CN108841134A - A kind of flame-retardant high-strength lightweight phenolic resin - Google Patents
A kind of flame-retardant high-strength lightweight phenolic resin Download PDFInfo
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- CN108841134A CN108841134A CN201810335177.5A CN201810335177A CN108841134A CN 108841134 A CN108841134 A CN 108841134A CN 201810335177 A CN201810335177 A CN 201810335177A CN 108841134 A CN108841134 A CN 108841134A
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- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
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- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
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- C08G8/12—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with monohydric phenols having only one hydrocarbon substituent ortho on para to the OH group, e.g. p-tert.-butyl phenol
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Abstract
The present invention relates to compound resin technical fields, a kind of flame-retardant high-strength lightweight phenolic resin is disclosed, the flame-retardant high-strength lightweight is made of raw material, and the flame-retardant high-strength lightweight is made of feedstock composition, on the basis of 100 parts by weight of raw material phenol, the feedstock composition includes：100 parts by weight of raw material phenol, 30~120 parts by weight of raw material aldehyde, 10~48 parts by weight of staple fiber, 10~30 parts by weight of long fibre, 12~40 parts by weight of improved silica, 6~20 parts by weight of foaming agent, 2~10 parts by weight of surfactant, 10~30 parts by weight of catalyst, 200~360 parts by weight of organic solvent, the length of the staple fiber are 0.3~2 micron；The long stapled length is 5~20 microns.Flame-retardant high-strength lightweight phenolic resin of the invention has high-intensitive, uniformity, also has good soundproof effect, additionally it is possible to play the role of buffering external force, have broad application prospects on car body material.
Description
Technical field
The present invention relates to compound resin technical fields, and in particular to a kind of flame-retardant high-strength lightweight phenolic resin.
Background technique
In recent years, automotive light weight technology has become the emphasis direction of automotive field development instantly, and Lightweight Technology can not only
It the problem of enough its environmental pollutions of effective solution, realizes the target of energy-saving and emission-reduction, also largely reduces automobile manufacture
Cost has very big economic benefit for present used automobile.
Currently, the method for automotive light weight technology mainly includes the section using light material and reduction door-plate.Reduce door-plate
Section namely reduces the thickness of door-plate, although can reduce the overall weight of automobile, it can also cause automobile door plate is strong
Degree reduces, and in collision, can generate serious deformation, reduce the safety of automobile.Using light material refer to using light weight,
The steel material of the current car door of the big material substitution of intensity, currently, common light material has aluminium alloy extrusions, high-strength complex
Resin and carbon fibre material.Wherein, high-intensity resin relies on itself small specific gravity, sound-insulating and heat-insulating, corrosion-resistant, absorption impact energy
Amount, many advantages, such as specific strength is high, at low cost, easy processing, good decorating effect, already as light material in automotive light weight technology
Development trend.
Phenolic resin starting material is easy to get, cheap, and production technology and equipment are simple, and product has excellent machinery
Property, heat resistance, cold resistance, electrical insulating property, dimensional stability, molding processibility, anti-flammability and smokiness, there is extensive use
On the way, still, conventional unmodified phenolic resin brittleness is big, poor toughness, largely limits the exploitation of high performance material.Very
The raising of the toughness and heat resistance of phenolic resin is difficult to and deposits in more situations, limits its application in the car.
Summary of the invention
It is of the existing technology the purpose of the invention is to overcome the problems, such as, a kind of flame-retardant high-strength lightweight phenolic aldehyde tree is provided
Rouge, it has the characteristics that lightweight, intensity height and good flame retardation effect, has great application prospect in preparing automobile cover plate.
To achieve the goals above, the present invention provides a kind of flame-retardant high-strength lightweight phenolic resin, the flame-retardant high-strength
Lightweight phenolic resin is made of raw material, and on the basis of 100 parts by weight of raw material phenol, the raw material includes the substance of following parts by weight：
100 parts by weight of raw material phenol, 10~48 parts by weight of staple fiber, 10~30 parts by weight of long fibre, change 30~120 parts by weight of raw material aldehyde
2~40 parts by weight of property silica 1,6~20 parts by weight of foaming agent, 2~10 parts by weight of surfactant, 10~30 weight of catalyst
Measure part, 200~360 parts by weight of organic solvent；
The length of the staple fiber is 0.3~2 micron；The long stapled length is 5~20 microns.
