CN108329656B - High-toughness solid buoyancy material containing elastic microspheres and preparation method thereof - Google Patents
High-toughness solid buoyancy material containing elastic microspheres and preparation method thereof Download PDFInfo
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- CN108329656B CN108329656B CN201810018626.3A CN201810018626A CN108329656B CN 108329656 B CN108329656 B CN 108329656B CN 201810018626 A CN201810018626 A CN 201810018626A CN 108329656 B CN108329656 B CN 108329656B
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K2003/2237—Oxides; Hydroxides of metals of titanium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The high-toughness solid buoyancy material containing elastic microspheres is prepared from 100 parts by mass of epoxy resin, 0-20 parts by mass of reactive diluent, 60-120 parts by mass of curing agent, 0-1 part by mass of accelerator, 0-20 parts by mass of toughening agent and 10-100 parts by mass of elastic microspheres. The elastic microspheres coated with the inorganic shell are used as the filler of the solid buoyancy material, so that the toughness of the final product is greatly improved, and the pressure resistance and the heat resistance of the final product are improved to a certain extent; meanwhile, after the surface modifier is added, the surface modification can be simultaneously carried out on the matrix resin and the elastic microspheres, so that the binding force between the inorganic matter shell on the surfaces of the elastic microspheres and the epoxy resin matrix is improved, and the overall toughness of the solid buoyancy material is improved.
Description
Technical Field
The invention relates to the field of characteristic engineering materials for marine environments, in particular to a high-toughness solid buoyancy material containing elastic microspheres and a preparation method thereof.
Background
With the vigorous development of ocean economy, China puts forward brand new requirements on further deep development of ocean. As an important marine special engineering material, the solid buoyancy material is widely applied to marine development equipment such as underwater robots, deep submergence vehicles, submerged buoy systems, underwater mining collectors, marine oil exploration and development marine risers and the like. The solid buoyancy material has low density, high compression strength, difficult water absorption and good corrosion resistance, and is a typical structure function integrated material.
At present, the solid buoyancy material is mainly prepared by taking liquid epoxy resin as a matrix and hollow glass beads as a filler through the processes of blending, mould pressing, curing and the like. Although the material has high compressive strength, the material still belongs to a brittle material, and is easy to be collided or impacted during the processes of transportation, installation and use after production so as to be damaged. Therefore, it is required to improve the toughness of the material to ensure safety during long-term use.
Chinese patent CN1844236 describes a method of improving the toughness of epoxy resin matrix by adding toughening modifier such as polysulfide rubber, liquid nitrile rubber or butyl hydroxyl to improve the overall toughness of the material. However, the hollow glass beads with poor toughness are the only fillers with large mass portion ratio, so the performance improvement is not obvious.
Chinese patent CN103172975 describes a method of improving the toughness of a material by using surface-modified ultra-high molecular weight polyethylene particles and hollow glass beads as a filler. The toughness of the buoyancy material prepared by the method is improved to a certain extent, but the hollow glass beads with poor toughness still occupy a main proportion in the filler, so that the performance is improved slightly.
Chinese patent CN106380786 describes a method of improving the overall toughness of a material by using hollow microspheres and foamed microspheres as fillers. The method mainly utilizes the thermal expansion of the foaming microspheres to reduce the density, improves the toughness by virtue of the thermoplastic spherical wall of the foaming microspheres, improves the toughness of the material to a certain extent, but the foaming microspheres deform seriously when the material is subjected to post-curing (generally higher than 100 ℃), so that more defects appear inside the material and the compressive strength is greatly influenced.
Chinese patent CN103665768 introduces a method of improving the overall toughness of the material by using hollow microspheres and fiber beads as a filler and polyether, nitrile rubber, polybutadiene and the like as toughening modified resin matrixes. The toughness of the buoyancy material prepared by the method is greatly improved compared with that of a pure buoyancy material, but the diameter and rigidity of the fiber pellets are large, and the specific surface area of the fiber pellets is far smaller than that of the hollow microspheres, so that interface damage is easy to occur when the material is pressed.
The above patents all adopt hollow glass microspheres or hollow microspheres as fillers to produce the solid buoyancy material, but the toughness of the finished solid buoyancy material product produced finally is not ideal due to the poor toughness of the hollow glass microspheres or hollow microspheres.
