CN107141716B - A kind of solid buoyancy material and preparation method thereof - Google Patents
A kind of solid buoyancy material and preparation method thereof Download PDFInfo
- Publication number
- CN107141716B CN107141716B CN201710235577.4A CN201710235577A CN107141716B CN 107141716 B CN107141716 B CN 107141716B CN 201710235577 A CN201710235577 A CN 201710235577A CN 107141716 B CN107141716 B CN 107141716B
- Authority
- CN
- China
- Prior art keywords
- solid buoyancy
- hollow glass
- stirring
- buoyancy material
- added
- 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.)
- Active
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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
-
- 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
- C08G59/4007—Curing agents not provided for by the groups C08G59/42 - C08G59/66
- C08G59/4014—Nitrogen containing compounds
- C08G59/4028—Isocyanates; Thioisocyanates
-
- 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
- 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
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
-
- 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
- C08G59/56—Amines together with other curing agents
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
Abstract
The present invention relates to a kind of solid buoyancy materials and preparation method thereof, epoxy resin after vacuum dehydration is added in double planetary mixers, it is warming up to 40~60 DEG C, powdered aromatic amine curing agent is added, at such a temperature, it vacuumizes while stirring, vacuum degree is maintained at -0.094~-0.10MPa, so that mixed liquor becomes limpid；Vacuum is removed, active epoxy diluent, blocked polyisocyanate class compound and coupling agent stirring are added under stirring so that system temperature is uniform；Hollow glass micropearl is added portionwise, and under vacuum conditions, is uniformly mixed；It opens double planetary mixers and takes out mixture, put it into the Guan Bi mould for being previously heated to 80~100 DEG C, be compacted and fasten mold, solidify to get solid buoyancy material.Compared with prior art, the present invention consumes the part of hydroxyl in cured product, and the amount of the residual hydroxyl after reducing epoxy resin cure increases the intensity of matrix resin, reduces the increased risk of long-time material water absorption rate.
Description
Technical field
The present invention relates to composite materials, more particularly, to a kind of solid buoyancy material and preparation method thereof.
Background technique
Solid buoyancy material be a kind of low-density, high intensity, low water absorption composite material, can be deep diving towed body, depth
Latent device and underwater equipment etc. provide the net buoyancy and payload when underwater operation floats, and guarantee that the underwater operations such as bathyscaph are set
Standby resistance to pressure and structural stability.Solid buoyancy material is the weight of a kind of important ocean engineering material and underwater equipment
Component part is wanted, gradually plays increasingly important role in ocean engineering application field.
The development in external solid buoyancy material field is started in the 1960s, being widely used to military, section at present
It grinds and commercial field.The solid buoyancy material of foreign countries' exploitation, mainly with light filler and the high-intensitive compound preparation of matrix resin
Based on pure syntactic foam.The deep diving buoyant material that foreign countries are developed, density is generally in 0.4~0.6g/cm3, pressure resistance
Degree then between 40~100MPa, covers the demand of most deep ocean works substantially.
The research that the country carries out solid buoyancy material is since the 1980s.Application No. is in 85106037
The hollow float bead that extracts is as packing material in the fine coal dust that state's patent of invention is discarded using power plant, uses epoxy resin as gluing
It connects agent and is prepared for a kind of buoyant material, density of material 0.6g/cm3, compressive resistance 6MPa, dive under water depth 500m.Application No. is
200610043524.4 Introduction To Cn Patent one kind using epoxy resin as matrix, using hollow glass bead be filler stirring
Even to be placed in pressure-cure machine, Pressurized-heated solidifies and solid buoyancy material is made, such density of material is 0.5g/cm3Left and right
When, compressive resistance is about 12.5MPa, density 0.6g/cm3Solid buoyancy material can apply to 5800m deepwater work.
The preparation of country's solid buoyancy material mainly uses epoxy resin as matrix resin at present, is made using amine or acid anhydrides
For curing agent, a large amount of hydroxyl or ester bond are generated in the molecular structure of the epoxy resin after solidification, there are long-time water absorption rates
The problem of increasing or causing performance to decline because of hydrolysis of ester group；On the other hand, high performance solid buoyancy material in order to obtain, is adopted more
Use aromatic amine as curing agent, but the usual fusing point of such curing agent is higher, during the preparation process, needs first through high temperature
Then melting is mixed with epoxy resin again, which increases operation difficulty, shortens the operating time.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of solid buoyancy materials
And preparation method thereof.
