CN102585442A - Underwater resin matrix light high-strength composite material and preparation method thereof - Google Patents
Underwater resin matrix light high-strength composite material and preparation method thereof Download PDFInfo
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Abstract
Provided are an underwater resin matrix light high-strength composite material and a preparation method thereof. The underwater resin matrix light high-strength composite material comprises the following components by weight: 80 to 100 parts of epoxy resin, 8 to 12 parts of curing agent, 5 to 20 parts of flexibilizer, 0 part to 5 parts of thinning agent, 1 part to 2 parts of coupling agent and 60 to 100 parts of cenosphere. The preparation method includes (1) adding the epoxy resin, the thinning agent and the flexibilizer into a reaction kettle, controlling temperature to be in a range from 60 to 80 DEG C and conducting pre-polymerization reaction for 30min to 60min; (2) adding the curing agent into a prepolymer in the reaction kettle to obtain resin glue solution; (3) conducting surface modification processing on the glass cenosphere through silane coupling agent; (4) adding the resin glue solution and the surface-modified glass cenosphere into a vacuum stirring machine to be mixed; (5) adding the mixed materials in the step4 into a three-roller mixing mill for mixing; (6) placing materials obtained in the step5 into a vacuum drying box for vacuum defoamation; and (7) pouring materials in the step6 into a mould for hot-pressing solidification formation. The underwater resin matrix light high-strength composite material is low in density, high in pressure resistant strength, simple in process and low in cost.
Description
Technical field
The present invention relates to buoyancy material under water, relate in particular to a kind of high-strength light of resin base under water matrix material and preparation method thereof.
Background technology
Since nineteen fifties, along with the fast development of countries in the world economic technology, the quick growth of population, people have become to restrict the key contradiction of human Future Development to the exhaustion day by day of the growing and land resources of the demand of natural resources.In order to alleviate this contradiction, people have turned one's attention to the ocean of taking up an area of the ball total area 70%.The vast oceans; Natural resources is richly stored with; Extensively the distributing oceanic multi-metal nodule of more than 70 kind of elements such as containing manganese, copper, cobalt, nickel, iron of depths, ocean all over the world; Also have richs in natural resources such as cobalt-bearing crust resource, hydrothermal solution sulfide resource, gas hydrate and abyssopelagic organism genetic resources, reality is the deep-sea oil resource the most, and submarine oil and natural gas reserves account for 45% of world's total amount.Yet ocean exploitation is equipped with exploring too busy to get away ocean, and as the universal material of deep-sea equipment, the research of buoyancy material under water more and more receives people's attention.
In recent years, the investigator of many countries has carried out extensive studies work to buoyancy material under water in the world, and at present, the development of advanced solid buoyancy material technology is mainly grasped in national hands such as the U.S., Russia, and its density of material is generally at 0.4-0.7g/cm
3Between, ultimate compression strength can be at 40-80MPa.China last century the mid-80 develop first-generation buoyancy material by Harbin Marine engineering school, its density is 0.55g/cm
3Withstand voltage 6MPa; After 2000, Inst. of Marine Chemical Engineering is developed density 0.55g/cm
3The buoyancy material of withstand voltage 50MPa, but by up to the present, the density of China's independent development is at 0.7g/cm
3Following compressive strength is that the buoyancy material of 80MPa still rarely has report, is the problem that domestic researcher is tried to explore and puted forth effort to solve about the density of deep water buoyancy material and the contradiction of ultimate compression strength all the time with unified relation.
Summary of the invention
Main purpose of the present invention is to overcome the above-mentioned shortcoming that currently available products exists; And a kind of high-strength light of resin base under water matrix material and preparation method thereof is provided; Its material prescription comprises epoxy resin, latent curing agent, toughner, dispersion agent, thinner, hollow glass micropearl and coupling agent; Its preparation method is with the moulding of formula materials hot-press solidifying, make density of material 0.35 to 0.7g/cm
3Between, compressive strength meets the requirement that universal material is equipped at the deep-sea 30 to 80MPa, good quality, and this forming method is lower to equipment requirements, and moulding process is simple, and cost is low.
The objective of the invention is to realize by following technical scheme.
The present invention is resin base high-strength light matrix material under water, it is characterized in that, the ratio of weight and number of its component is: epoxy resin is 80 to 100 parts; Solidifying agent is 8 to 12 parts, and toughner is 5 to 20 parts, and thinner is 0 to 5 part; Coupling agent is 1 to 2 part, and cenosphere is 60 to 100 parts.