Through the above technical solutions, the present invention has the following technical effects：
The present invention can intersect between long fibre and twine by the way that the different reinforcing fiber of two kinds of length is added in phenolic resin
It is wound on the inside of phenolic resin, plays the role of improving phenolic resin bending property, staple fiber can be dispersed in epoxy resin
Portion plays the role of improving epoxy resin intensity；In addition, staple fiber can also be dispersed in inside long fibre, long fibre mistake is avoided
Degree is reunited, and can not be dispersed, so that phenolic resin chemistry inside be made to be unevenly distributed, be improved the uniformity of phenolic resin.
Specific embodiment
The endpoint of disclosed range and any value are not limited to the accurate range or value herein, these ranges or
Value should be understood as comprising the value close to these ranges or value.For numberical range, between the endpoint value of each range, respectively
It can be combined with each other between the endpoint value of a range and individual point value, and individually between point value and obtain one or more
New numberical range, these numberical ranges should be considered as specific open herein.
In order to reduce the quality of phenolic resin, the intensity of phenolic resin is improved, it is light that the present invention provides a kind of flame-retardant high-strength
Matter phenolic resin, the flame-retardant high-strength lightweight are made of raw material, and on the basis of 100 parts by weight of raw material phenol, the raw material includes
The substance of following parts by weight：100 parts by weight of raw material phenol, 30~120 parts by weight of raw material aldehyde, 10~48 parts by weight of staple fiber, long fibre
Tie up 10~30 parts by weight, 12~40 parts by weight of improved silica, 6~20 parts by weight of foaming agent, 2~10 weight of surfactant
Part, 10~30 parts by weight of catalyst, 200~360 parts by weight of organic solvent.
The length of the staple fiber is 0.3~2 micron；The long stapled length is 5~20 microns.
In the present invention, by the way that the different reinforcing fiber of two kinds of length is added in phenolic resin, it can be handed between long fibre
Fork is wrapped in the inside of phenolic resin, plays the role of improving phenolic resin bending property, staple fiber can be dispersed in asphalt mixtures modified by epoxy resin
Inside rouge, play the role of improving epoxy resin intensity；In addition, staple fiber can also be dispersed in inside long fibre, long fibre is avoided
Undue agglomeration is tieed up, can not disperse, so that phenolic resin chemistry inside be made to be unevenly distributed, improve the uniform of phenolic resin
Property.
In the present invention, a large amount of functional group is contained by the surface of improved silica, it can be with phenolic resin strand
On functional group react, make to connect between improved silica and phenolic resin with the formation of chemical bond, to make dioxy
There is very high binding force between SiClx and phenolic resin, and can be uniformly dispersed in phenolic resin, it can not only be significant
The intensity of phenolic resin system is improved, while also improving the uniformity of phenolic resin.
It in the present invention, is used in mixed way by phenolic resin and foaming agent, phenolic resin foam, phenolic resin bubble can be generated
Foam can not only reduce the quality of system, additionally it is possible to play the role of buffering external force, sound insulation, improve automobile in the process of moving
Stability and soundproof effect.
In the present invention, the content of each substance is an important factor for influencing phenolic resin performance, under preferable case, with raw material phenol
On the basis of 100 parts by weight, the feedstock composition includes the substance of following parts by weight：100 parts by weight of raw material phenol, raw material aldehyde 30~
120 parts by weight, 24~36 parts by weight of staple fiber, 16~24 parts by weight of long fibre, 20~36 parts by weight of improved silica, foaming
6~20 parts by weight of agent, 2~10 parts by weight of surfactant, 10~30 parts by weight of catalyst, 240~300 weight of organic solvent
Part.
