CN116178893A - Solid buoyancy material for large depth and preparation method thereof - Google Patents
Solid buoyancy material for large depth and preparation method thereof Download PDFInfo
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Abstract
The invention provides a solid buoyancy material for large depth and a preparation method thereof, wherein the solid buoyancy material is prepared from the following raw materials of, by weight, 100 parts of epoxy resin, 60-150 parts of curing agent, 1-5 parts of diluent, 0.1-2 parts of catalyst, 20-150 parts of hollow glass microspheres, 1-6 parts of surface modifier and 0.1-2 parts of defoaming agent. The solid buoyancy material obtained by the invention has the advantages of low density, high strength, low internal porosity and compact structure, and can be applied to the water depth of 3000-11000 m.
Description
Technical Field
The invention belongs to the technical field of solid buoyancy materials, and in particular relates to a solid buoyancy material for large depth and a preparation method thereof.
Background
The solid buoyancy material is a two-phase or three-phase composite material obtained by resin and hollow filler through a certain preparation process, is widely applied to various underwater operation systems in the ocean field, is used as an important component of modern depth technology, provides buoyancy for a submersible vehicle, and increases the effective load of the submersible vehicle.
The Chinese patent CN112521706A discloses a deep sea solid buoyancy material and a preparation method thereof, and the hollow glass beads and millimeter-sized beads are filled into polydicyclopentadiene resin to prepare the buoyancy material used for the depth of 6000-11000 m. Chinese patent CN110628180A discloses a solid buoyancy material and a preparation method thereof, wherein two or three hollow glass beads are compounded to be used as a density regulator to be filled into epoxy resin to prepare the solid buoyancy material suitable for being used in a deep Brillouin zone of 1000-11000 m, and vacuum auxiliary defoaming is adopted in the mixing stage in the two patents, so that the obtained solid buoyancy material is not compact enough; chinese patent CN113683862a discloses a low-density solid buoyancy material suitable for deep sea and a preparation method thereof, which adopts a high-frequency vacuum vibration method to eliminate bubbles in the material as much as possible; chinese patent CN103085191a discloses a deep sea pressure-resistant processable buoyancy material and a production method thereof, wherein the material in the shaping of the mould is defoamed by vacuum vibration; in the two patents, although vacuum vibration defoamation is adopted in the casting molding process, the obtained buoyancy material is still not compact enough.
Disclosure of Invention
In order to solve the problems, the invention provides a solid buoyancy material for large depth and a preparation method thereof, and the obtained solid buoyancy material has the advantages of low density, high strength, low internal porosity and compact structure, and can be applied to the water depth of 3000-11000 m.
First, it is an object of the present invention to provide a solid buoyancy material for large depths.
Specifically, the solid buoyancy material is prepared from the following raw materials in parts by mass,
preferably, the components are as follows in parts by mass:
wherein the modified hollow glass microspheres are modified by a surface modifier, preferably 3-aminopropyl triethoxysilane.
Further, the preparation process of the modified glass beads is as follows:
adding the hollow glass beads into a solvent, uniformly stirring, adding a modifier for modification, wherein the modification reaction temperature is 50-60 ℃, the reaction time is 2-3 h, and obtaining the modified hollow glass beads after suction filtration, washing and drying. Wherein the mass of the added modifier is 1-5% of the mass of the hollow glass beads; the solvent is preferably ethanol.
Preferably, the epoxy resin is one or a combination of glycidyl ether type epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, alicyclic epoxy resin and mixed type epoxy resin.
Preferably, the curing agent is one or a combination of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, trialkyl tetrahydrophthalic anhydride, polydiphenyl substituted hexadecane dicarboxylic anhydride, methyl nadic anhydride, dodecenyl succinic anhydride and tung oil anhydride.
Preferably, the diluent is one of trimethylolpropane polyglycidyl ether, 1, 6-hexanediol diglycidyl ether, and C12-C14 alcohol glycidyl ether.
Preferably, the catalyst is one of tertiary amines, phenols or imidazoles; more preferably, the catalyst is 2,4, 6-tris (dimethylaminomethyl) phenol (DMP-30); the defoamer is polyether modified polydimethylsiloxane (BYK-065).
