CN103524968A - Method for preparing graphene reinforced PMI (polymethacrylimide) foam material - Google Patents
Method for preparing graphene reinforced PMI (polymethacrylimide) foam material Download PDFInfo
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Abstract
The invention discloses a method for preparing a graphene reinforced PMI (polymethacrylimide) foam material. Graphene is taken as a reinforcing material, methacrylonitrile and methacrylic acid are taken as a comonomer, an initiator, a crosslinking agent, a foaming agent, a nucleating agent and the like are added to prepare a foamable polymerized plate, and finally the foamable polymerized plate is freely foamed and subjected to thermal treatment in a drying oven so as to prepare polymethacrylimide rigid foam. Reactions of crosslinking, cyclization and the like are sufficiently conducted in the foaming and thermal treatment process, so as to harden copolymer molecular chain, and finally the foam plastic with excellent property is prepared. Due to adoption of the method, the tensile strength, the bending strength, the compression strength and the shearing strength of PMI are improved, and the electromagnetic shielding property and the anti-static property of the PMI foam are also improved. The PMI foam with excellent mechanical property can be widely applied to manufacturing of foam interlayer components in the fields of spaceflight, aviation, vessels, trains and the like.
Description
Technical field
The present invention relates to the preparation method that a kind of Graphene strengthens polymethacrylimide foam material.
Background technology
Graphene, as a kind of novel nano material, has the special property of a lot of excellences, and especially it has very high strength and stiffness, is the highest in current known materials.Graphene has so excellent strength and stiffness to be because in the atomic structure of Graphene, and the key becoming between carbon atom and carbon atom is the strongest chemical bond σ key.Graphene, except having very excellent strength and stiffness, also has excellent toughness and some special deformation mechanisms.
PMI porous plastics is the heat-resisting porous plastics that current strength and stiffness are the highest, and has excellent heat resistanceheat resistant creep property.The molecular structure of the strong polarity of PMI porous plastics, high rigidity and the foam structure of 100% closed pore have all guaranteed its thermotolerance, strength and stiffness.But the tensile strength of porous plastics and modulus, compressive strength and modulus, shearing resistance and modulus, flexural strength and modulus all obviously reduce along with reducing of foam plastic density, therefore can be by adding Graphene further to strengthen the mechanical property of PMI foam.But Graphene dispersion effect in the mother solution of preparation PMI foam is not good, very easily reunites.Make the PMI foam of preparing there will be mechanical heterogeneity, the unconspicuous phenomenon of reinforced effects.
Summary of the invention
In order to solve along with the tensile strength of PMI foam and the mechanical property such as modulus, compressive strength and modulus, shearing resistance and modulus, flexural strength and modulus reduce with density and obviously reduce this problem.The object of this invention is to provide the preparation method that a kind of Graphene strengthens polymethacrylimide foam material, the Graphene that the method has excellent in strength and rigidity by use further strengthens the mechanical mechanics property of PMI foam, and the Graphene of preparing high dispersing strengthens PMI foam.
The object of the invention is to be achieved through the following technical solutions:
A kind of Graphene strengthens the preparation method of polymethacrylimide foam material, it is characterized in that: the method is carried out the recipe ingredient of following weight part ratio that high-speed stirring is mixed to be incorporated in ultrasonic separating apparatus Graphene high dispersing in raw material, stock liquid is fed in glass mold, and in close die, polymerization reaction take place foaming form;
Graphene 2 ~ 20
Methacrylonitrile 40 ~ 60
Methacrylic acid 40 ~ 60
Initiator 0.1 ~ 0.3
Whipping agent 0.5 ~ 8.0
Linking agent 2.0 ~ 3.0
Nucleator 0.5 ~ 2.0
Concrete preparation process is as follows:
(1) monomer, initiator, linking agent, whipping agent, nucleator are mixed according to weight part ratio, under the bath temperature of 15-25 ℃, by 1000 ~ 3000r/min stirrer rotating speed, mix 1 ~ 3h reaction solution is stirred;
(2) Graphene is added in reaction solution, mixed solution is positioned in ultrasonic separating apparatus under 5kHz ~ 50kHz frequency, ultrasonic dispersion 20 ~ 50min, can be by Graphene high dispersing in raw material;
(3) stock liquid perfusion is entered in the closed grinding tool of being made by two blocks of unorganic glass plates and rubber, after injection stock liquid, by stainless steel clip, mould is clamped on four sides;
(4) the glass grinding tool that pours into stock liquid is put into and had recirculated water function water bath, adopt the bath temperature of 35 ~ 65 ℃, make stock liquid generation polymerization, polymerization time 48 ~ 72h, can obtain foamable polymeric plate;
(5) foamed polymeric plate top punching step (4) being obtained, hang on can the baking oven of free foaming in; Free foaming in 200 ~ 220 ℃ of strong recirculated hot airs, foamed time: 1h ~ 3h, obtains foam materials;
(6) foam materials step (5) being obtained is put into baking oven and is heat-treated, 150 ~ 200 ℃ of thermal treatment temps, and thermal treatment 10 ~ 20h, and naturally cool to room temperature, obtain Graphene and strengthen polymethacrylimide foam material.
