CN116874721A - Low-density porous material and preparation method and application thereof - Google Patents
Low-density porous material and preparation method and application thereof Download PDFInfo
- Publication number
- CN116874721A CN116874721A CN202211433481.6A CN202211433481A CN116874721A CN 116874721 A CN116874721 A CN 116874721A CN 202211433481 A CN202211433481 A CN 202211433481A CN 116874721 A CN116874721 A CN 116874721A
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- polyether polyol
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- 239000011148 porous material Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000006260 foam Substances 0.000 claims abstract description 41
- 239000000463 material Substances 0.000 claims abstract description 40
- 239000003063 flame retardant Substances 0.000 claims abstract description 37
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000003054 catalyst Substances 0.000 claims abstract description 35
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 28
- 229920000570 polyether Polymers 0.000 claims abstract description 28
- 229920005862 polyol Polymers 0.000 claims abstract description 28
- 150000003077 polyols Chemical class 0.000 claims abstract description 28
- 239000003381 stabilizer Substances 0.000 claims abstract description 23
- 239000002086 nanomaterial Substances 0.000 claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000012948 isocyanate Substances 0.000 claims abstract description 9
- 150000002513 isocyanates Chemical group 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 36
- 238000003756 stirring Methods 0.000 claims description 27
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 12
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 11
- 238000005187 foaming Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 230000000379 polymerizing effect Effects 0.000 claims description 9
- SVTBMSDMJJWYQN-UHFFFAOYSA-N 2-methylpentane-2,4-diol Chemical compound CC(O)CC(C)(C)O SVTBMSDMJJWYQN-UHFFFAOYSA-N 0.000 claims description 8
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 8
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052797 bismuth Inorganic materials 0.000 claims description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000012970 tertiary amine catalyst Substances 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 claims description 4
- OEOIWYCWCDBOPA-UHFFFAOYSA-N 6-methyl-heptanoic acid Chemical compound CC(C)CCCCC(O)=O OEOIWYCWCDBOPA-UHFFFAOYSA-N 0.000 claims description 4
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 4
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 4
- 208000005156 Dehydration Diseases 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims description 4
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229940037003 alum Drugs 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 4
- UQOQXWZPXFPRBR-UHFFFAOYSA-K bismuth dodecanoate Chemical compound [Bi+3].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O UQOQXWZPXFPRBR-UHFFFAOYSA-K 0.000 claims description 4
- NSPSPMKCKIPQBH-UHFFFAOYSA-K bismuth;7,7-dimethyloctanoate Chemical compound [Bi+3].CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O.CC(C)(C)CCCCCC([O-])=O NSPSPMKCKIPQBH-UHFFFAOYSA-K 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- -1 diamine modified MDI Chemical class 0.000 claims description 4
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 4
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229940051250 hexylene glycol Drugs 0.000 claims description 4
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 4
- 239000000600 sorbitol Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims 1
- 239000004814 polyurethane Substances 0.000 abstract description 11
- 229920002635 polyurethane Polymers 0.000 abstract description 11
- 238000010521 absorption reaction Methods 0.000 description 15
- 238000009413 insulation Methods 0.000 description 6
- 229920005830 Polyurethane Foam Polymers 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011496 polyurethane foam Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 3
- 239000004745 nonwoven fabric Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- HHDUMDVQUCBCEY-UHFFFAOYSA-N 4-[10,15,20-tris(4-carboxyphenyl)-21,23-dihydroporphyrin-5-yl]benzoic acid Chemical compound OC(=O)c1ccc(cc1)-c1c2ccc(n2)c(-c2ccc(cc2)C(O)=O)c2ccc([nH]2)c(-c2ccc(cc2)C(O)=O)c2ccc(n2)c(-c2ccc(cc2)C(O)=O)c2ccc1[nH]2 HHDUMDVQUCBCEY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FRCHKSNAZZFGCA-UHFFFAOYSA-N 1,1-dichloro-1-fluoroethane Chemical compound CC(F)(Cl)Cl FRCHKSNAZZFGCA-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention relates to a low-density porous material, a preparation method and application thereof, which mainly solves the problems of the prior art that the polyurethane porous material for vehicles existsThe invention adopts a low-density porous material, which consists of components A, B, C and D in parts by weight: b: c: d=100: 85-250: 0.5 to 10:10 to 55; the component A comprises polyether polyol A in parts by weight: 20-60 parts of polyether polyol B:20 to 50 parts of open-cell polyether polyol 0.5 to 11 parts of foam stabilizer 0.2 to 2.5 parts of water 3 to 18 parts; the component B is isocyanate; the component C is a composition of a small molecular compound and a catalyst; the component D is 1 in parts by weight: 1-10 of a combination of intumescent flame retardant material and porous nanomaterial; expansion multiplying power of the expansion flame-retardant material is more than 50; the particle size of the porous nano material is more than or equal to 3000 meshes, and the specific surface area is more than 10000cm 2 The technical scheme of/g and the preparation thereof well solves the problems and can be used in industrial application of automobile NVH materials.
