CN109486116A - A kind of deep-sea buoyant material and preparation method thereof - Google Patents
A kind of deep-sea buoyant material and preparation method thereof Download PDFInfo
- Publication number
- CN109486116A CN109486116A CN201811423172.4A CN201811423172A CN109486116A CN 109486116 A CN109486116 A CN 109486116A CN 201811423172 A CN201811423172 A CN 201811423172A CN 109486116 A CN109486116 A CN 109486116A
- Authority
- CN
- China
- Prior art keywords
- deep
- sea
- buoyant material
- graphene
- epoxy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention discloses a kind of deep-sea buoyant materials and preparation method thereof, are related to chemical material technical field.A kind of deep-sea buoyant material provided by the invention and preparation method thereof, for low bulk density, high-intensitive graphene designs modified technique, to improve evenly dispersed performance of the graphene in epoxy-resin systems, and by the preparation process of optimization by modified graphene and epoxy resin, curing agent prepares deep-sea buoyant material collectively as raw material, obtained deep-sea buoyant material has low-density, high hydrostatic pressure resistance intensity, the material property of low water absorption, the deep-sea buoyant material is applied to the preparation of deep-sea instrument and equipment, the use environment of deep-sea instrument and equipment can greatly be extended.The present invention can solve the technical problem that deep-sea buoyant material density is larger, resistance to hydrostatic pressure intensity is lower, reach the density of material for reducing deep-sea buoyant material, the technical effect for improving resistance to hydrostatic pressure intensity, reducing water absorption rate.
Description
Technical field
The present invention relates to chemical material technical field, in particular to a kind of deep-sea buoyant material and preparation method thereof.
Background technique
With the propulsion of global deep-sea strategy and the continuous development of deep-sea development technology, more and more deep-sea instruments and set
It is standby to come into operation.Since the usual hydrostatic pressure of the working environment of deep-sea instrument and equipment is high, the material of deep-sea instrument and equipment
It needs to provide net buoyancy using deep-sea buoyant material, so that it is guaranteed that deep-sea instrument and equipment are in the high working environment of hydrostatic pressing
Normal operation and safe retrieving, wherein the performances such as strong, water absorption rate of the density of deep-sea buoyant material, resistance to hydrostatic pressure are directly determined
The working performance and working depth of depthkeeping sea instrument and equipment.
The structure of existing deep-sea buoyant material is formed usually using epoxy resin as matrix by filler of hollow glass micropearl
Solid composite foam.For example, 101735566 A of Chinese patent CN discloses a kind of processable full sea-depth buoyancy material and manufacture
The resistance to hydrostatic pressure intensity of method, deep-sea buoyant material disclosed in the patent is about 115 MPa, but its density is higher, and about 0.70
g/cm3, to greatly limit it in deep-sea instrument and the use environment of equipment.
In the implementation of the present invention, inventor find the relevant technologies the prior art has at least the following problems:
Generally higher (>=0.50 g/cm of hollow glass micro-ball density used in the deep-sea buoyant material that the prior art provides3),
And hollow glass micro-ball is easy to that disrepair phenomenon occurs in process, and the close of hollow glass micro-ball is further increased
Degree, so that the subsequent deep-sea buoyant material density being prepared is also higher, limits it in the service performance of deep-sea buoyant material.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, the present invention provides a kind of deep-sea buoyant material and preparation method thereof,
The present invention prepares deep-sea buoyant material, buoyant material tool in deep-sea obtained by using modified graphene, epoxy resin, curing agent
There are the advantages such as density is low, resistance to hydrostatic pressure intensity is high, water absorption rate is low.Technical scheme is as follows:
First aspect according to an embodiment of the present invention provides a kind of preparation method of deep-sea buoyant material, which is characterized in that institute
The method of stating includes:
Pretreated epoxy resin is added to the agitator of vacuum defoamation blender, then heats the temperature of the agitator
To 80 ~ 90 °C, Xiang Suoshu agitator is added curing agent and carries out uniform stirring；
