CN110066495A - A kind of SiO2Aeroge fire-retarding epoxy resin composite material and preparation method thereof - Google Patents
A kind of SiO2Aeroge fire-retarding epoxy resin composite material and preparation method thereof Download PDFInfo
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- CN110066495A CN110066495A CN201910428529.6A CN201910428529A CN110066495A CN 110066495 A CN110066495 A CN 110066495A CN 201910428529 A CN201910428529 A CN 201910428529A CN 110066495 A CN110066495 A CN 110066495A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
Abstract
The present invention relates to a kind of SiO2Aeroge fire-retarding epoxy resin composite material and preparation method thereof belongs to the modified technical field of ethoxyline resin antiflaming.The present invention uses the SiO of high porosity2Aerogel material carries out epoxy resin flame-retardant modified.The preparation method is simple, easy post-processing and energy consumption is lower, and the fire-retarding epoxy resin composite material of preparation is non-halogen, less toxic and flame retardant effect is significant.Compared with pure epoxy resin, tensile strength and LOI value are obviously improved.
Description
Technical field
The invention belongs to the field of fire-proof technology of epoxy resin, and in particular to a kind of fire-retarding epoxy resin composite material and its
Preparation method.
Background technique
Epoxy resin is a kind of typical thermosetting resin, bonding action, mechanical property, electrical insulating property and chemical stability
Etc. haveing excellent performance, has many advantages, such as that shrinking percentage is low, machine-shaping is easy, is low in cost, led in aviation, building, military project, electronics etc.
Domain is widely used.In practical applications, ordinary epoxy resin thermal stability is poor, easy firing, and there are biggish fire hazards.To it
Carry out it is flame-retardant modified be further expansion its application range there is an urgent need to.Although traditional halogenated flame retardant hinders epoxy resin
Fuel efficiency fruit is obvious, but can generate a large amount of corrosivity and toxic gas when burning, be easy to cause secondary pollution, thus gradually
It is used by limitation.
To adapt to non-halogen, less toxicization, high efficiency, multifunction requirement, various fire-retardant new technologies obtain tremendous development,
Including fine and nanocrystallization technology, compound synergistic technology, process for modifying surface and microencapsulation technology etc..Currently, along with
The fast development of nanoscale science and technology, nano flame retardant technology has become important research direction in fire proofing field.
In terms of the relevant technologies, ZL201810487036.5 and ZL201210213076.3 proposition can be by adding carbon nanometer
Pipe is compound with epoxy resin, further improves the flame retardant property of epoxy resin, and ZL201310277964.6 is proposed titanium dioxide
Titanium nanotube is applied in epoxy resin to improve its thermal stability.ZL201610114987.9 passes through phosphorous small molecule-modified illiteracy
De- soil, which is added in epoxy resin, prepares fire retarding epoxide resin polymer.These methods are using inorganic nano-filler, step
It is cumbersome, although improving to some extent to its flame retardant property, in composite material preparation process, due to high specific surface area and work
The outer surface of jump, nanoparticle are particularly easy to form reunion.In addition lack sufficiently strong interface knot between filler and polymer chain
It closes, needs to add surfactant-based stabilizer or coupling agent modified, to increase the boundary between inorganic particle and polymeric matrix
Face compatibility.Therefore, it avoids nanofiller particle from reuniting in a polymer matrix and improves weak interfacial interaction still
It is the critical issue that the sector needs to overcome.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of non-halogen, less toxicization, high efficiency, multifunction it is new
Type fire-retarding epoxy resin composite material and preparation method thereof, the fire-retarding epoxy resin composite material have good mechanical property,
Flame retardant property.
In order to achieve the above object, the present invention adopts the following technical scheme that:
A kind of epoxy resin composite material, the component including following parts by weight: 80-100 parts of epoxy resin, SiO2Aeroge
25-65 parts, 2-5 parts of dispersing agent, 5-8 parts of curing agent, 2-4 parts of promotor, 20-30 parts of solvent.
Further, the epoxy resin is bisphenol A epoxide resin.
Further, the SiO2Aeroge drying mode includes one of constant pressure and dry and supercritical drying or two
Kind.
Further, the dispersing agent be one of stearate, calgon, neopelex or
It is a variety of.
Further, the curing agent is methyl tetrahydro phthalic anhydride.
Further, the promotor is N, N- dimethyl benzylamine.
Further, the organic solvent is one in acetone, ethyl alcohol, toluene, ethyl acetate and dimethylformamide
Kind is a variety of.