Description
Technical Field
The invention belongs to the field of polyurethane, and particularly relates to a low-density porous material, and a preparation method and application thereof.
Background
In 7 months of 2022, the Shenzhen global headquarters holds "Yue-Biedi automobile active sound quality sharing meeting", and the latest development result NVH active sound technology is disclosed to the outside for the first time; the NVH (Noise Vibration) of the automobile is a standard established by the international automobile community, namely three standards of Noise, vibration and smoothness (Harshness), is an important index for measuring the riding comfort of the automobile, directly influences the riding experience in the automobile, is an important aspect of the 'variety feel' of the automobile, and becomes a key index for measuring the market competitiveness of various brands of automobile types.
One of the main methods for reducing noise in a vehicle is to apply acoustic gaskets to various parts of the vehicle body, and the gaskets having excellent acoustic properties are required to exhibit both sound absorption and excellent sound insulation. Sound absorption refers to absorbing radiation noise in a vehicle, and sound insulation refers to isolating noise from outside noise sources that are transmitted into the vehicle, so developing an acoustic liner that has both sound absorption and sound insulation is an important method for improving NVH performance of a vehicle.
The traditional acoustic gaskets in automobiles are mostly manufactured by using felt, glass fiber and the like, namely, the felt/glass fiber, black non-woven fabrics and the like are manufactured by die pressing and punching, and the problems of pungent smell, floating cotton wool, high density and the like often exist; at present, non-woven fabrics, glue, light foam, glue, non-woven fabrics and aluminum lovers are generally adopted, wherein the light foam is light polyurethane foam, and the foam has the advantages of low density, easiness in forming and the like.
Chinese patent application CN103254386A discloses a polyurethane semi-rigid foam composition for an automobile ceiling, wherein the prepared polyurethane semi-rigid foam composition has higher foam aperture ratio and certain sound absorption performance, but does not give specific sound absorption coefficient at 3500-6000 HZ frequency, does not mention the condition of flame retardance, has higher density and does not meet the requirement of light weight of an automobile.
The Chinese patent application CN103910854A discloses a low-density flame-retardant semi-rigid polyurethane foam and a preparation method thereof, the prepared foam is a flame-retardant semi-rigid polyurethane foam, has a higher aperture ratio of more than or equal to 90 percent, partially meets the requirements of public PV3937, but the public flame-retardant standard is updated to TL1010-2008, has stricter requirements, does not see the patent of the follow-up related flame retardance of the low-density flame-retardant semi-rigid polyurethane foam, and in addition, the invention adopts 20-40 parts of halogenated phosphate such as TCPP and other flame retardants, which have larger odor and higher volatility, influence the environment in a vehicle and do not refer to the sound absorption performance condition of the foam.
Chinese patent application CN 110982030A discloses a continuous production method for preparing light polyurethane semi-rigid foam by a one-step method, and provides a one-step continuous production method, and the foam produced by the method has the advantages of small density and finer foam holes, but adopts phosphate flame retardant, is easy to volatilize and has large smell, does not meet the environmental protection requirement of development of automotive interiors, and the flame retardant property of the foam is not mentioned in the content.
