) -neodecanaote, and useful zinc-based catalysts include zinc-neodecanaote.
[0043] In yet another embodiment, non-tin-based catalysts or non-amine-based catalysts useful in the adhesive formulation include carboxylic acid blocked catalysts such as DBU carboxylic acid blocked catalysts. For example, a DBU carboxylic acid blocked catalyst can be TOYOCAT DB41 catalyst (a carboxylic DBU salt available from TOSOH) , POLYCAT SA-102 / 10 (a carboxylic DBU salt available from Air Products) , and mixtures thereof. Other useful catalysts include acid blocked amines including for example tertiary amines and organic acid-based catalysts such as TOYOCAT DB40, TOYOCAT DB60, and TOYOCAT DB70 available from TOSOH; 1H-1, 2, 4-triazole-based amine catalysts such as TOYOCAT DB30 available from TOSOH; and mixtures thereof. Any other known thermosensitive amine catalysts can also be used including TOYOCAT F22 available from TOSOH; triethylenediamine (TEDA) ; and mixtures thereof. In one embodiment, the catalyst useful can be selected from tin catalysts such as di-n-octyltin bis [isooctylmercaptoacetate] ; and from amine catalysts such as POLYCAT SA 1 / 10, and TOYOCAT DB60; and mixtures thereof.
[0044] In general, the amount of the catalyst in the adhesive formulation can be in the range of from 0.005 wt %to 2.0 wt %; from 0.01 wt %to 1.0 wt %; and from 0.015 wt. %to 0.07 wt %, based on either i) the total weight of the formulation or ii) the total weight of the first or second component of the formulation (i.e., the polyol or isocyanate component) . In one illustrative embodiment, for example when a tin catalyst such as di-n-octyltin bis [isooctylmercaptoacetate] is used in the adhesive formulation, the concentration of such catalyst in the formulation or in either component can be from 0.005 wt %to 1.0 wt %; from 0.02 wt %to 0.08 wt %; and from 0.03 wt. %to 0.05 wt based on the total weight of the formulation as a whole or either component thereof. In one embodiment, the catalyst is present in the second component at 0.005 to 0.1%by weight of the second component.
[0045] In another illustrative embodiment, when a thermosensitive amine catalyst such as POLYCAT SA 1 / 10 is used in the adhesive formulation, the concentration of such catalyst in the formulation can be from 0.01 wt %to 2.0 wt %; from 0.01 wt %to 1.0 wt %; and from 0.015 wt. %to 0.025 wt %based on the weight of the formulation as a whole or either component of the formulation.
[0046] In still another illustrative embodiment, when a catalyst such as TOYOCAT DB60 is used in the adhesive formulation, the concentration of such catalyst in the formulation can be from 0.01 wt %to 2.0 wt %; from 0.01 wt %to 1.0 wt %; and from 0.045 wt. %to 0.065 wt %, based on the weight of the formulation as a whole or either component of the formulation.
[0047] If the concentration of the catalyst is lower than 0.005 wt %by weight of the formulation as a whole, the catalyst used may not be effectively active in the formulation and the storage stability of the resulting formulation may be “poor, ” that is, any residual water present in the formulation can deactivate the small amounts of catalyst. If the concentration of the catalyst is more than 2.0 wt %, the reaction of the components present in the formulation may be too quick resulting in a short open time, that is, an open time of for example less than 3 minutes may occur. In addition, a high catalyst level (e.g., greater than 2.0 wt %) in the formulation may lead to an increase in handling and formulation costs for the resulting formulation. In one embodiment, the catalyst is present in the polyol component, and not present in the isocyanate component.
[0048] IV. Low Density Filler and other Additives
[0049] To maintain low weight of the potting material, embodiments of the formulation can comprise 0.1%to 50%by weight of the potting formulation of a low-density filler. The low density filler can be present in the first component, the second components, or both components. In general, the low-density filler is one that has a density of less than 1 g / cm3.
[0050] In some embodiments, the potting formulation comprises 2%to 20%by weight of the potting formulation of the low-density filler, which can be in either or both components. For example, in one embodiment, the formulation comprises 2%to 15%by weight of the first component of the low-density filler, e.g., 5-10%. In a further embodiment, the formulation comprises 2%to 15%by weight of the second component of the low-density filler, e.g., 5-10%.
[0051] Various low density fillers can be used. In some embodiments, the low-density filler comprises hollow microspheres. The hollow microspheres can be hollow glass microspheres, hollow silica microspheres, hollow phenolic resin microspheres, or a combination thereof.
[0052] Other additives commonly used in potting materials can be used. In one embodiment for example, the potting formulation can comprise 0.005 to 0.5%of a color paste by weight of either the first component or the second component, provided that the color paste is not present in both components.
