CN1718632A - Hollow microbead reinforced epoxy resin composite material and its preparation method - Google Patents
Hollow microbead reinforced epoxy resin composite material and its preparation method Download PDFInfo
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- CN1718632A CN1718632A CN 200510019168 CN200510019168A CN1718632A CN 1718632 A CN1718632 A CN 1718632A CN 200510019168 CN200510019168 CN 200510019168 CN 200510019168 A CN200510019168 A CN 200510019168A CN 1718632 A CN1718632 A CN 1718632A
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Abstract
A hollow microbead reinforced epoxy resin material with high strength, low density and low hydroscopicity is proportionally prepared from epoxy resin, solidifying agent diluent, coupling agent and hollow microbeads through screening and pretreating hollow microbeads, proportional mixing, pregelatinizing, and microwave solidifying.
Description
Technical field
The present invention relates to material field, particularly a kind of hollow microbead reinforced epoxy resin composite material and preparation method thereof.
Background technology
Resins, epoxy is a kind of composite resin matrix of high comprehensive performance.Advantage such as cenosphere has that density is low, compressive strength is high, resistivity is high, heat-conduction coefficient and Thermal Contraction Coefficient are little is that other light filler is incomparable.Hollow microbead reinforced epoxy resin composite material has low density, high-intensity characteristics because of it, and more and more be subject to people's attention, and be widely used in fields such as machinery, light industry, aerospace, boats and ships, building, particularly it has become the important component part of the modern deep diving technology of development as a kind of solid buoyancy material.China has progressively carried out the research work of this respect in recent years, has obtained certain achievement.But because the selecting for use and problem such as preparation technology of raw material, though prepared matrix material ultimate compression strength higher (26MPa～79MPa), the still higher (0.67g/cm of its density
3～0.9g/cm
3).And matrix material exist density distribution inhomogeneous, under high hydraulic pressure the water-intake rate problem of higher, be further improved.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of hollow microbead reinforced epoxy resin composite material and preparation method thereof, so that solve the problem of the higher and quality inequality of existing hollow glass micropearl reinforced epoxy composite density.This composite material by adopting is beneficial to the first pre-gelled of suitability for industrialized production, the technology of back microwave curing makes the resulting product excellent property.
The technical solution adopted for the present invention to solve the technical problems is as follows:
Hollow glass micropearl reinforced epoxy matrix material provided by the invention, count by weight, its component comprises: 60～130 parts of 100 parts of Resins, epoxy, 8～100 parts in solidifying agent, 10～35 parts of thinners, 6～13 parts of coupling agents and strongtheners, strongthener is a cenosphere.
The preparation process of hollow microbead reinforced epoxy resin composite material provided by the invention is:
(1) screening of cenosphere and pre-treatment:
Earlier with sieve with microballon dusting cover one time, then the microballon that will sieve sprinkles skim on the water surface, and uses ultrasonic dispersing, collection buoyant microballon is dried; The aqueous solution with coupling agent carries out pre-treatment, dry for standby then.
(2) pre-gelled of matrix material:
Elder generation is mixed in proportion cenosphere, Resins, epoxy, thinner, solidifying agent, stirs, and waters to cast from the mould; Again it after 5～15 minutes, is warming up to 70 ℃～100 ℃ in the vacuum drying oven vacuumizing and defoaming, and constant temperature kept 50～120 minutes, make gel complex material.
Count above-mentioned the ratio of each component is by weight: 100 parts of Resins, epoxy, 8～100 parts in solidifying agent, 10～35 parts of thinners, 6～13 parts of coupling agents, strongthener are 60～130 parts of cenospheres.
(3) the microwave after fixing of matrix material:
Place microwave field to be heating and curing gel complex material, treat the demoulding after the completely solidified, make hollow microbead reinforced epoxy resin composite material.
The present invention compared with prior art has following major advantage:
One. the Resins, epoxy that the present invention adopts is a kind of medium and high temperature epoxy resin solidifying system, can bring into play the performance of each component after compound to greatest extent with cenosphere, prepared composite materials property excellence, for example intensity height (14MPa～74MPa), the low (0.45g/cm of density
3～0.78g/cm
3) and controlled, water-intake rate is low.
They are two years old. and the preparation technology of first pre-gelled provided by the invention, back microwave curing can effectively control solidification process, the pre-gelled process of resin, and resin can not produce local implode phenomenon after preliminary crosslinked.
They are three years old. because the microwave later stage solidifies, are heated simultaneously inside and outside the matrix material, so homogeneous heating, composite material solidification is complete, and rate of expansion is identical on all directions, and gained matrix material quality is even.