A kind of preparation method of epoxy resin composite material, comprising the following specific steps
(1)SiO2The preparation of aeroge: SiO is prepared using sol-gel method2Aeroge, selection ethyl orthosilicate are silicon
Source, formation, aging, hydrophobically modified, dry preparation SiO through wet gel2Aeroge；
(2) by the SiO of preparation2Airsetting rubber pulverizing is crossed 50-200 mesh, is mixed in proportion with epoxy resin, is added organic
Solvent, dispersing agent, stirring heating；
(3) mixture in step (2) is then down to room temperature, is proportionally added into curing agent, promotor, mechanical stirring is equal
It is even, ultrasonic disperse；
(4) mixture in step (3) is transferred to de-bubble in vacuum oven, mixture is finally cast to steel die
Middle solidification is cooled to room temperature after the completion of solidification, is demoulded to get fire-retarding epoxy resin composite material.
Further, ultrasonic disperse 10-20min in the step (3).
Further, the temperature of de-bubble is 70-90 DEG C in vacuum oven in the step (4), time 10-20min.
Further, solidification temperature is 110-200 DEG C in the step (4), time 4-6h.
Nano flame retardant epoxy resin composite material prepared by the present invention has the advantages that compared with prior art
The present invention is by the SiO of excellent heat stability2Aerogel powder is mixed with epoxy resin in proportion, is arranged in pairs or groups organic molten
Agent, dispersing agent, curing agent, promotor can get the good epoxy resin composite wood of comprehensive performance using nano flame retardant technology
Material.
The present invention is by being added SiO2Aeroge, tensile strength is increased to from 40.8MPa compared with conventional epoxies
48.3-54.7MPa, LOI value are increased to 30% or more, UL-94 from 19% and reach V-0 grades.
And the present invention is halogen-free, and effect on environment is small, and preparation process is simple, easy post-processing and energy consumption is lower.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail, but protection scope of the present invention is not limited to
Following embodiments.All within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should all wrap
Containing within protection scope of the present invention.
Embodiment 1
A kind of aeroge fire-retarding epoxy resin composite material, each component are made of raw material from the following weight: epoxy resin
80 parts, SiO225 parts of aeroge, 2 parts of stearate, 5 parts of curing agent methyl tetrahydro phthalic anhydride, accelerant N, N- dimethyl benzylamine 2
Part, 20 parts of acetone.
Its it is specific the preparation method is as follows:
Using ethyl orthosilicate as silicon source, in the mixed system of second alcohol and water, ammonia is added after hydrochloric acid catalysis hydrolyzes
SiO is prepared through wet gel formation, aging, hydrophobically modified, drying in water2Aeroge.The SiO2Aeroge smashes, and crosses 50 meshes,
By SiO225 parts of aeroge mix with 80 parts of epoxy resin, 20 parts of acetone, 2 parts of stearate are then added, and stir heating.To
The mixture is down to room temperature, is proportionally added into 5 parts of curing agent methyl tetrahydro phthalic anhydride, accelerant N, 2 parts of N- dimethyl benzylamine, mechanical
It stirs evenly, ultrasonic disperse 10-20 minutes.The above mixture is transferred in vacuum oven, the froth in vacuum 25- at 80 DEG C
35min.Mixture is cast in steel die afterwards, in 110-200 DEG C of solidification 4-6h.It is cooled to room temperature, takes off after the completion of solidification
Mould obtains fire-retarding epoxy resin composite material.
It is real that obtained fire-retarding epoxy resin composite material is subjected to extension test analysis, oxygen index (OI) test and vertical combustion
Test examination.Tensile strength 48.3MPa is measured under the rate of extension of 50mm/min；Measuring its limit oxygen index (LOI) is
30.2%, flame retardant property is obviously improved, and flame extinguishes in 5s or so when twice combustion, and UL94 reaches V-0 grades.
Embodiment 2
A kind of aeroge fire-retarding epoxy resin composite material, each component are made of raw material from the following weight: epoxy resin
90 parts, SiO245 parts of aeroge, 4 parts of calgon, 7 parts of curing agent methyl tetrahydro phthalic anhydride, accelerant N, N- dimethyl benzylamine 3
Part, 25 parts of ethyl alcohol.
Its it is specific the preparation method is as follows:
Using ethyl orthosilicate as silicon source, in the mixed system of second alcohol and water, ammonia is added after hydrochloric acid catalysis hydrolyzes
SiO is prepared through wet gel formation, aging, hydrophobically modified, drying in water2Aeroge.The SiO2Airsetting rubber pulverizing crosses 150 mesh
Sieve, by SiO245 parts of aeroge mix with 90 parts of epoxy resin, 25 parts of ethyl alcohol, 4 parts of calgon are added, and stir heating.