According to the present invention, the raw material phenol can be o-cresol, m-cresol, p-cresol, to hydroxymethylphenol, neighbour
At least one of benzenediol, resorcinol and hydroquinone；Raw material aldehyde can be formaldehyde, acetaldehyde, propionic aldehyde, butyraldehyde, methacrylaldehyde,
At least one of cyclohexanone dimethylacetal, benzaldehyde, furfural, heterocyclic aldehydes, paraformaldehyde and metaformaldehyde.
In the present invention, the content of long fibre and staple fiber is an important factor for influencing phenolic resin mechanical property, if long
The content of fiber is low, then can reduce the tensile strength of phenolic resin, and the content of staple fiber is low can also reduce the strong of phenolic resin
Degree, in order to obtain high-intensitive phenolic resin, under preferable case, the staple fiber and the long stapled mass ratio be (1~
1.6)：1.
In the present invention, catalyst can promote the generation of phenolic resin, improve polymerization reaction efficiency, under preferable case, institute
Stating catalyst is alkaline matter, it is further preferred that the catalyst is selected from alkali metal hydroxide, alkaline-earth metal hydroxide
At least one of object, carbonate and bicarbonate.
According to the present invention, the present invention in reinforcing fiber be play enhancing phenolic resin mechanical property an important factor for, wherein
Staple fiber is to improve the important materials of phenolic resin intensity, under preferable case, the reinforcing fiber should intensity with higher,
In further preferred situation, the staple fiber is selected from calcium sulfate crystal whiskers, alumina whisker, silicon carbide whisker, carbonization boron whisker, two
Zirconium oxide whisker, aluminium nitride whisker, ZnOw, magnesium sulfate crystal whisker, glass fibre, potassium titanate crystal whisker, magnesium sulfate crystal whisker and
At least one of silicon nitride crystal whisker；And staple fiber of the invention has good thermal conductivity, avoids accumulation of heat, improves simultaneously
The intensity and flame retardant property of phenolic resin, under preferable case, the average diameter of the reinforcing fiber is 50~150nm.
The bending property and tensile strength of phenolic resin are improved in the present invention by long fibre, the long fibre should have
Higher intensity and high tenacity, under preferable case, the long fibre is polyethylene fibre, the Weight-average molecular of the polyethylene fibre
Measure Mw >=1 × 106。
In the present invention, foaming agent can occur to thermally decompose and form bubble inside phenolic resin at high temperature, thus shape
At foamed phenolic resin, since carburizing reagent can occur at high temperature for phenolic resin, foaming agent selected by the present invention
Decomposition temperature should be lower than the carburizing temperature of phenolic resin.Under preferable case, the foaming agent is selected from the double benzene sulfonyls of 4,4- oxo
Hydrazine, azodicarbonamide, N, at least one of N '-dinitrosopentamethlyene tetramine.
In the present invention, a large amount of active function groups are contained on the surface of the improved silica, can be with phenolic resin table
The functional group in face is chemically reacted, and makes to connect between improved silica and phenolic resin with the formation of chemical bond, to make
There is very high binding force between improved silica and phenolic resin, and can be uniformly dispersed in phenolic resin, not only
The intensity of phenolic resin system can be significantly improved, while also improving the uniformity of phenolic resin.It is described to change under preferable case
Property silica be selected from least one of hydroxyl modification silica and amino modified silica；Further preferred situation
Under, the average diameter of the improved silica is 100~300nm.
Under preferable case, the surfactant is selected from dodecyl alcohol polyoxyethylene ether sodium sulfate, dodecyl sulphate
Ammonium, lauryl sodium sulfate, dodecyl benzene sulfonic acid, sodium secondary alkyl sulfonate, fatty alcohol sodium isethionate, N- lauroyl musculamine
At least one of sour sodium, coconut acyl methyl taurine sodium, α-sodium olefin sulfonate, dodecyl phosphide ester triethanolamine.
The present invention does not have special requirement to the type of organic solvent, can be common organic molten in phenolic resin synthesis
Agent, under preferable case, the organic solvent is selected from acetone, n,N-Dimethylformamide, N-Methyl pyrrolidone, N, N- dimethyl
Acetamide, dimethyl acetamide, methylene chloride, triethyl phosphate, chloroform, toluene, ethyl alcohol, acetic acid, ethyl acetate, first
At least one of acid, chloroform, tetrahydrofuran, atoleine and dimethyl sulfoxide.