[0053] V. Process for Curing the Potting Formulation
[0054] Also disclosed is a cured potting formulation made by mixing the first and second components of the described potting formulation and allowing the mixture to cure. Similarly, this disclosure encompasses a process for curing the potting formulation, comprising mixing the first and second components of the potting formulation and allowing the mixture to cure. In some embodiments, the first and second components of the potting formulation are mixed at a ratio ranging from 2: 1 to 1: 2. In a further embodiment, the first and second components of the potting formulation are mixed at a ratio of 1: 1.
[0055] In one specific embodiment, the lightweight filler can optionally be dried for instance at above 100℃, e.g., 110℃, to achieve a desired maximum moisture content. The isocyanate component and polyol component can be prepared, respectively, by mixing for 30 min-1 hr under a maximum pressure, e.g., 80 mbar, under an inert atmosphere such as nitrogen. To pot the two components, the first and second components can be mixed at the desired mass ratio under vacuum for an adequate amount of time. For test methods, density of each component can be measured using a density cup. Flame retardant performance can be evaluated by the UL94 standard.
[0056] EXAMPLES
[0057] The following examples further illustrate this disclosure. The scope of the disclosure and claims is not limited by the scope of the following examples.
[0058] I. Materials
[0059] The raw materials described in Table 1 were used in the examples.
[0060] Table 1.
[0061] II. Comparative and Inventive Examples
[0062] Table 2 shows weight percentages of each material in Component A (isocyanate component, or “first component” ) and Component B (polyol component, or “second component” ) for the comparative and inventive examples.
[0063] Table 2.
[0064] Comparative example 1 represents a two-component ( “2K” ) polyurethane potting formulation without the light weight filler. The formulation of the isocyanate component contains prepolymer, isocyanate, filler, and flame retardant. The formulation of polyol component contains polyols, defoamer, color paste, and catalyst.
[0065] Comparative example 2 has 8 wt. %GS20 in both the isocyanate and polyol components, compared to Comparative example 1.
[0066] Comparative example 3 has 10 wt. %more TCPP in both the isocyanate and polyol components, compared to Comparative example 2.
[0067] Inventive examples 4, 5 and 6 have an additional flame retardant, FR-NP, in both the isocyanate and polyol components, compared to Comparative example 2.
[0068] Inventive examples 4, 5 and 6 have different amounts of FR-NP.
[0069] III. Methods
[0070] A. Prepolymers
[0071] The prepolymers were prepared in a 2L a four-necked flask with a mechanical stirring bar and thermometer. The prepolymer can be isolated and stored. The prepolymer preparation process is described based on the example of Inventive example 4. 300g of NJ-220 was added into a four-necked flask with a mechanical stirring bar and thermometer at room temperature. The reaction mixture was dried under reduced pressure at 110℃ for 1 h. When the temperature cooled to 50℃, 900 g of SUPRASEC 2020 was added into flask, and kept under reduced pressure at 80℃ for 2 h. Finally, the reaction was completed, and the prepolymer was stored hermetically.
[0072] The prepolymer was prepared with a significant stochiometric excess of MDI, resulting in end-capped polyols, according to the structure depicted in Scheme 1 below.
[0073] Scheme 1.
[0074] B. Polyurethane Potting and Test Methods
[0075] The isocyanate and the polyol components of the potting material were prepared in a 2L planetary mixer laboratory scale mixer. The potting preparation process described is based on the example of the isocyanate component of the Inventive example 4. Before potting was prepared, GS20 was dried in a 110℃ oven for more than 24 hours until moisture content was less than 500ppm. 506 g of prepolymer, 414 g TCPP and 80g dried GS20 were added into 2L planetary mixer laboratory scale mixer. The mixture was slowly stirred for 30 minutes. A vacuum of maximum 80 mbar was applied, and mixing was continued for an additional 30 minutes. Finally, the vacuum is broken with nitrogen. The polyol component was prepared in a similar manner.
[0076] For potting, the isocyanate component and the polyol component were mixed at a mass ratio of 1: 1, the mixture was stirred under 80 mbar vacuum for three minutes to yield the 2K polyurethane potting material.
[0077] For test methods, density of each component was measured using a density cup. Flame retardant performance was evaluated by the UL94 standard.
[0078] IV. Results
[0079] Results from the Comparative and Inventive examples are shown below in Table 3. Densities are in units of g / cm3.
[0080] Table 3.
[0081] Comparative example 1 was a 2K polyurethane potting material without any lightweight filler GS20. The density was 1.08. UL94 V0 can be achieved by 22.5 wt. %TCPP in the final product. However, the product density is higher than with the Inventive examples.
[0082] Comparative example 2 was a low-density polyurethane potting with 8 wt. %GS20. The density was 0.79, and only UL94 HB was achieved with 20.7 wt. %TCPP in the final product.
