CN106749837B - Preparation method of heat-conducting polymethacrylimide foam plastic - Google Patents

Preparation method of heat-conducting polymethacrylimide foam plastic Download PDF

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CN106749837B
CN106749837B CN201611087075.3A CN201611087075A CN106749837B CN 106749837 B CN106749837 B CN 106749837B CN 201611087075 A CN201611087075 A CN 201611087075A CN 106749837 B CN106749837 B CN 106749837B
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polymethacrylimide
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CN106749837A (en
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丁友家
陈敬清
彭本权
李德福
林杏江
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Haobo (fujian) New Material Technology Co Ltd
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Abstract

The invention discloses a preparation method of heat-conducting polymethacrylimide foamed plastic, which comprises the steps of uniformly dispersing heat-conducting filler into a mixed liquid formed by uniformly stirring and mixing (methyl) acrylic monomers, (methyl) acrylonitrile monomers, a foaming agent and an initiator at a material mixing stage, and sequentially carrying out polymerization reaction, pretreatment and foaming to prepare the heat-conducting polymethacrylimide foamed plastic. The prepared heat-conducting polymethacrylimide foamed plastic not only has good heat-conducting property, but also has excellent mechanical property, and can be widely applied to structural devices such as heat exchangers, heat-conducting pipes, coolers and the like.