Preferably, the hollow glass beads have a density distribution of 0.1 to 0.5g/cm 3 The particle size distribution is 10-150 mu m, and the strength is 250-27000 psi.
It is worth mentioning that the diluent is used for adjusting the viscosity of materials on one hand and matched with the defoamer for use, so that the structure of the buoyancy material is more compact, and the strength of the buoyancy material is improved; on the other hand, the hollow glass beads are more beneficial to be added into the resin matrix to be filled with more hollow glass beads for adjusting the density of the buoyancy material.
Next, the second object of the present invention is to provide a method for preparing the solid buoyancy material.
The method comprises the following steps:
(1) Fully mixing epoxy resin, a curing agent, a diluent, a catalyst and a defoaming agent, and removing air in the mixed system under a vacuum condition;
(2) Mixing the modified hollow glass beads with the mixed system in the step (1), and stirring under vacuum conditions to obtain a uniformly mixed deaerated material;
(3) Pouring the defoamed material in the step (2) into a sealing mould for molding;
(4) And (5) putting the mold into an oven for solidification, and demolding to obtain the solid buoyancy material.
Preferably, in the step (1), the air in the mixed system is removed by premixing for 5 to 10 minutes under the environment that the temperature is 50 to 70 ℃ and the vacuum degree is-0.095 MPa to-0.10 MPa.
Preferably, in the step (2), the mixed system is stirred for 20-30 min under the vacuum environment that the vacuum degree is-0.095 MPa to-0.10 MPa at the temperature of 70-90 ℃.
Preferably, in the step (3), the material is molded by adopting a close packing technology of vibrating and vacuumizing, the vibration amplitude is 3-5 mm, the vibration frequency is 40-50 Hz, the vacuum is stopped after the vacuum degree is kept at-0.095 MPa to-0.10 MPa for 10-60 min, and the vibration needs to be kept for 5-10 min after the vacuum is stopped. So as to be beneficial to the densification of materials in the forming process.
Preferably, in step (4), the mold is cured by a step-heating method, and the step temperature is changed to: the temperature is kept at 90-100 ℃ for 4-5 h, 120-130 ℃ for 4-5 h and 140-150 ℃ for 4-5 h, and then the furnace is cooled to room temperature.
The following technical scheme can be adopted:
(1) Adding epoxy resin, a curing agent, a diluent, a catalyst and a defoaming agent into a vacuum stirrer according to a proportion, premixing for 5-10 min at 50-70 ℃ under a vacuum environment, and removing air in the system;
(2) Weighing the modified hollow glass beads according to the proportion, adding the modified hollow glass beads into a pre-mixed resin system, and stirring the mixture in vacuum for about 30 minutes at the temperature of 70-90 ℃;
(3) Pouring the material which is subjected to vacuum defoaming and uniform mixing into a sealed cuboid mold, vacuumizing while vibrating, stopping vacuum after 10-60 min, and stopping vibrating after 5-10 min;
(4) Putting the die into an oven, and curing in a stepped heating mode: 4-5 h at 90-100 ℃, 4-5 h at 120-130 ℃, 4-5 h at 140-150 ℃ and 4-5 h, and demoulding to remove the outer surface to obtain the buoyancy material.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts the vacuum composite casting technology to prepare the solid buoyancy material for large depth, the technological process is simple and controllable, and the density of the prepared buoyancy material is 0.50-0.68 g/cm 3 The hydrostatic pressure strength can reach 30-150 MPa, the water absorption rate is less than 0.5% under the corresponding hydrostatic pressure environment, and the use depth can reach 11000 m.
2. The invention can adopt any one or more different resins, curing agents and modified hollow glass beads with certain particle size to prepare the buoyancy material, and meanwhile, the buoyancy material prepared under the same conditions has lower density, more compact structure, higher strength and better performance compared with the technology of adding diluents, defoaming agents and tightly stacking in the combined forming process, and can be applied to large-depth water areas of 3000-11000 m.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
The raw materials, reagents and the like used in the following examples were all from commercial products.
