CN103275350B - The method of epoxy resin/fiber composite material pretreatment layering - Google Patents
The method of epoxy resin/fiber composite material pretreatment layering Download PDFInfo
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- CN103275350B CN103275350B CN201310187185.7A CN201310187185A CN103275350B CN 103275350 B CN103275350 B CN 103275350B CN 201310187185 A CN201310187185 A CN 201310187185A CN 103275350 B CN103275350 B CN 103275350B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
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Abstract
The method that the invention provides a kind of epoxy resin/fiber composite material pretreatment layering, including: epoxy resin/fiber composite material is mixed with pretreatment fluid, reacts, obtain epoxy resin/fiber single piece of material；Described pretreatment fluid includes organic solvent and aminated compounds；Described organic solvent any one or more in alcohols solvent, phenol solvent and ether solvent.Aminated compounds and organic solvent are configured to pretreatment fluid by the present invention, mix with epoxy resin/fiber composite material, react, the epoxy resin making epoxy resin/fiber composite material interlayer decomposes, so that composite layering, thus it is more beneficial for the recovery of inorganic enhancing thing in composite；Meanwhile, the method for the pretreatment layering that the present invention uses is to carry out under conditions of normal pressure, it is not necessary to carrying out crushing or pulverizing to epoxy resin/fiber composite material, the single piece of material after layering is more beneficial for chopped, and the efficiency reprocessed improves the most further.
Description
Technical field
The present invention relates to waste polymer recovery and utilization technology field, particularly relate to a kind of epoxy resin/fiber
The method of composite pretreatment layering.
Background technology
Epoxy resin/fiber composite material is the composite with epoxy resin as matrix, its have intensity high,
Light weight, heat-resisting, chemicals-resistant, high reliability, thus it is widely used in electron electric power, friendship
Logical transport, Aero-Space, sports equipment, field of wind power generation.But, owing to epoxy resin is three
Dimension cross-linked structure so that epoxy resin-base composite material is difficult to again melt, again become after discarded
Type is processed, and therefore, currently mainly uses landfill and the method burned to process, both processing methods
Not only pollute environment, and waste metal expensive in composite or fiber.
At present, there is the method using chemical recovery that epoxy resin-base composite material is reclaimed, mainly
By heating or solvent soaking, the matrix resin in waste epoxy resin based composites is resolved into little point
Son, thus inorfil is reclaimed.It is multiple that prior art has been disclosed for multiple chemical recovery epoxy resin-matrix
The method of condensation material, as Chinese patent literature CN03132542.4 discloses a kind of with salpeter solution as solvent
The method that waste epoxy resin composite is decomposed；Chinese patent literature CN200610151145.7
Disclose one with partially hydrogenated aromatic compound, mainly naphthane or decahydronaphthalene for solvolysis
Thermosetting epoxy resin and the method for composite thereof；Chinese patent literature CN200710144538.X is open
A kind of with water as solvent, the method for decomposing thermoset epoxy resin composite at high temperature under high pressure；In
State patent documentation CN200910046524.3 disclose a kind of with water as solvent, heteropllyacids material be catalysis
Agent decomposing thermoset epoxy resin or the method for its composite；Patent 201010122570.X discloses one
Kind with the mixture of phenolic compound, water and alkali metal compound for the waste and old thermosetting resin of solvolysis or
The method of its composite.
But, these recovery methods, it is required for carrying out epoxide resin material soaking decomposing, and asphalt mixtures modified by epoxy resin
Fat/fibrous composite mostly is harder solid, and the material loaded in unit reactor is limited, and space
Bigger so that treatment effeciency is relatively low；This is accomplished by it is carried out chopped or pulverization process, but composite wood
Material quality is harder, bigger to chopped wear and tear in machines so that chopped is difficult to carry out.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of epoxy resin/fiber composite material
The method of material pretreatment layering, makes epoxy resin/fiber composite material separate into single piece of material, it is easier to short
Cut.
The method that the invention provides a kind of epoxy resin/fiber composite material pretreatment layering, including:
Epoxy resin/fiber composite material is mixed with pretreatment fluid, reacts, obtain epoxy resin/fiber list
Sheet material；
Described pretreatment fluid includes organic solvent and aminated compounds；Described organic solvent selected from alcohols solvent,
Any one or a few in phenol solvent and ether solvent.
