CN105034407A - Preparation method for bicontinuous resin-based cenosphere composite foamed material - Google Patents
Preparation method for bicontinuous resin-based cenosphere composite foamed material Download PDFInfo
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- CN105034407A CN105034407A CN201510594429.2A CN201510594429A CN105034407A CN 105034407 A CN105034407 A CN 105034407A CN 201510594429 A CN201510594429 A CN 201510594429A CN 105034407 A CN105034407 A CN 105034407A
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- cenosphere
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention relates to a preparation method for a resin-based composite foamed material, in particular to a preparation method for a bicontinuous resin-based cenosphere composite foamed material, and aims to solve the technical problems that in an existing resin-based composite foamed material, the solid content of cenospheres is low, the cenospheres are layered and uneven in structure, and escaping of pores is hard. The preparation method comprises the steps that 1, a cenosphere prefabricated body is prepared; 2, resin permeates into the cenosphere prefabricated body and is cured. The preparation method has the advantages that the resin-based cenosphere composite foamed material is light, high in strength and high in modulus, the cenospheres are even in distribution and are closely stacked, and the cenospheres and a resin matrix are of a bicontinuous structure; the compressive strength of the resin-based cenosphere composite foamed material is larger than 90.2%, and the modulus of compression of the resin-based cenosphere composite foamed material is larger than 3.7 GPa; the solid content of the cenospheres in the resin-based cenosphere composite foamed material is about 65%, the preparation process is simple, and high operability is achieved.
Description
Technical field
The present invention relates to a kind of preparation method of co-continuous resin-based composite foam material.
Background technology
Resin-based composite foam material has low-density, excellent compressive property, high specific strength, and the feature such as low water absorption rate, good thermal expansion and thermal conductivity factor, thus is more and more subject to people's attention.Composite foam material can be used for the buoyant material of deep-sea detection equipment, the weight-reducing material of Aeronautics and Astronautics and transport facility; The rudder of fighter plane, tail fairing, the engine of warship and submarine, the protective cover material of drive mechanism; Crashproof in transport facility, protecting against shock component, the sandwich material in multiply-plywood structure; Torpedo power system shell sound-absorbing material, the acoustic material in industrial or agricultural, transportation, building industry and insulation material etc.At present, China has carried out correlative study for many years in this field, achieves certain achievement, but due to problems such as preparation technologies, although the resin-based composite foam material compressive strength higher (68.5MPa) of gained, the higher (0.74gcm of density
-3), modulus of compressibility is up to 1.287GPa, Li Huijian, He Changjun, Liang Xi, Jia Yingguo. hollow glass micropearl filling epoxy resin composite materials property. composite journal, 2010,27 (4): 189-194.) problem that, composite foam material exists skewness, inside exists a large amount of defects etc.At present, the conventional method preparing resin-based Hollow Microspheres Reinforced Composite Materials is casting, utilize casting to prepare in the forming process of composite foam material and there is following problem: one, the density of cenosphere is generally lower than resin matrix, solidification process hollow core microballon floats, easily occur lamination, the uniformity of composite foam material is difficult to ensure; Two, cenosphere shear strength is low, and during stirring, stir speed (S.S.) is restricted; Three, cenosphere content is lower, and general volume fraction is 30% ~ 50%, and cenosphere solid concentration is difficult to improve; Four, when cenosphere solid concentration is higher, resin and cenosphere mixture viscosity are comparatively large, and the bubble of resin inside is difficult to removing, and after resin solidification, material internal exists a large amount of defect.
Summary of the invention
The present invention is that current resin-based composite foam material hollow core microballon solid concentration is low in order to solve, layering, uneven microstructure and pore are difficult to the technical problem of overflowing, and provides a kind of preparation method of co-continuous resin-based cenosphere composite foam material.