Object to be mixed is down to room temperature, is proportionally added into 7 parts of curing agent methyl tetrahydro phthalic anhydride, accelerant N, 3 parts of N- dimethyl benzylamine, mechanical
It stirs evenly, ultrasonic disperse 10-20 minutes.The above mixture is transferred in vacuum oven, the froth in vacuum 25- at 80 DEG C
35min.Mixture is cast in steel die afterwards, in 110-200 DEG C of solidification 4-6h.It is cooled to room temperature, takes off after the completion of solidification
Mould obtains fire-retarding epoxy resin composite material.
It is real that obtained fire-retarding epoxy resin composite material is subjected to extension test analysis, oxygen index (OI) test and vertical combustion
Test examination.Tensile strength 52.3MPa is measured under the rate of extension of 50mm/min；Measuring its limit oxygen index (LOI) is
31.8%, UL94 reach V-0 grades.
Embodiment 3
A kind of aeroge fire-retarding epoxy resin composite material of the present invention, each component are made of raw material from the following weight: ring
100 parts of oxygen resin, SiO265 parts of aeroge, 5 parts of neopelex, 8 parts of curing agent methyl tetrahydro phthalic anhydride, accelerant N,
4 parts of N- dimethyl benzylamine, 30 parts of toluene.
Its it is specific the preparation method is as follows:
Using ethyl orthosilicate as silicon source, in the mixed system of second alcohol and water, ammonia is added after hydrochloric acid catalysis hydrolyzes
SiO is prepared through wet gel formation, aging, hydrophobically modified, drying in water2Aeroge.The SiO2Airsetting rubber pulverizing crosses 200 mesh
Sieve, by SiO265 parts of aeroge mix with 100 parts of epoxy resin, 30 parts of toluene, 5 parts of neopelex are added, and stir
Mix heating.Object to be mixed is down to room temperature, is proportionally added into 8 parts of curing agent methyl tetrahydro phthalic anhydride, accelerant N, N- dimethyl benzylamine 4
Part, mechanical stirring is uniform, and ultrasonic disperse 10-20 minutes.The mixture is transferred in vacuum oven, the froth in vacuum at 80 DEG C
25-35min.Finally mixture is cast in steel die, in 110-200 DEG C of solidification 4-6h.Solidification is completed to be cooled to room temperature,
Demoulding, obtains fire-retarding epoxy resin composite material.
It is real that obtained fire-retarding epoxy resin composite material is subjected to extension test analysis, oxygen index (OI) test and vertical combustion
Test examination.Tensile strength 54.7MPa is measured under the rate of extension of 50mm/min；Measuring its limit oxygen index (LOI) is
34.9%, it burns and is put out from fire, UL-94 reaches V-0 grades, hence it is evident that improves the flame retardant property of material.
Claims (10)
1. a kind of SiO2Aeroge fire-retarding epoxy resin composite material, which is characterized in that the component including following parts by weight: epoxy
80-100 parts of resin, SiO225-65 parts of aeroge, 2-5 parts of dispersing agent, 5-8 parts of curing agent, 2-4 parts of promotor and organic solvent
20-30 parts.
2. requiring the preparation of the fire-retarding epoxy resin composite material according to right 1, it is characterised in that: including following parts by weight
Component: 80 parts of epoxy resin, SiO225 parts of aeroge, 2 parts of dispersing agent, 5 parts of curing agent, 2 parts of promotor and molten 20 parts organic.
3. requiring the preparation of the fire-retarding epoxy resin composite material according to right 1, it is characterised in that: including following parts by weight
Component: 90 parts of epoxy resin, SiO245 parts of aeroge, 4 parts of dispersing agent, 7 parts of curing agent, 3 parts of promotor and molten 25 parts organic.
4. requiring the preparation of the fire-retarding epoxy resin composite material according to right 1, it is characterised in that: including following parts by weight
Component: 100 parts of epoxy resin, SiO265 parts of aeroge, 5 parts of dispersing agent, 8 parts of curing agent, 4 parts of promotor and organic molten 30
Part.
5. requiring the preparation of the fire-retarding epoxy resin composite material according to right 1, it is characterised in that: the epoxy resin
For bisphenol A epoxide resin, the curing agent is methyl tetrahydro phthalic anhydride, and the promotor is N, N- dimethyl benzylamine.