Description

Preparation method of heat-conducting polymethacrylimide foam plastic
Technical Field
The invention relates to a preparation method of a foam material, in particular to a preparation method of heat-conducting polymethacrylimide foam plastic.
Background
The polymethacrylimide foamed plastic is a novel foamed plastic with high mechanical property, and is widely applied to the technical fields of aviation, aerospace, naval vessels, high-speed trains, wind power generation and the like. The composite material has outstanding heat resistance, excellent creep resistance and fatigue resistance at high temperature and the like, so that the composite material can be widely applied to the manufacture of composite material structural parts and the like. The polymethacrylimide foam plastic has the advantages of good mechanical property and the like, but has some defects such as poor electric conductivity and heat conductivity and the like, so that the application of the polymethacrylimide foam plastic in certain specific fields is limited.
The heat conduction material is widely applied to the fields of heat exchange engineering, heating engineering and the like. For a long time, metal materials are generally selected as heat conduction materials, but the corrosion resistance of the metal materials is poor, so that the application range of the metal materials is limited. In recent years, polymer materials have been the focus of research as heat conducting base materials, and the heat conducting polymer materials have the advantages of convenient processing and forming, uniform heat dissipation, high degree of freedom of product design, and the like, but the application of the heat conducting polymer materials commonly used at present, such as those using High Density Polyethylene (HDPE), Polystyrene (PS), and the like as base materials, in some specific fields is limited due to their poor mechanical properties, poor high temperature resistance, and the like.
At present, a plurality of patents relate to the preparation of polymethacrylimide foamed plastics, for example, patent applications with patent numbers of CN201410775265.9, CN200810031468.1, CN201510081558.1 and CN201510897014.2 all relate to a production method of polymethacrylimide foamed plastics, but the foamed materials produced by the above methods do not have heat-conducting property.
With the continuous development of the fields of aerospace, railway locomotives, ships, wind power generation and the like, the preparation of high polymer materials with high mechanical properties and good heat conductivity is imperative.
Disclosure of Invention
The invention aims to provide a preparation method of heat-conducting polymethacrylimide foam plastic with high mechanical property and good heat-conducting property.
In order to achieve the above purpose, the solution of the invention is:
a preparation method of heat-conducting polymethacrylimide foam plastic comprises the following steps:
(1) preparing materials: uniformly stirring and mixing a (meth) acrylic monomer, a (meth) acrylonitrile monomer, a foaming agent and an initiator to form a mixed liquid, uniformly dispersing a heat-conducting filler into the mixed liquid to obtain a suspension mixed liquid, wherein the amount of the (meth) acrylic monomer accounts for 40-60% of the weight of the monomer, the amount of the (meth) acrylonitrile monomer accounts for 40-60% of the total amount of the monomer, the initiator accounts for 0.01-0.5% of the total amount of the monomer, the foaming agent accounts for 5-30% of the total amount of the monomer, and the heat-conducting filler accounts for 1-20% of the total amount of the monomer, based on 100% of the total mass of the (meth) acrylic monomer and the (meth) acrylonitrile monomer;
(2) polymerization: the suspension mixed liquid obtained in the step (1) is subpackaged in a mould, then the mould is placed in a water tank for bulk polymerization, the polymerization temperature is controlled to be 25-60 ℃, and the mould is removed after 60-192 hours to obtain a heat-conducting (methyl) acrylic acid/(methyl) acrylonitrile copolymer plate;
(3) pretreatment: putting the heat-conducting (methyl) acrylic acid/(methyl) acrylonitrile copolymer plate obtained in the step (2) into a preheating oven, and heating the plate from 60 ℃ to 120 ℃ for cumulative baking for 24-48 hours;
(4) and (3) placing the heat-conducting (meth) acrylic acid/(meth) acrylonitrile copolymer plate obtained in the step (3) into a foaming furnace for foaming for 3-6 hours at the foaming temperature of 180-240 ℃, taking out the plate after foaming is finished, and cooling the plate to room temperature to obtain the heat-conducting polymethacrylimide foamed plastic.
In the step (1), the heat-conducting filler is one or a mixture of two or more of graphite, carbon fiber, carbon nanotube, graphene, aluminum nitride, silicon nitride, boron nitride, silicon carbide, boron carbide, aluminum powder and silver powder.
In the step (1), the foaming agent is one or a mixture of any several of formamide, acetamide, glycerol, ethylene glycol, 2-propanol, isopropanol, butanol, isobutanol, pentane, hexane, isohexane, octane and isooctane.
In the step (1), the initiator is one or a mixture of any more of azobisisobutyronitrile, azo di-tert-butyronitrile, azo dihydride, benzoyl peroxide, diacetyl peroxide, dibenzoyl peroxide, dioctanoyl peroxide, tert-butyl hydroperoxide and dicumyl peroxide.
After the technical scheme is adopted, the heat-conducting polymethacrylimide foamed plastic is prepared by uniformly dispersing the heat-conducting filler into the mixed liquid formed by uniformly stirring and mixing the (methyl) acrylic monomer, the (methyl) acrylonitrile monomer, the foaming agent and the initiator at the material preparation stage, and sequentially carrying out polymerization reaction, pretreatment and foaming steps. The prepared heat-conducting polymethacrylimide foamed plastic not only has good heat-conducting property, but also has excellent mechanical property, and can be widely applied to structural devices such as heat exchangers, heat-conducting pipes, coolers and the like.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
Preparation of polymethacrylimide foamed plastic
Examples 1 to 12:
(1) preparing materials: stirring 60 parts of methacrylic acid, 40 parts of methacrylonitrile, 0.5 part of initiator and 10 parts of foaming agent under a nitrogen atmosphere to obtain uniform mixed liquid, transferring the mixed liquid into an ultrasonic reaction tank with an ultrasonic dispersion instrument, adding 20 parts of heat-conducting filler, and performing ultrasonic treatment for 1 hour to uniformly disperse the heat-conducting filler into the mixed liquid to obtain suspended mixed liquid, wherein the used heat-conducting filler is shown in table 1 and is respectively marked as examples 1-12;
(2) polymerization: the suspension mixed liquid containing the heat-conducting filler is filled in a mold, then the mold is placed in a water tank for bulk polymerization, the reaction temperature is controlled to be 25-60 ℃, the reaction is carried out for 168 hours, and the mold is removed to obtain a heat-conducting (methyl) acrylic acid/(methyl) acrylonitrile copolymer plate;
(3) pretreatment: placing the heat-conducting (methyl) acrylic acid/(methyl) acrylonitrile copolymer plate into a preheating oven, baking for 6h at 60 ℃, baking for 12h at 80 ℃, and finally baking for 12h at 120 ℃ to obtain a further polymerized polymerization plate;
(4) foaming: and (4) placing the polymerization plate obtained in the step (3) in a foaming furnace, and foaming for 4 hours at the temperature of 220 ℃ to obtain the heat-conducting polymethacrylimide foam plastic.
Further, in the step (1), the foaming agent may be one or a mixture of any two of formamide, acetamide, glycerol, ethylene glycol, 2-propanol, isopropanol, butanol, isobutanol, pentane, hexane, isohexane, octane, and isooctane, and in order to ensure parallelism of data of the thermally conductive polymethacrylimide foam obtained in examples 1 to 12, the foaming agent is formamide.
In the step (1), the initiator may be one or a mixture of any several of azobisisobutyronitrile, azodi-tert-butyronitrile, azodihydride, benzoyl peroxide, diacetyl peroxide, dibenzoyl peroxide, dioctanoyl peroxide, tert-butyl hydroperoxide and dicumyl peroxide, and in order to ensure the parallelism of the data of the thermally conductive polymethacrylimide foam plastic obtained in embodiments 1 to 12, azobisisobutyronitrile is used as the initiator.
TABLE 1 Heat-conducting Filler for use in examples 1 to 12 and the amount thereof
Figure BDA0001167984290000061
Comparative example:
(1) preparing materials: stirring 60 parts of methacrylic acid, 40 parts of methacrylonitrile, 0.5 part of initiator azobisisobutyronitrile and 10 parts of foaming agent formamide under nitrogen atmosphere to obtain uniform mixed liquid;
(2) polymerization: the mixed liquid is subpackaged in a mold, then the mold is placed in a water tank for bulk polymerization, the reaction temperature is controlled to be 25-60 ℃, the reaction is carried out for 168 hours, and the mold is removed to obtain a (methyl) acrylic acid/(methyl) acrylonitrile copolymer plate;
(3) pretreatment: putting the (methyl) acrylic acid/(methyl) acrylonitrile copolymer plate into a preheating oven, baking for 6h at 60 ℃, baking for 12h at 80 ℃, and finally baking for 12h at 120 ℃ to obtain a further polymerized polymerization plate;
(4) foaming: and (4) placing the polymerization plate obtained in the step (3) in a foaming furnace, and foaming for 4 hours at the temperature of 220 ℃ to obtain the polymethacrylimide foamed plastic.
Secondly, testing the heat conduction performance:
the heat-conducting polymethacrylimide foamed plastics prepared in examples 1 to 12 and the polymethacrylimide foamed plastics prepared in proportion were respectively subjected to heat-conducting property tests, and the results are shown in table 2 and show that: the heat-conducting polymethacrylimide foamed plastic prepared in embodiments 1 to 12 has a heat-conducting property far better than that of the polymethacrylimide foamed plastic prepared in a comparative example, that is, the heat-conducting polymethacrylimide foamed plastic prepared by adding a heat-conducting filler in the preparation process has a good heat-conducting property, wherein the heat-conducting filler is aluminum powder, silver powder, or a mixture of graphite and aluminum powder, and the prepared heat-conducting polymethacrylimide foamed plastic has a particularly good heat-conducting property.
TABLE 2 evaluation of the thermal conductivity of polymethacrylimide foams
(test Standard ASTM C177-10)
Thirdly, testing mechanical properties:
mechanical property tests are respectively carried out on the heat-conducting polymethacrylimide foamed plastics prepared in examples 1-12 and the polymethacrylimide foamed plastics prepared in proportion, and the results are shown in table 3 and show that: compared with the mechanical properties of the polymethacrylimide foam plastics prepared in the comparative example, the mechanical properties of the heat-conducting polymethacrylimide foam plastics prepared in examples 1-12 are slightly inferior, but the difference is not large, namely the mechanical properties of the prepared heat-conducting polymethacrylimide foam plastics are better.
TABLE 3 evaluation of mechanical Properties of polymethacrylimide foams
The above embodiments are not intended to limit the form and style of the present invention, and any suitable changes or modifications made by those skilled in the art should be considered as not departing from the scope of the present invention.