To the agitator be added modified graphene, adjust the agitator vacuum degree be -0.08 ~ -0.10 atm, continue into
Row is stirring uniformly to obtain mixture；
The mixture is transferred to mold from the agitator, the temperature of the mold is then heated up to 120 ~ 140 °C, is protected
The curing molding of the mixture is completed after 5 ~ 10 h of temperature, then the mixture after curing molding is subjected to cooling demoulding, is made
Standby to obtain deep-sea buoyant material, the density of the deep-sea buoyant material is 0.50 ~ 0.56 g/cm3, resistance to hydrostatic pressure intensity be 115 ~
140 MPa, water absorption rate≤2%；
The mass parts ratio of the pretreated epoxy resin, the curing agent and the modified graphene be 100: 20 ~
40∶1~5。
In a preferred embodiment, the preparation method of the modified graphene includes:
30 ~ 90 min of ultrasonic disperse is added into dehydrated alcohol in graphene, graphene solution is prepared, the graphene is molten
The mass parts ratio of graphene and dehydrated alcohol is 1 ~ 5: 200 ~ 400 in liquid；
Dehydrated alcohol and deionized water are mixed to form mixed solution, Xiang Suoshu mixed solution adds acetic acid, adjusts the mixing
Then to 3.5 ~ 4.5 silane coupling agent is slowly added dropwise to the mixed solution, by the mixed solution high-speed stirring in the pH value of solution
30 ~ 60 min of dispersion is mixed, silane coupler solution is prepared, dehydrated alcohol, deionized water in the silane coupler solution
Mass parts ratio with silane coupling agent is 100 ~ 200: 20 ~ 60: 0.5 ~ 1.0；
The silane coupler solution is slowly added to the graphene solution and forms reaction solution, is controlled the reaction solution and is existed
4 ~ 8 h are reacted under 70 ~ 90 DEG C of reaction temperature, and the reaction solution is filtered, is dried, modified graphene is prepared.
In a preferred embodiment, the preprocess method of the epoxy resin includes:
Epoxy resin is warming up to 85 ~ 95 °C, when the epoxy resin is in complete molten condition, epoxy-reactive dilution is added
Agent after stirring evenly 10 ~ 20 min at a temperature of 85 ~ 95 °C, is cooled to 55 ~ 65 °C, pretreated epoxy is prepared
The mass parts ratio of resin, the epoxy resin and the epoxy active diluent is 100: 15 ~ 25.
In a preferred embodiment, the epoxy resin contain there are three or four epoxy groups, the epoxy-reactive
Diluent contains two epoxy groups.
In a preferred embodiment, the curing agent is aromatic amine curing agent.
In a preferred embodiment, the silane coupling agent is that gamma-aminopropyl-triethoxy-silane or γ-shrink are sweet
At least one of oily ether oxygen propyl trimethoxy silicane.
In a preferred embodiment, the density of the graphene is 0.01 ~ 0.10 g/cm3。
In a preferred embodiment, the operating pressure for the vulcanizer that curing molding process uses is 10 ~ 15 MPa.
The second aspect according to an embodiment of the present invention provides a kind of deep-sea buoyant material, which is characterized in that the deep-sea
Buoyant material is prepared by the preparation method of above-mentioned any one the deep-sea buoyant material shown, the deep-sea buoyant material packet
Include following component and its mass fraction: 80 ~ 120 parts of epoxy resin, 15 ~ 25 parts of epoxy active diluent, 20 ~ 40 parts of curing agent, 1
~ 5 parts of modified graphenes, the density of the deep-sea buoyant material are 0.50 ~ 0.56 g/cm3, resistance to hydrostatic pressure intensity is 115 ~ 140
MPa, water absorption rate≤2%.
Compared with prior art, a kind of deep-sea buoyant material provided by the invention and preparation method thereof has the advantage that
A kind of deep-sea buoyant material provided by the invention and preparation method thereof is set for low bulk density, high-intensitive graphene
Modified technique is counted, to improve evenly dispersed performance of the graphene in epoxy-resin systems, and passes through the preparation process of optimization
Modified graphene and epoxy resin, curing agent are prepared into deep-sea buoyant material, obtained deep-sea buoyant material collectively as raw material
Have low-density, high hydrostatic pressure resistance intensity, low water absorption material property, which is applied to deep-sea instrument and set
Standby preparation can greatly extend the use environment of deep-sea instrument and equipment.The present invention can solve deep-sea buoyant material density it is larger,
The lower technical problem of resistance to hydrostatic pressure intensity reaches the density of material for reducing deep-sea buoyant material, improves resistance to hydrostatic pressure intensity, drop
The technical effect of low water absorption.