The preparation method of a kind of co-continuous resin-based cenosphere composite foam material of the present invention carries out according to the following steps:
One, prepare cenosphere precast body: by after cenosphere and binding agent Homogeneous phase mixing under pressure is the condition of 0.1MPa ~ 1MPa compression molding to make a living base, then in muffle furnace with the heating rate of 0.5 DEG C/min ~ 2 DEG C/min from room temperature to 250 DEG C, be be incubated 1h ~ 2h under the condition of 250 DEG C in temperature, be 250 DEG C from temperature to continue to be warming up to 650 DEG C, be be incubated 1h ~ 2h under the condition of 650 DEG C in temperature, be 650 DEG C with the heating rate of 2.5 DEG C/min from temperature and be warming up to 700 DEG C, be be incubated 2h under the condition of 700 DEG C in temperature, cool to room temperature with the furnace, obtain cenosphere precast body, described binding agent and the mass ratio of cenosphere are 1:(20 ~ 100),
Two, resin infiltrates cenosphere precast body and solidifies: in mould, be coated with one deck releasing agent, cenosphere precast body step one obtained puts into mould, resin matrix is put into mould and on cenosphere precast body, in take the method for vacuum impregnation or pressure impregnation to be infiltrated by resin matrix cenosphere precast body that step one obtains, then solidify, retreat most mould, obtain co-continuous resin-based cenosphere composite foam material; The cenosphere precast body that described step one obtains and the mass ratio of resin matrix are 1:(1.22 ~ 1.67); The curing process that described solidification takes resin matrix self intrinsic carries out.
The present invention adopts binding agent bonding cenosphere, through mold pressing, binder removal, sintering process prepares cenosphere precast body, co-continuous resin-based cenosphere composite foam material is prepared by the method for vacuum impregnation or pressure impregnation, compared with the composite obtained with casting, the inventive method can be prepared cenosphere and be evenly distributed, and cenosphere and resin have bicontinuous structure, the composite foam material of excellent performance.
Advantage of the present invention:
One, the co-continuous resin-based cenosphere composite foam material prepared of the inventive method, resin and cenosphere have bicontinuous structure, and cenosphere is evenly distributed and tightly packed, and composite has the features such as lightweight, high-strength, high-modulus.Aeronautics and Astronautics weight-reducing material, ocean deep diving buoyant material, heat-insulating material etc. can be widely used in;
Two, the density adopting Archimedes's drainage to record cenosphere precast body prepared by the present invention is 0.2583gcm
-3~ 0.8030gcm
-3, open pore rate is less than 40%, and wherein cenosphere volume content is greater than 60%, and the compression strength of cenosphere precast body is 5.6MPa;
Three, the density of co-continuous resin-based cenosphere composite foam material that prepared by the present invention is 0.6121gcm
-3, compression strength > 90.2MPa, modulus of compressibility > 3.7GPa;
Four, the co-continuous resin-based cenosphere composite foam material hollow core microballon solid concentration prepared of the present invention is higher, can reach about 65%, and preparation technology is simple, workable.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the co-continuous resin-based cenosphere composite foam material that test two obtains;
Fig. 2 is the SEM figure of the co-continuous resin-based cenosphere composite foam material that test two obtains;
Fig. 3 is the SEM figure of the co-continuous resin-based cenosphere composite foam material that test two obtains, and in Fig. 3, arrow 1 indication is cenosphere wall, and arrow 2 indication is interface, and arrow 3 indication is resin matrix.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of preparation method of co-continuous resin-based cenosphere composite foam material, specifically carries out according to the following steps:
One, prepare cenosphere precast body: by after cenosphere and binding agent Homogeneous phase mixing under pressure is the condition of 0.1MPa ~ 1MPa compression molding to make a living base, then in muffle furnace with the heating rate of 0.5 DEG C/min ~ 2 DEG C/min from room temperature to 250 DEG C, be be incubated 1h ~ 2h under the condition of 250 DEG C in temperature, be 250 DEG C from temperature to continue to be warming up to 650 DEG C, be be incubated 1h ~ 2h under the condition of 650 DEG C in temperature, be 650 DEG C with the heating rate of 2.5 DEG C/min from temperature and be warming up to 700 DEG C, be be incubated 2h under the condition of 700 DEG C in temperature, cool to room temperature with the furnace, obtain cenosphere precast body, described binding agent and the mass ratio of cenosphere are 1:(20 ~ 100),
Two, resin infiltrates cenosphere precast body and solidifies: in mould, be coated with one deck releasing agent, cenosphere precast body step one obtained puts into mould, resin matrix is put into mould and on cenosphere precast body, in take the method for vacuum impregnation or pressure impregnation to be infiltrated by resin matrix cenosphere precast body that step one obtains, then solidify, retreat most mould, obtain co-continuous resin-based cenosphere composite foam material; The cenosphere precast body that described step one obtains and the mass ratio of resin matrix are 1:(1.22 ~ 1.67); The curing process that described solidification takes resin matrix self intrinsic carries out.