In the present invention, described primosome agent is Diisopropyl azodicarboxylate or benzoyl peroxide and Diisopropyl azodicarboxylate mixture.Preferably: Diisopropyl azodicarboxylate.Described whipping agent adopts propylene glycol or methane amide, preferably: adopt propylene glycol.Described linking agent adopts acrylamide or Methacrylamide, preferably: adopt Methacrylamide.Described nucleator adopts urea, MU or magnesium oxide, preferably: adopt urea.
The Graphene the present invention relates to strengthens polymethacrylimide plastic foam to be compared with the PMI foam of conventional type, has following some advantage:
1,, in the atomic structure due to Graphene, the key becoming between carbon atom and carbon atom is the strongest chemical bond σ key.Make Graphene except having very excellent strength and stiffness, also there are excellent toughness and some special deformation mechanisms.Therefore adding of Graphene strongthener the mechanical property of low density PMI foam is further improved, make PMI foam applications field more extensive.
2, Graphene dispersion effect in the mother solution of preparation PMI foam is not good, very easily reunites.Make the PMI foam of preparing there will be mechanical heterogeneity, the unconspicuous phenomenon of reinforced effects.The present invention utilizes ultrasonic separating apparatus to carry out ultrasonic dispersion, can make graphene powder high dispersing among the raw material of PMI foam, and not reunite.
3, the linking agent Methacrylamide adding can be used as the 3rd monomer, on Methacrylamide chain link
-CONH
2can with other molecular chain on-CONH
2there is deamination imidization reaction, can with other molecular chain-there is dehydration imidization reaction, molecular chain occurred crosslinked in COOH.Methacrylamide chain link-CONH
2can also with a CONH of adjacent link
2or-there is cyclization in COOH, improves molecular chain rigidity, is conducive to the stable curing of porous plastics abscess.
The present invention adds Graphene as strongthener in PMI foam makes it very in high level, improve tensile strength, flexural strength, compressive strength, the shearing resistance of PMI foam, and has also increased capability of electromagnetic shielding, the antistatic property of PMI foam simultaneously.The PMI foam that has very good mechanical properties can be widely used in the manufacture of the field foam layer members such as space flight, aviation, ships, train.
Accompanying drawing explanation
Fig. 1 is preparation flow figure of the present invention.
Embodiment
Graphene strengthens a preparation method for polymethacrylimide foam material, and Graphene strengthens polymethacrylimide foam and is comprised of Graphene, monomer, initiator, linking agent, whipping agent, nucleator.The recipe ingredient weight part ratio of concrete formula example 1,2,3,4 as shown in table 1.
Table 1 Graphene strengthens the embodiment of polymethacrylimide foam material
Concrete preparation process is as follows:
(1) monomer, initiator, linking agent, whipping agent, nucleator are mixed respectively according to the weight part ratio of example 1,2,3,4, under the bath temperature of 25 ℃, by the mixing of 3000r/min stirrer rotating speed, 3h stirs reaction solution;
(2) Graphene is added in material solution, mixed solution is positioned in ultrasonic separating apparatus under 50kHz frequency, ultrasonic dispersion 50min, can be by among Graphene high dispersing and raw material;
(3) stock liquid perfusion is entered in the closed grinding tool of being made by two blocks of unorganic glass plates and rubber.After injecting stock liquid, by stainless steel clip, mould is clamped on four sides;
(4) the glass grinding tool that pours into stock liquid is put into and had recirculated water function water bath, adopt 45 ℃ of waters bath with thermostatic control to make material solution generation polymerization, polymerization time 72h, can obtain foamable polymeric plate;
(5) by the foamed polymeric plate top punching obtaining, hang on can the baking oven of free foaming in.Free foaming in 210 ℃ of strong recirculated hot airs, foamed time: 2h, can obtain Graphene and strengthen polymethacrylimide foam material;
(6) foam materials obtaining is put into pump circulation air oven at this and heat-treat, 160 ℃ of thermal treatment temps, thermal treatment 10h; And naturally cool to room temperature, obtain Graphene and strengthen polymethacrylimide foam material.