Detailed description of the invention
The drawings herein are incorporated into the specification and forms part of this specification, and shows and meets implementation of the invention
Example, and be used to explain the principle of the present invention together with specification.
Fig. 1 is a kind of method flow diagram of the preparation method of deep-sea buoyant material shown according to an exemplary embodiment.
Fig. 2 is that a kind of modified graphene shown according to an exemplary embodiment prepares schematic diagram.
Specific embodiment
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
The present invention prepares deep-sea buoyancy material with epoxy resin, curing agent by being modified to graphene, then by it jointly
Material.The deep-sea buoyant material of preparation has the advantages that density is low, resistance to hydrostatic pressure intensity is high, water absorption rate is low etc., and the present invention passes through following
Technical solution is realized:
Fig. 1 is a kind of method flow diagram of the preparation method of deep-sea buoyant material shown according to an exemplary embodiment, such as Fig. 1
It is shown, this method comprises:
Step 101: pretreated epoxy resin being added to the agitator of vacuum defoamation blender, then by the agitator
Temperature is heated up to 80 ~ 90 °C, and Xiang Suoshu agitator is added curing agent and carries out uniform stirring.
In one possible implementation, the preprocess method of the epoxy resin includes:
Epoxy resin is warming up to 85 ~ 95 °C, when the epoxy resin is in complete molten condition, epoxy-reactive dilution is added
Agent after stirring evenly 10 ~ 20 min at a temperature of 85 ~ 95 °C, is cooled to 55 ~ 65 °C, pretreated epoxy is prepared
The mass parts ratio of resin, the epoxy resin and the epoxy active diluent is 100: 15 ~ 25.
Wherein, there are three the epoxy resin contains or four epoxy groups, the epoxy active diluent contain two rings
Oxygen groups.For example, the epoxy resin can be four tetraglycidel ether epoxy resin of resorcinol formaldehyde, 1,1,2,2- tetra- (right
Hydroxy phenyl) four tetraglycidel ether epoxy resin of ethane, triphenol methylmethane triglycidyl ether epoxy resin, 1,3,5-trihydroxybenzene three contracts
At least one of water glycerin ether epoxy resin.
The curing agent is aromatic amine curing agent.For example, curing agent can be m-xylene diamine, diamino-diphenyl first
Alkane, at least one of m-phenylene diamine (MPD).
Step 102: Xiang Suoshu agitator be added modified graphene, adjust the agitator vacuum degree be -0.08 ~ -
0.10 atm continues to be stirring uniformly to obtain mixture.
Wherein, the preparation method of the modified graphene includes:
(1) 30 ~ 90 min of ultrasonic disperse is added into dehydrated alcohol in graphene, graphene solution, the graphite is prepared
The mass parts ratio of graphene and dehydrated alcohol is 1 ~ 5: 200 ~ 400 in alkene solution.
Wherein, the density of the graphene is 0.01 ~ 0.10 g/cm3。
(2) dehydrated alcohol and deionized water are mixed to form mixed solution, Xiang Suoshu mixed solution adds acetic acid, adjusts institute
The pH value of mixed solution is stated to 3.5 ~ 4.5, silane coupling agent then is slowly added dropwise to the mixed solution, by the mixed solution
High-speed stirred disperses 30 ~ 60 min, and silane coupler solution is prepared, and dehydrated alcohol in the silane coupler solution is gone
The mass parts ratio of ionized water and silane coupling agent is 100 ~ 200: 20 ~ 60: 0.5 ~ 1.0.
Wherein, the silane coupling agent is gamma-aminopropyl-triethoxy-silane (KH-550) or γ-glycidyl ether oxygen third
At least one of base trimethoxy silane (KH-560).
(3) Xiang Suoshu graphene solution is slowly added to the silane coupler solution and forms reaction solution, controls described anti-
It answers solution to react 4 ~ 8 h under 70 ~ 90 DEG C of reaction temperature, the reaction solution is filtered, is dried, modification is prepared
Graphene.
