CN108891042B - Preparation method of machinable solid buoyancy material - Google Patents
Preparation method of machinable solid buoyancy material Download PDFInfo
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- CN108891042B CN108891042B CN201810675017.5A CN201810675017A CN108891042B CN 108891042 B CN108891042 B CN 108891042B CN 201810675017 A CN201810675017 A CN 201810675017A CN 108891042 B CN108891042 B CN 108891042B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/42—Shaping or impregnating by compression not applied for producing articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/54—Component parts, details or accessories; Auxiliary operations, e.g. feeding or storage of prepregs or SMC after impregnation or during ageing
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2309/00—Use of inorganic materials not provided for in groups B29K2303/00 - B29K2307/00, as reinforcement
- B29K2309/08—Glass
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- Organic Chemistry (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The invention belongs to the technical field of buoyancy materials, and discloses a preparation method of a machinable solid buoyancy material. The preparation method adopts a forming device, and the following materials are weighed according to parts by weight: 100 parts of epoxy resin, 60-150 parts of curing agent, 0.05-3 parts of accelerator, 0.2-5 parts of coupling agent and 10-50 parts of hollow glass microsphere, and then uniformly mixing all the materials; adding the uniformly mixed materials into a forming device, and applying a vertically downward pressure of 0.3-15 Mpa to a top cover of the forming device until no materials are discharged from the bottom of the forming device; curing the forming device and the materials inside the forming device according to a curing process of firstly preserving heat for 1-3 h at 80-90 ℃, then preserving heat for 2-4 h at 100-120 ℃ and finally preserving heat for 1-3 h at 140-160 ℃; and (4) disassembling the forming device after solidification is finished, and taking out the block attached to the bottom of the forming device to obtain the processable solid buoyancy material. The buoyancy material prepared by the invention has low density, high compressive strength and low water absorption.
Description
Technical Field
The invention belongs to the technical field of buoyancy materials, and particularly relates to a preparation method of a machinable solid buoyancy material.
Background
In recent years, the ocean technology in China is rapidly developed, great progress is made in the aspects of ocean exploration, detection and the like, and the deep-water high-strength buoyancy material becomes an important component for developing the modern deep-diving technology. The low-density and high-strength deep-water solid buoyancy material is more and more widely applied, the pressure borne by the deep submersible vehicle is sharply increased along with the increase of the depth of water, and the performance requirement on the deep-water solid buoyancy material is higher and higher.
The formation of solid buoyant materials can generally be divided into three stages: (1) in the plasticizing stage, the material is heated to a proper temperature to be softened and become a formable molten material; (2) filling and shaping, namely filling all parts of the cavity with pasty materials with flow property under certain pressure; (3) and in the curing stage, the completely shaped material is continuously heated in the cavity for a period of time until the material is completely cured. Methods for preparing the solid buoyant material generally include a casting method, a vacuum impregnation method, a liquid transfer molding method, a press molding method and the like.
In order to prepare the buoyancy material with low density, high compressive strength and low water absorption, the conventional preparation process usually has complicated equipment or process, such as defoaming treatment under the conditions of high temperature and high pressure or special complicated molds and demolding devices, so that the production cost is high, the efficiency is low, and the application of the buoyancy material is limited to a certain extent.