Disclosure of Invention
In order to solve the problem that the toughness of a product is not ideal due to the fact that hollow glass microspheres are used as fillers in a solid buoyancy material in the prior art, the invention provides a high-toughness solid buoyancy material containing elastic microspheres and a preparation method thereof, wherein the elastic microspheres coated with inorganic shells are used as the fillers of the solid buoyancy material, so that the toughness of the final product is greatly improved, and the pressure resistance and the heat resistance of the final product are also improved to a certain extent; meanwhile, after the surface modifier is added, the surface modification can be simultaneously carried out on the matrix resin and the elastic microspheres, so that the binding force between the inorganic matter shell on the surfaces of the elastic microspheres and the epoxy resin matrix is improved, and the overall toughness of the solid buoyancy material is improved.
The technical scheme adopted by the invention for solving the technical problems is as follows: a high-toughness solid buoyancy material containing elastic microspheres is prepared from 100 parts of epoxy resin, 0-20 parts of reactive diluent, 60-120 parts of curing agent, 0-1 part of accelerator, 0-20 parts of toughening agent and 10-100 parts of elastic microspheres in percentage by mass.
As another preferred embodiment of the present invention, the epoxy resin is a bisphenol a type epoxy resin or a bisphenol F type epoxy resin, and one of the designations E44, E51, E54, 170 may be used.
As another preferred embodiment of the present invention, the reactive diluent is Allyl Glycidyl Ether (AGE), Butyl Glycidyl Ether (BGE), diglycidyl aniline (DGA) or butanediol diglycidyl ether (BDGE), and the functions of the reactive diluent are to reduce the viscosity of the epoxy resin, improve the fluidity of the resin, increase the amount of the filler of the elastic beads, and reduce the density of the high-toughness solid buoyancy material.
As another preferred embodiment of the present invention, the curing agent is an acid anhydride-based or amine-based curing agent used in combination with the epoxy resin, such as methyltetrahydrophthalic anhydride, methylnadic anhydride, dodecenylsuccinic anhydride, low molecular weight polyamide 650, or aromatic polyamine DDM;
as another preferred embodiment of the present invention, the accelerator is imidazole or tertiary amine accelerator used in combination with the curing agent, and may be selected from one of 2-ethyl-4-methylimidazole, 1-benzyl-2-ethylimidazole, 1-aminoethyl-2-methylimidazole, DMP-30 or benzyldimethylamine.
As another preferred embodiment of the invention, the toughening agent is one or a mixture of several of liquid carboxyl-terminated nitrile rubber (CTBN), epoxy-terminated nitrile rubber (ETBN), polysulfide rubber, polyether ether ketone (PEEK) and polyether sulfone (PES) in any proportion.
As another preferred embodiment of the invention, the high-toughness solid buoyancy material further comprises 0-20 parts of a surface modifier, wherein the surface modifier is one or a mixture of several of a JN114 titanate coupling agent, a KH560 silane coupling agent, a 414 aluminate coupling agent and a lauryl alcohol ether phosphate anionic surfactant in any proportion.
The preparation method of the high-toughness solid buoyancy material containing the elastic microspheres comprises the following steps:
1) weighing the materials according to the proportion for later use;
2) mixing the other components except the elastic microspheres uniformly at normal temperature to prepare a resin glue solution for later use;
3) adding the elastic microspheres weighed in the step 1) into the resin glue solution prepared in the step 2), and uniformly mixing at a rotating speed of 25-50r/min to obtain a raw material mixture for later use;
4) feeding the raw material mixture prepared in the step 3) into a mold, molding under the pressure of 5-20MPa, curing at 80-100 ℃ for not less than 48 hours after molding, and demolding to obtain a blank for later use;
5) re-curing the blank obtained in the step 4) at the temperature of 120-140 ℃ for not less than 24h, and naturally cooling after curing to obtain the product.
Compared with the traditional hollow glass microspheres, the elastic microspheres coated with the inorganic shell have the advantages that the toughness is greatly improved under the same density, the pressure resistance and the heat resistance are far higher than those of the common polymer microspheres coated with the organic shell, and the condition that the size of the polymer microspheres is deformed to cause internal defects can not occur when the material is subjected to necessary post-curing; the average particle diameter is 10-120 μm, and the density is 0.10-0.20g/cm3And one or more of calcium carbonate, talcum or titanium oxide coated acrylonitrile-based polymer microspheres with compressive strength of 10-20 MPa.