It should be noted that conventional graphite alkene has low bulk density, high-intensitive characteristic, it is ensured that deep-sea buoyant material
Resistance to hydrostatic pressure intensity while, reduce its density.But conventional graphite alkene has the material property for being easy to reunite, itself is difficult to
It is dispersed in epoxy-resin systems, therefore the preparation of deep-sea buoyant material can not be applied to.The present invention passes through to low accumulation
Density, high-intensitive graphene are modified, to improve modified graphene evenly dispersed performance in epoxy-resin systems, are made
At deep-sea, the application of buoyant material has possibility.
Embodiment to the modified technique of graphene, show by the preparation that spy shows modified graphene in order to better illustrate the present invention
It is intended to, as shown in Figure 2.
Step 103: the mixture being transferred to mold from the agitator, is then heated up to the temperature of the mold
120 ~ 140 °C, the curing molding of the mixture is completed after keeping the temperature 5 ~ 10 h, then the mixture after curing molding is carried out
Cooling demoulding, is prepared deep-sea buoyant material, and the density of the deep-sea buoyant material is 0.50 ~ 0.56 g/cm3, resistance to hydrostatic
Compressive Strength is 115 ~ 140 MPa, water absorption rate≤2%.
It should be noted that the present invention carries out the work of vulcanizer used by curing molding process to the mixture in mold
Making pressure is 10 ~ 15 MPa.
It should be noted that pretreated epoxy resin described above, the curing agent and the modified graphene
Mass parts ratio be 100: 20 ~ 40: 1 ~ 5.
In conclusion a kind of deep-sea buoyant material provided by the invention and preparation method thereof, for low bulk density, high-strength
The graphene of degree designs modified technique, to improve evenly dispersed performance of the graphene in epoxy-resin systems, and by excellent
Modified graphene and epoxy resin, curing agent are prepared deep-sea buoyant material collectively as raw material by the preparation process of change, are obtained
Deep-sea buoyant material have low-density, high hydrostatic pressure resistance intensity, low water absorption material property, which is applied to
The preparation of deep-sea instrument and equipment can greatly extend the use environment of deep-sea instrument and equipment.The present invention can solve deep-sea buoyancy
The technical problem that density of material is larger, resistance to hydrostatic pressure intensity is lower reaches the density of material for reducing deep-sea buoyant material, improves resistance to
Hydrostatic pressing intensity, the technical effect for reducing water absorption rate.
The beneficial effect of the deep-sea buoyant material provided in order to better illustrate the present invention and preparation method thereof is shown following
Embodiment 1 ~ 3 is illustrated:
Embodiment 1
(1) preparation of modified graphene:
It calculates according to the mass fraction, is 0.04 g/cm by density35 parts of graphenes the ultrasonic disperse into 300 parts of dehydrated alcohols is added
60 min, are prepared graphene solution；200 parts of dehydrated alcohols and 40 parts of deionized waters are mixed to form mixed solution, to institute
Mixed solution addition acetic acid is stated, the pH value of the mixed solution is adjusted to 3.5 ~ 4.5, is then slowly added dropwise to the mixed solution
The mixed solution high-speed stirred is dispersed 60 min, silane coupler solution is prepared by 0.5 part of silane coupling agent；To institute
It states graphene solution and is slowly added to the silane coupler solution and form reaction solution, it is anti-at 80 DEG C to control the reaction solution
6 h are reacted at a temperature of answering, and the reaction solution is filtered, is dried, modified graphene is prepared.
(2) pretreatment of epoxy resin:
It calculates according to the mass fraction, by 15 parts of four tetraglycidel ether epoxy resins of resorcinol formaldehyde and 70 part 1,1,2,2 ~ tetra- is (right
Hydroxy phenyl) ethane four tetraglycidel ether epoxy resin be warming up to 90 °C, when each epoxy resin is in complete molten condition,
15 parts of ethylene glycol diglycidylethers are added, after 10 min are stirred evenly at a temperature of 90 °C, is cooled to 60 °C, is prepared
Pretreated epoxy resin.
(3) preparation of deep-sea buoyant material:
It calculates according to the mass fraction, 100 parts of pretreated epoxy resin is added to the agitator of vacuum defoamation blender, then will
The temperature of the agitator is heated up to 80 °C, and 20 parts of m-phenylene diamine (MPD)s and the blender using high shear force is added in Xiang Suoshu agitator
Carry out uniform stirring；To the agitator be added 5 parts of modified graphenes, adjust the agitator vacuum degree be -0.08 ~ -
0.10 atm continues to be stirring uniformly to obtain mixture；The mixture is transferred to mold from the agitator, using sulphur
Change machine carries out curing molding, and the temperature of the mold is then heated up to 120 °C, completes consolidating for the mixture after keeping the temperature 8 h
Chemical conversion type, then the mixture after curing molding is subjected to cooling demoulding, deep-sea buoyant material is prepared.