Detailed description of the invention two: the difference of present embodiment and detailed description of the invention one is: the cenosphere described in step one is hollow plastic microbead, hollow glass micropearl or hollow ceramic microspheres.Other are identical with detailed description of the invention one.
Detailed description of the invention three: the difference of present embodiment and detailed description of the invention one or two is: the particle diameter of the cenosphere described in step one is 1 μm ~ 5mm.Other are identical with detailed description of the invention one or two.
Detailed description of the invention four: the difference of present embodiment and detailed description of the invention one to three is: the binding agent described in step one to be mass fraction be 40% ~ 60% polyvinyl alcohol water solution, phosphate or organic siliconresin.Other are identical with detailed description of the invention one to three.
Detailed description of the invention five: the difference of present embodiment and detailed description of the invention one to four is: the releasing agent described in step 2 is dimethicone.Other are identical with detailed description of the invention one to four.
Detailed description of the invention six: the difference of present embodiment and detailed description of the invention one to five is: the cenosphere precast body that the step one described in step 2 obtains and the mass ratio of resin matrix are 1:1.22.Other are identical with detailed description of the invention one to five.
Detailed description of the invention seven: the difference of present embodiment and detailed description of the invention one to six is: the concrete grammar in take vacuum-impregnated method to be infiltrated by the resin matrix cenosphere precast body that step one obtains described in step 2 is: be 10 in vacuum by the mould that resin matrix and cenosphere precast body be housed
-1pa and temperature are be incubated 1h ~ 2h in the vacuum drying oven of 130 DEG C ~ 170 DEG C.Other are identical with detailed description of the invention one to six.
Detailed description of the invention eight: the difference of present embodiment and detailed description of the invention one to seven is: the concrete grammar in take the method for pressure impregnation to be infiltrated by the resin matrix cenosphere precast body that step one obtains described in step 2 is: be pressurize 1h ~ 2h under the condition of room temperature ~ 250 DEG C at pressure 0.5MPa ~ 1MPa and temperature by the mould that resin matrix and cenosphere precast body be housed.Other are identical with detailed description of the invention one to seven.
Detailed description of the invention nine: the difference of present embodiment and detailed description of the invention one to eight is: the resin matrix described in step 2 is epoxy resin, phenolic resins, cyanate ester resin or polyimide resin.Other are identical with detailed description of the invention one to eight.
Detailed description of the invention ten: present embodiment and detailed description of the invention four difference are: phosphate is aluminium dihydrogen phosphate or aluminum phosphate.Other are identical with detailed description of the invention four.
By following verification experimental verification beneficial effect of the present invention:
Test one: this test is a kind of preparation method of co-continuous resin-based cenosphere composite foam material, specifically carries out according to the following steps:
One, prepare cenosphere precast body: by after cenosphere and binding agent Homogeneous phase mixing under pressure is the condition of 0.5MPa compression molding to make a living base, then in muffle furnace with the heating rate of 0.5 DEG C/min from room temperature to 250 DEG C, be be incubated 1h under the condition of 250 DEG C in temperature, be 250 DEG C from temperature to continue to be warming up to 650 DEG C, be be incubated 2h under the condition of 650 DEG C in temperature, 700 DEG C are warming up to the heating rate of 2.5 DEG C/min, be be incubated 2h under the condition of 700 DEG C in temperature, cool to room temperature with the furnace, obtain cenosphere precast body; Described binding agent and the mass ratio of cenosphere are 1:100;
Two, resin infiltrates cenosphere precast body and solidifies: in mould, be coated with one deck releasing agent, cenosphere precast body step one obtained puts into mould, resin matrix is put into mould and on cenosphere precast body, in take the method for pressure impregnation to be infiltrated by resin matrix cenosphere precast body that step one obtains, solidification, retreat most mould, obtain co-continuous resin-based cenosphere composite foam material; The cenosphere precast body that described step one obtains and the mass ratio of resin matrix are 1:1.22.
