CN111848904A - Heat-conducting halogen-free flame-retardant polyurethane elastomer and preparation method thereof - Google Patents

Heat-conducting halogen-free flame-retardant polyurethane elastomer and preparation method thereof Download PDF

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CN111848904A
CN111848904A CN202010494628.7A CN202010494628A CN111848904A CN 111848904 A CN111848904 A CN 111848904A CN 202010494628 A CN202010494628 A CN 202010494628A CN 111848904 A CN111848904 A CN 111848904A
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polyurethane elastomer
halogen
flame retardant
free
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陈海良
孙志强
李涛
曹士强
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Shandong Dongda Inov Polyurethane Co Ltd
Shandong Inov Polyurethane Co Ltd
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Shandong Dongda Inov Polyurethane Co Ltd
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Priority to CN202010494628.7A priority Critical patent/CN111848904A/en
Priority to PCT/CN2020/102539 priority patent/WO2021243817A1/en
Publication of CN111848904A publication Critical patent/CN111848904A/en
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
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  • Polyurethanes Or Polyureas (AREA)

Abstract

The invention belongs to the technical field of polyurethane products, and particularly relates to a heat-conducting halogen-free flame-retardant polyurethane elastomer and a preparation method thereof. The polyurethane elastomer is prepared from a component A and a component B, wherein the mass ratio of the component A to the component B is 100: 90-110; carrying out reaction on polyoxypropylene ether polyol, polytetrahydrofuran ether polyol, diisocyanate and a plasticizer at 75-85 ℃ for 2-3 hours to prepare a prepolymer with the isocyanate content of 8.0-12.0%, namely a component A; and (2) uniformly mixing the amine chain extender, the polyoxypropylene ether polyol, the vegetable oil polyol, the flame retardant, the heat-conducting filler, the catalyst and the anti-aging agent, and then carrying out vacuum dehydration at 100-110 ℃ to obtain the component B. The polyurethane elastomer prepared by the invention has a V0-grade flame retardant grade, is environment-friendly, does not contain halogen, and has excellent heat conduction characteristics; the preparation method is scientific, reasonable, simple and feasible.

Description

Heat-conducting halogen-free flame-retardant polyurethane elastomer and preparation method thereof
Technical Field
The invention belongs to the technical field of polyurethane products, and particularly relates to a heat-conducting halogen-free flame-retardant polyurethane elastomer and a preparation method thereof.
Background
Polyurethane elastomers have entered into various fields of life by virtue of their excellent properties since their advent. The polyurethane pouring sealant is used as a composite special pouring material, and is increasingly applied to equipment and places requiring insulation, flame retardance, heat conduction, moisture resistance and the like, such as electrical appliance pouring, battery packaging, circuit board packaging and assembling and the like, due to the characteristics of moderate hardness, good elasticity, insulation, mildew resistance, shock resistance, corrosion resistance, high and low temperature impact resistance, high temperature and high humidity resistance, flame retardance, heat conduction and the like. After the polyurethane pouring sealant is cured by the pouring and sealing process, the influence of external environmental conditions on components can be reduced, the lithium battery and the matched components thereof can be ensured to run well under the standard working environment, the stability of the lithium battery and the matched components thereof can be improved, and the service life of the lithium battery can be prolonged. The polyurethane pouring sealant can be cured at room temperature, so that the damage and performance reduction of electronic and electrical parts caused by temperature rise in heating curing are avoided. As the encapsulating and curing are carried out at room temperature, huge heating and curing equipment is not needed, thus the encapsulating and curing material is an ideal encapsulating material in the lithium battery industry.
However, because the chain segment contains a large number of carbon-hydrogen bonds, the polyurethane elastomer can be continuously combusted when exposed to fire, so that the common polyurethane elastomer does not have self-extinguishing property, and therefore, in order to meet a certain flame-retardant requirement, a proper flame retardant must be added to improve the flame-retardant grade of the polyurethane elastomer. The halogen flame retardant serving as the traditional flame retardant with the largest output has the characteristics of good flame retardant effect and low price, but is gradually replaced by the halogen-free flame retardant due to the defects of large smoke quantity, high toxicity of decomposition products and the like when in use. Because the large-scale of lithium cell makes its surface area and volume compare relatively reduce, and the inside heat of battery is difficult for effluvium, more probably appears the inside temperature inequality, local temperature rise scheduling problem to further accelerate battery decay, shorten battery life, increase the potential safety hazard, consequently, the heat conduction of pouring sealant, fire behaviour direct relation to whole lithium cell assembly's safety.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the defects of the prior art are overcome, and the heat-conducting halogen-free flame-retardant polyurethane elastomer is provided, has a V0-grade flame-retardant grade, is environment-friendly, does not contain halogen, and has excellent heat-conducting property; the invention also provides a preparation method of the composition, which is scientific, reasonable, simple and feasible.