The aforesaid high-strength light of resin base under water matrix material, wherein epoxy resin is the mixture of bisphenol A-type and glycidyl ester type epoxy resin, the ratio of weight and number of this mixture is 0: 100 to 100: 0; This bisphenol A type epoxy resin is E51 or E44 type epoxy resin, and this glycidyl ester type epoxy resin is a TDE-85 type epoxy resin.
The aforesaid high-strength light of resin base under water matrix material, wherein solidifying agent is selected amido borine latent curing agent for use, and this amido borine latent curing agent is 2-(β-dimethylamino oxyethyl group)-1,3,6 trioxas-2-boron octane.
The aforesaid high-strength light of resin base under water matrix material, wherein said toughner is liquid nbr carboxyl terminal.
The aforesaid high-strength light of resin base under water matrix material, wherein thinner is single epoxy group(ing) reactive thinner, this list epoxy group(ing) reactive thinner is one or more in propenyl glycidyl ether, butylglycidyl ether, the phenyl glycidyl ether.
The aforesaid high-strength light of resin base under water matrix material, wherein coupling agent is a γ-An Bingjisanyiyangjiguiwan.
The aforesaid high-strength light of resin base under water matrix material, wherein cenosphere is a hollow glass microbead, it is a kind of of 70 μ m to 115 μ m or several that this hollow glass microbead is selected particle diameter for use.
The present invention is the preparation method of resin base high-strength light matrix material under water, it is characterized in that, may further comprise the steps:
(1) in parts by weight; Get mixture or single kind of epoxy resin, 0 to 5 part of thinner, 5 to 20 parts of the toughner of 80 to 100 parts of two kinds of epoxy resin, add in the reaction kettle, the control reactor temperature is at 60 to 80 ℃; Fully stir, prepolymerization reaction 30 is to 60min;
(2) in parts by weight, get 8 to 12 parts of solidifying agent and add in the performed polymer in the reaction kettle, mix, obtain resin adhesive liquid; Solidifying agent is with before performed polymer mixes, and solidifying agent and performed polymer are heated to 60 to 80 ℃ respectively, to improve Resin Flow and consistency;
(3), get 1 to 2 part of silane coupling agent 60 to 100 parts of hollow glass micropearls are carried out surface modification treatment in parts by weight;
(4) resin adhesive liquid and the surface-treated hollow glass micropearl that above-mentioned steps 2 and step 3 are obtained add in the vacuum mixer, and low speed mixing is even;
(5) mixture that obtains in the above-mentioned steps 4 is joined in the three roller mixing rolls of Controllable Temperature, adjust three roller spacings, repeated multiple times is mixing;
(6) material that above-mentioned steps 5 is obtained is put into vacuum drying oven, vacuum defoamation under 60 to 80 ℃ temperature condition;
(7) material that above-mentioned steps 6 is obtained is cast in the various moulds, presses the moulding of curing process hot-press solidifying.
The preparation method of the aforesaid high-strength light of resin base under water matrix material; Wherein the surface modification treatment of hollow glass micropearl adopts room temperature spraying type stirring at low speed hybrid system; Hollow glass micropearl is joined in the low-speed mixer; When following slow stirring, in stirrer, spray vaporific coupling agent through shower nozzle; Said three roller mixing roll melting temperatures are 60 to 80 ℃, and three roller spacings are between 3 to 5mm.
The preparation method of the aforesaid high-strength light of resin base under water matrix material, wherein, said epoxy resin is the mixture of bisphenol A-type and glycidyl ester type epoxy resin, the ratio of weight and number of this mixture is 0: 100 to 100: 0; This bisphenol A type epoxy resin model is E51 or E44, and this glycidyl ester type epoxy resin model is TDE-85; Said solidifying agent is selected amido borine latent curing agent for use, and this amido borine latent curing agent is 2-(β-dimethylamino oxyethyl group)-1,3,6 trioxas-2-boron octane; Said toughner is liquid nbr carboxyl terminal; Said thinner is single epoxy group(ing) reactive thinner, and this list epoxy group(ing) reactive thinner is one or more in propenyl glycidyl ether, butylglycidyl ether, the phenyl glycidyl ether; Said coupling agent is a γ-An Bingjisanyiyangjiguiwan; Said cenosphere is a hollow glass microbead, and it is a kind of of 70 μ m to 115 μ m or several that this hollow glass microbead is selected particle diameter for use.
The present invention is the beneficial effect of resin base high-strength light matrix material and preparation method thereof under water, and resin base high-strength light composite density is lower under water for this, is 0.35 to 0.7g/cm
3, compressive strength can be applicable to the depth of water at the above ocean environment of 7000m at 30MPa to 80MPa, is 0.7g/cm in density particularly
3The time still can reach compressive strength 80MPa, realize the relatively uniform of density of material and compressive strength, guaranteed the compressive strength low density characteristic under the prerequisite that meets the requirements, good quality; This forming method is lower to equipment requirements, and moulding process is simple, and cost is low.
