CN113021956B - Forming method of pressure-resistant composite material shell - Google Patents

Forming method of pressure-resistant composite material shell Download PDF

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Publication number
CN113021956B
CN113021956B CN202110139959.3A CN202110139959A CN113021956B CN 113021956 B CN113021956 B CN 113021956B CN 202110139959 A CN202110139959 A CN 202110139959A CN 113021956 B CN113021956 B CN 113021956B
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winding
resin
silane coupling
coupling agent
composite material
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CN113021956A (en
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郑志才
王明
陈艳
孟祥武
王尚
肖亚超
王强
魏化震
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Shandong Non Metallic Material Research Institute
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Shandong Non Metallic Material Research Institute
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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
    • B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
    • B29C70/681—Component parts, details or accessories; Auxiliary operations
    • B29C70/683—Pretreatment of the preformed part, e.g. insert
    • 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
    • B29C70/68—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts by incorporating or moulding on preformed parts, e.g. inserts or layers, e.g. foam blocks
    • B29C70/86—Incorporated in coherent impregnated reinforcing layers, e.g. by winding
    • 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
    • B29C70/88—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised primarily by possessing specific properties, e.g. electrically conductive or locally reinforced
    • B29C70/887—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts characterised primarily by possessing specific properties, e.g. electrically conductive or locally reinforced locally reinforced, e.g. by fillers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/14—Gas barrier composition
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Moulding By Coating Moulds (AREA)

Abstract

The invention discloses a molding method of a pressure-resistant composite material shell, and belongs to the field of molding of fiber composite material shells. The resin of the composite material shell containing the metal connecting piece prepared by the method contains nonpolar groups, has certain steric hindrance and can prevent gas from passing through; the hydroxyl can improve the wettability of a resin matrix and fibers, enhance the bonding property of resin and a metal surface, greatly improve the sealing property of the composite material shell and improve the safety coefficient of the composite material shell in the application process; the silane coupling agent contains epoxy groups and amino groups, and can participate in reaction in the heating and curing process of resin to improve the crosslinking density, so that the gas barrier property at the interface of the winding structure layer and the metal connecting piece is greatly improved.

Description

Forming method of pressure-resistant composite material shell
Technical Field
The invention belongs to the field of molding of fiber composite material shells, and particularly relates to a molding method of a high-gas-barrier-property pressure-resistant composite material shell.
Background
Based on the consideration of light weight, fiber reinforced resin matrix composite materials are widely applied to advanced rocket weapon systems, such as engine housings, launching barrel housings and the like. The composite material product bears complex load effects such as high temperature, high internal pressure and the like, a metal connecting piece is usually embedded at a port of a composite material shell, and under the action of pressure, a plurality of micropores are generated at an interface between a composite material structure layer and the metal connecting piece, so that the air leakage phenomenon exists, and how to improve the pressure resistance and the air tightness at the interface is a key for the application of the composite material shell.
At present, the air tightness is improved by adopting a mode of arranging a rubber layer between a composite material structure layer and a metal connecting piece, and the thickness of a shell can be greatly increased by the rubber layer in consideration of the characteristic of small-size space of a rocket weapon system, so that the filling amount of ammunition is influenced.
Disclosure of Invention
The invention aims to solve the problem of poor air tightness of an interface between a composite material structure layer and a metal connecting piece, and provides a method for forming a pressure-resistant composite material shell.
The invention aims to realize that the surface of the metal connecting piece after sand blasting treatment is bombarded by oxygen negative plasma to graft active groups, silane coupling agent solution with amino or/and epoxy groups is uniformly coated on the metal connecting piece, the metal connecting piece is dried to realize surface modification of the metal connecting piece, then the metal connecting piece is arranged on a winding mould, a composite material shell is formed by winding through a wet winding process, and the winding resin is epoxy resin mixed glue solution containing nonpolar branched chains and hydroxyl groups. The nonpolar group has certain steric hindrance and can block gas from passing through; the hydroxyl can improve the wettability of the resin matrix and the fiber and enhance the bonding property of the resin and the metal surface; the silane coupling agent contains epoxy groups and amino groups, and can participate in reaction in the heating and curing process of resin to improve the crosslinking density, so that the air tightness of the interface between the winding structure layer and the metal connecting piece is greatly improved.