The heat-conducting halogen-free flame-retardant polyurethane elastomer is prepared from a component A and a component B, wherein the mass ratio of the component A to the component B is 100: 90 to 110, wherein, in weight percent,
the component A comprises:
Figure BDA0002522323910000011
Figure BDA0002522323910000021
and B component:
Figure BDA0002522323910000022
the polyoxypropylene polyether polyol is one or more of polyoxypropylene polyols with the functionality of 2 or 3 and the number average molecular weight of 1000-6000;
the polytetrahydrofuran ether polyol is one or more of PTMG650, PTMG1000 or PTMG2000 with the molecular weight of 650-2000.
The diisocyanate is one or more of 4,4 '-diphenylmethane diisocyanate (MDI-100), modified liquefied 4, 4' -diphenylmethane diisocyanate (liquefied MDI), H12MDI, IPDI or Toluene Diisocyanate (TDI).
The plasticizer is one or more of dioctyl phthalate (DOTP), Butyl Benzyl Phthalate (BBP), dimethyl ethylene glycol phthalate (DMEP), dioctyl terephthalate, dipropylene glycol dibenzoate, diethylene glycol dibenzoate or Benzoflex TM 9-88SG, and preferably dioctyl phthalate.
The content of the diisocyanate can be reasonably adjusted within the range according to actual needs, and can be 35%, 40%, 45% and the like; the content of the polyoxypropylene ether polyol in the A component may be appropriately adjusted as necessary within the above range, and may be, for example, 25%, 30%, 35%, or the like; the content of the polytetrahydrofuran ether polyol in the component a may be appropriately adjusted within the above range as necessary, and may be, for example, 25%, 30%, 35%, or the like; the content of the plasticizer in the component a may be appropriately adjusted within the above range as necessary, and may be, for example, 15%, 20%, or the like; the reaction temperature may be adjusted within the above range according to the reaction conditions, and may be 79 ℃, 83 ℃, 85 ℃ or the like.
The amine chain extender is one or more of 3, 5-dimethylthiotoluenediamine, MCDEA, 740M, E100 or P1000, preferably E100.
The vegetable oil polyol is one or more of castor oil, palm oil or soybean oil, and castor oil is preferred.
The flame retardant is one or more of IPPP, TCP or RDP.
The heat-conducting filler is one or more of boron nitride, aluminum oxide, magnesium oxide or silicon micropowder, and preferably aluminum nitride.
The catalyst is one or more of organic bismuth, organic zinc or organic zirconium, and organic bismuth catalysts are preferred.
The anti-aging agent is one or more of 1076, 770, 292 or UV-1, preferably UV-1.
The preparation method of the heat-conducting halogen-free flame-retardant polyurethane elastomer comprises the following steps:
(1) the component A comprises: carrying out reaction on polyoxypropylene ether polyol, polytetrahydrofuran ether polyol, diisocyanate and a plasticizer at 75-85 ℃ for 2-3 hours to obtain a prepolymer with the content of isocyanic acid radical of 8.0-12.0%, and obtaining a component A;
(2) and B component: uniformly mixing an amine chain extender, a polyoxypropylene ether polyol, a vegetable oil polyol, a flame retardant, a heat-conducting filler, a catalyst and an anti-aging agent, and dehydrating under vacuum at the temperature of 100-110 ℃ and under the pressure of-0.095 MPa until the moisture content is less than 0.05% to obtain a component B;
(3) uniformly mixing the component A and the component B at 30-35 ℃, pouring the mixture with the viscosity of 800-1500 CPS into a mold with the temperature of 30 ℃ for reaction, wherein the operation time is 5-25 minutes, and curing at room temperature to obtain the polyurethane elastomer product with the Shore A hardness of 55-95.