They are four years old. and preparation method's technology provided by the invention is simple, and operation easily can be used the serialization of tunnel type micro wave equipment to produce, thereby be beneficial to suitability for industrialized production.
They are five years old. and have wide prospect in industrial application, this matrix material can be widely used in fields such as machinery, light industry, aerospace, boats and ships, building.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
Several Resins, epoxy intermediate temperature setting systems that the present invention is preferred, and be strongthener with the cenosphere adopt the preparation technology of pre-gelled-microwave curing to prepare the matrix material of a kind of high strength, low-density hollow microbead reinforced epoxy resin.Experiment shows, this composite material strength height, and density is lower than existing same type of material, and water-intake rate is low, is suitable as a kind of low density structures material fully and uses.
The invention will be further described below in conjunction with embodiment.
One. hollow microbead reinforced epoxy resin composite material
1. the component of hollow microbead reinforced epoxy resin composite material
Meter by weight, the component of this matrix material comprises: 60～130 parts of 100 parts of Resins, epoxy, 8～100 parts in solidifying agent, 10～35 parts of thinners, 6～13 parts of coupling agents and strongtheners, strongthener is a cenosphere.
Above-mentioned strongthener can adopt any in hollow glass micropearl, hollow ceramic microspheres, the hollow plastics microballon, or more than one mixtures.
Above-mentioned Resins, epoxy can adopt any among E-44, E-51, E-39D, CYD-127, CYD-128, CYD-144, F-54, the F-51, or more than one mixtures.
Above-mentioned curing agent for epoxy resin can adopt: MPDA (mphenylenediamine), 590 (mphenylenediamine derivative), LHB-236 (arylamine), LHB-238 (aromatic amine), LHY-906 (isomerized methyltetrahydro phthalic anhydride), LHY-908 (isomerized methyltetrahydro phthalic anhydride), LHY-918 (isomerized methyltetrahydro phthalic anhydride), LHY-807 (methyl hexahydrophthalic anhydride), THPA (Tetra Hydro Phthalic Anhydride), methylimidazole (EMI-2), 2-ethyl-4-methylimidazole (EMI-2,4), in the trimellitic acid 1,2-anhydride (TMA) any, or more than one compounds.
Above-mentioned thinner can adopt: polypropylene glycol diglycidyl ether, neopentylglycol diglycidyl ether, β-Jia Jihuanyanglvbingwan (MECH), glycidyl ether, ethylene glycol diglycidylether, lauryl diglycidyl ether, epoxy propane butyl ether (BGE), titanium dioxide vinyl cyclohexane (Unox206) and 3,4 epoxycyclohexyl formic acid-3, in the 4-epoxycyclohexyl manthanoate (Unox221) any, or more than one compounds.
Above-mentioned coupling agent can adopt any among KH-550 (γ-An Bingjisanyiyangjiguiwan), KH-560 (3-glycidyl ether oxygen propyl trimethoxy silicane), KH-570 (methacryloxypropyl trimethoxy silane), WD-50 (γ-An Bingjisanyiyangjiguiwan), WD-60 (γ-[(2,3) epoxy third oxygen] propyl trimethoxy silicane), the WD-70 (γ-(methacryloxypropyl) propyl trimethoxy silicane).
2. specific examples:
Example one. count by weight, each component prescription of hollow microbead reinforced epoxy resin composite material is as follows:
100 parts of CYD-127,35 parts of LHB-236,10 parts of epoxy propane butyl ethers, 7 parts of KH-550,70 parts of hollow glass micropearls.
Example two. count by weight, each component prescription of hollow microbead reinforced epoxy resin composite material is as follows:
100 parts of CYD-128,38 parts of LHB-238,15 parts of epoxy propane butyl ethers, 9 parts of KH-550,90 parts of hollow glass micropearls.
Example three. count by weight, each component prescription of hollow microbead reinforced epoxy resin composite material is as follows:
100 parts of E-44,10 parts of 2-ethyl-4-methylimidazoles, 10 parts of 15 parts of epoxy propane butyl ethers and ethylene glycol diglycidylethers, 11 parts of KH-560,110 parts of hollow ceramic microspheres.
Example four. count by weight, each component prescription of hollow microbead reinforced epoxy resin composite material is as follows:
100 parts of F-51,12 parts of 2-ethyl-4-methylimidazoles, 15 parts of 20 parts of epoxy propane butyl ethers and neopentylglycol diglycidyl ethers, 13 parts of KH-560,130 parts of hollow glass micropearls.