Example 1
Hollow glass bead K15 (true density of 0.15 g/cm) 3 D50:55 μm and the intensity is more than or equal to 300 Psi) is added into ethanol and stirred evenly, 3 percent of modifier KH-550 relative to the mass parts of the hollow glass beads is added, and the mixture is stirred for 2 hours at 55 ℃, filtered, washed and dried for standby. 618 resin, methyltetrahydrophthalic anhydride, methylnadic anhydride, C12-C14 alcohol glycidyl ether, DMP-30 and BYK-065 are added into a vacuum stirrer according to the mass ratio of 100:50:15:3:1.5:0.5, and are premixed for 7min at 60 ℃ under the vacuum environment with the vacuum degree of-0.098 MPa, so that the air in the system is removed. 50 parts of modified K15 hollow glass beads are weighed and added into a pre-mixed resin system, and stirred for 30min under the vacuum with the vacuum degree of-0.098 MPa at the temperature of 80 ℃. Pouring the material subjected to vacuum defoaming and uniform mixing into a sealed cuboid mold, vacuumizing while vibrating, keeping the amplitude at 4mm, keeping the vibration frequency at 46.67Hz, keeping the vacuum degree at-0.098 MPa for 30min, stopping vacuum, and stopping vibrating after 5 min. The die is placed into an oven to be solidified in a step heating mode, and the step temperature is changed into: removing the outer surface at 100 ℃ for 5 hours +130 ℃ for 5 hours +150 ℃ to obtain the buoyancy material, wherein the density of the buoyancy material is 0.503g/cm 3 The compression strength is 35MPa, the water absorption rate is 0.17% under the hydrostatic pressure environment of 30MPa, and the water absorption rate can be applied to 3000 m depth.
Example 2
Hollow glass beads XLD3000 and S32HS (XLD 3000 true density is 0.23 g/cm) 3 D50:30 μm, the intensity is more than or equal to 3000Psi; s32HS true density is 0.32g/cm 3 D50:25 μm, intensity not less than 6000 Ps) is added into ethanol according to the mass ratio of 5:1, and stirred evenly, KH-550 accounting for 4 percent of the mass parts of the hollow glass beads is added, stirred for 3 hours at 55 ℃, and then filtered, washed and dried for standby. 6101 resin, AFG-90, methyl hexahydrophthalic anhydride, trimethylolpropane polyglycidyl ether, DMP-30 and BYK-065 are added into a vacuum stirrer according to the mass ratio of 90:10:125:5:1:1.2, and are premixed for 5min at the temperature of 70 ℃ under the vacuum environment with the vacuum degree of-0.1 MPa, and the air in the system is removed. Weighing modified XLD3000 and S32HS hollow glass micro90 parts of beads are added to the pre-mixed resin system and stirred for 20min at 80℃under vacuum with a degree of vacuum of-0.1 MPa. Pouring the material subjected to vacuum defoaming and uniform mixing into a sealed cuboid mold, vacuumizing while vibrating, keeping the amplitude at 5mm, keeping the vibration frequency at 45Hz, keeping the vacuum degree at-0.1 MPa for 40min, stopping vacuum, and stopping vibrating after 5 min. The mold was placed in an oven for curing: removing the outer surface at 100 ℃ for 5 hours at +130 ℃ for 5 hours at +150 ℃ to obtain a buoyancy material with the density of 0.585g/cm 3 The compression strength is 69MPa, the water absorption rate is 0.28% under 60MPa hydrostatic pressure environment, and the water absorption rate can be applied to 6000 m water depth.