Chinese patent application CN102898815a discloses a soft and light PU foam board special for an automobile engine sound insulation pad, wherein the foam board is special for an engine sound insulation pad, but the invention uses HCFC-141b physical foaming agent in a large amount, which is not friendly to the environment, damages the environment and affects the health and safety of passengers, the use of such substances in automobile interior is forbidden, and in addition, TCPP and other flame retardants have a large odor, which pollute the environment in the automobile.
Disclosure of Invention
One of the technical problems to be solved by the invention is to solve the problems of high density, poor sound absorption and poor flame retardance of the polyurethane porous material for the vehicle in the prior art, and provide a low-density porous material which has the advantages of low density, good acoustic performance and good flame retardance.
The second technical problem to be solved by the invention is to provide a preparation method of the low-density porous material corresponding to one of the technical problems.
The third technical problem to be solved by the invention is to provide an application of the low-density porous material corresponding to one of the technical problems.
In order to solve one of the technical problems, the technical scheme provided by the invention is as follows: a low-density porous material consists of a component A, a component B, a component C and a component D, wherein the component A comprises the following components in parts by weight: component B: component C: component d=100: 85-250: 0.5 to 10:10 to 55; wherein, the component A comprises the following components in parts by weight: polyether polyol a: 20-60 parts of polyether polyol B: 20-50 parts of open-cell polyether polyol: 0.5-11 parts of foam stabilizer: 0.2 to 2.5 portions of water: 3-18 parts; the component B is isocyanate; the component C is a composition of a small molecular compound and a catalyst; the component D is prepared from the following components in parts by weight: 1-10 of a combination of intumescent flame retardant material and porous nanomaterial; wherein the foam stabilizer comprises the foam stabilizer A in parts by weight: 0.1 to 1.5 parts of foam stabilizer B:0.1 to 2.1 parts; the catalyst comprises the following components in parts by weight: 0.1 to 2.0 of tertiary amine catalyst A and organic metal catalyst B;
the polyether polyol A is prepared by polymerizing ethylene oxide and propylene oxide by taking glycerol as an initiator, has a functionality of 3, a molecular weight of 4000-6000 and a hydroxyl value of 25-45 mgKOH/g; the polyether polyol B is prepared by polymerizing propylene oxide by taking glycerol and sorbitol as mixed initiators, has a functionality of 3-6 and a molecular weight of 300-600; the open-cell polyether polyol is prepared by polymerizing ethylene oxide and propylene oxide by taking glycerol as a main initiator, has a functionality of 3-5, a molecular weight of 7000-9000, a hydroxyl value of 25-40 mgKOH/g and an EO content of 65-80%; the expansion multiplying power of the expansion flame-retardant material is more than 50; the particle size of the porous nano material is more than or equal to 3000 meshes, and the specific surface area is more than 10000cm 2 /g。
In the above technical scheme, preferably, the weight part ratio of the catalyst in the component A to the catalyst in the component C is 100:0.1 to 2.0; the weight part ratio of the component A to the small molecular compound in the component C is 100:0 to 10.
In the above technical scheme, preferably, the weight part ratio of the component A to the catalyst is 100:0.3 to 1.1; the weight part ratio of the component A to the small molecular compound is 100:2 to 8.
In the above technical scheme, preferably, the small molecular compound in the component C is at least one selected from CHE-220, CHE-210, CHE-204, PEG-200, PEG-400, diethanolamine, ethylenediamine, ethylene glycol, propylene glycol, butylene glycol, neopentyl glycol, hexylene glycol, diethylene glycol or dipropylene glycol, and the water content is less than or equal to 0.01wt% after dehydration treatment.
In the above technical solution, preferably, the tertiary amine catalyst a is at least one selected from NE1070, NE1090, NE317, LED103 and LE 15; the organic metal catalyst B is at least one selected from T-9, T-12, bismuth isooctanoate, bismuth laurate, bismuth neodecanoate or bismuth naphthenate.
In the above technical scheme, preferably, the weight part ratio of the catalyst in the component a to the catalyst in the component C is 100:0.1 to 2.0.
In the above technical solution, preferably, the intumescent flame retardant material in the component D is at least one selected from alumina, alum and expanded graphite.
