CN104072950A - Raw material formula and preparation method for solid buoyancy material solidified at room temperature - Google Patents
Raw material formula and preparation method for solid buoyancy material solidified at room temperature Download PDFInfo
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Abstract
The invention discloses a raw material formula for a solid buoyancy material solidified at the room temperature. The formula comprises the following components in parts by weight: 100 parts of epoxy resin, curing agents, 30-45 parts of a reactive diluent, 0-1.5 parts of an accelerant, 0-1.0 part of a disperser, 3-6 parts of a coupling agent, and hollow glass beads, wherein curing agents comprise 5 to 15 parts of an aliphatic amine type curing agent and 15-45 parts of an alicyclic amine type curing agent, and the mass ratio of the aliphatic amine type curing agent to the alicyclic amine type curing agent is 1:3; the hollow glass beads comprise 20-40 parts of hollow beads I of which the density degree is 0.15 g/cm<3> and the compressive strength is greater than 2 MPa and 10-20 parts of hollow beads II of which the density degree is 0.60 g/cm<3> and the compressive strength is greater than 60 MPa, and mass ratio of the hollow beads I to the hollow beads II is 2:1. The invention further discloses a method for preparing the solid buoyancy material solidified at the room temperature by adopting the formula. Through the adoption of the method to prepare the buoyancy material, the compactness of the material can be ensured, and meanwhile the solidification can be finished under the room temperature condition.
Description
Technical field
The present invention relates to composition of raw materials of a kind of solid buoyancy material and preparation method thereof, particularly composition of raw materials of a kind of solid buoyancy material of ambient cure and preparation method thereof.
Background technology
China is an oceanic resources big country, exceedes 20,000,000,000 tons, more than gas in place 15 tcms at Bohai and Yellow Seas, the explored petroleum-in-place in the East Sea and On The Northern Continental Shelf of South China Sea marine site; All kinds of mineral deposits, coastal waters have more than 200, ore deposit point more than 100 individual, and oceanic mineral resources is contained abundant, and there is manganese nodule at the South Sea, and there is the hydrothermal solution sulfide mineral deposit of Okinawa trough northwest in the East Sea, and the DEVELOPMENT PROSPECT of deep sea mineral resources is very wide.
In recent years, constantly expansion both in depth and in breadth of China's ocean exploitation.Follow the continuous expansion of marine minerals, petrol resources exploitation scale, the demand of all kinds of oceanographic engineering materials significantly increases.The solid buoyancy material of high-strength light is the important component part of modern deep diving, underwater prospecting and ocean engineering technology.In the middle of the solid buoyancy material of numerous kinds, the over-all properties of composite solid buoyancy material (Solid Buoyancy Material) is comparatively outstanding, and range of application is very extensive.Composite solid buoyancy material is to utilize cenosphere to be filled in organic polymer material, the solid compounds obtaining through physical-chemical reaction.This class material is keeping under more low-density prerequisite, and the more traditional buoyancy material of resistance to hydrostatic pressure intensity significantly promotes.Traditional ocean big country such as the U.S., Russia has just started the development of this class material in the sixties in last century, comparatively advanced at the aspect such as synthesis technique, product performance at present.In recent years, domestic researcher is developed a series of different solid buoyancy materials that use the degree of depth that are applicable to successively, and related technique mostly is vacuum impregnating mold forming method and compression molding method, and its salient features approaches with same kind of products at abroad.Because the organic polymer matrix of choosing generally need to be cured under environment more than 60 DEG C, while therefore adopting an injection molding and forming technology, scantling is subject to the restriction of the equipment sizes such as baking oven; As adopt the techniques such as compression molding, although first preparing buoyancy material base substrate then carries out bonding method and can synthesize large size test block, but technique is complicated compared with the former, and due to reasons such as dust impurity, coating processes, easily there is defect at bonding position in test block, thereby affects material monolithic performance.If in ensureing material density, the test block of casting can complete curing under room temperature environment, has solved an above-mentioned difficult problem.