The present invention is using hollow glass micropearl as density-adjusting media, and using epoxy resin as matrix resin, closure is added
Polyisocyanates is that auxiliary curing agent is put into mold after double planetary mixers mix and is consolidated using new process
Change, solid buoyancy material is prepared.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of solid buoyancy material, composed of the following components:
The epoxy resin is bisphenol A type epoxy resin, and epoxide number is between 0.40~0.60mol/100g, preferably
Be 0.48~0.56mol/100g.
The active epoxy diluent is selected from the mixture of one or more of following substance:
Benzyl glycidyl ether containing an epoxy group in structure, containing there are two the contractings of the neopentyl glycol two of epoxy group
Water glycerin ether, or containing there are three 4,5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl esters of epoxy group.
The aromatic amine curing agent is selected from one of two aminodiphenylmethane or two amido diphenyl sulfones.
The blocked polyisocyanate class compound is the closed methyl diphenylene diisocyanate of caprolactam.
The coupling agent is KH-550.
The hollow glass micropearl is the hollow glass micropearl that commercially available average grain diameter is 20~60 μm.
A kind of preparation method of solid buoyancy material, comprising the following steps:
(1) epoxy resin after vacuum dehydration is added in double planetary mixers, is warming up to 40~60 DEG C, is added powdered
Aromatic amine curing agent vacuumizes while stirring at such a temperature, and vacuum degree is maintained at -0.094~-0.10MPa, so that
Mixed liquor becomes limpid；
(2) remove vacuum, under stirring be added active epoxy diluent, blocked polyisocyanate class compound and
Coupling agent stirs so that system temperature is uniform；
(3) hollow glass micropearl is added portionwise, and under vacuum conditions, is uniformly mixed；
(4) double planetary mixers are opened and takes out mixture, put it into and be previously heated to 80~100 DEG C of Guan Bi mould
In, it is compacted and is fastened mold, is solidified to get solid buoyancy material.
Epoxy resin carries out vacuum dehydration by the following method: in the container equipped with stirring and vacuum evacuation device, being added
Epoxy resin stirring heating, and maintain vacuum degree in -0.094~-0.10MPa, temperature keeps 1h under the conditions of being 100~110 DEG C,
Vacuum dehydration is carried out, after dehydration, cooling down, is sealed spare while stirring.
Hollow glass bead is using preceding having carried out cleaning treatment, cleaning method are as follows: it is molten that hollow glass bead is poured into alkalinity
1~2h is rinsed in liquid, is cleaned hollow glass micropearl at least three times with deionized water, hollow glass micropearl is cleaned two again with ethyl alcohol
All over rear drying, save backup the hollow glass micropearl handled well is closed.
Compared with prior art, solid buoyancy material of the invention has the advantage that
1) operation temperature is lower in solid buoyancy material forming process, and operation is easy.
2) technology of preparing of existing solid buoyancy material, mainly using epoxy resin as matrix, solidification process is as follows:
It can be seen that a large amount of hydroxyl is formd during curing reaction, because hydroxyl easily forms hydrogen bond with hydrone,
To make material water imbibition enhance.Case type diisocyanate curing agent can unseal in Curing Process of Epoxy
Isocyanate group out, isocyanate group react to form carbamate groups with the hydroxyl in epoxy resin, to consume solidification
Part of hydroxyl in product, the amount of the residual hydroxyl after reducing epoxy resin cure increase the intensity of matrix resin, reduce
Long-time material water absorption rate increased risk.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1
Compound concentration is the sodium hydroxide solution of 0.1mol/L, is 40 μm or so by average grain diameter, density 0.38g/
cm3, compressive strength be 38MPa hollow glass micropearl pour into sodium hydroxide solution, 1h is rinsed under gentle agitation, is then taken out
Filter, removes sodium hydroxide solution, and then cleans hollow glass micropearl deionized water three times under gentle agitation state, takes out
Filter, then cleaned hollow glass micropearl again twice under gentle agitation with ethyl alcohol, it is dried after suction filtration, the hollow glass that will be handled well
Microballon is placed on closed in polybag save backup.
In the container equipped with stirring and vacuum evacuation device, the epoxy resin that epoxide number is 0.54mol/100g is added and stirs
Heating, when temperature reaches 60 DEG C, starts to vacuumize, vacuum degree is opened in -0.094~-0.10MPa when temperature reaches 100 DEG C
Beginning timing carries out vacuum dehydration in 100~110 DEG C of holding 1h.After dehydration, cooling down, is sealed spare while stirring.
