CN110105665A - A kind of thermosetting/thermoplastic copoly type composite foam and its preparation method and application - Google Patents

A kind of thermosetting/thermoplastic copoly type composite foam and its preparation method and application Download PDF

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Publication number
CN110105665A
CN110105665A CN201910414817.6A CN201910414817A CN110105665A CN 110105665 A CN110105665 A CN 110105665A CN 201910414817 A CN201910414817 A CN 201910414817A CN 110105665 A CN110105665 A CN 110105665A
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China
Prior art keywords
thermosetting
resin
composite foam
thermoplastic
copoly type
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Pending
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CN201910414817.6A
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Chinese (zh)
Inventor
陈智勇
刘建寿
康翔宇
姚永玉
李妙玲
程广伟
李彬
张广广
张俊锋
周方伟
杨洋
周超帆
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Luoyang Institute of Science and Technology
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Luoyang Institute of Science and Technology
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Priority to CN201910414817.6A priority Critical patent/CN110105665A/en
Publication of CN110105665A publication Critical patent/CN110105665A/en
Pending legal-status Critical Current

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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/18—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer of foamed material
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
    • B32B5/245—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it being a foam layer
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Abstract

The present invention relates to a kind of thermosetting/thermoplastic copoly type composite foam and its preparation method and application, preparation method: a, heated after mixing tiny balloon with coupling agent；B, thermosetting resin matrix and curing agent are stirred and evenly mixed；C, modified tiny balloon and resin matrix are stirred evenly, obtains tiny balloon/thermosetting resin；D, foaming agent, the maleic anhydride inoculated polypropylene by modification and thermoplastic resin matrix are stirred mixed；E, mixed resin is uniformly mixed with tiny balloon/thermosetting resin；F, it is put into extruder or injection molding machine prepares forming material or sheet material；G, profile or sheet material are heated, obtains novel thermosetting/thermoplastic copoly type composite foam.The sandwich foaming structure with thermoplastic and same with thermosetting compound material can be widely applied in composite foam of the invention, it is particularly suitable for the composite material sandwich structure of thin layer, the fields such as composite structure including automotive upholstery, all kinds of electronic product casings, the shell of spitkit, unmanned plane.