Although adopt alicyclic ring type solidifying agent or lard type solidifying agent cured epoxy resin in Chinese patent literature CN100378166C and CN103172975A, but material all uses vulcanizing press hot-forming and curing, single test block size is subject to the restriction of equipment and hot pressing die size, and base substrate profile is comparatively simple; Although propose to adopt the microballon/microballoon of different-grain diameter to mix and use as light filler in Chinese patent literature CN102936395A, its ratio range changes greatly, and and the undeclared foundation of selecting proportioning.
Summary of the invention
The present invention for solve the technical problem existing in known technology provide a kind of ambient cure solid buoyancy material composition of raw materials and adopt the solid buoyancy material preparation method of the ambient cure of this formula, adopt the buoyancy material of this preparation method's moulding in ensureing material density, can under room temperature environment, complete curingly, solve the problem that solid buoyancy material once shaped test specimen maximizes.
The technical scheme that the present invention takes for the technical problem existing in solution known technology is: a kind of composition of raw materials of solid buoyancy material of ambient cure, and the component of this formula and mass fraction thereof are:
Epoxy resin: bisphenol A type epoxy resin, by 100 parts;
Solidifying agent: fatty amines solidifying agent, 5-15 part; Alicyclic ring amine curing agent, 15-45 part, fatty amines solidifying agent and fatty amines solidifying agent mass ratio are 1:3;
Reactive thinner: polypropylene glycol diglycidyl ether, 30-45 part;
Promotor: three-(dimethylamino methyl) phenol, 0-1.5 part;
Dispersion agent: dispers630,0-1.0 part;
Coupling agent: γ-aminopropyl triethoxysilane, 3-6 part;
Hollow glass micropearl: density rating is 0.15g/cm
3, ultimate compression strength is greater than the I class cenosphere of 2MPa, 20-40 part; Density rating is 0.60g/cm
3, ultimate compression strength is greater than the II class cenosphere of 60MPa, 10-20 part, and I class and II class microballon mass ratio are 2:1.
The model of described epoxy resin is E51.
Described fatty amines solidifying agent adopts (2,3 dimethyl) two butylidene triamines, and described alicyclic ring amine curing agent adopts methyl ring pentamethylene diamine.
Another technical scheme that the present invention takes for the technical problem existing in solution known technology is: adopt the solid buoyancy material preparation method of the ambient cure of above-mentioned formula, adopt following steps:
One) by mass parts, by 100 parts of epoxy resin, 30-45 part reactive thinner, (0~1.0) part dispersion agent, 3-6 part coupling agent, 20-40 part I class cenosphere and 10-20 part II class cenosphere drop into normal temperature in vacuum stirring still to be mixed, and then under the vacuum state of 60-80 DEG C, at the uniform velocity stirs 20-30 minute, and reacting kettle inner pressure is-arrive-0.09MPa of 0.08MPa; Then naturally cool to room temperature, take out and obtain material A;
Two) by 5-15 part fatty amines solidifying agent, 15-45 part alicyclic ring amine curing agent and 0-1.5 part promotor are dropped in vacuum stirring still, at the uniform velocity stir 20-30 minute under the vacuum state of 60-80 DEG C, and reacting kettle inner pressure is-arrive-0.09MPa of 0.08MPa; Then naturally cool to room temperature, take out and obtain material B;
Three) material A is placed in to stirring at low speed 3-5 minute under kneader room temperature, then adds material B rapid stirring 15-20 minute, obtain mixed slurry; Mixed slurry is injected to mould, and adopt the method for vibration and stirring to make material fill densification at mould inside;
Four) material at room temperature leaves standstill 24-72 hour together with mould, obtains the base substrate of solid buoyancy material after the demoulding.