[0083] Comparative example 3 was a low-density polyurethane potting with 8 wt. %GS20. The density was 0.82, and only UL94 HB was achieved with 28.4 wt. %TCPP in the final product.
[0084] Inventive example 4 and 5 were low density polyurethane potting with 8 wt. %GS20. Their density was 0.80 and 0.82. For Inventive example 4, UL94 V2 can be achieved by 20.1 wt. %TCPP and 2.9 wt. %FR-NP. For Inventive example 5, UL94 V0 can be achieved by 19.5 wt. %TCPP and 5.7 wt. %FR-NP.
[0085] Inventive example 6 was a low density polyurethane potting with 9 wt. %GS20. The density was 0.78. UL94 V0 was achieved with 18.6 wt. %TCPP and 9.0 wt. %FR-NP.
[0086] Features and advantages of this disclosure are apparent from the detailed specification, and the claims cover all such features and advantages. Numerous variations will occur to those skilled in the art, and any variations equivalent to those described in this disclosure fall within the scope of this disclosure. Those skilled in the art will appreciate that the conception upon which this disclosure is based may be used as a basis for designing other compositions and methods for carrying out the several purposes of this disclosure. As a result, the claims should not be considered as limited by the description or examples.
Claims
1.An uncured, two-part polyurethane potting formulation having:a) a first component comprising:i) a prepolymer prepared by reacting a first polyol with an excess of an isocyanate such that the prepolymer is end-capped with one or more isocyanate residues; the prepolymer being present at 30%to 80%by weight of the first component;ii) a first flame retardant mixture comprising 1) a first halogenated organophosphate and 2) a first halogen-free phosphate; wherein the first flame retardant mixture is present at 10%to 65%by weight of the first component, and the mixture comprises more of the first halogenated organophosphate than the first halogen-free phosphate;b) a second component comprising:v) 40%to 80%of a second polyol by weight of the second component;vi) a second flame retardant mixture comprising 1) a second halogenated organophosphate and 2) a second halogen-free phosphate; wherein the second flame retardant mixture is present at 5%to 40%by weight of the second component, and wherein the second halogenated organophosphate and the second halogen-free phosphate are present in the second component at a weight ratio ranging from 5: 1 to 1: 2;vii) 0.01%to 5%of a defoamer by weight of the second component;viii) 0.005%to 0.2%of a catalyst capable of catalyzing the reaction of a hydroxyl group with an isocyanate group, by weight of the second component;c) 0.1%to 50%by weight of the potting formulation of a low-density filler, present in the first component, the second components, or both components, the low-density filler having a density of less than 1 g / cm3;wherein the uncured potting formulation is in the form of a kit in which the first and second components are not mixed prior to use; andwherein the first and second components have a first and second density, respectively, and the average of the first and second densities at 25℃ is less than 1 g / cm3.2.The potting formulation of claim 1, wherein the first or second polyol has a hydroxyl functionality ranging from 2 to 6.3.The potting formulation of claim 1, wherein the first or second polyol is a diol.4.The potting formulation of claim 1, wherein the first or second polyol has a molecular weight of 1,000-6,000 g / mol.5.The potting formulation of claim 1, wherein the first or second polyol is polypropylene glycol.6.The potting formulation of claim 5, wherein the polypropylene glycol has a molecular weight of 2,000 g / mol and a hydroxyl functionality of 2.7.The potting formulation of claim 1, wherein the isocyanate comprises an aromatic isocyanate, an aliphatic isocyanate, or a mixture thereof.8.The potting formulation of claim 1, wherein the isocyanate comprises isophorone diisocyanate (IPDI) , dicyclohexyl methane diisocyanate (HMDI) , hexamethylene diisocyanate (HDI) , 4, 4-diphenylmethane diisocyanate (MDI) or a polymeric variant thereof, 4, 4’-methylenediphenyl diisocyanate, or a mixture thereof.9.The potting formulation of claim 1, wherein the isocyanate comprises a mixture of polymeric 4, 4-diphenylmethane diisocyanate (MDI) , 4, 4-diphenylmethane diisocyanate (MDI) , and 4, 4’-methylenediphenyl diisocyanate.10.The potting formulation of claim 1, wherein the first or second halogenated organophosphate is tris- (1-chloro-2-propyl) phosphate (TCPP) .11.The potting formulation of claim 1, wherein the first or second halogen-free phosphate is melamine polyphosphate.12.The potting formulation of claim 1, wherein the low-density filler comprises hollow microspheres.13.The potting formulation of claim 12, wherein the hollow microspheres are hollow glass microspheres, hollow silica microspheres, hollow phenolic resin microspheres, or a combination thereof.14.A process for curing the potting formulation of claim 1, comprising mixing the first and second components of the potting formulation and allowing the mixture to cure.