Cenosphere described in step one is hollow glass micropearl, and bulk density is 0.26gcm
-3, real density is 0.40gcm
-3, compression strength is 28MPa, and median is d
50=55 μm; Binding agent described in step one to be mass fraction be 50% polyvinyl alcohol; Releasing agent described in step 2 is dimethicone;
Concrete grammar in take the method for pressure impregnation to be infiltrated by resin matrix cenosphere precast body that step one obtains described in step 2 is: mould pressurize 1h under pressure 0.5MPa and temperature are the condition of room temperature of resin matrix and cenosphere precast body will be housed;
Resin matrix described in step 2 is add butyl glycidyl ether after epoxy resin E51 mixes according to the mass ratio of 4:1 with curing agent (593), and stir 10min and obtain, the mass ratio of butyl glycidyl ether and epoxy resin E51 is 1:10; Solidification temperature is 50 DEG C, insulation 5h.
The density recording cenosphere precast body prepared by this test procedure one through Archimedes's drainage is 0.2787gcm
-3, open pore rate is 36.17%.
The density being recorded the resin-based cenosphere composite foam material of this test preparation by Archimedes's drainage is 0.61gcm
-3.
Test two: this test is a kind of preparation method of co-continuous resin-based cenosphere composite foam material, specifically carries out according to the following steps:
One, prepare cenosphere precast body: by after cenosphere and binding agent Homogeneous phase mixing under pressure is the condition of 0.5MPa compression molding to make a living base, then in muffle furnace with the heating rate of 0.5 DEG C/min from room temperature to 250 DEG C, be be incubated 1h under the condition of 250 DEG C in temperature, be 250 DEG C from temperature to continue to be warming up to 650 DEG C, be be incubated 2h under the condition of 650 DEG C in temperature, 700 DEG C are warming up to the heating rate of 2.5 DEG C/min, be be incubated 2h under the condition of 700 DEG C in temperature, cool to room temperature with the furnace, obtain cenosphere precast body; Described binding agent and the mass ratio of cenosphere are 1:100;
Two, resin infiltrates cenosphere precast body and solidifies: in mould, be coated with one deck releasing agent, cenosphere precast body step one obtained puts into mould, resin matrix is put into mould and on cenosphere precast body, in take vacuum-impregnated method to be infiltrated by resin matrix cenosphere precast body that step one obtains, solidification, retreat most mould, obtain co-continuous resin-based cenosphere composite foam material; The cenosphere precast body that described step one obtains and the mass ratio of resin matrix are 1:1.22.
Cenosphere described in step one is hollow glass micropearl, and bulk density is 0.26gcm
-3, real density is 0.40gcm
-3, compression strength is 28MPa, and median is d
50=55 μm; Binding agent described in step one to be mass fraction be 50% polyvinyl alcohol; Releasing agent described in step 2 is dimethicone;
Concrete grammar in take vacuum-impregnated method to be infiltrated by resin matrix cenosphere precast body that step one obtains described in step 2 for: the concrete grammar in take vacuum-impregnated method to be infiltrated by the resin matrix cenosphere precast body that step one obtains described in step 2 is: be 10 by the mould that resin matrix and cenosphere precast body be housed in vacuum
-1pa and temperature are be incubated 2h in the vacuum drying oven of 160 DEG C;
Resin matrix described in step 2 is cyanate ester resin; Curing process is that solidification temperature is 180 DEG C in earlier stage, insulation 2h, and cured later temperature is 240 DEG C, insulation 6h.
The density recording cenosphere precast body prepared by this test procedure one through Archimedes's drainage is 0.2787gcm
-3, open pore rate is 36.17%.
The density recording resin-based cenosphere composite foam material prepared by test two through Archimedes's drainage is 0.6121gcm
-3.Compression strength is 90.2MPa, and modulus of compressibility is 3.7GPa.
Fig. 1,2 and 3 is the SEM figure of the resin-based cenosphere composite foam material that test two obtains, and as can be seen from Figure 1 after compression molding, cenosphere is without fragmentation, and integrity degree is good, and after binder removal, sintering, cenosphere is without subsiding; As can be seen from Figure 2 after sintering, cenosphere and cenosphere contact position produce constriction (arrow indication), are connected to each other, and in co-continuous, this structure contributes to the mechanical property improving composite foam material; In Fig. 3,1 is cenosphere wall, and 2 is interface, and 3 is resin matrix, and as can be seen from Figure 3 after pressure impregnation resin, well, without cracking, in resin, pore-free exists for resin and cenosphere interface cohesion.