Preferably, described aminated compounds is selected from n-hexylamine, cyclohexylamine, positive heptyl amice, cycloheptylamine, the most pungent
Amine, ethanolamine, diethanolamine, triethanolamine, (2-hydroxyethyl)methylamine), 3-amino-1-propanol, 4-amino
-n-butyl alcohol, 2-amino-2-methyl-1-propanol, 5-amino-1-amylalcohol, piperidines, N-methyl piperidine, 4-diformazan
Aminopyridine, METHYLPYRROLIDONE, 2,3-dihydroxy-propylamine, diethyl-2 hydroxy ethylamine, diformazan
Any one or a few in base-2 hydroxy ethylamine.
Preferably, described alcohols solvent is selected from 2-methyl-1-butene alcohol, 3-methyl-1-butanol, 1-amylalcohol, 1-
Hexanol, 2-hexanol, Hexalin, 1 methyl cyclohexanol, 2 methyl cyclohexanol, 3 methyl cyclohexanol, 2-second
Base-hexanol, 1-heptanol, 2-enanthol, benzyl alcohol, phenethanol, ethylene glycol, 2-methyl cellosolve, 2-ethoxy
Base ethanol, 2-allyloxyethanol, butoxy ethanol, diethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol,
Any one or a few in 1,3 butylene glycol and 1,4-butanediol.
Preferably, described phenol solvent selected from phenol, orthoresol, metacresol, paracresol, xylenol,
Any one in 2-ethyl-phenol, 4-n-pro-pyl phenol, 2-isopropyl-phenol, guaiacol or eugenol
Or it is several.
Preferably, described ether solvent is selected from glycol dimethyl ether, ethylene glycol diethyl ether, diethylene glycol dimethyl
Any one or a few in ether and diethyl carbitol.
Preferably, the mass ratio of described aminated compounds and organic solvent is 0.001～0.1:1.
Preferably, described epoxy resin/fiber composite material includes inorfil.
Preferably, the temperature of described reaction is 120 DEG C～200 DEG C.
Preferably, the time of described reaction is 1h～5h.
Compared with prior art, the invention provides a kind of epoxy resin/fiber composite material pretreatment layering
Method, including: epoxy resin/fiber composite material is mixed with pretreatment fluid, reacts, obtain epoxy
Resin/fiber single piece of material；Described pretreatment fluid includes organic solvent and aminated compounds；Described organic molten
Agent any one or more in alcohols solvent, phenol solvent and ether solvent.The present invention is by amine
Compound and organic solvent are configured to pretreatment fluid, mix with epoxy resin/fiber composite material, react,
The epoxy resin making epoxy resin/fiber composite material interlayer decomposes, so that composite layering, layering
After single piece of material be more beneficial for chopped, thus be easier to the inorganic enhancing thing in composite is carried out back
Receive；Meanwhile, the single piece of material space after chopped is less so that unit reactor can process more thing
Material；It addition, the contact area of single piece of material is the biggest so that reaction efficiency improves further；Further,
The present invention use pretreatment layering method be to carry out under conditions of normal pressure, and without to epoxy resin/
Fibrous composite carries out crushing or pulverizing, to consersion unit require relatively low, corrode less, it is possible to reduce
Cost.
Accompanying drawing explanation
Fig. 1 is the comparison figure before and after the embodiment of the present invention 1 carries out layered shaping to composite.
Detailed description of the invention
The method that the invention provides a kind of epoxy resin/fiber composite material pretreatment layering, including:
Epoxy resin/fiber composite material is mixed with pretreatment fluid, reacts, obtain epoxy resin/fiber list
Sheet material；
Described pretreatment fluid includes organic solvent and aminated compounds；Described organic solvent selected from alcohols solvent,
Any one or more in phenol solvent and ether solvent.