It is sieved, seals standby by aromatic amine curing agent two aminodiphenylmethane grind into powder, and with 100 mesh screens
With.
By in 100 parts of addition double planetary mixers of above-mentioned epoxy resin, 40 DEG C are warming up to, powdered diamines is then added
It 25 parts of base diphenyl methane, at a temperature of 40~50 DEG C, vacuumizing while stirring, vacuum degree is maintained at -0.094~-
0.10MPa, so that mixed liquor becomes limpid.Then vacuum is removed, temperature is increased to 60~70 DEG C, is added and lives under stirring
10 parts of property epoxide diluent neopentylglycol diglycidyl ether, 10 parts of the closed methyl diphenylene diisocyanate of caprolactam and
It 4 parts of KH-550 coupling agent, stirs uniform to system temperature；100 parts of hollow glass micropearl are finally added portionwise, and in vacuum shape
Under state, it is uniformly mixed.It opens double planetary mixers and takes out mixture, put it into and be previously heated to 80 DEG C of Guan Bi mould
In, it is compacted and fastens mold.After 80 DEG C of solidification 2h, 130 DEG C of solidification 2h, 150 DEG C of solidification 3h, naturally cool to mold temperature
Room temperature demoulds up to solid buoyancy material.
Resulting solid buoyancy material, actual density 0.576g/cm3, resistance to hydrostatic pressure 75MPa, under the hydrostatic pressing for 24 hours
Water absorption rate < 0.9%.
Embodiment 2
It is 20 μm or so that hollow glass micropearl, which selects average grain diameter, density 0.46g/cm3, compressive strength be 114MPa
Hollow glass micropearl, cleaning and drying process such as embodiment 1.
In the container equipped with stirring and vacuum evacuation device, the epoxy resin that epoxide number is 0.54mol/100g is added and stirs
Heating, when temperature reaches 60 DEG C, starts to vacuumize, vacuum degree is opened in -0.094~-0.10MPa when temperature reaches 100 DEG C
Beginning timing carries out vacuum dehydration in 100~110 DEG C of holding 1h.After dehydration, cooling down, is sealed spare while stirring.
It is sieved, seals spare by two amido diphenyl sulfone grind into powder of aromatic amine curing agent, and with 100 mesh screens.
By in 100 parts of addition double planetary mixers of above-mentioned epoxy resin, 60 DEG C are warming up to, powdered diamines is then added
It 30 parts of base diphenyl sulfone, at a temperature of 60~70 DEG C, vacuumizing while stirring, vacuum degree is maintained at -0.094~-0.10MPa,
So that mixed liquor becomes limpid.Then vacuum is removed, keeps the temperature at 70 DEG C, it is new that active epoxy diluent is added under stirring
15 parts of the closed methyl diphenylene diisocyanate of 20 parts of neopentyl glycol diglycidyl glycerin ether, caprolactam and KH-550 coupling agent 6
Part, it stirs uniform to system temperature；180 parts of above-mentioned hollow glass micropearl is finally added portionwise, and under vacuum conditions, stirs
It is uniformly mixed.It opens double planetary mixers and takes out mixture, put it into the Guan Bi mould for being previously heated to 80 DEG C, compacting is simultaneously
Fasten mold.After 100 DEG C of solidification 2h, 160 DEG C of solidification 2h, 200 DEG C of solidification 3h, mold temperature is made to naturally cool to room temperature, taken off
Mould is up to solid buoyancy material.
Resulting solid buoyancy material, actual density 0.687g/cm3, resistance to hydrostatic pressure 120MPa, under the hydrostatic pressing
Water absorption rate < 0.9% for 24 hours.