The invention relates to a molding method of a pressure-resistant composite material shell, which is characterized by comprising the following steps of:
1) Preparing a silane coupling agent solution: mixing a silane coupling agent with amino or/and epoxy groups with ethanol according to the mass ratio of 1 (24-29), and adjusting the pH value to 4.5-5.5 by using acetic acid;
2) Performing plasma activation treatment on the surface of the metal connecting piece: carrying out plasma activation treatment on the surface of the metal connecting piece in a plasma generator chamber by using high-purity oxygen;
3) Preparing a resin glue solution for winding forming: according to the mass ratio of 1: (0.4-0.5): (0.3-0.4) mixing liquid bisphenol A epoxy resin, modified TDE-85 resin and amine curing agent to prepare epoxy resin mixed glue solution containing nonpolar branched chains and hydroxyl;
4) Grafting treatment of the surface of the metal connecting piece: brushing a silane coupling agent solution on the surface of the metal connecting piece, and drying;
5) Winding and forming: installing the metal connecting piece subjected to surface grafting treatment on a winding mould, pouring the prepared resin glue solution for winding forming into a glue tank, and winding and forming by using a wet winding process;
6) And (5) curing and forming.
The invention relates to a molding method of a pressure-resistant composite material shell, which is characterized by comprising the following steps: the silane coupling agent with amino is KH-550 or KH-540, and the silane coupling agent with epoxy group is KH-560 or KH-561.
The invention relates to a molding method of a pressure-resistant composite material shell, which is characterized by comprising the following steps: the silane coupling agent with amino and epoxy groups is KH-550 and KH-560, and the mass ratio of the silane coupling agent with amino and epoxy groups is 1 (0.5-0.7).
The invention relates to a molding method of a pressure-resistant composite material shell, which is characterized by comprising the following steps: the dosage of the silane coupling agent solution in the surface grafting treatment process of the metal connecting piece is 20-30 wt% of the dosage of the resin glue solution in the winding process.
The invention relates to a molding method of a pressure-resistant composite material shell, which is characterized by comprising the following steps: the vacuum degree of the chamber is not less than 10 in the plasma activation treatment process -3 Pa, oxygen flow rate of 40-50 sccm, bombardment power of 50-80W, and time of 30-60 min.
The invention relates to a molding method of a pressure-resistant composite material shell, which is characterized by comprising the following steps: the liquid bisphenol A type epoxy resin in the resin glue solution for winding molding is E-51, BE-188EL or a mixture of the E-51 and the BE-188 EL.
The modified TDE-85 resin is prepared by reacting one glycidyl group of the TDE-85 resin with a carboxyl group in methacrylic acid; the amine curing agent is DDM or DDS.
The invention relates to a molding method of a pressure-resistant composite material shell, which is characterized by comprising the following steps: the resin glue solution for winding molding comprises the following components in parts by mass: modified TDE-85 resin: curing agent =100 (43 to 46): (35-38).
The invention relates to a molding method of a pressure-resistant composite material shell, which is characterized by comprising the following steps: the resin glue solution consumption in the winding process is 30-40 wt% of the composite material shell.
The invention relates to a molding method of a pressure-resistant composite material shell, wherein a nonpolar group of the prepared composite material shell containing a metal connecting piece has certain steric hindrance and can block gas from passing through; the hydroxyl can improve the wettability of a resin matrix and fibers, enhance the bonding property of resin and a metal surface, greatly improve the sealing property of the composite material shell and improve the safety coefficient of the composite material shell in the application process; the silane coupling agent contains epoxy groups and amino groups, and can participate in reaction in the heating and curing process of resin to improve the crosslinking density, so that the pressure resistance and the air tightness of the interface between the winding structure layer and the metal connecting piece are greatly improved.
