CN103012670B - Isotrope polymethacrylimide foam material and preparation method thereof - Google Patents
Isotrope polymethacrylimide foam material and preparation method thereof Download PDFInfo
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- CN103012670B CN103012670B CN201210560479.5A CN201210560479A CN103012670B CN 103012670 B CN103012670 B CN 103012670B CN 201210560479 A CN201210560479 A CN 201210560479A CN 103012670 B CN103012670 B CN 103012670B
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- 239000006261 foam material Substances 0.000 title claims abstract description 44
- 229920007790 polymethacrylimide foam Polymers 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000178 monomer Substances 0.000 claims abstract description 33
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000013019 agitation Methods 0.000 claims abstract description 15
- 238000005187 foaming Methods 0.000 claims abstract description 14
- 239000004088 foaming agent Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 43
- 238000003756 stirring Methods 0.000 claims description 37
- 238000006116 polymerization reaction Methods 0.000 claims description 27
- -1 acrylic ester Chemical class 0.000 claims description 24
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 17
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 8
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- 150000003857 carboxamides Chemical class 0.000 claims description 6
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 claims description 5
- 239000007858 starting material Substances 0.000 claims description 5
- BEQKKZICTDFVMG-UHFFFAOYSA-N 1,2,3,4,6-pentaoxepane-5,7-dione Chemical compound O=C1OOOOC(=O)O1 BEQKKZICTDFVMG-UHFFFAOYSA-N 0.000 claims description 4
- SIQZJFKTROUNPI-UHFFFAOYSA-N 1-(hydroxymethyl)-5,5-dimethylhydantoin Chemical compound CC1(C)N(CO)C(=O)NC1=O SIQZJFKTROUNPI-UHFFFAOYSA-N 0.000 claims description 4
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 claims description 4
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 claims description 4
- 239000004160 Ammonium persulphate Substances 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N CuO Inorganic materials [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 4
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 4
- 229960004643 cupric oxide Drugs 0.000 claims description 4
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 4
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 claims description 4
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004159 Potassium persulphate Substances 0.000 claims description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 3
- 150000002978 peroxides Chemical class 0.000 claims description 3
- 229950010765 pivalate Drugs 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- 235000019394 potassium persulphate Nutrition 0.000 claims description 3
- PODWXQQNRWNDGD-UHFFFAOYSA-L sodium thiosulfate pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].[O-]S([S-])(=O)=O PODWXQQNRWNDGD-UHFFFAOYSA-L 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 150000002191 fatty alcohols Chemical class 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 230000003137 locomotive effect Effects 0.000 abstract description 3
- 235000015842 Hesperis Nutrition 0.000 abstract 1
- 235000012633 Iberis amara Nutrition 0.000 abstract 1
- 150000003926 acrylamides Chemical class 0.000 abstract 1
- 229920006397 acrylic thermoplastic Polymers 0.000 abstract 1
- 230000032798 delamination Effects 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 239000002667 nucleating agent Substances 0.000 abstract 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 abstract 1
- 239000003505 polymerization initiator Substances 0.000 abstract 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 abstract 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- LDHQCZJRKDOVOX-UHFFFAOYSA-N 2-butenoic acid Chemical compound CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 3
- NKKMVIVFRUYPLQ-UHFFFAOYSA-N but-2-enenitrile Chemical compound CC=CC#N NKKMVIVFRUYPLQ-UHFFFAOYSA-N 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- HPXRVTGHNJAIIH-UHFFFAOYSA-N cyclohexanol Chemical compound OC1CCCCC1 HPXRVTGHNJAIIH-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002984 plastic foam Substances 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000003949 imides Chemical class 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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Abstract
The invention discloses an isotrope polymethacrylimide foam material and a preparation method thereof. An acrylics monomer, an acrylamides monomer, a polymerization initiator, a foaming agent and a nucleating agent are mixed according to a weight part proportion; a transparent block body is obtained via high-temperature agitation prepolymerization and low-temperature repolymerization; and the isotrope polymethacrylimide foam is obtained via high-temperature foaming. According to the invention, the problem that a reaction system is non-uniform is solved, which is caused by serious monomer delamination during preparation process; and the obtained isotrope polymethacrylimide foam material has favorable performance, and can be directly applicable to the fields of carrier rockets, ships, fan blades, railway locomotives, sports equipment and the like.
Description
Technical field
The present invention relates to a kind of foam materials and preparation method thereof, be specifically related to a kind of homogeneous polymethacrylimide foam material and preparation method thereof.