In the above technical solution, preferably, the porous nanomaterial is at least one selected from activated carbon, nano calcium hydroxide, nano calcium carbonate and white carbon black.
In the above technical solution, preferably, the expansion ratio of the intumescent flame retardant material is greater than 200.
In the above technical scheme, preferably, the weight part ratio of the intumescent flame retardant material to the porous nanomaterial is 1:2 to 8.
In the above technical scheme, preferably, the weight part ratio of the component A to the component D is 100:30 to 55.
In the above technical solution, preferably, the foam stabilizer a is at least one selected from ECOADD S-2333, DC2525 and DC 193; the foam stabilizer B is at least one selected from L6915, B8409, B8450 or B8228.
In the above technical solution, preferably, the isocyanate is at least one selected from pure MDI, crude MDI, PM200, M20S, 5005, charred diamine modified MDI, MDI-50 or TDI.
In order to solve the second technical problem, the technical scheme provided by the invention is as follows: a method for preparing a low-density porous material, comprising the following steps:
(1) Preparing a component A: sequentially adding polyether polyol A into a container A according to parts by weight: 20-60 parts of polyether polyol B: 20-50 parts of open-cell polyether polyol: 0.5-11 parts of foam stabilizer: 0.2 to 2.5 portions of water: 3-18 parts of a stirring device, and controlling the temperature of the materials to be 19-22 ℃; wherein, the polyether polyol A takes glycerol as an initiator and is polymerized by ethylene oxide and propylene oxide, the functionality is 3, the molecular weight is 4000-6000, and the hydroxyl value is 25-45 mgKOH/g; the polyether polyol B is prepared by polymerizing propylene oxide by taking glycerol and sorbitol as mixed initiators, has a functionality of 3-6 and a molecular weight of 300-600; the open-cell polyether polyol is prepared by polymerizing ethylene oxide and propylene oxide by taking glycerol as a main initiator, has a functionality of 3-5, a molecular weight of 7000-9000, a hydroxyl value of 25-40 mgKOH/g and an EO content of 65-80%; the foam stabilizer comprises the following components in parts by weight: 0.1 to 1.5 parts of foam stabilizer B:0.1 to 2.1 parts;
(2) Preparing a component B: adding isocyanate component into the container B, and stirring uniformly;
(3) Preparing a component C: adding a small molecular compound into a reaction kettle, stirring and vacuumizing, controlling the temperature to be 60-90 ℃, drying until the water content is less than or equal to 0.01wt%, and dropwise adding a catalyst after nitrogen replacement, wherein the weight part ratio of the small molecular compound to the catalyst is 0-10: 0.1 to 2.0 parts by weight of catalyst, wherein the weight ratio of the catalyst is 0 to 0.8:0.1 to 2.0 of tertiary amine catalyst A and organic metal catalyst B, the weight portion ratio of component A to component C is 100:0.5 to 10 percent, and evenly stirring to prepare a component C;
(4) The intumescent flame retardant material and the porous nano material are mixed according to the weight part ratio of 1: 1-10, so that porous nano materials are uniformly attached to the surface of an intumescent flame retardant material, and are dried for 2 hours at the temperature of 60 ℃ to prepare a component D;
(5) The composition comprises the following components in parts by weight: component B: component C: component d=100: 85-250: 0.5 to 10: 10-55, controlling the ambient temperature to be 19-22 ℃, adding the component D into the component B, rapidly mixing and stirring, then adding the component A, stirring for 15-25 s, then adding the component C, immediately increasing the rotating speed, rapidly stirring for 5-25 s, and immediately pouring into a foaming box for foaming after uniform stirring, thus obtaining the low-density porous material product.
In the above technical scheme, preferably, the weight part ratio of the small molecular compound to the catalyst is 2-8: 0.3 to 1.1 percent of the total weight of the composite,
in the above technical scheme, preferably, the weight part ratio of the catalyst in the component A to the catalyst in the component C is 100:0.1 to 2.0; the weight part ratio of the component A to the small molecular compound in the component C is 100:0 to 10.