Detailed Description
The present invention will be further described with reference to the following examples, but the technical solution of the present invention is not limited to the specific embodiments listed below. The invention is not limited to the specific embodiments described above, but rather to specific embodiments described herein. The materials not specifically mentioned are all in parts by mass.
Example one
Weighing 2g of KH-550 silane coupling agent, pouring into a beaker, adding 48g of ethanol, stirring to dissolve, adjusting the pH of the solution to 4.5-5.5 with acetic acid, and treating for 10min with a 40KHz ultrasonic cleaner to obtain the silane coupling agent solution.
Weighing E-51 resin, modified TDE-85 resin and a DDM curing agent according to a mass ratio of 100.
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 1 x 10 -3 Pa, introducing high-purity oxygen with the flow rate of 40sccm, adjusting the power of the plasma generator to 50W, and enabling oxygen anions to bombard the metal pieceSurface, time control is 30min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 20wt% of resin glue solution for winding, brushing the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 70 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding and forming, adding the resin glue solution into a glue tank of a numerical control winding machine, winding by utilizing T-700S carbon fibers, wherein a winding layer is designed to be 2 layers of spiral winding layers → 1 layer of ring winding layers, the spiral direction winding angle is 45 degrees, and the using amount of the glue solution is controlled to be 30 degrees in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven, wherein the curing process comprises pre-curing at 80 ℃ for 40min, curing at 140 ℃ for 2h, and taking out the mold after curing to obtain the composite shell.
And performing a hydraulic bursting test on the composite material shell, wherein the result shows that the pressure is maintained for 5min under 5MPa, the shell has no water leakage phenomenon, and the bursting pressure is 7MPa.
Example two
Weighing 2g of KH-560 silane coupling agent, pouring into a beaker, adding 50g of ethanol, stirring to dissolve, adjusting the pH of the solution to 4.5-5.5 with acetic acid, and treating for 10min with a 40KHz ultrasonic cleaner to obtain a silane coupling agent solution.
Weighing BE-188EL resin, modified TDE-85 resin and DDS curing agent according to the mass ratio of 100 to 50, adding into a reaction kettle, controlling the temperature at 70 ℃, and stirring for 30min to prepare resin glue solution for winding molding.
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 5 x 10 -3 And Pa, introducing high-purity oxygen with the flow rate of 50sccm, adjusting the power of the plasma generator to 80W, and enabling oxygen anions to bombard the surface of the metal piece for 60min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 30wt% of resin glue solution for winding, brush-coating the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 70 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding forming, adding the resin glue solution into a glue groove of a numerical control winding machine, winding by using high-strength glass fiber yarns, wherein a winding layer is designed to be a 2-layer spiral winding layer → 1-layer circular winding layer, the spiral direction winding angle is 50 degrees, and the using amount of the glue solution is controlled to be 40 degrees in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven at 40min at 85 ℃ and 2h at 170 ℃, and taking out the mold after curing to obtain the composite shell.
And (3) performing a hydraulic bursting test on the composite material shell, wherein the result shows that the pressure is maintained for 5min under 2MPa, the shell has no water leakage phenomenon, and the bursting pressure is 4MPa.
EXAMPLE III
Weighing 2g of KH-540 silane coupling agent, pouring into a beaker, adding 52g of ethanol, stirring to dissolve, adjusting the pH of the solution to 4.5-5.5 with acetic acid, and treating for 10min by using a 40KHz ultrasonic cleaner to prepare the silane coupling agent solution.
Weighing E-51 resin, BE-188EL resin, modified TDE-85 resin and DDM curing agent according to a mass ratio of 60.