Background technology
Polymethacrylimide (PMI) foam materials is the highest foam materials of specific tenacity in all polymer foams, and its remarkable over-all properties shows: foam surface is smooth, structure and mechanical property is non-directional, can mechanical workout, organic solvent-resistant and good with various resin system compatibility; High specific strength, high heat distortion temperature (180～200 DEG C) and excellent incompressible creep property, the high specific pressure contracting intensity of PMI foam can be born the composite resin curing process of 180～200 DEG C dimensional stability requirement to foam.Polymethacrylimide (PMI) foam materials is with its remarkable over-all properties, be to manufacture the desirable core of Lightweight high-strength composite material sandwich structure, obtained a large amount of application at aspects such as airliner and conveyor, air fighter, vertiplane, bullet train, blade of wind-driven generator, satellite and launch vehicle and motion and medical devices.
Patent CN101857656A, CN102051012A, CN101289565A, CN102675795A, CN102675796A, CN102020821A are taking (methyl) vinylformic acid and (methyl) vinyl cyanide as principal monomer, prepare polymethacrylimide plastic foam, preparation method comprises three steps:
The first step: the static prepolymerization of low temperature: taking (methyl) vinylformic acid and (methyl) vinyl cyanide as principal monomer, add whipping agent etc. simultaneously and mix, at 35～50 DEG C of static placement 10～100h, obtain prepolymer;
Second step: comparatively high temps repolymerization: the prepolymer being obtained by the first step is warmed up to 50～115 DEG C of repolymerization and obtains transparent block;
The 3rd step: high temperature foaming obtains polymethacrylimide plastic foam.
Above-mentioned patent is all taking (methyl) vinylformic acid and (methyl) vinyl cyanide as principal monomer, this two classes monomer is all liquid at low temperature pre-polymerization temperature, consistency is better, but in the long-time static pre-polymerization process of (10～100h) low temperature, particularly as initiator, whipping agent etc. there is sedimentation phenomenon in meeting under action of gravity to some solid additives, cause the skewness of whole reaction system Raw, the mechanical property of the polymethacrylimide foam material finally obtaining is on the low side.
Along with the increase of civil area to polymethacrylimide foam material demand such as aircarrier aircraft, railway locomotive, boats and ships, wind power generation blade, sports goodss, in order to meet the needs of the national economic development, update existing preparation method, the polymethacrylimide foam material that processability is more excellent and kind will cause that people pay close attention to greatly.
Summary of the invention
The object of this invention is to provide a kind of homogeneous polymethacrylimide foam material and preparation method thereof.Adopting acrylic ester monomer and acrylamide monomers is main monomer, after batch mixing, prepares transparent block by high-temperature stirring prepolymerization and low temperature repolymerization, and then high temperature foaming makes homogeneous polymethacrylimide foam material.
The technical solution used in the present invention is:
One, a homogeneous polymethacrylimide foam material, made by the raw material of following weight part:
30～80 parts of acrylic ester monomers;
20～70 parts of acrylamide monomers;
0.1～3 part of polymerization starter;
5～20 parts of whipping agents;
0.5～5 part of nucleator;
The molecular chain that is characterized as of polymethacrylimide foam material has following repeating unit:
(note: R
1, R
2for H or-CH
3)
Two, a preparation method for homogeneous polymethacrylimide foam material, comprises the steps:
(1) batching: by 30～80 parts of acrylic ester monomers; 20～70 parts of acrylamide monomers; 0.1～3 part of polymerization starter; 5～20 parts of whipping agents; 0.5～5 part of nucleator, mixes by weight, is stirred and is stirred at normal temperatures 10～30min by electric stirring, magnetic agitation, ultrasonic agitation or shaking table, obtains uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 80～130 DEG C of electric stirrings, magnetic agitation, ultrasonic agitation or shaking table stirring reaction 5～60min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: described pre-polymerization liquid is injected in mould, and normal temperature is placed 1～30min, is then placed in 30～60 DEG C of water-baths, retains 70～100h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 150～240 DEG C, simultaneously to the mould 0～10MPa that exerts pressure, be cooled to normal temperature after retaining 0.5～7h, take out and obtain homogeneous polymethacrylimide foam material.
Described acrylic ester monomer be in methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, propyl methacrylate, methyl ester butyl acrylate any one or with both mixtures of arbitrary proportion.
Described acrylamide monomers be in acrylamide, Methacrylamide any one or with both mixtures of arbitrary proportion.
Described polymerization starter is the mixture of any one or any two kinds and above arbitrary proportion in dicumyl peroxide, dibenzoyl peroxide, di-cyclohexylperoxy dicarbonate, peroxy dicarbonate isopropyl ester, peroxide tert pivalate ester, dilauroyl peroxide, Potassium Persulphate, ammonium persulphate, Sulfothiorine, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile).