The present invention also provides a kind of preparation methods of flame-retardant high-strength lightweight phenolic resin, include the following steps：
(1) by raw material phenol, first part's raw material aldehyde, catalyst, the long fibre that length is 5~20 microns, modified titanium dioxide
In organic solvent after mixing, flow back 3~5h at 80~120 DEG C for silicon, foaming agent and surfactant, obtains pre-polymerization
Object；
(2) staple fiber and the second part raw material aldehyde that length is 0.3~2 micron, ultrasonic disperse 30 are added into prepolymer
~60min, then flow back at 90~110 DEG C 1~2h, forms gel；
(3) Gel heat-treatment：Gel is placed 1 in the steam that pressure is 150~500kPa, temperature is 130~200 DEG C
~3h, then cools to room temperature, and obtains flame-retardant high-strength lightweight phenolic resin.
In the present invention, phenolic resin monomer, catalyst, long fibre, improved silica and surfactant are existed first
Prepolymerization reaction is carried out in organic solvent, foaming agent is coated on inside phenolic resin performed polymer, and disperse long fibre uniformly
Inside phenolic resin, the binding force with higher between phenolic resin.Then adding staple fiber, the reaction was continued, can make
Staple fiber enters in phenolic resin that the reaction was continued, and staple fiber is inserted into the hole of long fibre and phenolic resin, improves length
The dispersion degree of fiber avoids the occurrence of the phenomenon that long fibre aggregation winds and causes phenolic resin internal structure otherness big.
Improved silica can be chemically reacted with the functional group of phenolic surface, and in the form of chemical bond with
Phenolic resin combines, and not only increases the binding force of silica and phenolic resin, while improving silica in phenolic aldehyde tree
Dispersing uniformity in rouge significantly improves the intensity of phenolic resin.The present invention finally to phenolic resin carry out high-temperature process, one
Aspect can make the progress of curing reaction, on the other hand, decompose foaming agent at high temperature, be formed inside phenolic resin more
Pore structure.
Phenolic resin containing foaming agent is carried out pyrolysis by the present invention in the steam of solvent, on the one hand can be made
Foaming agent decomposes at high temperature, generates stomata, on the other hand, additionally it is possible to due to avoid phenolic resin from occurring to occur admittedly because of solvent
Change reaction, avoids occurring the big phenomenon of material internal structure differentiation in integrated molding.Phenolic resin is carried out under high pressure
Pyrolysis makes phenolic resin by stronger external pressure, slows down the evolution of gas in phenolic resin, reduces the decomposition of foaming agent
Speed reduces the generating rate of bubble, improves the uniformity of pore opening, and foamed phenolic resin is made to have uniform internal junction
Structure.
According to the present invention, the weight ratio of first part's raw material aldehyde and second part raw material aldehyde is (3~6)：1.
The density for the flame-retardant high-strength lightweight phenolic resin being prepared according to the above method is 36.25~39.14kg/
m3。
The present invention also provides a kind of lightweight automotive cover boards, including inner core and coated in the coating of core surface, the core material
Using flame-retardant high-strength lightweight phenolic resin according to the present invention.
It is the coating packet in terms of 100 by the weight of epoxy resin under a preferable case of the invention in embodiment
Include the substance of following parts by weight：100 parts of phenolic resin, 30~58 parts of butyl methacrylate, redox graphene 5~15
Part, 2~6 parts of levelling agent, 10~18 parts of curing agent.