Description

A kind of thermosetting/thermoplastic copoly type composite foam and its preparation method and application
Technical field
The present invention relates to polymer matrix composites technical fields, and in particular to a kind of thermosetting/thermoplastic copoly type composite foam And its preparation method and application.
Background technique
Composite foam is also known as polymeric composite foam, syntactic foam, it is light by glass microsphere or ceramic microsphere etc. A kind of foam that the high-strength hollow ball of matter and matrix resin are combined into.This material can compared with low-density energy Enough intensity is kept, there is high compression-strength/weight ratio, the characteristic of low creep and low water absorption.Heat cured epoxy composite Foam has been widely used in underwater equipment, therefore also referred to as solid buoyancy material.In some high performance thin layer composite materials Used also as structural type foam core material in feed collet cored structure, it has been widely used in aerospace in composite material.Compound vacuole Its stiffness and strength of foam are much higher than conventional foam materials.
The density of composite foam is very low to be primarily due to evenly dispersed a large amount of hollow ball in basis material.It is used Tiny balloon have glass microsphere, polymer microballoon, ceramic microsphere, carbosphere, metallic microspheres etc..Diameter is at 20 to 150 microns Between, the partial size of tiny balloon determines the abscess-size of composite foam.Tiny balloon passes through after coupling agent surface treatment Advanced contour machining procedure is organically fused together with matrix resin, further enhances entire material property.To base The requirement of body material is that bonding force is strong, water absorption rate is low, hot property and excellent electrical properties.The total body density of composite foam can control In 0.40g/cm3To 0.65g/cm3Between.
Existing composite foam is divided into heat curing type and thermoplastics type, and heat curing type foam core material can only be with heat cured composite material Surface layer is bonded, and similarly, thermoplastic foam core material can only carry out be bonded with thermoplastic composite surface layer, and otherwise have can for pole The splitting phenomenon of composite faces and core material can occur, fail so as to cause the sandwich structure of composite material.For In the patent of thermoplastic composite foam at home and abroad, it is primarily related to glass microballoon filling thermoplastic resin's matrix；And for In the domestic and international patent of thermosetting property composite foam, what is related generally to is then glass microballoon filled thermoset resin matrix.This patent The thermosetting referred to/thermoplastic blending type composite foam and its to the adhering method of carbon fibre composite surface layer it is disclosed it is related specially There has been no data to refer in benefit and document.
Summary of the invention
The purpose of the present invention is deficiencies to solve above-mentioned technical problem, provide a kind of thermosetting/thermoplastic copoly type compound vacuole The sandwich foaming structure with thermoplastic and same with thermosetting compound material can be widely applied in foam and its preparation method and application, especially suitable For the composite material sandwich structure of thin layer, including automotive upholstery, all kinds of electronic product casings, spitkit shell, The fields such as the composite structure of unmanned plane.
The deficiency of the present invention to solve above-mentioned technical problem, used technical solution is: a kind of thermosetting/thermoplastic copoly type The preparation method of composite foam, comprising the following steps:
A, it is heated after mixing tiny balloon with coupling agent, obtains modified tiny balloon, it is spare；
B, thermosetting resin matrix is stirred and evenly mixed with curing agent, it is spare；
C, the resin matrix prepared in modification tiny balloon and step b prepared by step a is stirred evenly, obtain tiny balloon/ Thermosetting resin, it is spare；
D, foaming agent, maleic anhydride inoculated polypropylene and thermoplastic resin matrix are stirred and evenly mixed, obtains mixed resin, it is spare；
E, mixed resin prepared by step d is uniformly mixed with tiny balloon/thermosetting resin prepared by step c, is mixed Prefabricated material, it is spare；
F, the prefabricated material of mixing prepared by step e is put into the hopper of extruder or injection molding machine, prepares forming material or sheet material；
G, the step f profile prepared or sheet material are heated, solidifies the thermosetting resin in material sufficiently to get novel heat is arrived Gu/thermoplastic copoly type composite foam.
As a kind of advanced optimizing for preparation method of thermosetting/thermoplastic copoly type composite foam of the invention: described hollow Microballoon is glass microsphere, polymer microballoon, ceramic microsphere, carbosphere or metallic microspheres, and tiny balloon is set using preceding with baking It is standby to remove wherein remaining moisture.
As a kind of advanced optimizing for preparation method of thermosetting/thermoplastic copoly type composite foam of the invention: the thermosetting Property resin matrix be epoxy resin body, alkenyl esters resin, phenolic resin, unsaturated polyester resin or polyimide resin.
As a kind of advanced optimizing for preparation method of thermosetting/thermoplastic copoly type composite foam of the invention: the thermoplastic Property resin be acrylic resin, nylon, polyethylene, polyester, polyamide, polyformaldehyde or their copolymer.
As a kind of advanced optimizing for preparation method of thermosetting/thermoplastic copoly type composite foam of the invention: the foaming Agent is swellable polymer microballoon, azodicarbonamide or hydrocarbon blowing agents.