Embodiment 3
It is composed of the following components the present embodiment provides a kind of novel solid buoyant material:
The solid buoyancy material of the present embodiment is prepared according to following procedure:
(1) compound concentration is the sodium hydroxide solution of 0.1mol/L, and hollow glass bead is poured into alkaline solution and is rinsed
1h is cleaned hollow glass micropearl at least three times with deionized water, is dried after hollow glass micropearl is cleaned twice again with ethyl alcohol, will
The hollow glass micropearl handled well is placed on closed in polybag save backup；
(2) in the container equipped with stirring and vacuum evacuation device, the epoxy resin stirring heating is added, when temperature reaches
When to 60 DEG C, start to vacuumize, vacuum degree starts timing when temperature reaches 100 DEG C -0.094, keeps at 100~110 DEG C
1h carries out vacuum dehydration.After dehydration, cooling down, is sealed spare while stirring；
(3) it by the aromatic amine curing agent grind into powder, and is sieved, is sealed spare with 80 mesh screens；
(4) above-mentioned epoxy resin is added in double planetary mixers, is warming up to 40 DEG C, powdered solidification is then added
Agent vacuumizes while stirring at such a temperature, and vacuum degree is maintained at -0.094MPa, so that mixed liquor becomes limpid.Then it removes
Active epoxy diluent, blocked polyisocyanate class compound and coupling agent, stirring to body is added in vacuum under stirring
It is that temperature is uniform；Hollow glass micropearl is finally added portionwise, and under vacuum conditions, is uniformly mixed.Open double-planet
Mixer takes out mixture, puts it into the Guan Bi mould for being previously heated to 80 DEG C, is compacted and fastens mold.Solidification to get
Solid buoyancy material of the invention.
Resulting solid buoyancy material, actual density 0.438g/cm3, resistance to hydrostatic pressure 35MPa, under the hydrostatic pressing for 24 hours
Water absorption rate < 0.9%.
Embodiment 4
It is composed of the following components the present embodiment provides a kind of novel solid buoyant material:
The solid buoyancy material of the present embodiment is prepared according to following procedure:
(1) compound concentration is the sodium hydroxide solution of 0.1mol/L, and hollow glass bead is poured into and rinses 2 in alkaline solution
Hour, it is cleaned hollow glass micropearl at least three times with deionized water, is dried after hollow glass micropearl is cleaned twice again with ethyl alcohol,
The hollow glass micropearl handled well is placed on closed in polybag save backup；
(2) in the container equipped with stirring and vacuum evacuation device, the epoxy resin stirring heating is added, when temperature reaches
When to 60 DEG C, start to vacuumize, vacuum degree starts timing when temperature reaches 100 DEG C in -0.10MPa, protects at 100~110 DEG C
1h is held, vacuum dehydration is carried out.After dehydration, cooling down, is sealed spare while stirring；
(3) it by the aromatic amine curing agent grind into powder, and is sieved, is sealed spare with 120 mesh screens；
(4) above-mentioned epoxy resin is added in double planetary mixers, is warming up to 60 DEG C, powdered solidification is then added
Agent vacuumizes while stirring at such a temperature, and vacuum degree is maintained at -0.10MPa, so that mixed liquor becomes limpid.Then removal is true
Active epoxy diluent, blocked polyisocyanate class compound and coupling agent, stirring to system is added in sky under stirring
Temperature is uniform；Hollow glass micropearl is finally added portionwise, and under vacuum conditions, is uniformly mixed.It is mixed to open double-planet
Clutch takes out mixture, puts it into the Guan Bi mould for being previously heated to 100 DEG C, is compacted and fastens mold.Solidification is to get this
The solid buoyancy material of invention.
Resulting solid buoyancy material, actual density 0.687g/cm3, resistance to hydrostatic pressure 120MPa, under the hydrostatic pressing
Water absorption rate < 0.9% for 24 hours.
Embodiment 5
It is composed of the following components the present embodiment provides a kind of novel solid buoyant material:
The solid buoyancy material of the present embodiment is prepared according to following procedure:
(1) compound concentration is the sodium hydroxide solution of 0.1mol/L, and hollow glass bead is poured into alkaline solution and is rinsed
1.5h is cleaned hollow glass micropearl at least three times with deionized water, is dried after hollow glass micropearl is cleaned twice again with ethyl alcohol,
The hollow glass micropearl handled well is placed on closed in polybag save backup；
(2) in the container equipped with stirring and vacuum evacuation device, the epoxy resin stirring heating is added, when temperature reaches
When to 60 DEG C, start to vacuumize, vacuum degree starts timing when temperature reaches 100 DEG C in -0.096MPa, at 100~110 DEG C
1h is kept, vacuum dehydration is carried out.After dehydration, cooling down, is sealed spare while stirring；
(3) it by the aromatic amine curing agent grind into powder, and is sieved, is sealed spare with 100 mesh screens；
(4) above-mentioned epoxy resin is put into double planetary mixers, is warming up to 50 DEG C, powdered solidification is then added
Agent vacuumizes while stirring at such a temperature, and vacuum degree is maintained at -0.096MPa, so that mixed liquor becomes limpid.Then it removes
Active epoxy diluent, blocked polyisocyanate class compound and coupling agent, stirring to body is added in vacuum under stirring
It is that temperature is uniform；Hollow glass micropearl is finally added portionwise, and under vacuum conditions, is uniformly mixed.Open double-planet
Mixer takes out mixture, puts it into the Guan Bi mould for being previously heated to 90 DEG C, is compacted and fastens mold.Solidification to get
Solid buoyancy material of the invention.