Preferably, the levelling agent is selected from dimethyl silicone polymer and/or polymethylphenylsiloxane；The curing agent can
To use ethylenediamine, hexamethylene diamine, methyl cyclohexyl diamine, 1,4- butanediamine, 1,5- pentanediamine, 2- methyl-1,5- pentanediamine, 2- fourth
Base -2- ethyl -1,5- pentanediamine, 1,6- hexamethylene diamine, 2,2,4- trimethylhexane diamine, 2,4,4- trimethylhexane diamine, 1,8- are pungent
Diamines, 2- methyl-1,8- octamethylenediamine, 1,9-nonamethylene diamine, 1,10- decamethylene diamine, 1,11- hendecane diamines, 1,12- dodecane two
Amine, 1,13- tridecane diamine, 1,14- tetradecane diamines, 1,15- pentadecane diamines, 2- methyl -2,4-PD, 1,16- ten
At least one of six alkane diamines and 1,18-1,14- octadecamethylene diamine, dimethythiotoluene diamine.
The present invention also provides a kind of preparation methods of lightweight automotive cover board, include the following steps：
(1) prepared by core material：The core material is by flame-retardant high-strength lightweight phenolic resin punch forming according to the present invention
It is made, preparation method is referring to the present invention previously with regard to the description of the preparation method of flame-retardant high-strength lightweight phenolic resin.
(2) coating spraying：By modified epoxy, butyl methacrylate, redox graphene, levelling agent, wetting
Agent, curing agent are uniformly mixed in organic solvent, form coating emulsion, coating emulsion is then sprayed on core surfaces, are solidified
Afterwards, coating is formed.
Under preferable case, the stamping forming technique is：Press temperature is 60-140 DEG C, pressure 5-25MPa, punching press
Time is 2-20min, and after punching press, the temperature of stamping die and product is reduced to room temperature within 10min.
In the case of, according to the invention it is preferred to, the cure process is to solidify 30min at 120 DEG C.
In the present invention, core material using flame-retardant high-strength light-weight foam phenolic resin as automobile door plate, foamable phenolic tree
Rouge core material has the characteristics that light weight compared with existing steel core material, and the quality of automobile can be greatly lowered, in addition, this
Invention prepares automobile cover plate by integrally formed method, avoids the method connecting components using welding, further reduced
The quality of automobile cover plate reduces the oil consumption of automobile, plays energy-saving and emission-reduction to reduce the resistance that automobile generates during form
Work.
In the present invention, by the way that the different reinforcing fiber of two kinds of length is added in phenolic resin, it can be handed between long fibre
Fork is wrapped in the inside of phenolic resin, plays the role of improving phenolic resin bending property, staple fiber can be dispersed in asphalt mixtures modified by epoxy resin
Inside rouge, play the role of improving epoxy resin intensity, by the way that long fibre and staple fiber to be used cooperatively, staple fiber point can be made
It is dispersed in inside long fibre, avoids long fibre undue agglomeration, can not disperse, so that phenolic resin chemistry inside be made to be unevenly distributed
It is even, and influence the performance of phenolic resin.
In the present invention, a large amount of functional group is contained by the surface of improved silica, it can be with phenolic resin strand
On functional group react, make to connect between improved silica and phenolic resin with the formation of chemical bond, to make dioxy
There is very high binding force between SiClx and phenolic resin, and can be uniformly dispersed in phenolic resin, it can not only be significant
The intensity of phenolic resin system is improved, while also improving the uniformity of phenolic resin.
It in the present invention, is used in mixed way by phenolic resin and foaming agent, can play the role of buffering external force, improve automobile
Stability in the process of moving.Phenolic resin containing foaming agent is subjected to pyrolysis, a side in the steam of solvent
Face can be such that foaming agent decomposes at high temperature, generate stomata, on the other hand, additionally it is possible to avoid phenolic resin from occurring at high temperature molten
The phenomenon that agent volatilizees and the internal structure of phenolic resin is caused to solidify.Phenolic resin is subjected to pyrolysis under high pressure, is made
Phenolic resin is reduced the decomposition rate of foaming agent by stronger external pressure, reduces the generating rate of bubble, improves pore opening
Uniformity makes foamed phenolic resin have uniform internal structure.
The present invention will be described in detail by way of examples below.In following embodiment, various kinds is tested using drainage
The density of product.According to the tensile property of the method test each sample of GB/T1447-2005.According to the method for GB/T1449-2005
Survey the examination bending property of each sample.According to the elongation at break of the method test each sample of GB/T1040.1-2006.According to GB/
The impact flexibility of the method test each sample of T1451-2005.According to UL94《Equipment and the examination of the flammable performance of device component material
It tests》In testing vertical flammability method, determine the flame retardant rating of composite material.Batten size：Long 125 ± 5mm, wide by 13.0 ±
0.5mm, 1.5 ± 0.2mm of thickness.