6. requiring the preparation of the fire-retarding epoxy resin composite material according to right 1, it is characterised in that: the dispersing agent is
One of stearate, calgon, neopelex are a variety of, the organic solvent be acetone, ethyl alcohol,
One of toluene, ethyl acetate and dimethylformamide are a variety of.
7. the preparation method of fire-retarding epoxy resin composite material as claimed in any one of claims 1 to 6, which is characterized in that including
Following steps:
(1)SiO2The preparation of aeroge: aerosil is prepared using sol-gel method, selection ethyl orthosilicate is silicon
Source, formation, aging, hydrophobically modified, dry preparation SiO through wet gel2Aeroge；
(2) by the SiO of preparation2Airsetting rubber pulverizing is crossed 50-200 mesh, is mixed in proportion with epoxy resin, addition organic solvent,
Dispersing agent, and stir heating；
(3) mixture obtained in step (2) is then down to room temperature, is proportionally added into curing agent, promotor, mechanical stirring is equal
It is even, ultrasonic disperse；
(4) mixture in step (3) is transferred in vacuum oven, mixture is finally cast in steel die by de-bubble
Solidification is cooled to room temperature after the completion of solidification, is demoulded to get fire-retarding epoxy resin composite material.
8. preparation method as claimed in claim 7, which is characterized in that in the step (3), ultrasonic disperse time 10-
20min。
9. preparation method as claimed in claim 7, which is characterized in that in the step (4) in vacuum oven de-bubble temperature
Degree is 70-90 DEG C, time 10-20min.
10. preparation method as claimed in claim 7, which is characterized in that solidification temperature is 110-200 DEG C in the step (4),
Time is 4-6h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910428529.6A CN110066495A (en) | 2019-05-22 | 2019-05-22 | A kind of SiO2Aeroge fire-retarding epoxy resin composite material and preparation method thereof |
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| CN201910428529.6A CN110066495A (en) | 2019-05-22 | 2019-05-22 | A kind of SiO2Aeroge fire-retarding epoxy resin composite material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621120A (en) * | 2020-07-16 | 2020-09-04 | 贵阳学院 | Composite flame-retardant material and preparation method thereof |
| CN113201201A (en) * | 2021-04-29 | 2021-08-03 | 国网河南省电力公司周口供电公司 | Flame-retardant high-toughness carbon fiber composite material for overhead transmission conductor |
| CN113461907A (en) * | 2021-06-28 | 2021-10-01 | 中车青岛四方机车车辆股份有限公司 | Flame-retardant epoxy resin and preparation method and application thereof |
| CN116515438A (en) * | 2023-07-04 | 2023-08-01 | 建滔(广州)电子材料制造有限公司 | Anti-aging adhesive for copper-clad plate and preparation method thereof |
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| CN108424629A (en) * | 2018-01-31 | 2018-08-21 | 华南理工大学 | A kind of heat-insulating flame-retardant plastics and preparation method thereof |
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| CN108424629A (en) * | 2018-01-31 | 2018-08-21 | 华南理工大学 | A kind of heat-insulating flame-retardant plastics and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| JIUPENG ZHAO，ET AL: ""Studies on Thermal Property of Silica Aerogel/epoxy Composite"", 《MATERIALS SCIENCE FORUM》 * |
| SAEED SALIMIAN，ET AL: ""Silica Aerogel−Epoxy Nanocomposites: Understanding Epoxy Reinforcement in Terms of Aerogel Surface Chemistry and Epoxy− Silica Interface Compatibility"", 《ACS APPL. NANO MATER.》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111621120A (en) * | 2020-07-16 | 2020-09-04 | 贵阳学院 | Composite flame-retardant material and preparation method thereof |
| CN113201201A (en) * | 2021-04-29 | 2021-08-03 | 国网河南省电力公司周口供电公司 | Flame-retardant high-toughness carbon fiber composite material for overhead transmission conductor |
| CN113461907A (en) * | 2021-06-28 | 2021-10-01 | 中车青岛四方机车车辆股份有限公司 | Flame-retardant epoxy resin and preparation method and application thereof |
| CN113461907B (en) * | 2021-06-28 | 2023-11-21 | 中车青岛四方机车车辆股份有限公司 | Flame-retardant epoxy resin and preparation method and application thereof |
| CN116515438A (en) * | 2023-07-04 | 2023-08-01 | 建滔(广州)电子材料制造有限公司 | Anti-aging adhesive for copper-clad plate and preparation method thereof |
| CN116515438B (en) * | 2023-07-04 | 2023-09-15 | 建滔(广州)电子材料制造有限公司 | Anti-aging adhesive for copper-clad plate and preparation method thereof |
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Application publication date: 20190730 |
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