In the invention, the active diluent has the functions of reducing the viscosity of the epoxy resin, improving the fluidity of the resin, increasing the filling amount of the elastic microspheres and reducing the density of the high-toughness solid buoyancy material; the toughening agent improves the overall toughness of the buoyancy material from the perspective of modifying matrix resin; the surface modifier improves the integral toughness of the buoyancy material by improving the binding force between the inorganic matter shell on the surface of the elastic microsphere and the epoxy resin matrix.
Compared with the prior art, the invention has the following beneficial effects:
1) the elastic microspheres coated with the inorganic shell are used as the filler of the solid buoyancy material, so that the toughness of the final product is greatly improved, and the pressure resistance and the heat resistance of the final product are improved to a certain extent;
2) the surface modifier is added, so that the surface modification can be simultaneously carried out on the matrix resin and the elastic microspheres, and the binding force between the inorganic matter shell on the surfaces of the elastic microspheres and the epoxy resin matrix is further improved, so that the overall toughness of the solid buoyancy material is improved;
3) through detection, the product of the invention not only maintains the low density (0.45-0.55 g/cm) of the solid buoyancy material3) High strength (20-40 MPa) and low water absorption (not more than 1%), and greatly improves the toughness of the material (the elongation at break reaches 6-8%).
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The high-toughness solid buoyancy material containing the elastic microspheres is prepared from 100 parts of epoxy resin, 60 parts of curing agent and 10 parts of elastic microspheres according to mass percentage, wherein the epoxy resin is E51, the curing agent is aromatic polyamine DDM, the toughening agent is liquid carboxyl-terminated butadiene-acrylonitrile rubber, and the elastic microspheres are 40 micrometers in average particle size and 0.20g/cm in density3The calcium carbonate coats the acrylonitrile polymer microspheres;
the preparation method comprises the following steps:
1) weighing the materials according to the proportion for later use;
2) mixing the other components except the elastic microspheres uniformly at normal temperature to prepare a resin glue solution for later use;
3) adding the elastic microspheres weighed in the step 1) into the resin glue solution prepared in the step 2), and uniformly mixing at a rotating speed of 25r/min to obtain a raw material mixture for later use;
4) feeding the raw material mixture prepared in the step 3) into a mold, molding under the pressure of 5MPa, curing at the temperature of 80 ℃ for 58h after molding, and demolding to obtain a blank for later use;
5) and (3) curing the blank obtained in the step 4) at the temperature of 120 ℃ for 30h again, and naturally cooling to obtain the product.
Example 2
A high-toughness solid buoyancy material containing elastic microspheres is prepared from 100 parts of epoxy resin, 20 parts of reactive diluent, 120 parts of curing agent, 1 part of accelerator, 20 parts of toughening agent and 100 parts of elastic microspheres in percentage by massWherein the epoxy resin is E54, the active diluent is AGE, the curing agent is dodecenyl succinic anhydride, the accelerator is 2-ethyl-4-methylimidazole, the flexibilizer is epoxy-terminated butadiene-acrylonitrile rubber, the elastic microspheres are 80 microns in average particle size and 0.20g/cm in density3The talc coats the acrylonitrile polymer microspheres;
the preparation method comprises the following steps:
1) weighing the materials according to the proportion for later use;
2) mixing the other components except the elastic microspheres uniformly at normal temperature to prepare a resin glue solution for later use;
3) adding the elastic microspheres weighed in the step 1) into the resin glue solution prepared in the step 2), and uniformly mixing at a rotating speed of 50r/min to obtain a raw material mixture for later use;
4) feeding the raw material mixture prepared in the step 3) into a mold, molding under the pressure of 20MPa, curing at the temperature of 100 ℃ for 86 hours after molding, and demolding to obtain a blank for later use;
5) and (3) curing the blank obtained in the step 4) at the temperature of 140 ℃ for 48h, and naturally cooling to obtain the product.