Advantage and positively effect that the present invention has are: taking epoxy resin, solidifying agent, reactive thinner, promotor, dispersion agent, coupling agent, hollow glass bead as raw material, adopt molding process to prepare the solid buoyancy material of high-strength light, this material can complete curing under room temperature environment, and by regulating the means such as material fluidity, mechanical pudding to ensure the density of product, solve the problem that solid buoyancy material once shaped test specimen maximizes.
Specifically, the present invention is by the add-on of the compound solidifying agent of preparation, adjusting thinner and promotor, curing speed to resin and the exothermal efficiency in the time solidifying are optimized, both retained certain operating time (operation such as mix and blend and injection molding), and made again curing time control in 72 hours; The hollow glass bead of selecting different-grain diameter to distribute, calculates suitable mass ratio to reach closelypacked effect according to the radius ratio of two kinds of glass microballons; Fill a prescription and preparation technology by adjusting, density of material can be controlled in 0.39-0.67g/cm
3, hydrostaticpressure intensity 17-100MPa, water-intake rate is less than 1%, can serve the ocean environment of the 1400-8000 rice depth of water, can be in field widespread uses such as oceanographic engineering, subsea resource exploitation, hydrologic monitorings.
Embodiment
For further understanding summary of the invention of the present invention, Characteristic, hereby exemplify following examples and be described in detail as follows:
Three composition of raw materials of the solid buoyancy material of ambient cure and the material property that adopts this formula to prepare, refer to following table:
Known by upper table, the component of above-mentioned raw materials formula and mass fraction thereof are:
Epoxy resin: bisphenol A type epoxy resin, by 100 parts;
Solidifying agent: fatty amines solidifying agent, 5-15 part; Alicyclic ring amine curing agent, 15-45 part, fatty amines solidifying agent and fatty amines solidifying agent mass ratio are 1:3;
Reactive thinner: polypropylene glycol diglycidyl ether, 30-45 part;
Promotor: three-(dimethylamino methyl) phenol, 0-1.5 part;
Dispersion agent: dispers630,0-1.0 part;
Coupling agent: γ-aminopropyl triethoxysilane, 3-6 part;
Hollow glass micropearl: density rating is 0.15g/cm
3, ultimate compression strength is greater than the I class cenosphere of 2MPa, 20-40 part; Density rating is 0.60g/cm
3, ultimate compression strength is greater than the II class cenosphere of 60MPa, 10-20 part, and I class and II class microballon mass ratio are 2:1.
The preferred E51 of above-mentioned epoxy resin.But be not limited to this, above-mentioned epoxy resin can also be selected the model such as E44, E56, described fatty amines solidifying agent is (2,3 dimethyl) two butylidene triamines preferably, described alicyclic ring amine curing agent preferable methyl ring pentamethylene diamine.But be not limited to this, above-mentioned fatty amines solidifying agent can also be selected triethylene tetramine, diethyl amino propylamine etc., and above-mentioned alicyclic ring amine curing agent can also be selected methyl ring pentamethylene diamine etc.The preferred Minnesota Mining and Manufacturing Company of hollow glass micropearl hollow glass bead, (density rating is 0.15g/cm to K1
3), 20-40 part; (density rating is 0.60g/cm to S60HS
3), 10-20 part.
Adopt above-mentioned formula to prepare the method for the solid buoyancy material of ambient cure, adopt following steps:
One) by mass parts, by 100 parts of epoxy resin, 30-45 part reactive thinner, (0~1.0) part dispersion agent, 3-6 part coupling agent, 20-40 part I class cenosphere and 10-20 part II class cenosphere drop into normal temperature in vacuum stirring still to be mixed, and then under the vacuum state of 60-80 DEG C, at the uniform velocity stirs 20-30 minute, and reacting kettle inner pressure is-arrive-0.09MPa of 0.08MPa; Then naturally cool to room temperature, take out and obtain material A;
Two) by 5-15 part fatty amines solidifying agent, 15-45 part alicyclic ring amine curing agent and 0-1.5 part promotor are dropped in vacuum stirring still, at the uniform velocity stir 20-30 minute under the vacuum state of 60-80 DEG C, and reacting kettle inner pressure is-arrive-0.09MPa of 0.08MPa; Then naturally cool to room temperature, take out and obtain material B;
Three) material A is placed in to stirring at low speed 3-5 minute under kneader room temperature, then adds material B rapid stirring 15-20 minute, obtain mixed slurry; Mixed slurry is injected to mould, and adopt the method for vibration and stirring to make material fill densification at mould inside;
Four) material at room temperature leaves standstill 24-72 hour together with mould, obtains the base substrate of solid buoyancy material after the demoulding.