Embodiment 2
(1) preparation of modified graphene:
It calculates according to the mass fraction, is 0.03 g/cm by density34 parts of graphenes the ultrasonic disperse into 300 parts of dehydrated alcohols is added
90 min, are prepared graphene solution；200 parts of dehydrated alcohols and 40 parts of deionized waters are mixed to form mixed solution, to institute
Mixed solution addition acetic acid is stated, the pH value of the mixed solution is adjusted to 3.5 ~ 4.5, is then slowly added dropwise to the mixed solution
The mixed solution high-speed stirred is dispersed 60 min, silane coupler solution is prepared by 0.8 part of silane coupling agent；To institute
It states graphene solution and is slowly added to the silane coupler solution and form reaction solution, it is anti-at 80 DEG C to control the reaction solution
7 h are reacted at a temperature of answering, and the reaction solution is filtered, is dried, modified graphene is prepared.
(2) pretreatment of epoxy resin:
It calculates according to the mass fraction, 15 parts of four tetraglycidel ether epoxy resins of resorcinol formaldehyde and 70 parts of triphenol methylmethanes three is contracted
Water glycerin ether epoxy resin is warming up to 90 °C, and when each epoxy resin is in complete molten condition, 10 parts of ethylene glycol two are added
Glycidol ether and 5 parts of diglycidyl ethers, after stirring evenly 15min at a temperature of 90 °C, are cooled to 60 °C, are prepared into
To pretreated epoxy resin.
(3) preparation of deep-sea buoyant material:
It calculates according to the mass fraction, 100 parts of pretreated epoxy resin is added to the agitator of vacuum defoamation blender, then will
The temperature of the agitator is heated up to 90 °C, and 10 parts of m-phenylene diamine (MPD)s and 15 parts of diamino-diphenyl first are added in Xiang Suoshu agitator
Alkane simultaneously carries out uniform stirring using the blender of high shear force；4 parts of modified graphenes are added to the agitator, are stirred described in adjustment
The vacuum degree for mixing bucket is -0.08 ~ -0.10 atm, continues to be stirring uniformly to obtain mixture；The mixture is stirred from described
It mixes bucket and is transferred to mold, curing molding is carried out using vulcanizer, the temperature of the mold is then heated up to 130 °C, keeps the temperature 8 h
The curing molding of the mixture is completed afterwards, then the mixture after curing molding is subjected to cooling demoulding, and depth is prepared
Extra large buoyant material.
Embodiment 3
(1) preparation of modified graphene:
It calculates according to the mass fraction, is 0.02 g/cm by density33 parts of graphenes the ultrasonic disperse into 400 parts of dehydrated alcohols is added
90 min, are prepared graphene solution；200 parts of dehydrated alcohols and 60 parts of deionized waters are mixed to form mixed solution, to institute
Mixed solution addition acetic acid is stated, the pH value of the mixed solution is adjusted to 3.5 ~ 4.5, is then slowly added dropwise to the mixed solution
The mixed solution high-speed stirred is dispersed 60 min, silane coupler solution is prepared by 1.0 parts of silane coupling agents；To institute
It states graphene solution and is slowly added to the silane coupler solution and form reaction solution, it is anti-at 80 DEG C to control the reaction solution
8 h are reacted at a temperature of answering, and the reaction solution is filtered, is dried, modified graphene is prepared.
(2) pretreatment of epoxy resin:
It calculates according to the mass fraction, by 30 part 1,1,2,2- tetra- (p-hydroxybenzene) ethane, four tetraglycidel ether epoxy resin and 50 parts
1,3,5-trihydroxybenzene triglycidyl ether epoxy resin is warming up to 90 °C, when each epoxy resin is in complete molten condition, is added
10 parts of ethylene glycol diglycidylethers and 10 parts of diglycidyl ethers, after 20 min are stirred evenly at a temperature of 90 °C, cooling
To 60 °C, pretreated epoxy resin is prepared.