Aminated compounds and organic solvent are configured to pretreatment fluid by the present invention, with epoxy resin/fiber composite
Material mixing, reaction, make the epoxy resin of epoxy resin/fiber composite material interlayer decompose, so that multiple
Condensation material is layered, and obtains single piece of material, and compared with composite, single piece of material quality is softer, it is easier to
Chopped, thus it is more beneficial for the recovery of inorganic enhancing thing in composite；Meanwhile, what the present invention used is pre-
The method processing layering is to carry out under conditions of normal pressure, it is not necessary to carry out epoxy resin/fiber composite material
Broken or pulverize, consersion unit is required relatively low, corrode less, it is possible to reduce cost.
The method of the epoxy resin/fiber composite material pretreatment layering that the present invention provides, first by asphalt mixtures modified by epoxy resin
Fat/fibrous composite mixes with pretreatment fluid.
Described epoxy resin/fiber composite material preferably comprises inorfil, and preferably, does not comprise short
Fiber；Epoxy resin-base in described composite does not the most comprise ester cross-bond；In the present invention, institute
State epoxy resin/fiber composite material and be preferably employing prepreg by directly mold pressing, hands paste layer pressure, vacuum
Bag hot pressing, resin transfer molding or the method such as Wrapping formed are shaped the composite of machine-shaping.
Described pretreatment fluid preferably includes: organic solvent and aminated compounds；Described aminated compounds is preferred
For n-hexylamine, cyclohexylamine, positive heptyl amice, cycloheptylamine, 1-Aminooctane, ethanolamine, diethanolamine, three ethanol
Amine, (2-hydroxyethyl)methylamine), 3-amino-1-propanol, 4-amino-n-butyl alcohol, 2-amino-2-methyl-1-propanol,
5-amino-1-amylalcohol, piperidines, N-methyl piperidine, DMAP, METHYLPYRROLIDONE,
In 2,3-dihydroxy-propylamine, diethyl-2 hydroxy ethylamine, dimethyl-2 hydroxy ethylamine any one or several
Kind；More preferably ethanolamine, diethanolamine, triethanolamine, (2-hydroxyethyl)methylamine), piperidines, N-first
Any one or a few in phenylpiperidines, DMAP and METHYLPYRROLIDONE.
Described organic solvent be preferably in alcohols solvent, phenol solvent and ether solvent any one or several
Kind；Described alcohols solvent be preferably 2-methyl-1-butene alcohol, 3-methyl-1-butanol, 1-amylalcohol, 1-hexanol,
2-hexanol, Hexalin, 1 methyl cyclohexanol, 2 methyl cyclohexanol, 3 methyl cyclohexanol, 2-ethyl-hexanol,
1-heptanol, 2-enanthol, benzyl alcohol, phenethanol, ethylene glycol, 2-methyl cellosolve, cellosolvo,
2-allyloxyethanol, butoxy ethanol, diethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,3-fourth two
Any one or a few in alcohol and 1,4-butanediol；More preferably 1-hexanol, 2-hexanol, Hexalin,
Any one or a few in ethylene glycol, benzyl alcohol, phenethanol and diethylene glycol；Described phenol solvent is preferred
For phenol, orthoresol, metacresol, paracresol, xylenol, 2-ethyl-phenol, 4-n-pro-pyl phenol, 2-
Any one or a few in isopropyl-phenol, guaiacol or eugenol；More preferably phenol, adjacent first
Any one or a few in phenol, metacresol and paracresol；Described ether solvent is preferably glycol dinitrate
Any one or a few in ether, ethylene glycol diethyl ether, diethylene glycol dimethyl ether and diethyl carbitol.This
Invent the source to described aminated compounds and organic solvent and there is no particular/special requirement, can be the most commercially available,
Technical grade purity.
In the present invention, in described pretreatment fluid, the mass ratio of described aminated compounds and organic solvent is preferred
It is 0.001～0.1:1, more preferably 0.01～0.1:1.Described pretreatment fluid can decompose epoxy resin/fibre
The resin of dimension composite interlayer, thus composite is layered.