Example 3
Hollow glass beads S32HS and HGS8000X (S32 HS true density 0.32 g/cm) 3 D50:25 μm, the intensity is more than or equal to 6000Psi; HGS8000X true density is 0.42g/cm 3 D50:22 μm, the intensity is more than or equal to 8000 Psi) is added into ethanol according to the mass ratio of 1:1, and is stirred evenly, KH-550 accounting for 4 percent of the mass of the hollow glass beads is added, and the mixture is stirred for 3 hours at 55 ℃, filtered, washed and dried for standby. 618 resin, TGE-85, methyltetrahydrophthalic anhydride, tung oil anhydride, trimethylolpropane polyglycidyl ether, DMP-30 and BYK-065 are added into a vacuum stirrer according to the mass ratio of 80:20:70:40:4:0.5:1.5, and are premixed for 10min under the vacuum environment with the vacuum degree of-0.099 MPa at the temperature of 65 ℃ to remove the air in the system. 115 parts of modified S32HS and HGS8000X hollow glass beads are weighed and added into a pre-mixed resin system, and stirred for 30min under the vacuum with the vacuum degree of-0.099 MPa at the temperature of 80 ℃. Pouring the material subjected to vacuum defoaming and uniform mixing into a sealed cuboid mold, vacuumizing while vibrating, keeping the amplitude at 3mm, keeping the vibration frequency at 48Hz, keeping the vacuum degree at-0.099 MPa for 60min, stopping vacuum, and stopping vibrating after 5 min. The mold was placed in an oven for curing: removing the outer surface at 100 ℃ for 5 hours at 130 ℃ for 5 hours at 150 ℃ for 5 hours to obtain the buoyancy material with the density of 0.633g/cm 3 The compression strength is 82MPa, the water absorption rate is 0.11% under the hydrostatic pressure environment of 70MPa, and the water-absorbing agent can be applied to 7000 m depth of water.
Example 4
Micro-forming hollow glassBead IM16K (true density 0.46 g/cm) 3 D50:20 μm and intensity of not less than 16000 Psi) is added into ethanol and stirred evenly, KH-550 accounting for 3 percent of the mass parts of the hollow glass beads is added, and the mixture is stirred for 2 hours at 55 ℃, filtered, washed and dried for standby. 2040 resin, TGE-85, methyl hexahydrophthalic anhydride, polydiphenyl substituted hexadecane dicarboxylic anhydride, 1, 6-hexanediol diglycidyl ether, DMP-30 and BYK-065 are added into a vacuum stirrer according to the mass ratio of 50:50:90:30:3.5:0.5:1, and the mixture is premixed for 10 minutes in a vacuum environment at the temperature of 70 ℃ under the vacuum degree of-0.096 MPa, so that the air in the system is removed. 140 parts of modified IM16K hollow glass beads are weighed and added into a pre-mixed resin system, and the mixture is stirred for 30min under the vacuum degree of-0.096 MPa at the temperature of 90 ℃. Pouring the material subjected to vacuum defoaming and uniform mixing into a sealed cuboid mold, vacuumizing while vibrating, keeping the amplitude at 5mm, keeping the vibration frequency at 42Hz, keeping the vacuum degree at-0.096 MPa for 60min, stopping vacuum, and stopping vibrating after 5 min. The mold was placed in an oven for curing: removing the outer surface at 100 ℃ for 5 hours +130 ℃ for 5 hours +150 ℃ to obtain the buoyancy material, wherein the density of the buoyancy material is 0.668g/cm 3 The compression strength is 115MPa, the water absorption rate under the hydrostatic pressure environment is 0.14% of 110MPa, and the water absorption rate can be applied to 11000 m water depth.
Comparative example 1
Hollow glass bead K15 (true density of 0.15 g/cm) 3 D50:55 μm and the intensity is more than or equal to 300 Psi) is added into ethanol and stirred evenly, 3 percent of modifier KH-550 relative to the mass parts of the hollow glass beads is added, and the mixture is stirred for 2 hours at 55 ℃, filtered, washed and dried for standby. 618 resin, methyltetrahydrophthalic anhydride, methylnadic anhydride, DMP-30 and BYK-065 are added into a vacuum stirrer according to the mass ratio of 100:50:15:1.5:0.5, and are premixed for 7min under the vacuum environment with the vacuum degree of-0.098 MPa at the temperature of 60 ℃ to remove the air in the system. 45 parts of modified K15 hollow glass beads are weighed and added into a pre-mixed resin system, and stirred for 30min under the vacuum with the vacuum degree of-0.098 MPa at the temperature of 80 ℃. Pouring the materials subjected to vacuum defoaming and uniform mixing into a sealed cuboid mold, vacuumizing while vibrating, keeping the amplitude at 4mm, keeping the vibration frequency at 46.67Hz, and keeping the vacuum degree at-0.098 MPaAfter maintaining the vacuum for 30min, stopping the vacuum, and after 5min, stopping the vibration. The die is placed into an oven to be solidified in a step heating mode, and the step temperature is changed into: removing the outer surface at 100 ℃ for 5 hours +130 ℃ for 5 hours +150 ℃ to obtain the buoyancy material, wherein the density of the buoyancy material is 0.517g/cm 3 The compression strength is 39MPa, and the water absorption rate is 0.11 percent under the hydrostatic pressure environment of 30 MPa.