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 8 x 10 -3 And Pa, introducing high-purity oxygen with the flow rate of 45sccm, adjusting the power of the plasma generator to 65W, and enabling oxygen anions to bombard the surface of the metal piece for 45min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 23wt% of resin glue solution for winding, brush-coating the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 60 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding and forming, adding the resin glue solution into a glue tank of a numerical control winding machine, winding by utilizing T-700S carbon fiber yarns, wherein a winding layer is designed to be 2 layers of spiral winding layers → 1 layer of ring winding layers, the spiral direction winding angle is 55 degrees, and the using amount of the glue solution is controlled to be 35 percent in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven, wherein the curing process comprises pre-curing at 85 ℃ for 40min, curing at 130 ℃ for 2h, and taking out the mold after curing to obtain the composite material shell.
The composite shell is subjected to a hydraulic bursting test, and the result shows that the composite shell is kept for 5min under 5MPa, the shell has no water leakage phenomenon, and the bursting pressure is 8MPa.
Example four
Weighing 2g of KH-561 silane coupling agent, pouring into a beaker, adding 54g of ethanol solution, stirring to dissolve, adjusting the pH of the solution to 4.5-5.5 with acetic acid, and treating for 10min with a 40KHz ultrasonic cleaner to obtain the silane coupling agent solution.
Weighing E-51 resin, BE-188EL resin, modified TDE-85 resin and DDM curing agent according to the mass ratio of 35.
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 7 x 10 -3 And Pa, introducing high-purity oxygen with the flow of 46sccm, adjusting the power of the plasma generator to 64W, and enabling oxygen anions to bombard the surface of the metal piece for 42min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 27wt% of resin glue solution for winding, brush-coating the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 60 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding forming, adding the resin glue solution into a glue tank of a numerical control winding machine, winding by using high-strength glass fiber yarns, wherein a winding layer is designed to be 2 layers of spiral winding layers → 1 layer of ring winding layers, the spiral direction winding angle is 55 degrees, and the using amount of the glue solution is controlled to be 37 degrees in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven at 40min at 85 ℃ and 2h at 130 ℃, and taking out the mold after curing to obtain the composite shell.
And performing a hydraulic bursting test on the composite material shell, wherein the result shows that the pressure is maintained for 5min under 2MPa, the shell has no water leakage phenomenon, and the bursting pressure is 5MPa.
EXAMPLE five
Weighing 2g of KH-550 and KH-560 silane coupling agent in total according to the mass ratio of 1.
Weighing E-51 resin, BE-188EL resin, modified TDE-85 resin and DDS curing agent according to the mass ratio of 75.
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 6 x 10 -3 Pa, introducing high-purity oxygen with the flow rate of 42sccm, adjusting the power of the plasma generator to 55W, and enabling oxygen anions to bombard the surface of the metal piece for 35min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 20wt% of resin glue solution for winding, brush-coating the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 75 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding and forming, adding the resin glue solution into a glue tank of a numerical control winding machine, winding by utilizing T-700S carbon fiber, wherein a winding layer is designed to be 2 layers of spiral winding layers → 1 layer of ring winding layers, the spiral direction winding angle is 45 degrees, and the using amount of the glue solution is controlled to be 40 degrees in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven at 85 ℃ for 45min and 175 ℃ for 2h, and taking out the mold after curing to obtain the composite shell.
The composite shell is subjected to a hydraulic bursting test, the result shows that the composite shell is kept for 5min under 5MPa, the shell has no water leakage phenomenon, and the bursting pressure is 13MPa.
Example six
Weighing 2g of KH-550 and KH-560 silane coupling agents according to the mass ratio of 1.
Weighing BE-188EL resin, modified TDE-85 resin and DDM curing agent according to the mass ratio of (100).
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 5 multiplied by 10 -3 And Pa, introducing high-purity oxygen with the flow rate of 48sccm, adjusting the power of the plasma generator to 70W, and enabling oxygen anions to bombard the surface of the metal piece for 55min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 24wt% of resin glue solution for winding, brush-coating the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 64 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding forming, adding the resin glue solution into a glue tank of a numerical control winding machine, winding by using high-strength glass fiber yarns, wherein a winding layer is designed to be a 2-layer spiral winding layer → 1-layer circular winding layer, the spiral direction winding angle is 50 degrees, and the using amount of the glue solution is controlled to be 36 degrees in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven, wherein the curing process comprises pre-curing at 85 ℃ for 30min, curing at 136 ℃ for 2h, and taking out the mold after curing to obtain the composite shell.