The density ratio of the foam that four kinds of embodiment prepare is more approaching.The PMI foam of four kinds of embodiment being prepared according to relevant criterion carries out Mechanics Performance Testing, and test result is as shown in table 2 below.
The mechanical property of table 2 PMI foam
Adding along with Graphene strongthener as seen from Table 2, the compressive strength of PMI foam, tensile strength, flexural strength, shearing resistance are all multiplied, but while reaching 10 parts along with Graphene parts by weight, the trend that the mechanical property of foam strengthens slows down to some extent, may be due to the amount along with Graphene be increased to 10 parts of left and right time, make part Graphene occur reunite and to be difficult to the reason of disperseing at reaction solution camber at stock liquid.
Claims (5)
1. a Graphene strengthens the preparation method of polymethacrylimide foam material, it is characterized in that: the method is carried out the recipe ingredient of following weight part ratio that high-speed stirring is mixed to be incorporated in ultrasonic separating apparatus Graphene high dispersing in raw material, stock liquid is fed in glass mold, and in close die, polymerization reaction take place foaming form;
Graphene 2 ~ 20
Methacrylonitrile 40 ~ 60
Methacrylic acid 40 ~ 60
Initiator 0.1 ~ 0.3
Whipping agent 0.5 ~ 8.0
Linking agent 2.0 ~ 3.0
Nucleator 0.5 ~ 2.0
Concrete preparation process is as follows:
(1) monomer, initiator, linking agent, whipping agent, nucleator are mixed according to weight part ratio, under the bath temperature of 15-25 ℃, by 1000 ~ 3000r/min stirrer rotating speed, mix 1 ~ 3h reaction solution is stirred;
(2) Graphene is added in reaction solution, mixed solution is positioned in ultrasonic separating apparatus under 5kHz ~ 50kHz frequency, ultrasonic dispersion 20 ~ 50min, can be by Graphene high dispersing in raw material;
(3) stock liquid perfusion is entered in the closed grinding tool of being made by two blocks of unorganic glass plates and rubber, after injection stock liquid, by stainless steel clip, mould is clamped on four sides;
(4) the glass grinding tool that pours into stock liquid is put into and had recirculated water function water bath, adopt the bath temperature of 35 ~ 65 ℃, make stock liquid generation polymerization, polymerization time 48 ~ 72h, can obtain foamable polymeric plate;
(5) foamed polymeric plate top punching step (4) being obtained, hang on can the baking oven of free foaming in; Free foaming in 200 ~ 220 ℃ of strong recirculated hot airs, foamed time: 1h ~ 3h, obtains foam materials;
(6) foam materials step (5) being obtained is put into baking oven and is heat-treated, 150 ~ 200 ℃ of thermal treatment temps, and thermal treatment 10 ~ 20h, and naturally cool to room temperature, obtain Graphene and strengthen polymethacrylimide foam material.
2. according to the described Graphene of claim 1, strengthen the preparation method of polymethacrylimide foam material, it is characterized in that: described primosome agent is Diisopropyl azodicarboxylate or benzoyl peroxide and Diisopropyl azodicarboxylate mixture.
3. according to the described Graphene of claim 1, strengthen the preparation method of polymethacrylimide foam material, it is characterized in that: described whipping agent adopts propylene glycol or methane amide.
4. according to the described Graphene of claim 1, strengthen the preparation method of polymethacrylimide foam material, it is characterized in that: described linking agent adopts acrylamide or Methacrylamide.
5. according to the described Graphene of claim 1, strengthen the preparation method of polymethacrylimide foam material, it is characterized in that: described nucleator adopts urea, MU or magnesium oxide.