As a kind of advanced optimizing for preparation method of thermosetting/thermoplastic copoly type composite foam of the invention: step a is hollow The ratio between additional amount of heart microballoon and coupling agent is 100:0.1-10, the additional amount of thermosetting resin matrix and curing agent in step b The ratio between be 100:10-150, the ratio between modified tiny balloon and additional amount of resin matrix are 100:80-150, step d in step c The ratio between middle foaming agent, thermoplastic resin matrix, the additional amount of maleic anhydride inoculated polypropylene are 0.1-10:30-60:5-20, step The ratio between mixed resin and tiny balloon/thermosetting resin additional amount are 100:50-100 in rapid e.
As a kind of advanced optimizing for preparation method of thermosetting/thermoplastic copoly type composite foam of the invention: the step f The temperature of middle forming process setting is 190 DEG C, in step e by foam be put into drying chamber or baking oven be heated to after 120 DEG C of heat preservation 3h by Step is cooled to room temperature, and heating and cooling rate are controlled in 1 DEG C/min.
A kind of thermosetting/thermoplastic copoly type composite foam, is made by the preparation method of above-mentioned composite foam.
Above-mentioned thermosetting/thermoplastic copoly type composite foam is preparing the application in sandwich structure composite material.
Above-mentioned thermosetting/thermoplastic copoly type composite foam is preparing the application in sandwich structure composite material: taking polyester fine Fabric, carbon fiber/epoxy resin prepreg and composite foam are tieed up, is knitted according to carbon fiber/epoxy resin prepreg-polyester fiber Object-composite foam-dacron fabric-carbon fiber/epoxy resin prepreg sequence is laid with together, in the pressure of 1.0MPa Under, 150 DEG C of heat preservation 20min are warming up to, naturally cool to 50 DEG C, are taken out to get sandwich structure composite material is arrived.
Beneficial effect
One, the present invention is by selecting while including the thermosetting resin and thermoplastic resin of certain content, and combines certain content Hollow ball, the thermosetting being prepared/thermoplastic copoly type composite foam can be widely applied and thermoplastic and thermosetting property composite wood The sandwich foaming structure of material is particularly suitable for the composite material sandwich structure of thin layer, including automotive upholstery, each electron-like produce The fields such as composite structure of product shell, the shell of spitkit, unmanned plane；
Two, composite foam produced by the present invention can be respectively or same with thermosetting property and/or thermoplasticity carbon fibre composite surface layer Shi Jinhang bonding, and the composite foam and thermosetting property and/or the adhesive property of thermoplastic composite surface layer are good, are not in The splitting phenomenon of the composite foam and thermosetting property and/or thermoplastic composite surface layer.
Detailed description of the invention
Fig. 1 is the flow chart schematic diagram of composite foam preparation process of the present invention；
Fig. 2 is the connection mechanism schematic diagram of composite foam each component of the present invention；
Fig. 3 is the preparation process schematic diagram of composite foam of the present invention；
Fig. 4 is the preparation process schematic diagram of sandwich structure composite material of the present invention；
Fig. 5 is the stereoscan photograph of composite foam of the present invention；
Fig. 6 is the stereoscan photograph of sandwich structure composite material of the present invention；
The test chart of Fig. 7 adhesive strength between surface layer and core material；
Fig. 8 is the three-point bend test figure of sandwich structure composite material of the present invention.
Specific embodiment
Further technical solution of the present invention is illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of thermosetting/thermoplastic copoly type composite foam, preparation process and process are as shown in figures 1 and 3, including with Lower step:
Raw material inventory is as follows:
A, the hollow glass micro-ball K20 for taking 100Kg is surface-treated, heated baking with 1Kg coupling agent KH560, removes surface Solvent obtains modified hollow glass micro-ball, spare；
B, extracting epoxy resin 100Kg is added anhydride curing agent 80Kg, stirs evenly, vacuum method removes bubble removing, spare；
C, the resin matrix 107.8Kg stirring prepared in the modification hollow glass micro-ball 100Kg and step b for taking step a to prepare is equal It is even, hollow glass micro-ball/thermosetting resin is obtained, it is spare；
D, it takes swellable polymer microballoon 2Kg, polypropylene 80Kg, maleic anhydride inoculated polypropylene 80Kg to stir and evenly mix, is mixed Base-material, it is spare；
E, hollow glass micro-ball/thermosetting resin 86Kg that the mixed resin 100Kg for taking step d to prepare is prepared with step c is mixed Uniformly, it obtains mixing prefabricated material, it is spare；
F, the step e mixture prepared is put into the hopper of extruder or injection molding machine, the temperature of machine is set as 190 DEG C, system Standby forming material or sheet material；
G, by the step f profile prepared or sheet material be put into drying chamber or baking oven be heated to 120 DEG C of heat preservation 3h after be gradually cooled to room temperature, Heating and cooling rate are in 1 DEG C/min or so to get the novel thermosetting/thermoplastic copoly type compound vacuole for being 500kg/m3 to density Foam (SEM photograph that Fig. 5 is composite foam).
The chemical reaction mechanism of each component is as shown in Figure 2 in composite foam.Hydroxyl in methyl tetrahydro phthalic anhydride can be with sky Siloxy in heart glass microsphere reacts to form chemical bonds, while playing the role of cured epoxy resin again, epoxy resin Chemical bonds can occur with maleic anhydride modified polypropylene again, and there are physical entanglement between two kinds of polypropylene, from And composite foam is made to become an effective overall structure.
Embodiment 2
A kind of preparation method of thermosetting/thermoplastic copoly type composite foam, comprising the following steps:
A, the hollow glass micro-ball K20 for taking 100Kg is surface-treated, heated baking with 5Kg coupling agent KH560, removes surface Solvent obtains modified hollow glass micro-ball, spare；
B, extracting epoxy resin 100Kg is added anhydride curing agent 10Kg, stirs evenly, vacuum method removes bubble removing, spare；