Embodiment 1
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g o-cresol, 100g metaformaldehyde, 20g sodium hydroxide, the polyethylene fibre that 25g length is 15 microns
(Mw=4.5 × 106), 30g average diameter be 150 nanometers of amino modified silica, 15g azodicarbonamide and 5gN- month
In 280g N-Methyl pyrrolidone after mixing, flow back osmanthus acyl musculamine acid sodium 4h at 100 DEG C, obtains prepolymer；To pre-
30g length is added in polymers then to flow back at 100 DEG C for 1 micron of staple fiber and 20g metaformaldehyde, ultrasonic disperse 45min
1.5h forms gel；
Gel heat-treatment：Gel is placed in the N-Methyl pyrrolidone steam that pressure is 250kPa, temperature is 200 DEG C
1.5h is then cooled to room temperature, and obtains flame-retardant high-strength lightweight phenolic resin；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 100 DEG C in temperature, under conditions of pressure is 15MPa,
The temperature of stamping die and product after punching press, is reduced to room temperature within 10min by punching press 10min；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylate, 12g redox graphene, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamine are uniformly mixed in dimethyl acetamide, form coating emulsion, then by coating cream
Liquid is sprayed on core surfaces, solidifies 30min at 120 DEG C, forms coating；
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Embodiment 2
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g m-cresol, 100g paraformaldehyde, 15g sodium hydroxide, the polyethylene fibre that 16g length is 16 microns
(Mw=3 × 106), 20g average diameter be 200 nanometers amino modified silica, 10g 4,4- oxobenzenesulfonyl hydrazide and
In 240g atoleine after mixing, flow back 8g dodecyl benzene sulfonic acid 3.5h at 100 DEG C, obtains prepolymer；To pre-
The staple fiber and 25g paraformaldehyde that addition 24g length is 500 nanometers in polymers, ultrasonic disperse 45min, then next time at 100 DEG C
1h is flowed, gel is formed；
Gel heat-treatment：Gel is placed into 2h in the atoleine steam that pressure is 300kPa, temperature is 150 DEG C, so
After be cooled to room temperature, obtain flame-retardant high-strength lightweight phenolic resin；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 120 DEG C, pressure 20MPa in temperature, punching press
The temperature of stamping die and product after punching press, is reduced to room temperature within 10min by 5min；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylate, 12g redox graphene, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamine are uniformly mixed in dimethyl acetamide, form coating emulsion, then by coating cream
Liquid is sprayed on core surfaces, solidifies 30min at 120 DEG C, forms coating.
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Embodiment 3
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g p-methyl phenol, 30g formaldehyde, 25g magnesium hydroxide, the polyethylene fibre (Mw=9 that 24g length is 8 microns
×106), 36g average diameter be 250 nanometers hydroxyl modification silica, 18gN, N '-dinitrosopentamethlyene tetramine and
In 30g n,N-dimethylacetamide after mixing, flow back 6g fatty alcohol sodium isethionate 4.5h at 100 DEG C, obtains
Prepolymer；36g length is added into prepolymer then to exist for 1.5 microns of staple fiber and 10g formaldehyde, ultrasonic disperse 45min
Flow back 1.5h at 110 DEG C, forms gel；
Gel heat-treatment：Gel is put in the DMAC N,N' dimethyl acetamide steam that pressure is 200kPa, temperature is 180 DEG C
2.5h is set, is then cooled to room temperature, flame-retardant high-strength lightweight phenolic resin is obtained；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 80 DEG C, pressure 10MPa in temperature, punching press
The temperature of stamping die and product after punching press, is reduced to room temperature within 10min by 15min；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylate, 12g redox graphene, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamine are uniformly mixed in dimethyl acetamide, form coating emulsion, then by coating cream
Liquid is sprayed on core surfaces, after solidification, forms coating.