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| CN104004308A (en) * | 2014-06-20 | 2014-08-27 | 江苏兆鋆新材料股份有限公司 | Nanoscale calcium carbonate modified polymethacrylamide foam and preparing method thereof |
| CN105524466A (en) * | 2014-09-28 | 2016-04-27 | 中国科学院苏州纳米技术与纳米仿生研究所 | Porous graphene electromagnetic wave absorbing composite material, preparation method and applications thereof |
| EP3144344A1 (en) * | 2015-09-15 | 2017-03-22 | Evonik Röhm GmbH | Multifunctional alcohols as crosslinking agents for pmi foams |
| CN106749837A (en) * | 2016-12-01 | 2017-05-31 | 浩博（福建）新材料科技有限公司 | A kind of preparation method of heat conduction polymethacrylimide plastic foam |
| CN108638604A (en) * | 2018-05-15 | 2018-10-12 | 西安交通大学 | Graphene enhances PMI foams-pyramid sandwich plate composite construction and preparation method thereof |
| CN109096674A (en) * | 2017-06-21 | 2018-12-28 | 洛阳尖端技术研究院 | A kind of graphite oxide alkenyl foam wave absorption base material and preparation method thereof |
| CN110256716A (en) * | 2019-05-21 | 2019-09-20 | 湖南兆恒材料科技有限公司 | A kind of helicopter polymethacrylimide foam material and preparation method |
| CN110746638A (en) * | 2019-12-02 | 2020-02-04 | 南京航空航天大学 | Method for preparing carbon nanofiber reinforced polymethacrylimide foam through suspension polymerization |
| CN113150227A (en) * | 2021-04-01 | 2021-07-23 | 太仓博德房车科技有限公司 | High-strength light composite thermal insulation material for motor home |
| CN113733680A (en) * | 2021-09-14 | 2021-12-03 | 合肥晋怡科技有限公司 | Wave-absorbing polymethacrylimide foam composite material |
| WO2022071912A1 (en) * | 2020-10-02 | 2022-04-07 | Roketsan Roket Sanayi̇i̇ Ti̇caret A.Ş. | In-situ synthesized polymetacrilymide (pmi) foam with nanosized material and the production method thereof |
| CN115500067A (en) * | 2022-09-02 | 2022-12-20 | 苏州申赛新材料有限公司 | Low-reflection magnetic-electric dual-function electromagnetic shielding composite material with gradient structure |
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| CN104004308A (en) * | 2014-06-20 | 2014-08-27 | 江苏兆鋆新材料股份有限公司 | Nanoscale calcium carbonate modified polymethacrylamide foam and preparing method thereof |
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| CN106749837A (en) * | 2016-12-01 | 2017-05-31 | 浩博（福建）新材料科技有限公司 | A kind of preparation method of heat conduction polymethacrylimide plastic foam |
| CN109096674A (en) * | 2017-06-21 | 2018-12-28 | 洛阳尖端技术研究院 | A kind of graphite oxide alkenyl foam wave absorption base material and preparation method thereof |
| CN109096674B (en) * | 2017-06-21 | 2022-04-08 | 洛阳尖端技术研究院 | Graphene oxide-based foam wave-absorbing base material and preparation method thereof |
| CN108638604A (en) * | 2018-05-15 | 2018-10-12 | 西安交通大学 | Graphene enhances PMI foams-pyramid sandwich plate composite construction and preparation method thereof |
| CN110256716B (en) * | 2019-05-21 | 2022-03-18 | 湖南兆恒材料科技有限公司 | Polymethacrylimide foam material for helicopter and preparation method thereof |
| CN110256716A (en) * | 2019-05-21 | 2019-09-20 | 湖南兆恒材料科技有限公司 | A kind of helicopter polymethacrylimide foam material and preparation method |
| CN110746638A (en) * | 2019-12-02 | 2020-02-04 | 南京航空航天大学 | Method for preparing carbon nanofiber reinforced polymethacrylimide foam through suspension polymerization |
| WO2022071912A1 (en) * | 2020-10-02 | 2022-04-07 | Roketsan Roket Sanayi̇i̇ Ti̇caret A.Ş. | In-situ synthesized polymetacrilymide (pmi) foam with nanosized material and the production method thereof |
| CN113150227A (en) * | 2021-04-01 | 2021-07-23 | 太仓博德房车科技有限公司 | High-strength light composite thermal insulation material for motor home |
| CN113733680A (en) * | 2021-09-14 | 2021-12-03 | 合肥晋怡科技有限公司 | Wave-absorbing polymethacrylimide foam composite material |
| CN115500067A (en) * | 2022-09-02 | 2022-12-20 | 苏州申赛新材料有限公司 | Low-reflection magnetic-electric dual-function electromagnetic shielding composite material with gradient structure |
| CN115500067B (en) * | 2022-09-02 | 2023-08-29 | 苏州申赛新材料有限公司 | Electromagnetic shielding composite material with low-reflection magneto-electric dual-functional gradient structure |
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Address after: Jiangsu Zhenjiang Jurong City Huayang Road 212400 No. 99 Patentee after: Jiangsu Zhao Lam novel material limited-liability company Address before: 212400 Zhenjiang city of Jiangsu province Jurong City Huayang town Dongchang Road No. 20, Zhao Jun Patentee before: Jiangsu Zhaoyun New Material Technology Co.,Ltd. |
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