(3) preparation of deep-sea buoyant material:
It calculates according to the mass fraction, 100 parts of pretreated epoxy resin is added to the agitator of vacuum defoamation blender, then will
The temperature of the agitator is heated up to 80 °C, and Xiang Suoshu agitator is added 10 parts of m-phenylene diamine (MPD)s and 15 parts of m-xylene diamines and uses
The blender of high shear force carries out uniform stirring；3 parts of modified graphenes are added to the agitator, adjust the true of the agitator
Reciprocal of duty cycle is -0.08 ~ -0.10 atm, continues to be stirring uniformly to obtain mixture；The mixture is shifted from the agitator
To mold, curing molding is carried out using vulcanizer, the temperature of the mold is then heated up to 140 °C, is completed after keeping the temperature 10 h
The curing molding of the mixture, then the mixture after curing molding is subjected to cooling demoulding, deep-sea buoyancy is prepared
Material.
The deep-sea buoyant material that above-described embodiment 1 ~ 3 is prepared carries out mechanics detection, obtained properties data
It is as shown in Table 1:
| Density of material | Resistance to hydrostatic pressure intensity | Water absorption rate | |
| Embodiment 1 | 0.56 g/cm3 | 140 MPa | ≤2% |
| Embodiment 2 | 0.53 g/cm3 | 125 MP | ≤2% |
| Embodiment 3 | 0.50 g/cm3 | 115 MPa | ≤2% |
Table one
It should be noted that water absorption rate is test environment of each deep-sea buoyant material in 115 MPa hydrostatic pressing, 24 h in table one
Under measure.
By table one as it can be seen that the density for the deep-sea buoyant material that embodiment 1 is prepared is 0.56 g/cm3, resistance to hydrostatic pressure is strong
Degree is 140 MPa, water absorption rate≤2%；The density for the deep-sea buoyant material that embodiment 2 is prepared is 0.53 g/cm3, resistance to hydrostatic
Compressive Strength is 125 MPa, water absorption rate≤2%；The density for the deep-sea graphene buoyant material that embodiment 3 is prepared is 0.50 g/
cm3, resistance to hydrostatic pressure intensity is 115 MPa, water absorption rate≤2%.
It is clear that the resistance to hydrostatic pressure intensity for the deep-sea buoyant material that each embodiment is prepared is above 115 MPa,
And density of material is far below 0.70 g/cm3, therefore, the material property of deep-sea buoyant material provided by the invention is solid better than tradition
Body deep-sea buoyant material.
Items analysis test result shows: the deep-sea that the preparation method of deep-sea buoyant material provided by the invention is prepared
Buoyant material replaces traditional hollow glass micro-ball by low-density, high-intensitive modified graphene, so that deep-sea buoyancy material
The density of material is greatly reduced, and resistance to hydrostatic pressure intensity is enhanced, while keeping low water absorption, and deep sea equipment can be greatly improved
With the working performance of instrument, the use environment of deep sea equipment and instrument is widened.
In conclusion a kind of deep-sea buoyant material provided by the invention and preparation method thereof, for low bulk density, high-strength
The graphene of degree designs modified technique, to improve evenly dispersed performance of the graphene in epoxy-resin systems, and by excellent
Modified graphene and epoxy resin, curing agent are prepared deep-sea buoyant material collectively as raw material by the preparation process of change, are obtained
Deep-sea buoyant material have low-density, high hydrostatic pressure resistance intensity, low water absorption material property, which is applied to
The preparation of deep-sea instrument and equipment can greatly extend the use environment of deep-sea instrument and equipment.The present invention can solve deep-sea buoyancy
The technical problem that density of material is larger, resistance to hydrostatic pressure intensity is lower reaches the density of material for reducing deep-sea buoyant material, improves resistance to
Hydrostatic pressing intensity, the technical effect for reducing water absorption rate.
In addition, the preparation process of deep-sea buoyant material provided by the invention is relatively simple practical, it is suitable for the big rule of assembly line
Mould production.
Although having used general explanation, specific embodiment and test above, the present invention is described in detail,
But on the basis of the present invention, it can be modified or be improved, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Those skilled in the art will readily occur to of the invention other after considering specification and practice invention here
Embodiment.The present invention is directed to cover any variations, uses, or adaptations of the invention, these modifications, purposes or
Adaptive change follow general principle of the invention and including the undocumented common knowledge in the art of the present invention or
Conventional techniques.It should be understood that the invention is not limited to the accurate knots for being described above and being shown in the accompanying drawings
Structure, and various modifications and changes may be made without departing from the scope thereof.