The polyurethane elastomer prepared by the invention can be used for equipment and places requiring insulation, flame retardance, heat conduction, moisture resistance and the like, such as electrical appliance encapsulation, battery encapsulation, circuit board encapsulation, assembly and the like.
Compared with the prior art, the invention has the following beneficial effects:
(1) the heat-conducting halogen-free flame-retardant polyurethane elastomer reaches the V0-grade flame-retardant grade, is environment-friendly and free of halogen elements, has a heat conductivity coefficient of more than 0.3W/m.K, and has a wide application prospect in the lithium battery encapsulation industry.
(2) The heat-conducting halogen-free flame-retardant polyurethane elastomer has the advantages of high product forming speed and moderate operation time, and can adjust the production speed according to the requirement.
(3) The preparation method is scientific, reasonable, simple and feasible.
Detailed Description
The present invention is further described with reference to the following examples, which are not intended to limit the practice of the invention.
The materials used in the examples are illustrated below:
Figure BDA0002522323910000031
Figure BDA0002522323910000041
the raw materials used in the examples were all commercially available materials except those described above.
Example 1
The component A comprises: by weight percentage, DL-10008%, PTMG 65021%, MDI-10032.2%, CD-C13.8%, DOTP 25%, react at 80 ℃ for 2.5 hours to obtain prepolymer with isocyanate content of 12.0%;
and B component: e10020%, EP-360020%, castor oil 20.2%, IPPP 5034%, aluminum nitride 5%, CH-070.3% and UV-10.5% in percentage by weight, and dehydrating under vacuum at 105 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain a component B;
Preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 35 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction after being mixed, and the polyurethane elastomer product is obtained for standby test after room temperature curing.
Example 2
The component A comprises: according to weight percentage, DL-10008%, PTMG 65021%, MDI-10032.2%, CD-C13.8% and DOTP 25% react for 3 hours at 75 ℃ to obtain a prepolymer with isocyanate content of 12.0%;
and B component: e10020%, DL-200052.7%, castor oil 10%, RDP 11%, aluminum nitride 5%, CH-070.3%, UV-11.0%, and dehydrating under vacuum at 100 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain a component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 30 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction, and after curing at room temperature, the polyurethane elastomer product is obtained for standby test.
Example 3
The component A comprises: by weight percentage, DL-100012%, PTMG 65032%, MDI-10035.7%, CD-C15.3% and DOTP 5% react for 2 hours at 85 ℃ to obtain prepolymer with isocyanate content of 12.0%;
And B component: e10020%, EP-360020%, castor oil 20.2%, IPPP 5034%, aluminum nitride 5%, CH-070.3% and UV-10.5% in percentage by weight, and dehydrating under vacuum at 110 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain a component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 35 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction after being mixed, and the polyurethane elastomer product is obtained for standby test after room temperature curing.
Example 4
The component A comprises: by weight percentage, DL-100012%, PTMG 65032%, MDI-10035.7%, CD-C15.3% and DOTP 5% react for 2.5 hours at 80 ℃ to obtain prepolymer with isocyanate content of 12.0%;
and B component: e10020%, DL-200053.2%, castor oil 10%, RDP 11%, aluminum nitride 5%, CH-070.3%, UV-10.5%, and dehydrating under vacuum at 105 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain a component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 35 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction after being mixed, and the polyurethane elastomer product is obtained for standby test after room temperature curing.
Example 5
The component A comprises: according to weight percentage, EP-360024%, PTMG 200012%, MDI-10027.3%, CD-C11.7% and DOTP 25% react for 2 hours at 85 ℃ to obtain prepolymer with isocyanate content of 12.0%;
and B component: e10020%, EP-360020%, castor oil 20.2%, IPPP 5034%, aluminum nitride 5%, CH-070.3% and UV-10.5% in percentage by weight, and dehydrating under vacuum at 100 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain a component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 30 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction, and after curing at room temperature, the polyurethane elastomer product is obtained for standby test.
Example 6
The component A comprises: according to weight percentage, EP-360024%, PTMG 200012%, MDI-10027.3%, CD-C11.7% and DOTP 25% react for 3 hours at 75 ℃ to obtain a prepolymer with isocyanate content of 12.0%;
and B component: e10020%, DL-200053.2%, castor oil 10%, RDP 11%, aluminum nitride 5%, CH-070.3%, UV-10.5%, and dehydrating under vacuum at 110 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain a component B;
Preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 35 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction after being mixed, and the polyurethane elastomer product is obtained for standby test after room temperature curing.