Claims (3)

1. A preparation method of heat-conducting polymethacrylimide foamed plastic is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing materials: uniformly stirring and mixing a (methyl) acrylic monomer, a (methyl) acrylonitrile monomer, a foaming agent and an initiator to form a mixed liquid, uniformly dispersing a heat-conducting filler into the mixed liquid to obtain a suspension mixed liquid, wherein the (methyl) acrylic monomer accounts for 40-60% of the weight of the monomers, the (methyl) acrylonitrile monomer accounts for 40-60% of the total weight of the monomers, the initiator accounts for 0.01-0.5% of the total weight of the monomers, the foaming agent accounts for 5-30% of the total weight of the monomers, and the heat-conducting filler accounts for 1-20% of the total weight of the monomers according to 100% of the total weight of the (methyl) acrylic monomer and the (methyl) acrylonitrile monomer;
(2) polymerization: the suspension mixed liquid obtained in the step (1) is subpackaged in a mould, then the mould is placed in a water tank for bulk polymerization, the polymerization temperature is controlled to be 25-60 ℃, and the mould is removed after 60-192 hours to obtain a heat-conducting (methyl) acrylic acid/(methyl) acrylonitrile copolymer plate;
(3) pretreatment: putting the heat-conducting (methyl) acrylic acid/(methyl) acrylonitrile copolymer plate obtained in the step (2) into a preheating oven, and heating the plate from the stage of 60 ℃ to 120 ℃ for cumulative baking for 24-48 hours;
(4) placing the heat-conducting (meth) acrylic acid/(meth) acrylonitrile copolymer plate obtained in the step (3) in a foaming furnace for foaming for 3-6 hours at the foaming temperature of 180-240 ℃, and taking out and cooling to room temperature after foaming is completed to obtain the heat-conducting polymethacrylimide foamed plastic;
in the step (1), the heat-conducting filler is one or a mixture of any more of graphite, carbon fiber, carbon nano tube, aluminum nitride, silicon nitride, boron nitride, silicon carbide, boron carbide, aluminum powder and silver powder.
2. The method for preparing a heat-conducting polymethacrylimide foam as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the foaming agent is one or a mixture of any more of formamide, acetamide, glycerol, ethylene glycol, butanol, isobutanol, octane and isooctane.
3. The method for preparing a heat-conducting polymethacrylimide foam as claimed in claim 1, wherein the method comprises the following steps: in the step (1), the initiator is one or a mixture of any several of azodiisobutyronitrile, azodi-tert-butyronitrile, benzoyl peroxide, diacetyl peroxide, dioctanoyl peroxide, tert-butyl hydroperoxide and dicumyl peroxide.
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