Embodiment
The present invention is resin base high-strength light matrix material under water, and the ratio of weight and number of its component is: epoxy resin is 80 to 100 parts, and solidifying agent is 8 to 12 parts, and toughner is 5 to 20 parts, and thinner is 0 to 5 part, and coupling agent is 1 to 2 part, and cenosphere is 60 to 100 parts.
The present invention is resin base high-strength light matrix material under water, and wherein: epoxy resin is the mixture of bisphenol A-type and glycidyl ester type epoxy resin, and the ratio of weight and number of this mixture is 0: 100 to 100: 0; This bisphenol A type epoxy resin is E51 or E44 type epoxy resin, and this glycidyl ester type epoxy resin is a TDE-85 type epoxy resin; Solidifying agent is selected amido borine latent curing agent for use, and this amido borine latent curing agent is 2-(β-dimethylamino oxyethyl group)-1,3,6 trioxas-2-boron octane; Toughner is liquid nbr carboxyl terminal; Thinner is single epoxy group(ing) reactive thinner, and this list epoxy group(ing) reactive thinner is one or more in propenyl glycidyl ether, butylglycidyl ether, the phenyl glycidyl ether; Coupling agent is a γ-An Bingjisanyiyangjiguiwan; Cenosphere is a hollow glass microbead, and it is a kind of of 70 μ m to 115 μ m or several that this hollow glass microbead is selected particle diameter for use.
The present invention is the preparation method of resin base high-strength light matrix material under water, and it may further comprise the steps:
(1) in parts by weight; Get mixture or single kind of epoxy resin, 0 to 5 part of thinner, 5 to 20 parts of the toughner of 80 to 100 parts of two kinds of epoxy resin, add in the reaction kettle, the control reactor temperature is at 60 to 80 ℃; Fully stir, prepolymerization reaction 30 is to 60min;
(2) in parts by weight, get 8 to 12 parts of solidifying agent and add in the performed polymer in the reaction kettle, mix, obtain resin adhesive liquid; Solidifying agent is with before performed polymer mixes, and solidifying agent and performed polymer are heated to 60 to 80 ℃ respectively, to improve Resin Flow and consistency;
(3), get 1 to 2 part of silane coupling agent 60 to 100 parts of hollow glass micropearls are carried out surface modification treatment in parts by weight;
(4) resin adhesive liquid and the surface-treated hollow glass micropearl that above-mentioned steps 2 and step 3 are obtained add in the vacuum mixer, and low speed mixing is even;
(5) mixture that obtains in the above-mentioned steps 4 is joined in the three roller mixing rolls of Controllable Temperature, adjust three roller spacings, repeated multiple times is mixing;
(6) material that above-mentioned steps 5 is obtained is put into vacuum drying oven, vacuum defoamation under 60 to 80 ℃ temperature condition;
(7) material that above-mentioned steps 6 is obtained is cast in the various moulds, presses the moulding of curing process hot-press solidifying.
The present invention is the preparation method of resin base high-strength light matrix material under water; Wherein: the surface modification treatment of said hollow glass micropearl adopts room temperature spraying type stirring at low speed hybrid system; Hollow glass micropearl is joined in the low-speed mixer; When following slow stirring, in stirrer, spray vaporific coupling agent through shower nozzle; Said three roller mixing roll melting temperatures are 60 to 80 ℃, and three roller spacings are between 3 to 5mm; Said epoxy resin is the mixture of bisphenol A-type and glycidyl ester type epoxy resin, and the ratio of weight and number of this mixture is 0: 100 to 100: 0; This bisphenol A type epoxy resin model is E51 or E44, and this glycidyl ester type epoxy resin model is TDE-85; Said solidifying agent is selected amido borine latent curing agent for use, and this amido borine latent curing agent is 2-(β-dimethylamino oxyethyl group)-1,3,6 trioxas-2-boron octane; Said toughner is liquid nbr carboxyl terminal; Said thinner is single epoxy group(ing) reactive thinner, and this list epoxy group(ing) reactive thinner is one or more in propenyl glycidyl ether, butylglycidyl ether, the phenyl glycidyl ether; Said coupling agent is a γ-An Bingjisanyiyangjiguiwan; Said cenosphere is a hollow glass microbead, and it is a kind of of 70 μ m to 115 μ m or several that this hollow glass microbead is selected particle diameter for use.