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Embodiment 4
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g hydroquinone, 55g acetaldehyde, 10g potassium hydroxide, the polyethylene fibre (Mw=that 10g length is 20 microns
1.5×106), 12g average diameter be 100 nanometers of hydroxyl modification silica, 6g azodicarbonamide and 2g dodecyl sulphur
In 200g dimethyl acetamide after mixing, flow back sour sodium 5h at 80 DEG C, obtains prepolymer；It is added into prepolymer
The staple fiber and 10g acetaldehyde, ultrasonic disperse 30min that 10g length is 2 microns, then flow back at 110 DEG C 2h, forms gel；
Gel heat-treatment：Gel is placed in the dimethyl acetamide steam that pressure is 150kPa, temperature is 200 DEG C
1h is then cooled to room temperature, and obtains flame-retardant high-strength lightweight phenolic resin；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 60 DEG C, pressure 25MPa in temperature, punching press
The temperature of stamping die and product after punching press, is reduced to room temperature within 10min by 20min；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylate, 12g redox graphene, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamine are uniformly mixed in dimethyl acetamide, form coating emulsion, then by coating cream
Liquid is sprayed on core surfaces, solidifies 30min at 120 DEG C, forms coating.
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Embodiment 5
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
By 100g hydroquinone, 30g formaldehyde, 30g sodium hydroxide, 30g length be 5 microns polyethylene fibre (Mw=1 ×
106), 40g average diameter be 300 nanometers of amino modified silica, 20g4,4- oxobenzenesulfonyl hydrazide and 10g dodecane
In 360g tetrahydrofuran after mixing, flow back base alcohol polyethenoxy ether sodium sulfate 3h at 120 DEG C, obtains prepolymer；To
48g length is added in prepolymer then to flow back at 90 DEG C for 300 nanometers of staple fiber and 5g formaldehyde, ultrasonic disperse 60min
2h forms gel；
Gel is placed into 3h in the tetrahydrofuran steam that pressure is 500kPa, temperature is 130 DEG C, is subsequently cooled to room
Temperature obtains flame-retardant high-strength lightweight phenolic resin；
Flame-retardant high-strength lightweight phenolic resin is placed in mold, is 140 DEG C, pressure 5MPa, punching press 2min in temperature,
After punching press, the temperature of stamping die and product is reduced to room temperature within 10min；
(2) preparation of lightweight automotive cover board：
Using aforementioned flame-retardant high-strength lightweight phenolic resin as core material, in core surfaces spraying abrasion-proof layer, spraying abrasion-proof layer
The step of include：By 100g phenolic resin, 30g butyl methacrylate, 12g redox graphene, 3g polymethyl-benzene base silicon
Oxygen alkane, 16g 2,2,4- trimethylhexane diamine are uniformly mixed in dimethyl acetamide, form coating emulsion, then by coating cream
Liquid is sprayed on core surfaces, solidifies 30min at 120 DEG C, forms coating.
The performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Comparative example 1
According to the method for embodiment 3, the difference is that, short fibre is not added in the preparation of flame-retardant high-strength lightweight phenolic resin
Dimension, the performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Comparative example 2
According to the method for embodiment 3, the difference is that, do not add long fibre in the preparation of flame-retardant high-strength lightweight phenolic resin
Dimension, the performance test results of prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Comparative example 3
According to the method for embodiment 3, the difference is that, foaming is not added in the preparation of flame-retardant high-strength lightweight phenolic resin
The performance test results of agent, prepared flame-retardant high-strength lightweight phenolic resin are as shown in table 1.
Comparative example 4
According to the method for embodiment 1, unlike, Gel heat-treatment carries out under normal pressure, and specific step is as follows；
(1) prepared by flame-retardant high-strength lightweight phenolic resin：
Gel process for preparing is the same as embodiment 1；
Gel heat-treatment：Gel is placed into 1.5h in the N-Methyl pyrrolidone steam that temperature is 200 DEG C, is then cooled down
To room temperature, flame-retardant high-strength lightweight phenolic resin is obtained；
The punch forming process of flame-retardant high-strength lightweight phenolic resin is the same as embodiment 1；
(2) the preparation method is the same as that of Example 1 for lightweight automotive cover board, the property of prepared flame-retardant high-strength lightweight phenolic resin
Energy test result is as shown in table 1.