Resulting solid buoyancy material, actual density 0.562g/cm3, resistance to hydrostatic pressure 70MPa, under the hydrostatic pressing for 24 hours
Water absorption rate < 0.9%.
In above embodiments, density measurement is carried out using drainage.
Water absorption rate test method under hydrostatic pressing are as follows: at normal temperature, accurately weigh the quality m of sample0, then by the sample
It is placed in the hydrostatic pressure bucket that medium is distilled water, pressurization makes pressure in bucket rise to required pressure, and keep at this pressure
For 24 hours, then pressure release takes out sample to normal pressure from water, and wipes the moisture of specimen surface with paper handkerchief immediately, and weigh sample
Quality m1.Water absorption rate is calculated according to the following formula:
Water absorption rate (%)=(m1-m0)×100/m0
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (7)
1. a kind of solid buoyancy material, which is characterized in that the solid buoyancy material is composed of the following components:
The epoxy resin, is bisphenol A type epoxy resin, and the blocked polyisocyanate class compound is caprolactam
Closed methyl diphenylene diisocyanate；
The aromatic amine curing agent is selected from one of two aminodiphenylmethane or two amido diphenyl sulfones.
2. a kind of solid buoyancy material according to claim 1, which is characterized in that the active epoxy diluent is selected from
Benzyl glycidyl ether, neopentylglycol diglycidyl ether or 4, in 5- 7-oxa-bicyclo[4.1.0-1,2- dicarboxylic acid diglycidyl ester
One or more.
3. a kind of solid buoyancy material according to claim 1, which is characterized in that the coupling agent is KH-550.
4. a kind of solid buoyancy material according to claim 1, which is characterized in that the hollow glass micropearl is commercially available
Average grain diameter be 20~60 μm of hollow glass micropearl.
5. a kind of preparation method of solid buoyancy material as described in claim 1, which comprises the following steps:
(1) epoxy resin after vacuum dehydration is added in double planetary mixers, is warming up to 40~60 DEG C, powdered fragrance is added
Race's amine curing agent vacuumizes while stirring at such a temperature, and vacuum degree is maintained at -0.094~-0.10MPa, so that mixing
Liquid becomes limpid；
(2) vacuum is removed, active epoxy diluent, blocked polyisocyanate class compound and coupling are added under stirring
Agent, stirring keep system temperature uniform；
(3) hollow glass micropearl is added portionwise, and under vacuum conditions, is uniformly mixed；
(4) double planetary mixers are opened and take out mixture, added it in the Guan Bi mould for being preheating to 80~100 DEG C in advance,
It is compacted and is fastened mold, is solidified to get solid buoyancy material.
6. a kind of preparation method of solid buoyancy material according to claim 5, which is characterized in that epoxy resin by with
Lower method carries out vacuum dehydration:
In the container equipped with stirring and vacuum evacuation device, epoxy resin stirring heating is added, and maintain vacuum degree -0.094
~-0.10MPa, temperature keep 1h under the conditions of being 100~110 DEG C, carry out vacuum dehydration, after dehydration, cool down while stirring
It is cooling, it seals spare.