Embodiment:
Table 1 is six kinds of different ingredients of the present invention resin base high-strength light matrix material parts by weight of component under water
In table 1: solidifying agent can be selected 2-(β-dimethylamino oxyethyl group)-1,3,6 trioxas-2-boron octane for use; Toughner can be selected liquid nbr carboxyl terminal for use; Thinner can be selected one or more in propenyl glycidyl ether, butylglycidyl ether, the phenyl glycidyl ether for use; Coupling agent can be selected γ-An Bingjisanyiyangjiguiwan for use.
A representes that particle diameter is the hollow glass micropearl of 70 μ m in the table 1, and B representes that particle diameter is the hollow glass micropearl of 90 μ m, and C representes that particle diameter is the hollow glass micropearl of 115 μ m.
The high-strength light of the resin base under water composite wood of each embodiment moulding in the his-and-hers watches 1 carries out Performance Detection, and detected result is seen table 2.
Table 2 is the correlated performance of corresponding each embodiment in the table 1
From table 2, can see; The high-strength light of the resin base under water composite density that the present invention relates to is lower, is 0.35 to 0.7g/cm3, and compressive strength is from 30MPa to 80MPa; Can be applicable to the ocean environment of 7000m with headwater depth; Particularly when density is 0.7g/cm3, still can reach compressive strength 80MPa, realize the relatively uniform of density of material and compressive strength, guarantee the low density characteristic under the satisfactory prerequisite of compressive strength.Mechanical workouts such as still can sawing, dig, grind, inlay after this resin base high-strength light composite material solidification moulding under water and relevant processing treatment, and can select multiple flexible waterproof coating for use, and also its base material is bonding tight with finish paint.
The content that does not describe in the present embodiment is a prior art, so, give unnecessary details no longer in detail.
The present invention is the advantage of resin base high-strength light matrix material and preparation method thereof under water: material prescription is flexible, can use the depth of water in formula range, to adjust each amounts of components according to product, reaches and the light material that uses degree of depth coupling; Density of material according to the invention 0.35 to 0.7g/cm
3Between, compressive strength meets the requirement that universal material is equipped at the deep-sea 30 to 80MPa, good quality, and this forming method is lower to equipment requirements, and moulding process is simple, and cost is low.
Epoxy resin of the present invention is the mixture of glycidyl ester type epoxy resin and bisphenol A type epoxy resin; Wherein glycidyl ester type epoxy resin has the high-modulus characteristic; And the bisphenol A type epoxy resin manufacturability is good; Therefore can effectively improve the compressive strength of buoyancy material, possess excellent use characteristics simultaneously.
The hollow glass micropearl particle diameter that the present invention uses is even, its floatability is higher, and withstand voltage properties is good.
The solidifying agent that the present invention uses is selected LV, amido borine latent curing agent that reactive behavior is lower for use, can effectively increase the hollow glass micropearl loading level and prevent resin coking phenomenon in the solidification process, guarantees quality product.The toughner that uses is liquid nbr carboxyl terminal (CTBN), can be effectively and epoxy resin-base generation prepolymerization reaction, thus the small island structure of formation even compact, the toughness of increase body material is avoided material brittle destruction af-ter when stressed.The thinner that uses is single epoxy group(ing) reactive thinner; Used reactive thinner all contains epoxy group(ing); Can participate among the epoxy resin solidifying system, in solidification process, form reticulated structure closely, fully guarantee the strength property of cured product with epoxy matrix.The coupling agent that uses is γ-An Bingjisanyiyangjiguiwan, can form the molecule bridge mineral filler and resin matrix are combined closely effectively at the hollow glass micropearl surface grafting.It is one or more of 70 μ m to 115 μ m hollow glass microbeads that said hollow glass micropearl is selected particle diameter for use; Join principle according to the utmost point; Mix use through the different-grain diameter microballoon, realize closestpacking, so can select suitable specification for use according to the design density and the requirement of strength of goods.
The present invention joins high-intensity resin system, resting form curing system and high filler loading capacity ultralight hollow glass micropearl, organically combines and prepares according to the cure process of science through rationally long-pending; But the machining composite material of therefore preparing has lightweight, high-strength and performance characteristics that compactness is good; And the preparation method is simply efficient, is convenient to operation.
The above; It only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction, every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (10)
1. resin base high-strength light matrix material under water, it is characterized in that the ratio of weight and number of its component is: epoxy resin is 80 to 100 parts; Solidifying agent is 8 to 12 parts, and toughner is 5 to 20 parts, and thinner is 0 to 5 part; Coupling agent is 1 to 2 part, and cenosphere is 60 to 100 parts.