In the above technical scheme, preferably, the weight part ratio of the catalyst in the component A to the catalyst in the component C is 100:0.3 to 1.1; the weight part ratio of the component A to the small molecular compound in the component C is 100:2 to 8.
In the above technical scheme, preferably, the small molecular compound in the component C is at least one selected from CHE-220, CHE-210, CHE-204, PEG-200, PEG-400, diethanolamine, ethylenediamine, ethylene glycol, propylene glycol, butylene glycol, neopentyl glycol, hexylene glycol, diethylene glycol or dipropylene glycol, and the water content is less than or equal to 0.01wt% after dehydration treatment.
In the above technical solution, preferably, the tertiary amine catalyst a is at least one selected from NE1070, NE1090, NE317, LED103 and LE 15; the organic metal catalyst B is at least one selected from T-9, T-12, bismuth isooctanoate, bismuth laurate, bismuth neodecanoate or bismuth naphthenate.
In the above technical solution, preferably, the intumescent flame retardant material in the component D is at least one selected from alumina, alum and expanded graphite.
In the above technical solution, preferably, the porous nanomaterial is at least one selected from activated carbon, nano calcium hydroxide, nano calcium carbonate and white carbon black.
In the above technical solution, preferably, the expansion ratio of the intumescent flame retardant material is greater than 200.
In the above technical scheme, preferably, the weight part ratio of the intumescent flame retardant material to the porous nanomaterial is 1:2 to 8.
In the above technical scheme, preferably, the weight part ratio of the component A to the component D is 100:30 to 55.
In the above technical solution, preferably, the foam stabilizer a is at least one selected from ECOADD S-2333, DC2525 and DC 193; the foam stabilizer B is at least one selected from L6915, B8409, B8450 or B8228.
In the above technical solution, preferably, the isocyanate is at least one selected from pure MDI, crude MDI, PM200, M20S, 5005, charred diamine modified MDI, MDI-50 or TDI.
In order to solve the third technical problem, the technical scheme provided by the invention is as follows: low density porous materials are used in automotive NVH materials.
By adopting the technical scheme of the invention, the low-density porous material can be prepared, and the technical scheme has the following advantages: the first and the second intumescent flame retardant materials can expand rapidly after being heated, a compact carbonized layer is formed on the surface, free flow of oxygen is prevented, and the flame retardant property of the materials is further improved effectively; the porous nano material has larger specific surface area and excellent porous structure, is uniformly attached to the surface of the intumescent flame retardant material, and is more beneficial to forming a uniform sound-absorbing sea-island structure in the foam, namely the intumescent flame retardant material uniformly attached by the porous nano material forms islands, and other components form sea, so that the porous nano material is more beneficial to being uniformly distributed in the foam, on one hand, noise enters the holes to be subjected to multiple reflection, the energy is greatly reduced, and the sound-absorbing and noise-reducing performance can be improved; on the other hand, the inorganic nano material and the intumescent flame retardant material can form a synergistic effect to form a denser and thicker inorganic substance and carbon composite layer, so that the inorganic nano material is not easy to drip, and the flame retardance is more obvious; secondly, the open-cell polyether polyol is adopted to replace the pore opening agent, so that the consumption of small molecular oligomers is reduced, the generation of VOC is reduced from the root, and the foam has good pore opening property and mechanical property, is an important means for preparing foam products with high air permeability, and is also a key for ensuring the dimensional stability; thirdly, firstly adding the component D into the component B for rapid mixing and stirring, then adding the component A for stirring, then adding the component C, and immediately increasing the rotating speed, wherein the rapid mixing method can lead the components to fully react, and the product is more uniform and finer; the finally prepared low-density porous material has the advantages of small density, good sound absorption and insulation and good flame retardance, and achieves good technical effects.
The present invention is further illustrated by, but not limited to, the following examples.