7. a kind of preparation method of solid buoyancy material according to claim 5, which is characterized in that hollow glass bead makes
With preceding having carried out cleaning treatment, cleaning method are as follows:
Hollow glass bead is poured into 1~2h of rinsing in alkaline solution, is cleaned hollow glass micropearl at least three times with deionized water,
It dries after hollow glass micropearl is cleaned twice again with ethyl alcohol, saves backup the hollow glass micropearl handled well is closed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710235577.4A CN107141716B (en) | 2017-04-12 | 2017-04-12 | A kind of solid buoyancy material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710235577.4A CN107141716B (en) | 2017-04-12 | 2017-04-12 | A kind of solid buoyancy material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107141716A CN107141716A (en) | 2017-09-08 |
| CN107141716B true CN107141716B (en) | 2019-10-15 |
Family
ID=59773533
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710235577.4A Active CN107141716B (en) | 2017-04-12 | 2017-04-12 | A kind of solid buoyancy material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107141716B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108587070A (en) * | 2018-05-25 | 2018-09-28 | 潘荣强 | A kind of lightweight buoyancy material and preparation method thereof |
| CN110540706B (en) * | 2019-09-05 | 2022-06-10 | 上海阿莱德实业股份有限公司 | Preparation method of heat-conducting interface material |
| CN110628180B (en) * | 2019-09-26 | 2021-01-29 | 海洋化工研究院有限公司 | Solid buoyancy material and preparation method thereof |
| CN114957920A (en) * | 2022-06-20 | 2022-08-30 | 安徽众博新材料有限公司 | Preparation method of low-density epoxy resin buoyancy material |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101735566B (en) * | 2009-12-05 | 2011-08-10 | 海洋化工研究院 | Processable full sea-depth buoyancy material and manufacture method |
| CN103013050B (en) * | 2012-12-28 | 2016-04-06 | 青岛海洋新材料科技有限公司 | A kind of solid buoyancy material and manufacture method thereof |
| CN105566854A (en) * | 2015-12-04 | 2016-05-11 | 常州百思通复合材料有限公司 | Epoxy resin composition with special curing characteristics and composite thereof |
-
2017
- 2017-04-12 CN CN201710235577.4A patent/CN107141716B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107141716A (en) | 2017-09-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107141716B (en) | A kind of solid buoyancy material and preparation method thereof | |
| CN106866933B (en) | A kind of solid buoyancy material and preparation method thereof | |
| CN102702679B (en) | Preparation method for high-strength solid buoyancy material for deep submergence | |
| CN106893261B (en) | A kind of high-strength light porous metals composite damping material and preparation method thereof | |
| EP0574247B1 (en) | Open-cell porous material, method for preparing the material and mold for pressure-cast-molding ceramic article formed from the material | |
| CN101735566B (en) | Processable full sea-depth buoyancy material and manufacture method | |
| CN107446502B (en) | Self-repairing water-based epoxy/asphalt composite waterproof coating and preparation method thereof | |
| CN109749616A (en) | A kind of anti-fouling coating and preparation method thereof that can discharge anti-fouling agent | |
| US9522843B2 (en) | Apparatus and method for fabricating microcontainers | |
| CN109942314A (en) | A method of porous alumina ceramic is prepared using polyurethane | |
| CN103724985B (en) | A kind of hollow ceramic microspheres fills the preparation method of epoxy modified polyurethane | |
| CN103442828B (en) | For the production of the precast body of foam metal | |
| CN106497310A (en) | A kind of preparation method of high-cooling property machinery coating | |
| CN103497475B (en) | A kind of fiberglass and preparation method thereof | |
| CN110964216B (en) | ANF (artificial neural fiber) -reinforced HEC (high-energy carbon) film composite material and preparation method thereof | |
| CN109021897A (en) | A kind of adhesive and its application method | |
| CN107629753A (en) | Water process curtain type film assembly polyurethane pouring sealant and preparation method thereof | |
| CN101234300A (en) | Method for preparing polyvinylidene fluoride microporous filtering film | |
| CN108296477A (en) | A kind of 3D printing precoated sand and preparation method thereof | |
| CN114988775A (en) | Self-repairing high-performance concrete | |
| CN111021068B (en) | Impregnation treatment technology for impregnated aramid fiber ropes for polyurethane synchronous belt | |
| CN211842748U (en) | Environment-friendly epoxy recovery unit | |
| CN107376859A (en) | A kind of glutaraldehyde cross-linking chitosan/nickel hydroxide microballoon compound adsorbent preparation method | |
| CN210543515U (en) | Laboratory is with epoxy glue effectively bubble removal device | |
| CN114133836A (en) | Microcapsule type self-repairing fusion bonding epoxy coating and preparation method thereof |
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 | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 200437 No. 99, Handan Road, Shanghai, Hongkou District Patentee after: Shanghai Material Research Institute Co.,Ltd. Address before: 200437 No. 99, Handan Road, Shanghai, Hongkou District Patentee before: SHANGHAI Research Institute OF MATERIALS |
|
| CP01 | Change in the name or title of a patent holder |