Claims (10)
1. a preparation method for co-continuous resin-based cenosphere composite foam material, is characterized in that the preparation method of co-continuous resin-based cenosphere composite foam material carries out according to the following steps:
One, prepare cenosphere precast body: by after cenosphere and binding agent Homogeneous phase mixing under pressure is the condition of 0.1MPa ~ 1MPa compression molding to make a living base, then in muffle furnace with the heating rate of 0.5 DEG C/min ~ 2 DEG C/min from room temperature to 250 DEG C, be be incubated 1h ~ 2h under the condition of 250 DEG C in temperature, be 250 DEG C from temperature to continue to be warming up to 650 DEG C, be be incubated 1h ~ 2h under the condition of 650 DEG C in temperature, be 650 DEG C with the heating rate of 2.5 DEG C/min from temperature and be warming up to 700 DEG C, be be incubated 2h under the condition of 700 DEG C in temperature, cool to room temperature with the furnace, obtain cenosphere precast body, described binding agent and the mass ratio of cenosphere are 1:(20 ~ 100),
Two, resin infiltrates cenosphere precast body and solidifies: in mould, be coated with one deck releasing agent, cenosphere precast body step one obtained puts into mould, resin matrix is put into mould and on cenosphere precast body, in take the method for vacuum impregnation or pressure impregnation to be infiltrated by resin matrix cenosphere precast body that step one obtains, then solidify, retreat most mould, obtain co-continuous resin-based cenosphere composite foam material; The cenosphere precast body that described step one obtains and the mass ratio of resin matrix are 1:(1.22 ~ 1.67); The curing process that described solidification takes resin matrix self intrinsic carries out.
2. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 1, is characterized in that the cenosphere described in step one is hollow plastic microbead, hollow glass micropearl or hollow ceramic microspheres.
3. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 1, is characterized in that the particle diameter of the cenosphere described in step one is 1 μm ~ 5mm.
4. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 1, the binding agent that it is characterized in that described in step one to be mass fraction be 40% ~ 60% polyvinyl alcohol water solution, phosphate or organic siliconresin.
5. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 1, is characterized in that the releasing agent described in step 2 is dimethicone.
6. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 1, is characterized in that the mass ratio of the cenosphere precast body that the step one described in step 2 obtains and resin matrix is 1:1.22.
7. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 1, is characterized in that the concrete grammar in take vacuum-impregnated method to be infiltrated by the resin matrix cenosphere precast body that step one obtains described in step 2 is: be 10 by the mould that resin matrix and cenosphere precast body be housed in vacuum
-1pa and temperature are be incubated 1h ~ 2h in the vacuum drying oven of 130 DEG C ~ 170 DEG C.
8. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 1, is characterized in that the concrete grammar in take the method for pressure impregnation to be infiltrated by the resin matrix cenosphere precast body that step one obtains described in step 2 is: be pressurize 1h ~ 2h under the condition of room temperature ~ 250 DEG C at pressure 0.5MPa ~ 1MPa and temperature by the mould that resin matrix and cenosphere precast body be housed.
9. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 1, is characterized in that the resin matrix described in step 2 is epoxy resin, phenolic resins, cyanate ester resin or polyimide resin.
10. the preparation method of a kind of co-continuous resin-based cenosphere composite foam material according to claim 4, is characterized in that phosphate is aluminium dihydrogen phosphate or aluminum phosphate.
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| CN107253328A (en) * | 2017-06-21 | 2017-10-17 | 巩义市泛锐熠辉复合材料有限公司 | A kind of preparation method without macroscopic interface density gradation type composite foam |
| CN109251469A (en) * | 2018-08-17 | 2019-01-22 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of rock wool compound insulating material |
| CN109745928A (en) * | 2019-01-28 | 2019-05-14 | 清华大学 | The preparation method and applications of oily microcapsule |
| CN109745928B (en) * | 2019-01-28 | 2021-01-12 | 清华大学 | Preparation method and application of oil-containing microcapsule |
| CN112391052A (en) * | 2020-11-13 | 2021-02-23 | 航天特种材料及工艺技术研究所 | Foam material and preparation method thereof |
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