Detailed Description
TABLE 1 bill of materials
Note that: the mesh number of the nano calcium carbonate in Table 1 is 6000 mesh, 25000cm 2 /g。
[ example 1 ]
A method for preparing a low-density porous material, comprising the following steps:
(1) Preparing a component A: sequentially adding CHE-330N into a container A according to parts by weight: 59 parts, NJ-4110A:20 parts of CHK-350D:0.5 parts of DC-193:1.5 parts, B8228: 1.0 parts of water: 18 parts of a stirring device, and controlling the temperature of the materials to be 19-22 ℃;
(2) Preparing a component B: adding M20S into a container B: 100 parts of MIPS:150 parts of a stirring device;
(3) Preparing a component C: adding 5 parts of CHE-204 into a reaction kettle, stirring, vacuumizing, controlling the temperature at 80 ℃, drying until the water content is less than or equal to 0.01wt%, replacing 3 times with nitrogen, dropwise adding 2.0 parts of T-9, and uniformly stirring to obtain a component C;
(4) Uniformly mixing 5 parts of graphite ADT-802 and 30 parts of nano calcium carbonate to ensure that the nano calcium carbonate is uniformly adhered to the surface of the graphite ADT-802, and drying for 2 hours at the temperature of 60 ℃ to obtain a component D;
(5) The composition comprises the following components in parts by weight: component B: component C: component d=100: 250:2.5:35, controlling the ambient temperature to be 19-22 ℃, adding the component D into the component B, rapidly mixing and stirring, then adding the component A, stirring for 20s, then adding the component C, immediately increasing the rotating speed, rapidly stirring for 20s, uniformly stirring, immediately pouring into a foaming box, and foaming to obtain the low-density porous material, wherein the performance index data are shown in tables 4 and 5.
Examples 2 to 8
Examples 2 to 8 were carried out according to the steps of example 1, except that the reaction materials and the ratios of the materials in the foaming formulation were different, and the specific examples are shown in Table 2; the performance index data of the prepared low-density porous material are shown in tables 4 and 5.
Table 2 weight parts of the components in the foaming formulation of the low density porous materials of examples 1 to 8
Comparative examples 1 to 4
(1) Preparing raw materials according to the parts by weight of each component in the table 3;
(2) Preparing a component A: sequentially adding the weighed components into a container A according to the parts by weight in the step (1), stirring for 15 seconds, and fully mixing at the material temperature of 20 ℃;
(3) The environmental temperature is controlled to be 20 ℃, the component A and the component B are rapidly mixed and stirred, and immediately poured into a foaming box for foaming after being uniformly stirred, so that the polyurethane porous material is prepared, and the performance index data of the polyurethane porous material are shown in tables 4 and 5.
Table 3 comparative examples 1 to 4 parts by weight of each component in the foaming formulation of the polyurethane cellular material
Table 4 performance test data of porous materials of examples 1 to 8 and comparative examples 1 to 4
The criteria for performance detection in table 4 are as follows:
density: GB/T6343-2009;
compressive strength: GB/T8813-2020;
elongation at break: GB/T6344-2008;
opening ratio: GB/T10799-2008;
dimensional change rate: the test conditions are 120 ℃ and 5 hours; cycling for 3 times at 70 ℃ and 3 hours, wherein the test standard is GB/T8811-2008;
flame retardant properties: the general GMN3232-2011 and the public TL1010-2008, BR shows that the combustion rate is less than 100mm/min, and the flame retardant property test meets the standard requirement; fail indicates a burn rate >100mm/min and flame retardant performance tests do not meet standard requirements.
Table 5 sound absorption performance test data of porous materials of examples 1 to 8 and comparative examples 1 to 4
As can be seen from the data in table 4, the porous polyurethane materials prepared in examples 1 to 8 of the present invention have higher compressive strength, elongation at break, better dimensional stability and excellent flame retardancy on the premise of similar foam density; meanwhile, as shown in Table 5, the sound absorption coefficients of the examples 1-8 at different frequencies are better than those of the comparative examples 1-4 at the same frequency, the sound absorption coefficients of the examples are more than or equal to 1000HZ and more than or equal to 0.5, the sound absorption coefficients of the examples are more than or equal to 2000HZ and more than or equal to 0.8, the sound absorption coefficients of the examples are more than or equal to 4000HZ and more than or equal to 0.8, and the sound absorption coefficients of the examples are more than or equal to 6000HZ and more than or equal to 0.8, and the sound absorption properties are excellent; can meet the performance requirements of the automobile NVH material on the polyurethane porous material.