Disclosure of Invention
The invention aims to provide a preparation method of a machinable solid buoyancy material, which has the advantages of convenience in operation, high reliability, good controllability and the like, and the prepared buoyancy material has the characteristics of low density, high compressive strength, low water absorption and the like, and can be used for manufacturing 100-3000 m deep diving equipment.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a machinable solid buoyancy material adopts a molding device, wherein the molding device comprises a hollow cylindrical barrel, a top cover and a base; the top cover is a cylindrical cover plate, and the diameter of the cylindrical cover plate is matched with the inner diameter of the hollow cylindrical barrel so as to ensure that the cylindrical cover plate can slide up and down along the inner wall of the hollow cylindrical barrel; the base comprises a first cylindrical bottom plate and a second cylindrical bottom plate coaxially and fixedly arranged on the upper surface of the first cylindrical bottom plate, the diameter of the first cylindrical bottom plate is the same as the outer diameter of the hollow cylindrical barrel, the diameter of the second cylindrical bottom plate is matched with the inner diameter of the hollow cylindrical barrel so as to ensure that the second cylindrical bottom plate can be inserted into the inner cavity of the hollow cylindrical barrel and the outer wall of the second cylindrical bottom plate is tightly attached to the inner wall of the hollow cylindrical barrel, a plurality of through holes are uniformly formed in the second cylindrical bottom plate and extend towards the first cylindrical bottom plate until penetrating through the first cylindrical bottom plate, and the diameter of each through hole is 3-6 mm; a plurality of screw posts are uniformly arranged on the first cylindrical bottom plate around the second cylindrical bottom plate, and screw holes which are in one-to-one correspondence with the screw posts are formed in the outer wall of the bottom of the hollow cylindrical barrel; the top cover is positioned in the inner cavity at the top end of the hollow cylindrical barrel, the second cylindrical bottom plate is inserted into the inner cavity at the bottom of the hollow cylindrical barrel, and the base is fixedly connected to the bottom of the hollow cylindrical barrel through the screw thread fit between the screw column and the screw hole;
the preparation steps are as follows:
(1) weighing the following materials in parts by weight: 100 parts of epoxy resin, 60-150 parts of curing agent, 0.05-3 parts of accelerator, 0.2-5 parts of coupling agent and 10-50 parts of hollow glass microsphere, and then uniformly mixing all the materials;
(2) firstly, splitting the forming device into a hollow cylindrical barrel, a top cover and a base, then fixedly arranging the base at the bottom of the hollow cylindrical barrel, adding the uniformly mixed materials into an inner cavity of the hollow cylindrical barrel, then arranging the top cover in an inner cavity at the top end of the hollow cylindrical barrel, and at the moment, arranging the materials in the inner cavity of the hollow cylindrical barrel between the top cover and a second cylindrical bottom plate;
continuously applying a vertically downward pressure of 0.3-15 Mpa to the top cover until no material is discharged from the bottom of the forming device, and stopping applying the pressure;
(3) curing the forming device and the materials inside the forming device according to a curing process of firstly preserving heat for 1-3 hours at 80-90 ℃, then preserving heat for 2-4 hours at 100-120 ℃, and finally preserving heat for 1-3 hours at 140-160 ℃;
(4) and after the solidification is finished, disassembling the forming device, and taking out the block attached to the bottom of the forming device to obtain the processable solid buoyancy material.
Preferably, the epoxy resin is one or a mixture of two of epoxy resin E51 and epoxy resin E44.
Preferably, the curing agent is one or a mixture of more than two of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride and dodecenyl succinic anhydride.
Preferably, the accelerator is 2,4, 6-tris- (dimethylaminomethyl) phenol.
Preferably, the coupling agent is a silane coupling agent.
Preferably, the density of the hollow glass beads is 0.15-0.60 g/cm3。
Preferably, the first cylindrical bottom plate and the second cylindrical bottom plate are integrally formed.
The invention provides a preparation method of a machinable solid buoyancy material, which adopts a simple and easily-operated forming device to quickly realize the full impregnation of epoxy resin to hollow glass beads under the pressure and the gravity of the epoxy resin, is more favorable for improving the impregnation efficiency and uniformity of the resin and the hollow glass beads compared with the traditional impregnation method, and can be recycled after the impregnation of the resin and the hollow glass beads, and redundant epoxy resin and curing agent overflow through a through hole below the forming device; the method has the advantages of convenience in operation, high reliability, good controllability and the like, and the prepared buoyancy material has the characteristics of low density, high compressive strength, low water absorption and the like, and has great promotion significance for the application of the buoyancy material in deep submergence.