The performance table of each flame-retardant high-strength lightweight phenolic resin in 1 Examples 1 to 5 of table and comparative example 1~4
The preferred embodiment of the present invention has been described above in detail, and still, the present invention is not limited thereto.In skill of the invention
In art conception range, can with various simple variants of the technical solution of the present invention are made, including each technical characteristic with it is any its
Its suitable method is combined, and it should also be regarded as the disclosure of the present invention for these simple variants and combination, is belonged to
Protection scope of the present invention.
Claims (10)
1. a kind of flame-retardant high-strength lightweight phenolic resin, which is characterized in that the flame-retardant high-strength lightweight is by feedstock composition system
At, on the basis of 100 parts by weight of raw material phenol, the feedstock composition：100 parts by weight of raw material phenol, 30~120 weight of raw material aldehyde
Part, 10~48 parts by weight of staple fiber, 10~30 parts by weight of long fibre, 12~40 parts by weight of improved silica, foaming agent 6~20
Parts by weight, 2~10 parts by weight of surfactant, 10~30 parts by weight of catalyst, 200~360 parts by weight of organic solvent；
The length of the staple fiber is 0.3~2 micron；The long stapled length is 5~20 microns.
2. flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein on the basis of 100 parts by weight of raw material phenol,
The feedstock composition includes：100 parts by weight of raw material phenol, 30~120 parts by weight of raw material aldehyde, 24~36 parts by weight of staple fiber, length
16~24 parts by weight of fiber, 20~36 parts by weight of improved silica, 6~20 parts by weight of foaming agent, 2~10 weight of surfactant
Measure part, 10~30 parts by weight of catalyst, 240~300 parts by weight of organic solvent.
3. flame-retardant high-strength lightweight phenolic resin according to claim 2, wherein the staple fiber and described long stapled
Mass ratio is (1~1.6)：1.
4. flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein the raw material phenol be selected from o-cresol,
M-cresol, p-cresol, at least one of hydroxymethylphenol, catechol, resorcinol and hydroquinone；
The raw material aldehyde is selected from formaldehyde, acetaldehyde, propionic aldehyde, butyraldehyde, methacrylaldehyde, cyclohexanone dimethylacetal, benzaldehyde, furfural, miscellaneous
At least one of ring aldehyde, paraformaldehyde, metaformaldehyde.
5. flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein the catalyst is selected from alkali metal hydrogen-oxygen
At least one of compound, alkaline earth metal hydroxide, carbonate and bicarbonate.
6. flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein it is brilliant that the staple fiber is selected from calcium sulfate
Palpus, alumina whisker, silicon carbide whisker, carbonization boron whisker, zirconium dioxide whisker, aluminium nitride whisker, ZnOw, magnesium sulfate
At least one of whisker, glass fibre, potassium titanate crystal whisker, magnesium sulfate crystal whisker and silicon nitride crystal whisker；The staple fiber is averaged
Diameter is 50~150nm.
7. flame-retardant high-strength lightweight phenolic resin according to claim 1 or 6, wherein the long fibre is polyethylene fiber
Dimension, weight average molecular weight Mw >=1 × 10 of the polyethylene fibre6。
8. flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein it is double that the foaming agent is selected from 4,4- oxo
Benzene sulfonyl hydrazide, azodicarbonamide, N, at least one of N '-dinitrosopentamethlyene tetramine.
9. flame-retardant high-strength lightweight phenolic resin according to claim 1, wherein the improved silica is selected from hydroxyl
At least one of improved silica, amino modified silica；
The average diameter of the improved silica is 100~300nm.
10. flame-retardant high-strength lightweight phenolic resin as claimed in any of claims 1 to 9, wherein the fire-retardant height
The surface density of strength lightweight phenolic resin is 36.25~39.14kg/m3。
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