C, the resin matrix 80Kg prepared in the modification hollow glass micro-ball 100Kg and step b for taking step a to prepare is stirred evenly, Hollow glass micro-ball/thermosetting resin is obtained, it is spare；
D, it takes foaming agent 10Kg, epoxy resin-base 160Kg, maleic anhydride inoculated polypropylene 120Kg to stir and evenly mix, is mixed Base-material, it is spare；
E, tiny balloon/thermosetting resin 100Kg that the mixed resin 100Kg for taking step d to prepare is prepared with step c is mixed It is even, it obtains mixing prefabricated material, it is spare；
F, the step e mixture prepared is put into the hopper of extruder or injection molding machine, the temperature of machine is set as 190 DEG C, system Standby forming material or sheet material；
G, by the step f profile prepared or sheet material be put into drying chamber or baking oven be heated to 120 DEG C of heat preservation 3h after be gradually cooled to room temperature, Heating and cooling rate are in 1 DEG C/min or so to get the novel thermosetting/thermoplastic copoly type compound vacuole for being 500kg/m3 to density Foam.
H, preparing surface density is 30g/m22 layers of dacron fabric, 155 g/m of surface density2Carbon fiber/epoxy resin Two layers of prepreg, with a thickness of one layer of epoxy-modified composite material of 1.0mm, and laying is carried out in the way of Fig. 4；
I, by the sandwich composite material placed in sequence under the pressure of 1.0MPa, 150 DEG C of heat preservation 20min are warming up to, 50 DEG C are naturally cooled to, is taken out to get sandwich composite structure, thickness about 1.5mm, global density about 0.8g/cm is arrived3。 Fig. 6 is the metallograph of sandwich composite structure.
Embodiment 3:
A kind of preparation method of thermosetting/thermoplastic copoly type composite foam, comprising the following steps:
A, the hollow glass micro-ball K20 for taking 100Kg is surface-treated, heated baking with 0.5Kg coupling agent KH560, removes table Face solvent obtains modified tiny balloon, spare；
B, extracting epoxy resin 100Kg is added anhydride curing agent 20Kg, stirs evenly, vacuum method removes bubble removing, spare；
C, the resin matrix 150Kg prepared in the modification tiny balloon 100Kg and step b for taking step a to prepare is stirred evenly, and is obtained Tiny balloon/thermosetting resin, it is spare；
D, it takes foaming agent 2Kg, thermoplastic resin matrix 80Kg, maleic anhydride inoculated polypropylene 80Kg to stir and evenly mix, is mixed Base-material, it is spare；
E, tiny balloon/thermosetting resin 50Kg that the mixed resin 100Kg for taking step d to prepare is prepared with step c is uniformly mixed, It obtains mixing prefabricated material, it is spare；
F, the step e mixture prepared is put into the hopper of extruder or injection molding machine, the temperature of machine is set as 190 DEG C, system Standby forming material or sheet material；
G, by the step f profile prepared or sheet material be put into drying chamber or baking oven be heated to 120 DEG C of heat preservation 3h after be gradually cooled to room temperature, Heating and cooling rate are in 1 DEG C/min or so to get the novel thermosetting/thermoplastic copoly type compound vacuole for being 500kg/m3 to density Foam.
H, prepare 155 g/m of surface density2Two layers of carbon fiber/epoxy resin prepreg, with a thickness of the composite foam of 1.0mm One layer, composite foam is clipped between two layers of carbon fiber/epoxy resin prepreg and carries out laying；
I, by the composite material placed in sequence under the pressure of 1.0MPa, 150 DEG C of heat preservation 20min are warming up to, it is naturally cold But it to 50 DEG C, takes out to get the composite material of transition zone dacron fabric is free of.
The composite material that the composite material and embodiment 3 that Example 2 is prepared are prepared, uses hubbing opposite Adhesive strength between layer and core material compares test, and test chart is shown in that (a is before pull-out test, b is compound containing transition zone to Fig. 7 After material drawing, c be without transition layer composite drawing after).Test result is distributed as the pulling capacity containing transition zone 3.3MPa, the pulling capacity without transition zone are 0.5MPa.After the adhesive transition layer of core material and Pavement Composite Material is added, the two it Between adhesive effect be obviously improved.
Reference standard GB/T 1449-2005 fibre reinforced plastics bending property test method is knitted to transition zone PET is added Object and the sandwich composite structure progress three-point bend test for not adding transition zone, the sandwich structure after transition zone is added are multiple 650.7 MPa of condensation material crooked test intensity destroys position and does not occur lamination, the sandwich composite wood of depth was not added Material bending strength is 243.4MPa, is destroyed between the core material and carbon fiber surface layer that position occurs, it can be seen that apparent layering is existing As.
Embodiment 4-7:
A kind of preparation method of thermosetting/thermoplastic copoly type composite foam, other conditions are replaced respectively with embodiment 1, by epoxy resin It is changed to alkenyl esters resin, phenolic resin, unsaturated polyester resin and polyimide resin.
Embodiment 8-12:
A kind of preparation method of thermosetting/thermoplastic copoly type composite foam, other conditions distinguish acrylic resin with embodiment 1 Replace with nylon, polyethylene, polyester, polyamide and polyformaldehyde.
Embodiment 13-14:
A kind of preparation method of thermosetting/thermoplastic copoly type composite foam, other conditions are with embodiment 1, by swellable polymer microballoon Azodicarbonamide and hydrocarbon blowing agents are replaced with respectively.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make out a little change or repair Decorations are the equivalent embodiment of equivalent variations, but without departing from the technical solutions of the present invention, according to the technical essence of the invention Any simple modification, equivalent change and modification to the above embodiments, all of which are still within the scope of the technical scheme of the invention.