Example 7
The component A comprises: by weight percentage, EP 360037%, PTMG 200018%, MDI-10028%, CD-C12% and DOTP 5% react for 2.5 hours at 80 ℃ to obtain a prepolymer with isocyanate content of 12.0%;
and B component: e10020%, EP-360020%, castor oil 20.2%, IPPP 5034%, aluminum nitride 5%, CH-070.3% and UV-10.5% in percentage by weight, and dehydrating under vacuum at 105 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain a component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 35 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction after being mixed, and the polyurethane elastomer product is obtained for standby test after room temperature curing.
Example 8
The component A comprises: by weight percentage, EP 360037%, PTMG 200018%, MDI-10028%, CD-C12% and DOTP 5% react for 2.5 hours at 80 ℃ to obtain a prepolymer with isocyanate content of 12.0%;
And B component: e10020%, DL-200053%, castor oil 10%, RDP 11%, aluminum nitride 5%, CH-070.5%, UV-10.5%, and dehydrating under vacuum at 105 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain a component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 30 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction, and after curing at room temperature, the polyurethane elastomer product is obtained for standby test.
Example 9
The component A comprises: by weight percentage, DL-100014%, PTMG 65039%, MDI-10029.4%, CD-C12.6%, DOTP 5% react at 80 ℃ for 2.5 hours to obtain prepolymer with isocyanate content of 8.0%;
and B component: e1009%, EP-360034.2%, castor oil 30%, RDP 11%, aluminum nitride 15%, CH-070.3%, UV-10.5%, dehydrating under vacuum at 110 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 35 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction after being mixed, and the polyurethane elastomer product is obtained for standby test after room temperature curing.
Example 10
The component A comprises: by weight percentage, DL-100010%, PTMG 100019.6%, PTMG 20008.4%, MDI-10025.9%, CD-C11.1%, DOTP 25% react at 75 ℃ for 2 hours to obtain prepolymer with isocyanate content of 8.0%;
and B component: e1009%, EP-360034.2%, castor oil 30%, RDP 11%, aluminum nitride 15%, CH-070.3%, UV-10.5%, and dehydrating under vacuum at 105 ℃ and under-0.095 MPa until the moisture is less than 0.05% to obtain component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 35 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction after being mixed, and the polyurethane elastomer product is obtained for standby test after room temperature curing.
Example 11
The component A comprises: by weight percentage, DL-100010.6%, PTMG 65028.8%, MDI-10028.4%, CD-C12.2% and DOTP 20% react for 2 hours at 85 ℃ to obtain prepolymer with isocyanate content of 9.0%;
and B component: according to weight percentage, E1005 percent, DL-100068.2 percent, castor oil 10 percent, RDP 11 percent, aluminum nitride 5 percent, CH-070.3 percent and UV-10.5 percent are dehydrated under vacuum at the temperature of 110 ℃ and under the pressure of-0.095 MPa until the moisture is less than 0.05 percent to obtain a component B;
Preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 110, the mixing temperature is 30 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction, and after curing at room temperature, the polyurethane elastomer product is obtained for standby test.
Example 12
The component A comprises: according to weight percentage, EP-360022%, PTMG 200011%, MDI-10029.4%, CD-C12.6% and DOTP 25% react for 2.5 hours at 80 ℃ to obtain prepolymer with isocyanate content of 8.0%;
and B component: according to weight percentage, E1005 percent, DL-100068.2 percent, castor oil 10 percent, RDP 11 percent, aluminum nitride 5 percent, CH-070.3 percent and UV-10.5 percent are dehydrated under vacuum at 100 ℃ and under-0.095 MPa until the moisture is less than 0.05 percent to obtain a component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: 100, the mixing temperature is 30 ℃, the mixture is poured into a mold with the temperature of 30 ℃ for reaction, and after curing at room temperature, the polyurethane elastomer product is obtained for standby test.