Described whipping agent is the mixture that chemical foaming agent and two parts of pneumatogen form with arbitrary proportion:
(1) chemical foaming agent: any one in carboxamide, methane amide or both mixture with arbitrary proportion composition;
(2) pneumatogen: any one in the fatty alcohol that contains 2～8 carbon atoms or arbitrarily several mixtures with arbitrary proportion.
Described nucleator is the mixture of any one or any two kinds and above arbitrary proportion in magnesium oxide, calcium oxide, zinc oxide, cupric oxide.
Compared with background technology, the beneficial effect that the present invention has is:
The invention solves the problem of the serious layering of two monomers in preparation process.The monomer that the present invention adopts is acrylic ester monomer and acrylamide monomers, and the fusing point of acrylamide monomers is higher than 80 DEG C, and during lower than fusing point, acrylamide monomers is solid-state.If the preparation method of employing patent CN101857656A etc., after main raw material is mixed, first adopt the static prepolymerization of low temperature (35～50 DEG C), at this temperature, acrylamide monomers is solid-state, will deposit to very soon the bottom of reaction system, there is serious demixing phenomenon, that is: upper strata is liquid acrylic ester monomer, lower floor is solid-state acrylamide monomers, cause the serious layering of two monomers in whole reaction system, the skewness of raw material, cannot obtain the polymethacrylimide foam material of homogeneous.
First the present invention adopts high-temperature stirring prepolymerization after raw material is mixed, and now solid-state acrylamide monomers will change into liquid state, is dispersed in reaction system, obtains homogeneous reaction system.Then enter the low temperature repolymerization stage, although the temperature in this stage is lower than the fusing point of acrylamide monomers, but due to the solublization of the prepolymer generating in high-temperature stirring prepolymerisation stage, can make acrylamide monomers be dissolved in well in reaction system, whole reaction system presents transparent uniform state, and final high temperature foaming obtains the polymethacrylimide foam material of homogeneous.
Homogeneous polymethacrylimide foam material prepared by the present invention can directly be widely used in the fields such as aerospace, launch vehicle, railway locomotive, boats and ships, wind power generation blade, sports goods, has significant economic benefit and social benefit.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, but the present invention is not restricted to following examples.
embodiment 1:
(1) batching: 50g butyl methacrylate, 50g acrylamide, 0.1g dibenzoyl peroxide, 1g carboxamide, the 4g trimethyl carbinol, 0.5g magnesium oxide are mixed, stir at normal temperatures 10min by electric stirring, obtain uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 80 DEG C of magnetic agitation reaction 60min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: described pre-polymerization liquid is injected in mould, and normal temperature is placed 1min, is then placed in 30 DEG C of water-baths, retains 100h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 150 DEG C, simultaneously to the mould 10MPa that exerts pressure, be cooled to normal temperature after retaining 7h, take out and obtain homogeneous polymethacrylimide foam material.
The density of homogeneous polymethacrylimide foam material prepared by the present embodiment is 289kg/m
3, compressive strength is 8.65MPa.
embodiment 2:
(1) batching: 20g methyl methacrylate, 40g propyl acrylate, 40g acrylamide, 2g di-cyclohexylperoxy dicarbonate, 0.1g dicumyl peroxide, 0.2g Diisopropyl azodicarboxylate, 2g carboxamide, 6g hexalin, 0.5g calcium oxide, 0.5g magnesium oxide are mixed, stir at normal temperatures 15min by magnetic agitation, obtain uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 95 DEG C of electric stirring reaction 40min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: described pre-polymerization liquid is injected in mould, and normal temperature is placed 5min, is then placed in 45 DEG C of water-baths, retains 90h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 190 DEG C, simultaneously to the mould 9MPa that exerts pressure, be cooled to room temperature after retaining 6h, take out and obtain homogeneous polymethacrylimide foam material.
The density of homogeneous polymethacrylimide foam material prepared by the present embodiment is 220kg/m
3, compressive strength is 6.60MPa.
embodiment 3:
(1) batching: 30g butyl methacrylate, 50g methyl acrylate, 20g Methacrylamide, 0.1g Diisopropyl azodicarboxylate, 0.5g 2,2'-Azobis(2,4-dimethylvaleronitrile), 1g methane amide, 4g glycerol, 3g cupric oxide are mixed, stir at normal temperatures 20min by ultrasonic agitation, obtain uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 120 DEG C of shaking table stirring reaction 10min, is obtained to pre-polymerization liquid,
(3) low temperature repolymerization: described pre-polymerization liquid is injected in mould, and normal temperature is placed 30min, is then placed in 50 DEG C of water-baths, retains 85h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 200 DEG C, simultaneously to the mould 7MPa that exerts pressure, be cooled to normal temperature after retaining 5h, take out and obtain homogeneous polymethacrylimide foam material.