Therefore, the porous material prepared by the invention has the advantages of low density, high aperture ratio, good acoustic performance and good flame retardant property under the condition of meeting the performance requirements of compressive strength, elongation at break and dimensional change rate, and achieves better technical effect, and can be used in the industrial application of automobile NVH materials.
Claims (10)
1. A low-density porous material consists of a component A, a component B, a component C and a component D, wherein the component A comprises the following components in parts by weight: component B: component C: component d=100: 85-250: 0.5 to 10:10 to 55; wherein, the component A comprises the following components in parts by weight: polyether polyol a: 20-60 parts of polyether polyol B: 20-50 parts of open-cell polyether polyol: 0.5-11 parts of foam stabilizer: 0.2 to 2.5 portions of water: 3-18 parts; the component B is isocyanate; the component C is a composition of a small molecular compound and a catalyst; the component D is prepared from the following components in parts by weight: 1-10 of a combination of intumescent flame retardant material and porous nanomaterial; wherein the foam stabilizer comprises the foam stabilizer A in parts by weight: 0.1 to 1.5 parts of foam stabilizer B:0.1 to 2.1 parts; the catalyst comprises the following components in parts by weight: 0.1 to 2.0 of tertiary amine catalyst A and organic metal catalyst B;
the polyether polyol A is prepared by polymerizing ethylene oxide and propylene oxide by taking glycerol as an initiator, has a functionality of 3, a molecular weight of 4000-6000 and a hydroxyl value of 25-45 mgKOH/g; the polyether polyol B is prepared by polymerizing propylene oxide by taking glycerol and sorbitol as mixed initiators, has a functionality of 3-6 and a molecular weight of 300-600; the open-cell polyether polyol takes glycerol as a main initiator and consists of ethylene oxide andpropylene oxide is polymerized to obtain the polymer with the functionality of 3-5, the molecular weight of 7000-9000, the hydroxyl value of 25-40 mgKOH/g and the EO content of 65-80%; the expansion multiplying power of the expansion flame-retardant material is more than 50; the particle size of the porous nano material is more than or equal to 3000 meshes, and the specific surface area is more than 10000cm 2 /g。
2. The low-density porous material according to claim 1, wherein the weight part ratio of the catalyst in the component a to the catalyst in the component C is 100:0.1 to 2.0; the weight part ratio of the component A to the small molecular compound in the component C is 100:0 to 10.
3. The low-density porous material according to claim 2, wherein the weight ratio of the catalyst in the component a to the catalyst in the component C is 100:0.3 to 1.1; the weight part ratio of the component A to the small molecular compound in the component C is 100:2 to 8.
4. The low-density porous material according to claim 2, wherein the small molecular compound in the component C is at least one selected from CHE-220, CHE-210, CHE-204, PEG-200, PEG-400, diethanolamine, ethylenediamine, ethylene glycol, propylene glycol, butylene glycol, neopentyl glycol, hexylene glycol, diethylene glycol and dipropylene glycol, and the water content is less than or equal to 0.01wt% after dehydration treatment; tertiary amine catalyst a is selected from at least one of NE1070, NE1090, NE317, LED103 or LE 15; the organic metal catalyst B is at least one selected from T-9, T-12, bismuth isooctanoate, bismuth laurate, bismuth neodecanoate or bismuth naphthenate.
5. The low-density porous material according to claim 1, wherein the intumescent flame retardant material in component D is at least one selected from the group consisting of alumina, alum and expanded graphite; the porous nano material is selected from at least one of active carbon, nano calcium hydroxide, nano calcium carbonate or white carbon black.
6. The low density porous material of claim 1, wherein said intumescent flame retardant material has an expansion ratio of > 200; the weight part ratio of the intumescent flame retardant material to the porous nano material is 1:2 to 8; the weight part ratio of the component A to the component D is 100:30 to 55.
7. The low density porous material of claim 1, wherein said foam stabilizer a is selected from at least one of ECOADD S-2333, DC2525, or DC 193; the foam stabilizer B is at least one selected from L6915, B8409, B8450 or B8228; the isocyanate is at least one selected from pure MDI, crude MDI, PM200, M20S, 5005, carbonized diamine modified MDI, MDI-50 or TDI.
