CN111040379A - Low-temperature resin system used in liquid oxygen environment and preparation method and application thereof - Google Patents
Low-temperature resin system used in liquid oxygen environment and preparation method and application thereof Download PDFInfo
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- CN111040379A CN111040379A CN201911168467.6A CN201911168467A CN111040379A CN 111040379 A CN111040379 A CN 111040379A CN 201911168467 A CN201911168467 A CN 201911168467A CN 111040379 A CN111040379 A CN 111040379A
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- 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
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention relates to a low-temperature resin system used in a liquid oxygen environment, and a preparation method and application thereof, and discloses a low-temperature resin system which can be safely used in a liquid oxygen environment and can be used in the technical field of manufacturing of composite material gas cylinders in the liquid oxygen environment. The epoxy resin system meets the requirements of a wet winding process on viscosity and a shelf life, and can be compounded with carbon fibers to prepare a high-performance composite material. Meanwhile, the epoxy resin system has high low-temperature strength and toughness, flame retardance and compatibility with a liquid oxygen medium.
Description
Technical Field
The invention relates to a low-temperature resin system used in a liquid oxygen environment, and a preparation method and application thereof, and discloses a low-temperature resin system which can be safely used in a liquid oxygen environment and can be used in the technical field of manufacturing of composite material gas cylinders in the liquid oxygen environment.
Background
The new generation of nontoxic pollution-free low-temperature carrier rocket uses low-temperature propellant, and the subsequent new generation of manned rocket and heavy carrier rocket also uses low-temperature propellant. With the increasing demands on carrying capacity and efficiency, placing a high-pressure gas cylinder in a low-temperature propellant is a very effective scheme, and the weight of the rocket body structure can be obviously reduced.
The high-pressure gas cylinder used by the cold helium pressurization system of the new generation of carrier rocket is still made of metal materials, and the existing composite material gas cylinder is embrittled in the low-temperature environment of liquid oxygen of 90K and is incompatible with a liquid oxygen medium, so that the high-pressure gas cylinder cannot be applied to the cold helium pressurization system of the new generation of carrier rocket.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the resin system can be safely used in a liquid oxygen environment, has good strength and toughness at a low temperature of 77K, is compatible with a liquid oxygen medium, and can be safely applied to the liquid oxygen environment together with a composite material gas cylinder made of carbon fibers.
The technical solution of the invention is as follows:
a low-temperature resin system used in a liquid oxygen environment comprises epoxy resin, an active toughening agent, a modifier and a curing agent, wherein the epoxy resin comprises the following components in parts by mass based on 100 parts by mass:
epoxy resin 100 parts
5-25 parts of active toughening agent
5-25 parts of modifier
15-30 parts of curing agent
The epoxy resin is at least one of bisphenol A epoxy resin, bisphenol F epoxy resin and hydantoin epoxy resin;
the active toughening agent is one or a mixture of two of epoxy-terminated hyperbranched polyphosphate and epoxy-terminated polysiloxane, and is used for improving the low-temperature strength and low-temperature toughness of a resin system, reducing the viscosity of the resin system and simultaneously improving the liquid oxygen compatibility and heat resistance of the resin system;
the modifier is at least one of phosphorus-containing epoxy resin, brominated epoxy resin, phosphate flame retardant and cyclotriphosphazene flame retardant, and is used for improving the liquid oxygen compatibility of a resin system;
the curing agent is modified aromatic amine, the raw materials of the modified aromatic amine comprise at least two of diethyl toluene diamine, m-phenylenediamine, 4 '-diaminodiphenylmethane and 4, 4' -diaminodiphenylsulfone, and the modified aromatic amine is obtained by compounding the raw materials.
A method for preparing a low temperature resin system for use in a liquid oxygen environment, the method comprising the steps of:
(1) heating and uniformly stirring the epoxy resin, the active toughening agent and the modifier to obtain a transparent liquid A, wherein the heating temperature is 60-150 ℃, and the stirring speed is 100-500 RPM;
(2) heating and stirring the raw materials of the curing agent to obtain a brownish red transparent liquid B, wherein the heating temperature is 70-200 ℃, and the stirring speed is 100-500 RPM;
(3) mixing the transparent liquid A and the brownish red transparent liquid B, heating to 35-45 ℃, uniformly stirring, vacuumizing, degassing, heating and curing, wherein the mass ratio of A to B is 100:15-30, and the curing process conditions are as follows: keeping the temperature of 80-100 ℃ for 2-6h, keeping the temperature of 110-130 ℃ for 2-6h, keeping the temperature of 140-160 ℃ for 2-6h, and cooling to obtain a low-temperature resin system with high low-temperature strength, toughness, flame retardance and compatibility with liquid oxygen media.