Comparative example 2
Hollow glass bead K15 (true density of 0.15 g/cm) 3 D50:55 μm and the intensity is more than or equal to 300 Psi) is added into ethanol and stirred evenly, 3 percent of modifier KH-550 relative to the mass parts of the hollow glass beads is added, and the mixture is stirred for 2 hours at 55 ℃, filtered, washed and dried for standby. 618 resin, methyltetrahydrophthalic anhydride, methylnadic anhydride, glycidyl ether of C12-C14 alcohol and DMP-30 are added into a vacuum stirrer according to the mass ratio of 100:50:15:3:1.5, and are premixed for 7min under the vacuum environment with the vacuum degree of-0.098 MPa at the temperature of 60 ℃ to remove the air in the system. 50 parts of modified K15 hollow glass beads are weighed and added into a pre-mixed resin system, and stirred for 30min under the vacuum with the vacuum degree of-0.098 MPa at the temperature of 80 ℃. Pouring the material subjected to vacuum defoaming and uniform mixing into a sealed cuboid mold, vacuumizing while vibrating, keeping the amplitude at 4mm, keeping the vibration frequency at 46.67Hz, keeping the vacuum degree at-0.098 MPa for 30min, stopping vacuum, and stopping vibrating after 5 min. The die is placed into an oven to be solidified in a step heating mode, and the step temperature is changed into: removing the outer surface at 100 ℃ for 5 hours +130 ℃ for 5 hours +150 ℃ to obtain the buoyancy material, wherein the density of the buoyancy material is 0.500g/cm 3 The compression strength is 31MPa, and the water absorption rate is 0.31 percent under the hydrostatic pressure environment of 30 MPa.
Comparative example 3
Hollow glass bead K15 (true density of 0.15 g/cm) 3 D50:55 μm and the intensity is more than or equal to 300 Psi) is added into ethanol and stirred evenly, 3 percent of modifier KH-550 relative to the mass parts of the hollow glass beads is added, and the mixture is stirred for 2 hours at 55 ℃, filtered, washed and dried for standby. 618 resin, methyltetrahydrophthalic anhydride, methylnadic anhydride, glycidyl ether of C12-C14 alcohol, DMP-30 and BYK-065 are added into vacuum according to the mass ratio of 100:50:15:3:1.5:0.5Premixing in a stirrer at 60 ℃ under vacuum condition with vacuum degree of-0.098 MPa for 7min, and removing air in the system. 50 parts of modified K15 hollow glass beads are weighed and added into a pre-mixed resin system, and stirred for 30min under the vacuum with the vacuum degree of-0.098 MPa at the temperature of 80 ℃. And pouring the material which is subjected to vacuum defoamation and uniform mixing into a cuboid mould. The die is placed into an oven to be solidified in a step heating mode, and the step temperature is changed into: removing the outer surface at 100 ℃ for 5 hours +130 ℃ for 5 hours +150 ℃ to obtain the buoyancy material, wherein the density of the buoyancy material is 0.495g/cm 3 The compression strength is 28MPa, and the water absorption rate is 0.54 percent under the hydrostatic pressure environment of 30 MPa.