8. A method of preparing the low density porous material of claim 1, comprising the steps of:
(1) Preparing a component A: sequentially adding polyether polyol A into a container A according to parts by weight: 20-60 parts of polyether polyol B: 20-50 parts of open-cell polyether polyol: 0.5-11 parts of foam stabilizer: 0.2 to 2.5 portions of water: 3-18 parts of a material, uniformly stirring and controlling the temperature of the material to be 19-22; wherein, the polyether polyol A takes glycerol as an initiator and is polymerized by ethylene oxide and propylene oxide, the functionality is 3, the molecular weight is 4000-6000, and the hydroxyl value is 25-45 mgKOH/g; the polyether polyol B is prepared by polymerizing propylene oxide by taking glycerol and sorbitol as mixed initiators, has a functionality of 3-6 and a molecular weight of 300-600; the open-cell polyether polyol is prepared by polymerizing ethylene oxide and propylene oxide by taking glycerol as a main initiator, has a functionality of 3-5, a molecular weight of 7000-9000, a hydroxyl value of 25-40 mgKOH/g and an EO content of 65-80%; the foam stabilizer comprises the following components in parts by weight: 0.1 to 1.5 parts of foam stabilizer B:0.1 to 2.1 parts;
(2) Preparing a component B: adding isocyanate component into the container B, and stirring uniformly;
(3) Preparing a component C: adding a small molecular compound into a reaction kettle, stirring and vacuumizing, controlling the temperature to be 60-90 ℃, drying at the temperature until the water content is less than or equal to 0.01wt%, and dropwise adding a catalyst after nitrogen replacement, wherein the weight part ratio of the small molecular compound to the catalyst is 0-10: 0.1 to 2.0 parts by weight of catalyst, wherein the weight ratio of the catalyst is 0 to 0.8:0.1 to 2.0 of tertiary amine catalyst A and organic metal catalyst B, the weight portion ratio of component A to component C is 100:0.5 to 10 percent, and evenly stirring to prepare a component C;
(4) The intumescent flame retardant material and the porous nano material are mixed according to the weight part ratio of 1: 1-10, so that porous nano materials are uniformly attached to the surface of an intumescent flame retardant material, and are dried for 2 hours at the temperature of 60 ℃ to prepare a component D;
(5) The composition comprises the following components in parts by weight: component B: component C: component d=100: 85-250: 0.5 to 10: 10-55, controlling the environmental temperature to be 19-22, adding the component D into the component B, rapidly mixing and stirring, then adding the component A, stirring for 15-25 s, then adding the component C, immediately increasing the rotating speed, rapidly stirring for 5-25 s, uniformly stirring, and immediately pouring into a foaming box for foaming, thus obtaining the low-density porous material product.
9. The method for preparing a low-density porous material according to claim 8, wherein the small molecular compound is at least one selected from CHE-220, CHE-210, CHE-204, PEG-200, PEG-400, diethanolamine, ethylenediamine, ethylene glycol, propylene glycol, butylene glycol, neopentyl glycol, hexylene glycol, diethylene glycol and dipropylene glycol, and the water content is less than or equal to 0.01wt% after dehydration treatment; tertiary amine catalyst a is selected from at least one of NE1070, NE1090, NE317, LED103 or LE 15; the organic metal catalyst B is selected from at least one of T-9, T-12, bismuth isooctanoate, bismuth laurate, bismuth neodecanoate or bismuth naphthenate; the intumescent flame retardant material is at least one of alumina, alum or expanded graphite; the porous nano material is at least one of active carbon, nano calcium hydroxide, nano calcium carbonate or white carbon black; foam stabilizer A is selected from at least one of ECOADD S-2333, DC2525 or DC 193; the foam stabilizer B is at least one selected from L6915, B8409, B8450 or B8228; the isocyanate is at least one selected from pure MDI, crude MDI, PM200, M20S, 5005, carbonized diamine modified MDI, MDI-50 or TDI.
10. Use of the low density porous material of claim 1 in automotive NVH material.
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