Example five. count by weight, each component prescription of hollow microbead reinforced epoxy resin composite material is as follows:
100 parts of CYD-144,50 parts of LHY-906,10 parts of 10 parts of titanium dioxide vinyl cyclohexane and ethylene glycol diglycidylethers, 10 parts of KH-560,100 parts of hollow plastics microballons.
Two. the preparation of hollow microbead reinforced epoxy resin composite material
1. preparation
As shown in drawings, its preparation process comprises the screening of cenosphere and pre-treatment, the pre-gelled of matrix material and the microwave after fixing of matrix material, and is specific as follows:
(1) screening of cenosphere and pre-treatment
Earlier with sieve with microballon dusting cover one time, then the microballon that will sieve sprinkles skim on the water surface, and uses ultrasonic dispersing, collection buoyant microballon is dried; The aqueous solution with coupling agent carries out pre-treatment, dry for standby then.
(2) pre-gelled of matrix material
Set of dispense ratio by above-mentioned hollow microbead reinforced epoxy resin composite material mixes cenosphere, Resins, epoxy, thinner, solidifying agent earlier, stirs, and waters to cast from the mould; Again it after 5～15 minutes, is warming up to 70 ℃～100 ℃ in the vacuum drying oven vacuumizing and defoaming, and constant temperature kept 50～120 minutes, make gel complex material.
(3) the microwave after fixing of matrix material
Place microwave field to be heating and curing gel complex material, treat the demoulding after the completely solidified, make hollow microbead reinforced epoxy resin composite material.This performance of composites index can be referring to subordinate list.
2. the specific examples for preparing hollow glass micropearl reinforced epoxy matrix material
Example one.
With reference to the accompanying drawings, produce according to the following step:
(1) screening of hollow glass micropearl and pre-treatment:
Hollow glass micropearl is the smooth surface Ball-type packing, and grandson crack rate is low, and it is few that the pearl body is inhaled resin, can disperse preferably in polymeric matrix.For removing damaged glass microballon, get earlier a certain amount of hollow glass micropearl with sieve with microballon dusting cover one time, then the microballon that will sieve sprinkles skim on the water surface, and vibrates with ultrasonic dispersing, collection buoyant microballon takes by weighing 90g after the oven dry.In 1: 1 ratio (weight ratio) 9g KH-550 coupling agent is made into the aqueous solution, stirs.Solution is splashed in the hollow glass micropearl after the oven dry, stirred 40--60 minute, make treatment agent fully coat microballon.Microballon after will handling is then put in people's baking oven, and oven temperature remains on 80 ℃, and constant temperature is after 3 hours, and taking-up is put in people's sealed vessel standby.In the silane coupling agent-OC
2H
5After the hydrolysis can with the main component SiO of glass microballon
2By the combination of secondary valence bond power, and then the affinity between increase Resins, epoxy and the microballon, the mechanical property of matrix material is improved greatly.
(2) pre-gelled of matrix material:
Take by weighing CYD-127 Resins, epoxy 100g, the hollow glass micropearl 90g after the processing, epoxy propane butyl ether 10g, LHB-236 solidifying agent 35g mix, and mechanical stirring 10 minutes is watered and is cast from the mould.After 10 minutes, be warming up to 90 ℃ in the vacuum drying oven vacuumizing and defoaming, and constant temperature 50 minutes.
(3) the microwave after fixing of matrix material:
After 50 minutes, it is the 800W microwave field that jello is placed the microwave mean power, and type of heating is adjusted to intermittent type, heats and treats the demoulding after the completely solidified in 6 minutes.
Example two.
Press following proportioning weighing: E-44 Resins, epoxy 100g, the hollow glass micropearl 120g after the processing, epoxy propane butyl ether 15g, ethylene glycol diglycidylether 10g, 2-ethyl-4-methylimidazole 12g, its preparation method are substantially with example 1.The pre-gelled temperature is 80 ℃, and soaking time is 80 minutes, and microwave curing adopts the mode of intermittent type heating, 20 minutes heat-up times.
Example three.
Press following proportioning weighing: CYD-128 Resins, epoxy 100g, the hollow ceramic microspheres 120g after the processing, neopentylglycol diglycidyl ether 28g, LHY-908 solidifying agent 85g, its preparation method are substantially with example 1.The pre-gelled temperature is 100 ℃, and soaking time is 120 minutes, and microwave curing adopts the mode of intermittent type heating, 16 minutes heat-up times.
Example four.