Claims (9)
1. a kind of preparation method of deep-sea buoyant material, which is characterized in that the described method includes:
Pretreated epoxy resin is added to the agitator of vacuum defoamation blender, then heats the temperature of the agitator
To 80 ~ 90 °C, Xiang Suoshu agitator is added curing agent and carries out uniform stirring；
To the agitator be added modified graphene, adjust the agitator vacuum degree be -0.08 ~ -0.10 atm, continue into
Row is stirring uniformly to obtain mixture；
The mixture is transferred to mold from the agitator, the temperature of the mold is then heated up to 120 ~ 140 °C, is protected
The curing molding of the mixture is completed after 5 ~ 10 h of temperature, then the mixture after curing molding is subjected to cooling demoulding, is made
Standby to obtain deep-sea buoyant material, the density of the deep-sea buoyant material is 0.50 ~ 0.56 g/cm3, resistance to hydrostatic pressure intensity be 115 ~
140 MPa, water absorption rate≤2%；
The mass parts ratio of the pretreated epoxy resin, the curing agent and the modified graphene be 100: 20 ~
40∶1~5。
2. the method according to claim 1, wherein the preparation method of the modified graphene includes:
30 ~ 90 min of ultrasonic disperse is added into dehydrated alcohol in graphene, graphene solution is prepared, the graphene is molten
The mass parts ratio of graphene and dehydrated alcohol is 1 ~ 5: 200 ~ 400 in liquid；
Dehydrated alcohol and deionized water are mixed to form mixed solution, Xiang Suoshu mixed solution adds acetic acid, adjusts the mixing
Then to 3.5 ~ 4.5 silane coupling agent is slowly added dropwise to the mixed solution, by the mixed solution high-speed stirring in the pH value of solution
30 ~ 60 min of dispersion is mixed, silane coupler solution is prepared, dehydrated alcohol, deionized water in the silane coupler solution
Mass parts ratio with silane coupling agent is 100 ~ 200: 20 ~ 60: 0.5 ~ 1.0；
The silane coupler solution is slowly added to the graphene solution and forms reaction solution, is controlled the reaction solution and is existed
4 ~ 8 h are reacted under 70 ~ 90 DEG C of reaction temperature, and the reaction solution is filtered, is dried, modified graphene is prepared.
3. the method according to claim 1, wherein the preprocess method of the epoxy resin includes:
Epoxy resin is warming up to 85 ~ 95 °C, when the epoxy resin is in complete molten condition, epoxy-reactive dilution is added
Agent after stirring evenly 10 ~ 20 min at a temperature of 85 ~ 95 °C, is cooled to 55 ~ 65 °C, pretreated epoxy is prepared
The mass parts ratio of resin, the epoxy resin and the epoxy active diluent is 100: 15 ~ 25.
4. according to the method described in claim 3, it is characterized in that, the epoxy resin contain there are three or four epoxy groups,
The epoxy active diluent contains two epoxy groups.
5. the method according to claim 1, wherein the curing agent is aromatic amine curing agent.
6. according to the method described in claim 2, it is characterized in that, the silane coupling agent is gamma-aminopropyl-triethoxy silicon
At least one of alkane or γ-glycidyl ether oxygen propyl trimethoxy silicane.