The density of homogeneous polymethacrylimide foam material prepared by the present embodiment is 184kg/m
3, compressive strength is 5.52MPa.
embodiment 4:
(1) batching: 15g propyl acrylate, 15g propyl methacrylate, 35g Methacrylamide, 35g acrylamide, 0.5g Potassium Persulphate, 0.3g peroxide tert pivalate ester, 5g methane amide, 15g amylalcohol, 3g zinc oxide, 2g magnesium oxide are mixed, stir at normal temperatures 30min by electric stirring, obtain uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 115 DEG C of ultrasonic agitation reaction 15min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: by described pre-polymerization liquid is injected in mould, normal temperature is placed 25min, is then placed in 55 DEG C of water-baths, retains 80h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 210 DEG C, simultaneously to the mould 5MPa that exerts pressure, be cooled to normal temperature after retaining 4h, take out and obtain the poly-methyl-prop acid imide foam material of homogeneous.
The density of homogeneous polymethacrylimide foam material prepared by the present embodiment is 128kg/m
3, compressive strength is 3.63MPa.
embodiment 5:
(1) batching: 40g β-dimethyl-aminoethylmethacrylate, 40g acrylamide, 20g Methacrylamide, 0.6g Sulfothiorine, 1g 2,2'-Azobis(2,4-dimethylvaleronitrile), 5g carboxamide, 5g hexalin, 5g glycerol, 2g magnesium oxide, 2g calcium oxide are mixed, stir and stir at normal temperatures 30min by shaking table, obtain uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 130 DEG C of magnetic agitation reaction 5min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: described pre-polymerization liquid is injected in mould, and normal temperature is placed 22min, is then placed in 60 DEG C of water-baths, retains 70h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 185 DEG C, simultaneously to the mould 0.8MPa that exerts pressure, be cooled to normal temperature after retaining 3h, take out and obtain homogeneous polymethacrylimide foam material.
The density of homogeneous polymethacrylimide foam material prepared by the present embodiment is 163kg/m
3, compressive strength is 4.45MPa.
embodiment 6:
(1) batching: 30g β-dimethyl-aminoethylmethacrylate, 20g ethyl propenoate, 15g acrylamide, 35g Methacrylamide, 0.6g peroxy dicarbonate isopropyl ester, 1g Diisopropyl azodicarboxylate, 0.5g ammonium persulphate, 1g carboxamide, 8g methane amide, 5g n-Octanol, 1g calcium oxide, 2g cupric oxide are mixed, stir and stir at normal temperatures 20min by shaking table, obtain uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 115 DEG C of shaking table stirring reaction 25min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: described pre-polymerization liquid is injected in mould, and normal temperature is placed 30min, is then placed in 52 DEG C of water-baths, retains 88h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 240 DEG C, be cooled to normal temperature after reservation 0.5h, take out and obtain homogeneous polymethacrylimide foam material.
The density of homogeneous polymethacrylimide foam material prepared by the present embodiment is 183kg/m
3, compressive strength is 4.89MPa.
embodiment 7:
(1) batching: 20g methyl acrylate, 50g methyl methacrylate, 30g acrylamide, 1.6g peroxy dicarbonate isopropyl ester, 0.8g ammonium persulphate, 6g methane amide, 10g propyl carbinol, 1g magnesium oxide, 1.5g calcium oxide are mixed, stir and stir at normal temperatures 15min by shaking table, obtain uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 105 DEG C of ultrasonic agitation reaction 22min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: by shown in pre-polymerization liquid inject in mould, normal temperature is placed 15min, is then placed in 36 DEG C of water-baths, retains 90h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 230 DEG C, simultaneously to the mould 4.5MPa that exerts pressure, be cooled to normal temperature after retaining 4h, take out and obtain homogeneous polymethacrylimide foam material.