Press following proportioning weighing: F-51 Resins, epoxy 100g, hollow plastics microballon 100g, epoxy propane butyl ether 10g, titanium dioxide vinyl cyclohexane 10g, LHB-236 solidifying agent 40g, its preparation method are substantially with example 1, but the plastics microballon does not need pre-treatment.The pre-gelled temperature is 70 ℃, and soaking time is 60 minutes, and microwave curing adopts the mode of intermittent type heating, 8 minutes heat-up times.
Prepared hollow plastics microballon reinforced epoxy matrix material in above-mentioned four examples, its fundamental property is asked for an interview following subordinate list.
The hollow plastics microballon of subordinate list reinforced epoxy performance of composites index
Claims (8)
1. a hollow microbead reinforced epoxy resin composite material is characterized in that counting by weight, comprises following component:
100 parts of Resins, epoxy
8～100 parts in solidifying agent
10～35 parts of thinners
6～13 parts of coupling agents
60～130 parts of strongtheners
Above-mentioned strongthener is a cenosphere.
2. hollow microbead reinforced epoxy resin composite material according to claim 1 is characterized in that cenosphere is any in hollow glass micropearl, hollow ceramic microspheres, the hollow plastics microballon, or more than one mixtures.
3. hollow microbead reinforced epoxy resin composite material according to claim 1 is characterized in that Resins, epoxy adopts: any among E-44, E-51, E-39D, CYD-127, CYD-128, CYD-144, F-54, the F-51, or more than one mixtures.
4. hollow microbead reinforced epoxy resin composite material according to claim 1, it is characterized in that epoxy curing agent adopts: any in mphenylenediamine, mphenylenediamine derivative, arylamine, aromatic amine, isomerized methyltetrahydro phthalic anhydride, isomerized methyltetrahydro phthalic anhydride, isomerized methyltetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride, Tetra Hydro Phthalic Anhydride, methylimidazole, 2-ethyl-4-methylimidazole, the trimellitic acid 1,2-anhydride, or more than one compounds.
5. hollow microbead reinforced epoxy resin composite material according to claim 1, it is characterized in that thinner adopts: polypropylene glycol diglycidyl ether, neopentylglycol diglycidyl ether, β-Jia Jihuanyanglvbingwan, glycidyl ether, ethylene glycol diglycidylether, lauryl diglycidyl ether, epoxy propane butyl ether, titanium dioxide vinyl cyclohexane and 3,4 epoxycyclohexyl formic acid-3, in the 4-epoxycyclohexyl manthanoate any, or more than one compounds.
6. hollow microbead reinforced epoxy resin composite material according to claim 1, it is characterized in that coupling agent adopts: any in γ-An Bingjisanyiyangjiguiwan, 3-glycidyl ether oxygen propyl trimethoxy silicane, methacryloxypropyl trimethoxy silane, γ-An Bingjisanyiyangjiguiwan, γ-[(2,3)-epoxy third oxygen] propyl trimethoxy silicane and γ-(methacryloxypropyl) propyl trimethoxy silicane.
7. the preparation method of a hollow microbead reinforced epoxy resin composite material is characterized in that comprising screening and pre-treatment, the pre-gelled of matrix material and the microwave after fixing preparation process of matrix material to cenosphere, and is specific as follows:
(1) screening of cenosphere and pre-treatment
Earlier with sieve with microballon dusting cover one time, then the microballon that will sieve sprinkles skim on the water surface, and uses ultrasonic dispersing, collection buoyant microballon is dried; The aqueous solution with coupling agent carries out pre-treatment then, dry for standby,
(2) pre-gelled of matrix material
Elder generation is mixed in proportion cenosphere, Resins, epoxy, thinner, solidifying agent, stirs, and waters to cast from the mould; Again with it in the vacuum drying oven vacuumizing and defoaming after 5～15 minutes, be warming up to 70 ℃～100 ℃, and constant temperature kept 50～120 minutes, made gel complex material, by weight meter, above-mentioned the ratio of each component is: 100 parts of Resins, epoxy, 8～100 parts in solidifying agent, 10～35 parts of thinners, 6～13 parts of coupling agents, strongthener is 60～130 parts of cenospheres
(3) the microwave after fixing of matrix material
Place microwave field to be heating and curing gel complex material, treat the demoulding after the completely solidified, make hollow microbead reinforced epoxy resin composite material.
8. the preparation method of hollow microbead reinforced epoxy resin composite material according to claim 7 is characterized in that prepared hollow microbead reinforced epoxy resin composite material, and its intensity is 14～74MPa, and density is 0.45～0.78g/cm
3
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