Claims (10)

1. a kind of thermosetting/thermoplastic copoly type composite foam preparation method, it is characterised in that: the following steps are included:
A, it is heated after mixing tiny balloon with coupling agent, obtains modified tiny balloon, it is spare；
B, thermosetting resin matrix is stirred and evenly mixed with curing agent, it is spare；
C, the resin matrix prepared in modification tiny balloon and step b prepared by step a is stirred evenly, obtain tiny balloon/ Thermosetting resin, it is spare；
D, foaming agent, maleic anhydride inoculated polypropylene and thermoplastic resin matrix are stirred and evenly mixed, obtains mixed resin, it is spare；
E, mixed resin prepared by step d is uniformly mixed with tiny balloon/thermosetting resin prepared by step c, is mixed Prefabricated material, it is spare；
F, the prefabricated material of mixing prepared by step e is put into the hopper of extruder or injection molding machine, prepares forming material or sheet material；
G, the step f profile prepared or sheet material are heated, solidifies the thermosetting resin in material sufficiently to get novel heat is arrived Gu/thermoplastic copoly type composite foam.
2. a kind of preparation method of thermosetting/thermoplastic copoly type composite foam as described in claim 1, it is characterised in that: the sky Heart microballoon is glass microsphere, polymer microballoon, ceramic microsphere, carbosphere or metallic microspheres, and tiny balloon is using baking using preceding Equipment removes wherein remaining moisture.
3. a kind of preparation method of thermosetting/thermoplastic copoly type composite foam as described in claim 1, it is characterised in that: the heat Thermosetting resin matrix is epoxy resin, alkenyl esters resin, phenolic resin, unsaturated polyester resin or polyimide resin.
4. a kind of preparation method of thermosetting/thermoplastic copoly type composite foam as described in claim 1, it is characterised in that: the heat Plastic resin is acrylic resin, nylon, polyethylene, polyester, polyamide, polyformaldehyde or their copolymer.
5. a kind of preparation method of thermosetting/thermoplastic copoly type composite foam as described in claim 1, it is characterised in that: the hair Infusion is swellable polymer microballoon, azodicarbonamide or hydrocarbon blowing agents.
6. a kind of preparation method of thermosetting/thermoplastic copoly type composite foam as described in claim 1, it is characterised in that: in step a The ratio between additional amount of tiny balloon and coupling agent is 100:0.1-10, the addition of thermosetting resin matrix and curing agent in step b The ratio between amount is 100:10-150, and the ratio between modified tiny balloon and the additional amount of resin matrix are 100:80-150, step in step c The ratio between additional amount of foaming agent, thermoplastic resin matrix, maleic anhydride inoculated polypropylene is 0.1-10:30-60:5-20, step in d The ratio between mixed resin and tiny balloon/thermosetting resin additional amount are 100:50-100 in rapid e.
7. a kind of preparation method of thermosetting/thermoplastic copoly type composite foam as described in claim 1, it is characterised in that: the step The temperature of forming process setting is 190 DEG C in rapid f, foam is put into drying chamber in step e or after baking oven is heated to 120 DEG C of heat preservation 3h It is gradually cooled to room temperature, heating and cooling rate are controlled in 1 DEG C/min.
8. a kind of thermosetting/thermoplastic copoly type composite foam, it is characterised in that: composite foam is any described multiple by claim 1-7 The preparation method for closing foam is made.
9. a kind of thermosetting/thermoplastic copoly type composite foam is preparing the application in sandwich structure composite material.
10. thermosetting as claimed in claim 9/thermoplastic copoly type composite foam is preparing answering in sandwich structure composite material With, it is characterised in that: dacron fabric, carbon fiber/epoxy resin prepreg and composite foam are taken, according to carbon fiber/epoxy Resin prepreg material-dacron fabric-composite foam-dacron fabric-carbon fiber/epoxy resin prepreg sequence is laid with Together, under the pressure of 1.0MPa, 150 DEG C of heat preservation 20min are warming up to, naturally cool to 50 DEG C, are taken out to get sandwich is arrived Structural composite material.
CN201910414817.6A 2019-05-17 2019-05-17 A kind of thermosetting/thermoplastic copoly type composite foam and its preparation method and application Pending CN110105665A (en)

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