The composite shell is subjected to a hydraulic bursting test, and the result shows that the composite shell is kept for 5min under 2MPa, the shell has no water leakage phenomenon, and the bursting pressure is 12MPa.
EXAMPLE seven
Weighing 2g of KH-550 and KH-560 silane coupling agents according to the mass ratio of 1.
Weighing E-51 resin, BE-188EL resin, modified TDE-85 resin and DDS curing agent according to the mass ratio of 50.
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 8 x 10 -3 Pa, introducing high-purity oxygen with the flow of 44sccm, adjusting the power of the plasma generator to 60W, and enabling the oxygen anions to bombard the surface of the metal piece for 40min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 26wt% of resin glue solution for winding, brush-coating the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 65 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding forming, adding the resin glue solution into a glue tank of a numerical control winding machine, winding by utilizing T-700S carbon fiber yarns, wherein a winding layer is designed to be 2 layers of spiral winding layers → 1 layer of ring winding layers, the spiral direction winding angle is 55 degrees, and the using amount of the glue solution is controlled to be 30 percent in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven at 84 ℃ for 45min and 165 ℃ for 2h, and taking out the mold after curing to obtain the composite shell.
The composite shell is subjected to a hydraulic bursting test, the result shows that the composite shell is kept for 5min under 5MPa, the shell has no water leakage phenomenon, and the bursting pressure is 11MPa.
Example eight
Weighing 2g of KH-550 and KH-560 silane coupling agent according to the mass ratio of 1.
Weighing E-51 resin, modified TDE-85 resin and DDS curing agent according to a mass ratio of 100.
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 6 x 10 -3 And Pa, introducing high-purity oxygen with the flow rate of 40sccm, adjusting the power of the plasma generator to 50W, and enabling oxygen anions to bombard the surface of the metal piece for 30min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 30wt% of resin glue solution for winding, brush-coating the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 66 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding forming, adding the resin glue solution into a glue tank of a numerical control winding machine, winding by utilizing T-700S carbon fiber, wherein a winding layer is designed to be 2 layers of spiral winding layers → 1 layer of ring winding layers, the spiral direction winding angle is 48 degrees, and the using amount of the glue solution is controlled to be 30 percent in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven, wherein the curing process comprises pre-curing at 83 ℃ for 40min, curing at 170 ℃ for 2.5h, and taking out the mold after curing to obtain the composite shell.
The composite shell is subjected to a hydraulic bursting test, and the result shows that the composite shell is kept for 5min under 5MPa, the shell has no water leakage phenomenon, and the bursting pressure is 8.5MPa.
Example nine
Weighing 2g of KH-550 and KH-560 silane coupling agent in total according to the mass ratio of 2.
Weighing BE-188EL resin, modified TDE-85 resin and DDM curing agent according to the mass ratio of (100) - (48), adding into a reaction kettle, controlling the temperature at 63 ℃, and stirring for 30min to obtain the resin glue solution for winding forming.
Cleaning the surface of the metal piece subjected to sand blasting by using acetone, then placing the metal piece into a plasma generator chamber, and vacuumizing the chamber to 5 multiplied by 10 -3 And Pa, introducing high-purity oxygen with the flow rate of 50sccm, adjusting the power of the plasma generator to 80W, and enabling oxygen anions to bombard the surface of the metal piece for 60min.