After being mixed with pretreatment fluid by epoxy resin/fiber composite material, it is carried out reacting by heating,
Obtain epoxy resin/fiber single piece of material；The temperature of described reaction is preferably 120 DEG C～200 DEG C, more preferably
It it is 140 DEG C～180 DEG C；Showing after deliberation, layered effect is had a significant effect by reaction temperature, reaction temperature mistake
Low, composite layering is inconspicuous, and reaction temperature is too high, then the composite being layered likely scatters,
Making follow-up chopped be difficult to carry out, the temperature range that the present invention provides is optimal stratification temperature；And this
The temperature that invention uses is below the boiling point of solvent, therefore for reacting under condition of normal pressure so that reaction
Mild condition, beneficially industrialized production.
The time of described reaction is preferably 1h～5h, more preferably 2h～4h, and research shows, the response time pair
Layered effect has a significant effect equally, and the response time is too short, and composite layering is inconspicuous, overlong time,
Then can cause process energy consumption and the increase of cost, the response time that the present invention provides is optimal heat time heating time.
After reaction, i.e. can get epoxy resin/fiber single piece of material, it is preferred that the material obtained is entered
Row purification, concrete, reaction system is cooled to room temperature, described room temperature is specially 10 DEG C～30 DEG C, then
Solid matter in reaction system is taken out, is carried out with acetone, filters and be dried, obtain purification
Epoxy resin/fiber single piece of material.
The method provided by the present invention, is carried out pretreatment to epoxy resin/fiber composite material, obtains
Single piece of material is only layered, and will not scatter, and quality is softer, it is easy to carry out chopped, and the effect reprocessed
Rate improves the most further.
Aminated compounds and organic solvent are configured to pretreatment fluid by the present invention, with epoxy resin/fiber composite
Material mixing, reaction, make the epoxy resin of epoxy resin/fiber composite material interlayer decompose, so that multiple
Condensation material is layered, and obtains single piece of material, and compared with composite, single piece of material quality is softer, it is easier to
Chopped, thus it is more beneficial for the recovery of inorganic enhancing thing in composite；Meanwhile, what the present invention used is pre-
The method processing layering is to carry out under conditions of normal pressure, it is not necessary to carry out epoxy resin/fiber composite material
Broken or pulverize, consersion unit is required relatively low, corrode less, it is possible to reduce cost.
In order to further illustrate the present invention, the epoxy resin/fiber present invention provided below in conjunction with embodiment
The method of composite pretreatment layering is described in detail.
Embodiment 1
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is
In the beaker of 1000mL, then carry out being mixed and heated 200 DEG C by itself and the above-mentioned composite of 10g,
Reaction 3h；Then reaction system is cooled to room temperature, solid matter is taken out, with acetone to solid matter
It is carried out, filters and be dried, obtain the single piece of material that thickness is 0.3mm；Experimental result is shown in Fig. 1,
Fig. 1 is the comparison figure before and after the embodiment of the present invention 1 carries out layered shaping to composite, wherein, upside
For undressed composite, downside is the single piece of material obtained after layering；As shown in Figure 1,
After treatment, composite is layered as the single piece of material of thickness about 0.3mm.
Embodiment 2
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 200 DEG C with the above-mentioned composite of 10g, reacts 5h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness 0.3mm's
Single piece of material.
Embodiment 3
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 200 DEG C with the above-mentioned composite of 10g, reacts 1h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite portions is layered as thickness 0.3mm's
Single piece of material.
Embodiment 4
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 160 DEG C with the above-mentioned composite of 10g, reacts 3h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness 0.3mm's
Single piece of material.
Embodiment 5
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 120 DEG C with the above-mentioned composite of 10g, reacts 3h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite portions is layered as thickness 0.3mm's
Single piece of material.
Embodiment 6
Using matrix resin is that 2-ethyl-4-methylimidazole solidifies bisphenol-A diglycidyl ether type asphalt mixtures modified by epoxy resin
Fat, reinforcing material be the composite of carbon fiber be raw material, its epoxy resin accounts for the quality of composite
Degree is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 160 DEG C with the above-mentioned composite of 10g, reacts 3h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness 0.3mm's
Single piece of material.