As is clear from examples 1 and comparative examples 1 to 3, the system viscosity was high and the amount of added beads was small without adding a diluent, and the density of the obtained buoyancy material was increased, the strength was increased, and the water absorption was decreased; under the condition that no defoamer is added, bubbles (especially micro bubbles) in the obtained buoyancy material remain, the density of the buoyancy material is slightly reduced, the strength is reduced, and the water absorption rate is increased; under the condition that a close packing technology is not adopted, the obtained buoyancy material has more internal bubbles, the density and strength of the buoyancy material can be reduced, and the water absorption rate can be greatly increased. Thus, the invention provides a method for preparing the buoyancy material with low density, high strength, low internal porosity and compact structure by combining the diluent, the defoamer and the close packing method in the raw materials.
Claims (10)
1. A solid buoyancy material for large depth is characterized in that the solid buoyancy material is prepared from the following raw materials in parts by weight,
the modified hollow glass beads are modified by a surface modifier.
2. The solid buoyancy material for large depths according to claim 1, wherein each component is calculated in parts by weight,
the preparation of the modified hollow glass beads comprises the following steps:
the mass of the added surface modifier is 1-5% of the mass of the hollow glass beads, the modification reaction temperature is 50-60 ℃, and the reaction time is 2-3 h;
the surface modifier is 3-aminopropyl triethoxysilane.
3. The solid buoyant material for large depths according to claim 1 wherein,
the epoxy resin is one or a combination of glycidyl ether type epoxy resin, glycidyl ester type epoxy resin, glycidyl amine type epoxy resin, alicyclic epoxy resin and mixed type epoxy resin.
4. The solid buoyant material for large depths according to claim 1 wherein,
the curing agent is one or a combination of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, trialkyl tetrahydrophthalic anhydride, polydiphenyl substituted hexadecane dicarboxylic anhydride, methyl nadic anhydride, dodecenyl succinic anhydride and tung oil anhydride.
5. The solid buoyant material for large depths according to claim 1 wherein,
the diluent is one of trimethylolpropane polyglycidyl ether, 1, 6-hexanediol diglycidyl ether and C12-C14 alcohol glycidyl ether.
6. The solid buoyant material for large depths according to claim 1 wherein,
the catalyst is one of tertiary amines, phenols or imidazoles, preferably 2,4, 6-tris (dimethylaminomethyl) phenol;
the defoamer is polyether modified polydimethylsiloxane.
7. The solid buoyant material for large depths according to claim 1 wherein,
the density distribution of the hollow glass beads is 0.1-0.5 g/cm 3 The particle size distribution is 10-150 mu m, and the strength is 250-27000 psi.
8. The method for producing a solid buoyancy material for large depths according to any one of claims 1 to 7, comprising the steps of:
(1) Fully mixing epoxy resin, a curing agent, a diluent, a catalyst and a defoaming agent, and removing air in the mixed system under a vacuum condition;
(2) Mixing the modified hollow glass beads with the mixed system in the step (1), and stirring under vacuum conditions to obtain a uniformly mixed deaerated material;
(3) Pouring the defoamed material in the step (2) into a sealing mould for molding;
(4) And (5) putting the mold into an oven for solidification, and demolding to obtain the solid buoyancy material.
9. The method for producing a solid buoyancy material for large depths according to claim 8,
in the step (1), premixing is carried out for 5-10 min under the environment that the temperature is 50-70 ℃ and the vacuum degree is minus 0.095MPa to minus 0.10 MPa;
in the step (2), the mixed system is stirred for 20-30 min at 70-90 ℃ and the vacuum degree of minus 0.095MPa to minus 0.10 MPa;
in the step (3), the material is molded by adopting a close packing technology of vibrating and vacuumizing, the vibration amplitude is 3-5 mm, the vibration frequency is 40-50 Hz, the vacuum degree is-0.095 MPa to-0.10 MPa for 10-60 min, and the vibration needs to be kept for 5-10 min after the vacuum is stopped.
10. The method of producing a solid buoyancy material for large depths according to claim 8, wherein in the step (4), the solidification adopts a step-up method, and the step temperature is changed to: the temperature is kept at 90-100 ℃ for 4-5 h, 120-130 ℃ for 4-5 h and 140-150 ℃ for 4-5 h, and then the furnace is cooled to room temperature.
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