Example 3
The high-toughness solid buoyancy material containing the elastic microspheres is prepared from 100 parts of epoxy resin, 10 parts of reactive diluent, 90 parts of curing agent, 0.5 part of accelerator, 10 parts of toughening agent and 55 parts of elastic microspheres according to mass percentage, wherein the epoxy resin is No. 170 epoxy resin, the reactive diluent is DGA, the curing agent is low-molecular polyamide 650, the accelerator is DMP-30, the toughening agent is polyether ether ketone, the elastic microspheres are 120 micrometers in average particle size and 0.15g/cm in density3The titanium oxide of (2) coats the acrylonitrile polymer microspheres;
the preparation method comprises the following steps:
1) weighing the materials according to the proportion for later use;
2) mixing the other components except the elastic microspheres uniformly at normal temperature to prepare a resin glue solution for later use;
3) adding the elastic microspheres weighed in the step 1) into the resin glue solution prepared in the step 2), and uniformly mixing at a rotating speed of 40r/min to obtain a raw material mixture for later use;
4) feeding the raw material mixture prepared in the step 3) into a mold, molding under the pressure of 12MPa, curing at the temperature of 90 ℃ for 49 hours after molding, and demolding to obtain a blank for later use;
5) and (3) curing the blank obtained in the step 4) at the temperature of 130 ℃ for 25h again, and naturally cooling to obtain the product.
Example 4
The high-toughness solid buoyancy material containing the elastic microspheres is prepared from 100 parts of epoxy resin, 5 parts of reactive diluent, 75 parts of curing agent, 0.4 part of accelerator, 15 parts of toughening agent, 40 parts of elastic microspheres and 10 parts of surface modifier in percentage by mass, wherein the epoxy resin is E44, the reactive diluent is BDGE, the curing agent is methylnadic anhydride, the accelerator is 1-aminoethyl-2-methylimidazole, the toughening agent is polysulfide rubber, the elastic microspheres are 10 micrometers in average particle size and 0.20g/cm in density3The acrylonitrile polymer microspheres are coated with the calcium carbonate, and the surface modifier is JN114 titanate coupling agent;
the preparation method comprises the following steps:
1) weighing the materials according to the proportion for later use;
2) mixing the other components except the elastic microspheres uniformly at normal temperature to prepare a resin glue solution for later use;
3) adding the elastic microspheres weighed in the step 1) into the resin glue solution prepared in the step 2), and uniformly mixing at a rotating speed of 40r/min to obtain a raw material mixture for later use;
4) feeding the raw material mixture prepared in the step 3) into a mold, molding under the pressure of 10MPa, curing at the temperature of 85 ℃ for 56 hours after molding, and demolding to obtain a blank for later use;
5) and (3) curing the blank obtained in the step 4) for 40 hours at the temperature of 125 ℃, and naturally cooling to obtain the product.
Example 5
The high-toughness solid buoyancy material containing the elastic microspheres is prepared from 100 parts of epoxy resin, 15 parts of reactive diluent, 90 parts of curing agent, 0.8 part of accelerating agent, 5 parts of toughening agent, 60 parts of elastic microspheres and 20 parts of surface modifier according to mass percentage, wherein the epoxy resin is E54, the reactive diluent is AGE, the curing agent is methyltetrahydrophthalic anhydride, the accelerating agent is 1-benzyl-2-ethylimidazole, the toughening agent is polyether sulfone, the elastic microspheres are 40 micrometers in average particle size and 0.10g/cm in density3The titanium oxide coats the acrylonitrile polymer microsphere, and the surface modifier is 414 aluminate coupling agent;
the preparation method comprises the following steps:
1) weighing the materials according to the proportion for later use;
2) mixing the other components except the elastic microspheres uniformly at normal temperature to prepare a resin glue solution for later use;
3) adding the elastic microspheres weighed in the step 1) into the resin glue solution prepared in the step 2), and uniformly mixing at a rotating speed of 25-50r/min to obtain a raw material mixture for later use;
4) feeding the raw material mixture prepared in the step 3) into a mold, molding under the pressure of 15MPa, curing at the temperature of 95 ℃ for 72 hours after molding, and demolding to obtain a blank for later use;
5) and (3) curing the blank obtained in the step 4) at the temperature of 135 ℃ for 28h again, and naturally cooling to obtain the product.