2. the high-strength light of resin base under water matrix material according to claim 1 is characterized in that said epoxy resin is the mixture of bisphenol A-type and glycidyl ester type epoxy resin, and the ratio of weight and number of this mixture is 0: 100 to 100: 0; This bisphenol A type epoxy resin model is E51 or E44, and this glycidyl ester type epoxy resin model is TDE-85.
3. according to claims 1 described high-strength light of resin base under water matrix material; It is characterized in that: said solidifying agent is selected amido borine latent curing agent for use; This amido borine latent curing agent is 2-(β-dimethylamino oxyethyl group)-1,3,6 trioxas-2-boron octane.
4. according to claims 1 described high-strength light of resin base under water matrix material, it is characterized in that: said toughner is liquid nbr carboxyl terminal.
5. according to claims 1 described high-strength light of resin base under water matrix material; It is characterized in that: said thinner is single epoxy group(ing) reactive thinner, and this list epoxy group(ing) reactive thinner is one or more in propenyl glycidyl ether, butylglycidyl ether, the phenyl glycidyl ether.
6. according to claims 1 described high-strength light of resin base under water matrix material, it is characterized in that: said coupling agent is a γ-An Bingjisanyiyangjiguiwan.
7. the high-strength light of resin base under water matrix material according to claim 1, it is characterized in that: said cenosphere is a hollow glass microbead, it is a kind of of 70 μ m to 115 μ m or several that this hollow glass microbead is selected particle diameter for use.
8. the preparation method of the high-strength light of a resin base under water matrix material as claimed in claim 1 is characterized in that, may further comprise the steps:
(1) in parts by weight; Get mixture or single kind of epoxy resin, 0 to 5 part of thinner, 5 to 20 parts of the toughner of 80 to 100 parts of two kinds of epoxy resin, add in the reaction kettle, the control reactor temperature is at 60 to 80 ℃; Fully stir, prepolymerization reaction 30 is to 60min;
(2) in parts by weight, get 8 to 12 parts of solidifying agent and add in the performed polymer in the reaction kettle, mix, obtain resin adhesive liquid; Solidifying agent is with before performed polymer mixes, and solidifying agent and performed polymer are heated to 60 to 80 ℃ respectively, to improve Resin Flow and consistency;
(3), get 1 to 2 part of coupling agent 60 to 100 parts of hollow glass micropearls are carried out surface modification treatment in parts by weight;
(4) resin adhesive liquid and the surface-treated hollow glass micropearl that above-mentioned steps 2 and step 3 are obtained add in the vacuum mixer, and low speed mixing is even;
(5) mixture that obtains in the above-mentioned steps 4 is joined in the three roller mixing rolls of Controllable Temperature, adjust three roller spacings, repeated multiple times is mixing;
(6) material that above-mentioned steps 5 is obtained is put into vacuum drying oven, vacuum defoamation under 60 to 80 ℃ temperature condition;
(7) material that above-mentioned steps 6 is obtained is cast in the various moulds, presses the moulding of curing process hot-press solidifying.
9. the preparation method of the high-strength light of resin base under water matrix material according to claim 8; It is characterized in that; The surface modification treatment of said hollow glass micropearl adopts spraying type stirring at low speed hybrid system under the room temperature; Hollow glass micropearl is joined in the low-speed mixer, when following slow stirring, in stirrer, spray vaporific coupling agent through shower nozzle; Said three roller mixing roll melting temperatures are 60 to 80 ℃, and three roller spacings are between 3 to 5mm.
10. the preparation method of the high-strength light of resin base under water matrix material according to claim 8; It is characterized in that; Said epoxy resin is the mixture of bisphenol A-type and glycidyl ester type epoxy resin, and the ratio of weight and number of this mixture is 0: 100 to 100: 0; This bisphenol A type epoxy resin model is E-51 or E-44, and this glycidyl ester type epoxy resin model is TDE-85; Said solidifying agent is selected amido borine latent curing agent for use, and this amido borine latent curing agent is 2-(β-dimethylamino oxyethyl group)-1,3,6 trioxas-2-boron octane; Said toughner is liquid nbr carboxyl terminal; Said thinner is single epoxy group(ing) reactive thinner, and this list epoxy group(ing) reactive thinner is one or more in propenyl glycidyl ether, butylglycidyl ether, the phenyl glycidyl ether; Said coupling agent is a γ-An Bingjisanyiyangjiguiwan; Said cenosphere is a hollow glass microbead, and it is a kind of of 70 μ m to 115 μ m or several that this hollow glass microbead is selected particle diameter for use.
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