In the above-described embodiments, in the time that the amount of hollow glass bead increases, step 1) in temperature of charge should improve vacuum stirring time, when needs≤80 DEG C, to reduce viscosity, material is more easily mixed.
Base substrate after solidifying can be processed according to user demand by means such as saw, milling, mills, can come into operation material is carried out after surface reinforcing and WATER REPELLENT.Density of material is 0.39-0.67g/cm
3, corresponding uniaxial compressive strength is 14-83MPa, all sample water-intake rates are all less than 1%.According to unmanned underwater vehicle's buoyancy compensation material convention, in the time that safety coefficient is 1.2, the product that adopts this preparation method to obtain can be served the ocean environment of the 1400-8000 rice depth of water.Adopt the product that this preparation method obtains need to be processed into certain size profile according to using, can be widely used in the fields such as oceanographic engineering, underwater towing, marine petroleum exploitation, submarine mining and seafari.
Principle of the present invention:
The composite normal temperature solidifying agent that the present invention selects is fatty amines solidifying agent and alicyclic ring amine curing agent (both ratios are 1:3).As everyone knows, in the middle of conventional epoxy curing agent, this two classes solidifying agent curing speed is very fast and can complete at normal temperatures curing.The curing speed of fatty amines solidifying agent is faster compared with alicyclic ring amine, can complete at short notice the primary solidification of resin/microballon mixed slurry, but the too fast meeting of curing speed causes the mechanical property of resin to reduce, and therefore adds a part of alicyclic ring amine curing agent to reduce the curing speed of mixture.Epoxy resin and solidifying agent are by being cross-linked to form three-dimensional net structure, and the too fast meeting of curing speed makes to form more defect in resin, causes mechanical properties decrease; On the other hand, the too fast meeting of curing speed causes the rapid release of reaction heat, causes resin internal temperature sharply to raise, and also can cause disadvantageous effect to the mechanical property of material, and therefore in compound solidifying agent, alicyclic ring amine proportion is more.
The volume density of buoyancy material declines with the increase of microballon add-on, and ultimate compression strength also declines thereupon simultaneously, and how in keeping density of material, to improve material mechanical performance is the key of preparing high-performance solid buoyancy material.When the hollow glass bead of same particle size range forms when tightly packed, space between microballon is by resin filling, if adopt the less microballon of particle diameter to replace this part resin, the volume density of material can further reduce, and mechanical property does not have obvious change in theory.Adopt two kinds of hollow glass micropearls that size-grade distribution is different, and a kind of particle diameter of microballon is approximately 1/2 of another kind of microballon particle diameter, according to theory of close packing, K1 forms tightly packed, S60HS is positioned at octahedral central position that K1 forms, both theoretical molar are than being 1:1, and in conjunction with the real density reckoning of microballon, both form closelypacked optimum quality ratio is 1:2.Resin/microballon the composite structure forming under this proportioning should have best strength/density ratio.
Although above the preferred embodiments of the present invention are described; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not departing from the scope situation that aim of the present invention and claim protect, can also make a lot of forms, within these all belong to protection scope of the present invention.