Example 13
The component A comprises: by weight percentage, DL-100032%, EP-360012%, PTMG 200014%, MDI-10020.3%, CD-C16.7%, DOTP 5%, reacting for 2.5 hours at 80 ℃ to obtain prepolymer with isocyanate content of 8.0%;
And B component: according to weight percentage, E1005 percent, DL-100068.4 percent, soybean oil 10 percent, RDP 11 percent, aluminum nitride 5 percent, CH-070.1 percent and UV-10.5 percent are dehydrated under vacuum at the temperature of 110 ℃ and under the pressure of-0.095 MPa until the moisture is less than 0.05 percent to obtain a component B;
preparing a polyurethane elastomer: the component A and the component B are 100 percent by mass: and 90, mixing at 35 ℃, pouring the mixture into a mold at 30 ℃ for reaction, and curing at room temperature to obtain the polyurethane elastomer product for later test.
The elastomers prepared in the above examples were tested according to the following criteria:
the hardness is measured according to GB/T531.1-2008 standard;
viscosity was measured according to GB/T12008.8-1992;
gel time was measured using a stopwatch;
the flame retardant rating is tested according to UL-94 standard;
the thermal conductivity was tested according to GB/T3139-2005 standard.
Table 1 example test results
Figure BDA0002522323910000081

Claims (10)

1. A heat-conducting halogen-free flame-retardant polyurethane elastomer is characterized in that: the paint is prepared from a component A and a component B, wherein the mass ratio of the component A to the component B is 100: 90 to 110, wherein, in weight percent,
the component A comprises:
Figure FDA0002522323900000011
and B component:
Figure FDA0002522323900000012
the polyoxypropylene polyether polyol is polyoxypropylene polyol with the functionality of 2 or 3 and the number average molecular weight of 1000-6000;
The polytetrahydrofuran ether polyol is one or more of PTMG650, PTMG1000 or PTMG 2000.
2. The thermally conductive, halogen-free, flame retardant polyurethane elastomer of claim 1, wherein: the diisocyanate is one or more of MDI-100, liquefied MDI, H12MDI, IPDI or TDI.
3. The thermally conductive, halogen-free, flame retardant polyurethane elastomer of claim 1, wherein: the plasticizer is one or more of dioctyl phthalate, butyl benzyl phthalate, dimethyl glycol phthalate, dioctyl terephthalate, dipropylene glycol dibenzoate, diethylene glycol dibenzoate or Benzoflex TM 9-88 SG.
4. The thermally conductive, halogen-free, flame retardant polyurethane elastomer of claim 1, wherein: the amine chain extender is one or more of 3, 5-dimethylthiotoluenediamine, MCDEA, 740M, E100 or P1000.
5. The thermally conductive, halogen-free, flame retardant polyurethane elastomer of claim 1, wherein: the vegetable oil polyol is one or more of castor oil, palm oil or soybean oil.
6. The thermally conductive, halogen-free, flame retardant polyurethane elastomer of claim 1, wherein: the flame retardant is one or more of IPPP, TCP or RDP.
7. The thermally conductive, halogen-free, flame retardant polyurethane elastomer of claim 1, wherein: the heat-conducting filler is one or more of boron nitride, aluminum oxide, magnesium oxide or silicon micropowder.
8. The thermally conductive, halogen-free, flame retardant polyurethane elastomer of claim 1, wherein: the catalyst is one or more of organic bismuth, organic zinc or organic zirconium.
9. The thermally conductive, halogen-free, flame retardant polyurethane elastomer of claim 1, wherein: the anti-aging agent is one or more of 1076, 770, 292 or UV-1.
10. A method for preparing the heat-conducting halogen-free flame-retardant polyurethane elastomer according to any one of claims 1 to 9, wherein the method comprises the following steps: the method comprises the following steps:
(1) the component A comprises: carrying out reaction on polyoxypropylene ether polyol, polytetrahydrofuran ether polyol, diisocyanate and a plasticizer at 75-85 ℃ for 2-3 hours to obtain a prepolymer with the content of isocyanic acid radical of 8.0-12.0%, and obtaining a component A;
(2) and B component: uniformly mixing an amine chain extender, a polyoxypropylene ether polyol, a vegetable oil polyol, a flame retardant, a heat-conducting filler, a catalyst and an anti-aging agent, and dehydrating under vacuum at the temperature of 100-110 ℃ and under the pressure of-0.095 MPa until the moisture content is less than 0.05% to obtain a component B;
(3) And uniformly mixing the component A and the component B at the temperature of 30-35 ℃, pouring the mixture into a mold, and curing to obtain the polyurethane elastomer product.
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