The solid buoyancy material prepared in each example was subjected to various performance tests, and the test results were as follows:
example 1: the density was 0.49g/cm3The compressive strength is 25MPa, the water absorption is 0.9 percent, and the elongation at break is 7.3 percent;
example 2: the density was 0.47g/cm3The compressive strength is 27MPa, the water absorption is 0.5 percent, and the elongation at break is 6.5 percent;
example 3: the density was 0.53g/cm3The compressive strength is 33MPa, the water absorption is 0.7 percent, and the elongation at break is 6.9 percent;
example 4: the density was 0.51g/cm3The compressive strength is 38MPa, the water absorption is 0.6 percent, and the elongation at break is 8.3 percent;
example 5: the density was 0.49g/cm3The compressive strength was 41MPa, the water absorption was 0.5%, and the elongation at break was 8.5%.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (8)
1. A high-toughness solid buoyancy material containing elastic microspheres is characterized in that: according to the mass percentage, the material is prepared from 100 parts of epoxy resin, 0-20 parts of reactive diluent, 60-120 parts of curing agent, 0-1 part of accelerator, 0-20 parts of toughening agent and 10-100 parts of elastic microspheres, wherein the elastic microspheres have the average particle size of 10-120 micrometers and the density of 0.10-0.20g/cm3And one or more of calcium carbonate, talc or titanium oxide coated acrylonitrile polymer microspheres with compressive strength of 10-20 MPa.
2. The high tenacity solid buoyant material comprising elastomeric microspheres of claim 1 wherein: the epoxy resin is bisphenol A type epoxy resin or bisphenol F type epoxy resin.
3. The high tenacity solid buoyant material comprising elastomeric microspheres of claim 1 wherein: the reactive diluent is allyl glycidyl ether, butyl glycidyl ether, diglycidyl aniline or butanediol diglycidyl ether.
4. The high tenacity solid buoyant material comprising elastomeric microspheres of claim 1 wherein: the curing agent is an acid anhydride or amine curing agent matched with the epoxy resin.
5. The high tenacity solid buoyant material comprising elastomeric microspheres of claim 1 wherein: the accelerator is imidazole or tertiary amine accelerator matched with the curing agent.
6. The high tenacity solid buoyant material comprising elastomeric microspheres of claim 1 wherein: the toughening agent is one or a mixture of more of liquid carboxyl-terminated nitrile rubber, epoxy-terminated nitrile rubber, polysulfide rubber, polyether-ether-ketone and polyether sulfone in any proportion.
7. The high tenacity solid buoyant material comprising elastomeric microspheres of claim 1 wherein: the high-toughness solid buoyancy material also contains 0-20 parts of a surface modifier, wherein the surface modifier is one or a mixture of more of a JN114 titanate coupling agent, a KH560 silane coupling agent, a 414 aluminate coupling agent and a lauryl alcohol ether phosphate anionic surfactant in any proportion.
8. The method for preparing the high-toughness solid buoyancy material containing the elastic microspheres according to claim 1 or 7, wherein the method comprises the following steps:
1) weighing the materials according to the proportion of claim 1 or 7 for later use;
2) mixing the other components except the elastic microspheres uniformly at normal temperature to prepare a resin glue solution for later use;
3) adding the elastic microspheres weighed in the step 1) into the resin glue solution prepared in the step 2), and uniformly mixing at a rotating speed of 25-50r/min to obtain a raw material mixture for later use;
4) feeding the raw material mixture prepared in the step 3) into a mold, molding under the pressure of 5-20MPa, curing at 80-100 ℃ for not less than 48 hours after molding, and demolding to obtain a blank for later use;
5) re-curing the blank obtained in the step 4) at the temperature of 120-140 ℃ for not less than 24h, and naturally cooling after curing to obtain the product.
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| WO2023183119A3 (en) * | 2022-03-01 | 2024-01-25 | Huntsman Advanced Materials Americas Llc | Surface tolerant adhesive |
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| CN112961570B (en) * | 2021-02-06 | 2024-07-12 | 杭州每步材料科技有限公司 | Environment-friendly underwater toughened epoxy resin adhesive and preparation method thereof |
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| JPH03166929A (en) * | 1989-11-27 | 1991-07-18 | Yokohama Rubber Co Ltd:The | Buoyancy material |
| CN106832789A (en) * | 2017-03-21 | 2017-06-13 | 钟东南 | A kind of integrated molding solid buoyancy material and preparation method thereof |
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2018
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03166929A (en) * | 1989-11-27 | 1991-07-18 | Yokohama Rubber Co Ltd:The | Buoyancy material |
| CN106832789A (en) * | 2017-03-21 | 2017-06-13 | 钟东南 | A kind of integrated molding solid buoyancy material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 耐水型环氧树脂增韧剂的制备及应用;苗琦;《塑料科技》;20081231;第36卷(第12期);第80-83页 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023183119A3 (en) * | 2022-03-01 | 2024-01-25 | Huntsman Advanced Materials Americas Llc | Surface tolerant adhesive |
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