Claims (4)
1. a composition of raw materials for the solid buoyancy material of ambient cure, is characterized in that, the component of this formula and mass fraction thereof are:
Epoxy resin: bisphenol A type epoxy resin, by 100 parts;
Solidifying agent: fatty amines solidifying agent, 5-15 part; Alicyclic ring amine curing agent, 15-45 part, fatty amines solidifying agent and fatty amines solidifying agent mass ratio are 1:3;
Reactive thinner: polypropylene glycol diglycidyl ether, 30-45 part;
Promotor: three-(dimethylamino methyl) phenol, 0-1.5 part;
Dispersion agent: dispers630,0-1.0 part;
Coupling agent: γ-aminopropyl triethoxysilane, 3-6 part;
Hollow glass micropearl: density rating is 0.15g/cm
3, ultimate compression strength is greater than the I class cenosphere of 2MPa, 20-40 part; Density rating is 0.60g/cm
3, ultimate compression strength is greater than the II class cenosphere of 60MPa, 10-20 part, and I class and II class microballon mass ratio are 2:1.
2. the composition of raw materials of the solid buoyancy material of ambient cure according to claim 1, is characterized in that, the model of described epoxy resin is E51.
3. the composition of raw materials of the solid buoyancy material of ambient cure according to claim 2, is characterized in that, described fatty amines solidifying agent adopts (2,3 dimethyl) two butylidene triamines, and described alicyclic ring amine curing agent adopts methyl ring pentamethylene diamine.
4. adopt the solid buoyancy material preparation method of the ambient cure of formula as claimed in claim 1, it is characterized in that, adopt following steps:
One) by mass parts, by 100 parts of epoxy resin, 30-45 part reactive thinner, (0~1.0) part dispersion agent, 3-6 part coupling agent, 20-40 part I class cenosphere and 10-20 part II class cenosphere drop into normal temperature in vacuum stirring still to be mixed, and then under the vacuum state of 60-80 DEG C, at the uniform velocity stirs 20-30 minute, and reacting kettle inner pressure is-arrive-0.09MPa of 0.08MPa; Then naturally cool to room temperature, take out and obtain material A;
Two) by 5-15 part fatty amines solidifying agent, 15-45 part alicyclic ring amine curing agent and 0-1.5 part promotor are dropped in vacuum stirring still, at the uniform velocity stir 20-30 minute under the vacuum state of 60-80 DEG C, and reacting kettle inner pressure is-arrive-0.09MPa of 0.08MPa; Then naturally cool to room temperature, take out and obtain material B;
Three) material A is placed in to stirring at low speed 3-5 minute under kneader room temperature, then adds material B rapid stirring 15-20 minute, obtain mixed slurry; Mixed slurry is injected to mould, and adopt the method for vibration and stirring to make material fill densification at mould inside;
Four) material at room temperature leaves standstill 24-72 hour together with mould, obtains the base substrate of solid buoyancy material after the demoulding.
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Cited By (6)
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CN105542219A (en) * | 2016-02-26 | 2016-05-04 | 天津中材工程研究中心有限公司 | Preparation method for light high-strength composite hollow sphere |
CN109651764A (en) * | 2018-12-26 | 2019-04-19 | 天津中材工程研究中心有限公司 | A kind of solid buoyancy material and preparation method thereof of microballon compounding |
CN110628180A (en) * | 2019-09-26 | 2019-12-31 | 海洋化工研究院有限公司 | Solid buoyancy material and preparation method thereof |
US10611100B2 (en) | 2015-06-12 | 2020-04-07 | 3M Innovative Properties Company | Buoyancy module |
CN111303589A (en) * | 2020-04-07 | 2020-06-19 | 华北电力大学(保定) | Preparation method of composite insulating cross arm core body |
CN111378244A (en) * | 2018-12-29 | 2020-07-07 | 中国科学院理化技术研究所 | Solid buoyancy material and preparation method and application thereof |
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CN103421278A (en) * | 2013-08-10 | 2013-12-04 | 滕州市华海新型保温材料有限公司 | Low-density high-strength solid buoyancy material and preparation method thereof |
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CN111303589A (en) * | 2020-04-07 | 2020-06-19 | 华北电力大学(保定) | Preparation method of composite insulating cross arm core body |
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