The liquid oxygen environment is compounded with carbon fibers by using the low-temperature resin system to prepare a carbon fiber composite material, the prepared carbon fiber composite material is wound by a wet method to prepare a composite material gas cylinder, and the prepared composite material gas cylinder can be safely used in the liquid oxygen environment.
Advantageous effects
(1) The low-temperature resin has good low-temperature mechanical properties, the tensile strength of a resin casting body at a low temperature of 77K is not less than 100MPa, the elongation at break is not less than 2 percent, and the impact toughness is not less than 20kJ/m2And the use in a 90K liquid oxygen temperature region is completely met. After the resin casting body is subjected to multiple room temperature-liquid oxygen temperature impacts, the mechanical properties of the resin casting body are not changed at room temperature and 77K;
(2) the spontaneous combustion temperature in the pure oxygen of the low-temperature resin casting body exceeds 300 ℃, and the oxygen index is more than 22%;
(3) the composite gas cylinder manufactured by winding the low-temperature resin system/the carbon fiber can be safely used in a liquid oxygen environment.
(4) The epoxy resin system meets the requirements of a wet winding process on viscosity and a shelf life, and can be compounded with carbon fibers to prepare a high-performance composite material. Meanwhile, the epoxy resin system has high low-temperature strength and toughness, flame retardance and compatibility with a liquid oxygen medium.
Detailed Description
The present invention will be described in further detail with reference to examples, wherein the parts are by mass.
Example 1
(1) Heating and uniformly stirring 75 parts of bisphenol A epoxy resin, 15 parts of epoxy-terminated hyperbranched polyphosphate and 10 parts of phosphorus-containing epoxy resin to obtain transparent liquid A, wherein the heating temperature is 60 ℃, and the stirring speed is 100 RPM;
(2) heating and stirring 12 parts of diethyl toluenediamine and 12 parts of 4, 4' -diaminodiphenylmethane to obtain a brownish red transparent liquid B, wherein the heating temperature is 90 ℃, and the stirring speed is 100 RPM;
(3) mixing 100 parts of transparent liquid A and 24 parts of brownish red transparent liquid B, heating to 40 ℃, uniformly stirring, vacuumizing, degassing, and heating for curing. The curing process conditions are as follows: keeping the temperature at 80 ℃ for 5h, keeping the temperature at 110 ℃ for 4h, and keeping the temperature at 140 ℃ for 3 h.
Example 2
(1) Heating and uniformly stirring 80 parts of bisphenol F epoxy resin, 8 parts of epoxy-terminated polysiloxane and 12 parts of brominated epoxy resin to obtain transparent liquid A, wherein the heating temperature is 60 ℃, and the stirring speed is 300 RPM;
(2) heating and stirring 15 parts of diethyl toluenediamine and 12 parts of 4, 4' -diamino diphenyl sulfone to obtain a brownish red transparent liquid B, wherein the heating temperature is 150 ℃, and the stirring speed is 200 RPM;
(3) mixing 100 parts of transparent liquid A and 27 parts of brownish red transparent liquid B, heating to 40 ℃, uniformly stirring, vacuumizing, degassing, and heating for curing. The curing process conditions are as follows: keeping the temperature at 90 ℃ for 5h, keeping the temperature at 120 ℃ for 3h, and keeping the temperature at 150 ℃ for 3 h.
Example 3
(1) Heating and uniformly stirring 30 parts of bisphenol A epoxy resin, 30 parts of bisphenol F epoxy resin, 20 parts of epoxy-terminated hyperbranched polyphosphate and 20 parts of brominated epoxy resin to obtain transparent liquid A, wherein the heating temperature is 60 ℃, and the stirring speed is 400 RPM;
(2) heating and stirring 10 parts of diethyl toluenediamine, 5 parts of m-phenylenediamine and 5 parts of 4, 4' -diaminodiphenylmethane to obtain a brownish red transparent liquid B, wherein the heating temperature is 70 ℃, and the stirring speed is 300 RPM;
(3) mixing 100 parts of the transparent liquid A and 30 parts of the brownish red transparent liquid B, heating to 45 ℃, uniformly stirring, vacuumizing, degassing, and heating for curing. The curing process conditions are as follows: keeping the temperature at 80 ℃ for 6h, keeping the temperature at 120 ℃ for 3h, and keeping the temperature at 160 ℃ for 2 h.
Example 4
(1) Heating and uniformly stirring 40 parts of bisphenol A epoxy resin, 40 parts of hydantoin epoxy resin, 15 parts of epoxy-terminated hyperbranched polyphosphate and 5 parts of cyclotriphosphazene flame retardant to obtain transparent liquid A, wherein the heating temperature is 120 ℃, and the stirring speed is 300 RPM;
(2) heating 8 parts of diethyl toluenediamine and 12 parts of 4, 4' -diaminodiphenylmethane and stirring to obtain a brownish red transparent liquid B, wherein the heating temperature is 100 ℃, and the stirring speed is 200 RPM;
(3) mixing 100 parts of the transparent liquid A and 20 parts of the brownish red transparent liquid B, heating to 45 ℃, uniformly stirring, vacuumizing, degassing, and heating for curing. The curing process conditions are as follows: keeping the temperature at 90 ℃ for 5h, keeping the temperature at 120 ℃ for 3h, and keeping the temperature at 150 ℃ for 3 h.
Example 5
(1) Heating and uniformly stirring 40 parts of bisphenol F epoxy resin, 30 parts of hydantoin epoxy resin, 5 parts of epoxy-terminated hyperbranched polyphosphate, 10 parts of phosphate flame retardant and 15 parts of cyclotriphosphazene flame retardant to obtain transparent liquid A, wherein the heating temperature is 100 ℃, and the stirring speed is 300 RPM;
(2) heating and stirring 15 parts of diethyl toluene diamine and 3 parts of m-phenylenediamine to obtain a brownish red transparent liquid B, wherein the heating temperature is 70 ℃, and the stirring speed is 200 RPM.
(3) Mixing 100 parts of transparent liquid A and 18 parts of brownish red transparent liquid B, heating to 35 ℃, uniformly stirring, vacuumizing, degassing, and heating for curing. The curing process conditions are as follows: keeping the temperature at 100 ℃ for 3h, keeping the temperature at 130 ℃ for 5h, and keeping the temperature at 160 ℃ for 3 h.
Comparative example 1
(1) Heating 85 parts of bisphenol A epoxy resin and 15 parts of epoxy-terminated butadiene-acrylonitrile rubber, and uniformly stirring to obtain transparent liquid A, wherein the heating temperature is 70 ℃, and the stirring speed is 300 RPM;
(2) mixing 100 parts of transparent liquid A and 20 parts of diethyl toluenediamine, heating to 45 ℃, uniformly stirring, vacuumizing, degassing, and heating for curing. The curing process conditions are as follows: keeping the temperature at 100 ℃ for 5h, keeping the temperature at 130 ℃ for 3h, and keeping the temperature at 150 ℃ for 3 h.
Comparative example 2
(1) Heating and uniformly stirring 40 parts of bisphenol F epoxy resin, 45 parts of hydantoin epoxy resin and 15 parts of epoxy-terminated butadiene-acrylonitrile rubber to obtain transparent liquid A, wherein the heating temperature is 70 ℃, and the stirring speed is 300 RPM;
(2) mixing 100 parts of transparent liquid A and 25 parts of diethyl toluenediamine, heating to 40 ℃, uniformly stirring, vacuumizing, degassing, and heating for curing. The curing process conditions are as follows: keeping the temperature at 100 ℃ for 5h, keeping the temperature at 130 ℃ for 3h, and keeping the temperature at 160 ℃ for 3 h.
The above examples and comparative examples were subjected to a liquid oxygen compatibility test in accordance with ASTM G86-17, and a low temperature tensile property test and a low temperature impact property test in accordance with GB/T2567-2008. The test results are shown in table 1:
TABLE 1
Claims (10)
1. A low-temperature resin system used in a liquid oxygen environment is characterized in that: the resin system comprises epoxy resin, an active toughening agent, a modifier and a curing agent, and the mass parts of the epoxy resin are 100 parts, and the mass parts of the components are as follows:
epoxy resin 100 parts
5-25 parts of active toughening agent
5-25 parts of modifier
15-30 parts of a curing agent;
the epoxy resin is at least one of bisphenol A epoxy resin, bisphenol F epoxy resin and hydantoin epoxy resin;
the active toughening agent is one or a mixture of two of epoxy-terminated hyperbranched polyphosphate and epoxy-terminated polysiloxane;
the modifier is at least one of phosphorus-containing epoxy resin, brominated epoxy resin, phosphate flame retardant and cyclotriphosphazene flame retardant;
the curing agent is modified aromatic amine, and the raw materials of the modified aromatic amine comprise at least two of diethyl toluene diamine, m-phenylenediamine, 4 '-diaminodiphenylmethane and 4, 4' -diaminodiphenylsulfone.
2. A method for preparing a low-temperature resin system used in a liquid oxygen environment is characterized by comprising the following steps:
(1) mixing epoxy resin, an active toughening agent and a modifier, stirring and heating to obtain liquid A;
(2) mixing and heating raw materials of a curing agent to obtain liquid B;
(3) and (3) mixing the liquid A obtained in the step (1) and the liquid B obtained in the step (2), stirring, heating to 35-45 ℃, vacuumizing, degassing, and curing to obtain a low-temperature resin system.
3. The method for preparing a low-temperature resin system for liquid oxygen environment according to claim 2, wherein the low-temperature resin system comprises the following steps: in the step (1), the stirring speed is 100-500 RPM.
4. The method for preparing a low-temperature resin system for liquid oxygen environment according to claim 2, wherein the low-temperature resin system comprises the following steps: in the step (1), the heating temperature is 60-150 ℃.
5. The method for preparing a low-temperature resin system for liquid oxygen environment according to claim 2, wherein the low-temperature resin system comprises the following steps: in the step (2), the stirring speed is 100-500 RPM.
6. The method for preparing a low-temperature resin system for liquid oxygen environment according to claim 2, wherein the low-temperature resin system comprises the following steps: in the step (2), the heating temperature is 70-200 ℃.
7. The method for preparing a low-temperature resin system for liquid oxygen environment according to claim 2, wherein the low-temperature resin system comprises the following steps: in the step (3), the mass ratio of the liquid A to the liquid B is 100: 15-30.
8. The method for preparing a low-temperature resin system for liquid oxygen environment according to claim 2, wherein the low-temperature resin system comprises the following steps: in the step (3), the curing conditions are as follows: firstly, preserving heat for 2-6h at the temperature of 80-100 ℃, then heating to the temperature of 110-130 ℃, preserving heat for 2-6h, finally heating to the temperature of 140-160 ℃, preserving heat for 2-6h, and cooling to the room temperature.
9. The application of the low-temperature resin system used in the liquid oxygen environment is characterized in that: the low-temperature resin system is compounded with carbon fibers to prepare a carbon fiber composite material, and the prepared carbon fiber composite material is wound by a wet method to prepare a composite material gas cylinder.
10. Use of a low temperature resin system for liquid oxygen environments according to claim 9, wherein: the prepared composite material gas cylinder can be safely used in a liquid oxygen environment.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393805A (en) * | 2020-04-23 | 2020-07-10 | 重庆大学 | Epoxy resin system for composite liquid oxygen storage tank and preparation method thereof |
| CN112066240A (en) * | 2020-08-04 | 2020-12-11 | 上海航天精密机械研究所 | High-pressure low-temperature composite material gas cylinder used in liquid oxygen environment and manufacturing method |
| CN116515364A (en) * | 2023-04-26 | 2023-08-01 | 山东新美达科技材料有限公司 | Preparation method of epoxy-polyester back paint |
| CN116515247A (en) * | 2023-04-21 | 2023-08-01 | 大连理工大学 | Epoxy resin system for liquid oxygen storage tank and preparation method of composite material of epoxy resin system |
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| CN109721711A (en) * | 2018-12-25 | 2019-05-07 | 武汉理工大学 | A kind of tough epoxy resin system compatible with liquid oxygen |
| CN110467795A (en) * | 2019-08-09 | 2019-11-19 | 大连理工大学 | A kind of low viscosity liquid oxygen compatible epoxy system and preparation method thereof for wet laid fiber winding |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393805A (en) * | 2020-04-23 | 2020-07-10 | 重庆大学 | Epoxy resin system for composite liquid oxygen storage tank and preparation method thereof |
| CN112066240A (en) * | 2020-08-04 | 2020-12-11 | 上海航天精密机械研究所 | High-pressure low-temperature composite material gas cylinder used in liquid oxygen environment and manufacturing method |
| CN116515247A (en) * | 2023-04-21 | 2023-08-01 | 大连理工大学 | Epoxy resin system for liquid oxygen storage tank and preparation method of composite material of epoxy resin system |
| CN116515364A (en) * | 2023-04-26 | 2023-08-01 | 山东新美达科技材料有限公司 | Preparation method of epoxy-polyester back paint |
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Application publication date: 20200421 |