Embodiment 7
Using matrix resin is that 2-ethyl-4-methylimidazole solidifies bisphenol-A diglycidyl ether type asphalt mixtures modified by epoxy resin
Fat, reinforcing material be the composite of carbon fiber be raw material, its epoxy resin accounts for the quality of composite
Degree is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g benzyl alcohol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 160 DEG C with the above-mentioned composite of 10g, reacts 3h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness 0.3mm's
Single piece of material.
Embodiment 8
Using matrix resin is polyamide cure bisphenol-A diglycidyl ether type epoxy resin, reinforcing material
Composite for carbon fiber is raw material, and its epoxy resin accounts for the mass percentage content of composite and is
40%, the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 160 DEG C with the above-mentioned composite of 10g, reacts 3h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness 0.3mm's
Single piece of material.
Embodiment 9
Using matrix resin is dicyandiamide cure bisphenol-A diglycidyl ether type epoxy resin, reinforcing material
Composite for carbon fiber is raw material, and its epoxy resin accounts for the mass percentage content of composite and is
40%, the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 160 DEG C with the above-mentioned composite of 10g, reacts 3h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness 0.3mm's
Single piece of material.
Embodiment 10
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g diethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 160 DEG C with the above-mentioned composite of 10g, reacts 3h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness 0.3mm's
Single piece of material.
Embodiment 11
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 1mm, and size is 20mm × 30mm.
100g phenol and 5g METHYLPYRROLIDONE being mixed and be made into pretreatment fluid, joining volume is
In the flask of 250mL, then itself and the above-mentioned composite of 10g are carried out being mixed and heated 160 DEG C, instead
Answer 3h；Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is entered
Row cleans, and filters and is dried, obtains single piece of material；Reaction result is that composite is all layered as thickness
The single piece of material of 0.25mm.
Embodiment 12
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2mm, and size is 20mm × 30mm.
100g benzyl alcohol and 5g METHYLPYRROLIDONE are mixed and is made into pretreatment fluid, join volume
For in the flask of 250mL, then carry out being mixed and heated 200 DEG C by itself and the above-mentioned composite of 10g,
Reaction 3h；Then reaction system is cooled to room temperature, solid matter is taken out, with acetone to solid matter
It is carried out, filters and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness
The single piece of material of degree 0.2mm.
Embodiment 13
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 3mm, and size is 20mm × 30mm.
100g glycol dimethyl ether and 5g ethanolamine being mixed and be made into pretreatment fluid, joining volume is
In the flask of 250mL, then itself and the above-mentioned composite of 10g are carried out being mixed and heated 160 DEG C, instead
Answer 3h；Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is entered
Row cleans, and filters and is dried, obtains single piece of material；Reaction result is that composite is all layered as thickness
The single piece of material of 0.3mm.
Embodiment 14
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 0.1g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is
In the flask of 250mL, then itself and the above-mentioned composite of 10g are carried out being mixed and heated 160 DEG C, instead
Answer 3h；Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is entered
Row cleans, and filters and is dried, obtains single piece of material；Reaction result is that composite is all layered as thickness
The single piece of material of 0.3mm.
Embodiment 15
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of carbon fiber be raw material, its epoxy resin accounts for the mass percent of composite and contains
Amount is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g Hexalin and 10g4-dimethylamino naphthyridine being mixed and be made into pretreatment fluid, joining volume is
In the flask of 250mL, then itself and the above-mentioned composite of 10g are carried out being mixed and heated 160 DEG C, instead
Answer 3h；Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is entered
Row cleans, and filters and is dried, obtains single piece of material；Reaction result is that composite is all layered as thickness
The single piece of material of 0.3mm.
Embodiment 16
Using matrix resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, enhancing
Material be the composite of glass fibre be raw material, its epoxy resin accounts for the mass percent of composite
Content is 40%, and the thickness of composite is 2.7mm, and size is 20mm × 30mm.
100g ethylene glycol and 5g N-methyl piperidine being mixed and be made into pretreatment fluid, joining volume is 250mL
Flask in, then it is carried out being mixed and heated 200 DEG C with the above-mentioned composite of 10g, reacts 3h；
Then reaction system is cooled to room temperature, solid matter is taken out, with acetone, solid matter is carried out,
Filter and be dried, obtain single piece of material；Reaction result is that composite is all layered as thickness 0.3mm's
Single piece of material.