Drawings
FIG. 1: a schematic front view structure diagram of the forming die;
FIG. 2: a longitudinal sectional view of the molding die;
FIG. 3: the schematic view of the bottom structure of the hollow cylindrical barrel body;
FIG. 4: a schematic view of the base;
FIG. 5: a schematic top view structure of the base;
wherein the reference numerals are: 1-hollow cylindrical barrel, 11-screw hole; 2-a top cover; 3-base, 31-first cylindrical bottom plate, 32-second cylindrical bottom plate, 33-through hole, 34-screw column.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example 1
A preparation method of a machinable solid buoyancy material adopts a forming device, as shown in figures 1-5, wherein the forming device comprises a hollow cylindrical barrel 1, a top cover 2 and a base 3; the top cover 2 is a cylindrical cover plate, and the diameter of the cylindrical cover plate is matched with the inner diameter of the hollow cylindrical barrel 1 so as to ensure that the cylindrical cover plate can slide up and down along the inner wall of the hollow cylindrical barrel 1; the base 3 comprises a first cylindrical bottom plate 31 and a second cylindrical bottom plate 32 which is coaxially and integrally formed on the upper surface of the first cylindrical bottom plate 31, the diameter of the first cylindrical bottom plate 31 is the same as the outer diameter of the hollow cylindrical barrel 1, the diameter of the second cylindrical bottom plate 32 is matched with the inner diameter of the hollow cylindrical barrel 1 so as to ensure that the second cylindrical bottom plate 32 can be inserted into the inner cavity of the hollow cylindrical barrel 1 and the outer wall of the second cylindrical bottom plate 32 is tightly attached to the inner wall of the hollow cylindrical barrel 1, a plurality of through holes 33 are uniformly formed in the second cylindrical bottom plate 32 and extend towards the first cylindrical bottom plate 31 until penetrating through the first cylindrical bottom plate 31, and the diameter of each through hole 33 is; a plurality of screw posts 34 are uniformly arranged on the first cylindrical bottom plate 31 around the second cylindrical bottom plate 32, and screw holes 11 corresponding to the screw posts 34 one by one are arranged on the outer wall of the bottom of the hollow cylindrical barrel 1; the top cover 2 is positioned in the top end inner cavity of the hollow cylindrical barrel 1, the second cylindrical bottom plate 32 is inserted into the bottom inner cavity of the hollow cylindrical barrel 1, and the base 3 is fixedly connected to the bottom of the hollow cylindrical barrel 1 through the screw thread fit between the screw column 34 and the screw hole 11;
the preparation steps are as follows:
(1) weighing the following materials in parts by weight: 100 g of epoxy resin, 100 g of curing agent, 2 g of accelerator, 4 g of coupling agent and 40 g of hollow glass beads, and then uniformly mixing all the materials; wherein the epoxy resin is epoxy resin E44; the curing agent is methyl tetrahydrophthalic anhydride; the accelerator is 2,4, 6-tri- (dimethylaminomethyl) phenol; the coupling agent is KH-560; the hollow glass beads are K20 produced by 3M company and have the density of 0.20 g/cm3；
(2) Firstly, splitting a forming device into a hollow cylindrical barrel 1, a top cover 2 and a base 3 (a screw column 34 can be unscrewed firstly, then the base 3 is taken out of the inner cavity of the hollow cylindrical barrel 1, and finally the top cover 2 is pressed downwards until the hollow cylindrical barrel 1 is pushed out, which is not described in detail below), then fixing the base 3 at the bottom of the hollow cylindrical barrel 1, adding the uniformly mixed materials into the inner cavity of the hollow cylindrical barrel 1, then placing the top cover 2 in the inner cavity at the top end of the hollow cylindrical barrel 1, and then placing the materials in the inner cavity of the hollow cylindrical barrel 1 between the top cover 2 and a second cylindrical bottom plate 32;
continuously applying a vertical downward pressure of 10 Mpa to the top cover 2 (realizing effective and sufficient impregnation of the epoxy resin to the hollow glass beads, simultaneously discharging the redundant epoxy resin and curing agent from a hole structure at the lower part, and recycling the redundant epoxy resin and curing agent, which is not described in detail below) until no material is discharged from the bottom of the forming device, and stopping applying the pressure;
(3) placing the forming device and the materials inside the forming device in a drying oven, and curing according to a curing process of firstly preserving heat at 80 ℃ for 2 h, then preserving heat at 100 ℃ for 3 h and finally preserving heat at 140 ℃ for 2 h;
(4) and after the solidification is finished, disassembling the forming device, and taking out the block attached to the bottom of the forming device to obtain the machinable solid buoyancy material (the surface of the block can be further flattened through processes of turning, milling, sawing and the like according to actual needs to prepare the buoyancy material with a required shape, which is not described in detail below).
Example 2
The molding apparatus was the same as in example 1; the preparation steps are as follows:
(1) weighing the following materials in parts by weight: 100 g of epoxy resin, 80 g of curing agent, 1 g of accelerator, 3 g of coupling agent and 30 g of hollow glass beads, and then uniformly mixing all the materials; wherein the epoxy resin is epoxy resin E44; the curing agent is methyl hexahydrophthalic anhydride; the accelerator is 2,4, 6-tri- (dimethylaminomethyl) phenol; the coupling agent is KH-560; the hollow glass beads are a mixture of XLD3000 and VS5500 produced by 3M company, and the density of the XLD3000 is 0.23 g/cm3The weight percentage of the space core glass micro-beads is 70 percent, and the density of VS5500 is 0.38 g/cm3Filling 30 percent of the glass micro-beads by mass;
(2) firstly, splitting a forming device into a hollow cylindrical barrel 1, a top cover 2 and a base 3, then fixedly arranging the base 3 at the bottom of the hollow cylindrical barrel 1, adding the uniformly mixed materials into the inner cavity of the hollow cylindrical barrel 1, then arranging the top cover 2 in the inner cavity at the top end of the hollow cylindrical barrel 1, and at the moment, arranging the materials in the inner cavity of the hollow cylindrical barrel 1 between the top cover 2 and a second cylindrical bottom plate 32;
continuously applying a vertical downward pressure of 6 Mpa to the top cover 2 until no material is discharged from the bottom of the forming device, and stopping applying the pressure;
(3) placing the forming device and the materials inside the forming device in a drying oven, and curing according to a curing process of firstly preserving heat at 80 ℃ for 1 h, then preserving heat at 110 ℃ for 2 h and finally preserving heat at 150 ℃ for 1.5 h;
(4) and after the solidification is finished, disassembling the forming device, and taking out the block attached to the bottom of the forming device to obtain the processable solid buoyancy material.
Example 3
The molding apparatus was the same as in example 1; the preparation steps are as follows:
(1) weighing the following materials in parts by weight: 100 g of epoxy resin, 120 g of curing agent, 3 g of accelerator, 4 g of coupling agent and 25 g of hollow glass beads, and then uniformly mixing all the materials; wherein the epoxy resin is epoxy resin E51; the curing agent is dodecenyl succinic anhydride; the accelerator is 2,4, 6-tri- (dimethylaminomethyl) phenol; the coupling agent is KH-560; the hollow glass beads are a mixture of VS5500 and IM16K produced by 3M company, and the density of the VS5500 is 0.38 g/cm3The weight percentage of the space core glass micro-beads is 30 percent, and the density of IM16K is 0.46 g/cm3Filling 70 percent of the glass microspheres in percentage by mass;
(2) firstly, splitting a forming device into a hollow cylindrical barrel 1, a top cover 2 and a base 3, then fixedly arranging the base 3 at the bottom of the hollow cylindrical barrel 1, adding the uniformly mixed materials into the inner cavity of the hollow cylindrical barrel 1, then arranging the top cover 2 in the inner cavity at the top end of the hollow cylindrical barrel 1, and at the moment, arranging the materials in the inner cavity of the hollow cylindrical barrel 1 between the top cover 2 and a second cylindrical bottom plate 32;
continuously applying a pressure of 12 Mpa vertically downwards to the top cover 2 until no material is discharged from the bottom of the forming device, and stopping applying the pressure;
(3) placing the forming device and the materials inside the forming device in a drying oven, and curing according to a curing process of firstly preserving heat at 90 ℃ for 3 hours, then preserving heat at 120 ℃ for 4 hours and finally preserving heat at 160 ℃ for 1 hour;
(4) and after the solidification is finished, disassembling the forming device, and taking out the block attached to the bottom of the forming device to obtain the processable solid buoyancy material.
The solid buoyancy material obtained in the above embodiment is subjected to performance detection, and the detection results are as follows:
from the above table, it can be seen that: the buoyancy material prepared by the method has the characteristics of low density, high compressive strength, low water absorption and the like, and can be respectively used for manufacturing 100-3000 m deep submersible equipment.
Claims (7)
1. A preparation method of a machinable solid buoyancy material is characterized by comprising the following steps: the preparation method adopts a forming device, and the forming device comprises a hollow cylindrical barrel, a top cover and a base; the top cover is a cylindrical cover plate, and the diameter of the cylindrical cover plate is matched with the inner diameter of the hollow cylindrical barrel so as to ensure that the cylindrical cover plate can slide up and down along the inner wall of the hollow cylindrical barrel; the base comprises a first cylindrical bottom plate and a second cylindrical bottom plate coaxially and fixedly arranged on the upper surface of the first cylindrical bottom plate, the diameter of the first cylindrical bottom plate is the same as the outer diameter of the hollow cylindrical barrel, the diameter of the second cylindrical bottom plate is matched with the inner diameter of the hollow cylindrical barrel so as to ensure that the second cylindrical bottom plate can be inserted into the inner cavity of the hollow cylindrical barrel and the outer wall of the second cylindrical bottom plate is tightly attached to the inner wall of the hollow cylindrical barrel, a plurality of through holes are uniformly formed in the second cylindrical bottom plate and extend towards the first cylindrical bottom plate until penetrating through the first cylindrical bottom plate, and the diameter of each through hole is 3-6 mm; a plurality of screw posts are uniformly arranged on the first cylindrical bottom plate around the second cylindrical bottom plate, and screw holes which are in one-to-one correspondence with the screw posts are formed in the outer wall of the bottom of the hollow cylindrical barrel; the top cover is positioned in the inner cavity at the top end of the hollow cylindrical barrel, the second cylindrical bottom plate is inserted into the inner cavity at the bottom of the hollow cylindrical barrel, and the base is fixedly connected to the bottom of the hollow cylindrical barrel through the screw thread fit between the screw column and the screw hole;
the preparation steps are as follows:
(1) weighing the following materials in parts by weight: 100 parts of epoxy resin, 60-150 parts of curing agent, 0.05-3 parts of accelerator, 0.2-5 parts of coupling agent and 10-50 parts of hollow glass microsphere, and then uniformly mixing all the materials;
(2) firstly, splitting the forming device into a hollow cylindrical barrel, a top cover and a base, then fixedly arranging the base at the bottom of the hollow cylindrical barrel, adding the uniformly mixed materials into an inner cavity of the hollow cylindrical barrel, then arranging the top cover in an inner cavity at the top end of the hollow cylindrical barrel, and at the moment, arranging the materials in the inner cavity of the hollow cylindrical barrel between the top cover and a second cylindrical bottom plate;
continuously applying a vertically downward pressure of 0.3-15 Mpa to the top cover until no material is discharged from the bottom of the forming device, and stopping applying the pressure;
(3) curing the forming device and the materials inside the forming device according to a curing process of firstly preserving heat for 1-3 hours at 80-90 ℃, then preserving heat for 2-4 hours at 100-120 ℃, and finally preserving heat for 1-3 hours at 140-160 ℃;
(4) and after the solidification is finished, disassembling the forming device, and taking out the block attached to the bottom of the forming device to obtain the processable solid buoyancy material.
2. The method of claim 1, wherein: the epoxy resin is one or a mixture of two of epoxy resin E51 and epoxy resin E44.
3. The method of claim 1, wherein: the curing agent is one or a mixture of more than two of methyl tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride and dodecenyl succinic anhydride.
4. The method of claim 1, wherein: the accelerant is 2,4, 6-tri- (dimethylaminomethyl) phenol.
5. The method of claim 1, wherein: the coupling agent is a silane coupling agent.
6. The method of claim 1, wherein: the density of the hollow glass beads is 0.15-0.60 g/cm3。
7. The method of claim 1, wherein: the first cylindrical bottom plate and the second cylindrical bottom plate are integrally formed.
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| 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 |
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| CN102702679B (en) * | 2012-05-31 | 2015-03-25 | 中国海洋大学 | Preparation method for high-strength solid buoyancy material for deep submergence |
| CN103692685B (en) * | 2013-12-12 | 2016-02-10 | 中国海洋大学 | Compression molding device of a kind of environment protection type easy demoulding and uses thereof |
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