Weighing silane coupling agent solution, controlling the using amount of the silane coupling agent solution to be 25wt% of resin glue solution for winding, brush-coating the silane coupling agent solution on the surface of a metal piece treated by plasma, drying at 70 ℃, cleaning the surface of a winding mould of a composite material shell, coating a release agent, installing the metal piece on the mould, erecting the mould on a winding machine, weighing 100g of resin glue solution for winding forming, adding the resin glue solution into a glue groove of a numerical control winding machine, winding by using high-strength glass fiber yarns, wherein a winding layer is designed to be a 2-layer spiral winding layer → 1-layer circular winding layer, the spiral direction winding angle is 50 degrees, and the using amount of the glue solution is controlled to be 40 degrees in the winding process. And taking down the mold after winding, curing in a rotary curing drying oven at 85 ℃ for 45min and 136 ℃ for 2.5h, and taking out the mold after curing to obtain the composite shell.
The composite shell is subjected to a hydraulic bursting test, and the result shows that the composite shell is kept for 5min under 2MPa, the shell has no water leakage phenomenon, and the bursting pressure is 5MPa.

Claims (8)

1. A molding method of a pressure-resistant composite material shell comprises the following operation steps:
1) Preparation of silane coupling agent solution: mixing a silane coupling agent with amino or/and epoxy groups with ethanol according to the mass ratio of 1 (24-29), and adjusting the pH value to 4.5-5.5 by using acetic acid;
2) Performing plasma activation treatment on the surface of the metal connecting piece: carrying out plasma activation treatment on the surface of the metal connecting piece in a plasma generator chamber by using high-purity oxygen;
3) Preparing a resin glue solution for winding forming: according to the mass ratio of 1: (0.4-0.5): (0.3-0.4) mixing liquid bisphenol A epoxy resin, modified TDE-85 resin prepared by reacting one glycidyl group of the TDE-85 resin with a carboxyl group in methacrylic acid and an amine curing agent to prepare epoxy resin mixed glue solution containing a nonpolar branched chain and a hydroxyl group;
4) Grafting treatment of the surface of the metal connecting piece: brushing a silane coupling agent solution on the surface of the metal connecting piece, and drying;
5) Winding and forming: installing the metal connecting piece subjected to surface grafting treatment on a winding mould, pouring the prepared resin glue solution for winding forming into a glue tank, and winding and forming by using a wet winding process;
6) And (5) curing and forming.
2. The method of molding a pressure resistant composite shell as recited in claim 1, wherein: the silane coupling agent with amino is KH-550 or KH-540, and the silane coupling agent with epoxy group is KH-560 or KH-561.
3. The method of molding a pressure resistant composite shell as claimed in claim 1, wherein: the silane coupling agent with amino and epoxy groups is KH-550 and KH-560, and the mass ratio of the silane coupling agent with amino and epoxy groups is 1 (0.5-0.7).
4. The method of molding a pressure resistant composite shell as recited in claim 1, wherein: the dosage of the silane coupling agent solution in the surface grafting treatment process of the metal connecting piece is 20-30 wt% of the dosage of the resin glue solution in the winding process.
5. The method of molding a pressure resistant composite shell as recited in claim 1, wherein: in the surface plasma activation treatment process of the metal connecting piece, the vacuum degree of a cavity is not less than 1 multiplied by 10 -3 Pa, the flow rate of the high-purity oxygen is 40-50 sccm, the bombardment power is 50-80W, and the time is 30-60 min.
6. The method of molding a pressure resistant composite shell as recited in claim 1, wherein: the resin glue solution consumption in the winding process is 30-40 wt% of the composite material shell.
7. The method of molding a pressure resistant composite shell as claimed in claim 1, wherein: the liquid bisphenol A type epoxy resin in the resin glue solution for winding molding is E-51, BE-188EL or a mixture of the E-51 and the BE-188 EL; the amine curing agent is DDM or DDS.
8. The method of molding a pressure resistant composite shell as claimed in claim 1, wherein: in the process of preparing the resin glue solution for winding and forming, the bisphenol A epoxy resin: modified TDE-85 resin: the mass ratio of the curing agent is 1 (0.43-0.46): (0.35-0.38).
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