The density of homogeneous polymethacrylimide foam material prepared by the present embodiment is 171kg/m
3, compressive strength is 3.68MPa.
embodiment 8:
(1) batching: by 30g ethyl propenoate, 50g propyl methacrylate, 20g Methacrylamide, 1.5g di-cyclohexylperoxy dicarbonate, 1.5g dilauroyl peroxide, 3g methane amide, 3g n-Heptyl alcohol, 1.5g magnesium oxide, stir at normal temperatures 25min by electric stirring, obtain uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 110 DEG C of electric stirring reaction 15min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: described pre-polymerization liquid is injected in mould, and normal temperature is placed 20min, is then placed in 48 DEG C of water-baths, retains 80h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 210 DEG C, simultaneously to the mould 5.5MPa that exerts pressure, be cooled to normal temperature after retaining 3h, take out and obtain homogeneous polymethacrylimide foam material.
The density of homogeneous polymethacrylimide foam material prepared by the present embodiment is 277kg/m
3, compressive strength is 8.30MPa.
Claims (6)
1. a preparation method for homogeneous polymethacrylimide foam material, is characterized in that the step of the method is as follows:
(1) batching: by 30～80 parts of acrylic ester monomers; 20～70 parts of acrylamide monomers; 0.1～3 part of polymerization starter; 5～20 parts of whipping agents; 0.5～5 part of nucleator, mixes by weight, is stirred and is stirred at normal temperatures 10～30min by electric stirring, magnetic agitation, ultrasonic agitation or shaking table, obtains uniform mixing liquid;
(2) high-temperature stirring prepolymerization: described uniform mixing liquid, at 80～130 DEG C of electric stirrings, magnetic agitation, ultrasonic agitation or shaking table stirring reaction 5～60min, is obtained to pre-polymerization liquid;
(3) low temperature repolymerization: described pre-polymerization liquid is injected in mould, and normal temperature is placed 1～30min, is then placed in 30～60 DEG C of water-baths, retains 70～100h, takes out and obtains transparent block;
(4) high temperature foaming: described transparent block is put into mould, die temperature is maintained to 150～240 DEG C, simultaneously to the mould 0～10MPa that exerts pressure, be cooled to normal temperature after retaining 0.5～7h, take out and obtain homogeneous polymethacrylimide foam material.
2. the preparation method of a kind of homogeneous polymethacrylimide foam material according to claim 1, is characterized in that: described acrylic ester monomer be in methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate, methyl methacrylate, β-dimethyl-aminoethylmethacrylate, propyl methacrylate, methyl ester butyl acrylate any one or with both mixtures of arbitrary proportion.
3. the preparation method of a kind of homogeneous polymethacrylimide foam material according to claim 1, is characterized in that: described acrylamide monomers be in acrylamide, Methacrylamide any one or with both mixtures of arbitrary proportion.
4. the preparation method of a kind of homogeneous polymethacrylimide foam material according to claim 1, is characterized in that: described polymerization starter is the mixture of any one or any two kinds and above arbitrary proportion in dicumyl peroxide, dibenzoyl peroxide, di-cyclohexylperoxy dicarbonate, peroxy dicarbonate isopropyl ester, peroxide tert pivalate ester, dilauroyl peroxide, Potassium Persulphate, ammonium persulphate, Sulfothiorine, Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile).
5. the preparation method of a kind of homogeneous polymethacrylimide foam material according to claim 1, is characterized in that: described whipping agent is the mixture that chemical foaming agent and two parts of pneumatogen form with arbitrary proportion:
(1) chemical foaming agent: any one in carboxamide, methane amide or both mixture with arbitrary proportion composition;
(2) pneumatogen: any one in the fatty alcohol that contains 2～8 carbon atoms or arbitrarily several mixtures with arbitrary proportion.
6. the preparation method of a kind of homogeneous polymethacrylimide foam material according to claim 1, is characterized in that: described nucleator is the mixture of any one or any two kinds and above arbitrary proportion in magnesium oxide, calcium oxide, zinc oxide, cupric oxide.
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| CN104045952B (en) * | 2014-06-23 | 2015-11-04 | 浙江理工大学 | A kind of ungauged regions multipolymer and preparation method thereof |
| CN104045764B (en) * | 2014-06-23 | 2016-04-13 | 浙江理工大学 | A kind of preparation method of polymethacrylimide plastic foam |
| DE102014009338A1 (en) * | 2014-06-27 | 2015-12-31 | Evonik Röhm Gmbh | Pressure-dependent foam molding of poly (meth) acrylimide particles in closed tools for the production of rigid foam cores |
| CN106349419B (en) * | 2016-09-19 | 2019-03-08 | 浙江中科恒泰新材料科技有限公司 | A kind of polymethacrylimide foam and preparation method thereof |
| CN110256715B (en) * | 2019-06-20 | 2022-03-22 | 湖南兆恒材料科技有限公司 | Small-aperture polymethacrylimide foam and preparation method thereof |
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