7. according to the method described in claim 2, it is characterized in that, the density of the graphene is 0.01 ~ 0.10 g/cm3。
8. the method according to claim 1, wherein the operating pressure for the vulcanizer that curing molding process uses for
10~15 MPa。
9. a kind of deep-sea buoyant material, which is characterized in that the deep-sea buoyant material is by any one shown in claim 1 ~ 8
The preparation method of deep-sea buoyant material is prepared, and the deep-sea buoyant material includes following component and its mass fraction: epoxy
80 ~ 120 parts of resin, 15 ~ 25 parts of epoxy active diluent, 20 ~ 40 parts of curing agent, 1 ~ 5 part of modified graphene, the deep-sea buoyancy
The density of material is 0.50 ~ 0.56 g/cm3, resistance to hydrostatic pressure intensity is 115 ~ 140 MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811423172.4A CN109486116B (en) | 2018-11-27 | 2018-11-27 | Deep sea buoyancy material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811423172.4A CN109486116B (en) | 2018-11-27 | 2018-11-27 | Deep sea buoyancy material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109486116A true CN109486116A (en) | 2019-03-19 |
| CN109486116B CN109486116B (en) | 2021-03-12 |
Family
ID=65696669
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811423172.4A Active CN109486116B (en) | 2018-11-27 | 2018-11-27 | Deep sea buoyancy material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109486116B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732037A (en) * | 2011-04-08 | 2012-10-17 | 中国科学院金属研究所 | Graphene foam/polymer high-conductivity composite material preparation method and application thereof |
| CN103483773A (en) * | 2013-09-24 | 2014-01-01 | 滕州市华海新型保温材料有限公司 | Deep-sea solid buoyancy material and manufacture method thereof |
| CN105566857A (en) * | 2016-03-10 | 2016-05-11 | 四川大学 | Light-weight epoxy resin composite material and preparation method thereof |
| CN107474486A (en) * | 2017-09-13 | 2017-12-15 | 北京理工大学 | A kind of solid buoyancy material and preparation method thereof |
-
2018
- 2018-11-27 CN CN201811423172.4A patent/CN109486116B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732037A (en) * | 2011-04-08 | 2012-10-17 | 中国科学院金属研究所 | Graphene foam/polymer high-conductivity composite material preparation method and application thereof |
| CN103483773A (en) * | 2013-09-24 | 2014-01-01 | 滕州市华海新型保温材料有限公司 | Deep-sea solid buoyancy material and manufacture method thereof |
| CN105566857A (en) * | 2016-03-10 | 2016-05-11 | 四川大学 | Light-weight epoxy resin composite material and preparation method thereof |
| CN107474486A (en) * | 2017-09-13 | 2017-12-15 | 北京理工大学 | A kind of solid buoyancy material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109486116B (en) | 2021-03-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111205597B (en) | High-performance epoxy resin and preparation method thereof | |
| CN106633649B (en) | One kind being suitable for microwave curing resin matrix and preparation method | |
| CN110079052A (en) | It is a kind of with strong microwave-absorbing resin matrix and preparation method thereof | |
| CN107385920B (en) | High-temperature-resistant carbon fiber sizing agent containing graphene oxide and preparation method thereof | |
| CN101709130B (en) | Ultra-low density solid buoyant material and manufacture method | |
| CN110218069A (en) | A kind of water-fast 3D printing gypsum mortar and preparation method thereof | |
| WO2020135779A1 (en) | Solid buoyancy material and preparation method therefor and use thereof | |
| CN103421278A (en) | Low-density high-strength solid buoyancy material and preparation method thereof | |
| CN106893322A (en) | A kind of Graphene/cyanate composite material and its production and use | |
| CN110028763A (en) | The preparation method of low-density high magnification epoxy resin poromerics | |
| CN112812503A (en) | Composite material containing epoxidized hydroxyl-terminated polybutadiene and preparation method thereof | |
| CN102936395A (en) | Method for manufacturing high-strength solid buoyancy material | |
| CN106117980B (en) | A kind of original position self reinforcing resin system and preparation method thereof | |
| CN104448719B (en) | Organic and inorganic hollow microsphere compounded deepwater buoyancy material and preparation method thereof | |
| CN106739397A (en) | The preparation method of high-orientation absorbing material | |
| CN109486116A (en) | A kind of deep-sea buoyant material and preparation method thereof | |
| JPH0554496B2 (en) | ||
| CN103087339A (en) | Method for preparing prepreg through regulating and controlling viscosity of epoxy resin system and fluidity of prepreg by chemorheology | |
| JP5521572B2 (en) | Resin composition for syntactic foam | |
| CN108752871A (en) | A kind of epoxy foams and preparation method thereof | |
| CN108084543A (en) | A kind of polyethylene feed pipe material and preparation method thereof | |
| CN110815619A (en) | Method for producing epoxy resin-based composite material by using ultrasonic mixing | |
| CN109575522A (en) | A kind of epoxy resin is composite porous and its preparation method and application | |
| CN106832791A (en) | A kind of low-density and high-strength structural foam preparation method | |
| RU2584013C1 (en) | Nano-modified epoxy binder for composite materials |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |