CN110437584A - Hot setting resin and the preparation method and application thereof - Google Patents
Hot setting resin and the preparation method and application thereof Download PDFInfo
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- CN110437584A CN110437584A CN201910725567.8A CN201910725567A CN110437584A CN 110437584 A CN110437584 A CN 110437584A CN 201910725567 A CN201910725567 A CN 201910725567A CN 110437584 A CN110437584 A CN 110437584A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
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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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2453/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2481/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2481/06—Polysulfones; Polyethersulfones
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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
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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
Abstract
Present invention discloses a kind of hot setting resin and the preparation method and application thereof, the hot setting resin is blended by resin matrix and additive, and hot setting resin includes: 40~100 parts of multiple functionality epoxide resin by mass parts；5~25 parts of low viscosity resin；5~20 parts of toughener；10~30 parts of curing agent；0.1~10 part of curing accelerator.Hot setting resin preparation process of the invention is simple, and preparation cost is low, can be suitable for hot melt technique and prepare prepreg；The prepreg product of preparation has excellent viscosity, paving good manufacturability；The composite material of hot setting resin preparation has the excellent properties such as high-fire resistance, high intensity, high impact-resistant, high resistance to corrosion.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of hot setting resin and preparation method thereof with answer
With.
Background technique
In recent years, the application with epoxy resin-base composite material in aerospace field deepens continuously, due to using item
The harshness of part proposes more strict requirements to its performance.Compared with conventional composite, answering based on aerospace applications
Condensation material will also have good high temperature resistance other than meeting basic mechanical property requirements.And composite material is resistance to
The formula of the hot structure for being heavily dependent on matrix resin and curing system improves resistance to for epoxy-resin systems
It is hot mainly to set about in terms of two, first is that lead people's new construction by epoxy resin or curing agent itself, as polyfunctionality, phenyl ring,
Condensed ring, acid imide, liquid crystal structure etc., to improve its heat resistance；Second is that being changed using the methods of blending, copolymerization to epoxy resin
Property, such as thermoplastic polymer, organosilicon, nano material.
In the application process of composite material, prepreg is a kind of main application form.Hot melt prepreg is molten
Grow up on the basis of liquid infusion process, have many advantages, such as to control precision high, volatile matter content is low, non-environmental-pollution.And it is hot
Molten method technique manufacture prepreg is stringenter to the craftsmanship requirement of resin, including mobility, viscosity, operability etc..Therefore,
A kind of hot setting resin suitable for hot melt prepreg is developed, in addition to other than guaranteeing to reach performance requirement, it is necessary to have
Good craftsmanship, to meet production requirement.
Therefore, in view of the above technical problems, it is necessary to which a kind of hot setting resin and the preparation method and application thereof is provided.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of hot setting resins and the preparation method and application thereof.
To achieve the goals above, the technical solution that one embodiment of the invention provides is as follows:
A kind of hot setting resin, the hot setting resin are blended by resin matrix and additive, hot setting
Resin includes: by mass parts
40~100 parts of multiple functionality epoxide resin；
5~25 parts of low viscosity resin；
5~20 parts of toughener；
10~30 parts of curing agent；
0.1~10 part of curing accelerator.
In one embodiment, the multiple functionality epoxide resin includes four glycidyl group dimethylphenylene diamine, four glycidols
Base diaminodiphenyl-methane, four glycidyl amine of m-xylene diamine, -1,2 dioctyl phthalate two of 4,5 epoxy 7-oxa-bicyclo[4.1.0 shrink sweet
One of grease, triglycidyl group-p- amino-phenol are a variety of.
In one embodiment, viscosity of low viscosity resin at a temperature of 25 DEG C is less than or equal to 15PaS.
In one embodiment, the toughener includes nanopowder thermoplastic toughening agent or methyl methacrylate-propylene
One of acid butyl ester-methyl methacrylate triblock copolymer is a variety of.
In one embodiment, the curing agent is aromatic amine curing agent, and aromatic amine curing agent includes 4,4 '-diamino two
One of benzene sulfone, 4,4 '-diaminodiphenylmethane, m-phenylene diamine (MPD), m-xylene diamine are a variety of.
In one embodiment, the curing accelerator includes modified imidazole, organic phosphorus compound, in boron trifluoride complex
One or more, the modified imidazole includes one of 2-ethyl-4-methylimidazole, 2-methylimidazole or a variety of, described to have
Machine phosphorus compound includes one of boron trifluoride triethyl phosphine, boron trifluoride triisopropyl phosphorus, trimethyl phosphorus, phosphamidon compound
Or it is a variety of, the boron trifluoride complex includes Boron Trifluoride Ethylamine.
Another embodiment of the present invention provides technical solution it is as follows:
A kind of preparation method of hot setting resin, the preparation method include:
S1, be poured into after preheating the multiple functionality epoxide resin of 40~100 mass parts in baking oven temperature 150 DEG C~
In 160 DEG C of reaction kettle, the toughener of 5~25 mass parts is added in reaction kettle, stirring to toughener is all melted and mixed
Solution uniformity is closed, component A is obtained；
S2, the curing accelerator of the curing agent of 10~30 mass parts and 0.1~10 mass parts is added to 5~25 mass parts
Low viscosity resin in, be stirred, obtain B component；
S3, component A is added in 60 DEG C~70 DEG C of reaction kettle and is stirred, then B component is added in reaction kettle, not high
It is stirred at a temperature of 75 DEG C, obtains hot setting resin.
In one embodiment, after the step S3 further include:
Hot setting resin is put into the mold being preheated by curing process, is then placed in autoclave and is carried out
Solidification natural cooling and demoulds after solidification.
In one embodiment, the curing process successively includes the first cure stage, the second cure stage and third solidification rank
Section, wherein 120 DEG C of solidification temperature T1, T2, T3 satisfaction of the first cure stage, the second cure stage and third cure stage≤
T3≤180 DEG C T1 < T2 <, curing time t1, t2, t3 of the first cure stage, the second cure stage and third cure stage are full
Sufficient 1h≤t1=t2=t3≤3h.
The technical solution that yet another embodiment of the invention provides is as follows:
A kind of application according to above-mentioned hot setting resin in hot melt technique manufacture prepreg.
Compared with prior art, it is had the advantages that in the present invention
Hot setting resin preparation process of the invention is simple, and preparation cost is low, can be suitable for hot melt technique and prepare
Prepreg；
The prepreg product of preparation has excellent viscosity, paving good manufacturability；
The composite material of hot setting resin preparation has the superiority such as high-fire resistance, high intensity, high impact-resistant, high resistance to corrosion
Energy.
Specific embodiment
Below with reference to each embodiment, the present invention will be described in detail.But the embodiments such as this are not intended to limit this hair
Bright, component that those skilled in the art are made according to the embodiments such as this, method or transformation functionally include
Within the scope of the present invention.
The invention discloses a kind of hot setting resin, the hot setting resin be blended by resin matrix and additive and
At hot setting resin includes: by mass parts
40~100 parts of multiple functionality epoxide resin；
5~25 parts of low viscosity resin；
5~20 parts of toughener；
10~30 parts of curing agent；
0.1~10 part of curing accelerator.
Preferably, multiple functionality epoxide resin includes four glycidyl group dimethylphenylene diamine, four glycidyl group diamino
Diphenyl methane, four glycidyl amine of m-xylene diamine, -1,2 dicarboxylic acid diglycidyl ester of 4,5 epoxy 7-oxa-bicyclo[4.1.0, three
One of glycidyl-p- amino-phenol etc. is a variety of.
Preferably, viscosity of low viscosity resin at a temperature of 25 DEG C is less than or equal to 15PaS.
Preferably, toughener includes nanopowder thermoplastic toughening agent or methyl methacrylate-butyl acrylate-first
One of base methyl acrylate triblock copolymer etc. is a variety of.
Preferably, curing agent is aromatic amine curing agent, and aromatic amine curing agent includes 4,4 '-diaminodiphenylsulfones, 4,
One of 4 '-diaminodiphenylmethane, m-phenylene diamine (MPD), m-xylene diamine etc. are a variety of.
Preferably, curing accelerator includes one of modified imidazole, organic phosphorus compound, boron trifluoride complex or more
Kind, modified imidazole includes one of 2-ethyl-4-methylimidazole, 2-methylimidazole etc. or a variety of, and organic phosphorus compound includes
One of boron trifluoride triethyl phosphine, boron trifluoride triisopropyl phosphorus, trimethyl phosphorus, phosphamidon compound etc. or a variety of, trifluoro
Changing boron complex includes Boron Trifluoride Ethylamine etc..
The invention also discloses a kind of preparation methods of hot setting resin, comprising:
S1, be poured into after preheating the multiple functionality epoxide resin of 40~100 mass parts in baking oven temperature 150 DEG C~
In 160 DEG C of reaction kettle, the toughener of 5~25 mass parts is added in reaction kettle, stirring to toughener is all melted and mixed
Solution uniformity is closed, component A is obtained.
Preferably, oven temperature is 150 DEG C, preheating time 30min, and mixing time is 3~4h.
S2, the curing accelerator of the curing agent of 10~30 mass parts and 0.1~10 mass parts is added to 5~25 mass parts
Low viscosity resin in, be stirred, obtain B component.
Preferably, mixing time is 30~45min.
S3, component A is added in 60 DEG C~70 DEG C of reaction kettle and is stirred, then B component is added in reaction kettle, not high
It is stirred at a temperature of 75 DEG C, obtains hot setting resin.
Preferably, first step mixing time is 15~20min, and second step mixing time is 20~25min.
Specifically, after step S3 further include:
Hot setting resin is put into the mold being preheated by curing process, is then placed in autoclave and is carried out
Solidification natural cooling and demoulds after solidification.
Preferably, curing process successively includes the first cure stage, the second cure stage and third cure stage, wherein
Solidification temperature T1, T2, T3 of first cure stage, the second cure stage and third cure stage meet 120 DEG C≤T1 < T2 <
T3≤180 DEG C, curing time t1, t2, t3 of the first cure stage, the second cure stage and third cure stage meet 1h≤t1
=t2=t3≤3h.Such as curing process in a specific embodiment are as follows: 120 DEG C/2h+150 DEG C/2h+180 DEG C/2h.
Mechanical property and the heat resistance etc. of resin can be tested after curing process according to corresponding testing standard.
Hot setting resin in the present invention is suitable for hot melt technique manufacture prepreg, hot setting resin is added
Heat fusing becomes flow regime, and prepreg can be prepared by impregnating fiber or fabric with it.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
Hot setting resin in the present embodiment includes: the multiple functionality epoxide resin of 80 mass parts, 10 matter by mass parts
Measure the low viscosity resin of part, the toughener of 10 mass parts, the curing accelerator of the curing agent of 20 mass parts and 0.3 mass parts.
Wherein, multiple functionality epoxide resin is four glycidyl group diaminodiphenyl-methane, and low viscosity resin is bisphenol-A-type asphalt mixtures modified by epoxy resin
Rouge E51, toughener are nanopowder thermoplastic toughening agent polyether sulfone (PES), 4,4 '-diaminodiphenylsulfone of curing agent, solidification
Promotor is boron trifluoride complex (Boron Trifluoride Ethylamine).
Equipment needed for preparing hot setting resin in the present embodiment include: equipped with heating blender, temperature controller and
The pyroreaction kettle and medium temperature reaction kettle of pumped vacuum systems, vacuum drying oven, vacuum pump, blast dry oven.
Hot setting process for preparing resins specifically:
S11,150 DEG C of preheated multiple functionality epoxide resins of 80 mass parts are poured into reaction of the temperature at 150 DEG C
In kettle.The toughener of 15 mass parts is added in reaction kettle, 3h is stirred, until toughener all melts, until mixed solution is uniform
Unanimously, which is known as component A；
S12, the low viscosity resin that the curing agent of 20 mass parts and 0.3 mass parts curing accelerator are added to 10 mass parts
In, it is stirred, mixing time 30min, referred to as B component；
S13, the component A of 95 mass parts is added in 60~70 DEG C of reaction kettle, mixing time 15min, then by 30.3
The B component of mass parts is added in reaction kettle, and temperature is not higher than 75 DEG C, and mixing time 20min presoaks to get to suitable for hot melt
The hot setting resin of material.
The above-mentioned hot setting resin prepared is put into the mold being preheated, is then placed in autoclave,
Setting pressurization size and pressing time, curing process are as follows: 120 DEG C/2h+150 DEG C/2h+180 DEG C/2h.Then, natural cooling,
Demoulding, further according to the mechanical property and heat resistance of corresponding testing standard test resin, performance test data is shown in Table 1.
Embodiment 2:
Hot setting resin in the present embodiment includes: the multiple functionality epoxide resin of 75 mass parts, 15 matter by mass parts
Measure the low viscosity resin of part, the toughener of 13 mass parts, the curing accelerator of the curing agent of 20 mass parts and 6 mass parts.Its
In, multiple functionality epoxide resin is four glycidyl amine of m-xylene diamine, and low viscosity resin is bisphenol-A-type epoxy resin E51, is increased
Tough dose is methyl methacrylate-butyl acrylate-methyl methacrylate triblock copolymer M52N, and curing agent is isophthalic two
Amine (mpda), curing accelerator are organic phosphorus compound (boron trifluoride triethyl phosphine).
Equipment needed for preparing hot setting resin in the present embodiment include: equipped with heating blender, temperature controller and
The pyroreaction kettle and medium temperature reaction kettle of pumped vacuum systems, vacuum drying oven, vacuum pump, blast dry oven.
Hot setting process for preparing resins specifically:
S21,150 DEG C of preheated multiple functionality epoxide resins of 75 mass parts are poured into reaction of the temperature at 160 DEG C
In kettle.The toughener of 13 mass parts is added in reaction kettle, 4h is stirred, until toughener all melts, until mixed solution is uniform
Unanimously, which is known as component A；
S22, the low viscosity resin that the curing agent of 20 mass parts and 6 mass parts curing accelerators are added to 15 mass parts
In, it is stirred, mixing time 45min, referred to as B component；
S23, the component A of 88 mass parts is added in 60~70 DEG C of reaction kettle, mixing time 20min, then by 41 matter
The B component for measuring part is added in reaction kettle, and temperature is not higher than 75 DEG C, and mixing time 25min is to get to suitable for hot melt prepreg
Hot setting resin.
Casting resin is prepared with embodiment 1, performance test data is shown in Table 1.
Embodiment 3:
Hot setting resin in the present embodiment includes: the multiple functionality epoxide resin of 70 mass parts, 10 matter by mass parts
Measure the low viscosity resin of part, the toughener of 20 mass parts, the curing accelerator of the curing agent of 25 mass parts and 0.3 mass parts.
Wherein, multiple functionality epoxide resin is four glycidyl group dimethylphenylene diamine, and low viscosity resin is bisphenol-A-type epoxy resin E51,
Toughener is nanopowder thermoplastic toughening agent polyether sulfone (PES), and curing agent is m-xylene diamine (mxda), and curing accelerator is
Boron trifluoride complex (Boron Trifluoride Ethylamine).
Equipment needed for preparing hot setting resin in the present embodiment include: equipped with heating blender, temperature controller and
The pyroreaction kettle and medium temperature reaction kettle of pumped vacuum systems, vacuum drying oven, vacuum pump, blast dry oven.
Hot setting process for preparing resins specifically:
S31,150 DEG C of preheated multiple functionality epoxide resins of 70 mass parts are poured into reaction of the temperature at 155 DEG C
In kettle.The toughener of 11 mass parts is added in reaction kettle, 3.5h is stirred, until toughener all melts, until mixed solution is equal
Even consistent, which is known as component A；
S32, by 25 mass parts curing agent and 0.3 mass parts curing accelerator be added to the low viscosity trees of 20 mass parts
It in rouge, is stirred, mixing time 35min, referred to as B component；
S33, the component A of 81 mass parts is added in 65 DEG C of reaction kettle, mixing time 17min, then by 45.3 mass
The B component of part is added in reaction kettle, and temperature is not higher than 75 DEG C, and mixing time 22min is to get to suitable for hot melt prepreg
Hot setting resin.
Casting resin is prepared with embodiment 1, performance test data is shown in Table 1.
Embodiment 4:
Hot setting resin in the present embodiment includes: the multiple functionality epoxide resin of 65 mass parts, 25 matter by mass parts
Measure the low viscosity resin of part, the toughener of 9 mass parts, the curing accelerator of the curing agent of 25 mass parts and 5 mass parts.Its
In, 4,5 epoxy 7-oxa-bicyclo[4.1.0-1,2 dicarboxylic acid diglycidyl ester of multiple functionality epoxide resin, low viscosity resin is bis-phenol
A type epoxy resin E44, toughener are methyl methacrylate-butyl acrylate-methyl methacrylate triblock copolymer,
Curing agent is 4,4 '-diaminodiphenylsulfones, and 4,4 '-diaminodiphenylmethane, curing accelerator is that organic phosphorus compound is (borontrifluoride
Boron triisopropyl phosphorus).
Equipment needed for preparing hot setting resin in the present embodiment include: equipped with heating blender, temperature controller and
The pyroreaction kettle and medium temperature reaction kettle of pumped vacuum systems, vacuum drying oven, vacuum pump, blast dry oven.
Hot setting process for preparing resins specifically:
S41,150 DEG C of preheated multiple functionality epoxide resins of 65 mass parts are poured into reaction of the temperature at 158 DEG C
In kettle.The toughener of 9 mass parts is added in reaction kettle, 3.5h is stirred, until toughener all melts, until mixed solution is uniform
Unanimously, which is known as component A；
S42, by 25 mass parts curing agent and 5 mass parts curing accelerators be added to the low viscosity resins of 25 mass parts
In, it is stirred, mixing time 40min, referred to as B component；
S43, the component A of 74 mass parts is added in 68 DEG C of reaction kettle, mixing time 18min, then by 55 mass parts
B component be added reaction kettle in, temperature be not higher than 75 DEG C, mixing time 24min to get to suitable for hot melt prepreg height
Warm solidified resin.
Casting resin is prepared with embodiment 1, performance test data is shown in Table 1.
Embodiment 5:
Hot setting resin in the present embodiment includes: the multiple functionality epoxide resin of 40 mass parts, 5 mass by mass parts
The low viscosity resin of part, the toughener of 5 mass parts, the curing accelerator of the curing agent of 10 mass parts and 0.1 mass parts.Its
In, multiple functionality epoxide resin is triglycidyl group-p- amino-phenol, and low viscosity resin is bisphenol A type epoxy resin E44,
Toughener is nanopowder thermoplastic toughening agent, and curing agent is m-phenylene diamine (MPD) (mpda), and curing accelerator is organic phosphorus compound
(trimethyl phosphorus).
Hot setting process for preparing resins specifically:
S51,150 DEG C of preheated multiple functionality epoxide resins of 40 mass parts are poured into reaction of the temperature at 150 DEG C
In kettle.The toughener of 5 mass parts is added in reaction kettle, 3h is stirred, until toughener all melts, until mixed solution uniform one
It causes, which is known as component A；
S52, by 10 mass parts curing agent and 0.1 mass parts curing accelerator be added to the low viscosity trees of 5 mass parts
It in rouge, is stirred, mixing time 30min, referred to as B component；
S53, the component A of 45 mass parts is added in 60 DEG C of reaction kettle, 15~20min of mixing time, then by 15.1
The B component of mass parts is added in reaction kettle, and temperature is not higher than 75 DEG C, and mixing time 20min presoaks to get to suitable for hot melt
The hot setting resin of material.
Casting resin is prepared with embodiment 1, performance test data is shown in Table 1.
Embodiment 6:
Hot setting resin in the present embodiment includes: the multiple functionality epoxide resin of 100 mass parts, 25 matter by mass parts
Measure the low viscosity resin of part, the toughener of 20 mass parts, the curing accelerator of the curing agent of 30 mass parts and 10 mass parts.
Wherein, multiple functionality epoxide resin is four glycidyl group diaminodiphenyl-methane, and low viscosity resin is bisphenol type epoxy tree
Rouge E44, toughener is methyl methacrylate-butyl acrylate-methyl methacrylate triblock copolymer, between curing agent is
Benzene dimethylamine (mxda), curing accelerator are organic phosphorus compound (phosphamidon compound).
Hot setting process for preparing resins specifically:
S61,150 DEG C of preheated multiple functionality epoxide resins of 100 mass parts are poured into reaction of the temperature at 160 DEG C
In kettle.The toughener of 20 mass parts is added in reaction kettle, 4h is stirred, until toughener all melts, until mixed solution is uniform
Unanimously, which is known as component A；
S62, by 30 mass parts curing agent and 10 mass parts curing accelerators be added to the low viscosity trees of 25 mass parts
It in rouge, is stirred, mixing time 45min, referred to as B component；
S63, the component A of 120 mass parts is added in 70 DEG C of reaction kettle, mixing time 20min, then by 65 mass parts
B component be added reaction kettle in, temperature be not higher than 75 DEG C, mixing time 25min to get to suitable for hot melt prepreg height
Warm solidified resin.
Casting resin is prepared with embodiment 1, performance test data is shown in Table 1.
Table 1: embodiment 1-6 high temperature solidified resin performance data table
As can be seen from the above technical solutions, the invention has the following advantages:
Hot setting resin preparation process of the invention is simple, and preparation cost is low, can be suitable for hot melt technique and prepare
Prepreg；
The prepreg product of preparation has excellent viscosity, paving good manufacturability；
The composite material of hot setting resin preparation has the superiority such as high-fire resistance, high intensity, high impact-resistant, high resistance to corrosion
Energy.
Claims (10)
1. a kind of hot setting resin, which is characterized in that the hot setting resin is blended by resin matrix and additive,
Hot setting resin includes: by mass parts
40~100 parts of multiple functionality epoxide resin；
5~25 parts of low viscosity resin；
5~20 parts of toughener；
10~30 parts of curing agent；
0.1~10 part of curing accelerator.
2. hot setting resin according to claim 1, which is characterized in that the multiple functionality epoxide resin includes four contractings
Water glyceryl dimethylphenylene diamine, four glycidyl group diaminodiphenyl-methane, four glycidyl amine of m-xylene diamine, 4,5 rings
One of -1,2 dicarboxylic acid diglycidyl ester of oxygen 7-oxa-bicyclo[4.1.0, triglycidyl group-p- amino-phenol are a variety of.
3. hot setting resin according to claim 1, which is characterized in that the low viscosity resin is 25 DEG C at a temperature of
Viscosity is less than or equal to 15PaS.
4. hot setting resin according to claim 1, which is characterized in that the toughener includes nanopowder thermoplasticity
One of toughener or methyl methacrylate-butyl acrylate-methyl methacrylate triblock copolymer are a variety of.
5. hot setting resin according to claim 1, which is characterized in that the curing agent is aromatic amine curing agent,
Aromatic amine curing agent include 4,4' diaminodiphenyl sulfone, 4,4 '-diaminodiphenylmethane, m-phenylene diamine (MPD), in m-xylene diamine
It is one or more.
6. hot setting resin according to claim 1, which is characterized in that the curing accelerator include modified imidazole,
One of organic phosphorus compound, boron trifluoride complex are a variety of, the modified imidazole include 2-ethyl-4-methylimidazole,
One of 2-methylimidazole is a variety of, and the organic phosphorus compound includes boron trifluoride triethyl phosphine, three isopropyl of boron trifluoride
One of base phosphorus, trimethyl phosphorus, phosphamidon compound are a variety of, and the boron trifluoride complex includes Boron Trifluoride Ethylamine.
7. a kind of preparation method of hot setting resin, which is characterized in that the preparation method includes:
S1, temperature is poured into after preheating the multiple functionality epoxide resin of 40~100 mass parts in baking oven 150 DEG C~160
DEG C reaction kettle in, the toughener of 5~25 mass parts is added in reaction kettle, stirring all melt and mix molten to toughener
Liquid uniformity, obtains component A；
S2, the curing accelerator of the curing agent of 10~30 mass parts and 0.1~10 mass parts is added to the low of 5~25 mass parts
It in viscosity resin, is stirred, obtains B component；
S3, component A is added in 60 DEG C~70 DEG C of reaction kettle and is stirred, then B component is added in reaction kettle, be not higher than 75
It is stirred at a temperature of DEG C, obtains hot setting resin.
8. the preparation method of hot setting resin according to claim 7, which is characterized in that also wrapped after the step S3
It includes:
Hot setting resin is put into the mold being preheated, is then placed in autoclave and is solidified by curing process,
It natural cooling and is demoulded after solidification.
9. the preparation method of hot setting resin according to claim 8, which is characterized in that the curing process successively wraps
Include the first cure stage, the second cure stage and third cure stage, wherein the first cure stage, the second cure stage and
Solidification temperature T1, T2, T3 of three cure stages meet T3≤180 DEG C 120 DEG C≤T1 < T2 <, and the first cure stage, second are consolidated
Curing time t1, t2, t3 of change stage and third cure stage meet 1h≤t1=t2=t3≤3h.
10. it is a kind of according to claim 1~any one of 6 described in hot setting resin in hot melt technique manufacture prepreg
Application.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111253553A (en) * | 2020-03-13 | 2020-06-09 | 东风汽车集团有限公司 | Epoxy resin for carbon fiber reinforced composite material and application thereof |
| CN112741558A (en) * | 2020-12-30 | 2021-05-04 | 深圳市捷安纳米复合材料有限公司 | Antibacterial sweeper and manufacturing process of garbage storage bin of antibacterial sweeper |
| CN113861385A (en) * | 2021-10-27 | 2021-12-31 | 航天特种材料及工艺技术研究所 | High-thermal-conductivity epoxy resin cured product and preparation method thereof |
| CN113956611A (en) * | 2021-06-30 | 2022-01-21 | 航天材料及工艺研究所 | High-toughness liquid molding resin and composite material based on phase control technology and preparation method thereof |
| CN115124958A (en) * | 2022-08-23 | 2022-09-30 | 绵阳惠利电子材料有限公司 | Matte high-temperature-resistant damp-heat-resistant two-component epoxy compound and preparation method thereof |
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| CN109852004A (en) * | 2019-01-04 | 2019-06-07 | 恩莱登（北京）工业技术有限公司 | Epoxy resin-base composition, epoxy resin-base and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111253553A (en) * | 2020-03-13 | 2020-06-09 | 东风汽车集团有限公司 | Epoxy resin for carbon fiber reinforced composite material and application thereof |
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| CN113956611A (en) * | 2021-06-30 | 2022-01-21 | 航天材料及工艺研究所 | High-toughness liquid molding resin and composite material based on phase control technology and preparation method thereof |
| CN113861385A (en) * | 2021-10-27 | 2021-12-31 | 航天特种材料及工艺技术研究所 | High-thermal-conductivity epoxy resin cured product and preparation method thereof |
| CN115124958A (en) * | 2022-08-23 | 2022-09-30 | 绵阳惠利电子材料有限公司 | Matte high-temperature-resistant damp-heat-resistant two-component epoxy compound and preparation method thereof |
| CN115124958B (en) * | 2022-08-23 | 2023-08-15 | 绵阳惠利电子材料有限公司 | Matte high-temperature-resistant and damp-heat-resistant double-component epoxy compound and preparation method thereof |
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Application publication date: 20191112 |