From above-described embodiment, aminated compounds and organic solvent are configured to pretreatment fluid by the present invention,
Then carry out hybrid reaction with epoxy resin/fiber composite material, make composite be layered as single piece of material,
It is more easy to carry out chopped.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.Should
Point out, for those skilled in the art, under the premise without departing from the principles of the invention,
The present invention can also be carried out some improvement and modification, these improve and modification also falls into right of the present invention and wants
In the protection domain asked.
Claims (8)
1. a method for epoxy resin/fiber composite material pretreatment layering, including:
Epoxy resin/fiber composite material is mixed with pretreatment fluid, reacts, obtain epoxy resin/fiber list
Sheet material；
Described pretreatment fluid includes organic solvent and aminated compounds；Described organic solvent selected from alcohols solvent,
Any one or a few in phenol solvent and ether solvent；
Described aminated compounds appointing in triethanolamine, N-methyl piperidine, METHYLPYRROLIDONE
Anticipate one or more；
Described epoxy resin is that triethylene tetramine solidifies bisphenol-A diglycidyl ether type epoxy resin, 2-ethyl
-4-methylimidazole solidification bisphenol-A diglycidyl ether type epoxy resin, polyamide cure bisphenol-A two shrink
Ethoxylated glycerol type epoxy resin or dicyandiamide cure bisphenol-A diglycidyl ether type epoxy resin.
Method the most according to claim 1, it is characterised in that described alcohols solvent is selected from 2-methyl
-n-butyl alcohol, 3-methyl-1-butanol, 1-amylalcohol, 1-hexanol, 2-hexanol, Hexalin, 1 methyl cyclohexanol,
2 methyl cyclohexanol, 3 methyl cyclohexanol, 2-ethyl-hexanol, 1-heptanol, 2-enanthol, benzyl alcohol, benzene second
Alcohol, ethylene glycol, 2-methyl cellosolve, cellosolvo, 2-allyloxyethanol, butoxy ethanol,
In diethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,3 butylene glycol and 1,4-butanediol any one or
Several.
Method the most according to claim 1, it is characterised in that described phenol solvent selected from phenol,
Orthoresol, metacresol, paracresol, xylenol, 2-ethyl-phenol, 4-n-pro-pyl phenol, 2-cumene
Any one or a few in phenol, guaiacol or eugenol.
Method the most according to claim 1, it is characterised in that described ether solvent is selected from ethylene glycol
Any one or a few in dimethyl ether, ethylene glycol diethyl ether, diethylene glycol dimethyl ether and diethyl carbitol.
Method the most according to claim 1, it is characterised in that described aminated compounds and organic molten
The mass ratio of agent is 0.001～0.1:1.
Method the most according to claim 1, it is characterised in that described epoxy resin/fiber composite material
Material includes inorfil.
Method the most according to claim 1, it is characterised in that the temperature of described reaction is 120 DEG C
～200 DEG C.
Method the most according to claim 1, it is characterised in that the time of described reaction is 1h～5h.
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| WO2023097534A1 (en) * | 2021-12-01 | 2023-06-08 | Solvay Sa | Chemoenzymatic degradation of epoxy composites |
| CN114736425B (en) * | 2022-04-17 | 2024-02-09 | 西北工业大学 | Method for recycling carbon fiber reinforced bismaleimide resin matrix composite material |
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| CN101787145A (en) * | 2010-03-12 | 2010-07-28 | 中国科学院长春应用化学研究所 | Method for recovering fiber from epoxy resin/fiber composite material |
| CN102634061A (en) * | 2012-05-04 | 2012-08-15 | 中国科学院长春应用化学研究所 | Decomposition method for epoxy resin or composite materials thereof |
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| CN101787145A (en) * | 2010-03-12 | 2010-07-28 | 中国科学院长春应用化学研究所 | Method for recovering fiber from epoxy resin/fiber composite material |
| CN102634061A (en) * | 2012-05-04 | 2012-08-15 | 中国科学院长春应用化学研究所 | Decomposition method for epoxy resin or composite materials thereof |
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